Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Kavitha, V. T.; Wariar, P. R. S.

2018-05-01

Nanocrystalline pyrochlore material Dysprosium Titanate (Dy2Ti2O7) has been synthesized through a single step optimized combustion route. The phase purity and phase formation of the combustion product has been characterized using X-Ray diffraction analysis (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. X-Ray diffraction analysis (XRD) reveal that Dy2Ti2O7 is highly crystalline in nature with cubic structure in the Fd3m space group. The microstructures and average particle size of the prepared nanopowder were examined by High Resolution Transmission Electron Microscopy (HR-TEM). The optical band gap of the Dy2Ti2O7 nanoparticles is determined from the absorption spectrum, was attributed to direct allowed transitions through optical band gap of 3.98 eV. The frequency dependent dielectric measurements have been carried out on the sintered pellet in the frequency range 1 Hz-10 MHz. The measured value of dielectric constant (ℇ') was ˜ 43 and loss tangent (tan δ) was 4×10-3 at 1 MHz, at room temperature.

Luminescence study of ZnSe/PVA (polyvinyl alcohol) composite film

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

Lahariya, Vikas

The ZnSe nanocrystals have been prepared into poly vinyl alcohol(PVA) polymer matrix on glass using ZnCl2 and Na2SeSO3 as zinc and selenium source respectively. Poly vinyl Alcohol (PVA) used as polymer matrix cum capping agent due to their high viscosity and water solubility. It is transparent for visible region and prevents Se- ions to photo oxidation. The ZnSe/PVA composite film was deposited on glass substrate. The film was characterized by X Ray Diffraction (XRD) and UV-Visible absorption Spectroscopy and Photoluminescence. The X Ray Diffraction (XRD) study confirms the nanometer size (10 nm) particle formation within PVA matrix with cubic zinc blendmore » crystal structure. The UV-Visible Absorption spectrum of ZnSe/PVA composite film shown blue shift in absorption edge indicating increased band gap due to quantum confinement. The calculated energy band gap from the absorption edge using Tauc relation is 3.4 eV. From the Photoluminescence study a broad peak at 435 nm has been observed in violet blue region due to recombination of surface states.« less

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

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

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

2016-03-25

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

Williamson-Hall analysis and optical properties of small sized ZnO nanocrystals

NASA Astrophysics Data System (ADS)

Kalita, Amarjyoti; Kalita, Manos P. C.

2017-08-01

We apply Williamson-Hall (WH) method of X-ray diffraction (XRD) line profile analysis for lattice strain estimation of small sized ZnO nanocrystals (crystallite size≈4 nm). The ZnO nanocrystals are synthesized by room temperature chemical co-precipitation followed by heating at 40 °C. Zinc acetate, sodium hydroxide and 2-mercaptoethanol (ME) are used for the synthesis of the nanocrystals. {100}, {002}, {101} and {200}, {112}, {201} line profiles in the XRD pattern are significantly merged, therefore determination of the full width at half maximum values and peak positions of the line profiles required for WH analysis has been carried out by executing Rietveld refinement of the XRD pattern. Lattice strain of the 4 nm sized ZnO nanocrystals is found to be 5.8×10-3 which is significantly higher as compared to the literature reported values for larger ones (crystallite size≈17-47 nm). Role of ME as capping agent is confirmed by Fourier transform infrared spectroscopy. The band gap of the nanocrystals is determined from the UV-Visible absorption spectrum and is found to be 3.68 eV. The photoluminescence spectrum exhibits emissions in the visible (408 nm-violet, 467 nm-blue and 538 nm-green) regions showing presence of zinc interstitial and oxygen vacancy in the ZnO nanocrystals.

Properties of thin silver films with different thickness

NASA Astrophysics Data System (ADS)

Zhao, Pei; Su, Weitao; Wang, Reng; Xu, Xiaofeng; Zhang, Fengshan

2009-01-01

In order to investigate optical properties of silver films with different film thickness, multilayer composed of thin silver film sandwiched between ZnS films are sputtered on the float glass. The crystal structures, optical and electrical properties of films are characterized by various techniques, such as X-ray diffraction (XRD), spectrum analysis, etc. The optical constants of thin silver film are calculated by fitting the transmittance ( T) and reflectance ( R) spectrum of the multilayer. Electrical and optical properties of silver films thinner than 6.2 nm exhibit sharp change. However, variation becomes slow as film thickness is larger than 6.2 nm. The experimental results indicate that 6.2 nm is the optimum thickness for properties of silver.

Lignin-based Biochar/graphene Oxide Composites as Supercapacitor Electrode Materials

NASA Astrophysics Data System (ADS)

Cai, Z.; Jiang, C.; Xiao, X. F.; Zhang, Y. S.; Liang, L.

