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

PubMed Central

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

2013-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2003-02-01

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

Surface phenomena of hydroxyapatite film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants.

PubMed

Kim, Eun-Ju; Jeong, Yong-Hoon; Choe, Han-Cheol

2013-03-01

In this study, surface phenomena of hydroxyapatite (HA) film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants have been investigated by electron beam physical vapor deposition (EB-PVD), field emission scanning electron microscope (FE-SEM), X-ray diffractometer (XRD), potentiostat and contact angle. The microstructure of Ti-29Nb-xZr alloys exhibited equiaxed structure and alpha" phase decreased, whereas beta phase increased as Zr content increased. The increment of Zr contents in HA coated nanotubular Ti-29Nb-xZr alloys showed good corrosion potential in 0.9% NaCI solution. The wettability of HA coated nanotubular surface was higher than that of non-coated samples.

An X-Ray Diffractometer for Mineralogical Analysis of Exomars Mission

NASA Astrophysics Data System (ADS)

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

2006-12-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

Structural and magnetic analysis of Cu, Co substituted NiFe{sub 2}O{sub 4} thin films

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

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

2016-05-23

In the present work we prepared NiFe{sub 2}O{sub 4}, Ni{sub 0.95}Cu{sub 0.05}Fe{sub 2}O{sub 4} and Ni{sub 0.94}Cu{sub 0.05}Co{sub 0.01} Fe{sub 2}O{sub 4} thin films by metallo-organic decomposition method (MOD) using spin coating technique. The thin films were analyzed by X-ray diffractometer (XRD) and Atomic force microscope (AFM) for structural studies. The XRD patterns confirmed the ferrite phase of thin films. From AFM, we analyzed surface morphology, calculated grain size (GS) and root mean square roughness (RMSR). Room temperature magnetic properties were investigated by vibrating sample magnetometer (VSM).

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

PubMed

Nakaya, Masafumi; Tanaka, Itaru; Muramatsu, Atsushi

2012-12-01

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

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

NASA Technical Reports Server (NTRS)

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

A temperature-controlled cell for X-ray study of liquid systems using a commercial DRON-UM1 diffractometer

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

Petrun`kin, S.P.; Garavina, E.V.; Trostin, V.N.

1995-02-01

A container (cell) and a temperature-control system have been designed enabling one to carry out x-ray diffraction study of liquid samples both at a fixed temperature and within a certain temperature range using a commercial DRON-UMl x-ray diffractometer. Special features of the cell and the materials used for it allow one to study both chemically inert and corrosive liquids.

A novel X-ray diffractometer for studies of liquid-liquid interfaces.

PubMed

Murphy, Bridget M; Greve, Matthais; Runge, Benjamin; Koops, Christian T; Elsen, Annika; Stettner, Jochim; Seeck, Oliver H; Magnussen, Olaf M

2014-01-01

The study of liquid-liquid interfaces with X-ray scattering methods requires special instrumental considerations. A dedicated liquid surface diffractometer employing a tilting double-crystal monochromator in Bragg geometry has been designed. This diffractometer allows reflectivity and grazing-incidence scattering measurements of an immobile mechanically completely decoupled liquid sample, providing high mechanical stability. The available energy range is from 6.4 to 29.4 keV, covering many important absorption edges. The instrument provides access in momentum space out to 2.54 Å(-1) in the surface normal and out to 14.8 Å(-1) in the in-plane direction at 29.4 keV. Owing to its modular design the diffractometer is also suitable for heavy apparatus such as vacuum chambers. The instrument performance is described and examples of X-ray reflectivity studies performed under in situ electrochemical control and on biochemical model systems are given.

Sample holder for X-ray diffractometry

DOEpatents

Hesch, Victor L.

1992-01-01

A sample holder for use with X-ray diffractometers with the capability to rotate the sample, as well as to adjust the position of the sample in the x, y, and z directions. Adjustment in the x direction is accomplished through loosening set screws, moving a platform, and retightening the set screws. Motion translators are used for adjustment in the y and z directions. An electric motor rotates the sample, and receives power from the diffractometer.

Doping effect on SILAR synthesized crystalline nanostructured Cu-doped ZnO thin films grown on indium tin oxide (ITO) coated glass substrates and its characterization

NASA Astrophysics Data System (ADS)

Dhaygude, H. D.; Shinde, S. K.; Velhal, Ninad B.; Takale, M. V.; Fulari, V. J.

2016-08-01

In the present study, a novel chemical route is used to synthesize the undoped and Cu-doped ZnO thin films in aqueous solution by successive ionic layer adsorption and reaction (SILAR) method. The synthesized thin films are characterized by x-ray diffractometer (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive x-ray analysis (EDAX), contact angle goniometer and UV-Vis spectroscopic techniques. XRD study shows that the prepared films are polycrystalline in nature with hexagonal crystal structure. The change in morphology for different doping is observed in the studies of FE-SEM. EDAX spectrum shows that the thin films consist of zinc, copper and oxygen elements. Contact angle goniometer is used to measure the contact angle between a liquid and a solid interface and after detection, the nature of the films is initiated from hydrophobic to hydrophilic. The optical band gap energy for direct allowed transition ranging between 1.60-2.91 eV is observed.

Facile Synthesis and Characterization of ZrO₂ Nanoparticles via Modified Co-Precipitation Method.

PubMed

Ramachandran, M; Subadevi, R; Liu, Wei-Ren; Sivakumar, M

2018-01-01

The crystalline Zirconium oxide (ZrO2) nano particles were synthesized using optimized content of Zirconium nitrate (Zr(NO3)2·3H2O) with varying KOH concentration (0.5, 1 and 1.5 M) by co-precipitation method. The thermal history of the precursor was carefully analyzed through Thermogravimetric (TG/DTA) measurement. The as prepared samples were characterized to ensure structural, functional, morphological, compositional, chemical composition and band gap by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), Laser Raman, scanning electron microscopy (SEM), High resolution Transverse Electron Microscopy (HR-TEM), X-ray photo electron spectroscopy (XPS), EDX, Photo luminescence spectroscopy (PL). The monoclinic structure with space group P21/c has been confirmed from XRD (JCPDS 89-9066). The Zr-O stretching vibration and Zr-O2-Zr bending vibrations were confirmed through FTIR analysis. The well dispersed particles with spherical morphology were confirmed through SEM and TEM analysis. The oxidation states of Zr, O and C were confirmed through XPS analysis. The oxygen vacancies and band gap of the particles were investigated through PL analysis.

La+3 effectiveness replacement on the ferrite material (Cu0,2Zn0,45LaxFe2-xO4 ) On the structural and electrical and magnetic features

NASA Astrophysics Data System (ADS)

Hussain, Farouq I.; Alaa Najem, Rusul

2018-05-01

Nano ferrite with chemical formula (Ni 0.35 Cu 0.2 Zn 0.45 Lax Fe 2-x O 4), were chemically collected utilizing sol-gel auto – combustion procedure for the values of (X=0.0, 0.025, 0.05 and 0.075). The prepared samples were calcined at (900°C) for (2h), the formation of ferrite was assured using (XRD) and (SEM) techniques. X-ray diffractometer result shows that ferrite have spinal cubic phase with a particle size ranging from (22-29 nm),the Lattice constant and density (ρx-ray) increased with La+3content while the porosity was noticed to decrease. And have been studied dielectric properties It was also observed that the value of the dielectric constant and the dielectric loss factor decreased by increasing the frequency. The increase in alternating conductivity (σa.c) was also observed with increasing frequency.

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

NASA Technical Reports Server (NTRS)

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

2015-01-01

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

X-ray diffraction studies of shocked lunar analogs

NASA Technical Reports Server (NTRS)

Hanss, R. E.

1979-01-01

The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

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

PubMed

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

2014-10-01

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

Simultaneous recovery of phosphorus and potassium as magnesium potassium phosphate from synthetic sewage sludge effluent.

PubMed

Nakao, Satoshi; Nishio, Takayuki; Kanjo, Yoshinori

2017-10-01

Bench-scale experiments were performed to investigate simultaneous recovery of phosphorus and potassium from synthetic sewage sludge effluent as crystals of magnesium potassium phosphate (MPP or struvite-(K), MgKPO 4 ·6H 2 O). The optimal pH of MPP formation was 11.5. A phosphorus level of at least 3 mM and K:P molar ratio over 3 were necessary to form MPP, which showed higher content rate of phosphorus and potassium in precipitate. MPP crystallization was confirmed by analysing the precipitates using a scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDX) apparatus and an X-ray Diffractometer (XRD). Inhibition of MPP crystallization by iron and aluminium was confirmed by precipitation experiments and SEM-EDX analysis. Potassium ratio against magnesium in precipitate decreased for iron concentrations greater than over 0.2 mM and aluminium concentrations over 0.05 mM.

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

NASA Astrophysics Data System (ADS)

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

2016-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

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.

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

NASA Astrophysics Data System (ADS)

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

2014-08-01

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

Electrical and magnetic properties of nano-sized magnesium ferrite

NASA Astrophysics Data System (ADS)

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

2015-02-01

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

Synthesis and magnetic properties of NiFe2-xSmxO4 nanopowder

NASA Astrophysics Data System (ADS)

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

2016-07-01

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

Portable X-ray powder diffractometer for the analysis of art and archaeological materials

NASA Astrophysics Data System (ADS)

Nakai, Izumi; Abe, Yoshinari

2012-02-01

Phase identification based on nondestructive analytical techniques using portable equipment is ideal for the analysis of art and archaeological objects. Portable(p)-XRF and p-Raman are very widely used for this purpose, yet p-XRD is relatively rare despite its importance for the analysis of crystalline materials. This paper overviews 6 types of p-XRD systems developed for analysis of art and archaeological materials. The characteristics of each system are compared. One of the p-XRD systems developed by the authors was brought to many museums as well as many archeological sites in Egypt and Syria to characterize the cultural heritage artifacts, e.g., amulet made of Egyptian blue, blue painted pottery, and Islamic pottery from Egypt, jade from China, variscite from Syria, a Japanese classic painting drawn by Korin Ogata, and oil paintings drawn by Taro Okamoto. Practical application data are shown to demonstrate the potential ability of the method for analysis of various art and archaeological materials.

Crystal structure and magnetic properties of Cr doped barium hexaferrite

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Supriya, Sweety; Pandey, Rabichandra; Pradhan, Lagen Kumar; Kar, Manoranjan

2018-04-01

The Cr3+ substituted BaFe12O19 has been synthesized by modified sol-gel method to tailor the magnetic anisotropy and coercivity for technological applications. Some basic studies have revealed that this substitution leads to unusual interactions among the magnetic sublattices of the M-type hexaferrite. In order to investigate these interactions, BaFe12-xCrxO19 (x = 0.0, 0.5, 1.0, 2.0, and 4.0) M-type hexaferrites were characterized by employing XRD (X-ray Diffractometer). It is confirmed that, all the samples are in nanocrystalline and single phase, no impurity has been detected within the XRD limit. The magnetic hysteresis (m-H) loops revealed the ferromagnetic nature of nanoparticles (NPs). The coercive field were increasing with the increasing Cr3+ content, but after the percolation limit it decreases. The magnetocrystalline anisotropy is increasing with the Cr3+ concentration in samples and high values of magnetocrystalline anisotropy revealed that all samples are hard magnetic materials. Magnetic hysteresis loops were analyzed using the Law of Approach to Saturation method.

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

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

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

NASA Astrophysics Data System (ADS)

Ai, Lunhong; Jiang, Jing

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

Calibration of X-Ray diffractometer by the experimental comparison method

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

Dudka, A. P., E-mail: dudka@ns.crys.ras.ru

2015-07-15

A software for calibrating an X-ray diffractometer with area detector has been developed. It is proposed to search for detector and goniometer calibration models whose parameters are reproduced in a series of measurements on a reference crystal. Reference (standard) crystals are prepared during the investigation; they should provide the agreement of structural models in repeated analyses. The technique developed has been used to calibrate Xcalibur Sapphire and Eos, Gemini Ruby (Agilent) and Apex x8 and Apex Duo (Bruker) diffractometers. The main conclusions are as follows: the calibration maps are stable for several years and can be used to improve structuralmore » results, verified CCD detectors exhibit significant inhomogeneity of the efficiency (response) function, and a Bruker goniometer introduces smaller distortions than an Agilent goniometer.« less

90-kilobar diamond-anvil high-pressure cell for use on an automatic diffractometer.

PubMed

Schiferl, D; Jamieson, J C; Lenko, J E

1978-03-01

A gasketed diamond-anvil high-pressure cell is described which can be used on a four-circle automatic diffractometer to collect x-ray intensity data from single-crystal samples subjected to truly hydrostatic pressures of over 90 kilobars. The force generating system exerts only forces normal to the diamond faces to obtain maximum reliability. A unique design allows exceptionally large open areas for maximum x-ray access and is particularly well suited for highly absorbing materials, as the x rays are not transmitted through the sample. Studies on ruby show that high-pressure crystal structure determinations may be done rapidly, reliably, and routinely with this system.

Vacuum and low oxygen pressure influence on BaFe12O19 film deposited by pulse laser deposition

NASA Astrophysics Data System (ADS)

Kumar, Pawan; Gaur, Anurag; Choudhary, R. J.

2018-05-01

BaFe12O19 hexaferrite thin films are deposited on Si (111) substrate by the pulse laser deposition (PLD) technique in high vacuum 10-6 Torr and low oxygen pressure (10 mTorr) at 650°C substrate temperature. The effects of high vacuum and low pressure on magnetic and optical properties are studied. These films are characterized by the x-ray diffractometer (XRD), SQUID-VSM magnetometer, and Photo-luminescence spectroscopy. XRD pattern reveals that the BaFe12O19 film well formed in both environments without any impurity pick. High magnetic saturazation 317 emu/cm3 and coercivity 130 Oe are observed for the film deposited in vacuum. Photoluminescence emission spectrum of BaFe12O19 film reveals that the higher intensity emission peak at ˜372 nm under the excitation wavelength of 270 nm is observed for the film grown in vacuum.

Synthesis and characterization of nickel oxide particulate annealed at different temperatures

NASA Astrophysics Data System (ADS)

Sharma, Khem Raj; Thakur, Shilpa; Negi, N. S.

2018-04-01

Nickel oxide has been synthesized by solution combustion technique. The nickel oxide ceramic was annealed at 600°C and 1000°C for 2 hours. Structural, electrical, dielectric and magnetic properties were analyzed which are strongly dependent upon the synthesis method. Structural properties were examined by X-ray diffractometer (XRD), which confirmed the purity and cubic phase of nickel oxide. XRD data reveals the increase in crystallite size and decrease in full width half maximum (FWHM) as the annealing temperature increases. Electrical conductivity is found to increase from 10-6 to 10-5 (Ω-1cm-1) after annealing. Dielectric constant is observed to increase from 26 to 175 when the annealing temperature is increased from 600°C to 1000°C. Low value of coercive field is found which shows weak ferromagnetic behavior of NiO. It is observed that all the properties of NiO particulate improve with increasing annealing temperature.

Structural and optical studies of CuO nanostructures

NASA Astrophysics Data System (ADS)

Chand, Prakash; Gaur, Anurag; Kumar, Ashavani

2014-04-01

In the present study, copper oxide (CuO) nanostructures have been synthesized at 140 °C for different aging periods, 1, 24, 48 and 96 hrs by hydrothermal method to investigate their effects on structural and optical properties. The X-ray diffractometer (XRD) pattern indicates the pure phase formation of CuO and the particle size, calculated from XRD data, has been found to be increasing from 21 to 36 nm for the samples synthesized at different aging periods. Field emission scanning electron microscope (FESEM) analysis also shows that the average diameter and length of these rectangular nano flakes increases with increasing the aging periods. Moreover Raman spectrums also confirm the phase formation of CuO. The optical band gaps calculated through UV-visible spectroscopy are found to be decreasing from 2.92 to 2.69 eV with increase in aging periods, 1 to 96 hrs, respectively.

In situ synthesis of hydroxyapatite coating by laser cladding.

PubMed

Wang, D G; Chen, C Z; Ma, J; Zhang, G

2008-10-15

HA bioceramic coatings were synthesized on titanium substrate by laser cladding using cheap calcium carbonate and calcium hydrogen phosphate. The thermodynamic condition for synthesizing HA was calculated by software Matlab 5.0, the microstructure and phase analysis of laser clad HA bioceramic coatings were studied by electron probe microanalyser (EPMA), X-ray diffractometer (XRD) and transmission electron microscopy (TEM). The theoretical results show that the Gibbs free enthalpy for the synthesis of HA phase is satisfied, and the presence of HA phase in the clad coatings was then further verified by XRD and the selected area diffraction patterns. When the laser power is 600W and the scanning speed is 3.5mm/s, the compact HA bioceramic coatings were obtained, which have cellular dendritic structure and consist of the phases of HA, alpha-Ca(2)P(2)O(7), CaO and CaTiO(3).

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

Non-platinum metal-organic framework based electro-catalyst for promoting oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Das, Dipanwita; Raut, Vrushali; Kireeti, Kota V. M. K.; Jha, Neetu

2018-04-01

We developed two non-precious Metal Organic Framework (MOF) based electrocatalysts, MOF-5 and MOF-i using solvothermal and refluxing methods. The MOFs prepared has been characterized by powder X-ray diffractometer (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM) for structural and morphological insights. SEM images reveal cubic shape for solvothermally synthesized MOF-5, whereas refluxing method leads to platelet morphology of MOF-i. The synthesized MOFs has been investigated for Oxygen Reduction Reaction (ORR) studies using Cyclic Voltammetry (CV) and Linear Sweep Voltammetry (LSV), with MOF modified Glassy Carbon (GC) as working electrode. The electrochemical data suggests higher activity of MOF-5 towards ORR compared to MOF-i.

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

PubMed Central

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

2015-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Growth and characterization of novel organic 3-Hydroxy Benzaldehyde-N-methyl 4 Stilbazolium Tosylate crystals for NLO applications.

PubMed

Jagannathan, K; Umarani, P; Ratchagar, V; Ramesh, V; Kalainathan, S

2016-01-15

The 3-Hydroxy Benzaldehyde-N-methyl 4-Stilbazolium Tosylate (3- HBST) is a new organic NLO crystal and it is a new derivative in stilbazolium tosylate family. In this work we have synthesized 3-HBST and the single crystal was grown by conventional slow cooling method. The structure and lattice parameters of the grown crystal were determined by the single crystal X-ray diffraction (XRD) technique and it is exhibiting good crystalline nature which is observed from the powder XRD. In order to check the crystalline quality the rocking curve was recorded using multi crystal X-ray diffractometer. The functional groups were identified from both FTIR and NMR spectral analyses. The π-π* and n-π* optical transition energy levels were estimated from the absorption peaks. The NLO property was confirmed by measuring relative SHG efficiency by Kurtz powder test; it shows 24 times higher SHG efficiency than that of urea. In order to test the mechanical stability the Vickers and Knoop micro hardness measurement were carried out and found that the micro hardness number decreases with increasing load. The melting point was determined from Differential Scanning Colorimetry (DSC). Copyright © 2015 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Wei, Qiong; Chen, Donghua

2009-09-01

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

Multifunctionality of nanocrystalline lanthanum ferrite

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

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

2016-05-06

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

Multifunctionality of nanocrystalline lanthanum ferrite

NASA Astrophysics Data System (ADS)

Rai, Atma; Thakur, Awalendra K.

2016-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

DTIC Science & Technology

2018-03-19

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

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

Structural and optical properties of Na-doped ZnO films

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Role of Bi3+ substitution on structural, magnetic and optical properties of cobalt spinel ferrite

NASA Astrophysics Data System (ADS)

Anjum, Safia; Sehar, Fatima; Awan, M. S.; Zia, Rehana

2016-04-01

Bismuth-doped cobalt ferrite CoBi x Fe(2- x)O4 with x = 0, 0.1,0.2, 0.3, 0.4, 0.5 have been prepared using powder metallurgy route. The structural, morphological, elemental, magnetic and optical properties have been investigated using X-ray diffractometer, Fourier transform infrared spectroscopy, scanning electron microscope, energy dispersive X-rays, vibrating sample magnetometer and ultraviolet-visible spectrometer, respectively. X-ray diffractometer analysis confirms the formation of single-phase cubic spinel structure. As the substitution of larger ionic radii Bi3+ ions increases in cobalt ferrite which is responsible to increase the lattice parameters and decrease the crystallite size. SEM micrographs revealed the spherical shape of the particles with the nonuniform grain boundaries. The saturation magnetization decreases and bandgap energy increases as the concentration of non-magnetic Bi3+ ions increases.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

NASA Technical Reports Server (NTRS)

Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

2015-01-01

The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

Highly crumpled solar reduced graphene oxide electrode for supercapacitor application

NASA Astrophysics Data System (ADS)

Mohanapriya, K.; Ahirrao, Dinesh J.; Jha, Neetu

2018-04-01

Highly crumpled solar reduced graphene oxide (CSRGO) was synthesized by simple and rapid method through freezing the solar reduced graphene oxide aqueous suspension using liquid nitrogen and used as electrode material for supercapacitor application. This electrode material was characterized by transmission electron microscope (TEM), X-Ray diffractometer (XRD) and Raman Spectroscopy techniques to understand the morphology and structure. The electrochemical performance was studied by cyclic voltammetry (CV), galvanostatic charge/discharge (CD) and electrochemical impedance spectroscopy (EIS) using 6M KOH electrolyte. The CSRGO exhibit high specifc capacitance of 210.1 F g-1 at the current density of 0.5 A g-1 and shows excellent rate capability. These features make the CSRGO material as promising electrode for high-performance supercapacitors.

Mechanical properties of Al-Cu alloy-SiC composites

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

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

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

Synthesis, characterization, and photocatalytic properties of nanocrystalline NZO thin films

NASA Astrophysics Data System (ADS)

Aryanto, D.; Hastuti, E.; Husniya, N.; Sudiro, T.; Nuryadin, B. W.

2018-03-01

Nanocrystalline Ni-doped ZnO (NZO) thin films were synthesized on glass substrate using sol-gel spin coating methods. The effect of annealing on the structural and optical properties of nanocrystalline thin film was studied using X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), UV-VIS spectrophotometry, and photoluminescence (PL). The results showed that the annealing temperature strongly influenced the physical properties of nanocrystalline NZO thin films. The photocatalytic properties of nanocrystalline NZO thin films were evaluated using an aqueous solution of Rhodamine-B. The photocatalytic activity of nanocrystalline NZO thin films increased with the increase of annealing temperature. The results indicated that the structure, morphology, and band gap energy of nanocrystalline NZO thin films played an important role in photocatalytic activity.

Morphological and spectroscopic analysis of cellulose nanocrystals extracted from oil palm empty fruit bunch fiber

NASA Astrophysics Data System (ADS)

Dasan, Y. K.; Bhat, A. H.; Faiz, A.

2015-07-01

This work evaluates the use of oil palm empty fruit bunch (OPEFB) fiber as a source of cellulose to obtain nanocrystalline cellulose (CNC) by acid hydrolysis reaction. The raw OPEFB fibers were pretreated with aqueous Sodium hydroxide at 80°C followed by bleaching treatment and further hydrolyzed with Sulphuric acid at 45°C with limited range of hydrolysis time and acid concentration. The resulting CNC's were characterized for spectroscopic, crystallographic and morphological properties using Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffractometer (XRD), Transmission Electron Microscope (TEM) and Atomic Force Microscopy (AFM). Finding of this study shows that the properties of CNC's are strongly dependent on the hydrolysis time and acid concentration.

Mechanical properties of Al-Cu alloy-SiC composites

NASA Astrophysics Data System (ADS)

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

2014-09-01

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

Remote analysis of planetary soils: X-ray diffractometer development

NASA Technical Reports Server (NTRS)

Gregory, J. C.

1973-01-01

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

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

NASA Astrophysics Data System (ADS)

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

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

Preparation and characterization of ultrafine nanoparticles of Cu doped lithium tetraborate

NASA Astrophysics Data System (ADS)

Khalilzadeh, Nasrin; Saion, Elias Bin; Mirabolghasemi, Hamed; Crouse, Karen A.; Shaari, Abdul Halim Bin; Hashim, Mansor Bin

This study details an innovative single-step thermal synthesis of nano-sized lithium tetraborate doped with 0.1 %wt copper and its characterization. The heating temperature for the synthesis of the nanoparticle material was optimized by variation between 200 and 850 °C. The optimum amount of polyvinyl pyrrolidone (PVP) the capping agent was determined to be 0.027 mol per 1 g LTB-Cu. The calcination time was 2 h. Characterization of the samples was carried out using Thermogravimetry Analysis (TGA), Derivative Thermogravimetry (DTG), Differential Scanning Calorimetry (DSC), Fourier Transform Infrared (FTIR) Spectroscopy, X-ray diffractometer (XRD), transmission electron microscopy (TEM) and Ultraviolet-Visible (UV-Vis) spectroscopy. The product was thermally stable above 450 °C. FTIR, XRD and TEM results confirmed the formation of pure nano-crystalline copper doped lithium tetraborate between 450 and 750 °C. The optical bandgap was estimated to be 5.02-6.05 eV in the presence of different amounts of PVP at various calcination temperatures.

Synthesis of Zinc Oxide Nanoparticles using Anthocyanin as a Capping Agent

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

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

NASA Technical Reports Server (NTRS)

Blake, David F.

2015-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2016-01-01

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

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

PubMed

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

2016-01-01

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

In vitro behavior of MC3T3-E1 preosteoblast with different annealing temperature titania nanotubes.

PubMed

Yu, W Q; Zhang, Y L; Jiang, X Q; Zhang, F Q

2010-10-01

Titanium oxide nanotube layers by anodization have excellent potential for dental implants because of good bone cell promotion. It is necessary to evaluate osteoblast behavior on different annealing temperature titania nanotubes for actual implant designs.  Scanning Electron Microscopy, X-Ray polycrystalline Diffractometer (XRD), X-ray photoelectron Spectroscope, and Atomic Force Microscopy (AFM) were used to characterize the different annealing temperature titania nanotubes. Confocal laser scanning microscopy, MTT, and Alizarin Red-S staining were used to evaluate the MC3T3-E1 preosteoblast behavior on different annealing temperature nanotubes.  The tubular morphology was constant when annealed at 450°C and 550°C, but collapsed when annealed at 650°C. XRD exhibited the crystal form of nanotubes after formation (amorphous), after annealing at 450°C (anatase), and after annealing at 550°C (anatase/rutile). Annealing led to the complete loss of fluorine on nanotubes at 550°C. Average surface roughness of different annealing temperature nanotubes showed no difference by AFM analysis. The proliferation and mineralization of preostoblasts cultured on anatase or anatase/rutile nanotube layers were shown to be significantly higher than smooth, amorphous nanotube layers.  Annealing can change the crystal form and composition of nanotubes. The nanotubes after annealing can promote osteoblast proliferation and mineralization in vitro. © 2010 John Wiley & Sons A/S.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Portable X-ray diffractometer equipped with XRF for archaeometry

NASA Astrophysics Data System (ADS)

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

2005-09-01

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

Diagenesis in the Murray Formation, Gale Crater, Mars

NASA Technical Reports Server (NTRS)

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

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

PubMed Central

Liu, Yanhui; Qu, Weicheng; Su, Yu

2016-01-01

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

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

PubMed

Liu, Yanhui; Qu, Weicheng; Su, Yu

2016-09-30

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

Temperature-Dependent Magnetic Response of Antiferromagnetic Doping in Cobalt Ferrite Nanostructures.

PubMed

Nairan, Adeela; Khan, Maaz; Khan, Usman; Iqbal, Munawar; Riaz, Saira; Naseem, Shahzad

2016-04-18

In this work Mn x Co 1- x Fe₂O₄ nanoparticles (NPs) were synthesized using a chemical co-precipitation method. Phase purity and structural analyses of synthesized NPs were performed by X-ray diffractometer (XRD). Transmission electron microscopy (TEM) reveals the presence of highly crystalline and narrowly-dispersed NPs with average diameter of 14 nm. The Fourier transform infrared (FTIR) spectrum was measured in the range of 400-4000 cm -1 which confirmed the formation of vibrational frequency bands associated with the entire spinel structure. Temperature-dependent magnetic properties in anti-ferromagnet (AFM) and ferromagnet (FM) structure were investigated with the aid of a physical property measurement system (PPMS). It was observed that magnetic interactions between the AFM (Mn) and FM (CoFe₂O₄) material arise below the Neel temperature of the dopant. Furthermore, hysteresis response was clearly pronounced for the enhancement in magnetic parameters by varying temperature towards absolute zero. It is shown that magnetic properties have been tuned as a function of temperature and an externally-applied field.

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

NASA Astrophysics Data System (ADS)

Koteswara Reddy, G.; Yarakkula, Kiran

2017-11-01

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

Morphological and spectroscopic analysis of cellulose nanocrystals extracted from oil palm empty fruit bunch fiber

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

Dasan, Y. K., E-mail: aamir.bhat@petronas.com.my; Bhat, A. H., E-mail: aamir.bhat@petronas.com.my; Faiz, A., E-mail: faizahmad@petronas.com.my

2015-07-22

This work evaluates the use of oil palm empty fruit bunch (OPEFB) fiber as a source of cellulose to obtain nanocrystalline cellulose (CNC) by acid hydrolysis reaction. The raw OPEFB fibers were pretreated with aqueous Sodium hydroxide at 80°C followed by bleaching treatment and further hydrolyzed with Sulphuric acid at 45°C with limited range of hydrolysis time and acid concentration. The resulting CNC’s were characterized for spectroscopic, crystallographic and morphological properties using Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffractometer (XRD), Transmission Electron Microscope (TEM) and Atomic Force Microscopy (AFM). Finding of this study shows that the properties of CNC’s aremore » strongly dependent on the hydrolysis time and acid concentration.« less

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

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

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

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

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

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.

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

NASA Astrophysics Data System (ADS)

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

2012-02-01

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

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

Sun, Cheng-Jun, E-mail: cjsun@aps.anl.gov; Brewe, Dale L.; Heald, Steve M.

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 absorptionmore » near edge structure for Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} 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.« less

Low dose radiation damage effects in silicon strip detectors

NASA Astrophysics Data System (ADS)

Wiącek, P.; Dąbrowski, W.

2016-11-01

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

Use of a priori spectral information in the measurement of x-ray flux with filtered diode arrays

DOE PAGES

Marrs, R. E.; Widmann, K.; Brown, G. V.; ...

2015-10-29

Filtered x-ray diode (XRD) arrays are often used to measure x-ray spectra vs. time from spectrally continuous x-ray sources such as hohlraums. A priori models of the incident x-ray spectrum enable a more accurate unfolding of the x-ray flux as compared to the standard technique of modifying a thermal Planckian with spectral peaks or dips at the response energy of each filtered XRD channel. A model x-ray spectrum consisting of a thermal Planckian, a Gaussian at higher energy, and (in some cases) a high energy background provides an excellent fit to XRD-array measurements of x-ray emission from laser heated hohlraums.more » If high-resolution measurements of part of the x-ray emission spectrum are available, that information can be included in the a priori model. In cases where the x-ray emission spectrum is not Planckian, candidate x-ray spectra can be allowed or excluded by fitting them to measured XRD voltages. Here, examples are presented from the filtered XRD arrays, named Dante, at the National Ignition Facility and the Laboratory for Laser Energetics.« less

[Preparation and characterization of magnetic nano-particles with radiofrequency-induced hyperthermia for cancer treatment].

PubMed

Fan, Xiangshan; Zhang, Dongsheng; Zheng, Jie; Gu, Ning; Ding, Anwei; Jia, Xiupeng; Qing, Hongyun; Jin, Liqiang; Wan, Meiling; Li, Qunhui

2006-08-01

Mn0.5Zn0.5Fe2O4 nano-particles were prepared by the chemical co-precipitation, their characteristics were observed with transmission electron microscope (TEM), X-ray diffractometer (XRD) and thermal analysis system, and etc. The temperature changes of the nano-particles of Mn0.5Zn0.5Fe2O4 and its magnetic fluid explored in radiofrequency(RF,200 KHz, 4 KW) were measured. The proliferation ratio of L929 cells cultured in soak of Mn0.5Zn0.5Fe2O4 nano-particles were observed. The experiment indicates that the magnetic particles were about 40 nm diameter in average, round, had strong magnetism, and were proved to be consistent with the standard data of chart of XRD. Its magnetic fluid exposed to RF could be heated up to temperature range from 40 degrees C to 51 degrees C due to the amount of the magnetic nano-particles and intensity of the alternating magnetic field. Magnetic nano-particles were found to have no obvious cytotoxicity to L929 cells.

Influence of Iron Doping on Structural, Optical and Magnetic Properties of TiO2 Nanoparticles

NASA Astrophysics Data System (ADS)

Zahid, R.; Manzoor, M.; Rafiq, A.; Ikram, M.; Nafees, M.; Butt, A. R.; Hussain, S. G.; Ali, S.

2018-05-01

In this study, various concentrations of Fe doped TiO2 nanoparticles have been successfully synthesized using the sol-gel method. A variety of characterization techniques as ultra-violet visible (UV-Vis) spectroscopy, X-ray diffractometer (XRD), vibrating sample magnetometry (VSM) and field emission scanning electron microscopy (FESEM) were employed to analyze the prepared nanopowders. XRD measurement confirmed the substitution of Fe ion without disturbing the tetragonal crystal system of TiO2. The crystallite size was found to decrease and lattice strain increases upon doping estimated by Williamson Hall plot. Furthermore, the average grain size calculated by FESEM found was between 10 and 30 nm for pure and doped TiO2. UV-Vis spectroscopy showed an increase in absorption accompanied red shift and increase in band gap energies from 3.36 to 3.62 eV with the addition of Fe. The FTIR spectroscopy was employed to confirm the presence of functional groups in the fabricated nanopowders. Upon mixing the saturation magnetization (Ms) varying from (2.12 to 1.51)10-2 emu/g was observed.

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

NASA Astrophysics Data System (ADS)

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

2011-09-01

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

Effect of annealing temperature on physical properties of solution processed nickel oxide thin films

NASA Astrophysics Data System (ADS)

Sahoo, Pooja; Thangavel, R.

2018-05-01

In this report, NiO thin films were prepared at different annealing temperatures from nickel acetate precursor by sol-gel spin coating method. These films were characterized by different analytical techniques to obtain their structural, optical morphological and electrical properties using X-ray diffractometer (XRD), Field emission scanning electron microscopy (FESEM), UV-Vis NIR double beam spectrophotometer and Keithley 2450 source meter respectively. FESEM images clearly indicates the formation of a homogenous and porous films. Due to their porosity, they can be used in sensing applications. The optical absorption spectra elucidated that the films are highly transparent and have a suitable band gap which are in similar agreement with earlier reports. The current enhancement under illumination shows the suitability of nanostructured NiO thin films in its application in photovoltaics.

Synthesis, Characterization and Comparative Luminescence Studies of Rare-Earth-Doped Gd2O3 Nanoparticles

NASA Astrophysics Data System (ADS)

Pyngrope, D.; Singh, L. R.; Prasad, A. I.; Bora, A.

2018-04-01

A facile direct precipitation method was used for the synthesis of luminescence nanomaterial. Gd2O3 doped with rare earth element Eu3+ is synthesized by polyol route. The synthesized nanoparticles show their characteristic red emission. The nanoparticles are characterized by x-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and photoluminescence (PL) study. The synthesized nanoparticles are spherical particles with 30 nm size. The photoluminescence studies show the characteristic Eu3+ red emission. The PL study shows the intensity of the magnetic dipole transition ( 5 D0 \\to 7 F1 ) at 592 nm compared to that of the electronic dipole transition ( 5 D0 \\to 7 F2 ) at 615 nm. The nanomaterials can show significant application in various display devices and biomedical applications for tracking.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Significant enhancement in volumetric and gravimetric capacitance of Cu-TiO2/PPY composite for supercapacitor application

NASA Astrophysics Data System (ADS)

Purty, B.; Choudhary, R. B.

2018-04-01

Copper doped titanium dioxide-polypyrrole (Cu-TiO2/PPY) composite was successfully synthesized via chemical oxidative in-situ polymerization process. The structural and morphological properties of Cu-TiO2/PPY composite were investigated using X-ray diffractometer (XRD), field emission electron microscopy (FESEM) and transmission electron microscopy(TEM) techniques. The electrochemical properties of as-synthesized composite were studied using cyclic voltammetry (CV), galvanostatic charge discharge (GCD) and electrochemical impedance spectroscopic (EIS) techniques. The novel Cu-TiO2/PPY composite showed enhanced volumetric capacitance ˜714 F cm-1 and gravimetric capacitance ˜674 F g-1 at 1 A g-1. In addition an excellent coulombic efficiency and comparabley low charge transfer resistance than pure PPY suggests improved supercapacitive performance of Cu-TiO2/PPY composite as an electrode material.