2018-05-01

The lignin-based biochar/graphene composites were effectively obtained via an easy and rapid co-precipitation method. The chemical structure, microstructure, electrochemical properties of lignin/graphene oxide composites before and after carbonization were investigated by Fourier transformation infrared spectrum (FTIR), Scanning electron microscope (SEM), x-ray diffraction (XRD) and cyclic voltammetry (CV). FTIR results confirmed that the oxygen-containing groups of lignin, GO and their composites were partly removed after 800 °C carbonization and GO had a positive impact on the formation of graphitic structure for lignin. XRD results showed that lignin could completely block the restacking of GO sheets. The electrochemical test presented that lignin/graphene oxide composites exhibited a typical CV curve and the specific capacitance reached ∼103F/g at a scan rate of 20mv/s.

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

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

2015-01-01

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

The functionalization and characterization of multi-walled carbon nanotubes (MWCNTs)

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

Abdullah, Mohd Pauzi; Center of Water Analysis and Research; Zulkepli, Siti Aminah

2015-09-25

Functionalization is the process of introducing chemical functional groups on the surface of the material. In this study, a multi-walled carbon nanotube (MWCNTs) was functionalized by oxidation treatment using concentrated nitric acid. The functionalized and pristine MWCNTs were analyzed by using Fourier Transform Infrared Spectroscopy (FT-IR) and X-Ray Diffraction (XRD). The XRD patterns exhibit the graphitic properties for all samples. Besides, the XRD results also demonstrate that the percent of crystallinity of MWCNTs increases as the duration of acid treatment increases. The percent of crystallinity increases from 66% to 80% when the pristine MWCNT treated for 12 hours with additionalmore » 12 hours reflux process with nitric acid. The IR spectrum for the 12 hours-treated MWCNTs shows the formation of carboxyl functional group. Additional 12 hours reflux process with nitric acid on the 12 hours-treated MWCNTs have shown the loss of existing carboxyl group and only hydroxyl group formed.« less

Spectroscopic investigations on oxidized multi-walled carbon nanotubes

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

Anandhi, C. M. S.; Premkumar, S.; Asath, R. Mohamed

2016-05-06

The pristine multi-walled carbon nanotubes (MWCNTs) were oxidized by the ultrasonication process. The oxidized MWCNTs were characterized by the X-ray diffraction (XRD), ultraviolet–visible (UV-Vis) and Fourier transform -Raman (FT-Raman) spectroscopic techniques. The XRD analysis confirms that the oxidized MWCNTs exist in a hexagonal structure and the sharp XRD peak corresponds to the (002) Bragg’s reflection plane, which indicates that the MWCNTs have higher crystalline nature. The UV-Vis analysis confirms that the MWCNTs functionalized with the carboxylic acid. The red shift was observed corresponds to the D band in the Raman spectrum, which reveals that the reduced disordered graphitic structure ofmore » oxidized MWCNTs. The strong Raman peak was observed at 2563 cm{sup -1} corresponds to the overtone of the D band, which is the characteristic vibrational mode of oxidized MWCNTs. The carboxylic acid functionalization of MWCNTs enhances the dispersibility, which paves the way for potential applications in the field of biosensors and targeted drug delivery.« less

Extracellular synthesis of silver nanoparticles using the leaf extract of Coleus amboinicus Lour

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

Narayanan, Kannan Badri; Sakthivel, Natarajan, E-mail: puns2005@gmail.com

2011-10-15

Highlights: {yields} Synthesis of AgNPs using the leaf extract of Coleus amboinicus L. was described. {yields} UV-vis absorption spectra showed the formation of isotrophic AgNPs at 437 nm in 6 h. {yields} XRD analysis showed intense peaks corresponding to fcc structure of AgNPs. {yields} HR-TEM analysis revealed the formation of stable anisotrophic and isotrophic AgNPs. -- Abstract: In the present investigation, Coleus amboinicus Lour. leaf extract-mediated green chemistry approach for the synthesis of silver nanoparticles was described. The nanoparticles were characterized by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and transmissionmore » electron microscopy (TEM). The influence of leaf extract on the control of size and shape of silver nanoparticles is reported. Upon an increase in the concentration of leaf extract, there was a shift in the shape of nanoparticles from anisotrophic nanostructures like triangle, decahedral and hexagonal to isotrophic spherical nanoparticles. Crystalline nature of fcc structured nanoparticles was confirmed by XRD spectrum with peaks corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes and bright circular spots in the selected-area electron diffraction (SAED). Such environment friendly and sustainable methods are non-toxic, cheap and alternative to hazardous chemical procedures.« less

Synthesis and photosensor study of as-grown CuZnO thin film by facile chemical bath deposition

NASA Astrophysics Data System (ADS)

Gubari, Ghamdan M. M.; Ibrahim Mohammed S., M.; Huse, Nanasaheb P.; Dive, Avinash S.; Sharma, Ramphal

2018-05-01

We have successfully deposited CuZnO thin film on a glass substrate by facile chemical bath deposition method at 85 °C for 1 hr. Structural, topographical, Optical and Electrical properties of the prepared Thin Films were investigated by XRD, Raman spectrum, AFM, UV-Visible Spectrophotometer and I-V Measurement System respectively. The X-ray diffraction (XRD) pattern confirmed the formation of the CuZnO composition when compared with standard JCPDS card (JCPDF # 75-0576 & # 36-1451). The Raman analysis shows a major peak at 458 cm-1 with E2 (High) vibrational mode. AFM images revealed uniform deposition over an entire glass substrate with 66.2 nm average roughness of the film. From the optical absorption spectrum, clear band edge around ˜407 nm was observed which results in a wide energy band gap of ˜3.04 eV. The electrical properties were measured at room temperature in the voltage range ±5 V, showed a drastic enhancement in current under light illumination with the highest photosensitivity of ˜99.9 % for 260 W.

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...

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

Crystalline perfection, optical and piezoelectric properties of a novel semi-organic single crystal: Zinc guanidinium sulphate

NASA Astrophysics Data System (ADS)

Nandhini, S.; Murugakoothan, P.

2018-04-01

Zinc Guanidinium Sulfate (ZGuS), a semi-organic single crystal, was synthesized using slow evaporation solution growth technique. It is a non-centrosymmetric crystal with space group I4 ¯2d . The crystalline nature of the crystal and the strain were determined using powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was revealed using HR-XRD analysis. The UV-vis-NIR transmittance spectrum depicts 60% transparency with lower-cut off wavelength of 210 nm. The emission spectrum of the crystal was determined using photoluminescence study. Piezoelectricity was confirmed by determining the piezoelectric charge coefficient (d33). These findings shows that the title compound can be employed for photonic and transducer applications.

Effect of PbO on optical properties of tellurite glass

NASA Astrophysics Data System (ADS)

Elazoumi, S. H.; Sidek, H. A. A.; Rammah, Y. S.; El-Mallawany, R.; Halimah, M. K.; Matori, K. A.; Zaid, M. H. M.

2018-03-01

Binary (1 - x)(TeO2) - x(PbO), x = 0, 0.10, 0.15, 0.20, 0.25, 0.30 mol% glass system was fabricated using melt quenching method. X-ray diffraction (XRD) technique was employed to confirm the amorphous nature. The microanalysis of the major components was performed using energy dispersive EDX and X-ray spectrometry. Both the molar volume and the density were measured. FTIR and UV spectra were recorded at 400-4000 cm-1 and 220-800 nm, respectively. The optical band gap (Eopt), Urbach's energy (Eu), index of refraction (n) were calculated using absorption spectrum fitting (ASF) and derivation of absorption spectrum fitting (DASF) methods. Molar refraction Rm and molecular polarizability αm have been calculated according to (ASF) method.

[A new method for the preparation of potassium ferrate and spectroscopic characterization].

PubMed

Zheng, Huai-li; Deng, Lin-li; Ji, Fang-ying; Jiang, Shao-jie; Zhang, Peng

2010-10-01

Calcium hypochlorite was used as the raw material for preparation of the high purity potassium ferrate. The study includes the effects of reaction temperature, recrystallization temperature, reaction time, Ca(ClO)2 dosage, and the amount of calcium hypochlorite on the yield. It was determined that when the reaction temperature was 25 degrees C, recrystallization temperature 0 degree C and reaction time 40 min, the yield was more than 75%. The purity was detected by direct spectrophotometric method to be more than 92%. The product was characterized by infrated spectrum(IR), X-ray diffraction (XRD) and ultraviolet spectrum (UV) methods and proved to be potassium ferrate that was prepared by calcium hypochlorite as the raw material.

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.

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

Mechanical and tribological property of single layer graphene oxide reinforced titanium matrix composite coating

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Li, Yue; Fan, Xueliang; Chen, Feng; Xu, Jiale

2018-04-01

Single layer grapheme oxide Nano sheets and Nano titanium powder were dispersed in deionized water by ultrasonic dispersion. Then the mixed solution was pre-coating on AISI4140 substrate. Using laser sintering process to fabricated grapheme oxide and Ti composite coating. Microstructures and composition of the composite coating was studied by Scanning Electron Microscopy (SEM), x-ray diffract meter (XRD) and Raman spectroscopy. Raman spectrum, XRD pattern and SEM results proved that grapheme oxide sheets were dispersed in the composite coating. The composite coating had much higher average Vickers hardness values than that of pure Ti coating. The tribological performance of the composite coatings became better while the suitable GO content was selected. For the 2.5wt. % GO content coating, the friction coefficient was reduced to near 0.1.