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

DOE PAGES

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

2016-01-05

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

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

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Preparation, Structural and Dielectric Behaviors of CoxMn1-xMn2O4 (0 ≤ x ≤ 1) Nanoparticles

NASA Astrophysics Data System (ADS)

Taufiq, A.; Muzammil, M.; Fuad, A.; Hidayat, N.; Sunaryono, S.; Mufti, N.; Hidayat, A.; Diantoro, M.; Munasir, M.

2018-05-01

Cobalt-manganese oxide nanoparticles become remarkable metal oxides due to their physical characters, for example, their electrical properties. In this paper, we report the synthesis of Co x Mn1-x Mn2O4 (0 ≤ x ≤ 1) nanoparticles via a precipitation method. The structural and dielectric properties were investigated by means of X-ray diffractometer (XRD) and LCR-meter. From the data analysis, it was found that the Co x Mn1-x Mn2O4 particles structured spinel cubic with the particle size ranging from 22.7 to 28.6 nm. Increasing Co2+ ions led to declining lattice and crystal volume of the Co x Mn1-x Mn2O4 nanoparticles. Such phenomenon was originated from the substitution process of Co2+ ions that change the metal construction both at the octahedral and tetrahedral sites. Furthermore, the Co2+ ion substitution resulted in an increase in the dielectric properties of the Co x Mn1-x Mn2O4 nanoparticles regarding with dipole moment. Interestingly, the increase was also influenced by reducing the particle size and crystal volume of the Co x Mn1-x Mn2O4 nanoparticles.

Titration of a Solid Acid Monitored by X-Ray Diffraction

ERIC Educational Resources Information Center

Dungey, Keenan E.; Epstein, Paul

2007-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2015-04-01

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

Effect of Sc{sup 3+} on structural and magnetic properties of Mn-Zn nano ferrites

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

Angadi, Jagadeesha V.; Matteppanavar, Shidaling; Srinatha, N.

2016-05-23

In the present investigation, for the first time, we report on the effect of Sc{sup 3+} on the structural and magnetic properties of Mn{sub 0.5}Zn{sub 0.5}Sc{sub y}Fe{sub 2-y}O{sub 4} (y = 0.01, 0.03 and 0.05) nanoferrites synthesized by solution combustion method using the mixture of fuels. As synthesized powders were characterized for the detailed structural analysis by X-ray diffractometer (XRD), Fourier transmission infrared spectroscopy (FTIR) and room temperature magnetic properties by using vibrating sample magnetometer (VSM). The results of XRD and FTIR confirm that the formation of nano crystalline, single-phased Mn-Zn ferrite with cubic spinel structure belongs to Fd-3m spacemore » group. The room temperature magnetic studies shows that, the saturation magnetization (M{sub S}), remanence magnetization (M{sub R}) and magnetic moment (η{sub B}), magnetic particle size (D{sub m}) have found to increase with Sc{sup 3+} ion concentration up to x = 0.3 and then decrease. The values of αY-K and the magnetic particle size (D{sub m}) are found to be in the range of 68-75° and 10-19 nm respectively, with Sc{sup 3+} concentration.« less

Green synthesis of Copper nanoparticle using ionic liquid-based extraction from Polygonum minus and their applications.

PubMed

Ullah, Habib; Wilfred, Cecilia Devi; Shaharun, Maizatul Shima

2018-06-06

The present work reports the extraction of phenolic compounds from Polygonum minus using ionic liquid as extracting solvent. In this work, 1-Butyl-3-methylimidazolium hydrogen sulfate [BMIM][HSO 4 ] was used for the extraction of bioactive compounds. Accordingly, ionic liquids based microwave-assisted extraction treatment for separating of bioactive compounds from polygonum minus was first performed in the present study. The results obtained in this work have high extraction yield in comparison with conventional solvent. UV/Vis results showed that microwave synthesis was fast, well dispersed and nanosized copper nanoparticle (CuNPs) in comparison with conventional synthesis. CuNPs was characterized by X-Rays diffractometer (XRD), Fourier transform infrared (FTIR), dynamic light scattering (DLS), field emission scanning electron microscopy combined with energy dispersive x-rays (FESEM-EDX), and thermogravimetric analysis (TGA). All the instrumental analyses confirmed the particles were nanosized. Furthermore, the antibacterial activity of as-synthesized CuNPs showed effective inhibitory zone against three different bacteria. The photocatalytic degradation of copper nanoparticles was studied using methylene blue (MB) and methyl orange (MO) dyes under UV light and degraded 99.9% within short time 8 and 7 minutes.

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

PubMed

Verma, Tarkeshwari; Agrawal, Sadhana

2018-01-01

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

Copper diffusion in Ti Si N layers formed by inductively coupled plasma implantation

NASA Astrophysics Data System (ADS)

Ee, Y. C.; Chen, Z.; Law, S. B.; Xu, S.; Yakovlev, N. L.; Lai, M. Y.

2006-11-01

Ternary Ti-Si-N refractory barrier films of 15 nm thick was prepared by low frequency, high density, inductively coupled plasma implantation of N into TixSiy substrate. This leads to the formation of Ti-N and Si-N compounds in the ternary film. Diffusion of copper in the barrier layer after annealing treatment at various temperatures was investigated using time-of-flight secondary ion mass spectrometer (ToF-SIMS) depth profiling, X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) and sheet resistance measurement. The current study found that barrier failure did not occur until 650 °C annealing for 30 min. The failure occurs by the diffusion of copper into the Ti-Si-N film to form Cu-Ti and Cu-N compounds. FESEM surface morphology and EDX show that copper compounds were formed on the ridge areas of the Ti-Si-N film. The sheet resistance verifies the diffusion of Cu into the Ti-Si-N film; there is a sudden drop in the resistance with Cu compound formation. This finding provides a simple and effective method of monitoring Cu diffusion in TiN-based diffusion barriers.

Corrosion Behavior and Microhardness of Ni-P-SiO2-Al2O3 Nano-composite Coatings on Magnesium Alloy

NASA Astrophysics Data System (ADS)

Sadreddini, S.; Rahemi Ardakani, S.; Rassaee, H.

2017-05-01

In the present work, nano-composites of Ni-P-SiO2-Al2O3 were coated on AZ91HP magnesium alloy. The surface morphology of the nano-composite coating was studied by field emission scanning electron microscopy (FESEM). The amount of SiO2 in the coating was determined by energy-dispersive analysis of x-ray (EDX), and the crystalline structure of the coating was examined by x-ray diffractometer (XRD). All the experiments concerning the corrosion behavior of the coating carried out in 3.5 wt.% NaCl solution and evaluated by electrochemical impedance spectroscopy (EIS) and polarization technique. The results showed that an incorporation of SiO2 and Al2O3 in Ni-P coating at the SiO2 concentration of 10 g/Land 14 g/LAl2O3 led to the lowest corrosion rate ( i corr = 1.3 µA/cm2), the most positive E corr and maximum microhardness (496 VH). Furthermore, Ni-P-SiO2-Al2O3 nano-composite coating possesses less porosity than that in Ni-P coating, resulting in improving corrosion resistance.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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

ERIC Educational Resources Information Center

Ouseph, P. J.; And Others

1982-01-01

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

An X-ray diffractometer using mirage diffraction

PubMed Central

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

2014-01-01

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

Solvothermal synthesis of nickel-tungsten sulfides for 2-propanol dehydration.

PubMed

Gómez-Gutiérrez, Claudia M; Luque, P A; Guerra-Rivas, G; López-Sánchez, J A; Armenta, M A; Quintana, J M; Olivas, A

2015-01-01

The bimetallic nickel-tungsten catalysts were prepared via solvothermal method. The X-ray Diffractometer (XRD) analysis revealed that the corresponding peaks at 14°, 34°, and 58° were for tungsten disulfide (WS2 ) hexagonal phase. The catalysts displayed different crystalline phase with nickel addition, and as an effect the WS2 surface area decreased from 74.7 to 2.0 m(2) g(--1) . In this sense, high-resolution transmission electron microscopy (HRTEM) showed the layers set in direction (002) with an onion-like morphology, and in the center of the particles there is a large amount of nickel contained with 6-8 layers covering it. The catalytic dehydration of 2-propanol was selective to propene in 100% at 250 °C for the sample with 0.7 of atomic ratio of Ni/Ni + W. © Wiley Periodicals, Inc.

Investigation of structural, optical and electrical properties of Co3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Bhargava, Richa; Khan, Shakeel; Ahmad, Naseem; Ansari, Mohd Mohsin Nizam

2018-05-01

In the current work, we report the synthesis of Cobalt oxide (Co3O4) NPs (NPs) by co-precipitation method. The structural analysis was confirmed by using X-ray diffractometer (XRD) which shows that the Co3O4 NPs have cubic phase. The average crystallite size and the lattice parameter were calculated for Co3O4 NPs. The functional groups of the as-synthesized sample were examined by Fourier transform infrared spectroscopy (FTIR). The optical band gap of Co3O4 NPs was estimated by using UV diffuse reflectance spectroscopy and the Band gap was evaluated by using Tauc relation. The temperature dependence of dielectric constant and dielectric loss were studied over a range of temperature 50-300 °C. The DC electrical resistivity of Co3O4 NPs shows a semiconducting behaviour and the value of activation energy was calculated by using Arrhenius equation.

The effect of calcination temperature on the formation and magnetic properties of ZnMn2O4 spinel

NASA Astrophysics Data System (ADS)

Hermanto, B.; Ciswandi; Afriani, F.; Aryanto, D.; Sudiro, T.

2018-03-01

The spinel based on transition-metal oxides has a typical composition of AB2O4. In this study, the ZnMn2O4 spinel was synthesized using a powder metallurgy technique. The Zn and Mn metallic powders with an atomic ratio of 1:2 were mechanically alloyed for 3 hours in aqueous solution. The mixed powder was then calcined in a muffle furnace at elevated temperature of 400, 500 and 600 °C. The X-ray Diffractometer (XRD) was used to evaluate the formation of a ZnMn2O4 spinel structure. The magnetic properties of the sample at varying calcination temperatures were characterized by a Vibrating Sample Magnetometer (VSM). The results show that the fraction of ZnMn2O4 spinel formation increases with the increase of calcination temperature. The calcination temperature also affects the magnetic properties of the samples.

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

PubMed

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

2016-02-01

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

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

PubMed

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

2014-01-01

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

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

PubMed

Hafez, Hoda S; El-Fadaly, E

2012-09-01

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

Remote X-Ray Diffraction and X-Ray Fluorescence Analysis on Planetary Surfaces

NASA Technical Reports Server (NTRS)

Blake, David F.; DeVincenzi, D. (Technical Monitor)

1999-01-01

The legacy of planetary X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) began in 1960 when W. Parish proposed an XRD instrument for deployment on the moon. The instrument was built and flight qualified, but the Lunar XRD program was cancelled shortly before the first human landing in 1969. XRF chemical data have been collected in situ by surface landers on Mars (Viking 1 & 2, Pathfinder) and Venus (Venera 13 & 14). These highly successful experiments provide critical constraints on our current understanding of surface processes and planetary evolution. However, the mineralogy, which is more critical to planetary surface science than simple chemical analysis, will remain unknown or will at best be imprecisely constrained until X-ray diffraction (XRD) data are collected. Recent progress in X-ray detector technology allows the consideration of simultaneous XRD (mineralogic analysis) and high-precision XRF (elemental analysis) in systems miniaturized to the point where they can be mounted on fixed landers or small robotic rovers. There is a variety of potential targets for XRD/XRF equipped landers within the solar system, the most compelling of which are the poles of the moon, the southern highlands of Mars and Europa.

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

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

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

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

Diagnosing x-ray power and energy of tungsten wire array z-pinch with a flat spectral response x-ray diode

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

Wang, Kun-lun; Ren, Xiao-dong; Huang, Xian-bin, E-mail: caephxb2003@aliyun.com

2015-11-15

Fast z-pinch is a very efficient way of converting electromagnetic energy to radiation. With an 8-10 MA current on primary test stand facility, about 1 MJ electromagnetic energy is delivered to vacuum chamber, which heats z-pinch plasma to radiate soft x-ray. To develop a pulsed high power x-ray source, we studied the applicability of diagnosing x-ray power from tungsten wire array z-pinch with a flat spectral response x-ray diode (FSR-XRD). The detector was originally developed to diagnose radiation of a hohlraum in SG-III prototype laser facility. It utilized a gold cathode XRD and a specially configured compound gold filter tomore » yield a nearly flat spectral response in photon energy range of 0.1-4 keV. In practice, it was critical to avoid surface contamination of gold cathode. It is illustrated that an exposure of an XRD to multiple shots caused a significant change of response. Thus, in diagnosing x-ray power and energy, we used each XRD in only one shot after calibration. In a shot serial, output of FSR-XRD was compared with output of a nickel bolometer. In these shots, the outputs agreed with each other within their uncertainties which were about 12% for FSR-XRD and about 15% for bolometer. Moreover, the ratios between the FSR-XRD and the bolometer among different shots were explored. In 8 shots, the standard deviation of the ratio was 6%. It is comparable to XRD response change of 7%.« less

Study the target effect on the structural, surface and optical properties of TiO2 thin film fabricated by RF sputtering method

NASA Astrophysics Data System (ADS)

Vyas, Sumit; Tiwary, Rohit; Shubham, Kumar; Chakrabarti, P.

2015-04-01

The effect of target (Ti metal target and TiO2 target) on Titanium Dioxide (TiO2) thin films grown on ITO coated glass substrate by RF magnetron sputtering has been investigated. A comparative study of both the films was done in respect of crystalline structure, surface morphology and optical properties by using X-ray diffractometer (XRD), Atomic Force Microscopy (AFM) studies and ellipsometric measurements. The XRD results confirmed the crystalline structure and indicated that the deposited films have the intensities of anatase phase. The surface morphology and roughness values indicated that the film using Ti metal target has a smoother surface and densely packed with grains as compared to films obtained using TiO2 target. A high transmission in the visible region, and direct band gap of 3.67 eV and 3.75 eV for films derived by using Ti metal and TiO2 target respectively and indirect bandgap of 3.39 eV for the films derived from both the targets (Ti metal and TiO2 target) were observed by the ellipsometric measurements.

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

NASA Astrophysics Data System (ADS)

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

2014-02-01

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

Hidroxyapatite Coating on CoCrMo Alloy Titanium Nitride Coated Using Biomimetic Method

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

Unusual effect of water vapor pressure on dehydration of dibasic calcium phosphate dihydrate.

PubMed

Kaushal, Aditya M; Vangala, Venu R; Suryanarayanan, Raj

2011-04-01

Dibasic calcium phosphate occurs as an anhydrate (DCPA; CaHPO₄) and as a dihydrate (DCPD; CaHPO₄•2H₂O). Our objective was to investigate the unusual behavior of these phases. Dibasic calcium phosphate dihydrate was dehydrated in a (i) differential scanning calorimeter (DSC) in different pan configurations; (ii) variable-temperature X-ray diffractometer (XRD) at atmospheric and under reduced pressure, and in sealed capillaries; and (iii) water vapor sorption analyzer at varying temperature and humidity conditions. Dehydration was complete by 210°C in an open DSC pan and under atmospheric pressure in the XRD. Unlike "conventional" hydrates, the dehydration of DCPD was facilitated in the presence of water vapor. Variable-temperature XRD in a sealed capillary and DSC in a hermetic pan with pinhole caused complete dehydration by 100°C and 140°C, respectively. Under reduced pressure, conversion to the anhydrate was incomplete even at 300°C. The increase in dehydration rate with increase in water vapor pressure has been explained by the Smith-Topley effect. Under "dry" conditions, a coating of poorly crystalline product is believed to form on the surface of particles and act as a barrier to further dehydration. However, in the presence of water vapor, recrystallization occurs, creating cracks and channels and facilitating continued dehydration. Copyright © 2010 Wiley-Liss, Inc.

Structural studies of ZnO nanostructures by varying the deposition parameters

NASA Astrophysics Data System (ADS)

Yunus, S. H. A.; Sahdan, M. Z.; Ichimura, M.; Supee, A.; Rahim, S.

2017-01-01

The effect of Zinc Oxide (ZnO) thin film on the growth of ZnO nanorods (NRs) was investigated. The structures of ZnO NRs were synthesized by chemical bath deposition (CBD) method in aqueous solution of N2O6Zn.6H2O and C6H12N4 at 90°C of deposition temperature. One of the ZnO NRs samples was deposited on a ZnO seed layer coated on a glass substrate to investigate the properties of ZnO NRs without receiving effect of other materials. Next, for diode application, the ZnO NRs was deposited on tin monosulfide (SnS) coated on indium-tin-oxide (ITO) coated glass substrate (SnS/ITO). The next, the ZnO structural properties were studied from surface morphology, X-ray diffractometer (XRD) spectra, and chemical composition by using field emission scanning electron microscope (FESEM), XRD and energy dispersive X-ray Spectroscopy (EDX). The growth of ZnO NRs on ZnO seed layer was investigated by ZnO seed layer condition while the growth of ZnO NRs on SnS/ITO was investigated by deposition time and deposition temperature parameters. From FESEM images, aligned ZnO NRs were obtained, and the diameters of ZnO NRs were 0.024-3.94 µm. The SnS thin film was affected by the diameter of ZnO NRs which are the ZnO NRs grow on SnS thin films has a larger diameter compared to ZnO NRs grow on ZnO seed layer. Besides that, all of ZnO peaks observed from XRD corresponding to the wurzite structure and preferentially oriented along the c-axis. In addition, EDX shows a high composition of zinc (Zn) and oxygen (O) signals, which indicated that the NRs are indeed made up of Zn and O.

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

PubMed

Benea, Lidia; Celis, Jean-Pierre

2016-04-06

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

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

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

Properties of CoO doped in Glasses Prepared from Rice Hush Fly Ash in Thailand

NASA Astrophysics Data System (ADS)

Ruangtaweep, Y.; Kaewkhao, J.; Kirdsiri, K.; Kedkaew, C.; Limsuwan, P.

2011-10-01

In this work, properties of glass from local rice husk ash (RHA) in Thailand have been investigated. RHA was sintered in different temperature. Compositions and phases of RHA were analyzed by energy dispersive x-ray fluorescence spectrometer (EDXRF) and X-ray diffractometer (XRD). The glasses were melt from RHA in formula 20 Na2O : 1.0 Al2O3 : 13 B2O3 : 6.3 CaO : 0.2 Sb2O3 : 4.5 BaO : 55SiO2 (using RHA as a SiO2 source) The density values of all RHA glasses are comparable and larger than glass from pure SiO2 under same glass formula and preparing condition. These results are corresponding with refractive index values. The RHA glasses showing colorless with absorption edge in ultraviolet region were obtained. The dark blue color glasses were melted from RHA with different CoO concentration. From this part, not found to be the relation of density and refractive index of glass with CoO concentration in glass matrix. From absorption spectra, the absorption peak were appeared around 600 nm, and peak intensity are increased, with increase CoO, correspond to 4A2(4F) → 4T1(4P) state of Co2+ in tetrahedral symmetry.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

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

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

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

2012-10-15

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

XRD monitoring of α self-irradiation in uranium-americium mixed oxides.

PubMed

Horlait, Denis; Lebreton, Florent; Roussel, Pascal; Delahaye, Thibaud

2013-12-16

The structural evolution under (241)Am self-irradiation of U(1-x)Am(x)O(2±δ) transmutation fuels (with x ≤ 0.5) was studied by X-ray diffraction (XRD). Samples first underwent a preliminary heat treatment performed under a reducing atmosphere (Ar/H2(4%)) aiming to recover the previously accumulated structural defects. Over all measurements (carried out over up to a full year and for integrated doses up to 1.5 × 10(18) α-decay events·g(-1)), only fluorite U(1-x)Am(x)O(2±δ) solid solutions were observed. Within a few days after the end of the heat treatment, each of the five studied samples was slowly oxidized as a consequence of their move to air atmosphere, which is evidenced by XRD by an initial sharp decrease of the unit cell parameter. For the compounds with x ≤ 0.15, this oxidation occurred without any phase transitions, but for U0.6Am0.4O(2±δ) and U0.5Am0.5O(2±δ), this process is accompanied by a transition from a first fluorite solid solution to a second oxidized one, as the latter is thermodynamically stable in ambient conditions. In the meantime and after the oxidation process, (241)Am α self-irradiation caused a structural swelling up to ∼0.8 vol %, independently of the sample composition. The kinetic constants of swelling were also determined by regression of experimental data and are, as expected, dependent on x and thus on the dose rate. The normalization of these kinetic constants by sample α-activity, however, leads to very close swelling rates among the samples. Finally, evolutions of microstrain and crystallite size were also monitored, but for the considered dose rates and cumulated doses, α self-irradiation was found, within the limits of the diffractometer used, to have almost no impact on these characteristics. Microstrain was found to be influenced instead by the americium content in the materials (i.e., by the impurities associated with americium starting material and the increase of cationic charge heterogeneity with increasing americium content).

Fundamental Parameters Line Profile Fitting in Laboratory Diffractometers

PubMed Central

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

2004-01-01

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

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

DTIC Science & Technology

1987-09-01

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

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

PubMed Central

Anfinrud, Philip

2010-01-01

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

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

PubMed

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

2010-04-20

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

Band alignment of atomic layer deposited MgO/Zn0.8Al0.2O heterointerface determined by charge corrected X-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Yan, Baojun; Liu, Shulin; Yang, Yuzhen; Heng, Yuekun

2016-05-01

Pure magnesium (MgO) and zinc oxide doped with aluminum oxide (Zn0.8Al0.2O) were prepared via atomic layer deposition. We have studied the structure and band gap of bulk Zn0.8Al0.2O material by X-ray diffractometer (XRD) and Tauc method, and the band offsets and alignment of atomic layer deposited MgO/Zn0.8Al0.2O heterointerface were investigated systematically using X-ray photoelectron spectroscopy (XPS) in this study. Different methodologies, such as neutralizing electron gun, the use of C 1s peak recalibration and zero charging method, were applied to recover the actual position of the core levels in insulator materials which were easily influenced by differential charging phenomena. Schematic band alignment diagram, valence band offset (ΔEV) and conduction band offset (ΔEC) for the interface of the MgO/Zn0.8Al0.2O heterostructure have been constructed. An accurate value of ΔEV = 0.72 ± 0.11 eV was obtained from various combinations of core levels of heterojunction with varied MgO thickness. Given the experimental band gaps of 7.83 eV for MgO and 5.29 eV for Zn0.8Al0.2O, a type-II heterojunction with a ΔEC of 3.26 ± 0.11 eV was found. Band offsets and alignment studies of these heterojunctions are important for gaining deep consideration to the design of various optoelectronic devices based on such heterointerface.

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

NASA Astrophysics Data System (ADS)

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

2016-01-01

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

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

PubMed

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

2015-01-01

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

Unified Theory for Decoding the Signals from X-Ray Florescence and X-Ray Diffraction of Mixtures.

PubMed

Chung, Frank H

2017-05-01

For research and development or for solving technical problems, we often need to know the chemical composition of an unknown mixture, which is coded and stored in the signals of its X-ray fluorescence (XRF) and X-ray diffraction (XRD). X-ray fluorescence gives chemical elements, whereas XRD gives chemical compounds. The major problem in XRF and XRD analyses is the complex matrix effect. The conventional technique to deal with the matrix effect is to construct empirical calibration lines with standards for each element or compound sought, which is tedious and time-consuming. A unified theory of quantitative XRF analysis is presented here. The idea is to cancel the matrix effect mathematically. It turns out that the decoding equation for quantitative XRF analysis is identical to that for quantitative XRD analysis although the physics of XRD and XRF are fundamentally different. The XRD work has been published and practiced worldwide. The unified theory derives a new intensity-concentration equation of XRF, which is free from the matrix effect and valid for a wide range of concentrations. The linear decoding equation establishes a constant slope for each element sought, hence eliminating the work on calibration lines. The simple linear decoding equation has been verified by 18 experiments.

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

PubMed Central

Zhang, Chenyang; Wang, Jincheng

2017-01-01

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

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

NASA Astrophysics Data System (ADS)

Cerchier, Pietrogiovanni; Dabalà, Manuele; Brunelli, Katya

2017-09-01

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

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NASA Technical Reports Server (NTRS)

Singer, J.; Fielder, W. L.; Garlick, R. G.; Negas, T.

1987-01-01

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Organic Field Effect Transistor Using Amorphous Fluoropolymer as Gate Insulating Film

NASA Astrophysics Data System (ADS)

Kitajima, Yosuke; Kojima, Kenzo; Mizutani, Teruyoshi; Ochiai, Shizuyasu

Organic field effect transistors are fabricated by the active layer of Regioregular poly (3-hexylthiophene-2,5-diy)(P3HT) thin film. CYTOP thin film made from Amorphous Fluoropolymer and fabricated by spin-coating is adopted to a gate dielectric layer on Polyethylenenaphthalate (PEN) thin film that is the substrate of an organic field effect transistor. The surface morphology and molecular orientation of P3HT thin films is observed by atomic force microscope (AFM) and X-Ray diffractometer (XRD). Grains are observed on the CYTOP thin film via an AFM image and the P3HT molecule is oriented perpendicularly on the CYTOP thin film. Based on the performance of the organic field effect transistor, the carrier mobility is 0.092 cm2/Vs, the ON/OFF ratio is 7, and the threshold voltage is -12 V. The ON/OFF ratio is relatively low and to improve On/Off ratio, the CYTOP/Polyimide double gate insulating layer is adopted to OFET.

Correlation of film thickness to optical band gap of Sol-gel derived Ba0.9Gd0.1TiO3 thin films for optoelectronic applications

NASA Astrophysics Data System (ADS)

Teh, Yen Chin; Saif, Ala'eddin A.; Azhar Zahid Jamal, Zul; Poopalan, Prabakaran

2017-11-01

Ba0.9Gd0.1TiO3 thin films have been fabricated on SiO2/Si and fused silica by sol-gel method. The films are prepared through a spin coating process and annealed at 900 °C to obtain crystallized films. The effect of film thickness on the microstructure and optical band gap has been investigated using X-ray diffractometer, atomic force microscope and ultraviolet-visible spectroscopy, respectively. XRD patterns confirm that the films crystallized with tetragonal phase perovskite structure. The films surface morphology is analysed through amplitude parameter analysis to find out that the grain size and surface roughness are increased with the increase of films thickness. The transmittance and absorbance spectra reveal that all films exhibit high absorption in UV region. The evaluated optical band gap is obtained in the range of 3.67 - 3.78 eV and is found to be decreased as the thickness increase.

The influences of target properties and deposition times on pulsed laser deposited hydroxyapatite films

NASA Astrophysics Data System (ADS)

Bao, Quanhe; Chen, Chuanzhong; Wang, Diangang; Liu, Junming

2008-11-01

Hydroxyapatite films were produced by pulsed laser deposition from three kinds of hydroxyapatite targets and with different deposition times. A JXA-8800R electron probe microanalyzer (EPMA) with a Link ISIS300 energy spectrum analyzer was used to give the secondary electron image (SE) and determine the element composition of the films. The phases of thin film were analyzed by a D/max-γc X-ray diffractometer (XRD). The Fourier-transform infrared spectroscopy (FT-IR) was used to characterize the hydroxyl, phosphate and other functional groups. The results show that deposited films were amorphous which mainly composed of droplet-like particles and vibration of PO 43- groups. With the target sintering temperature deposition times increasing, the density of droplets is decreased. While with deposition times increasing, the density of droplets is increased. With the target sintering temperature and deposition time increasing, the ratio of Ca/P is increasing and higher than that of theoretical value of HA.

Advance concepts for the conversion of syngas liquids. Quarterly report {number_sign}5, October 30, 1995--January 31, 1996

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

Szostak, R.; Ingram, C.

Research efforts for the report period have been focused on the characterization of catalyst samples, mainly by ion exchange and spectroscopic techniques. Other activities included the preparation of more variants of the MeAPO-36 family containing various types and amounts of metals in their frameworks. Characterization of these samples by X-ray diffraction analysis was delayed due to malfunction of the Diffractometer since October of 1995. The instrument was back in working condition only since the ending of January and XRD analysis has resumed since then. Efforts from the research group were also concentrated on the preparation of manuscripts for publication. Workmore » in progress includes: synthesis of MnAPO5 and MgAPO5; synthesis of CoAPO5; chemical analysis; preliminary investigation of ion exchange capacities of zeolites; uptake kinetics on the Na-exchanged MnAPO5 and MgAPO5 with alkali and alkali earth metals.« less

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

Dave, V., E-mail: vdaditya1000@gmail.com; Rao, G. P., E-mail: ragrao38@gmail.com; Tiwari, G. S., E-mail: tiwarigsin@yahoo.com

Cultivator, one of the agriculture farm tool, extensively suffers from the wear problem. In this paper, we report nanostructured chromium nitrite (CrN) coating for the cultivator shovels to mitigate wear problem. The (CrN) coating was developed using DC magnetron sputtering technique at 200 °C. The structural, morphological, hydrophobic and wear properties were investigated using X-ray diffractometer, scanning electron microscope, contact angle goniometer and custom designed soil bin assembly. The XRD reveals that the deposited coating was polycrystalline in nature with cubic structure. Also, The deposited coating was found to be anti wear resistant as well as hydrophobic in nature. Themore » gravimetric wear for the coating developed at 200 °C coated was found out to be 8.15 gm and for non coated it was 14.48 gm tested for 100 hrs. The roughness of the coating plays an important role in determining the hydrophobicity of the coated film. Roughness and contact angle measured for 200 °C coated shovel was found out to be 11.17 nm and 105 ° respectively.« less

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

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

Don Pellinen and Michael Griffin

2009-01-23

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

Microstructure and magnetic behavior of Mn doped GeTe chalcogenide semiconductors based phase change materials

NASA Astrophysics Data System (ADS)

Adam, Adam Abdalla Elbashir; Cheng, Xiaomin; Abuelhassan, Hassan H.; Miao, Xiang Shui

2017-06-01

Phase-change materials (PCMs) are the most promising candidates to be used as an active media in the universal data storage and spintronic devices, due to their large differences in physical properties of the amorphous-crystalline phase transition behavior. In the present study, the microstructure, magnetic and electrical behaviors of Ge0.94Mn0.06Te thin film were investigated. The crystallographic structure of Ge0.94Mn0.06Te thin film was studied sing X-ray diffractometer (XRD) and High Resolution Transmission Electron Microscope (HR-TEM). The XRD pattern showed that the crystallization structure of the film was rhombohedral phase for GeTe with a preference (202) orientation. The HR-TEM image of the crystalline Ge0.94Mn0.06Te thin film demonstrated that, there were two large crystallites and small amorphous areas. The magnetization as a function of the magnetic field analyses of both amorphous and crystalline states showed the ferromagnetic hysteretic behaviors. Then, the hole carriers concentration of the film was measured and it found to be greater than 1021 cm-3 at room temperature. Moreover, the anomalous of Hall Effect (AHE) was clearly observed for the measuring temperatures 5, 10 and 50 K. The results demonstrated that the magnitude of AHE decreased when the temperature was increasing.

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

DTIC Science & Technology

2016-07-11

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

Comparative investigation of Fourier Transform Infrared (FT-IR) spectroscopy and X-ray Diffraction (XRD) in the determination of cotton fiber crystallinity

USDA-ARS?s Scientific Manuscript database

Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI) from the X-ray diffraction (XRD) measurement, in its present state XRD procedure can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous po...

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

PubMed Central

Benea, Lidia; Celis, Jean-Pierre

2016-01-01

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

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

PubMed

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

2016-08-01

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

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

PubMed

Rezayi, Toktam; Entezari, Mohammad H

2016-02-01

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

Biosynthesis of titanium dioxide nanoparticles using Bacillus amyloliquefaciens culture and enhancement of its photocatalytic activity for the degradation of a sulfonated textile dye Reactive Red 31.

PubMed

Khan, Razia; Fulekar, M H

2016-08-01

The present study aims at exploiting Bacillus amyloliquefaciens for the biosynthesis of titanium dioxide nanoparticles and also investigates role of bacterial enzymes in the biosynthesis of titanium dioxide nanoparticles. Bacterial synthesized as well as metal doped titanium dioxide nanoparticles were characterized by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), Energy dispersive X-ray spectroscopy (EDAX). Amylase activity (43.37IU) in culture supernatant evinced a potential involvement of extracellular enzyme in TiO2 nanoparticle biosynthesis. Crystallite size of bio-synthesized nanoparticles was found to be in the range of 15.23-87.6nm. FTIR spectroscopy and native-PAGE (Polyacrylamide Gel Electrophoresis) clearly indicated involvement of alpha amylase in biosynthesis of TiO2 nanoparticles and in their stabilization. TEM micrographs of the synthesized titanium dioxide nanoparticles revealed the formation of spherical nanoparticles with a size range of 22.11-97.28nm. Photocatalytic degradation of Reactive Red 31 (RR31) dye was carried out using bio-synthesized TiO2 nanoparticles under UV radiation. Photocatalytic activity of synthesized nanoparticles was enhanced by Ag, La, Zn and Pt doping. Platinum doped TiO2 showed highest potential (90.98%) in RR31 degradation as compared to undoped (75.83%). Copyright © 2016 Elsevier Inc. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2013-04-01

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

Effects of laser remelting on microstructures and immersion corrosion performance of arc sprayed Al coating in 3.5% NaCl solution

NASA Astrophysics Data System (ADS)

Sun, Ze; Zhang, Donghui; Yan, Baoxu; Kong, Dejun

2018-02-01

An arc sprayed aluminum (Al) coating on S355 steel was processed using a laser remelting (LR). The microstructures, chemical element composition, and phases of the obtained Al coating were analyzed using a field mission scanning electronic microscope (FESEM), energy dispersive spectrometer (EDS), and X-ray diffractometer (XRD), respectively, and the residual stresses were measured using an X-ray diffraction stress tester. The immersion corrosion tests and potentiodynamic polarization of Al coating in 3.5% NaCl solution were performed to investigate the effects of LR on its immersion corrosion behaviors, and the corrosion mechanism of Al coating was also discussed. The results show that the arc sprayed Al coating is composed of Al phase, while that by LR is composed of Al-Fe and AlO4FeO6 phases, and the porosities and cracks in the arc sprayed Al coating are eliminated by LR, The residual stress of arc sprayed Al coating is -5.6 ± 18 MPa, while that after LR is 137.9 ± 12 MPa, which deduces the immersion corrosion resistance of Al coating. The corrosion mechanism of arc sprayed Al coating is pitting corrosion and crevice corrosion, while that by LR is uniform corrosion and pitting corrosion. The corrosion potential of arc sprayed Al coating by LR shifts positively, which improves its immersion corrosion resistance.

Corrosion effect of microorganisms and their metabolite on cement mortar lined pipelines in reclaimed water distribution systems

NASA Astrophysics Data System (ADS)

Yang, Fan; Chen, Minning

2018-06-01

The reclaimed water containing high salinity, great amounts of organic matters and high nutrients can easily lead to growth of biofilms in reclaimed water distribution systems (RWDSs). The microbes colonize the cement surface and microbial metabolites can cause cement biodeterioration. To understand the effect of microbial involvement in the degradation, this study investigated the transformation characteristics of cement-mortar lining and microbial biomass in the simulated RWDS for 1 year by X-ray diffractometer (XRD), X-Ray Fluorescenc (XRF), Heterophic bacteria count (HPC) and DAPI staining. Microbial metabolites were analyzed by GC/MS. The result shows that the carbonation reaction took place in the surface of the eroded cement-mortar lining where the content of CaCO3 was continuously increasing while the content of hydrated compounds were decreasing. The depositing layer of CaSO4·2H2O, CaAl2Si2O8·4H2O and Mg4Al2(OH)14·3H2O on the lining surface were formed by minerals such as Ca, Si, Al and Mg lost from the degraded hydrated compounds. Microbial biomass in the RWDS has maintained an increasing trend during the study. The main microbial metabolites of the biofilm on the cement surface are fatty acids, amino acids, and carbohydrate.

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

PubMed Central

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

2017-01-01

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

Microstructure control of SOFC cathode material: The role of dispersing agent

NASA Astrophysics Data System (ADS)

Ismail, Ismariza; Jani, Abdul Mutalib Md; Osman, Nafisah

2017-09-01

In the present works, La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) cathode powders were synthesized by a sol-gel method with the aid of ethylene glycol which served as the dispersing agent. The phase formation and morphology of the powders were examined by X-Ray diffractometer (XRD) and field emission scanning electron microscopy (FESEM), respectively. The electrochemical properties of the synthesized cathode were obtained using an electrochemical impedance spectroscopy (EIS). The characteristic peaks for LSCF phase appears in the X-ray diffractogram after calcined at 500 °C and complete formation of LSCF single phase was attained at 700 °C. FESEM micrographs showed the presence of spherical particles of the powders with approximate particle size between 10 to 60 nm along with agglomerate morphologies. Well dispersed particles and fewer aggregates were observed for samples prepared with addition of ethylene glycol as the synthesizing aid. The surface area obtained for powder sample prepared with the aid of dispersing agent is 12.0 m2g-1. The EIS measurement results depicts a lower area specific resistance (ASR) obtained for sample prepared with addition of the ethylene glycol as compared to the pristine sample. The present results encourage the optimization of the cathode particle design in order to further improve the cathode performance.

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

PubMed

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

2013-09-01

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

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

ERIC Educational Resources Information Center

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

2010-01-01

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

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

PubMed

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

2013-11-01

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

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

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

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

2016-09-15

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

Deconvolving the temporal response of photoelectric x-ray detectors for the diagnosis of pulsed radiations

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

Zou, Shiyang; Song, Peng; Pei, Wenbing

2013-09-15

Based on the conjugate gradient method, a simple algorithm is presented for deconvolving the temporal response of photoelectric x-ray detectors (XRDs) to reconstruct the resolved time-dependent x-ray fluxes. With this algorithm, we have studied the impact of temporal response of XRD on the radiation diagnosis of hohlraum heated by a short intense laser pulse. It is found that the limiting temporal response of XRD not only postpones the rising edge and peak position of x-ray pulses but also smoothes the possible fluctuations of radiation fluxes. Without a proper consideration of the temporal response of XRD, the measured radiation flux canmore » be largely misinterpreted for radiation pulses of a hohlraum heated by short or shaped laser pulses.« less

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

DTIC Science & Technology

2015-07-20

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

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

NASA Astrophysics Data System (ADS)

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

2001-05-01

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

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

PubMed

Nesterets; Punegov

2000-11-01

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

Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

PubMed Central

Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

2003-01-01

Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (μ-XRD) techniques. Rietveld refinement analyses of XRD and μ-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

Structural changes in shock compressed silicon observed using time-resolved x-ray diffraction at the Dynamic Compression Sector

NASA Astrophysics Data System (ADS)

Turneaure, Stefan; Zdanowicz, E.; Sinclair, N.; Graber, T.; Gupta, Y. M.

2015-06-01

Structural changes in shock compressed silicon were observed directly using time-resolved x-ray diffraction (XRD) measurements at the Dynamic Compression Sector at the Advanced Photon Source. The silicon samples were impacted by polycarbonate impactors accelerated to velocities greater than 5 km/s using a two-stage light gas gun resulting in impact stresses of about 25 GPa. The 23.5 keV synchrotron x-ray beam passed through the polycarbonate impactor, the silicon sample, and an x-ray window (polycarbonate or LiF) at an angle of 30 degrees relative to the impact plane. Four XRD frames (~ 100 ps snapshots) were obtained with 153.4 ns between frames near the time of impact. The XRD measurements indicate that in the peak shocked state, the silicon samples completely transformed to a high-pressure phase. XRD results for both shocked polycrystalline silicon and single crystal silicon will be presented and compared. Work supported by DOE/NNSA.

X-Ray Diffraction Reference Intensity Ratios of Amorphous and Poorly Crystalline Phases: Implications for CheMin on the Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Morris, R. V.; Achilles, C. N.; Chipera, S. J.; Ming, D. W.; Rampe, E. B.

2013-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity is an X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of providing the mineralogical and chemical compositions of rocks and soils on the surface of Mars. CheMin uses a microfocus X-ray tube with a Co target, transmission geometry, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. Piezoelectric vibration of the cell is used to randomize the sample to reduce preferred orientation effects. Instrument details are provided in [1, 2, 3]. Analyses of rock and soil samples by the Mars Exploration Rovers (MER) show nanophase ferric oxide (npOx) is a significant component of the Martian global soil [4] and is thought to be one of the major contributing phases that the Curiosity rover will encounter if a soil sample is analyzed in Gale Crater. Because of the nature of this material, npOx will likely contribute to an X-ray amorphous or short-order component of a XRD pattern measured by the CheMin instrument.

X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

NASA Astrophysics Data System (ADS)

Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

2011-12-01

The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I., Baliva, A., Stevoli, A., Ambrosi, R., Critani, F., Delhez, R., Scandelli, L., Holland, A., Nelms, N. & the Mars-XRD Team, Proceedings of the 38th Lunar and Planetary Science Conference, 12 - 16 March 2007, League City, Texas, USA. [2] L. Marinangeli, I. B. Hutchinson, A. Stevoli, G. Adami, R. Ambrosi, R. Amils, V. Assis Fernandes, A. Baliva, A. T. Basilevsky, G. Benedix, P. Bland, A. J. Böttger, J. Bridges, G. Caprarelli, G. Cressey, F. Critani, N. d'Alessandro, R. Delhez, C. Domeneghetti, D. Fernandez-Remolar, R. Filippone, A. M. Fioretti, J. M. Garcia Ruiz, M. Gilmore, G. M. Hansford, G. Iezzi, R. Ingley, M. Ivanov, G. Marseguerra, L. Moroz, C. Pelliciari, P. Petrinca, E. Piluso, L. Pompilio, J. Sykes, F. Westall and the MARS-XRD Team, EPSC-DPS Joint Meeting 2011, 3 - 7 October 2011, La Cité Internationale des Congrès Nantes Métropole, Nantes, France.

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

X-ray diffraction and X-ray K absorption near edge studies of copper (II) complexes with amino acids

NASA Astrophysics Data System (ADS)

Sharma, P. K.; Mishra, Ashutosh; Malviya, Varsha; Kame, Rashmi; Malviya, P. K.

2017-05-01

Synthesis of copper (II) complexes [CuL1L2X].nH2O, where n=1, 2,3 (X=Cl,Br,NO3) (L1is 2,2’-bipyridine and L2 is L-tyrosine) by the chemical root method. The XRD data for the samples have been recorded. EXAFS spectra have also been recorded at the K-edge of Cu using the dispersive beam line BL-8 at 2.5 Gev Indus-2 Synchrotron radiation source at RRCAT, Indore, India. XRD and EXAFS data have been analysed using the computer software. X-ray diffraction studies of all complexes indicate their crystalline nature. Lattice parameter, bond length, particle size have been determined from XRD data.

Aging Effects on the Structural and Magnetic Properties of Terbium-Aluminium Co-doping of Yttrium Iron Garnet Films Prepared Using the Sol-Gel Method

NASA Astrophysics Data System (ADS)

Aldbea, Ftema W.; Yusrianto, Efil; Ibrahim, N. B.

2018-06-01

The terbium-aluminium co-doped yttrium iron garnet (Tb0.2Y2.8Al1Fe4O12) nanoparticles films, prepared via a sol-gel method, were aged variously for 2 days, 3 days, 4 days and 5 days. The films were deposited on quartz substrates using a spin coating technique then annealed at 900°C in air for 2 h. The microstructural and magnetic properties of the films were measured using an x-ray diffractometer (XRD), a field emission scanning electron microscope and a vibrating sample magnetometer. The XRD results showed that all the resultant films were a single phase regardless of aging time. A change in the lattice parameter's behavior was observed at the longer aging times. At an aging time of 5 days, the films became highly agglomerated and exhibited the greatest thickness value of 458.9 nm. The saturation magnetization, M s, of the films decreased from 31 kA/m to 6 kA/m as the aging time was increased from 2 days to 5 days, due to the increasing Fe-O bond length resulting from larger grain sizes. The increase in aging time to 5 days caused a reduction in the coercivity, H c, of films due to the multi-domain formation.

Bio-synthesis and antimicrobial activity of silver nanoparticles using anaerobically digested parthenium slurry.

PubMed

Adur, Alaknanda J; Nandini, N; Shilpashree Mayachar, K; Ramya, R; Srinatha, N

2018-06-01

Silver nanoparticles were prepared through eco-friendly, cost effective, bio-mediated technique using anaerobically digested Parthenium hysterophorous digested slurry (PDS) for the first time. The synthesized nanoparticles were characterized through different techniques such as UV-Vis spectrophotometer for optical properties; X-ray diffractometer (XRD), high resolution transmission electron spectroscopy (HR-TEM) and Fourier Transform Infra Red (FTIR) Spectroscopy for structural property investigations. It was observed that the prepared silver nanoparticles were crystallized in face centered cubic crystal structure with an average particle size of 19 nm as confirmed from XRD. Also HR-TEM studies reveal the formation of nano-sized silver particles with face centered cubic nano structure. In addition, absorption spectra exhibit Surface Plasmon Resonance (SPR) which suggests the formation of silver nanoparticles. FTIR results show the presence of different characteristic functional groups and their stretching / bending vibrations in turn responsible for the bioreduction of silver ions in Parthenium digested slurry. Further investigations on antimicrobial activity were done by subjecting the synthesized silver nanoparticles on E-coli and Pseudomonas as marker organisms for the group of gram negative bacteria by well plate method on enrichment media. The result obtained shows a clear zone of inhibition confirming the antibacterial activity. Overall, the investigated results confirm the biosynthesized silver nanoparticles are potential candidates for antimicrobial activity applications. Copyright © 2018 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2015-04-01

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

The porosity formation mechanism in the laser-MIG hybrid welded joint of Invar alloy

NASA Astrophysics Data System (ADS)

Zhan, Xiaohong; Gao, Qiyu; Gu, Cheng; Sun, Weihua; Chen, Jicheng; Wei, Yanhong

2017-10-01

The porosity formation mechanism in the laser-metal inter gas (MIG) multi-layer hybrid welded (HW) joint of 19.05 mm thick Invar alloy is investigated. The microstructure characteristics and energy dispersive spectroscopy (EDS) are analyzed. The phase identification was conducted by the X-ray diffractometer (XRD). Experimental results show that the generation of porosity is caused by the relatively low laser power in the root pass and low current in the cover pass. It is also indicated that the microstructures of the welded joints are mainly observed to be columnar crystal and equiaxial crystal, which are closely related to the porosity formation. The EDS results show that oxygen content is significantly high in the inner wall of the porosity. The XRD results indicate that the BM and the WB of laser-MIG HW all are composed of Fe0.64Ni0.36 and γ-(Fe,Ni). When the weld pool is cooled quickly, [NiO] [FeO] and [MnO] are formed that react on C to generate CO/CO2 gases. The porosity of laser-MIG HW for Invar alloy is oxygen pore. The root source of metallurgy porosity formation is that the dissolved gases are hard to escape sufficiently and thus exist in the weld pool. Furthermore, 99.99% pure Argon is recommended as protective gas in the laser-MIG HW of Invar alloy.

Synthesis and characterization of γ-Fe2O3 NPs on silicon substrate for power device application

NASA Astrophysics Data System (ADS)

Hussein Nurul Athirah, Abu; Bee Chin, Ang; Yew Hoong, Wong; Boon Hoong, Ong; Aainaa Aqilah, Baharuddin

2018-06-01

Maghemite nanoparticles (γ-Fe2O3 NPs) were synthesized using Massart procedure. The formation reaction were optimized by varying the concentration of ferric nitrate solution (Fe(NO3)3) (0.1, 0.3, 0.5, 0.7 and 1.0 M). All samples were characterized by means of x-ray Diffractometer (XRD), Raman Spectroscopy, Transmission Electron Microscope (TEM) and Alternating Gradient Magnetometer (AGM). The smallest size of the NPs were chosen to be deposited on Silicon (100) substrate by spin coating technique. Annealing process of the samples were performed in Argon ambient at different temperatures (600, 700, 800 and 900°) for 20 min. Metal-oxide-semiconductor capacitors were then fabricated by depositing Aluminium as the gate electrode. The effect of the annealing process on the structural and electrical properties of γ-Fe2O3 NPs thin film were investigated. The structural properties of the deposited thin film were evaluated by XRD analysis, Atomic Force Microscopy (AFM) and Raman Analysis. On the other hand, the electrical properties was conducted by current-voltage analysis. It was revealed that the difference in the annealing temperature affect the grain size, surface roughness, distribution of the nanoparticles as well as the electrical performance of the samples where low annealing temperature (600 °C) gives low leakage current while high annealing temperature (900 °C) gives high electrical breakdown.

Synthesis of mullite (3Al2O32SiO2) from local kaolin for radiation shielding

NASA Astrophysics Data System (ADS)

Ripin, Azuhar; Mohamed, Faizal; Aman, Asyraf

2018-04-01

Raw kaolin from Kota Tinggi, Johor was used in this study to produce ceramic mullite (3Al2O22SiO2) for radiation shielding materials. In this work, an attempt was made to study the potential of local minerals to be used as a shielding barrier for diagnostic radiology radiation facilities in hospitals and medical centers throughout Malaysia. The conventional ceramic processing route was employed in the study using different pressing strength and sintering time. The obtained samples were characterized using X-ray diffractometer (XRD) for phase identification of each of the samples. The lead equivalent (LE) test was carried out using 15.05 mCi Cobalt-57 with gamma energy of 122 keV to compute the abilities of the mullite ceramic samples to attenuate the radiation. XRD patterns of prepared ceramics revealed the presence of orthorhombic mullite, hexagonal quartz and orthorhombic sillimanite structures. Furthermore, the radiation test displayed the ability of ceramics to shield of 70 % of gamma radiation at the distance of 60 cm from the radiation source. The highest lead equivalent thickness is 1.0 mm Pb and the lowest is about 0.06 mm Pb. From the result, it is shown that the ceramic has the potential to use as a shielding barrier in diagnostic radiology facilities due to the ability of reducing the radiation dose up to 70 % from its initial value.

Mineralogy by X-ray Diffraction on Mars: The Chemin Instrument on Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bristow, T. F.; Bish, D. L.; Ming, D. W.; Blake, D. F.; Morris, R. V.; Rampe, E. B.; Chipera, S. J.; Treiman, A. H.; Morrison, S. M.;

In situ X-ray diffraction analysis of (CF x) n batteries: signal extraction by multivariate analysis

DOE PAGES

Rodriguez, Mark A.; Keenan, Michael R.; Nagasubramanian, Ganesan

2007-11-10

In this study, (CF x) n cathode reaction during discharge has been investigated using in situ X-ray diffraction (XRD). Mathematical treatment of the in situ XRD data set was performed using multivariate curve resolution with alternating least squares (MCR–ALS), a technique of multivariate analysis. MCR–ALS analysis successfully separated the relatively weak XRD signal intensity due to the chemical reaction from the other inert cell component signals. The resulting dynamic reaction component revealed the loss of (CF x) n cathode signal together with the simultaneous appearance of LiF by-product intensity. Careful examination of the XRD data set revealed an additional dynamicmore » component which may be associated with the formation of an intermediate compound during the discharge process.« less

Sol-Gel Synthesis of Fe-Doped TiO2 Nanocrystals

NASA Astrophysics Data System (ADS)

Marami, Mohammad Bagher; Farahmandjou, Majid; Khoshnevisan, Bahram

2018-03-01

Fe-doped TiO2 powders were synthesized by the sol-gel method using titanium (IV) isopropoxide (TTIP) as the starting material, ethanol as solvent, and ethylene glycol (EG) as stabilizer. These prepared samples were characterized by x-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), Fourier-transform infrared (FTIR) spectroscopy, diffuse reflection spectroscopy (DRS), energy-dispersive x-ray spectroscopy (EDX), and photoluminescence (PL) analyses to study their structure, morphology, and optical properties. The particle size of Fe-doped TiO2 was in the range of 18-39 nm and the minimum crystallite size was achieved for 4 mol.% of Fe. The XRD result of the samples that were doped with Fe showed a tetragonal structure. It also revealed the coexistence of the anatase and rutile phases, and showed that their ratio changed with various molar concentrations of Fe dopant. FTIR spectroscopy showed the presence of the Ti-O vibration band in the samples. PL analysis revealed the PL property in the UV region. Visible irradiation and the intensity of PL spectra were both reduced by doping TiO2 with 3 mol.% of Fe as compared to the pure variety. The spectra from the DRS showed a red shift and a reduction of 2.6 eV in the band gap energy for 4 mol.% Fe-doped TiO2. The optimum level of impurity (4 mol.%) for Fe-doped TiO2 nanoparticles (NPs), which improve the optical and electrical properties by using new precursors and can be used in solar cells and electronic devices, was determined. The novelty of this work consists of: the Fe/TiO2 NPs are synthesized by new precursors from sol-gel synthesis of iron and TTIP using acetic acid-catalyzed solvolysis (original idea) and the optical properties optimized with a mixture of phases (anatase/rutile) of Fe-doped TiO2 by this facile method.

Sol-Gel Synthesis of Fe-Doped TiO2 Nanocrystals

NASA Astrophysics Data System (ADS)

Marami, Mohammad Bagher; Farahmandjou, Majid; Khoshnevisan, Bahram

2018-07-01

Fe-doped TiO2 powders were synthesized by the sol-gel method using titanium (IV) isopropoxide (TTIP) as the starting material, ethanol as solvent, and ethylene glycol (EG) as stabilizer. These prepared samples were characterized by x-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), Fourier-transform infrared (FTIR) spectroscopy, diffuse reflection spectroscopy (DRS), energy-dispersive x-ray spectroscopy (EDX), and photoluminescence (PL) analyses to study their structure, morphology, and optical properties. The particle size of Fe-doped TiO2 was in the range of 18-39 nm and the minimum crystallite size was achieved for 4 mol.% of Fe. The XRD result of the samples that were doped with Fe showed a tetragonal structure. It also revealed the coexistence of the anatase and rutile phases, and showed that their ratio changed with various molar concentrations of Fe dopant. FTIR spectroscopy showed the presence of the Ti-O vibration band in the samples. PL analysis revealed the PL property in the UV region. Visible irradiation and the intensity of PL spectra were both reduced by doping TiO2 with 3 mol.% of Fe as compared to the pure variety. The spectra from the DRS showed a red shift and a reduction of 2.6 eV in the band gap energy for 4 mol.% Fe-doped TiO2. The optimum level of impurity (4 mol.%) for Fe-doped TiO2 nanoparticles (NPs), which improve the optical and electrical properties by using new precursors and can be used in solar cells and electronic devices, was determined. The novelty of this work consists of: the Fe/TiO2 NPs are synthesized by new precursors from sol-gel synthesis of iron and TTIP using acetic acid-catalyzed solvolysis (original idea) and the optical properties optimized with a mixture of phases (anatase /rutile) of Fe-doped TiO2 by this facile method.

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

DOEpatents

Carpenter, Donald A.

1995-01-01

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

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

DOEpatents

Carpenter, D.A.

1995-05-23

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

Effect of thermal annealing on structural and optical properties of In{sub 2}S{sub 3} thin films

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

Choudhary, Sonu, E-mail: sonuchoudhary1983@gmail.com

2015-08-28

There is a highly need of an alternate of toxic materials CdS for solar cell applications and indium sulfide is found the most suitable candidate to replace CdS due to its non-toxic and environmental friendly nature. In this paper, the effect of thermal annealing on the structural and optical properties of indium sulfide (In{sub 2}S{sub 3}) thin films is undertaken. The indium sulfide thin films of 121 nm were deposited on glass substrates employing thermal evaporation method. The films were subjected to the X-ray diffractometer and UV-Vis spectrophotometer respectively for structural and optical analysis. The XRD pattern show that themore » as-deposited thin film was amorphous in nature and crystallinity is found to be varied with annealing temperature. The optical analysis reveals that the optical band gap is varied with annealing. The optical parameters like absorption coefficient, extinction coefficient and refractive index were calculated. The results are in good agreement with available literature.« less

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

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

PubMed

Yi, Yuan-Rong; Han, Min-Fang

2012-07-01

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

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

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

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

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

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

NASA Astrophysics Data System (ADS)

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

2016-12-01

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

Synthesis, characterization and properties of carbon nanotubes microspheres from pyrolysis of polypropylene and maleated polypropylene

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

Zhang, Junhao, E-mail: jhzhang6@mail.ustc.edu.cn; Department of Chemistry, University of Science and Technology of China, Heifei, Anhui 230026; Du, Jin

Microspheres assembled from carbon nanotubes (MCNTs), with the diameters ranging from 5.5 to 7.5 {mu}m, were synthesized by means of pyrolysis of polypropylene and maleated polypropylene in an autoclave. The characterization of structure and morphology was carried out by X-ray diffractometer (XRD), field-emission scanning electron microscopy (FESEM), (high resolution) transmission electron microscope [(HR)TEM)], selected-area electron diffraction (SAED) and Raman spectrum. As a typical morphology, the possible growth process of MCNTs was also investigated and discussed. The results of nitrogen adsorption-desorption indicate that the Brunauer-Emett-Teller (BET) surface area (140.6 m{sup 2}/g) of the MCNTs obtained at 600 {sup o}C is aboutmore » twice as that (74.5 m{sup 2}/g) of carbon nanotubes obtained at 700 {sup o}C. The results of catalytic experiment show that MCNTs based catalyst has higher catalytic activity than the carbon nanotubes based catalyst for the preparation of methanol and dimethoxy-ethane by oxidation of dimethyl ether.« less

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

NASA Astrophysics Data System (ADS)

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

2015-08-01

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

Comparison of characteristics of hydroxyapatite powders synthesized from cuttlefish bone via precipitation and ball milling techniques

NASA Astrophysics Data System (ADS)

Faksawat, K.; Kaewwiset, W.; Limsuwan, P.; Naemchanthara, K.

2017-09-01

The aim of this work was to compare characteristics of hydroxyapatite synthesized by precipitation and ball milling techniques. The cuttlefish bone powder was a precursor in calcium source and the di ammonium hydrogen orthophosphate powders was a precursor in phosphate source. The hydroxyapatite was synthesized by the both techniques such as precipitation and ball milling techniques. The phase formation, chemical structure and morphology of the both hydroxyapatite powders have been examined by X-ray diffractometer (XRD), Fourier transform infrared spectroscope (FTIR) and field emission scanning electron microscope (FESEM), respectively. The results show that the hydroxyapatite synthesized by precipitation technique formed hydroxyapatite phase slower than the hydroxyapatite synthesized by ball milling technique. The FTIR results show the chemical structures of sample in both techniques are similar. The morphology of the hydroxyapatite from the both techniques were sphere like shapes and particle size was about in nano scale. The average particle size of the hydroxyapatite by ball milling technique was less than those synthesized by precipitation technique. This experiment indicated that the ball milling technique take time less than the precipitation technique in hydroxyapatite synthesis.

Study of DDT and its derivatives DDD, DDE adsorption and degradation over Fe-SBA-15 at low temperature.

PubMed

Wang, Hailin; Tian, Hua; Hao, Zhengping

2012-01-01

Mesoporous SBA-15 with different Fe2O3 loading were synthesized by an in-situ coating progress for removals of dichlorodiphenyltrichloroethane (DDT) and its derivatives, i.e., 1,1-dichloro-2,2-bis-(p-chlorophenyl)ethane (DDD) and 1,1-dichloro-2,2-bis-(4-chloro -phenyl) ethane (DDE). The results from XRD (X-ray diffractometer), TEM (transmission electron microscopy) indicated that the iron could be well dispersed on SBA-15 within 6 wt.% Fe2O3 loading. Nitrogen adsorption-desorption tests indicated that the synthesized materials were characterized by ordered meso-structure, high surface area and large pore volume. DDTs were removed from aqueous media in 12-hr treatment and high removal efficiency of DDTs was achieved at over 94%. DDTs could be completely degraded at 350 degrees C under the existence of SBA-15 with 4 wt.% Fe2O3 loading. The final degradation products of DDT were dichlorobenzophenone (DCB) and bis-(4-chloro-phenyl) methane (DDM), suggesting a complete dechlorination from trichloromethyl.

Nanostructured wear resistant coating for reversible cultivator shovels: An experimental investigation

NASA Astrophysics Data System (ADS)

Dave, V.; Rao, G. P.; Tiwari, G. S.; Sanger, A.; Kumar, A.; Chandra, R.

2016-04-01

Cultivator, one of the agriculture farm tool, extensively suffers from the wear problem. In this paper, we report nanostructured chromium nitrite (CrN) coating for the cultivator shovels to mitigate wear problem. The (CrN) coating was developed using DC magnetron sputtering technique at 200 °C. The structural, morphological, hydrophobic and wear properties were investigated using X-ray diffractometer, scanning electron microscope, contact angle goniometer and custom designed soil bin assembly. The XRD reveals that the deposited coating was polycrystalline in nature with cubic structure. Also, The deposited coating was found to be anti wear resistant as well as hydrophobic in nature. The gravimetric wear for the coating developed at 200 °C coated was found out to be 8.15 gm and for non coated it was 14.48 gm tested for 100 hrs. The roughness of the coating plays an important role in determining the hydrophobicity of the coated film. Roughness and contact angle measured for 200 °C coated shovel was found out to be 11.17 nm and 105 ° respectively.

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

NASA Astrophysics Data System (ADS)

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

2007-10-01

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

Characterization of Calcite Mineral Precipitation Process by EICP in Porous Media

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Biocompatible Er, Yb co-doped fluoroapatite upconversion nanoparticles for imaging applications

NASA Astrophysics Data System (ADS)

Anjana, R.; K. M., Kurias; M. K., Jayaraj

2017-08-01

Upconversion luminescence, visible emission on infra red (IR) excitation was achieved in a biocompatible material, fluoroapatite. Fluoroapatite crystals are well known biomaterials, which is a component of tooth enamel. Also it can be considered as an excellent host material for lanthanide doping since the ionic radii of lanthanide is similar to that of calcium ion(Ca2+) hence successful incorporation of dopants within the lattice is possible. Erbium (Er), Ytterbium (Yb) co-doped fluorapatite (FAp) nanoparticles were prepared by precipitation method. The particles show intense visible emission when excited with 980 nm laser. Since upconversion luminescence is a multiphoton process the excitation power dependence on emission will give number of photons involved in the emission of single photon. Excitation power dependence studies show that two photons are involved in the emission of single photons. The value of slope was different for different emission peak because of the difference in intermediate energy level involved. The crystal structure and morphology of the particle were determined using X-ray diffractometer (XRD) and field emission scanning electron microscope (FESEM). These particles with surface functionalisation can be used for live cell imaging.

Supercrystallization of KCl from solution irradiated by soft X-rays

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

Effects of Co contents on the microstructures and properties of the electrodeposited NiCo–Zr composite coatings

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

Cai, Fei; Jiang, Chuanhai, E-mail: chuanhaijiang1963@163.com; Zhao, Yuantao

2015-05-15

Highlights: • The novel NiCo–Zr coatings were prepared by electro-deposition. • Surface morphology, crystal structure, grain size and microstrain were examined. • Texture, residual stress and corrosion resistance were investigated. • Addition of Co increased the hardness and corrosion resistance of the coatings. - Abstract: In this study, the NiCo–Zr composite coatings were prepared from the electrolytes with different Co{sup 2+} concentrations by electrodeposition method. The effects of Co contents on the crystal structure, surface morphology, grain size, microstrain and residual stress were examined by X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), Energy dispersive X-ray spectroscopy (EDX) andmore » atomic force microscope (AFM). The corrosion resistance of the composite coatings was also examined by the potentiodynamic polarization and electrochemical impedance (EIS) measurements. The results revealed that the crystal structures of the coatings were dependent on the Co contents and addition of Co content of 58 wt% resulted in the formation of hexagonal (hcp) Co. The increasing Co contents in the NiCo–Zr composite coatings resulted in the smoother and more compact surface, decreased the grain size and increased the microstrain. The micro-hardness and residual stress also increased with increasing Co contents. The addition of Co increased the corrosion resistance of the NiCo–Zr composite coatings compared with the Ni–Zr coating while the corrosion resistance of the NiCo–Zr composite coatings decreased as the Co contents increased.« less

Development of TiN particulates reinforced SS316 based metal matrix composite by direct metal laser sintering technique and its characterization

NASA Astrophysics Data System (ADS)

Hussain, Manowar; Mandal, Vijay; Kumar, Vikas; Das, A. K.; Ghosh, S. K.

2017-12-01

The present study describes the fabrication of TiN particulates reinforced SS316 based Metal Matrix Composites (MMCs) in nitrogen and argon atmosphere. The influence of sintering process parameters on microstructure, density, porosity, wear rate and microhardness of the fabricated samples has been analyzed. The input variable process parameters, such as, laser power density (range: 4.13-5.57 W/cm2 (× 104)), scanning speed (range: 3500-4500 mm/min) and the constant parameters, such as, laser beam diameter (0.4 mm), hatching distance (0.2 mm) and layer thickness (0.4 mm) have been considered in the process. It has been observed from Field Emission Scanning Electron Microscopy (FESEM) analysis that TiN and SS316 powder mixture can be sintered in which chromium acts as a binder. Fine gaps are not found at the interface between TiN and SS316 when the mixture is sintered in nitrogen atmosphere. With an increase in the percentage of TiN, the density and wear rate decreases. However, when the reinforcement is taken beyond 18% by weight, the wear rate starts increasing. The microhardness also increases with an increase in the percentage of TiN. The microstructure, elemental compositions and phase characterization of the developed sintered MMCs have been examined by FESEM, EDX (Energy-dispersive X-ray spectroscopy) and XRD (X-ray diffractometer) analysis, respectively. The results have demonstrated the suitability of the TiN reinforced SS316 MMCs for industrial applications.

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

NASA Astrophysics Data System (ADS)

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

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

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

PubMed

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

2017-03-01

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

DEVELOPMENT OF ISOTOPICALLY ENRICHED BORON-DOPED ALUMINA DOSIMETER FOR THERMAL NEUTRONS.

PubMed

Sato, Fuminobu; Maekawa, Tatsuro; Kariba, Tomoharu; Kusaka, Sachie; Tanaka, Teruya; Murata, Isao

2017-12-01

A novel optically stimulated luminescence (OSL) detector containing isotopically enriched boron was developed for thermal neutron dosimetry. Alumina containing isotopically enriched boron (Al2O3:B) was synthesised by the sol-gel method. The Al2O3:B was annealed up to ~1800 K. For X-ray diffractometer (XRD) analysis, the diffraction pattern of the Al2O3:B had reflex peaks corresponding to α-Al2O3. The sensitivity of Al2O3:B to photons was slightly 2% of that of a commercial Al2O3:C. The Al2O3:B detector had satisfactory linearity in X-ray dose measurement. A thermal neutron field was constructed using a 241Am-Be neutron source and graphite blocks. A pair of Al2O3:10B and Al2O3:11B detectors were set in the thermal neutron field. The response of Al2O3:10B was larger than that of Al2O3:11B owing to the 10B(n,α)7Li reactions. The sensitivity of Al2O3:10B to thermal neutrons was estimated to be two orders less than the photon sensitivity. Therefore, the pair of Al2O3:10B and Al2O3:11B detectors were useful for thermal neutron dosimetry. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Quantitative shock stage assessment in olivine and pyroxene bearing meteorites via in situ micro-XRD

NASA Astrophysics Data System (ADS)

McCausland, P. J.; Flemming, R. L.; Izawa, M. R.

2010-12-01

Shock metamorphism is observed in most meteorites and impact structures [1]. Qualitative petrographic observations underpin a shock classification system [1-3] based on the deformation features in common silicates and on textural relations such as the development of maskelynite from feldspars, mobility of sulphides and metal in veins and local Fe-reduction in silicates. Shock deformation of minerals produces streaks (mosaicity) rather than discrete spots in 2D X-ray diffraction patterns, representing the progressive disruption of the crystal lattice into a mosaic of rotated domains [4,5]. Here we use in situ micro-XRD [5,6] to measure the mosaicity of olivine and pyroxene in ordinary chondrites of increasing shock stages S1 to S5 and then apply the method to achondrites with qualitatively low to high shock. X-ray diffraction data were collected in situ on polished thin sections and slab cut surfaces using a Bruker D8 Discover micro X-ray diffractometer [5], operated using CuKα radiation generated at 40 kV and 40 mA with a beam diameter of 500 μm. Diffracted X-rays were recorded with a 2D detector, giving images with information in both the 2-theta and chi dimensions, in which each lattice plane (hkl) will have a diffraction spot or streak lying along an arc in chi of radius 2-theta (hkl). Individual reflections can be indexed and then integrated as a function of chi angle, allowing examination of the peak shape and quantitative analysis of the mosaic peak FWHM along chi. We find that both forsterite and enstatite exhibit greater mosaicity in chi with increasing shock stage: Forsterite chi ranges from <1° for S1 to >6° for S5. Enstatite chi values from the same meteorites show a more subdued growth of streak length with shock state, from ~1° to ~4°. A slab of the olivine shergottite DaG 476 exhibits forsterite mosaicity of 6.9°+/-1.1°, indicating that it has experienced shock stage S5, with shock pressures 30-45 GPa [1,4], consistent with the 40-45 GPa shock pressure estimated for DaG 476 by plagioclase refractive index [7]. These observations show that shock classification -and potentially shock pressure calibration- can be done using in situ XRD mineral data. [1] Stoffler, D. et al., (1991) GCA 55, 3845-3867. [2] Scott, E.R.D. et al., (1992) GCA 56, 4281-4293. [3] Rubin, A.E. et al., (1997) GCA 61, 847-858. [4] Horz, F. and Quiade, W.I. (1973) The Moon 6, 45-86. [5] Flemming, R.L. (2007) Can. Jour. Earth Sci. 44, 1333-1346. [6] Izawa, M.R.M. et al., (2009) LPSC XV. [7] Fritz, J. et al., (2005) MAPS 40, 1393-1411.

Simultaneous Femtosecond X-ray Spectroscopy and Diffraction of Photosystem II at Room Temperature

PubMed Central

Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J.; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Miahnahri, Alan; Schafer, Donald W.; Messerschmidt, Marc; Seibert, M. Marvin; Koglin, Jason E.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J.; Grosse-Kunstleve, Ralf W.; Zwart, Petrus H.; White, William E.; Glatzel, Pieter; Adams, Paul D.; Bogan, Michael J.; Williams, Garth J.; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K.; Yachandra, Vittal K.; Bergmann, Uwe; Yano, Junko

2013-01-01

Intense femtosecond X-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous X-ray diffraction (XRD) and X-ray emission spectroscopy (XES) of microcrystals of Photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD/XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies. PMID:23413188

Simultaneous femtosecond X-ray spectroscopy and diffraction of photosystem II at room temperature.

PubMed

Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; Difiore, Dörte; Milathianaki, Despina; Fry, Alan R; Miahnahri, Alan; Schafer, Donald W; Messerschmidt, Marc; Seibert, M Marvin; Koglin, Jason E; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J; Grosse-Kunstleve, Ralf W; Zwart, Petrus H; White, William E; Glatzel, Pieter; Adams, Paul D; Bogan, Michael J; Williams, Garth J; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K; Yachandra, Vittal K; Bergmann, Uwe; Yano, Junko

2013-04-26

Intense femtosecond x-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous x-ray diffraction (XRD) and x-ray emission spectroscopy (XES) of microcrystals of photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD-XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation-sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies.

Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

PubMed

Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

2015-06-01

This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

Method of Generating X-Ray Diffraction Data for Integral Detection of Twin Defects in Super-Hetero-Epitaxial Materials

NASA Technical Reports Server (NTRS)

Park, Yeonjoon (Inventor); Choi, Sang Hyouk (Inventor); King, Glen C. (Inventor); Elliott, James R. (Inventor)

2009-01-01

A method provides X-ray diffraction (XRD) data suitable for integral detection of a twin defect in a strained or lattice-matched epitaxial material made from components having crystal structures having symme try belonging to different space groups. The material is mounted in a n X-ray diffraction (XRD) system. In one embodiment, the XRD system's goniometer angle Omega is set equal to (Theta(sub B)-Beta) where The ta(sub B) is a Bragg angle for a designated crystal plane of the allo y that is disposed at a non-perpendicular orientation with respect to the {111) crystal plane, and Beta is the angle between the designate d crystal plane and a { 111 } crystal plane of one of the epitaxial components. The XRD system's detector angle is set equal to (Theta(su b B)+Beta). The material can be rotated through an angle of azimuthal rotation Phi about the axis aligned with the material. Using the det ector, the intensity of the X-ray diffraction is recorded at least at the angle at which the twin defect occurs.

Single Crystal Diffractometry

NASA Astrophysics Data System (ADS)

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

2009-06-01

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

A Curved Image-Plate Detector System for High-Resolution Synchrotron X-ray Diffraction

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

Sarin, P.; Haggerty, R; Yoon, W

2009-01-01

The developed curved image plate (CIP) is a one-dimensional detector which simultaneously records high-resolution X-ray diffraction (XRD) patterns over a 38.7 2{theta} range. In addition, an on-site reader enables rapid extraction, transfer and storage of X-ray intensity information in {le}30 s, and further qualifies this detector to study kinetic processes in materials science. The CIP detector can detect and store X-ray intensity information linearly proportional to the incident photon flux over a dynamical range of about five orders of magnitude. The linearity and uniformity of the CIP detector response is not compromised in the unsaturated regions of the image plate,more » regardless of saturation in another region. The speed of XRD data acquisition together with excellent resolution afforded by the CIP detector is unique and opens up wide possibilities in materials research accessible through X-ray diffraction. This article presents details of the basic features, operation and performance of the CIP detector along with some examples of applications, including high-temperature XRD.« less

An Investigation of the Interatomic Bonding Characteristics of a Ti - 51at.% Al Alloy by X-Ray Diffraction

DTIC Science & Technology

1991-06-01

GROUP SUBGROUP X-ray Diffraction, XRD, TiAI, titanium , aluminum, bonding characteristics, titanium aluminides , Debye-Waller temperature factor...XRD Powder Particles (575X) .............. 47 viii I. INTRODUCTION Titanium aluminides are recognized for their high specific strength, particularly at...bonding characteristics of binary titanium aluminides . Upon the introduction of a third element to the system, a rearrangement of the valence

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

DTIC Science & Technology

2006-03-02

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

Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

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

Liu, Ying, E-mail: liu.ying.48r@st.kyoto-u.ac.jp; Imashuku, Susumu; Sasaki, Nobuharu

In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient tomore » determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.« less

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

PubMed

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

1998-03-01

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

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

PubMed

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

2014-09-01

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

Detection Limit of Smectite by Chemin IV Laboratory Instrument: Preliminary Implications for Chemin on the Mars Science Laboratory Mission

NASA Technical Reports Server (NTRS)

Archilles, Cherie; Ming, D. W.; Morris, R. V.; Blake, D. F.