Photoluminescence study of ZnS and ZnS:Pb nanoparticles

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

Virpal,, E-mail: virpalsharma.sharma@gmail.com; Hastir, Anita; Kaur, Jasmeet

2015-05-15

Photoluminescence (PL) study of pure and 5wt. % lead doped ZnS prepared by co-precipitation method was conducted at room temperature. The prepared nanoparticles were characterized by X-ray Diffraction (XRD), UV-Visible (UV-Vis) spectrophotometer, Photoluminescence (PL) and Raman spectroscopy. XRD patterns confirm cubic structure of ZnS and PbS in doped sample. The band gap energy value increased in case of Pb doped ZnS nanoparticles. The PL spectrum of pure ZnS was de-convoluted into two peaks centered at 399nm and 441nm which were attributed to defect states of ZnS. In doped sample, a shoulder peak at 389nm and a broad peak centered atmore » 505nm were observed. This broad green emission peak originated due to Pb activated ZnS states.« less

Extracellular synthesis of mycogenic silver nanoparticles by Cylindrocladium floridanum and its homogeneous catalytic degradation of 4-nitrophenol.

PubMed

Narayanan, Kannan Badri; Park, Hyun Ho; Sakthivel, Natarajan

2013-12-01

Green synthesis of extracellular mycogenic silver nanoparticles using the fungus, Cylindrocladium floridanum is reported. The synthesized mycogenic silver nanoparticles were characterized using UV-Vis absorption spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) techniques. The nanoparticles exhibit fcc structure with Bragg's reflections of (111), (200), (220) and (311) was evidenced by XRD pattern, high-resolution TEM lattice fringes and circular rings in selected-area electron diffraction (SAED) pattern. The morphology of nanoparticles was roughly spherical in shape with an average size of ca. 25 nm. From FTIR spectrum, it was found that the biomolecules with amide I and II band were involved in the stabilization of nanoparticles. These mycogenic silver nanoparticles exhibited the homogeneous catalytic potential in the reduction of pollutant, 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) using sodium borohydride, which followed a pseudo-first-order kinetic model. Thus, the synthesis of metal nanoparticles using sustainable microbial approach opens up possibilities in the usage of mycogenic metal nanoparticles as catalysts in various chemical reactions. Copyright © 2013 Elsevier B.V. All rights reserved.

Poly (N-ethyl aniline)/Ag Nanocomposite as Humidity Sensor

NASA Astrophysics Data System (ADS)

Pande, Nishigandh S.; Jaspal, Dipika; Ambekar, Jalindar

Poly (N-ethyl aniline)/Ag organic-inorganic composite has been synthesized by a single step in situ chemical oxidative polymerization method. The synthesis of Poly (N-ethyl aniline)/Ag nanocomposite has been confirmed by X-ray diffraction (XRD), Ultraviolet-Vis Spectroscopy (UV-visible), Fourier transform infrared analysis (FTIR) and FE-SEM investigations. XRD spectral study exhibited major diffraction in the range 20-80∘ (2θ) and indicated the semicrystalline nature of poly (N-ethyl aniline)/Ag nanocomposite. Characteristic peaks in UV-visible and FTIR spectra of poly (N-ethyl aniline) switched to higher wave numbers in poly (N-ethyl aniline)/Ag nanocomposite. Peaks at 1789cm-1, 1595cm-1, 667cm-1 and 501cm-1 in FTIR spectrum confirmed the formation of poly (N-ethyl aniline)/Ag nanocomposite. FE-SEM photographs reported agglomerated granular particulate nature of poly (N-ethyl aniline)/Ag nanocomposite. Synthesized poly (N-ethyl aniline)/Ag nanocomposite exhibited a high response to humidity, good reproducibility and stability at room temperature. An appreciable response was shown in the presence of 40% humid atmosphere for up to successive four cycles. Composite sensitivity has been found to increase with the increasing concentration of humidity, at room temperature.

Synthesis, crystal growth, optical, thermal, and mechanical properties of a nonlinear optical single crystal: ammonium sulfate hydrogen sulphamate (ASHS)

NASA Astrophysics Data System (ADS)

Sudhakar, K.; Nandhini, S.; Muniyappan, S.; Arumanayagam, T.; Vivek, P.; Murugakoothan, P.

2018-04-01

Ammonium sulfate hydrogen sulphamate (ASHS), an inorganic nonlinear optical crystal, was grown from the aqueous solution by slow evaporation solution growth technique. The single-crystal XRD confirms that the grown single crystal belongs to the orthorhombic system with the space group of Pna21. Powder XRD confirms the crystalline nature and the diffraction planes were indexed. Crystalline perfection of grown crystal was analysed by high-resolution X-ray diffraction rocking curve technique. UV-Vis-NIR studies revealed that ASHS crystal has optical transparency 65% and lower cut-off wavelength at 218 nm. The violet light emission of the crystal was identified by photoluminescence studies. The particle size-dependent second-harmonic generation efficiency for ASHS crystal was evaluated by Kurtz-Perry powder technique using Nd:YAG laser which established the existence of phase matching. Surface laser damage threshold value was evaluated using Nd:YAG laser. Optical homogeneity of the crystal was evaluated using modified channel spectrum method through birefringence study. Thermal analysis reveals that ASHS crystal is stable up to 213 °C. The mechanical behaviour of the ASHS crystal was analysed using Vickers microhardness study.