2011-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) is an miniature X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of detecting the mineralogical and elemental compositions of rocks, outcrops and soils on the surface of Mars. CheMin uses a microfocus-source Co X-ray tube, a transmission sample cell, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CRISM and OMEGA have identified the presence of phyllosilicates at several locations on Mars including the four candidate MSL landing sites. The objective of this study was to conduct preliminary studies to determine the CheMin detection limit of smectite in a smectite/olivine mixed mineral system.

Electrochemical fabrication of SrTiO3 nanowires with nanoporous alumina template.

PubMed

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

2007-11-01

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

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

PubMed

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

2011-01-01

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

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

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

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

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

In situ flow cell for combined X-ray absorption spectroscopy, X-ray diffraction, and mass spectrometry at high photon energies under solar thermochemical looping conditions

NASA Astrophysics Data System (ADS)

Rothensteiner, Matthäus; Jenni, Joel; Emerich, Hermann; Bonk, Alexander; Vogt, Ulrich F.; van Bokhoven, Jeroen A.

2017-08-01

An in situ/operando flow cell for transmission mode X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), and combined XAS/XRD measurements in a single experiment under the extreme conditions of two-step solar thermochemical looping for the dissociation of water and/or carbon dioxide was developed. The apparatus exposes materials to relevant conditions of both the auto-reduction and the oxidation sub-steps of the thermochemical cycle at ambient temperature up to 1773 K and enables determination of the composition of the effluent gases by online quadrupole mass spectrometry. The cell is based on a tube-in-tube design and is heated by means of a focusing infrared furnace. It was tested successfully for carbon dioxide splitting. In combined XAS/XRD experiments with an unfocused beam, XAS measurements were performed at the Ce K edge (40.4 keV) and XRD measurements at 64.8 keV and 55.9 keV. Furthermore, XRD measurements with a focused beam at 41.5 keV were carried out. Equimolar ceria-hafnia was auto-reduced in a flow of argon and chemically reduced in a flow of hydrogen/helium. Under reducing conditions, all cerium(iv) was converted to cerium(iii) and a cation-ordered pyrochlore-type structure was formed, which was not stable upon oxidation in a flow of carbon dioxide.

In situ flow cell for combined X-ray absorption spectroscopy, X-ray diffraction, and mass spectrometry at high photon energies under solar thermochemical looping conditions.

PubMed

Rothensteiner, Matthäus; Jenni, Joel; Emerich, Hermann; Bonk, Alexander; Vogt, Ulrich F; van Bokhoven, Jeroen A

2017-08-01

An in situ/operando flow cell for transmission mode X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), and combined XAS/XRD measurements in a single experiment under the extreme conditions of two-step solar thermochemical looping for the dissociation of water and/or carbon dioxide was developed. The apparatus exposes materials to relevant conditions of both the auto-reduction and the oxidation sub-steps of the thermochemical cycle at ambient temperature up to 1773 K and enables determination of the composition of the effluent gases by online quadrupole mass spectrometry. The cell is based on a tube-in-tube design and is heated by means of a focusing infrared furnace. It was tested successfully for carbon dioxide splitting. In combined XAS/XRD experiments with an unfocused beam, XAS measurements were performed at the Ce K edge (40.4 keV) and XRD measurements at 64.8 keV and 55.9 keV. Furthermore, XRD measurements with a focused beam at 41.5 keV were carried out. Equimolar ceria-hafnia was auto-reduced in a flow of argon and chemically reduced in a flow of hydrogen/helium. Under reducing conditions, all cerium(iv) was converted to cerium(iii) and a cation-ordered pyrochlore-type structure was formed, which was not stable upon oxidation in a flow of carbon dioxide.

Structure and properties of solid polymer electrolyte based on chitosan and ZrO{sub 2} nanoparticle for lithium ion battery

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

Sudaryanto,, E-mail: dryanto@batan.go.id; Yulianti, Evi, E-mail: yulianti@batan.go.id; Patimatuzzohrah, E-mail: pzohrah@yahoo.com

In order to develop all solid lithium ion battery, study on the structure and properties of solid polymer electrolytes (SPE) based on chitosan has been done. The SPE were prepared by adding Zirconia (ZrO{sub 2}) nanoparticle and LiClO{sub 4} as lithium salt into the chitosan solution followed by casting method. Effect of the ZrO{sub 2} and salt concentration to the structure and properties of SPE were elaborated using several methods. The structure of the SPE cast film, were characterized mainly by using X-ray diffractometer (XRD). While the electrical properties of SPE were studied by electrochemical impedance spectrometer (EIS) and ionmore » transference number measurement. XRD profiles show that the addition of ZrO{sub 2} and LiClO{sub 4} disrupts the crystality of chitosan. The decrease in sample crytalinity with the nanoparticle and salt addition may increase the molecular mobility result in the increasing sample conductivity and cathionic transference number as determined by EIS and ion transference number measurement, respectively. The highest ionic conductivity (3.58×10{sup −4} S cm{sup −1}) was obtained when 4 wt% of ZrO{sub 2} nanoparticle and 40 wt% of LiClO{sub 4} salt were added to the chitosan. The ion transference number with that composition was 0.55. It is high enough to be used as SPE for lithium ion battery.« less

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Roosevelt Hot Springs, Utah FORGE X-Ray Diffraction Data

DOE Data Explorer

Nash, Greg; Jones, Clay

2018-02-07

This dataset contains X-ray diffraction (XRD) data taken from wells and outcrops as part of the DOE GTO supported Utah FORGE project located near Roosevelt Hot Springs. It contains an Excel spreadsheet with the XRD data, a text file with sample site names, types, and locations in UTM, Zone 12, NAD83 coordinates, and a GIS shapefile of the sample locations with attributes.

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

PubMed

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

2010-09-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

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

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

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

2014-04-01

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

X-Ray Amorphous Phases in Terrestrial Analog Volcanic Sediments: Implications for Amorphous Phases in Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Smith, R. J.; Horgan, B.; Rampe, E.; Dehouck, E.; Morris, R. V.

2017-01-01

X-ray diffraction (XRD) amorphous phases have been found as major components (approx.15-60 wt%) of all rock and soil samples measured by the CheMin XRD instrument in Gale Crater, Mars. The nature of these phases is not well understood and could be any combination of primary (e.g., glass) and secondary (e.g., allophane) phases. Amorphous phases form in abundance during surface weathering on Earth. Yet, these materials are poorly characterized, and it is not certain how properties like composition and structure change with formation environment. The presence of poorly crystalline phases can be inferred from XRD patterns by the appearance of a low angle rise (< or approx.10deg 2(theta)) or broad peaks in the background at low to moderate 2(theta) angles (amorphous humps). CheMin mineral abundances combined with bulk chemical composition measurements from the Alpha Particle X-ray Spectrometer (APXS) have been used to estimate the abundance and composition of the XRD amorphous materials in soil and rock samples on Mars. Here we apply a similar approach to a diverse suite of terrestrial samples - modern soils, glacial sediments, and paleosols - in order to determine how formation environment, climate, and diagenesis affect the abundance and composition of X-ray amorphous phases.

Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity.

PubMed

Liu, Yongliang; Thibodeaux, Devron; Gamble, Gary; Bauer, Philip; VanDerveer, Don

2012-08-01

Despite considerable efforts in developing curve-fitting protocols to evaluate the crystallinity index (CI) from X-ray diffraction (XRD) measurements, in its present state XRD can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous fraction in a sample. The greatest barrier to establishing quantitative XRD is the lack of appropriate cellulose standards, which are needed to calibrate the XRD measurements. In practice, samples with known CI are very difficult to prepare or determine. In a previous study, we reported the development of a simple algorithm for determining fiber crystallinity information from Fourier transform infrared (FT-IR) spectroscopy. Hence, in this study we not only compared the fiber crystallinity information between FT-IR and XRD measurements, by developing a simple XRD algorithm in place of a time-consuming and subjective curve-fitting process, but we also suggested a direct way of determining cotton cellulose CI by calibrating XRD with the use of CI(IR) as references.

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...

Study on preferred crystal orientations of Mg-Zr-O composite protective layer in AC-PDP

NASA Astrophysics Data System (ADS)

Bingang, G.; Chunliang, L.; Zhongxiao, S.; Liu, L.; Yufeng, F.; Xing, X.; Duowang, F.

2006-11-01

In order to study the preferred crystal orientations of Mg-Zr-O composite protective layers in PDP, Mg-Zr-O composite protective layers were deposited by Electron-beam Evaporator using (MgO+ZrO{2}) powder mixture as evaporation source material. X-ray diffractometer (XRD) was used to determine preferred crystal orientations of Mg-Zr-O composite protective layers, surface morphologies of films were analyzed by FESEM and voltage characteristics were examined in a testing macroscopic discharge cell of AC-PDP. On the basis of experimental analysis, the influence of oxide addition and deposition conditions on preferred orientations of Mg-Zr-O composite protective layers were investigated. The results showed that the preferred orientations of Mg-Zr-O films were determined by lattice distortion of MgO crystal. The deposition conditions have great effects on the preferred orientations of Mg-Zr-O films. The preferred orientations affect voltage characteristics through affecting surface morphology of Mg-Zr-O films. A small amount of Zr solution in MgO can decrease firing voltage compared with using pure MgO film. Firing voltage is closely related with the [ ZrO{2}/(MgO+ZrO{2})] ratio of evaporation source materials.

Synthesis and characterization of Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles as a magnetic drug delivery system

NASA Astrophysics Data System (ADS)

Ansari, Mohammad; Bigham, Ashkan; Hassanzadeh-Tabrizi, S. A.; Abbastabar Ahangar, H.

2017-10-01

Mixed spinel ferrite nanoparticles are being applied in biomedical applications due to their biocompatibility, antibacterial activity, particular magnetic and electronic properties with chemical and thermal stabilities. The Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles are synthesized through the thermal treatment method. Polyvinyl alcohol (PVA) is used as the capping agent to stabilize the particles and prevent their agglomeration. The synthesized nanoparticles are characterized through X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), N2 adsorption-desorption, field emission scanning electron microscopy (FESEM), and transmission electron microscope (TEM). The magnetic characterization is made on a vibrating sample magnetometer (VSM), which displayed super-paramagnetic behavior of the synthesized sample. Potential application of the Cu0.3Zn0.5Mg0.2Fe2O4 nanoparticles as a drug delivery agent is assessed in vitro by estimating their release properties. The obtained results indicate that the amount of ibuprofen (IBU) adsorbed into the nanocarrier of Cu0.3Zn0.5Mg0.2Fe2O4 is 104 mg/g and the drug release is sustained up to 72 h.

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

PubMed

Karuppuchamy, S; Brundha, C

2016-12-01

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

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

NASA Astrophysics Data System (ADS)

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

2012-10-01

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

Characterization and Surface Treatment of Materials Used in MADEAL S.A. Industry Productive Process of Rims by Plasma Assisted Repetitive Pulsed Arcs Technique

NASA Astrophysics Data System (ADS)

Jiménez, H.; Salazar, V. H.; Devia, A.; Jaramillo, S.; Velez, G.

2006-12-01

A study of materials used in the molds production to aluminium rims manufacture in the MADEAL S.A. factory was carried out for apply a plasma assisted surface treatment consists in growing TiAlN hard coatings that it protects this molds in the productive process. This coating resists high oxidation temperatures, of the other of 800 °C, high hardness (2800 Vickers) and low friction coefficient. A plasma assisted repetitive pulsed arcs mono-evaporator system was used in the grow of the TiAlN coatings, the TiAlN target is a sinterized 50% Ti and 50% Al, in the substrate they were used two types of steel that compose the molds injection pieces for the rims production. These materials were subjected to linear and fluctuating thermal changes in the Bruker axs X-Ray diffractometer temperature chamber, what simulated the molds thermal variation in the rims production process and they were compared with TiAlN coatings subjected to same thermal changes. The Materials characterization, before and later of thermal process, was carried out using XRD, SPM and EDS techniques, to analyze the crystallographic, topographic and chemical surface structure behaviours.

Characterization of Sb-doped Bi(2)UO(6) solid solutions by X-ray diffraction and X-ray absorption spectroscopy.

PubMed

Misra, N L; Yadav, A K; Dhara, Sangita; Mishra, S K; Phatak, Rohan; Poswal, A K; Jha, S N; Sinha, A K; Bhattacharyya, D

2013-01-01

The preparation and characterization of Sb-doped Bi(2)UO(6) solid solutions, in a limited composition range, is reported for the first time. The solid solutions were prepared by solid-state reactions of Bi(2)O(3), Sb(2)O(3) and U(3)O(8) in the required stoichiometry. The reaction products were characterized by X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) measurements at the Bi and U L(3) edges. The XRD patterns indicate the precipitation of additional phases in the samples when Sb doping exceeds 4 at%. The chemical shifts of the Bi absorption edges in the samples, determined from the XANES spectra, show a systematic variation only up to 4 at% of Sb doping and support the results of XRD measurements. These observations are further supported by the local structure parameters obtained by analysis of the EXAFS spectra. The local structure of U is found to remain unchanged upon Sb doping indicating that Sb(+3) ions replace Bi(+3) during the doping of Bi(2)UO(6) by Sb.

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

NASA Technical Reports Server (NTRS)

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

1986-01-01

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

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

NASA Technical Reports Server (NTRS)

2003-01-01

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

Performance of RF sputtered p-Si/n-ZnO nanoparticle thin film heterojunction diodes in high temperature environment

NASA Astrophysics Data System (ADS)

Singh, Satyendra Kumar; Hazra, Purnima

2017-04-01

In this article, temperature-dependent current-voltage characteristics of n-ZnO/p-Si nanoparticle thin film heterojunction diode grown by RF sputtering technique are analyzed in the temperature range of 300-433 k to investigate the performance of the device in high temperature environment. The microstructural, morphological, optical and temptrature dependent electrical properties of as-grown nanoparticle thin film were characterized by X-ray diffractometer (XRD), atomic force microscopy (AFM), field emmision scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), variable angle ellipsometer and semiconductor device analyzer. XRD spectra of as-grown ZnO films are exhibited that highly c-axis oriented ZnO nanostructures are grown on p- Si〈100〉 substrate whereas AFM and FESEM images confirm the homogeneous deposition of ZnO nanoparticles on surface of Si substratewith minimum roughness.The optical propertiesof as-grown ZnO nanoparticles have been measured in the spectral range of 300-800 nm using variable angle ellipsometer.To measure electrical parameters of the device prototype in the temperature range of room temperature (300 K) to 433 K, large area ohmic contacts were fabricated on both side of the ZnO/Si heterostructure. From the current-voltage charcteristics of ZnO/Si heterojunction device, it is observed that the device exhibits rectifing nature at room temperature. However, with increase in temperature, reverse saturation current and barrier height are found to increase, whereas ideality factor is started decreasing. This phenomenon confirms that barrier inhomogeneities are present at the interface of ZnO/Si heterojunction, as a result of lattice constant and thermal coefficient mismatch between Si and ZnO. Therefore, a modified value of Richardson constant [33.06 Acm-2K-2] has been extracted from the temperature-dependent electrical characteristics after assuming the Gaussian distribution of special barrier height inhomogeneities across the Si/ZnO interface which is close to its theoretical value [32 Acm-2K-2]. This result indicates that regardless of presence of barrier height inmogeneities, ZnO/Si heterojunction diode still hasability to perform well in high temperature environment.

Performing Mineral Hydration Experiments in the CheMin Diffractometer on Mars

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Yen, A. S.; Rampe, E. B.; Blake, D. F.; Chipera, S. J.; Morookian, J. M.; Ming, D. W.; Bristow, T. F.; Morris, R. V.; Geller, R.;

Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

NASA Technical Reports Server (NTRS)

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

2001-01-01

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

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

DTIC Science & Technology

2015-03-31

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

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

NASA Astrophysics Data System (ADS)

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

2008-08-01

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

Spectral properties of Dy3+ doped ZnAl2O4 phosphor

NASA Astrophysics Data System (ADS)

Prakash, Ram; Kumar, Sandeep; Mahajan, Rubby; Khajuria, Pooja; Kumar, Vinay; Choudhary, R. J.; Phase, D. M.

2018-05-01

Herein, Dy3+ doped ZnAl2O4 phosphor was synthesized by the solution combustion method. The synthesized phosphor was characterized by X-ray diffraction (XRD), photoluminescence (PL) spectroscopy, UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS). The phase purity of the phosphor was confirmed by the XRD studies that showed cubic symmetry of the synthesized phosphor. Under UV excitation (388 nm) the PL emission spectrum of the phosphor shows characteristic transition from the Dy3+ ion. A band gap of 5.2 eV was estimated from the diffused reflectance spectroscopy. The surface properties of the phosphor were studied using the X-ray photoelectron spectroscopy.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

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

NASA Astrophysics Data System (ADS)

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

2015-03-01

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

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

PubMed

Takayama, Yuki; Yonekura, Koji

2016-03-01

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

Laser-induced Multi-energy Processing in Diamond Growth

DTIC Science & Technology

2012-05-01

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

Photocatalyst of Perovskite CaTiO3 Nanopowder Synthesized from CaO derived from Snail Shell in Comparison with The Use of CaO and CaCO3

NASA Astrophysics Data System (ADS)

Fatimah, I.; Rahmadianti, Y.; Pudiasari, R. A.

2018-04-01

Calcium titanate belongs to the important group of compounds with a perovskite structure having high dielectric loss for various applications including photocatalysis mechanism. Refer to the principles of green chemistry, in this work preparation of CaTiO3 was conducted by using CaO derived from snail shell. Aim of this research are to study the physicochemical character of perovskite derived from snail shell and its comparison with CaO and CaCO3 as Ca sources. Material preparation was performed by solid reaction of Ca sources with TiO2 under comparison with CaO and CaCO3 precursors. Mixture of Ca sources with TiO2 in certain proportion were ground and calcined at the temperature of 200 °C for 2 hs. Materials were characterized by using X-ray diffractometer (XRD), Fourier Transform-Infra Red (FTIR) and the photocatalytic activity was tested by using methylene blue photooxidation. Perovskite synthesized using CaO derived from snail shell exhibits the similar XRD pattern with that were prepared by using CaO and CaCO3. From the photooxidation activity test, it is proven that CaTiO3 shows similar photocatalytic activity correspond to that were prepared by CaO and CaCO3. Utilazation of shell as agricultural waste of the synthesis of CaTiO3 perovskite is the novelty of this work. Furthermore, the study on material structure and photoactivity is the main focuses for the application in industry and environment.

X-ray absorption fine structure and x-ray diffraction studies of crystallographic grains in nanocrystalline FePd:Cu thin films

NASA Astrophysics Data System (ADS)

Krupinski, M.; Perzanowski, M.; Polit, A.; Zabila, Y.; Zarzycki, A.; Dobrowolska, A.; Marszalek, M.

2011-03-01

FePd alloys have recently attracted considerable attention as candidates for ultrahigh density magnetic storage media. In this paper we investigate FePd thin alloy film with a copper admixture composed of nanometer-sized grains. [Fe(0.9 nm)/Pd(1.1 nm)/Cu(d nm)]×5 multilayers were prepared by thermal deposition at room temperature in UHV conditions on Si(100) substrates covered by 100 nm SiO2. The thickness of the copper layer has been changed from 0 to 0.4 nm. After deposition, the multilayers were rapidly annealed at 600 °C in a nitrogen atmosphere, which resulted in the creation of the FePd:Cu alloy. The structure of alloy films obtained this way was determined by x-ray diffraction (XRD), glancing angle x-ray diffraction, and x-ray absorption fine structure (EXAFS). The measurements clearly showed that the L10 FePd:Cu nanocrystalline phase has been formed during the annealing process for all investigated copper compositions. This paper concentrates on the crystallographic grain features of FePd:Cu alloys and illustrates that the EXAFS technique, supported by XRD measurements, can help to extend the information about grain size and grain shape of poorly crystallized materials. We show that, using an appropriate model of the FePd:Cu grains, the comparison of EXAFS and XRD results gives a reasonable agreement.

Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

PubMed

Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

2009-09-01

Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

FT-IR and Zeta potential measurements on TiO nanoparticles

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

Singh, Jaiveer; Rathore, Ravi; Kaurav, Netram, E-mail: netramkaurav@yahoo.co.uk

2016-05-23

In the present investigation, ultrafine TiO particles have been synthesized successfully by thermal decomposition method. The sample was characterized by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. As-synthesized TiO nanoparticles have a cubic structure as characterized by power X-ray diffraction (XRD), which shows that TiO nanoparticles have narrow size distribution with particle size 11.5 nm. FTIR data shows a strong peak at 1300 cm{sup −1}, assignable to the Ti-O stretching vibrations mode.

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

NASA Astrophysics Data System (ADS)

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

2001-06-01

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

Touch-free in situ investigation of ancient Egyptian pigments.

PubMed

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

2000-06-01

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

The binary system K2SO4CaSO4

USGS Publications Warehouse

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

1965-01-01

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

Growth and magnetoelectric properties of (00l)-oriented La{sub 0.67}Sr{sub 0.33}MnO{sub 3}/PbZr{sub 0.52}Ti{sub 0.48}O{sub 3} heterostructure films

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

Yan, Fuxue, E-mail: yanfuxue@126.com; Han, Kai, E-

2017-02-15

C-axis oriented La{sub 0.67}Sr{sub 0.33}MnO{sub 3}(LSMO)/PbZr{sub 0.52}Ti{sub 0.48}O{sub 3}(PZT) films are fabricated successfully by sol-gel method on LaAlO{sub 3} (00l) substrates. The structure, composition and morphology of the films are investigated by X-ray diffractometer (XRD, θ-2θ scan, ω-scan and ϕ-scan), X-ray photoelectron spectroscope (XPS), field emission scanning electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). The electric and magnetic properties of randomly and c-axis oriented LSMO/PZT films are studied comparably using ferroelectric testing apparatus and physical property measurement system (PPMS). It is found that the epitaxial LSMO/PZT composite films show well controlled growth along c-axis, and much bettermore » magnetoelectric properties than the randomly oriented ones. The ME voltage coefficient increases from 23 mV cm{sup −1} Oe{sup −1} for the randomly oriented LSMO/PZT composite films to 52 mV cm{sup −1} Oe{sup −1} for c-axis oriented ones prepared using the low cost sol-gel method presented in this study, which shows high potential in promising applications. - Highlights: •Epitaxial LSMO/PZT films were fabricated successfully by sol-gel method on LAO (00l) substrate. •The prepared films exhibit well-defined multiferroic properties for the epitaxial LSMO/PZT films. •Epitaxial LSMO/PZT films show superior magnetoelectric properties to the randomly oriented ones.« less

Adsorption of Benzoic Acid in Aqueous Solution by Bagasse Fly Ash

NASA Astrophysics Data System (ADS)

Suresh, S.

2012-09-01

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

Effects of low-alkalinity binders on stabilization/solidification of geogenic As-containing soils: Spectroscopic investigation and leaching tests.

PubMed

Li, Jiang-Shan; Wang, Lei; Cui, Jin-Li; Poon, Chi Sun; Beiyuan, Jingzi; Tsang, Daniel C W; Li, Xiang-Dong

2018-08-01

The low-alkalinity stabilization/solidification (S/S) treatment of the soil containing high concentrations of geogenic As by physical encapsulation is considered as a proper management before land development; however, the choice of an effective binder and the leaching potential of As remain uncertain. In this study, the influence of S/S binders (cement blended with fuel ash (FA), furnace bottom ash (FBA), or ground granulated blast furnace slag (GGBS)) on the speciation and leaching characteristics of geogenic As was studied. The results of X-ray diffractometer (XRD) and X-ray photoelectron spectroscopy (XPS) showed the reduced amount of calcium silicate hydrate phase and the decrease in oxidation state of As(V)-O on the surface of Fe(III) oxides/hydroxides in the low-alkalinity S/S treated soils. This might be due to the binder incorporation and change in pH conditions, which slightly affected the As-Fe interaction and increased the non-specifically sorbed species of As. Therefore, the S/S treatment increased the leachability and bioaccessibility of geogenic As to varying degree but decreased the phyto-extractable As. The S/S treatment by cement incorporating 25% of class C fly ash (O4C1) could achieve comparable or better performance, while reducing the risk assessment code (RAC) to a greater extent compared to that of using cement only. This study illustrates the effectiveness and limitations of low-alkalinity binders (e.g., O4C1) for geogenic As immobilization and encapsulation, which provides a new insight for determining the appropriate S/S binder in soil remediation. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-01-01

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

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

NASA Astrophysics Data System (ADS)

Song, Xiaolan; Wang, Yi; An, Chongwei

2018-06-01

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

Anisotropically biaxial strain in non-polar (112-0) plane In x Ga1-x N/GaN layers investigated by X-ray reciprocal space mapping.

PubMed

Zhao, Guijuan; Li, Huijie; Wang, Lianshan; Meng, Yulin; Ji, Zesheng; Li, Fangzheng; Wei, Hongyuan; Yang, Shaoyan; Wang, Zhanguo

2017-07-03

In this study, the indium composition x as well as the anisotropically biaxial strain in non-polar a-plane In x Ga 1-x N on GaN is studied by X-ray diffraction (XRD) analysis. In accordance with XRD reciprocal lattice space mapping, with increasing indium composition, the maximum of the In x Ga 1-x N reciprocal lattice points progressively shifts from a fully compressive strained to a fully relaxed position, then to reversed tensile strained. To fully understand the strain in the ternary alloy layers, it is helpful to grow high-quality device structures using a-plane nitrides. As the layer thickness increases, the strain of In x Ga 1-x N layer releases through surface roughening and the 3D growth-mode.

Unusual Thermal Stability of High-Entropy Alloy Amorphous Structure

DTIC Science & Technology

2012-06-20

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

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

NASA Astrophysics Data System (ADS)

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

2002-10-01

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

A comparison of techniques for nondestructive composition measurements in CdZnTe substrates

NASA Astrophysics Data System (ADS)

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

1995-05-01

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

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.

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

DTIC Science & Technology

2010-08-24

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

X-ray peak profile analysis of zinc oxide nanoparticles formed by simple precipitation method

NASA Astrophysics Data System (ADS)

Pelicano, Christian Mark; Rapadas, Nick Joaquin; Magdaluyo, Eduardo

2017-12-01

Zinc oxide (ZnO) nanoparticles were successfully synthesized by a simple precipitation method using zinc acetate and tetramethylammonium hydroxide. The synthesized ZnO nanoparticles were characterized by X-ray Diffraction analysis (XRD) and Transmission Electron Microscopy (TEM). The XRD result revealed a hexagonal wurtzite structure for the ZnO nanoparticles. The TEM image showed spherical nanoparticles with an average crystallite size of 6.70 nm. For x-ray peak analysis, Williamson-Hall (W-H) and Size-Strain Plot (SSP) methods were applied to examine the effects of crystallite size and lattice strain on the peak broadening of the ZnO nanoparticles. Based on the calculations, the estimated crystallite sizes and lattice strains obtained are in good agreement with each other.

First X-Ray Diffraction Results from Mars Science Laboratory: Mineralogy of Rocknest Aeolian Bedform at Gale Crater

NASA Technical Reports Server (NTRS)

Bish, D. L.; Blake, D. F.; Vaniman, D. T.; Chipera, S. J.; Sarrazin, P.; Morris, R. V.; Ming, D. W.; Treiman, A. H.; Downs, R. T.; Morrison, S. M.;

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

PubMed

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

2016-07-04

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

Structure, Elastic Constants and XRD Spectra of Extended Solids under High Pressure

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

Batyrev, I. G.; Coleman, S. P.; Ciezak-Jenkins, J. A.

We present results of evolutionary simulations based on density functional calculations of a potentially new type of energetic materials called extended solids: P-N and N-H. High-density structures with covalent bonds generated using variable and fixed concentration methods were analysed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction (XRD) spectra. X-ray diffraction spectra were calculated using a virtual diffraction algorithm that computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculated XRD patterns were used to search for the structure of extended solids present at experimental pressures by optimizing data accordingmore » to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Elastic constants has been calculated for thermodynamically stable structures of P-N system.« less

In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Blake, D.; Vaniman, D.; Chang, Sherwood (Technical Monitor)

1996-01-01

Remote observations of Mars have led scientists to believe that its early climate was similar to that of the early Earth, having had abundant liquid water and a dense atmosphere. One of the most fascinating questions of recent times is whether simple bacterial life developed on Mars (as it did on the Earth) during this early element period. Analyses of SNC meteorites have broadened considerably our knowledge of the chemistry of certain types of Martian rocks, underscoring the tantalizing possibility of early hydrothermal systems and even of ancient bacterial life. Detailed analyses of SNC meteorites in Terrestrial laboratories utilize the most sophisticated organic, isotopic and microscopic techniques in existence. Indeed; it is unlikely that the key biogenic indicators used in McKay et al (ibid) could be identified by a remote instrument on the surface of Mars. As a result, it is probable that any robotic search for evidence of an ancient Martian biosphere will have as its focus the identification of key minerals in likely host rocks rather than the direct detection of organic or isotopic biomarkers. Even on a sample return mission, mineralogical screening will be utilized to choose the most likely candidate rocks. X-ray diffraction (XRD) is the only technique that can provide a direct determination of the crystal structures of the phases present within a sample. When many different crystalline phases are present, quantitative analysis is better constrained if used in conjunction with a determination of elemental composition, obtainable by X-ray fluorescence (XRF) using the same X-ray source as for XRD. For planetary surface analysis, a remote instrument combining XRD and XRF could be used for mineralogical characterization of both soils and rocks. We are designing a remote XRD/XRF instrument with this objective in mind. The instrument concept pays specific attention to constraints in sample preparation, weight, volume, power, etc. Based on the geometry of a pinhole camera (transmission geometry, flat two-dimensional detector perpendicular to the direct beam), the instrument (which we call CHEMIN, for Chemistry and Mineralogy) uses an X-ray sensitive CCD detector which will allow concurrent positional and energy-dispersive analysis of collected photons. Thus XRF (energy) and XRD (geometry) analysis of transmitted X-rays will be performed at the same time. Tests performed with single minerals and simple mixtures give promising results. Refinements of the prototype promise interpretable results on complex samples.

Applications of High Throughput (Combinatorial) Methodologies to Electronic, Magnetic, Optical, and Energy-Related Materials

DTIC Science & Technology

2013-06-17

of the films without having to fabricate capacitors. In addition, the use of X - ray diffraction (XRD) analysis enabled Chikyow et al.40 to identify an...effects of Al doping and annealing on the thermal stabil- ity of the Y2O3/Si gate stack were studied by X - ray photoemission spectroscopy (XPS) and X - ray ...the major diffraction features in the phase distribution. For a given structural phase, the X - ray peak intensity allows one to track the compositional

X-ray scattering signatures of β-thalassemia

NASA Astrophysics Data System (ADS)

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

2009-08-01

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

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

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

Final Report for X-ray Diffraction Sample Preparation Method Development

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

Ely, T. M.; Meznarich, H. K.; Valero, T.

WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

Synthesis and Properties of Ortho-Nitro-Fe Complex

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

Mishra, A.; Mishra, Niyati; Sharma, R.

2011-07-15

Ortho-Nitro-Fe complex (Transition metal complex) has synthesized by chemical route method and properties of made complex has characterized by X-Ray diffraction (XRD), Moessbauer spectroscopy, Fourier transformation infra-red spectroscopy (FTIR) and X-Ray photoelectron spectroscopy (XPS). XRD analysis shows that sample is crystalline in nature and having particle size in the range of few nano meters. Moessbauer spectroscopy at room temperature shows the oxidation state of Iron (central metal ion) after complaxasion. FTIR spectra of the complex confirms the coordination of metal ion with ligand.

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.

Texture analysis at neutron diffractometer STRESS-SPEC

NASA Astrophysics Data System (ADS)

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

2011-06-01

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

X-ray physico-chemical imaging during activation of cobalt-based Fischer-Tropsch synthesis catalysts

NASA Astrophysics Data System (ADS)

Beale, Andrew M.; Jacques, Simon D. M.; Di Michiel, Marco; Mosselmans, J. Frederick W.; Price, Stephen W. T.; Senecal, Pierre; Vamvakeros, Antonios; Paterson, James

2017-11-01

The imaging of catalysts and other functional materials under reaction conditions has advanced significantly in recent years. The combination of the computed tomography (CT) approach with methods such as X-ray diffraction (XRD), X-ray fluorescence (XRF) and X-ray absorption near-edge spectroscopy (XANES) now enables local chemical and physical state information to be extracted from within the interiors of intact materials which are, by accident or design, inhomogeneous. In this work, we follow the phase evolution during the initial reduction step(s) to form Co metal, for Co-containing particles employed as Fischer-Tropsch synthesis (FTS) catalysts; firstly, working at small length scales (approx. micrometre spatial resolution), a combination of sample size and density allows for transmission of comparatively low energy signals enabling the recording of `multimodal' tomography, i.e. simultaneous XRF-CT, XANES-CT and XRD-CT. Subsequently, we show high-energy XRD-CT can be employed to reveal extent of reduction and uniformity of crystallite size on millimetre-sized TiO2 trilobes. In both studies, the CoO phase is seen to persist or else evolve under particular operating conditions and we speculate as to why this is observed. This article is part of a discussion meeting issue 'Providing sustainable catalytic solutions for a rapidly changing world'.

Phosphorus Effects of Mesoporous Bioactive Glass on Occlude Exposed Dentin

PubMed Central

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

2013-01-01

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

Nonstoichiometric Zn Ferrite and ZnFe2O4/Fe2O3 Composite Spheres: Preparation, Magnetic Properties, and Chromium Removal

NASA Astrophysics Data System (ADS)

Hang, Chun-Liang; Yang, Li-Xia; Sun, Chang-Mei; Liang, Ying

2018-03-01

Monodisperse and porous nonstoichiometric Zn ferrite can be prepared by a solvothermal method. Such non-Zn ferrite was used to be the precursor for synthesis of ZnFe2O4/Fe2O3 composite via calcination at 600°C for 3 h in air. X-ray powder diffractometer (XRD) and Energy Dispersive Spectrometer (EDS) proved the nonstoichiometry of Zn ferrite synthesized by solvothermal method and the formation of ZnFe2O4/Fe2O3 composite via calcination. TEM image showed that non-Zn ferrite spheres with wormlike nanopore structure were made of primary nanocrystals. BET surface area of non-Zn ferrite was much higher than that of ZnFe2O4/Fe2O3 composite. Saturation magnetization of non-Zn ferrites was significantly higher than that of ZnFe2O4/Fe2O3 composites. Calcination of non-Zn ferrite resulted in the formation of large amount of non-magnetic Fe2O3,which caused a low magnetization of composite. Because of higher BET surface area and higher saturation magnetization, non-Zn ferrite presented better Cr6+ adsorption property than ZnFe2O4/Fe2O3 composites.

Surface properties, crystallinity and optical properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

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

Chuan, Lee Te, E-mail: gd130079@siswa.uthm.edu.my; Abdullah, Hasan Zuhudi, E-mail: hasan@uthm.edu.my; Idris, Maizlinda Izwana, E-mail: izwana@uthm.edu.my

Anodic oxidation is an electrochemical method for the production of ceramic films on a metallic substrate. It had been widely used to deposit the ceramic coatings on the metals surface. This method has been widely used in surface modification of biomaterials especially for dental implants. In this study, the surface morphology, crystallinity and optical properties of titanium foil was modified by anodising in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA). The experiments were carried out at high voltage (350 V), different anodising time (5 and 10 minutes) and current density (10-70 mA.cm{sup −2}) at room temperature. Anodisedmore » titanium was characterised by using field emission scanning electron microscopy (FESEM), X-ray diffractometer (XRD), and UV-Vis spectrometry. The result of the experiment showed that surface morphology, crystallinity and optical properties depended strongly on the current density and anodising time. More porous surface and large amount of anatase and rutile was produced at higher current density and longer anodising time. Apart from that, it is also revealed that the energy band gap of anodised titanium increases as the increase in current density due to the presence of anatase and rutile TiO{sub 2}.« less

Role of annealing temperature on microstructural and electro-optical properties of ITO films produced by sputtering

NASA Astrophysics Data System (ADS)

Senol, Abdulkadir; Gulen, Mahir; Yildirim, Gurcan; Ozturk, Ozgur; Varilci, Ahmet; Terzioglu, Cabir; Belenli, Ibrahim

2013-03-01

In this study, we investigate the effect of annealing temperature on electrical, optical and microstructural properties of indium tin oxide (ITO) films deposited onto Soda lime glass substrates by conventional direct current (DC) magnetron reactive sputtering technique at 100 watt using an ITO ceramic target (In2O3:SnO2, 90:10 wt. %) in argon atmosphere at room temperature. The films obtained are exposed to the calcination process at different temperature up to 700 ° C. Resistivity, Hall Effect, X-ray diffractometer (XRD), ultra violet-visible spectrometer (UV-vis) and atomic force microscopy (AFM) measurements are performed to characterize the samples. Moreover, phase purity, surface morphology, optical and photocatalytic properties of the films are compared with each other. Furthermore, mobility, carrier density and conductivity characteristics of the samples prepared are carried out as function of temperature in the range of 80-300 K at the magnetic field of 0.550 T. The results obtained show that all the properties depend strongly on the annealing temperature and in fact the film annealed at 400 ° C obtains the better optical properties due to the high refractive index while the film produced at 100 °C exhibits much better photoactivity than the other films as a result of the large optical energy band gap.

Degradation phenomena of magnetic attachments used clinically in the oral environment

NASA Astrophysics Data System (ADS)

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

2006-08-01

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

Correlating capacity and Li content in layered material for Li-ion battery using XRD and particle size distribution measurements

NASA Astrophysics Data System (ADS)

Al-Tabbakh, A. A. A.; Al-Zubaidi, A. B.; Kamarulzaman, N.

2016-03-01

A lithiated transition-metal oxide material was successfully synthesized by a combustion method for Li-ion battery. The material was characterized using thermogravimetric and particle size analyzers, scanning electron microscope and X-ray diffractometer. The calcined powders of the material exhibited a finite size distribution and a single phase of pure layered structure of space group Roverline{3} m . An innovative method was developed to calculate the material electrochemical capacity based on considerations of the crystal structure and contributions of Li ions from specified unit cells at the surfaces and in the interiors of the material particles. Results suggested that most of the Li ions contributing to the electrochemical current originated from the surface region of the material particles. It was possible to estimate the thickness of the most delithiated region near the particle surfaces at any delithiation depth accurately. Furthermore, results suggested that the core region of the particles remained electrochemically inaccessible in the conventional applied voltages. This result was justified by direct quantitative comparison of specific capacity values calculated from the particle size distribution with those measured experimentally. The present analysis is believed to be of some value for estimation of the failure mechanism in cathode compounds, thus assisting the development of Li-ion batteries.

A Nanoporous Carbon/Exfoliated Graphite Composite For Supercapacitor Electrodes

NASA Astrophysics Data System (ADS)

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

2010-12-01

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

Geochemical Identification in Sediment Provenance during Glacial/Interglacial Period: the Southern Drake Passage

NASA Astrophysics Data System (ADS)

Park, Y. K.; Jung, J.; Lee, J. I.; Yoo, K. C.; Kim, J. W.

2016-12-01

Clay mineralogy and crystal size distribution in marine sediment is used for the indication of a sediment provenance and climatic changes. Objective of this study is to trace the sediment provenances in the Southern Drake Passage with clay mineralogy, elemental composition and crystal size distributions (CSDs) of clay mineral. In the present study, X-Ray Diffractometer (XRD) measurements showed that smectite, illite and chlorite are dominant phases. The semi-quantitative analysis showed that the relatively proportion of smectite is 50 - 60% in interglacial stage, 30 - 39% in glacial stage. Comparing with REE data, sediments supply was influenced by Weddell sea current and Antarctic Circumpolar Current (ACC). Moreover, elemental composition and microscopic analysis of smectites were carried by Transmission Electron Microscopy (TEM) and energy dispersive spectroscopy (EDS). The composition of smectite clay minerals were plotted on the tertiary diagram indicating that Smectite in Drake Passage was transported from three provenances: South Shetland island, east and west side of Antarctic peninsula during glacial - interglacial period. The CSDs of smectite also indicate the various source of smectite. The variation in the values of α (mean thickness) and β2 (shape or uniformity of the distribution) of smectite grain size will be discussed in terms of the sediment provenance.

Investigation of magnetic properties on spin-ordering effects of FeGa2S4 and FeIn2S4

NASA Astrophysics Data System (ADS)

Myoung, Bo Ra; Lim, Jung Tae; Kim, Chul Sung

2017-09-01

We have studied crystal and magnetic properties of chalcogenides FeGa2S4 and FeIn2S4 with X-ray diffractometer (XRD), magnetic property measurement system (MPMS), magnetometer, physical property measurement system (PPMS), and Mössbauer spectrometer. The crystal structure has 2-dimension triangular lattice structure with P-3m1 of FeGa2S4, while FeIn2S4 has inverse spinel with space group Fd3m. The AC magnetic susceptibility measurements show that FeGa2S4 is an insulating spin glass material, exhibiting geometrical frustration, unlike in the antiferromagnetic [AFM] metallic spin glass FeIn2S4. From hysteresis (M-H) curves at 4.2 K, FeGa2S4 has spin-flop behavior with an angle of 120° of triangle, as against linear slope of FeIn2S4 due to anti-parallel spin. The gap energy by splitting of 5T2g, Δ1 and electric quadrupole splitting ΔEQ of FeIn2S4 are much higher than that of FeGa2S4 at 4.2 K because FeGa2S4 is geometrically frustrated magnet having degenerate ground state at low temperature.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Surface properties, crystallinity and optical properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

NASA Astrophysics Data System (ADS)

Chuan, Lee Te; Abdullah, Hasan Zuhudi; Idris, Maizlinda Izwana

2015-07-01

Anodic oxidation is an electrochemical method for the production of ceramic films on a metallic substrate. It had been widely used to deposit the ceramic coatings on the metals surface. This method has been widely used in surface modification of biomaterials especially for dental implants. In this study, the surface morphology, crystallinity and optical properties of titanium foil was modified by anodising in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA). The experiments were carried out at high voltage (350 V), different anodising time (5 and 10 minutes) and current density (10-70 mA.cm-2) at room temperature. Anodised titanium was characterised by using field emission scanning electron microscopy (FESEM), X-ray diffractometer (XRD), and UV-Vis spectrometry. The result of the experiment showed that surface morphology, crystallinity and optical properties depended strongly on the current density and anodising time. More porous surface and large amount of anatase and rutile was produced at higher current density and longer anodising time. Apart from that, it is also revealed that the energy band gap of anodised titanium increases as the increase in current density due to the presence of anatase and rutile TiO2.

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

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

Nagler, Stephen E; Mook Jr, Herbert A

2008-01-01

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

Structural investigations in helium charged titanium films using grazing incidence XRD and EXAFS spectroscopy

NASA Astrophysics Data System (ADS)

Wan, Chubin; Zhou, Xiaosong; Wang, Yuting; Li, Shina; Ju, Xin; Peng, Shuming

2014-01-01

The crystal structure and local atomic arrangements surrounding Ti atoms were determined for He-charged hexagonal close-packed (hcp) Ti films and measured at glancing angles by synchrotron radiation X-ray diffraction (XRD) and extended X-ray absorption fine structure (EXAFS) spectroscopy, respectively. The charged specimens were prepared by direct current magnetron sputtering with a He/Ar mixture. He atoms with a relatively medium concentration (He/Ti atomic ratio as high as 17 at.%) were incorporated evenly in the deposited films. XRD results showed the changes in the peak intensities in Ti films with different He contents. EXAFS Fourier Transform analysis indicated that the average Ti-Ti distance decreased significantly, and proved the existence of phase transition.

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

DOE PAGES

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

2016-06-16

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

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

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

Soft x-ray measurements using photoconductive type-IIa and single-crystal chemical vapor deposited diamond detectors

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

Moore, A. S.; Bentley, C. D.; Foster, J. M.

2008-10-15

Photoconductive detectors (PCDs) are routinely used alongside vacuum x-ray diodes (XRDs) to provide an alternative x-ray flux measurement at laser facilities such as HELEN at AWE Aldermaston, UK, and Omega at the Laboratory for Laser Energetics. To evaluate diamond PCDs as an alternative to XRD arrays, calibration measurements made at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory are used to accurately calculate the x-ray flux from a laser-heated target. This is compared to a flux measurement using the Dante XRD diagnostic. Estimates indicate that the photoinduced conductivity from measurements made at Omega are too large, and calculationsmore » using the radiometric calibrations made at the NSLS agree with this hypothesis. High-purity, single-crystal, chemical vapor deposited (CVD) diamond samples are compared to natural type-IIa PCDs and show promising high resistivity effects, the corollary of which preliminary results show is a slower response time.« less

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

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

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

2015-03-15

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

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

PubMed

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

2004-10-01

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

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

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

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

2014-11-15

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

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

NASA Astrophysics Data System (ADS)

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

2014-11-01

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

Intrinsic ferromagnetism in nanocrystalline Mn-doped ZnO depending on Mn concentration.

PubMed

Subramanian, Munisamy; Tanemura, Masaki; Hihara, Takehiko; Soga, Tetsuo; Jimbo, Takashi

2011-04-01

The physical properties of Zn(1-x)Mn(x)O nanoparticles synthesized by thermal decomposition are extensively investigated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman light scattering and Hysteresis measurements. XRD and XPS spectra reveal the absence of secondary phase in nanocrystalline ZnO doped with 5% or less Mn; and, later confirms that the valance state of Mn to be 2+ for all the samples. Raman spectra exhibit a peak at 660 cm(-1) which we attribute to the intrinsic lattice defects of ZnO with increasing Mn concentration. Overall, our results demonstrate that ferromagnetic properties can be realized while Mn-doped ZnO obtained in the nanocrystalline form.

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

The first X-ray diffraction measurements on Mars.

PubMed

Bish, David; Blake, David; Vaniman, David; Sarrazin, Philippe; Bristow, Thomas; Achilles, Cherie; Dera, Przemyslaw; Chipera, Steve; Crisp, Joy; Downs, R T; Farmer, Jack; Gailhanou, Marc; Ming, Doug; Morookian, John Michael; Morris, Richard; Morrison, Shaunna; Rampe, Elizabeth; Treiman, Allan; Yen, Albert

2014-11-01

The Mars Science Laboratory landed in Gale crater on Mars in August 2012, and the Curiosity rover then began field studies on its drive toward Mount Sharp, a central peak made of ancient sediments. CheMin is one of ten instruments on or inside the rover, all designed to provide detailed information on the rocks, soils and atmosphere in this region. CheMin is a miniaturized X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that uses transmission geometry with an energy-discriminating CCD detector. CheMin uses onboard standards for XRD and XRF calibration, and beryl:quartz mixtures constitute the primary XRD standards. Four samples have been analysed by CheMin, namely a soil sample, two samples drilled from mudstones and a sample drilled from a sandstone. Rietveld and full-pattern analysis of the XRD data reveal a complex mineralogy, with contributions from parent igneous rocks, amorphous components and several minerals relating to aqueous alteration. In particular, the mudstone samples all contain one or more phyllosilicates consistent with alteration in liquid water. In addition to quantitative mineralogy, Rietveld refinements also provide unit-cell parameters for the major phases, which can be used to infer the chemical compositions of individual minerals and, by difference, the composition of the amorphous component.

Casein phosphopeptide-amorphous calcium phosphate remineralization of primary teeth early enamel lesions.

PubMed

Zhou, Chunhua; Zhang, Dongliang; Bai, Yuxing; Li, Song

2014-01-01

Early childhood caries (ECC) is a serious problem that progresses rapidly and often goes untreated. Current traumatic treatments may be replaced by safe and effective remineralization at very early stages. The aim of this in vitro study was to evaluate the remineralization effects of casein phosphopeptide-amorphous calcium phosphate (CPP-ACP) paste on enamel lesions by assessing ultrastructure, nanomechanical properties, and compound and elemental analysis. Enamel specimens from 6-year-old children were divided into groups: (1) native enamel; (2) water as negative control; (3) 500ppm NaF as positive control; and (4-7) CPP-ACP paste for 4, 8, 12, and 24h, as test groups. Ultrastructure and roughness were observed by atomic force microscopy (AFM); nanohardness and elastic modulus were measured by nanoindentation; compound and crystal size of enamel surface patterns were investigated by X-ray diffractometer (XRD). An electron microprobe (EPMA) was used for element analysis. Data were analyzed using one-way ANOVA. The CPP-ACP paste repaired the microstructure of enamel, including prism and interprism, through significantly increased hydroxyapatite crystal size (12.06±0.21nm) and Ca/P molar ratios (1.637±0.096) as compared with NaF (8.56±0.13nm crystal size and 1.397±0.086 Ca/P, p<0.01). Both CPP-ACP and NaF decrease roughness, and increase the nanohardness and elastic modulus, with no significant differences between the materials. The CPP-ACP paste is more suitable for children than NaF, due to advantages for remineralization. The AFM, nanoindentation, EPMA, and XRD are very helpful methods for further understanding of microscale and nanoscale remineralization mechanisms. Copyright © 2013 Elsevier Ltd. All rights reserved.

Characterizing the Phyllosilicate Component of the Sheepbed Mudstone in Gale Crater, Mars Using Laboratory XRD and EGA

NASA Technical Reports Server (NTRS)

Rampe, E. B.; Morris, R. V.; Ming, D. W.; Archer, P. D.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Blake, D. F.; Bristow, T. F.; Sutter, B.;

Chemical Characterization of an Ayurvedic Herbo-Mineral Formulation - Vasantakusumākara Rasa: A Potential Tool for Quality Assurance.

PubMed

Ota, Sarada; Singh, Arjun; Srikanth, Narayana; Sreedhar, Bojja; Ruknuddin, Galib; Dhiman, Kartar Singh

2017-01-01

Herbo-mineral formulations of Ayurveda contain specified metals or minerals as composition, which have their beneficial effects on biological systems. These metals or minerals are transformed into non-toxic forms through meticulous procedures explained in Ayurveda. Though literature is available on quality aspects of such herbo-mineral formulations; contemporary science is raising concerns at regular intervals on such formulations. Thus, it becomes mandate to develop quality profiles of all formulations that contain metals or minerals in their composition. Considering this, it is planned to evaluate analytical profile of Vasantakusumākara Rasa . To prepare Vasantakusumākara Rasa as per Standard operating Procedures (SoP) mentioned in classical text and to characterize it chemically using modern analytical techniques. The drug ( Vasantakusumākara Rasa ) in three batches was prepared in GMP certified pharmacy. Physico-chemical analysis, Assay of elements and HPTLC were carried out as per API. XRD was conducted using Rigaku Ultima-IV X-ray diffractometer. The analysis shown the presence of Mercury, Tin, Gold, Silver, Iron, Zinc and Calcium etc., and HPTLC revealed presence of organic constituents from plant material. The XRD indicated the presence of cinnabar (mercury sulphide from Rasa Sindhura ), cassiterite (tin oxide from Vaṅga Bhasma ), massicot (lead oxide from Nāga bhasma ) and Magnetite (di-iron oxide from Loha bhasma ). The physico chemical analysis reveals that VKR prepared by following classical guidelines is very effective in converting the macro elements into therapeutically effective medicines in micro form. Well prepared herbo-mineral drugs offer many advantages over plant medicines due to their longer shelf life, lesser doses, easy storing facilities, better palatability etc. The inferences and the standards laid down in this study certainly can be utilized as baseline data of standardization and QC.

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

PubMed

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

2001-06-01

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

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.

Room Temperature Tunable Multiferroic Properties in Sol-Gel-Derived Nanocrystalline Sr(Ti1−xFex)O3−δ Thin Films

PubMed Central

Wang, Yi-Guang; Liu, Qiu-Xiang; Jiang, Yan-Ping; Jiang, Li-Li

2017-01-01

Sr(Ti1−xFex)O3−δ (0 ≤ x ≤ 0.2) thin films were grown on Si(100) substrates with LaNiO3 buffer-layer by a sol-gel process. Influence of Fe substitution concentration on the structural, ferroelectric, and magnetic properties, as well as the leakage current behaviors of the Sr(Ti1−xFex)O3−δ thin films, were investigated by using the X-ray diffractometer (XRD), atomic force microscopy (AFM), the ferroelectric test system, and the vibrating sample magnetometer (VSM). After substituting a small amount of Ti ion with Fe, highly enhanced ferroelectric properties were obtained successfully in SrTi0.9Ti0.1O3−δ thin films, with a double remanent polarization (2Pr) of 1.56, 1.95, and 9.14 μC·cm−2, respectively, for the samples were annealed in air, oxygen, and nitrogen atmospheres. The leakage current densities of the Fe-doped SrTiO3 thin films are about 10−6–10−5 A·cm−2 at an applied electric field of 100 kV·cm−1, and the conduction mechanism of the thin film capacitors with various Fe concentrations has been analyzed. The ferromagnetic properties of the Sr(Ti1−xFex)O3−δ thin films have been investigated, which can be correlated to the mixed valence ions and the effects of the grain boundary. The present results revealed the multiferroic nature of the Sr(Ti1−xFex)O3−δ thin films. The effect of the annealing environment on the room temperature magnetic and ferroelectric properties of Sr(Ti0.9Fe0.1)O3−δ thin films were also discussed in detail. PMID:28885579

Destination Innovation: Episode 4 CheMin

NASA Image and Video Library

2012-08-02

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

Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

PubMed Central

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

Structural analysis of emerging ferrite: Doped nickel zinc ferrite

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

Kumar, Rajinder; Kumar, Hitanshu; Singh, Ragini Raj

2015-08-28

Ni{sub 0.6-x}Zn{sub 0.4}Co{sub x}Fe{sub 2}O{sub 4} (x = 0, 0.033, 0.264) nanoparticles were synthesized by sol-gel method and annealed at 900°C. Structural properties of all prepared samples were examined with X-ray diffraction (XRD). The partial formation of hematite (α-Fe{sub 2}O{sub 3}) secondary phase with spinel phase cubic structure of undoped and cobalt doped nickel zinc ferrite was found by XRD peaks. The variation in crystallite size and other structural parameters with cobalt doping has been calculated for most prominent peak (113) of XRD and has been explained on the basis of cations ionic radii difference.

Structural, magnetic and electronic structural properties of Mn doped CeO2 nanoparticles

NASA Astrophysics Data System (ADS)

Kumari, Kavita; Vij, Ankush; Hashim, Mohd.; Chae, K. H.; Kumar, Shalendra

2018-05-01

Nanoparticles of Ce1-xMnxO2, (x=0.0, 0.01, and 0.05) have been synthesized by using co-precipitation method, and then characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), near edge x-ray absorption fine structure (NEXAFS) spectroscopy and dc magnetization measurements. XRD results clearly showed that the all the samples have single phase nature and exclude the presence of any secondary phase. The average particle size calculated using XRD TEM measurements found to decrease with increase in Mn doping in the range of 4.0 - 9.0 nm. The structural parameters such as strain, interplaner distance and lattice parameter is observed to decrease with increase in doping. The morphology of Ce1-xMnxO2 nanoparticles measured using TEM micrographs indicate that nanoparticle have spherical shape morphology. Magnetic hysteresis curve for Ce1-xMnxO2, (x = 0.0, 0.01, and 0.05) confirms the ferromagnetic ordering room temperature. The value of saturation magnetization is observed to decrease with increase in temperature from 10 K to 300 K. The NEXAFS spectra measured at Ce M4,5 edge reveals that Ce-ions are in +4 valance state.

X-Ray Diffraction (XRD) Characterization Methods for Sigma=3 Twin Defects in Cubic Semiconductor (100) Wafers

NASA Technical Reports Server (NTRS)

Park, Yeonjoon (Inventor); Kim, Hyun Jung (Inventor); Skuza, Jonathan R. (Inventor); Lee, Kunik (Inventor); Choi, Sang Hyouk (Inventor); King, Glen C. (Inventor)

2017-01-01

An X-ray defraction (XRD) characterization method for sigma=3 twin defects in cubic semiconductor (100) wafers includes a concentration measurement method and a wafer mapping method for any cubic tetrahedral semiconductor wafers including GaAs (100) wafers and Si (100) wafers. The methods use the cubic semiconductor's (004) pole figure in order to detect sigma=3/{111} twin defects. The XRD methods are applicable to any (100) wafers of tetrahedral cubic semiconductors in the diamond structure (Si, Ge, C) and cubic zinc-blend structure (InP, InGaAs, CdTe, ZnSe, and so on) with various growth methods such as Liquid Encapsulated Czochralski (LEC) growth, Molecular Beam Epitaxy (MBE), Organometallic Vapor Phase Epitaxy (OMVPE), Czochralski growth and Metal Organic Chemical Vapor Deposition (MOCVD) growth.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise.

PubMed

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; Ramebäck, Henrik; Marie, Olivier; Ravat, Brice; Delaunay, François; Young, Emma; Blagojevic, Ned; Hester, James R; Thorogood, Gordon; Nelwamondo, Aubrey N; Ntsoane, Tshepo P; Roberts, Sarah K; Holliday, Kiel S

2018-01-01

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2 , U 3 O 8 and an intermediate species U 3 O 7 in the third material.

Structural analysis of the industrial grade calcite

NASA Astrophysics Data System (ADS)

Shah, Rajiv P.; Raval, Kamlesh G.

2017-05-01

The chemical, optical and structural characterization of the industrial grade Calcite by EDAX, FT-IR and XRD. EDAX is a widely used technique to analyze the chemical components in a material, FT-IR stands for Fourier Transform Infra-Red, the preferred method of infrared spectroscopy. The resultant spectrum represents the molecular absorption and transmission, creating a molecular fingerprint of the sample, The atomic planes of a crystal cause an incident beam of X-rays to interfere with one another as they leave the crystal. The phenomenon is called X ray diffraction.(XRD). Data analysis of EDAX, FT-IR and XRD has been carried out with help of various instruments and software and find out the results of the these industrial grade materials which are mostly used in ceramics industries

SORPTION OF LEAD ON A RUTHENIUM COMPOUND: A MACROSCOPIC AND MICROSCOPIC STUDY

EPA Science Inventory

The objective of this study was to elucidate the sorption mechanism of Pb on the high-affinity ruthenium compound with time at pH 6 employing batch methods and X-ray absorption fine structure (XAFS) and X-ray diffraction (XRD) spectroscopies. For the spectroscopic studies, Pb so...

PyXRD v0.6.7: a free and open-source program to quantify disordered phyllosilicates using multi-specimen X-ray diffraction profile fitting

NASA Astrophysics Data System (ADS)

Dumon, M.; Van Ranst, E.

2016-01-01

This paper presents a free and open-source program called PyXRD (short for Python X-ray diffraction) to improve the quantification of complex, poly-phasic mixed-layer phyllosilicate assemblages. The validity of the program was checked by comparing its output with Sybilla v2.2.2, which shares the same mathematical formalism. The novelty of this program is the ab initio incorporation of the multi-specimen method, making it possible to share phases and (a selection of) their parameters across multiple specimens. PyXRD thus allows for modelling multiple specimens side by side, and this approach speeds up the manual refinement process significantly. To check the hypothesis that this multi-specimen set-up - as it effectively reduces the number of parameters and increases the number of observations - can also improve automatic parameter refinements, we calculated X-ray diffraction patterns for four theoretical mineral assemblages. These patterns were then used as input for one refinement employing the multi-specimen set-up and one employing the single-pattern set-ups. For all of the assemblages, PyXRD was able to reproduce or approximate the input parameters with the multi-specimen approach. Diverging solutions only occurred in single-pattern set-ups, which do not contain enough information to discern all minerals present (e.g. patterns of heated samples). Assuming a correct qualitative interpretation was made and a single pattern exists in which all phases are sufficiently discernible, the obtained results indicate a good quantification can often be obtained with just that pattern. However, these results from theoretical experiments cannot automatically be extrapolated to all real-life experiments. In any case, PyXRD has proven to be useful when X-ray diffraction patterns are modelled for complex mineral assemblages containing mixed-layer phyllosilicates with a multi-specimen approach.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

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

NASA Astrophysics Data System (ADS)

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

2005-06-01

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

Imaging Research With Non-Periodic Multilayers for Inertial Confinement Fusion Diagnostic Experiments

NASA Astrophysics Data System (ADS)

L. Wang, F.; Mu, B. Z.; Wang, Z. S.; Gu, C. S.; Zhang, Z.; Qin, S. J.; Chen, L. Y.

A grazing Kirkpatrick-Baez (K-B) microscope was designed for hard x-ray (8keV; Cu Ka radiation) imaging in Inertial Confinement Fusion (ICF) diagnostic experiments. Ray tracing software was used to simulate optical system performance. The optimized theoretical resolution of K-B microscope was about 2 micron and better than 10 micron in 200 micron field of view. Tungsten and boron carbide were chosen as multilayer materials and the multilayer was deposited onto the silicon wafer substrate and the reflectivity was measured by x-ray diffraction (XRD). The reflectivity of supermirror was about 20 % in 0.3 % of bandwidth. 8keV Cu target x-ray tube source was used in x-ray imaging experiments and the magnification of 1x and 2x x-ray images were obtained.

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.

Low Energy X-Ray and γ-Ray Detectors Fabricated on n-Type 4H-SiC Epitaxial Layer

NASA Astrophysics Data System (ADS)

Mandal, Krishna C.; Muzykov, Peter G.; Chaudhuri, Sandeep K.; Terry, J. Russell

2013-08-01

Schottky barrier diode (SBD) radiation detectors have been fabricated on n-type 4H-SiC epitaxial layers and evaluated for low energy x- and γ-rays detection. The detectors were found to be highly sensitive to soft x-rays in the 50 eV to few keV range and showed 2.1 % energy resolution for 59.6 keV gamma rays. The response to soft x-rays for these detectors was significantly higher than that of commercial off-the-shelf (COTS) SiC UV photodiodes. The devices have been characterized by current-voltage (I-V) measurements in the 94-700 K range, thermally stimulated current (TSC) spectroscopy, x-ray diffraction (XRD) rocking curve measurements, and defect delineating chemical etching. I-V characteristics of the detectors at 500 K showed low leakage current ( nA at 200 V) revealing a possibility of high temperature operation. The XRD rocking curve measurements revealed high quality of the epitaxial layer exhibiting a full width at half maximum (FWHM) of the rocking curve 3.6 arc sec. TSC studies in a wide range of temperature (94-550 K) revealed presence of relatively shallow levels ( 0.25 eV) in the epi bulk with a density 7×1013 cm-3 related to Al and B impurities and deeper levels located near the metal-semiconductor interface.

Structural Order-Disorder Transformations Monitored by X-Ray Diffraction and Photoluminescence

ERIC Educational Resources Information Center

Lima, R. C.; Paris, E. C.; Leite, E. R.; Espinosa, J. W. M.; Souza, A. G.; Longo, E.

2007-01-01

A study was conducted to examine the structural order-disorder transformation promoted by controlled heat treatment using X-ray diffraction technique (XRD) and photoluminescence (PL) techniques as tools to monitor the degree of structural order. The experiment was observed to be versatile and easily achieved with low cost which allowed producing…

Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction.

PubMed

Huang, Zhifeng; Bartels, Matthias; Xu, Rui; Osterhoff, Markus; Kalbfleisch, Sebastian; Sprung, Michael; Suzuki, Akihiro; Takahashi, Yukio; Blanton, Thomas N; Salditt, Tim; Miao, Jianwei

2015-07-01

In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br(-) + hv → Br + e(-) and e(-) + Ag(+) → Ag(0). The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s(-1) and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

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

NASA Astrophysics Data System (ADS)

Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

2017-01-01

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

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

PubMed

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

2014-12-10

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

Effect of intrinsic zinc oxide coating on the properties of Al-doped zinc oxide nanorod arrays

NASA Astrophysics Data System (ADS)

Saidi, S. A.; Mamat, M. H.; Ismail, A. S.; Malek, M. F.; Yusoff, M. M.; Sin, N. D. Md.; Zoolfakar, A. S.; Khusaimi, Z.; Rusop, M.

2018-05-01

The aim of this study was to explore the influence of intrinsic zinc oxide (ZnO) coating fabricated by a simple immersion method. X-ray powder diffraction (XRD) analysis indicated that the Al-doped ZnO nanorod arrays films had a hexagonal wurtzite structure, similar to that of an intrinsic ZnO coating. Structural properties of the samples were characterised using field emission scanning electron microscopy (FESEM; JEOL JSM-7600F) and optical properties using X-ray diffraction (XRD). The XRD results showed that all films were crystallized under hexagonal wurtzite structure and presented a preferential orientation along the c-axis (002) was obtained. The XRD results showed that the intrinsic ZnO coating material had a strong orientation, whereas the ZnO was randomly oriented. Overall these results indicate that intrinsic ZnO coating are pontetial for the creation of functional materials such as barrier protection, optoelectronic devices, humidity sensor and ultraviolet photoconductive sensor.

TOMOX : An X-rays tomographer for planetary exploration

NASA Astrophysics Data System (ADS)

Marinangeli, Lucia; Pompilio, Loredana; Chiara Tangari, Anna; Baliva, Antonio; Alvaro, Matteo; Chiara Domeneghetti, Maria; Frau, Franco; Melis, Maria Teresa; Bonanno, Giovanni; Consolata Rapisarda, Maria; Petrinca, Paolo; Menozzi, Oliva; Lasalvia, Vasco; Pirrotta, Simone

2017-04-01

The TOMOX instrument has recently been founded under the ASI DC-EOS-2014-309 call. The TOMOX objective is to acquire both X-ray fluorescence and diffraction measurements from a sample in order to: a) achieve its chemical and mineralogical composition; b) reconstruct a 3D tomography of the sample exposed surface; c) give hints regarding the sample age. Nevertheless, this technique has applicability in several disciplines other than planetary geology, especially archaeology. The word 'tomography' is nowadays used for many 3D imaging methods, not just for those based on radiographic projections, but also for a wider range of techniques that yield 3D images. Fluorescence tomography is based on the signal produced on an energy-sensitive detector, generally placed in the horizontal plane at some angle with respect to the incident beam caused by photons coming from fluorescence emission. So far, a number of setups have been designed in order to acquire X-rays fluorescence tomograms of several different sample types. The proposed instrument is based on the MARS-XRD heritage, an ultra miniaturised XRD and XRF instrument developed for the ESA ExoMars mission. The general idea of TOMOX is to distribute both sources and detectors along a moving hemispherical support around the target sample. As a result, both sources move integrally with the detectors while the sample is observed from a fixed position, thus preserving the geometry of observation. In that way, the whole sample surface is imagined and XRD and XRF measurements are acquired continuously along all the scans. We plan to irradiate the target sample with X-rays emitted from 55Fe and 109Cd radioactive sources. 55Fe and 109Cd radioisotopes are commonly used as X-ray sources for analysis of metals in soils and rocks. The excitation energies of 55Fe and 109Cd are 5.9 keV, and 22.1 and 87.9 keV, respectively. Therefore, the elemental analysis ranges are Al to Mn with K lines excited with 55Fe; Ca to Rh, with K lines excited with 109Cd. 55Fe will be primarily dedicated to XRD measurements, as it has been already tested for the MARS-XRD development. 109Cd will be used to reinforce the efficiency of 55Fe source in the production of fluorescent X-rays generated in the sample as a consequence of irradiation and to extend the analytical range of elements. Two different detectors will be used in order to increase the total amount of events collected and allow the spatial distribution of events to be recorded as well. The detectors we plan to use are SDD (Silicon Drift Detector) and stand-alone CCD (Coupled Charge Detector). SDD has higher count rate and stability and has been successfully used for XRF applications. CCD is able to record the spatial position of each event of X-ray emission, together with its energy. Therefore, we plan to dedicate this detector to XRD measurements, where the spatial position of the event is directly correlated to the type of crystal through the Bragg's law. A prototype of the instrument will be likely completed by the end of this year.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

PubMed

Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

A Potential Waste to be Selected as Media for Metal and Nutrient Removal

NASA Astrophysics Data System (ADS)

Zayadi, N.; Othman, N.; Hamdan, R.

2016-07-01

This study describes the potential of application of cassava peel, banana peel, coconut shell, and coconut coir to be selected as metal removal while limestone and steel slag for nutrient removal. The media were characterized by X-Ray Fluorescence (XRF), Fourier Transform Infrared (FTIR), Field Emission Scanning Electron Microscopy-Energy Dispersive X-Ray (FESEM-EDX), and X-Ray Powder Diffraction (XRD). The results of XRF analysis medias show the present of calcium oxide, CaO which confirm the high efficiency in adsorbing metal ions and nutrient which is in agreement with the result of XRD. The characteristics of medias by FTIR analysis also confirmed the involvement of alcohol, carboxylic, alkanes, amines and ethers which play important role to reduce ions while FESEM-EDX indicates the porous structures of study medias. The characterization analysis highlight that cassava peel and steel slag were selected as a potential media in this study.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

NASA Astrophysics Data System (ADS)

Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

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

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

DOE PAGES

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; ...

2018-01-24

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

PubMed

Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

2017-06-12

The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

The effect of doped zinc on the structural properties of nano-crystalline (Se0.8Te0.2)100-xZnx

NASA Astrophysics Data System (ADS)

Kumar, Arun; Singh, Harkawal; Gill, P. S.; Goyal, Navdeep

2016-05-01

The effect of metallic zinc (Zn) on the structural properties of (Se0.8Te0.2)1-XZnX (x=0, 2, 6, 8, 10) samples analyzed by X-ray Diffraction (XRD). The presence of sharp peaks in XRD patterns confirmed the crystalline nature of the samples and is indexed in orthorhombic crystal structure. XRD studies predicts that the average particle size of all the samples are about 46.29 nm, which is less than 100 nm and hence have strong tendency of agglomeration. Williamson-Hall plot method was used to evaluate the lattice strain. The dislocation density and no. of unit cells of the samples were calculated which show the inverse relation with each other. Morphology index derived from FWHM of XRD data explains the direct relationship with the particle size.

Cadmium effect on structural properties of Cu{sub 2}Zn{sub 1-x}Cd{sub x}SnS{sub 4} quinternary alloys nanostructures

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

Ibraheam, A. S.; Al-Douri, Y., E-mail: yaldouri@yahoo.com; Hashim, U.

The study report novel sensing plat of extended quinternart materials, Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures were fabricated onto oxidized silicon substrate by sol-gel method and characterized were synthesized by X-ray diffraction (XRD). The XRD peaks were shifted towered the lower angle side with increasing cadmium content. The practical size average of the Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures between 34.55 to 63.30 nm.

Astrobiological Significance of Definitive Mineralogical Analysis of Martian Surface Samples Using the CheMin XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

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

2004-01-01

The search for evidence of habitability, or of extant or extinct life on Mars, will initially be a search for evidence of past or present conditions supportive of life. The three key requirements for the emergence of life are thought to be liquid water; a suitable energy source; and chemical building blocks. CheMin is a miniaturized XRD/XRF (X-Ray diffraction / X-ray fluorescence) instrument which has been developed for definitive mineralogic analysis of soils and rocks on the Martian surface. The CheMin instrument can provide information that is highly relevant to each of these habitability requirements as summarized below.

On-the-fly segmentation approaches for x-ray diffraction datasets for metallic glasses

DOE PAGES

Ren, Fang; Williams, Travis; Hattrick-Simpers, Jason; ...

2017-08-30

Investment in brighter sources and larger detectors has resulted in an explosive rise in the data collected at synchrotron facilities. Currently, human experts extract scientific information from these data, but they cannot keep pace with the rate of data collection. Here, we present three on-the-fly approaches—attribute extraction, nearest-neighbor distance, and cluster analysis—to quickly segment x-ray diffraction (XRD) data into groups with similar XRD profiles. An expert can then analyze representative spectra from each group in detail with much reduced time, but without loss of scientific insights. As a result, on-the-fly segmentation would, therefore, result in accelerated scientific productivity.

Identification of green pigments from fragments of Roman mural paintings of three Roman sites from north of Germania Superior

NASA Astrophysics Data System (ADS)

Debastiani, Rafaela; Simon, Rolf; Goettlicher, Joerg; Heissler, Stefan; Steininger, Ralph; Batchelor, David; Fiederle, Michael; Baumbach, Tilo

2016-10-01

Roman mural green pigment painting fragments from three Roman sites in the north of the Roman province Germania Superior: Koblenz Stadtwald Remstecken (KOSR), Weißenthurm " Am guten Mann" (WEIS) and Mendig Lungenkärchen (MELU), dating from second and third centuries AD were analyzed. The experiments were performed nondestructively using synchrotron-based scanning macro-X-ray fluorescence (SR-MA-XRF), synchrotron-based scanning micro-X-ray fluorescence (SR-μ-XRF), synchrotron-based X-ray diffraction (SR-XRD) and Raman spectroscopy. Correlation between SR-MA-XRF, SR-μ-XRF elemental map distributions and optical images of scanned areas was mainly found for the elements Ca, Fe and K. With XRF, Fe and K were identified correlated with green pigment, but in samples from two sites, Mendig Lungenkärchen and Weißenthurm " Am guten Mann", also Cu was detected in minor concentration. The results of SR-XRD and Raman spectroscopy were limited to one sample from Weißenthurm " Am guten Mann". In this sample, green earth and calcium carbonate were identified by SR-XRD and, additionally, malachite by Raman spectroscopy.