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

Simulation study of an X-ray diffraction system for breast tumor detection

NASA Astrophysics Data System (ADS)

Marticke, F.; Montémont, G.; Paulus, C.; Michel, O.; Mars, J. I.; Verger, L.

2017-09-01

X-ray diffraction (XRD) is a powerful technique used to determine the molecular structure of biological tissues. In breast tissues for example, the scattering signatures of dense fibroglandular tissue and carcinoma have been shown to be significantly different. In this study, XRD was used as a second control level when conventional mammography results were unclear, for instance because of overly high breast density. A system optimized for this issue, called multifocal XRD, was developed combining energy dispersive spectral information at different scattering angles. This system allows depth-imaging in one go but needs an x,y-direction scan to image the region conventional mammography identified as suspect. The scan-time for about 10 cm3 with an incident flux of about 4 . 8 ṡ 107 photons per second would be around 2 s. For this study, breast phantoms with and without cancerous nodule were simulated to assess the separation power of the method and to determine the radiation dose required to obtain nearly ideal separation. For tumors situated in the center of the breast, the required dose was only about 0.3 mGy, even for breasts with high density. The tumor position was shown to have a low impact on detectability provided it remained in a zone where the system was sufficiently sensitive. The influence of incident spectrum maximum energy was also studied. The required dose remained very low with any of the incident spectra tested. Finally, an image slice was reconstructed in the x-direction and showed that the system can detect the presence of a small tumor (4 mm). Hence, XRD is a very promising tool to reduce the number of unnecessary invasive breast biopsies.

Periodic Density Functional Theory Study of the Structure, Raman Spectrum, and Mechanical Properties of Schoepite Mineral.

PubMed

Colmenero, Francisco; Cobos, Joaquín; Timón, Vicente

2018-04-16

The structure and Raman spectrum of schoepite mineral, [(UO 2 ) 8 O 2 (OH) 12 ]·12H 2 O, was studied by means of theoretical calculations. The computations were carried out by using density functional theory with plane waves and pseudopotentials. A norm-conserving pseudopotential specific for the U atom developed in a previous work was employed. Because it was not possible to locate H atoms directly from X-ray diffraction (XRD) data by structure refinement in previous experimental studies, all of the positions of the H atoms in the full unit cell were determined theoretically. The structural results, including the lattice parameters, bond lengths, bond angles, and powder XRD pattern, were found to be in good agreement with their experimental counterparts. However, the calculations performed using the unit cell designed by Ostanin and Zeller in 2007, involving half of the atoms of the full unit cell, led to significant errors in the computed powder XRD pattern. Furthermore, Ostanin and Zeller's unit cell contains hydronium ions, H 3 O + , which are incompatible with the experimental information. Therefore, while the use of this schoepite model may be a very useful approximation requiring a much smaller amount of computational effort, the full unit cell should be used to study this mineral accurately. The Raman spectrum was also computed by means of density functional perturbation theory and compared with the experimental spectrum. The results were also in agreement with the experimental data. A normal-mode analysis of the theoretical spectra was performed to assign the main bands of the Raman spectrum. This assignment significantly improved the current empirical assignment of the bands of the Raman spectrum of schoepite mineral. In addition, the equation of state and elastic properties of this mineral were determined. The crystal structure of schoepite was found to be stable mechanically and dynamically. Schoepite can be described as a brittle material exhibiting small anisotropy and large compressibility in the direction perpendicular to the layers, which characterize its structure. The calculated bulk modulus, B, was ∼35 GPa.

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

Effects on structural, optical, and magnetic properties of pure and Sr-substituted MgFe2O4 nanoparticles at different calcination temperatures

NASA Astrophysics Data System (ADS)

Loganathan, A.; Kumar, K.

2016-06-01

In the present work, pure and Sr2+ ions substituted Mg ferrite nanoparticles (NPs) had been prepared by co-precipitation method and their structural, optical, and magnetic properties at different calcination temperatures were studied. On this purpose, thermo gravimetric and differential thermal analysis (TG-DTA), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy, UV-Visible diffused reflectance spectroscopy, impedance spectroscopy, and vibrating sample magnetometer were carried out. The exo- and endothermic processes of synthesized precursors were investigated by TG-DTA measurements. The structural properties of the obtained products were examined by XRD analysis and show that the synthesized NPs are in the cubic spinel structure. The existence of two bands around 578-583 and 430-436 cm-1 in FT-IR spectrum also confirmed the formation of spinel-structured ferrite NPs. The lattice constants and particle size are estimated using XRD data and found to be strongly dependent on calcination temperatures. The optical, electrical, and magnetic properties of ferrite compositions also investigated and found to be strongly dependant on calcination temperatures.