Analysis of doping concentration and composition in wide bandgap AlGaN:Si by wavelength dispersive x-ray spectroscopy

NASA Astrophysics Data System (ADS)

Kusch, Gunnar; Mehnke, Frank; Enslin, Johannes; Edwards, Paul R.; Wernicke, Tim; Kneissl, Michael; Martin, Robert W.

2017-03-01

Detailed knowledge of the dopant concentration and composition of wide band gap Al x Ga{}1-x{{N}} layers is of crucial importance for the fabrication of ultra violet light emitting diodes. This paper demonstrates the capabilities of wavelength dispersive x-ray (WDX) spectroscopy in accurately determining these parameters and compares the results with those from high resolution x-ray diffraction (HR-XRD) and secondary ion mass spectrometry (SIMS). WDX spectroscopy has been carried out on different silicon-doped wide bandgap Al x Ga{}1-x{{N}} samples (x between 0.80 and 1). This study found a linear increase in the Si concentration with the SiH4/group-III ratio, measuring Si concentrations between 3× {10}18 cm-3 and 2.8× {10}19 cm-3, while no direct correlation between the AlN composition and the Si incorporation ratio was found. Comparison between the composition obtained by WDX and by HR-XRD showed very good agreement in the range investigated, while comparison of the donor concentration between WDX and SIMS found only partial agreement, which we attribute to a number of effects.

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

DTIC Science & Technology

2011-09-01

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

The Influence of Growth Temperature on Sb Incorporation in InAsSb, and the Temperature-dependent Impact of Bi Surfactants

DTIC Science & Technology

2014-01-01

resolution X - ray diffraction (XRD) were collected for all samples, and reciprocal space maps (RSMs) were collected from selected samples. The complete data...exposure. The lines represent the model fit. 19 13 Figure 1. Triple axis x - ray diffraction from the bi-layered InAsSb structures grown on GaSb at...Applied Physics, Structural properties of bismuth‐bearing semiconductor alloys, 63 (1988) 107. 18 12 Figure Captions Figure 1. Triple axis x - ray

Effects of Peripheral Architecture on the Properties of Aryl Polyhedral Oligomeric Silsesquioxanes

DTIC Science & Technology

2012-07-26

POSS) molecules are described. These POSS materials were synthesized in our laboratory and characterized by single-crystal and powder X - ray diffraction ...powder X - ray diffraction (XRD), where applicable. 1H, 13C, and 29Si NMR spectra were obtained on Bruker 300 and 400 MHz spectrometers using 5 mm o.d...degree of cage ordering during precipitation. Referring back to Figure 14, strong X - ray scattering peaks in the spectra for 1 in the d- spacing range

Simple X-ray diffraction algorithm for direct determination of cotton crystallinity

USDA-ARS?s Scientific Manuscript database

Traditionally, XRD had been used to study the crystalline structure of cotton celluloses. Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI), in its present state, XRD measurement can only provide a qualitative or semi-quantitative assessme...

High T(sub c) superconductor/ferroelectric heterostructures

NASA Astrophysics Data System (ADS)

Ryder, Daniel F., Jr.

1994-12-01

Thin films of the ferroelectric perovskite, Ba(x) Sr(1-x) TiO3 (BST), were deposited on superconducting (100)YBa2Cu3O(x)(YBCO)/ (100)Yttria-stabilized zirconia(YSZ) substrates and (100)Si by ion-beam sputtering. Microstructural and compositional features of the ceramic bilayer were assessed by a combination of x-ray diffraction (XRD) and scanning electron microscopy. The films were smooth and featureless, and energy dispersive x-ray spectroscopy (EDX) data indicated that film composition closely matched target composition. XRD analysis showed that films deposited on YBCO substrates were highly c-axis textured, while the films deposited on (100)Si did not exhibit any preferred growth morphology. The superconducting properties of the YBCO substrate layer were maintained throughout the processing stages and, as such, it was demonstrated that ion beam sputtering is a viable method for the deposition of Ferroelectric/YBCO heterostructures.

Textural, Structural and Biological Evaluation of Hydroxyapatite Doped with Zinc at Low Concentrations

PubMed Central

Predoi, Daniela; Iconaru, Simona Liliana; Deniaud, Aurélien; Chevallet, Mireille; Michaud-Soret, Isabelle; Buton, Nicolas; Prodan, Alina Mihaela

2017-01-01

The present work was focused on the synthesis and characterization of hydroxyapatite doped with low concentrations of zinc (Zn:HAp) (0.01 < xZn < 0.05). The incorporation of low concentrations of Zn2+ ions in the hydroxyapatite (HAp) structure was achieved by co-precipitation method. The physico-chemical properties of the samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), zeta-potential, and DLS and N2-BET measurements. The results obtained by XRD and FTIR studies demonstrated that doping hydroxyapatite with low concentrations of zinc leads to the formation of a hexagonal structure with lattice parameters characteristic to hydroxyapatite. The XRD studies have also shown that the crystallite size and lattice parameters of the unit cell depend on the substitutions of Ca2+ with Zn2+ in the apatitic structure. Moreover, the FTIR analysis revealed that the water content increases with the increase of zinc concentration. Furthermore, the Energy Dispersive X-ray Analysis (EDAX) and XPS analyses showed that the elements Ca, P, O, and Zn were found in all the Zn:HAp samples suggesting that the synthesized materials were zinc doped hydroxyapatite, Ca10−xZnx(PO4)6(OH), with 0.01 ≤ xZn ≤ 0.05. Antimicrobial assays on Staphylococcus aureus and Escherichia coli bacterial strains and HepG2 cell viability assay were carried out. PMID:28772589

Real-time x-ray diffraction measurements of shocked polycrystalline tin and aluminum.

PubMed

Morgan, Dane V; Macy, Don; Stevens, Gerald

2008-11-01

A new, fast, single-pulse x-ray diffraction (XRD) diagnostic for determining phase transitions in shocked polycrystalline materials has been developed. The diagnostic consists of a 37-stage Marx bank high-voltage pulse generator coupled to a needle-and-washer electron beam diode via coaxial cable, producing line and bremsstrahlung x-ray emission in a 35 ns pulse. The characteristic K(alpha) lines from the selected anodes of silver and molybdenum are used to produce the diffraction patterns, with thin foil filters employed to remove the characteristic K(beta) line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 3 x 6 mm(2) spot and 1 degrees full width half maximum angular divergence in a Bragg-reflecting geometry. For the experiments described in this report, the angle between the incident beam and the sample surface was 8.5 degrees . A Debye-Scherrer diffraction image was produced on a phosphor located 76 mm from the polycrystalline sample surface. The phosphor image was coupled to a charge-coupled device camera through a coherent fiber-optic bundle. Dynamic single-pulse XRD experiments were conducted with thin foil samples of tin, shock loaded with a 1 mm vitreous carbon back window. Detasheet high explosive with a 2-mm-thick aluminum buffer was used to shock the sample. Analysis of the dynamic shock-loaded tin XRD images revealed a phase transformation of the tin beta phase into an amorphous or liquid state. Identical experiments with shock-loaded aluminum indicated compression of the face-centered-cubic aluminum lattice with no phase transformation.

Stacked, filtered multi-channel X-ray diode array

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

MacNeil, Lawrence; Dutra, Eric; Raphaelian, Mark

2015-08-01

There are many types of X-ray diodes used for X-ray flux or spectroscopic measurements and for estimating the spectral shape of the VUV to soft X-ray spectrum. However, a need exists for a low-cost, robust X-ray diode to use for experiments in hostile environments on multiple platforms, and for experiments that utilize forces that may destroy the diode(s). Since the typical proposed use required a small size with a minimal single line-of-sight, a parallel array could not be used. So, a stacked, filtered multi-channel X-ray diode array was developed, called the MiniXRD. To achieve significant cost savings while maintaining robustnessmore » and ease of field setup, repair, and replacement, we designed the system to be modular. The filters were manufactured in-house and cover the range from 450 eV to 5000 eV. To achieve the line-of-sight accuracy needed, we developed mounts and laser alignment techniques. We modeled and tested elements of the diode design at NSTec Livermore Operations (NSTec / LO) to determine temporal response and dynamic range, leading to diode shape and circuitry changes to optimize impedance and charge storage. The authors fielded individual and stacked systems at several national facilities as ancillary "ride-along" diagnostics to test and improve the design usability. This paper presents the MiniXRD system performance, which supports consideration as a viable low-costalternative for multiple-channel low-energy X-ray measurements. This diode array is currently at Technical Readiness Level (TRL) 6.« less

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.

Aerogel as a Sample Collector and Sample Mount for Transmission XRD Analysis

NASA Technical Reports Server (NTRS)

Bish, D. L.; Vaniman, D. T.; Chipera, S. J.; Yen, A. S.; Jones, S. M.

2001-01-01

Silica aerogel can be used for dust collection and in situ X-ray analysis. Aerogels can be less absorbing than Be, and it is feasible to obtain X-ray transmission factors >50% using typical aerogels together with a 100-micrometer Be backing foil. Additional information is contained in the original extended abstract.

Using Variable Temperature Powder X-Ray Diffraction to Determine the Thermal Expansion Coefficient of Solid MgO

ERIC Educational Resources Information Center

Corsepius, Nicholas C.; DeVore, Thomas C.; Reisner, Barbara A.; Warnaar, Deborah L.

2007-01-01

A laboratory exercise was developed by using variable temperature powder X-ray diffraction (XRD) to determine [alpha] for MgO (periclase)and was tested in the Applied Physical Chemistry and Materials Characterization Laboratories at James Madison University. The experiment which was originally designed to provide undergraduate students with a…

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

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

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

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

Study on the Effect of Various Sol-Gel Concentration to the Electrical, Structural and Optical Properties of the Nanostructured Titanium Dioxide Thin Films

NASA Astrophysics Data System (ADS)

Ahmad, M. K.; Rusop, M.

2009-06-01

Nanostructured Titanium Dioxide (TiO2) thin film with various sol-gel concentration has been successfully prepared using sol-gel spin coating method. The sol-gel concentration of nanostructured TiO2 thin films are varied at 0.1 M, 0.2 M, 0.3 M and 0.4 M, respectively. The effects of different sol-gel concentration of nanostructured TiO2 thin film structural, electrical and optical properties have been studied. The effects of these properties were characterized using X-Ray Diffractometer (XRD), 2-point probe I-V measurement and UV-Vis-NIR Spectrophotometer. For electrical properties, 0.2 M of sol-gel concentration gives the lowest sheet resistance among other concentrated sol-gels. As for structural properties, 0.1 M of concentration gives very weak peak, and continues stronger as in comes to 0.2 M until 0.4 M. It is due to amount of solute (i.e Titanium Isopropoxide) increases in the solution and therefore the intensity of (101) planes become higher. The optical transmission in the visible region (450-1000 nm) for 0.1 M and 0.2 M are the highest (>80%), indicating that the films are transparent in the visible region. The transmission decreases sharply near the ultraviolet region due to the band gap absorption.

Paraequilibrium Carburization of Duplex and Ferritic Stainless Steels

NASA Astrophysics Data System (ADS)

Michal, G. M.; Gu, X.; Jennings, W. D.; Kahn, H.; Ernst, F.; Heuer, A. H.

2009-08-01

AISI 301 and E-BRITE stainless steels were subjected to low-temperature (743 K) carburization experiments using a commercial technology developed for carburization of 316 austenitic stainless steels. The AISI 301 steel contained ~40 vol pct ferrite before carburization but had a fully austenitic hardened case, ~20- μm thick, and a surface carbon concentration of ~8 at. pct after treatment; this “colossal” paraequilibrium carbon supersaturation caused an increase in lattice parameter of ~3 pct. The E-BRITE also developed a hardened case, 12- to 18- μm thick, but underwent a more modest (~0.3 pct) increase in lattice parameter; the surface carbon concentration was ~10 at. pct. While the hardened case on the AISI 301 stainless steel appeared to be single-phase austenite, evidence for carbide formation was apparent in X-ray diffractometer (XRD) scans of the E-BRITE. Paraequilibrium phase diagrams were calculated for both AISI 301 and E-BRITE stainless steels using a CALPHAD compound energy-based interstitial solid solution model. In the low-temperature regime of interest, and based upon measured paraequilibrium carbon solubilities, more negative Cr-carbon interaction parameters for austenite than those in the current CALPHAD data base may be appropriate. A sensitivity analysis involving Cr-carbon interaction parameters for ferrite found a strong dependence of carbon solubility on relatively small changes in the magnitude of these parameters.

Development of in-Situ Al-Si/CuAl₂ Metal Matrix Composites: Microstructure, Hardness, and Wear Behavior.

PubMed

Tash, Mahmoud M; Mahmoud, Essam R I

2016-06-02

In the present work, in-situ metal matrix composites were fabricated through squeeze casting. The copper particles were dispersed with different weight percentages (3%, 6%, 10%, and 15%) into Al-12% Si piston alloy. Also, heat treatments were performed at 380 °C and 450 °C for holding times of 6 and 18 h. The microstructures, X-ray diffractometer (XRD) pattern, hardness, and wear characteristics were evaluated. The results showed that these copper particles have reacted with the aluminum under all of the aforementioned processing conditions resulting in the formation of fine copper aluminide intermetallics. Most of the intermetallics were CuAl₂, while AlCu appeared in a small ratio. Additionally, these intermetallics were homogenously distributed within the alloy matrix with up to 6% Cu addition. The amounts of those intermetallics increased after performing heat treatment. Most of these intermetallics were CuAl₂ at 380 °C, while the Cu-rich intermetallics appeared at 450 °C. Increasing the holding time to 18 h, however, led to grain coarsening and resulted in the formation of some cracks. The hardness of the resulting composite materials was improved. The hardness value reached to about 170 HV after heat treating at 380 °C for 8 h. The wear resistance of the resulting composite materials was remarkably improved, especially at lower additions of Cu and at the lower heat treatment temperature.

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

Geotechnical characterization of some Indian fly ashes

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

Das, S.K.; Yudhbir

2005-10-01

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

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

NASA Technical Reports Server (NTRS)

Smyth, J. R.

1974-01-01

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

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

PubMed

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

2006-11-01

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

Viscosity studies of water based magnetite nanofluids

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

Anu, K.; Hemalatha, J.

2016-05-23

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

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

PubMed

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

2016-05-01

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

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

PubMed Central

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

2016-01-01

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

Non-conventional applications of a noninvasive portable X-ray diffraction/fluorescence instrument

NASA Astrophysics Data System (ADS)

Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

2016-11-01

Noninvasive techniques have become widespread in the cultural heritage analytical domain. The popular handheld X-ray fluorescence (XRF) devices give the elemental composition of all the layers that X-rays can penetrate, but no information on how atoms are bound together or at which depth they are located. A noninvasive portable X-ray powder diffraction/X-ray fluorescence (XRD/XRF) device may offer a solution to these limitations, since it can provide information on the composition of crystalline materials. This paper introduces applications of XRD beyond simple phase recognition. The two fundamental principles for XRD are: (1) the crystallites should be randomly oriented, to ensure proper intensity to all the diffraction peaks, and (2) the material should be positioned exactly in the focal plane of the instrument, respecting its geometry, as any displacement of the sample would results in 2 θ shifts of the diffraction peaks. In conventional XRD, the sample is ground and set on the properly positioned sample holder. Using a noninvasive portable instrument, these two requirements are seldom fulfilled. The position, size and orientation of a given crystallite within a layered structure depend on the object itself. Equation correlating the displacement (distance from the focal plane) versus peak shift (angular difference in 2 θ from the standard value) is derived and used to determine the depth at which a given substance is located. The quantitative composition of two binary Cu/Zn alloys, simultaneously present, was determined measuring the cell volume and using Vegard's law. The analysis of the whole object gives information on the texture and possible preferred orientations of the crystallites, which influences the peak intensity. This allows for the distinction between clad and electroplated daguerreotypes in the case of silver and between ancient and modern gilding for gold. Analyses of cross sections can be carried out successfully. Finally, beeswax, used in Roman-Egyptian paintings as "encaustic" and in form of emulsion (modified wax), can be detected and, based on the shape of the peaks, these two ways of applying the wax can be distinguished from one another.

Effect of substrate temperature in the synthesis of BN nanostructures

NASA Astrophysics Data System (ADS)

Sajjad, M.; Zhang, H. X.; Peng, X. Y.; Feng, P. X.

2011-06-01

Boron nitride (BN) nanostructures were grown on molybdenum discs at different substrate temperatures using the short-pulse laser plasma deposition technique. Large numbers of randomly oriented nanorods of fiber-like structures were obtained. The variation in the length and diameter of the nanorods as a function of the substrate temperature was systematically studied. The surface morphologies of the samples were studied using scanning electron microscopy. Energy dispersive x-ray spectroscopy confirmed that both the elements boron and nitrogen are dominant in the nanostructure. The x-ray diffraction (XRD) technique was used to analyse BN phases. The XRD peak that appeared at 26° showed the presence of hexagonal BN phase, whereas the peak at 44° was related to cubic BN content in the samples. Raman spectroscopic analysis showed vibrational modes of sp2- and sp3-type bonding in the sample. The Raman spectra agreed well with XRD results.

Nano-crystalline hydroxyapatite bio-mineral for the treatment of strontium from aqueous solutions.

PubMed

Handley-Sidhu, Stephanie; Renshaw, Joanna C; Yong, Ping; Kerley, Robert; Macaskie, Lynne E

2011-01-01

Hydroxyapatites were analysed using electron microscopy, X-ray diffraction (XRD) and X-ray fluorescence (XRF) analysis. Examination of a bacterially produced hydroxyapatite (Bio-HA) by scanning electron microscopy showed agglomerated nano-sized particles; XRD analysis confirmed that the Bio-HA was hydroxyapatite, with an organic matter content of 7.6%; XRF analysis gave a Ca/P ratio of 1.55, also indicative of HA. The size of the Bio-HA crystals was calculated as ~25 nm from XRD data using the Scherrer equation, whereas Comm-HA powder size was measured as ≤ 50 μm. The nano-crystalline Bio-HA was ~7 times more efficient in removing Sr(2+) from synthetic groundwater than Comm-HA. Dissolution of HA as indicated by the release of phosphate into the solution phase was higher in the Comm-HA than the Bio-HA, indicating a more stable biomaterial which has a potential for the remediation of contaminated sites.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

NASA Astrophysics Data System (ADS)

YangDai, Tianyi; Zhang, Li

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Experimental determination of spin-dependent electron density by joint refinement of X-ray and polarized neutron diffraction data.

PubMed

Deutsch, Maxime; Claiser, Nicolas; Pillet, Sébastien; Chumakov, Yurii; Becker, Pierre; Gillet, Jean Michel; Gillon, Béatrice; Lecomte, Claude; Souhassou, Mohamed

2012-11-01

New crystallographic tools were developed to access a more precise description of the spin-dependent electron density of magnetic crystals. The method combines experimental information coming from high-resolution X-ray diffraction (XRD) and polarized neutron diffraction (PND) in a unified model. A new algorithm that allows for a simultaneous refinement of the charge- and spin-density parameters against XRD and PND data is described. The resulting software MOLLYNX is based on the well known Hansen-Coppens multipolar model, and makes it possible to differentiate the electron spins. This algorithm is validated and demonstrated with a molecular crystal formed by a bimetallic chain, MnCu(pba)(H(2)O)(3)·2H(2)O, for which XRD and PND data are available. The joint refinement provides a more detailed description of the spin density than the refinement from PND data alone.

Characterization of mineral phases of agricultural soil samples of Colombian coffee using Mössbauer spectroscopy and X-ray diffraction

NASA Astrophysics Data System (ADS)

Rodríguez, Humberto Bustos; Lozano, Dagoberto Oyola; Martínez, Yebrayl Antonio Rojas; Pinilla, Marlene Rivera; Alcázar, German Antonio Pérez

2012-03-01

Soil chemical analysis, X-ray diffraction (XRD) and Mössbauer spectrometry (MS) of 57Fe were used to characterize mineral phases of samples taken from the productive layer (horizon A) of agricultural coffee soil from Tolima (Colombia). Chemical analysis shows the chemical and textural parameters of samples from two different regions of Tolima, i.e., Ibagué and Santa Isabel. By XRD phases like illite (I), andesine (A) and quartz (Q) in both samples were identified. The quantity of these phases is different for the two samples. The MS spectra taken at room temperature were adjusted by using five doublets, three of them associated to Fe + 3 type sites and the other two to Fe + 2 type sites. According to their isomer shift and quadrupole splitting the presence of phases like illite (detected by DRX), nontronite and biotite (not detected by XRD) can be postulated.

A new approach for the recovery of precious metals from solution and from leachates derived from electronic scrap.

PubMed

Macaskie, L E; Creamer, N J; Essa, A M M; Brown, N L

2007-03-01

A new approach is described for the recovery of precious metals (PMs: Au, Pd and Ag) with >99% efficiency from aqueous solution utilising biogas produced during the aerobic growth of Klebsiella pneumoniae. Gold was recovered from electronic scrap leachate ( approximately 95%) by this method, with some selectivity against Cu. The recovered PM solids all contained metal and sulphur as determined by energy dispersive X-ray microanalysis (EDX). X-ray powder diffraction analysis (XRD) showed no crystalline metal sulphur compounds but a crystalline palladium amine was recorded. Silver was recovered as a sulphide (found by EDX), carbonate and oxide (found by XRD). EDX analysis of the Au-precipitate showed mainly gold and sulphur, with some metallic Au(0) detected by XRD. The gold compound was shock-sensitive; upon grinding it detonated to leave a sooty black deposit.

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

NASA Astrophysics Data System (ADS)

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

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

[Study on bamboo treated with gamma rays by X-ray diffraction].

PubMed

Sun, Feng-Bo; Fei, Ben-Hua; Jiang, Ze-Hui; Yu, Zi-Xuan; Tian, Gen-Lin; Yang, Quan-Wen

2011-06-01

The microfibril angle and crystallinity of bamboo treated with gamma rays were tested by X-ray diffraction (XRD). The result indicated that crystallinity in bamboo increased when irradiation dose was less than 100 kGy, while the irradiation dose was raised to about 100 kGy, crystallinity in bamboo reduced. But during the whole irradiation process, the influence on microfibril angle was not obvious, so it was not the dominant factors on variation in physical-mechanical properties of bamboo during the process of irradiation.

In situ X-ray diffraction strain-controlled study of Ti–Nb–Zr and Ti–Nb–Ta shape memory alloys: crystal lattice and transformation features

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

Dubinskiy, S.; National University of Science and Technology “MISIS”, 4, Leninskiy prosp., Moscow 119049; Prokoshkin, S.

2014-02-15

Phase and structure transformations in biomedical Ti–21.8Nb–6.0Zr (TNZ) and Ti–19.7Nb–5.8Ta (TNT) shape memory alloys (at.%) under and without load in the − 150 to 100 °S temperature range are studied in situ using an original tensile module for a low-temperature chamber of an X-ray diffractometer. Alpha″- and beta-phase lattice parameters, the crystallographic resource of recovery strain, phase and structure transformation sequences, and microstress appearance and disappearance are examined, compared and discussed. For both alloys, the crystallographic resource of recovery strain decreases with temperature increase to become 4.5% for TNZ and 2.5% for TNT alloy (at RT). Loading at low temperaturesmore » leads to additional α″-phase formation and reorientation. Heating under load, as compared to strain-free heating, affects the reverse transformation sequence of both alloys in different ways. For TNZ alloy, strain-free heating results in simultaneous ω→β and α″→β transformations, whereas during heating under stress, they are sequential: β + ω→α″ precedes α″→β. For TNT alloy, strain-free heating results in reverse α″→β transformation, whereas during heating under stress, α″→β transformation is preceded by α″-phase reorientation. - Highlights: • Comparative in situ XRD analysis of Ti–Nb–Zr(Ta) shape memory alloys is realized. • Lattice parameters of β- and α″-phases are calculated in the − 150 to + 100 °C range. • The higher the temperature, the lower the α″→β transformation strain. • Loading at low temperatures results in α″-phase formation and reorientation. • Transformation sequences upon heating with and without loading are different.« less

Fabrication of zirconia composite membrane by in-situ hydrothermal technique and its application in separation of methyl orange.

PubMed

Kumar, R Vinoth; Ghoshal, Aloke Kumar; Pugazhenthi, G

2015-11-01

The main objective of the work was preparation of zirconia membrane on a low cost ceramic support through an in-situ hydrothermal crystallization technique for the separation of methyl orange dye. To formulate the zirconia film on the ceramic support, hydrothermal reaction mixture was prepared using zirconium oxychloride as a zirconia source and ammonia as a precursor. The synthesized zirconia powder was characterized by X-ray diffractometer (XRD), N2 adsorption/desorption isotherms, Thermogravimetric analysis (TGA), Fourier transform infrared analysis (FTIR), Energy-dispersive X-ray (EDX) analysis and particle size distribution (PSD) to identify the phases and crystallinity, specific surface area, pore volume and pore size distribution, thermal behavior, chemical composition and size of the particles. The porosity, morphological structure and pure water permeability of the prepared zirconia membrane, as well as ceramic support were investigated using the Archimedes' method, Field emission scanning electron microscopy (FESEM) and permeability. The specific surface area, pore volume, pore size distribution of the zirconia powder was found to be 126.58m(2)/g, 3.54nm and 0.3-10µm, respectively. The porosity, average pore size and pure water permeability of the zirconia membrane was estimated to be 42%, 0.66µm and 1.44×10(-6)m(3)/m(2)skPa, respectively. Lastly, the potential of the membrane was investigated with separation of methyl orange by means of flux and rejection as a function of operating pressure and feed concentration. The rejection was found to decrease with increasing the operating pressure and increases with increasing feed concentrations. Moreover, it showed a high ability to reject methyl orange from aqueous solution with a rejection of 61% and a high permeation flux of 2.28×10(-5)m(3)/m(2)s at operating pressure of 68kPa. Copyright © 2015 Elsevier Inc. All rights reserved.

Visible light photocatalytic activities of template free porous graphitic carbon nitride-BiOBr composite catalysts towards the mineralization of reactive dyes

NASA Astrophysics Data System (ADS)

Kanagaraj, Thamaraiselvi; Thiripuranthagan, Sivakumar; Paskalis, Sahaya Murphin Kumar; Abe, Hideki

2017-12-01

Template free porous g-C3N4 (pGCN) and flower like bismuth oxybromide catalysts were synthesized by poly condensation and precipitation methods respectively. Various weight percentages of porous GCN-BiOBr composite catalysts (x% pGCN-BiOBr where x = 5, 10, 30, 50 & 70 wt% of pGCN) were synthesized by impregnation method. All the synthesized catalysts were characterized by X-Ray diffractometer, Fourier transform infrared spectrophotometer, BET surface area analyzer, UV Visible diffuse reflectance spectrophotometer, X-Ray photoelectron spectrophotometer, SEM with Energy dispersive X-ray analyzer (SEM/EDAX) and elemental mapping, Transmission electron microscope, Photoluminescence spectrophotometer and Electrochemical impedance. Photocatalytic degradation of all the synthesized catalysts were tested towards the harmful reactive dyes such as reactive blue 198 (RB 198), reactive black 5 (RB 5) and reactive yellow 145 (RY 145) in presence of visible irradiation. Among the catalysts 30% pGCN-BiOBr resulted in the highest photocatalytic activity towards the degradation of all the three dyes in presence of UV, visible and solar irradiations. Kinetics studies on the photocatalytic mineralization of dyes indicated that it followed pseudo first order. HPLC, TOC and COD studies confirm that the dyes are mineralized into CO2, water and mineral salts.

Measurement of fundamental illite particle thicknesses by X-ray diffraction using PVP-10 intercalation

USGS Publications Warehouse

Eberl, D.D.; Nüesch, R.; Šucha, Vladimír; Tsipursky, S.

1998-01-01

The thicknesses of fundamental illite particles that compose mixed-layer illite-smectite (I-S) crystals can be measured by X-ray diffraction (XRD) peak broadening techniques (Bertaut-Warren-Averbach [BWA] method and integral peak-width method) if the effects of swelling and XRD background noise are eliminated from XRD patterns of the clays. Swelling is eliminated by intercalating Na-saturated I-S with polyvinylpyrrolidone having a molecular weight of 10,000 (PVP-10). Background is minimized by using polished metallic silicon wafers cut perpendicular to (100) as a substrate for XRD specimens, and by using a single-crystal monochromator. XRD measurements of PVP-intercalated diagenetic, hydrothermal and low-grade metamorphic I-S indicate that there are at least 2 types of crystallite thickness distribution shapes for illite fundamental particles, lognormal and asymptotic; that measurements of mean fundamental illite particle thicknesses made by various techniques (Bertant-Warren-Averbach, integral peak width, fixed cation content, and transmission electron microscopy [TEM]) give comparable results; and that strain (small differences in layer thicknesses) generally has a Gaussian distribution in the log-normal-type illites, but is often absent in the asymptotic-type illites.

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

The Phase Transformation and Crystal Structure Studies of Strontium Substituted Barium Monoferrite

NASA Astrophysics Data System (ADS)

Mulyawan, A.; Adi, W. A.; Mustofa, S.; Fisli, A.

2017-03-01

Unlike other AFe2O4 ferrite materials, Barium Monoferrite (BaFe2O4) have an orthorhombic structure which is very interesting to further study the crystal structure and phase formation. In this study, Strontium substituted Barium Monoferrite in the form of Ba(1-x)Sr(x)Fe2O4 has successfully been synthesized through solid state reaction method which includes BaCO3, SrCO3, and Fe2O3 as starting materials. Ba(1-x)Sr(x)Fe2O4 was made by varying the dopant composition of Strontium (Sr2+) from x = 0, 0.1, 0.3, and 0.5. Each composition was assisted by ethanol and continued to the milling process for 5 hours then followed by sintering process at 900 °C for 5 hours. The phase transformation was studied by using X-ray diffractometer (XRD) and Rietveld refinement using General Structure Analysis System (GSAS) also 3D crystal visualization using VESTA. Referring to the refinement results, a single phase of BaFe2O4 was formed in x = 0 and 0.1. The composition has orthorhombic structure, space group B b21m, and lattice parameters of a = 19.0229, b = 5.3814 c = 8.4524 Å, α = β = γ = 90° and a = 18.9978, b = 5.3802 c = 8.4385 Å, α = β = γ = 90° respectively. In the composition of x = 0.3 it was found that the phase of BaSrFe4O8 begin to form due to the overload expansion of the Sr2+ occupancy which made the distortion of the initial lattice parameters and finally in the x = 0.5 composition the single phase of BaSrFe4O8 was clearly formed. Energy Dispersive Spectroscopy (EDS) was used to confirm the change of the material structure by measuring the elemental compound composition ratio. The result of EDS spectra clearly exhibited the dominant elements were Barium (Ba), Strontium (Sr), Iron (Fe), and Oxygen (O) with the compound ratio (Atomic percentage and mass percentage) correspond to the BaFe2O4 and BaSrFe4O8 phase.

Zeta-potential and particle size studies of silver sulphide nanoparticles

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

Sharma, Vikash, E-mail: vikash@csr.res.in; Tarachand,; Ganesan, V.

Silver sulfide (Ag{sub 2}S) nanoparticles (NPs) were prepared successfully for the first time using diethylene glycol (DEG) as a surfactant. X-ray diffraction (XRD) data revealed single phase nature of the compound and energy-dispersive X-ray (EDX) confirmed its nominal composition. Their sizes were 43 nm from XRD, 50 nm from atomic force microscopy (AFM) and 19 nm & 213 nm from dynamic light scattering (DLS); their differences have been discussed. Autotitration study of zeta potential of these NPs in deionized water by DLS at different pH values confirmed an isoelectric point at pH = 5.14 and their very unstable nature in deionized water.

Structural phase analysis and photoluminescence properties of Mg-doped TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ali, T.; Ashraf, M. Anas; Ali, S. Asad; Ahmed, Ateeq; Tripathi, P.

2018-05-01

In this paper, we report the synthesis, characterization and photoluminescence properties of Mg-doped TiO2 nanoparticles (NPs). The samples were synthesized by sol-gel method and characterized using the standard analytical techniques such as X-ray diffraction (XRD), Transmission electron microscope (TEM), Energy dispersive X-ray spectroscopy (EDX), UV-visible and photoluminescence spectroscopy. The powder XRD spectra revealed that the synthesized samples are pure and crystalline in nature and showing tetragonal anatase phase of TiO2 NPs. UV-visible spectrum illustrates that an absorption edge shifts toward the visible region. This study may provide a new insight for making the nanomaterials which can be used in photocatalytic applications.

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

PubMed Central

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

2012-01-01

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

High pressure single-crystal micro X-ray diffraction analysis with GSE_ADA/RSV software

NASA Astrophysics Data System (ADS)

Dera, Przemyslaw; Zhuravlev, Kirill; Prakapenka, Vitali; Rivers, Mark L.; Finkelstein, Gregory J.; Grubor-Urosevic, Ognjen; Tschauner, Oliver; Clark, Simon M.; Downs, Robert T.

2013-08-01

GSE_ADA/RSV is a free software package for custom analysis of single-crystal micro X-ray diffraction (SCμXRD) data, developed with particular emphasis on data from samples enclosed in diamond anvil cells and subject to high pressure conditions. The package has been in extensive use at the high pressure beamlines of Advanced Photon Source (APS), Argonne National Laboratory and Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. The software is optimized for processing of wide-rotation images and includes a variety of peak intensity corrections and peak filtering features, which are custom-designed to make processing of high pressure SCμXRD easier and more reliable.

Synthesis and Characterization of YVO4-Based Phosphor Doped with Eu3+ Ions for Display Devices

NASA Astrophysics Data System (ADS)

Thakur, Shashi; Gathania, Arvind K.

2015-10-01

YVO4:Eu nanophosphor has been synthesized by the sol-gel method. Samples were characterized by x-ray diffraction (XRD), energy-dispersive x-ray spectroscopy, Fourier-transform infrared spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, photoluminescence, and Raman spectroscopy. The XRD profile confirms the tetragonal phase of the Eu3+-doped YVO4 nanophosphor. The efficiency of the prepared phosphor was analyzed by means of its emission spectral profile. We also observed rich red emission from the prepared phosphor on excitation by an ultraviolet source. The calculated Commission International de l'Éclairage coordinates reveal excellent color purity efficiency. Such luminescent powder is useful as red phosphor in display device applications.

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

X-ray Photoelectron Spectroscopy study of CaV1-xMoxO3-δ

NASA Astrophysics Data System (ADS)

Belyakov, S. A.; Kuznetsov, M. V.; Shkerin, S. N.

2018-06-01

An investigation was carried out on perovskite-based derivatives of CaV1-xMoxO3-δ using X-ray Photoelectron Spectroscopy (XPS). According to the XRD pattern, the area of homogeneity covers the region from x = 0 to x = 0.6. Wide XPS-peaks of Ca, V, Mo and O are observed, signalling that elements are presented in multiple states. A model for explaining the large chemical shifts of XPS peaks due to different charging effects on different parts of the sample surface is proposed.

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science.

PubMed

Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka

2010-09-01

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

Effect of gold photocathode contamination on a flat spectral response X-ray diode

NASA Astrophysics Data System (ADS)

Wang, Kun-lun; Zhang, Si-qun; Zhou, Shao-tong; Huang, Xian-bin; Ren, Xiao-dong; Dan, Jia-kun; Xu, Qiang

2018-03-01

A detector with an approximately flat spectral response is important for diagnosing intense thermal X-ray flux. A flat-spectral-response X-ray diode (FSR-XRD) utilizes a gold photocathode X-ray diode and a specially configured gold filter to give rise to a nearly flat spectral response in the photon energy range of 100-4000 eV. It has been observed that the spectral responses of several FSR-XRDs changed after a few shots of z-pinch experiments on the Primary Test Stand facility. This paper presents an analysis of the changes by fitting the spectral responses of the gold photocathodes using a model with a free parameter which characterizes the thickness of the contamination. The spectral responses of FSR-XRDs were calibrated with synchrotron radiation, and several cleaning methods were tested with the calibration. Considering the results of model and cleaning, it may be anticipated that contamination was the major reason of the response changing. Contamination worsened the flatness of the spectral response of the FSR-XRD and decreased the averaged response, hence it is important to avoid contamination. Current results indicate a requirement of further study of the contamination.

Feasibility of an integrated X-ray instrument for Mars exobiology and geology. [Abstract only

NASA Technical Reports Server (NTRS)

Fonda, M. L.; Schwartz, D. E.; Koppel, L. N.; Franco, E. D.; Kerner, J. A.

1994-01-01

By employing an integrated X-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details relevant to the possibility of the origin and evolution of life on Mars will be acquired. An integrated combined X Ray Fluorescence/X Ray Detection (XRF/XRD) instrument has been breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for Mars Environmental Survey (MESUR) and future Mars missions. Among others, primary objectives for the exploration of Mars include: the intense study of local areas on Mars to 'establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epochs; and to establish the global chemical and physical characteristics of the Martian surface'. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment.

Projection of the Liquidus Surface of the Co - Sn - Bi System

NASA Astrophysics Data System (ADS)

Abilov, Ch. I.; Allazov, M. R.; Sadygova, S. G.

2016-11-01

The crystallization behavior of phases in alloys of the Co - Sn - Bi system is studied by the methods of differential thermal (DTA), x-ray phase (XRP) and x-ray diffraction (XRD) analyses and hardness measurement. The projection of the liquidus surface is plotted. The boundaries of layering, the development of the monovariant processes, and the coordinates of the nonvariant equilibrium compositions are determined. Compositions of (Co3Sn2)1 - x Bi x solid solutions suitable for the production of antifriction materials are suggested.

Interface morphology of a Cr(001)/Fe(001) superlattice determined by scanning tunneling microscopy and x-ray diffraction: A comparison

NASA Astrophysics Data System (ADS)

Schmidt, C. M.; Bürgler, D. E.; Schaller, D. M.; Meisinger, F.; Güntherodt, H.-J.; Temst, K.

2001-01-01

A Cr(001)/Fe(001) superlattice with ten bilayers grown by molecular beam epitaxy on a Ag(001) substrate is studied by in situ scanning tunneling microscopy (STM) and ex situ x-ray diffraction (XRD). Layer-resolved roughness parameters determined from STM images taken in various stages of the superlattice fabrication are compared with average values reported in the literature or obtained from the fits of our XRD data. Good agreement is found for the rms roughnesses describing vertical roughness and for the lateral correlation lengths characterizing correlated as well as uncorrelated interface roughness if peculiarities of STM and XRD are taken into account. We discuss in detail (i) the possible differences between the STM topography of a free surface and the morphology of a subsequently formed interface, (ii) contributions due to chemical intermixing at the interfaces, (iii) the comparison of XRD parameters averaged over all interfaces versus layer-resolved STM parameters, and (iv) the question of the coherent field of view for the determination of rms values.

Probing Phase Transformations and Microstructural Evolutions at the Small Scales: Synchrotron X-ray Microdiffraction for Advanced Applications in [Phase 3 Memory,] 3D IC (Integrated Circuits) and Solar PV (Photovoltaic) Devices

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

Radchenko, I.; Tippabhotla, S. K.; Tamura, N.

2016-10-21

Synchrotron x-ray microdiffraction (μXRD) allows characterization of a crystalline material in small, localized volumes. Phase composition, crystal orientation and strain can all be probed in few-second time scales. Crystalline changes over a large areas can be also probed in a reasonable amount of time with submicron spatial resolution. However, despite all the listed capabilities, μXRD is mostly used to study pure materials but its application in actual device characterization is rather limited. This article will explore the recent developments of the μXRD technique illustrated with its advanced applications in microelectronic devices and solar photovoltaic systems. Application of μXRD in microelectronicsmore » will be illustrated by studying stress and microstructure evolution in Cu TSV (through silicon via) during and after annealing. Here, the approach allowing study of the microstructural evolution in the solder joint of crystalline Si solar cells due to thermal cycling will be also demonstrated.« less

X-Ray Diffraction of different samples of Swarna Makshika Bhasma.

PubMed

Gupta, Ramesh Kumar; Lakshmi, Vijay; Jha, Chandra Bhushan

2015-01-01

Shodhana and Marana are a series of complex procedures that identify the undesirable effects of heavy metals/minerals and convert them into absorbable and assimilable forms. Study on the analytical levels is essential to evaluate the structural and chemical changes that take place during and after following such procedures as described in major classical texts to understand the mystery behind these processes. X-Ray Diffraction (XRD) helps to identify and characterize minerals/metals and fix up the particular characteristics pattern of prepared Bhasma. To evaluate the chemical changes in Swarna Makshika Bhasma prepared by using different media and methods. In this study, raw Swarna Makshika, purified Swarna Makshika and four types of Swarna Makshika Bhasma prepared by using different media and methods were analyzed by XRD study. XRD study of different samples revealed strongest peaks of iron oxide in Bhasma. Other phases of Cu2O, FeS2, Cu2S, FeSO4, etc., were also identified in many of the samples. XRD study revealed that Swarna Makshika Bhasma prepared by Kupipakwa method is better, convenient, and can save time.

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

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

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

2012-01-15

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

Growth, characterization and estimation of lattice strain and size in CdS nanoparticles: X-ray peak profile analysis

NASA Astrophysics Data System (ADS)

Solanki, Rekha Garg; Rajaram, Poolla; Bajpai, P. K.

2018-05-01

This work is based on the growth, characterization and estimation of lattice strain and crystallite size in CdS nanoparticles by X-ray peak profile analysis. The CdS nanoparticles were synthesized by a non-aqueous solvothermal method and were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman and UV-visible spectroscopy. XRD confirms that the CdS nanoparticles have the hexagonal structure. The Williamson-Hall (W-H) method was used to study the X-ray peak profile analysis. The strain-size plot (SSP) was used to study the individual contributions of crystallite size and lattice strain from the X-rays peaks. The physical parameters such as strain, stress and energy density values were calculated using various models namely, isotropic strain model, anisotropic strain model and uniform deformation energy density model. The particle size was estimated from the TEM images to be in the range of 20-40 nm. The Raman spectrum shows the characteristic optical 1LO and 2LO vibrational modes of CdS. UV-visible absorption studies show that the band gap of the CdS nanoparticles is 2.48 eV. The results show that the crystallite size estimated from Scherrer's formula, W-H plots, SSP and the particle size calculated by TEM images are approximately similar.

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.

Pressure-induced kinetics of the α to ω transition in zirconium

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

Jacobsen, M. K.; Velisavljevic, N., E-mail: nenad@lanl.gov; Sinogeikin, S. V.

Diamond anvil cells (DAC) coupled with x-ray diffraction (XRD) measurements are one of the primary techniques for investigating structural stability of materials at high pressure-temperature (P-T) conditions. DAC-XRD has been predominantly used to resolve structural information at set P-T conditions and, consequently, provides P-T phase diagram information on a broad range of materials. With advances in large scale synchrotron x-ray facilities and corresponding x-ray diagnostic capabilities, it is now becoming possible to perform sub-second time resolved measurements on micron sized DAC samples. As a result, there is an opportunity to gain valuable information about the kinetics of structural phase transformationsmore » and extend our understanding of material behavior at high P-T conditions. Using DAC-XRD time resolved measurements, we have investigated the kinetics of the α to ω transformation in zirconium. We observe a clear time and pressure dependence in the martensitic α-ω transition as a function of pressure-jump, i.e., drive pressure. The resulting data are fit using available kinetics models, which can provide further insight into transformation mechanism that influence transformation kinetics. Our results help shed light on the discrepancies observed in previous measurements of the α-ω transition pressure in zirconium.« less

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.

An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

NASA Technical Reports Server (NTRS)

Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

1993-01-01

By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

Pressure-induced kinetics of the α to ω transition in zirconium

DOE PAGES

Jacobsen, M. K.; Velisavljevic, N.; Sinogeikin, S. V.

2015-07-13

Diamond anvil cells (DAC) coupled with x-ray diffraction (XRD) measurements are one of the primary techniques for investigating structural stability of materials at high pressure-temperature (P-T) conditions. DAC-XRD has been predominantly used to resolve structural information at set P-T conditions and, consequently, provides P-T phase diagram information on a broad range of materials. With advances in large scale synchrotron x-ray facilities and corresponding x-ray diagnostic capabilities, it is now becoming possible to perform sub-second time resolved measurements on micron sized DAC samples. As a result, there is an opportunity to gain valuable information about the kinetics of structural phase transformationsmore » and extend our understanding of material behavior at high P-T conditions. Using DAC-XRD time resolved measurements, we have investigated the kinetics of the α to ω transformation in zirconium. We observe a clear time and pressure dependence in the martensitic α-ω transition as a function of pressure-jump, i.e., drive pressure. The resulting data are fit using available kinetics models, which can provide further insight into transformation mechanism that influence transformation kinetics. Our results help shed light on the discrepancies observed in previous measurements of the α-ω transition pressure in zirconium.« less

Effects of copper on the preparation and characterization of Na-Ca-P borate glasses.

PubMed

Shailajha, S; Geetha, K; Vasantharani, P; Sheik Abdul Kadhar, S P

2015-03-05

Glasses in the system Na2O-CaO-B2O3-P2O5: CuO have been prepared by melt quenching at 1200°C and rapidly cooling at room temperature. The structural, optical and thermal properties have been investigated using X-ray diffraction (XRD), ultraviolet-visible (UV-VIS) spectroscopy, thermogravimetric-differential thermal analysis (TG-DTA), Fourier transform infrared (FTIR) spectroscopy, high resolution scanning electron microscopy (HRSEM) with energy dispersive X-ray (EDX) spectroscopy and high resolution transmission electron microscope (HRTEM) with energy dispersive X-ray (EDAX). The amorphous and crystalline nature of these samples was verified by XRD. Glass transition, crystallization and thermal stability were determined by TG-DTA investigations. Direct optical energy band gaps before and after doping with different percents of copper oxide were evaluated from 4.81eV to 2.99eV indicated the role of copper in the glassy matrix by UV spectra. FTIR spectrum reveals characteristic absorption bands due to various groups of triangular and tetrahedral borate network. Due to the amorphous nature, the particles like agglomerates on the glass surface were investigated by the HRSEM analysis. The crystalline nature of the samples in XRD is confirmed by SAED pattern using HRTEM. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali silica reaction in concrete structures

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

Dähn, R.; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This particular high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating themore » sample. Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. Furthermore, it is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali–silica reaction in concrete structures

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

Dähn, R., E-mail: rainer.daehn@psi.ch; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating the sample.more » Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. It is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

Characterization of pulsed laser deposition grown V2O3 converted VO2

NASA Astrophysics Data System (ADS)

Majid, Suhail; Shukla, D. K.; Rahman, F.; Gautam, Kamini; Sathe, V. G.; Choudhary, R. J.; Phase, D. M.

2016-10-01

Controllable tuning of Metal-insulator transition in VxOy thin film has been a field of extensive research. However controlled synthesis of desired Vanadium oxide phase is a challenging task. We have successfully achieved VO2 phase on Silicon substrate after post deposition annealing treatment to the PLD grown as deposited V2O3 thin films. The annealed thin film was characterized by x-ray diffraction (XRD), resistivity, Raman spectroscopy, X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS) measurements. XRD confirms the crystalline nature and growth of VO2 phase in thin film. The characteristic MIT was observed from resistivity measurements and transition temperature appeared at lower value around 336 K, compared to bulk VO2. The structural transition accompanied with MIT from lower temperature monoclinic phase to higher temperature Rutile phase became evident from temperature dependent Raman measurements. Chemical state of vanadium was examined using XAS and XPS measurements which confirm the presence of +4 oxidation state of vanadium in thin film.

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.

Studying Ultradisperse Diamond Structure within Explosively Synthesized Samples via X-Ray Techniques

NASA Astrophysics Data System (ADS)

Sharkov, M. D.; Boiko, M. E.; Ivashevskaya, S. N.; Belyakova, N. S.

2013-08-01

XRD (X-Ray Diffraction) and SAXS (Small-Angle X-Ray Scattering) data have been measured for a pair of samples produced with the help of explosives. XRD peaks have shown the both samples to contain crystal diamond components as well as graphite ones. Basing on SAXS analysis, possible presence of grains with radii up to 30-50 nm within all the samples has been shown. Structure components with fractal dimension between 1 and 2 in the sample have been detected, this fact being in agreement with the assumption of diamond grain coating similarity to onion shells. In order to broad rocking curves analysis, the standard SAXS treatment technique has been complemented by a Fourier filtering procedure. For the sample #1, rocking curve components corresponding to individual interplanar distances with magnitudes from 5 nm up to 15 nm have been separated. A hypothesis relating these values to the distances between concentric onion-like shells of diamond grains has been formulated.

Indentation size effects in single crystal copper as revealed by synchrotron x-ray microdiffraction

NASA Astrophysics Data System (ADS)

Feng, G.; Budiman, A. S.; Nix, W. D.; Tamura, N.; Patel, J. R.

2008-08-01

For a Cu single crystal, we find that indentation hardness increases with decreasing indentation depth, a phenomenon widely observed before and called the indentation size effect (ISE). To understand the underlying mechanism, we measure the lattice rotations in indentations of different sizes using white beam x-ray microdiffraction (μXRD); the indentation-induced lattice rotations are directly measured by the streaking of x-ray Laue spots associated with the indentations. The magnitude of the lattice rotations is found to be independent of indentation size, which is consistent with the basic tenets of the ISE model. Using the μXRD data together with an ISE model, we can estimate the effective radius of the indentation plastic zone, and the estimate is consistent with the value predicted by a finite element analysis. Using these results, an estimate of the average dislocation densities within the plastic zones has been made; the findings are consistent with the ISE arising from a dependence of the dislocation density on the depth of indentation.

A study on micro-structural and optical parameters of InxSe1-x thin film

NASA Astrophysics Data System (ADS)

Patel, P. B.; Desai, H. N.; Dhimmar, J. M.; Modi, B. P.

2018-04-01

Thin film of Indium Selenide (InSe) has been deposited by thermal evaporation technique onto pre cleaned glass substrate under high vacuum condition. The micro-structural and optical properties of InxSe1-x (x = 0.6, 1-x = 0.4) thin film have been characterized by X-ray diffractrometer (XRD) and UV-Visible spectrophotometer. The XRD spectra showed that InSe thin film has single phase hexagonal structure with preferred orientation along (1 1 0) direction. The micro-structural parameters (crystallite size, lattice strain, dislocation density, domain population) for InSe thin film have been calculated using XRD spectra. The optical parameters (absorption, transmittance, reflectance, energy band gap, Urbach energy) of InSe thin film have been evaluated from absorption spectra. The direct energy band gap and Urbach energy of InSe thin film is found to be 1.90 eV and 235 meV respectively.

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

Glass transition in ferroic glass K x (ND4)1-x D2PO4: a complete x-ray diffraction line shape analysis

NASA Astrophysics Data System (ADS)

Ranjan Choudhury, Rajul; Chitra, R.; Jayakrishnan, V. B.

2016-03-01

Quenching of dynamic disorder in glassy systems is termed as the glass transition. Ferroic glasses belong to the class of paracrystalline materials having crystallographic order in-between that of a perfect crystal and amorphous material, a classic example of ferroic glass is the solid solution of ferroelectric deuterated potassium dihydrogen phosphate and antiferroelectric deuterated ammonium dihydrogen phosphate. Lowering temperature of this ferroic glass can lead to a glass transition to a quenched disordered state. The subtle atomic rearrangement that takes place at such a glass transition can be revealed by careful examination of the temperature induced changes occurring in the x-ray powder diffraction (XRD) patterns of these materials. Hence we report here results of a complete diffraction line shape analysis of the XRD patterns recorded at different temperatures from deuterated mixed crystals DK x A1-x DP with mixing concentration x ranging as 0 < x < 1. Changes observed in diffraction peak shapes have been explained on the basis of structural rearrangements induced by changing O-D-O hydrogen bond dynamics in these paracrystals.

X-ray diffraction study of low-temperature phase transformations in nickel-titanium orthodontic wires.

PubMed

Iijima, M; Brantley, W A; Guo, W H; Clark, W A T; Yuasa, T; Mizoguchi, I

2008-11-01

Employ conventional X-ray diffraction (XRD) to analyze three clinically important nickel-titanium orthodontic wire alloys over a range of temperatures between 25 and -110 degrees C, for comparison with previous results from temperature-modulated differential scanning calorimetry (TMDSC) studies. The archwires selected were 35 degrees C Copper Ni-Ti (Ormco), Neo Sentalloy (GAC International), and Nitinol SE (3M Unitek). Neo Sentalloy, which exhibits superelastic behavior, is marketed as having shape memory in the oral environment, and Nitinol SE and 35 degrees C Copper Ni-Ti also exhibit superelastic behavior. All archwires had dimensions of 0.016in.x0.022in. (0.41 mm x 0.56 mm). Straight segments cut with a water-cooled diamond saw were placed side-by-side to yield a 1 cm x 1cm test sample of each wire product for XRD analysis (Rint-Ultima(+), Rigaku) over a 2theta range from 30 degrees to 130 degrees and at successive temperatures of 25, -110, -60, -20, 0 and 25 degrees C. The phases revealed by XRD at the different analysis temperatures were in good agreement with those found in previous TMDSC studies of transformations in these alloys, in particular verifying the presence of R-phase at 25 degrees C. Precise comparisons are not possible because of the approximate nature of the transformation temperatures determined by TMDSC and the preferred crystallographic orientation present in the wires. New XRD peaks appear to result from low-temperature transformation in martensite, which a recent transmission electron microscopy (TEM) study has shown to arise from twinning. While XRD is a useful technique to study phases in nickel-titanium orthodontic wires and their transformations as a function of temperature, optimum insight is obtained when XRD analyses are combined with complementary TMDSC and TEM study of the wires.

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

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

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

2015-06-15

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

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

NASA Astrophysics Data System (ADS)

Niu, Lei; Kang, Zhixin

2017-11-01

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

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

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

Fraass, Benedick Andrew

1980-01-01

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

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

Native structure of photosystem II at 1.95 Å resolution viewed by femtosecond X-ray pulses.

PubMed

Suga, Michihiro; Akita, Fusamichi; Hirata, Kunio; Ueno, Go; Murakami, Hironori; Nakajima, Yoshiki; Shimizu, Tetsuya; Yamashita, Keitaro; Yamamoto, Masaki; Ago, Hideo; Shen, Jian-Ren

2015-01-01

Photosynthesis converts light energy into biologically useful chemical energy vital to life on Earth. The initial reaction of photosynthesis takes place in photosystem II (PSII), a 700-kilodalton homodimeric membrane protein complex that catalyses photo-oxidation of water into dioxygen through an S-state cycle of the oxygen evolving complex (OEC). The structure of PSII has been solved by X-ray diffraction (XRD) at 1.9 ångström resolution, which revealed that the OEC is a Mn4CaO5-cluster coordinated by a well defined protein environment. However, extended X-ray absorption fine structure (EXAFS) studies showed that the manganese cations in the OEC are easily reduced by X-ray irradiation, and slight differences were found in the Mn-Mn distances determined by XRD, EXAFS and theoretical studies. Here we report a 'radiation-damage-free' structure of PSII from Thermosynechococcus vulcanus in the S1 state at a resolution of 1.95 ångströms using femtosecond X-ray pulses of the SPring-8 ångström compact free-electron laser (SACLA) and hundreds of large, highly isomorphous PSII crystals. Compared with the structure from XRD, the OEC in the X-ray free electron laser structure has Mn-Mn distances that are shorter by 0.1-0.2 ångströms. The valences of each manganese atom were tentatively assigned as Mn1D(III), Mn2C(IV), Mn3B(IV) and Mn4A(III), based on the average Mn-ligand distances and analysis of the Jahn-Teller axis on Mn(III). One of the oxo-bridged oxygens, O5, has significantly longer distances to Mn than do the other oxo-oxygen atoms, suggesting that O5 is a hydroxide ion instead of a normal oxygen dianion and therefore may serve as one of the substrate oxygen atoms. These findings provide a structural basis for the mechanism of oxygen evolution, and we expect that this structure will provide a blueprint for the design of artificial catalysts for water oxidation.

Interplay of structural, optical and magnetic properties in Gd doped CeO{sub 2}

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

Soni, S.; Dalela, S., E-mail: sdphysics@rediffmail.com; Kumar, Sudish

In this research wok systematic investigation on the synthesis, characterization, optical and magnetic properties of Ce{sub 1-x}Gd{sub x}O{sub 2} (where x=0.02, 0.04, 0.06, and 0.10) synthesized using the Solid-state method. Structural, Optical and Magnetic properties of the samples were investigated by X-ray diffraction (XRD), UV-VIS-NIR spectroscopy and VSM. Fluorite structure is confirmed from the XRD measurement on Gd doped CeO{sub 2} samples. Magnetic studies showed that the Gd doped polycrystalline samples display room temperature ferromagnetism and the ferromagnetic ordering strengthens with the Gd concentration.

In situ X-ray measurements of MOVPE growth of InxGa1-xN single quantum wells

NASA Astrophysics Data System (ADS)

Ju, Guangxu; Fuchi, Shingo; Tabuchi, Masao; Takeda, Yoshikazu

2013-05-01

GaN/InxGa1-xN/GaN single quantum wells (SQWs) have been grown on c-plane GaN/sapphire substrates using MOVPE system. PL (photoluminescence) and AFM (atomic force microscope) measurements demonstrate good quality of after-growth thermal-annealed SQWs. In situ XRD (X-ray diffraction), XRR (X-ray reflectivity), and X-ray CTR (crystal truncation rod) scattering measurements were successfully conducted on the SQWs under the NH3+N2 ambient at 1103 K. The analysis results of the XRR and the X-ray CTR spectra at 1103 K and at 300 K on the same sample matched well. It demonstrated that In0.09Ga0.91N SQW structure with several ML (monolayer) InGaN thicknesses was successfully investigated using the XRR and CTR scattering measurements at 1103 K.

Effects of X-ray irradiation on the Eu3+ → Eu2+ conversion in CaAl2O4 phosphors

NASA Astrophysics Data System (ADS)

Gomes, Manassés A.; Carvalho, Jéssica C.; Andrade, Adriano B.; Rezende, Marcos V.; Macedo, Zélia S.; Valerio, Mário E. G.

2018-01-01

This paper reports structural and luminescence properties of Eu-doped CaAl2O4 produced by an alternative sol-gel method using coconut water. Results of differential thermal analysis (DTA), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) allowed us to identify the best synthesis conditions for sample preparation. Simultaneous measurements of X-ray absorption spectroscopy (XAS) and X-ray excited optical luminescence (XEOL) were also performed in the X-ray energy range of the Eu LIII edge. Results from photoluminescence (PL) showed only the characteristic Eu3+ emission. However, radioluminescence emission spectra from Eu-doped CaAl2O4 shows a process of conversion of Eu3+ to Eu2+, which is induced by X-ray irradiation and is dependent on the radiation dose energy. X-ray absorption near edge structure (XANES) measurements corroborate Eu reduction due to irradiation, showing that only the Eu3+ ion is present in stable form in the CaAl2O4.

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.

Investigation of La and Al substitution on the spontaneous polarization and lattice dynamics of the Pb(1-x)LaxTi(1-x)AlxO3 ceramics

NASA Astrophysics Data System (ADS)

Yadav, Arun Kumar; Verma, Anita; Kumar, Sunil; Srihari, Velaga; Sinha, A. K.; Reddy, V. Raghavendra; Liu, Shun Wei; Biring, Sajal; Sen, Somaditya

2018-03-01

The phase purity and crystal structure of Pb(1-x)LaxTi(1-x)AlxO3 (0 ≤ x ≤ 0.25) samples (synthesized via the sol-gel process) were confirmed using synchrotron x-ray powder diffraction (XRD) (wavelength, λ = 0.44573 Å). Rietveld analyses of powder x-ray diffraction data confirmed the tetragonal structure for compositions with x ≤ 0.18 and cubic structure for the sample with x = 0.25. Temperature-dependent XRD was performed to investigate the structural change from tetragonal to cubic structure phase transition. Raman spectroscopy at room temperature also confirmed this phase transition with compositions. Field emission scanning electron microscopy (FESEM) provided information about the surface morphology while an energy dispersive x-ray spectrometer attached with FESEM confirmed the chemical compositions of samples. Temperature and frequency dependent dielectric studies showed that the tetragonal to cubic phase transition decreased from 680 K to 175 K with an increase in the x from 0.03 to 0.25, respectively. This is correlated with the structural studies. Electric field dependent spontaneous polarization showed a proper ferroelectric loop for 0.06 ≤ x ≤ 0.18 belonging to a tetragonal phase, while for x ≥ 0.25, the spontaneous polarization vanishes. Bipolar strain versus electric field revealed a butterfly loop for 0.06 ≤ x ≤ 0.18 compositions. Energy storage efficiency initially increases nominally with substitution but beyond x = 0.18 enhances considerably.

Rietveld refinement and FTIR analysis of bulk ceramic Co3-xMnxO4 compositions

NASA Astrophysics Data System (ADS)

Meena, P. L.; Kumar, Ravi; Sreenivas, K.

2013-02-01

Co3-xMnxO4 (x = 0.0, 0.6, 1.2) prepared by solid state reaction method and characterized by powder X-ray diffraction (XRD) and Fourier transform infrared (FTIR). Lattice parameters (a), oxygen parameter (u), and ionic radii of cations have been determined through Rietveld analysis. Both a and u parameters are related to expansion of octahedral site as Mn content in Co3O4. Analysis of XRD data show that Mn (x ≤ 1.2) is accommodated at the octahedral site, while retaining the cubic spinel structure. FTIR results also confirm the same and signify strong interactions due to overlapping of Co and Mn octahedra.

Ellipsometric study of Si(0.5)Ge(0.5)/Si strained-layer superlattices

NASA Technical Reports Server (NTRS)

Sieg, R. M.; Alterovitz, S. A.; Croke, E. T.; Harrell, M. J.

1993-01-01

An ellipsometric study of two Si(0.5)Ge(0.5)/Si strained-layer super lattices grown by MBE at low temperature (500 C) is presented, and results are compared with x ray diffraction (XRD) estimates. Excellent agreement is obtained between target values, XRD, and ellipsometry when one of two available Si(x)Ge(1-x) databases is used. It is shown that ellipsometry can be used to nondestructively determine the number of superlattice periods, layer thicknesses, Si(x)Ge(1-x) composition, and oxide thickness without resorting to additional sources of information. It was also noted that we do not observe any strain effect on the E(sub 1) critical point.

Application of Mythen detector: In-situ XRD study on the thermal expansion behavior of metal indium

NASA Astrophysics Data System (ADS)

Du, Rong; Chen, ZhongJun; Cai, Quan; Fu, JianLong; Gong, Yu; Wu, ZhongHua

2016-07-01

A Mythen detector has been equipped at the beamline 4B9A of Beijing Synchrotron Radiation Facility (BSRF), which is expected to enable BSRF to perform time-resolved measurement of X-ray diffraction (XRD) full-profiles. In this paper, the thermal expansion behavior of metal indium has been studied by using the in-situ XRD technique with the Mythen detector. The indium was heated from 303 to 433 K with a heating rate of 2 K/min. The in-situ XRD full-profiles were collected with a rate of one profile per 10 seconds. Rietveld refinement was used to extract the structural parameters. The results demonstrate that these collected quasi-real-time XRD profiles can be well used for structural analysis. The metal indium was found to have a nonlinear thermal expansion behavior from room temperature to the melting point (429.65 K). The a-axis of the tetragonal unit cell expands with a biquadratic dependency on temperature, while the c-axis contracts with a cubic dependency on temperature. By the time-resolved XRD measurements, it was observed that the [200] preferred orientation can maintain to about 403.15 K. While (110) is the last and detectable crystal plane just before melting of the polycrystalline indium foil. This study is not only beneficial to the application of metal indium, but also exhibits the capacity of in-situ time-resolved XRD measurements at the X-ray diffraction station of BSRF.

An X-ray diffraction method for semiquantitative mineralogical analysis of Chilean nitrate ore

USGS Publications Warehouse

Jackson, J.C.; Ericksent, G.E.

1997-01-01

Computer analysis of X-ray diffraction (XRD) data provides a simple method for determining the semiquantitative mineralogical composition of naturally occurring mixtures of saline minerals. The method herein described was adapted from a computer program for the study of mixtures of naturally occurring clay minerals. The program evaluates the relative intensities of selected diagnostic peaks for the minerals in a given mixture, and then calculates the relative concentrations of these minerals. The method requires precise calibration of XRD data for the minerals to be studied and selection of diffraction peaks that minimize inter-compound interferences. The calculated relative abundances are sufficiently accurate for direct comparison with bulk chemical analyses of naturally occurring saline mineral assemblages.

An x-ray diffraction method for semiquantitative mineralogical analysis of chilean nitrate ore

USGS Publications Warehouse

John, C.; George, J.; Ericksen, E.

1997-01-01

Computer analysis of X-ray diffraction (XRD) data provides a simple method for determining the semiquantitative mineralogical composition of naturally occurring mixtures of saline minerals. The method herein described was adapted from a computer program for the study of mixtures of naturally occurring clay minerals. The program evaluates the relative intensities of selected diagnostic peaks for the minerals in a given mixture, and then calculates the relative concentrations of these minerals. The method requires precise calibration of XRD data for the minerals to be studied and selection of diffraction peaks that minimize inter-compound interferences. The calculated relative abundances are sufficiently accurate for direct comparison with bulk chemical analyses of naturally occurring saline mineral assemblages.

Compressional residual stress in Bastogne boudins revealed by synchrotron X-ray microdiffraction

DOE PAGES

Chen, Kai; Kunz, Martin; Li, Yao; ...

2016-06-22

Lattice distortions in crystals can be mapped at the micron scale using synchrotron X-ray Laue microdiffraction (μXRD). From lattice distortions the shape and orientation of the elastic strain tensor can be derived and interpreted in terms of residual stress. We apply the new method to vein quartz from the original boudinage locality at Bastogne, Belgium. Furthermore, a long-standing debate surrounds the kinematics of the Bastogne boudins. The μXRD measurements reveal a shortening residual elastic strain, perpendicular to the vein wall, corroborating the model that the Bastogne boudins formed by layer-parallel shortening and not by layer-parallel extension, as is in themore » geological community generally inferred by the process of boudinage.« less

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).

Structural and optical properties of nanostructured nickel

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

Singh, J., E-mail: jaiveer24singh@gmail.com; Pandey, J.; Gupta, R.

2016-05-06

Metal nanoparticles are attractive because of their special structure and better optical properties. Nickel nanoparticles (Ni-Np) have been synthesized successfully by thermal decomposition method in the presence of trioctyl phosphine (TOP) and oleylamine (OAm). The samples were characterized by X-ray diffraction (XRD), Zetapotential measurement and Fourier transforms infrared (FTIR) spectroscopy. The size of Ni nanoparticles can be readily tuned from 13.86 nm. As-synthesized Ni nanoparticles have hexagonal closed pack (hcp) cubic structure as characterized by power X-ray diffraction (XRD) prepared at 280°C. The possible formation mechanism has also been phenomenological proposed for as synthesized Ni-Np. The value of Zeta potential wasmore » found 12.25 mV.« less

Deactivation of Zeolite Catalyst H-ZSM-5 during Conversion of Methanol to Gasoline: Operando Time- and Space-Resolved X-ray Diffraction.

PubMed

Rojo-Gama, Daniel; Mentel, Lukasz; Kalantzopoulos, Georgios N; Pappas, Dimitrios K; Dovgaliuk, Iurii; Olsbye, Unni; Lillerud, Karl Petter; Beato, Pablo; Lundegaard, Lars F; Wragg, David S; Svelle, Stian

2018-03-15

The deactivation of zeolite catalyst H-ZSM-5 by coking during the conversion of methanol to hydrocarbons was monitored by high-energy space- and time-resolved operando X-ray diffraction (XRD) . Space resolution was achieved by continuous scanning along the axial length of a capillary fixed bed reactor with a time resolution of 10 s per scan. Using real structural parameters obtained from XRD, we can track the development of coke at different points in the reactor and link this to a kinetic model to correlate catalyst deactivation with structural changes occurring in the material. The "burning cigar" model of catalyst bed deactivation is directly observed in real time.

Role of triton X-100 and hydrothermal treatment on the morphological features of nanoporous hydroxyapatite nanorods.

PubMed

Iyyappan, E; Wilson, P; Sheela, K; Ramya, R

2016-06-01

Hydroxyapatite (HA) particles were synthesized using Ca(NO3)2·4H2O and (NH4)2HPO4 as precursors with varying contents of non-ionic surfactant viz., triton X-100 (organic modifier) via co-precipitation method followed by hydrothermal treatment. The prepared HA particles have been characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FT-IR), Energy Dispersive X-ray Analysis (EDX), High Resolution Scanning Electron Microscopy (HRSEM), High Resolution Transmission Electron Microscopy (HRTEM) and Nitrogen adsorption-desorption experiments. The XRD and FTIR studies indicate the formation of HA phase in all the synthesized samples. The specific roles of triton X-100 and hydrothermal treatment in dispersing and in directing the crystal growth respectively have been discussed by comparing the observations from individual experiments using triton X-100 and hydrothermal treatment with that of combined protocol involving both. The plausible mechanism for the individual roles of both triton X-100 and hydrothermal treatment have been proposed. Copyright © 2016 Elsevier B.V. All rights reserved.

X-Ray Diffraction for In-Situ Mineralogical Analysis of Planetesimals.

NASA Astrophysics Data System (ADS)

Sarrazin, P.; Blake, D. F.; Dera, P.; Downs, R. T.; Taylor, J.

2017-12-01

X-ray diffraction (XRD) is a general purpose technique for definitive, quantitative mineralogical analysis. When combined with XRF data for sample chemistry, XRD analyses yield as complete a characterization as is possible by any spacecraft-capable techniques. The MSL CheMin instrument, the first XRD instrument flown in space, has been used to establish the quantitative mineralogy of the Mars global soil, to discover the first habitable environment on another planet, and to provide the first in-situ evidence of silicic volcanism on Mars. CheMin is now used to characterize the depositional and diagenetic environments associated with the mudstone sediments of lower strata of Mt. Sharp. Conventional powder XRD requires samples comprised of small grains presented in random orientations. In CheMin, sample cells are vibrated to cause loose powder to flow within the cell, driven by granular convection, which relaxes the requirement for fine grained samples. Nevertheless, CheMin still requires mechanisms to collect, crush, sieve and deliver samples before analysis. XTRA (Extraterrestrial Regolith Analyzer) is an evolution of CheMin intended to analyze fines in as-delivered surface regolith, without sample preparation. Fine-grained regolith coats the surfaces of most airless bodies in the solar system, and because this fraction is typically comminuted from the rocky regolith, it can often be used as a proxy for the surface as a whole. HXRD (Hybrid-XRD) is concept under development to analyze rocks or soils without sample preparation. Like in CheMin, the diffracted signal is collected with direct illumination CCD's. If the material is sufficiently fine-grained, a powder XRD pattern of the characteristic X-ray tube emission is obtained, similar to CheMin or XTRA. With coarse grained crystals, the white bremsstrahlung radiation of the tube is diffracted into Laue patterns. Unlike typical Laue applications, HXRD uses the CCD's capability to distinguish energy and analyze the "colors" of each Laue spot, which enable phase identification. The concept was demonstrated with prototypes and dedicated crystallographic software was developed for identification the minerals responsible for the Laue patterns. High TRL subsystems are under development for future deployment opportunities of these new XRD instruments.

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.

Synthesis of AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) alloy powders by mechanical alloying

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

Maulik, Ornov; Kumar, Vinod, E-mail: vkt.meta@mnit.ac.in; Adjunct Faculty, Materials Research Centre, Malaviya National Institute of Technology, Jaipur 302017

2015-12-15

Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7 mol) high-entropy alloys (HEAs) were synthesized by mechanical alloying. The effect of Mg content on the phase evolution of HEAs was investigated using X-Ray diffractometry (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) pattern analysis. The particle morphology and composition of HEAs were investigated by scanning electron microscopy (SEM). Thermodynamic parameters were calculated and analyzed to explain the formation of a solid solution. XRD analysis revealed BCC as major phase and FCC as a minor phase in as-milled AlFeCuCr and AlFeCuCrMg{sub 0.5} HEAs. Also, XRD analysis of as-milledmore » AlFeCuCrMg, AlFeCuCrMg{sub 1.7} confirmed the formation of two BCC phases (BCC 1 and BCC 2). TEM–SAED analysis of AlFeCuCrMg{sub x} HEAs concurred with XRD results. Microstructural features and mechanism for solid solution formation have been conferred in detail. Phase formation of the present HEAs has been correlated with calculated thermodynamic parameters. Differential thermal analysis (TGA-DTA) of these alloys confirmed that there is no substantial phase change up to 500 °C. - Highlights: • Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) HEAs were prepared by mechanical alloying. • Phase evolution and lattice parameter were studied by X-Ray Diffraction. • Crystallite size and lattice microstrain calculated failed to obey the Williamson–Hall method. • Criterions for formation of simple solid solution were compared to the thermodynamic parameters of the present HEAs. • Increase in the Mg concentration in AlMg{sub x}FeCuCr (x = 0, 0.5, 1, 1.7) HEAs supports the formation of BCC phase.« less

Uranium speciation as a function of depth in contaminated hanford sediments--a micro-XRF, micro-XRD, and micro- and bulk-XAFS study.