[Raman spectrum of nano-graphite synthesized by explosive detonation].

PubMed

Wen, Chao; Li, Xun; Sun, De-Yu; Guan, Jin-Qing; Liu, Xiao-Xin; Lin, Ying-Rui; Tang, Shi-Ying; Zhou, Gang; Lin, Jun-De; Jin, Zhi-Hao

2005-01-01

The nano-graphite powder synthesized by the detonation of explosives with negative oxygen balance is a new powder material with potential applications. In this work, the preparation of nano-graphite powder in steel chamber by pure TNT (trinitrotoluene) explosives has been introduced. In the synthesis process, the protective gases in the steel chamber are N2, CO2 and Ar, and the pressure is 0.25-2 atm. Raman spectrum of the nano-graphite was measured. The characteristic Raman band assigned to sp2 of graphite has been observed at about 1 585 cm(-1) with half-peak width of 22 cm(-1). The peak shifted to a higher frequency by 5 cm(-1) compared with that of bulk graphite. The authors explain this blue shift phenomenon by size effect. The average size of nanographite from Raman measurement is 2.97-3.97 nm. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to measure the structure and particle size of the nano-graphite. The crystallite size of nano-graphite estimated from XRD andTEM are 2.58 nm (acid untreated) and 1.86 nm (acid treated) respectively, which is in accord with the results of the measurement approximately.

Role of Mn2+ concentration in the linear and nonlinear optical properties of Ni1-xMnxSe nanoparticles

NASA Astrophysics Data System (ADS)

Anugop, B.; Prasanth, S.; Rithesh Raj, D.; Vineeshkumar, T. V.; Pranitha, S.; Mahadevan Pillai, V. P.; Sudarsanakumar, C.

2016-12-01

Ni1-xMnxSe nanoparticles (x = 0.1, 0.3, 0.5, 0.7, 0.9) were successfully synthesized by chemical co-precipitation method and their structural and optical properties were studied using X-ray diffraction, transmission electron microscopy, UV-Visible absorption and photo luminescence spectroscopy. XRD pattern reveals the hexagonal structure of the particles and the peak positions were shifted to higher 2θ values with increase in Mn2+ concentration. The average particle size determined from XRD varies from 6 to 11 nm. The UV-Visible absorption spectrum shows absorption edge around the blue region and is red-shifted with increasing Mn2+ concentration consequently the optical bandgap energy is decreasing. The PL emission spectrum shows a broad emission around 380 nm, and the intensity of the emission decreases with increase in Mn2+ concentration. The nonlinear optical properties of the samples were analysed using Z-scan technique and the samples show optical limiting behaviour and the 2 PA coefficient increases with increasing Mn2+ concentration. Overall, manganese concentration influences the linear and nonlinear optical properties of Ni1-xMnxSe nanoparticles.

A High Sensitivity Isopropanol Vapor Sensor Based on Cr₂O₃-SnO₂ Heterojunction Nanocomposites via Chemical Precipitation Route.

PubMed

Jawaher, K Rackesh; Indirajith, R; Krishnan, S; Robert, R; Pasha, S K Khadheer; Deshmukh, Kalim; Sastikumar, D; Das, S Jerome

2018-08-01

Cr2O3-SnO2 heterojunction nanocomposites were prepared via chemical precipitation method. The prepared samples were characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectra and Field Emission Electron Microscopy (FESEM). The XRD spectrum confirms the presence of both tetragonal rutile SnO2 and rhombohedral corundum Cr2O3 structure. Further investigation into the gas sensing performances of the prepared Cr2O3-SnO2 nanocomposites exhibited an enhanced sensitivity towards VOPs such as isopropanol, acetone, ethanol and formaldehyde. Especially, isopropanol vapor sensor shows excellent sensitivity at an operating temperature of 100 °C. The highest sensitivity for Cr2O3-SnO2 heterojunction nanocomposites indicate that these materials can be a good candidate for the production of high-performance isopropanol sensors.

Banana peel reductant for leaching medium grade manganese ore in sulfuric acid solution

NASA Astrophysics Data System (ADS)

Aripin, H.; Joni, I. Made; Busaeri, Nundang; Usrah, Ifkar; Sudiana, I. Nyoman; Sabchevski, Svilen

2017-03-01

In this investigation, manganese has been produced from medium grade manganese ore from Karangnunggal mine (West Java, Indonesia). The effects of weighed amount of banana peels on the structural and leaching properties have been studied. The material's properties have been characterized on the basis of the experimental data obtained using X-ray fluorescence (XRF), X-ray diffraction (XRD), and Fourier transforms infrared (FTIR) spectroscopy. It has been found that an increase of the weighed amount of banana peels up to 4 g leads to an increase of the leaching efficiency of manganese from manganese ore. Above 4 g, however, the leaching efficiency does not change significantly. The analysis based on the interpretation of both XRD patterns and FTIR spectrum allows one to explain the increase in the leaching efficiencies of manganese by the reduction of MnO2 minerals and by the removal of hemicelluloses groups of banana peel in the samples.