PubMed

Singer, David M; Zachara, John M; Brown, Gordon E

2009-02-01

The distribution and speciation of U and Cu in contaminated vadose zone and aquifer sediments from the U.S. DOE Hanford site (300 Area) were determined using a combination of synchrotron-based micro-X-ray fluorescence (microXRF) imaging, micro-X-ray absorption near edge structure (microXANES) spectroscopy, and micro-X-ray diffraction (microXRD) techniques combined with bulk U LIII-edge X-ray absorption fine structure (XAFS) spectroscopy. Samples were collected from within the inactive North Process Pond (NPP2) at 8 ft (2.4 m, NPP2-8) depth and 12 ft (3.7 m, NPP2-12) depth in the vadose zone, and fines were isolated from turbid groundwater just below the water Table (12-14 ft, approximately 4 m, NPP2-GW). microXRF imaging, microXRD, and microXANES spectroscopy revealed two major U occurrences within the vadose and groundwater zones: (1) low to moderate concentrations of U(VI) associated with fine-textured grain coatings that were consistently found to contain clinochlore (referred to here as chlorite) observed in all three samples, and (2) U(VI)-Cu(II) hotspots consisting of micrometer-sized particles associated with surface coatings on grains of muscovite and chlorite observed in samples NPP2-8' and NPP2-GW. In the aquifer fines (NPP2-GW), these particles were identified as cuprosklodowskite (cps: Cu[(UO2)(SiO2OH)]2 x 6H2O) and metatorbernite (mtb: Cu(UO2)2(PO4)2 x 8H2O). In contrast, the U-Cu-containing particles in the vadose zone were X-ray amorphous. Analyses of U LIII-edge XAFS spectra by linear-combination fitting indicated that U speciation consisted of (1) approximately 75% uranyl sorbed to chlorite and approximately 25% mtb-like X-ray amorphous U-Cu-phosphates (8 ft depth), (2) nearly 100% sorbed uranyl (12 ft depth), and (3) approximately 70% uranyl sorbed to chlorite and approximately 30% cps/mtb (groundwater zone). These findings suggest that dissolution of U(VI)-Cu(II)-bearing solids as well as desorption of U(VI), mainly from phyllosilicates, are important persistent sources of U(VI) to the associated uranium groundwater plume in Hanford Area 300.

XRD and EBSD analysis of anisotropic microstructure development in cold rolled F138 stainless steel

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

De Vincentis, N.S., E-mail: devincentis@ifir-conic

The microstructural characteristics of deformation-processed materials highly influence their mechanical properties. For a complete characterization of a microstructure both local and global information must be gathered, which requires the combination of different analysis techniques. X-ray and Electron Backscatter Diffraction were used in the present paper to characterize the deformation induced in a cold rolled F138 austenitic stainless steel sample. The results obtained using laboratory and synchrotron X-ray sources were compared and combined with EBSD quantitative results, allowing the global and local characterization and orientation dependence of the deformation microstructure. A particular behavior was observed in the XRD data corresponding tomore » the planes with < 220 >∥ ND, likely due to a smaller amount of defects accumulated in the crystals with that particular orientation. EBSD was used to separate the scans data into partitions and to calculate misorientation variables and parameters, showing that this behavior can be attributed to a combination of larger grain sizes, lower local boundary misorientations and dislocation densities for crystals having < 220 >∥ ND. Several conclusions, of general validity for the evaluation of microstructure anisotropy, can be extracted from the results. - Highlights: •Combined XRD and EBSD for studying microstructure gave a superb insight on anisotropic accumulation of defects. •W-H and CMWP methods were applied for checking consistency of results. •XRD showed that a smaller accumulation of defects occurred in crystals with < 220 >∥ ND. •High brilliance X-ray beam allowed to study the anisotropy of defect accumulation.« less

Evolved Gas Analysis and X-Ray Diffraction of Carbonate Samples from the 2009 Arctic Mars Analog Svalbard Expedition: Implications for Mineralogical Inferences from the Mars Science Laboratory

NASA Technical Reports Server (NTRS)

McAdam, A. C.; Mahaffy, P. R.; Blake, D. F.; Ming, D. W.; Franz, H. B.; Eigenbrode, J. L.; Steele, A.

2010-01-01

The 2009 Arctic Mars Analog Svalbard Expedition (AMASE) investigated several geologic settings using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return (MSR). AMASE-related research comprises both analyses conducted during the expedition and further analyses of collected samples using laboratory facilities at a variety of institutions. The Sample Analysis at Mars (SAM) instrument suite, which will be part of the Analytical Laboratory on MSL, consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser spectrometer (TLS). An Evolved Gas Analysis Mass Spectrometer (EGA-MS) was used during AMASE to represent part of the capabilities of SAM. The other instrument included in the MSL Analytical Laboratory is CheMin, which uses X-Ray Diffraction (XRD) and X-Ray Fluorescence (XRF) to perform quantitative mineralogical characterization of samples. Field-portable versions of CheMin were used during the AMASE 2009. Here, we discuss the preliminary interpretation of EGA and XRD analyses of selected AMASE carbonate samples and implications for mineralogical interpretations from MSL. Though CheMin will be the primary mineralogical tool on MSL, SAM EGA could be used to support XRD identifications or indicate the presence of volatile-bearing minerals which may be near or below XRD detection limits. Data collected with instruments in the field and in comparable laboratory setups (e.g., the SAM breadboard) will be discussed.

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

PubMed Central

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

2016-01-01

Zuotai (gTso thal) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100–800 nm, which commonly further aggregate into 1–30 μm loosely amorphous particles. XRD test shows that β-HgS, S8, and α-HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai, and it would play a positive role in interpreting this mysterious Tibetan drug. PMID:27738409

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

PubMed

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

2016-01-01

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

Application of x-ray absorption fine structure (XAFS) to local-order analysis in Fe-Cr maghemite-like materials

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

Montero-Cabrera, M. E., E-mail: elena.montero@cimav.edu.mx; Fuentes-Cobas, L. E.; Macías-Ríos, E.

2015-07-23

The maghemite-like oxide system γ-Fe{sub 2-x}Cr{sub x}O{sub 3} (x=0.75, 1 and 1.25) was studied by X-ray absorption fine structure (XAFS) and by synchrotron radiation X-ray diffraction (XRD). Measurements were performed at the Stanford Synchrotron Radiation Lightsource at room temperature, at beamlines 2-1, 2-3 and 4-3. High-resolution XRD patterns were processed by means of the Rietveld method. In cases of atoms being neighbors in the Periodic Table, the order/disorder degree of the considered solutions is indiscernible by “normal” (absence of “anomalous scattering”) diffraction experiments. Thus, maghemite-like materials were investigated by XAFS in both Fe and Cr K-edges to clarify, via short-rangemore » structure characterization, the local ordering of the investigated system. Athena and Artemis graphic user interfaces for IFEFFIT and FEFF8.4 codes were employed for XAFS spectra interpretation. Pre-edge decomposition and theoretical modeling of X-ray absorption near edge structure (XANES) transitions were performed. By analysis of the Cr K-edge XANES, it has been confirmed that Cr is located in an octahedral environment. Fitting of the extended X-ray absorption fine structure (EXAFS) spectra was performed under the consideration that the central atom of Fe is allowed to occupy octa- and tetrahedral positions, while Cr occupies only octahedral ones. Coordination number of neighboring atoms, interatomic distances and their quadratic deviation average were determined for x=1, by fitting simultaneously the EXAFS spectra of both Fe and Cr K-edges. The results of fitting the experimental spectra with theoretical standards showed that the cation vacancies tend to follow a regular pattern within the structure of the iron-chromium maghemite (FeCrO{sub 3})« less

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

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

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

2015-06-24

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

Investigating the Defect Structures in Transparent Conducting Oxides Using X-ray and Neutron Scattering Techniques

PubMed Central

González, Gabriela B.

2012-01-01

Transparent conducting oxide (TCO) materials are implemented into a wide variety of commercial devices because they possess a unique combination of high optical transparency and high electrical conductivity. Created during the processing of the TCOs, defects within the atomic-scale structure are responsible for their desirable optical and electrical properties. Therefore, studying the defect structure is essential to a better understanding of the behavior of transparent conductors. X-ray and neutron scattering techniques are powerful tools to investigate the atomic lattice structural defects in these materials. This review paper presents some of the current developments in the study of structural defects in n-type TCOs using x-ray diffraction (XRD), neutron diffraction, extended x-ray absorption fine structure (EXAFS), pair distribution functions (PDFs), and x-ray fluorescence (XRF). PMID:28817010

Laser-driven powerful kHz hard x-ray source

NASA Astrophysics Data System (ADS)

Li, Minghua; Huang, Kai; Chen, Liming; Yan, Wenchao; Tao, Mengze; Zhao, Jiarui; Ma, Yong; Li, Yifei; Zhang, Jie

2017-08-01

A powerful hard x-ray source based on laser plasma interaction is developed. By introducing the kHz, 800 nm pulses onto a rotating molybdenum (Mo) disk target, intense Mo Kα x-rays are emitted with suppressed bremsstrahlung background. Results obtained with different laser intensities suggest that the dominant absorption mechanism responsible for the high conversion efficiency is vacuum heating (VH). The high degree of spatial coherence is verified. With the high average flux and a source size comparable to the laser focus spot, absorption contrast imaging and phase contrast imaging are carried out to test the imaging capability of the source. Not only useful for imaging application, this compact x-ray source is also holding great potential for ultrafast x-ray diffraction (XRD) due to the intrinsic merits such as femtosecond pulse duration and natural synchronization with the driving laser pulses.

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

NASA Astrophysics Data System (ADS)

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

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

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

NASA Technical Reports Server (NTRS)

Garlick, R. G.; Lowell, C.

1973-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2013-11-01

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

Raman structural studies of the nickel electrode

NASA Technical Reports Server (NTRS)

Cornilsen, Bahne C.

1994-01-01

The objectives of this investigation have been to define the structures of charged active mass, discharged active mass, and related precursor materials (alpha-phases), with the purpose of better understanding the chemical and electrochemical reactions, including failure mechanisms and cobalt incorporation, so that the nickel electrode may be improved. Although our primary tool has been Raman spectroscopy, the structural conclusions drawn from the Raman data have been supported and augmented by three other analysis methods: infrared spectroscopy, powder X-ray Diffraction (XRD), and x-ray absorption spectroscopy (in particular EXAFS, Extended X-ray Absorption Fine Structure spectroscopy).

Local symmetry breaking in SnO2 nanocrystals with cobalt doping and its effect on optical properties.

PubMed

Roy, S; Joshi, Amish G; Chatterjee, S; Ghosh, Anup K

2018-06-07

X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to study the structural and morphological characteristics of cobalt doped tin(iv) oxide (Sn1-xCoxO2; 0 ≤ x ≤ 0.04) nanocrystals synthesized by a chemical co-precipitation technique. Electronic structure analysis using X-ray photoemission spectroscopy (XPS) shows the formation of tin interstitials (Sni) and reduction of oxygen vacancies (VO) in the host lattice on Co doping and that the doped Co exists in mixed valence states of +2 and +3. Using XRD, the preferential position of the Sni and doped Co in the unit cell of the nanocrystals have been estimated. Rietveld refinement of XRD data shows that samples are of single phase and variation of lattice constants follows Vegard's law. XRD and TEM measurements show that the crystallite size of the nanocrystals decrease with increase in Co doping concentration. SAED patterns confirm the monocrystalline nature of the samples. The study of the lattice dynamics using Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy shows the existence of many disorder activated forbidden optical phonon modes, along with the corresponding classical modes, signifying Co induced local symmetry breaking in the nanocrystals. UV-Vis spectroscopy shows that the optical band gap has red shifted with increase in doping concentration. The study of Urbach energy confirms the increase in disorder in the nanocrystals with Co doping. Local symmetry breaking induced UV emission along with violet, blue and green luminescence has been observed from the PL study. The spectral contribution of UV emission decreases and green luminescence increases with increase in doping. Using PL, in conjunction with Raman spectroscopy, the type of oxygen vacancy induced in the nanocrystals on Co doping has been confirmed and the position of the defect levels in the forbidden zone (w.r.t. the optical band gap) has been studied.

Combining µXANES and µXRD mapping to analyse the heterogeneity in calcium carbonate granules excreted by the earthworm Lumbricus terrestris

PubMed Central

Brinza, Loredana; Schofield, Paul F.; Hodson, Mark E.; Weller, Sophie; Ignatyev, Konstantin; Geraki, Kalotina; Quinn, Paul D.; Mosselmans, J. Frederick W.

2014-01-01

The use of fluorescence full spectral micro-X-ray absorption near-edge structure (µXANES) mapping is becoming more widespread in the hard energy regime. This experimental method using the Ca K-edge combined with micro-X-ray diffraction (µXRD) mapping of the same sample has been enabled on beamline I18 at Diamond Light Source. This combined approach has been used to probe both long- and short-range order in calcium carbonate granules produced by the earthworm Lumbricus terrestris. In granules produced by earthworms cultured in a control artificial soil, calcite and vaterite are observed in the granules. However, granules produced by earthworms cultivated in the same artificial soil amended with 500 p.p.m. Mg also contain an aragonite. The two techniques, µXRD and µXANES, probe different sample volumes but there is good agreement in the phase maps produced. PMID:24365942

Unraveling submicron-scale mechanical heterogeneity by three-dimensional X-ray microdiffraction

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

Li, Runguang; Xie, Qingge; Wang, Yan-Dong

Shear banding is a ubiquitous phenomenon of severe plastic deformation, and damage accumulation in shear bands often results in the catastrophic failure of a material. Despite extensive studies, the microscopic mechanisms of strain localization and deformation damage in shear bands remain elusive due to their spatial-temporal complexities embedded in bulk materials. Here we conducted synchrotron-based X-ray microdiffraction (μXRD) experiments to map out the 3D lattice strain field with a submicron resolution around fatigue shear bands in a stainless steel. Both in situ and postmortem μXRD results revealed large lattice strain gradients at intersections of the primary and secondary shear bands.more » Such strain gradients resulted in severe mechanical heterogeneities across the fatigue shear bands, leading to reduced fatigue limits in the high-cycle regime. The ability to spatially quantify the localized strain gradients with submicron resolution through μXRD opens opportunities for understanding the microscopic mechanisms of damage and failure in bulk materials.« less

X-ray Diffraction and Rietveld Refinement in Deferrified Clays for Forensic Science.

PubMed

Prandel, Luis V; Melo, Vander de F; Brinatti, André M; Saab, Sérgio da C; Salvador, Fábio A S

2018-01-01

Soil vestiges might provide information about a crime scene. The Rietveld method with X-ray diffraction data (RM-XRD) is a nondestructive technique that makes it possible to characterize minerals present in the soils. Soil clays from the metropolitan region of Curitiba (Brazil) were submitted to DCB treatment and analyzed using XRD with CuK α radiation in the step-scan mode (0.02° 2θ/5 s). The GSAS+EXPGUI software was used for RM refinement. The RM-XRD results, together with the principal component analysis (PCA) (52.6% total variance), showed the kaolinite predominance in most analyzed samples and the highest quartz contents in "site 1." Higher anatase, and gibbsite and muscovite contents influenced discrimination, mainly in "site 3" and "site 1," respectively. These results were enough to discriminate clays of four sites and two horizons using a reduced amount of sample showing that the technique can be applied to the investigation into soil vestiges. © 2017 American Academy of Forensic Sciences.

Structural, XPS and magnetic studies of pulsed laser deposited Fe doped Eu{sub 2}O{sub 3} thin film

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

Kumar, Sandeep; Prakash, Ram, E-mail: rpgiuc@gmail.com; Choudhary, R.J.

2015-10-15

Highlights: • Growth of Fe doped Eu{sub 2}O{sub 3} thin films by PLD. • XRD and Raman’s spectroscopy used for structure confirmation. • The electronic states of Eu and Fe are confirmed by XPS. • Magnetic properties reveals room temperature magnetic ordering in deposited film. - Abstract: Fe (4 at.%) doped europium (III) oxide thin film was deposited on silicon (1 0 0) substrate by pulsed laser deposition technique. Structural, spectral and magnetic properties were studied by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and magnetization measurements. XRD and Raman spectroscopy reveal that the grown film is singlemore » phased and belongs to the cubic structure of Eu{sub 2}O{sub 3}. XPS study of the Eu{sub 1.92}Fe{sub 0.08}O{sub 3} film shows that Fe exists in Fe{sup 3+} ionic state in the film. The film exhibits magnetic ordering at room temperature.« less

Boron-doped diamond synthesized at high-pressure and high-temperature with metal catalyst

NASA Astrophysics Data System (ADS)

Shakhov, Fedor M.; Abyzov, Andrey M.; Kidalov, Sergey V.; Krasilin, Andrei A.; Lähderanta, Erkki; Lebedev, Vasiliy T.; Shamshur, Dmitriy V.; Takai, Kazuyuki

2017-04-01

The boron-doped diamond (BDD) powder consisting of 40-100 μm particles was synthesized at 5 GPa and 1500-1600 °C from a mixture of 50 wt% graphite and 50 wt% Ni-Mn catalyst with an addition of 1 wt% or 5 wt% boron powder. The size of crystal domains of doped and non-doped diamond was evaluated as a coherent scattering region by X-ray diffraction (XRD) and using small-angle neutron scattering (SANS), being ≥180 nm (XRD) and 100 nm (SANS). Magnetic impurities of NiMnx originating from the catalyst in the synthesis, which prevent superconductivity, were detected by magnetization measurements at 2-300 K. X-ray photoelectron spectroscopy, the temperature dependence of the resistivity, XRD, and Raman spectroscopy reveal that the concentration of electrically active boron is as high as (2±1)×1020 cm-3 (0.1 at%). To the best of our knowledge, this is the highest boron content for BDD synthesized in high-pressure high-temperature process with metal catalysts.

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

PubMed

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

2014-06-01

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

Unraveling submicron-scale mechanical heterogeneity by three-dimensional X-ray microdiffraction

DOE PAGES

Li, Runguang; Xie, Qingge; Wang, Yan-Dong; ...

2017-12-28

Shear banding is a ubiquitous phenomenon of severe plastic deformation, and damage accumulation in shear bands often results in the catastrophic failure of a material. Despite extensive studies, the microscopic mechanisms of strain localization and deformation damage in shear bands remain elusive due to their spatial-temporal complexities embedded in bulk materials. Here we conducted synchrotron-based X-ray microdiffraction (μXRD) experiments to map out the 3D lattice strain field with a submicron resolution around fatigue shear bands in a stainless steel. Both in situ and postmortem μXRD results revealed large lattice strain gradients at intersections of the primary and secondary shear bands.more » Such strain gradients resulted in severe mechanical heterogeneities across the fatigue shear bands, leading to reduced fatigue limits in the high-cycle regime. The ability to spatially quantify the localized strain gradients with submicron resolution through μXRD opens opportunities for understanding the microscopic mechanisms of damage and failure in bulk materials.« less

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.

Step-by-step fabrication of a highly oriented crystalline three-dimensional pillared-layer-type metal-organic framework thin film confirmed by synchrotron X-ray diffraction.

PubMed

Otsubo, Kazuya; Haraguchi, Tomoyuki; Sakata, Osami; Fujiwara, Akihiko; Kitagawa, Hiroshi

2012-06-13

Fabrication of a crystalline ordered thin film based on the porous metal-organic frameworks (MOFs) is one of the practical applications of the future functional nanomaterials. Here, we report the creation of a highly oriented three-dimensional (3-D) porous pillared-layer-type MOF thin film on a metal substrate using a step-by-step approach based on liquid-phase epitaxy. Synchrotron X-ray diffraction (XRD) study clearly indicates that the thin film is crystalline and its orientation is highly controlled in both horizontal and vertical directions relative to the substrate. This report provides the first confirmation of details of not only the crystallinity but also the orientation of 3-D MOF thin film using synchrotron XRD. Moreover, we also demonstrate its guest adsorption/desorption behavior by using in situ XRD measurements. The results presented here would promise useful insights for fabrication of MOF-based nanodevices in the future.

Unraveling submicron-scale mechanical heterogeneity by three-dimensional X-ray microdiffraction

PubMed Central

Li, Runguang; Xie, Qingge; Wang, Yan-Dong; Liu, Wenjun; Wang, Mingguang; Wu, Guilin; Li, Xiaowu; Zhang, Minghe; Lu, Zhaoping; Geng, Chang; Zhu, Ting

2018-01-01

Shear banding is a ubiquitous phenomenon of severe plastic deformation, and damage accumulation in shear bands often results in the catastrophic failure of a material. Despite extensive studies, the microscopic mechanisms of strain localization and deformation damage in shear bands remain elusive due to their spatial−temporal complexities embedded in bulk materials. Here we conducted synchrotron-based X-ray microdiffraction (μXRD) experiments to map out the 3D lattice strain field with a submicron resolution around fatigue shear bands in a stainless steel. Both in situ and postmortem μXRD results revealed large lattice strain gradients at intersections of the primary and secondary shear bands. Such strain gradients resulted in severe mechanical heterogeneities across the fatigue shear bands, leading to reduced fatigue limits in the high-cycle regime. The ability to spatially quantify the localized strain gradients with submicron resolution through μXRD opens opportunities for understanding the microscopic mechanisms of damage and failure in bulk materials. PMID:29284751

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.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

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

Leonardo da Vinci's drapery studies: characterization of lead white pigments by µ-XRD and 2D scanning XRF

NASA Astrophysics Data System (ADS)

Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Wallez, Gilles; Mottin, Bruno

2015-11-01

This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of µ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Département des Arts Graphiques, Musée du Louvre and in the Musée des Beaux- Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special µ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique.

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

PubMed

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

2015-12-01

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

An investigation into the role of polyethyleneimine in chemical bath deposition of zinc oxide nanowires

NASA Astrophysics Data System (ADS)

Eskandari, Alireza; Abdizadeh, Hossein; Pourshaban, Erfan; Golobostanfard, Mohammad Reza

2018-01-01

Zinc oxide nanowires are considered as promising materials for wide range of optoelectrical and chemical devices, thanks to their desirable structural and optoelectrical properties. Over the past decade, chemical bath deposition (CBD) has been widely used to synthesize these nanostructures due to its low cost and controllability. Since improving the aspect ratio and length of nanowires is a vital issue in growing one-dimensional nanostructures, the influence of polyethyleneimine (PEI) as a complexing and chelating agent on the structural, morphological, and optoelectrical properties of ZnO nanowires has been studied in this report. As-grown ZnO nanowires synthesized by mixing deionized water, zinc acetate dihydrate, hexamethylenetetramine, and PEI were characterized with field emission scanning electron microscope (FESEM), X-ray diffractometer (XRD), and photoluminescence spectroscopy (PL). FESEM results unambiguously show that increasing PEI concentration (from 0 to 0.2 g in 50 ml DI water) reduces the diameter and density of nanowires from ˜120 to 56 nm and from ˜85% to 65%, respectively. Interestingly, although adding more PEI decreases nanowires diameter, over-increasing of PEI brings about an inappropriate nanostructures growth. Moreover, XRD patterns demonstrate that all the samples have wurtzite structure with a preferred orientation along c-axis which may be improved or deteriorated by adding PEI into the chemical bath. Accordingly, it is crucial to optimize the amount of PEI in CBD method. Near-band edge (NBE) region in PL spectrum also confirms wide bandgap of ZnO (˜3.3 eV). In addition, comparing the appearance of PEI free with PEI assisted solutions show a considerable difference in their colors, which may be attributed to the formation of new chemical compounds. Considering these results, PEI plays a couple of determining roles in synthesizing ZnO nanowires; making nanowires thinner, with selectively absorption to the non-polar, lateral facets of wurtzite lattice, and controlling deposition rate by forming the PEI-Zn2+-HCHO complex compounds.

[Effect of three kinds of rare earth oxides on chromaticity and mechanical properties of zirconia ceramic].

PubMed

Huang, Hui; Zhang, Fu-qiang; Sun, Jing; Gao, Lian

2006-06-01

To evaluate the colouration of zirconia ceramic by adding three kinds of rare earth oxides. The influence of the pigments concentration on the mechanical properties and the microstructure was also analyzed. Added different concentrations of CeO(2), Er(2)O(3) and Pr(6)O(11) in tetragonal zirconia poly crystals stabilized with 3 mol% yttria (3Y-T2P) powder, compacted at 200 MPa using cold isostatic pressure, and sintered to 1 400 degrees C. The heating rate was 150 degrees C/h and the dwelling time was 2 hours. The chromaticity of sintered bodies was measured with chroma meter. The relative density, hardness, flexure strength and fracture toughness were investigated as well. The phase stability of the colorized and pure zirconia was evaluated by X-ray diffraction (XRD) using an automated diffractometer. The microstructures of the specimens were evaluated by scanning electron microscope (SEM). Several kinds of color achieved by the different pigments praseodym oxide, cerium oxide and erbium oxide were presented in the CIELab system. The a* value increased with the added amount of Er(2)O(3), while b* value rose with the increasing amount of CeO(2) and Pr(6)O(11). However, three pigments failed to decrease L* value and the sintered body appeared too bright. Adding three pigments influenced flexure strength of zirconia ceramic significantly, but had little influence on the hardness and fracture toughness. Microscopy revealed the relationship between the porosity and shapes of grains was correlated to strength of the diphase ceramics. No additional phase could be detected by XRD, except t-ZrO(2) in all colorized samples after sintering at 1 400 degrees C for 120 min. Zirconia ceramic can be colorized by CeO(2), Er(2)O(3), and Pr(6)O(11). Pigments even in a small amount influence the mechanical properties of the colorized zirconia material, which necessitates further investigation.

Electrochemical synthesis of nanostructured Se-doped SnS: Effect of Se-dopant on surface characterizations

NASA Astrophysics Data System (ADS)

Kafashan, Hosein; Azizieh, Mahdi; Balak, Zohre

2017-07-01

SnS1-xSex nanostructures with different Se-dopant concentrations were deposited on fluorine doped tin oxide (FTO) substrate through cathodic electrodeposition technique. The pH, temperature, applied potential (E), and deposition time remained were 2.1, 60 °C, -1 V, and 30 min, respectively. SnS1-xSex nanostructures were characterized using X-ray diffraction (XRD), field emission scanning electron microcopy (FESEM), energy dispersive X-ray spectroscopy (EDX), room temperature photoluminescence (PL), and UV-vis spectroscopy. The XRD patterns revealed that the SnS1-xSex nanostructures were polycrystalline with orthorhombic structure. FESEM showed various kinds of morphologies in SnS1-xSex nanostructures due to Se-doping. PL and UV-vis spectroscopy were used to evaluate the optical properties of SnS1-xSex thin films. The PL spectra of SnS1-xSex nanostructures displayed four emission peaks, those are a blue, a green, an orange, and a red emission. UV-vis spectra showed that the optical band gap energy (Eg) of SnS1-xSex nanostructures varied between 1.22-1.65 eV, due to Se-doping.

Long- and Short-Range Structure of Ferrimagnetic Iron-Chromium Maghemites.

PubMed

García-Guaderrama, Marco; Montero-Cabrera, María E; Morán, Emilio; Alario-Franco, Miguel A; Fuentes-Cobas, Luis E; Macías-Ríos, Edgar; Esparza-Ponce, Hilda E; Fuentes-Montero, María E

2015-12-07

Maghemite-like materials containing Fe(3+) and Cr(3+) in comparable amounts have been prepared by solution-combustion synthesis. The conditions of synthesis and the magnetic properties are described. These materials are ferrimagnetic and are much more stable than pure iron maghemite since their maghemite-hematite transformation takes place at about ∼ 700 °C instead of ∼ 300 °C, as usually reported. These materials were studied by synchrotron radiation X-ray diffraction (XRD) and by X-ray absorption fine structure (XAFS) of the K-absorption edge of two elements. High-resolution XRD patterns were processed by means of the Rietveld method. Thus, maghemites were studied by XAFS in both Fe and Cr K-edges to clarify the short-range structure of the investigated systems. Pre-edge decomposition and theoretical modeling of X-ray absorption near edge structure transitions were performed. The extended X-ray absorption fine structure (EXAFS) spectra were fitted considering the facts that the central atom of Fe is able to occupy octahedral and tetrahedral sites, each with a weight adjustment, while Cr occupies only octahedral sites. Interatomic distances were determined for x = 1, by fitting simultaneously both Fe and Cr K-edges average EXAFS spectra. The results showed that the cation vacancies tend to follow a regular pattern within the structure of the iron-chromium maghemite (FeCrO3).

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.

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Chongad, L. S.; Sharma, A.; Banerjee, M.; Jain, A.

2016-10-01

Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H2S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD.

Synchrotron WAXS and XANES studies of silica (SiO2) powders synthesized from Indonesian natural sands

NASA Astrophysics Data System (ADS)

Muchlis, Khairanissa; Aini Fauziyah, Nur; Soontaranon, Siriwat; Limpirat, Wanwisa; Pratapa, Suminar

2017-01-01

In this study, we have investigated polymorphic silica (SiO2) powders using, Wide Angle X-ray Scattering (WAXS) and X-Ray Absorption Near Edge Spectroscopy (XANES), laboratory X-Ray Diffraction (XRD) instruments. The WAXS and XANES spectra were collected using synchrotron radiation at Synchrotron Light Research Institute (SLRI), Nakhon Ratchasima, Thailand. The silica powders were obtained by processing silica sand from Tanah Laut, South Kalimantan, Indonesia. Purification process of silica sand was done by magnetic separation and immersion with HCl. The purification step was needed to reduce impurity or undesirable non Si elements. Three polymorphs of silica were produced, i.e. amorphous phase (A), quartz (B), and cristobalite (C). WAXS profile for each phase was presented in terms of intensity vs. 2θ prior to analyses. Both XRD (λCuKα=1.54056 Å) and WAXS (λ=1.09 Å) patttern show that (1) A sample contains no crystallites, (2) B sample is monophasic, contains only quartz, and (3) C sample contains cristobalite and trydimite. XRD quantitative analysis using Rietica gave 98,8 wt% cristobalite, while the associated WAXS data provided 98.7 wt% cristobalite. Si K-edge XANES spectra were measured at energy range 1840 to 1920 eV. Qualitatively, the pre-edge and edge features for all phases are similar, but their main peaks in the post-edge region are different.

Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

NASA Astrophysics Data System (ADS)

Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

2009-12-01

Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

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

Treesearch

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

2017-01-01

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

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

PubMed Central

2013-01-01

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1H and 13C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1H and 13C chemical shifts for directly bonded 13C–1H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure. PMID:24386493

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids.

PubMed

Dudenko, Dmytro V; Williams, P Andrew; Hughes, Colan E; Antzutkin, Oleg N; Velaga, Sitaram P; Brown, Steven P; Harris, Kenneth D M

2013-06-13

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1 H and 13 C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1 H and 13 C chemical shifts for directly bonded 13 C- 1 H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure.

Field-induced polarization rotation and phase transitions in 0.70 Pb ( M g 1 / 3 N b 2 / 3 ) O 3 – 0.30 PbTi O 3 piezoceramics observed by in situ high-energy x-ray scattering

DOE PAGES

Hou, Dong; Usher, Tedi -Marie; Fulanovic, Lovro; ...

2018-06-12

Changes to the crystal structure of 0.70Pb(Mg 1/3Nb 2/3)O 3–0.30PbTiO 3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic Cm at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF resultsmore » show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. Furthermore, this study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-xPT piezoceramics.« less

Field-induced polarization rotation and phase transitions in 0.70 Pb ( M g 1 / 3 N b 2 / 3 ) O 3 – 0.30 PbTi O 3 piezoceramics observed by in situ high-energy x-ray scattering

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

Hou, Dong; Usher, Tedi -Marie; Fulanovic, Lovro

Changes to the crystal structure of 0.70Pb(Mg 1/3Nb 2/3)O 3–0.30PbTiO 3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic Cm at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF resultsmore » show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. Furthermore, this study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-xPT piezoceramics.« less

Field-induced polarization rotation and phase transitions in 0.70 Pb (M g1 /3N b2 /3 ) O3-0.30 PbTi O3 piezoceramics observed by in situ high-energy x-ray scattering

NASA Astrophysics Data System (ADS)

Hou, Dong; Usher, Tedi-Marie; Fulanovic, Lovro; Vrabelj, Marko; Otonicar, Mojca; Ursic, Hana; Malic, Barbara; Levin, Igor; Jones, Jacob L.

2018-06-01

Changes to the crystal structure of 0.70 Pb (M g1 /3N b2 /3 ) O3-0.30 PbTi O3 (PMN-0.30PT) piezoceramic under application of electric fields at the long-range and local scale are revealed by in situ high-energy x-ray diffraction (XRD) and pair-distribution function (PDF) analyses, respectively. The crystal structure of unpoled samples is identified as monoclinic C m at both the long-range and local scale. In situ XRD results suggest that field-induced polarization rotation and phase transitions occur at specific field strengths. A polarization rotation pathway is proposed based on the Bragg-peak behaviors and the Le Bail fitting results of the in situ XRD patterns. The PDF results show systematic changes to the structures at the local scale, which is in agreement with the changes inferred from the in situ XRD study. More importantly, our results prove that polarization rotation can be detected and determined in a polycrystalline relaxor ferroelectric. This study supports the idea that multiple contributions, specifically ferroelectric-ferroelectric phase transition and polarization rotation, are responsible for the high piezoelectric properties at the morphotropic phase boundary of PMN-x PT piezoceramics.

DSC and Raman studies of silver borotellurite glasses

NASA Astrophysics Data System (ADS)

Kaur, Amandeep; Khanna, Atul; Gonzàlez, Fernando

2016-05-01

Silver borotellurite glasses of composition: xAg2O-yB2O3-(100-x-y)TeO2 (x=20-mol%, y = 0, 10, 20 and 30-mol%) were prepared and characterized by density, X-ray diffraction (XRD), differential scanning calorimetry, and Raman spectroscopy. XRD confirmed the amorphous structure of all samples. Density of glasses decreases while the glass transition temperature increases with increase in B2O3 content from 10 to 30-mol%. Raman study shows that coordination number of Te with oxygen decreases steadily from 3.42 to 3.18 on adding B2O3 due to the transformation of TeO4 into TeO3 units.

Adsorption of antibiotics on microplastics.

PubMed

Li, Jia; Zhang, Kaina; Zhang, Hua

2018-06-01

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

Development of in-Situ Al-Si/CuAl2 Metal Matrix Composites: Microstructure, Hardness, and Wear Behavior

PubMed Central

Tash, Mahmoud M.; Mahmoud, Essam R. I.

2016-01-01

In the present work, in-situ metal matrix composites were fabricated through squeeze casting. The copper particles were dispersed with different weight percentages (3%, 6%, 10%, and 15%) into Al-12% Si piston alloy. Also, heat treatments were performed at 380 °C and 450 °C for holding times of 6 and 18 h. The microstructures, X-ray diffractometer (XRD) pattern, hardness, and wear characteristics were evaluated. The results showed that these copper particles have reacted with the aluminum under all of the aforementioned processing conditions resulting in the formation of fine copper aluminide intermetallics. Most of the intermetallics were CuAl2, while AlCu appeared in a small ratio. Additionally, these intermetallics were homogenously distributed within the alloy matrix with up to 6% Cu addition. The amounts of those intermetallics increased after performing heat treatment. Most of these intermetallics were CuAl2 at 380 °C, while the Cu-rich intermetallics appeared at 450 °C. Increasing the holding time to 18 h, however, led to grain coarsening and resulted in the formation of some cracks. The hardness of the resulting composite materials was improved. The hardness value reached to about 170 HV after heat treating at 380 °C for 8 h. The wear resistance of the resulting composite materials was remarkably improved, especially at lower additions of Cu and at the lower heat treatment temperature. PMID:28773564

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

PubMed

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

2017-02-01

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

Microstructural inhomogeneity in plasma-sprayed hydroxyapatite coatings and effect of post-heat treatment

NASA Astrophysics Data System (ADS)

Lu, Yu-Peng; Xiao, Gui-Yong; Li, Shi-Tong; Sun, Rui-Xue; Li, Mu-Sen

2006-01-01

The microstructural inhomogeneity in the plasma-sprayed hydroxyapatite (HA) coatings was characterized by using electron probe microanalyser (EPMA). A simple and artful method was developed to detect the interface characteristics. All the samples for observation were ground and polished along the direction parallel to the coating surfaces. The BSE images directly and clearly showed the inhomogeneity in the as-sprayed coatings with the amorphous regions being bright gray and crystalline regions being dark gray. X-ray diffractometer (XRD) patterns indicated that after immersion in deionized water for 20 days, bone-like apatite and α-Ca 2P 2O 7 precipitated on the polished surfaces of the as-sprayed HA coatings. The post-heat treatment could eliminate the microstructural inhomogeneity in the coatings. Only β-Ca 2P 2O 7 precipitated on the surfaces of the heat-treated HA coatings. The immersed samples were re-polished till tiny substrate was bared to investigate the effect of immersion on interface. It was shown that the immersion decreased the cohesive strength of the as-sprayed coatings. There were more and broader cracks in the splats that came into contact with the substrate and amorphous phase increased toward the coating-substrate interface. Post-heat treatment was proved to reduce the peeling off of coating during re-polishing operation. It was proposed that the distributions of amorphous phase and cracks in as-sprayed coatings are detrimental to coating properties and should be modified through improving the plasma spraying processing.

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

NASA Astrophysics Data System (ADS)

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

2017-08-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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