Investigation of tin oxide nanofibers synthesized via bio-template technique

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

Kundu, Virender Singh, E-mail: vskundu-kuk@rediffmail.com; Dhiman, Jonny; Kumar, Suresh

In the present paper tin oxide nanofibers have been by synthesized using cotton as bio-template via sol-gel route. This is comparatively a new synthesis technique. The structure and morphology of the obtained SnO{sub 2} nanofibers were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDX). The optical properties of the same have been studied by using UV-Vis spectroscopy. The observed XRD pattern showed that peaks are very narrow and sharp which indicates crystalline nature of samples. SEM images gave an idea about the sample morphology and confirm that the obtained sample were nanofibers. The optical absorbancemore » spectrum of the sample under study was recorded in UV-visible region (200nm- 800nm). The band gap of the sample was found to be 3.95 eV which is higher than their bulk counterpart.« less

Characterization of the Phase Composition of Nanosized Lithium Titanates Synthesized by Inductive Thermal Plasma

NASA Astrophysics Data System (ADS)

Quesnel, François; Soucy, Gervais; Veilleux, Jocelyn; Hovington, Pierre; Zhu, Wen; Zaghib, Karim

The properties of lithium titanates anodes in Li-ion batteries are highly dependent on their secondary constituents. While their main phase is usually constituted of Li4Ti5O12, significant quantity of lithium titanates compounds of various stoichiometry are often present, due to either the processing, usage or aging of the material. These may go underreported, as many of these spectrums overlap or display low signal in X-ray diffraction (XRD). Samples of nanosized lithium titanates synthetized by inductive plasma were characterized by XRD and scanning electron microscopy (SEM), as they provide a regular yet typical crystallite size and shape including multiple phases. A Rietveld refinement was developed to extract the composition of these samples. Mass balance through further annealing and differential scanning calorimetry (DSC) enthalpy measurements from phase transformations were also used as identification and validation techniques.

Photoluminescence Properties of Ca3Si2O7: Pr3+ Orange-Red Phosphors Prepared by High-Temperature Solid-State Method

NASA Astrophysics Data System (ADS)

Peng, Zhi-Qing; Chen, Rong; Feng, Wen-Lin

2018-06-01

Novel luminescent materials Ca3-xSi2O7: xPr3+ were successfully prepared by the high-temperature solid-state method. The crystal structure, morphology, and optical spectrum were characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), and spectroscopy, respectively. The XRD patterns of the samples indicate that the crystal structure is monoclinic symmetry. The SEM shows that the selected sample has good crystallinity although its appearance is irregular and scalelike. The peak of the excitation spectrum of the sample is located at around 449 nm, corresponding to 3H4→3P2 transition of Pr3+. The peak of the emission spectrum of the sample is situated at around 612 nm which is attributed to 3P0→3H6 transition of Pr3+, and the colour is orange-red. The optimum concentration for Pr3+ replaced Ca2+ sites in Ca3Si2O7: Pr3+ is 0.75 mol%. The lifetime (8.48 μs) of a typical sample (Ca2.9925Pr0.0075)Si2O7 is obtained. It reveals that orange-red phosphors Ca3-xSi2O7: xPr3+ possess remarkable optical properties and can be used in white light emitting devices.

Green synthesis of gold nanoparticles using Citrus maxima peel extract and their catalytic/antibacterial activities.

PubMed

Yuan, Chun-Gang; Huo, Can; Gui, Bing; Cao, Wei-Ping

2017-08-01

The peel of Citrus maxima ( C. maxima ) is the primary byproducts during the process of fruit or juice in food industries, and it was always considered as biomass waste for further treatments. In this study, the authors reported a simple and eco-friendly method to synthesise gold nanoparticles (AuNPs) using C. maxima peel extract as reducing and capping agents. The synthesised AuNPs were characterised by UV-visible spectrum, X-ray diffraction (XRD), transmission electron microscope (TEM) and Fourier-transform infrared spectroscopy (FTIR). The UV-visible spectrum of the AuNPs colloid showed a characteristic peak at 540 nm. The peaks of XRD analysis at (2 θ ) 38.30°, 44.28°, 64.62°, 77.57° and 81.75° were assigned to (111), (200), (220), (311) and (222) planes of the face-centered cubic (fcc) lattice of gold. The TEM images showed that AuNPs were nearly spherical in shape with the size of 8-25 nm. The FTIR spectrum revealed that some bioactive compounds capped the surface of synthesised AuNPs. The biosynthesised AuNPs performed strong catalytic activity in degradation of 4-nitrophenol to 4-aminophenol and good antibacterial activity against both gram negative ( Escherichia coli ) and gram positive ( Staphylococcus aureus ) bacterium. The synthesis procedure was proved simple, cost effective and environment friendly.

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.

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.;

Diamonds in detonation soot

NASA Technical Reports Server (NTRS)

Greiner, N. Roy; Phillips, Dave; Johnson, J. D.; Volk, Fred

1990-01-01

Diamonds 4 to 7 nm in diameter have been identified and partially isolated from soot formed in detonations of carbon-forming composite explosives. The morphology of the soot has been examined by transmission electron microscopy (TEM), and the identity of the diamond has been established by the electron diffraction pattern of the TEM samples and by the X-ray diffraction (XRD) pattern of the isolated solid. Graphite is also present in the form of ribbons of turbostatic structure with a thickness of 2 to 4 nm. A fraction, about 25 percent of the soot by weight, was recovered from the crude soot after oxidation of the graphite with fuming perchloric acid. This fraction showed a distinct XRD pattern of diamond and the diffuse band of amorphous carbon. The IR spectrum of these diamonds closely matches that of diamonds recovered from meteorites (Lewis et al., 1987), perhaps indicating similar surface properties after the oxidation. If these diamonds are produced in the detonation itself or during the initial expansion, they exhibit a phenomenal crystal growth rate (5 nm/0.00001 s equal 1.8 m/hr) in a medium with a very low hydrogen/carbon ratio. Because the diamonds will be carried along with the expanding gases, they will be accelerated to velocities approaching 8 km/s.

Rapid green synthesis of spherical gold nanoparticles using Mangifera indica leaf

NASA Astrophysics Data System (ADS)

Philip, Daizy

2010-11-01

This paper reports the rapid biological synthesis of spherical gold nanoparticles at room temperature using fresh/dry leaf extract of Mangifera indica. This is a simple, cost-effective, stable for long time and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au nanoparticles of size ˜20 nm and 17 nm. The nanoparticles were obtained within 2 min of addition of the extract to the solution of HAuCl 4·3H 2O and the colloid is found to be stable for more than 5 months. Smaller and more uniformly distributed particles could be obtained with dried leaf extract. The nanoparticles obtained are characterized by UV-vis, transmission electron microscopy (TEM) and X-ray diffraction (XRD). Crystalline nature of the nanoparticles in the fcc structure is confirmed by the peaks in the XRD pattern corresponding to (1 1 1), (2 0 0), (2 2 0), (3 1 1) and (2 2 2) planes, bright circular spots in the selected area electron diffraction (SAED) and clear lattice fringes in the high-resolution TEM image. The possible biomolecules responsible for efficient stabilization are suggested by studying the FTIR spectrum of the sample. This environmentally benign method provides much faster synthesis and colloidal stability comparable to those of chemical reduction.

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.

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.

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.

Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

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

Cummins, Dustin Ray; Vogel, Sven C.; Hollis, Kendall Jon

2016-10-18

This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffractionmore » data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to the process and analysis can be made, and neutron diffraction can become a viable and efficient technique for gamma/alpha phase composition determination for nuclear fuels.« less

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.

Studies on Optical and Electrical Properties of Hafnium Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Jayaraman, Venkatachalam; Sagadevan, Suresh; Sudhakar, Rajesh

2017-07-01

In this paper, the synthesis and physico-chemical properties of hafnium oxide nanoparticles (HfO2 NPs) are analyzed and reported. The synthesis was carried out by the precipitation route by using hafnium tetrachloride (HfCl4) as precursor material with potassium hydroxide (KOH) dissolved in Millipore water. In the precipitation technique, the chemical reaction is comparatively simple, low-cost and non-toxic compared to other synthetic methods. The synthesized HfO2 NPs were characterized by using powder x-ray diffraction (PXRD), ultraviolet-visible (UV-Vis) spectroscopy, Raman analysis, and high-resolution transmission electron microscopy (HRTEM). The monoclinic structure of the HfO2 NPs was resolved utilizing x-ray diffraction (XRD). The optical properties were studied from the UV-Vis absorption spectrum. The optical band gap of the HfO2NPs was observed to be 5.1 eV. The Raman spectrum shows the presence of HfO2 NPs. The HRTEM image showed that the HfO2 NPs were of spherical shape with an average particle size of around 28 nm. The energy-dispersive x-ray spectroscopy (EDS) spectrum obviously demonstrated the presence of HfO2 NPs. Analysis and studies on the dielectric properties of the HfO2 NPs such as the dielectric constant, the dielectric loss, and alternating current (AC) conductivity were carried out at varying frequencies and temperatures.

Study on industrial wastewater treatment using superconducting magnetic separation

NASA Astrophysics Data System (ADS)

Zhang, Hao; Zhao, Zhengquan; Xu, Xiangdong; Li, Laifeng

2011-06-01

The mechanism of industrial wastewater treatment using superconducting magnetic separation is investigated. Fe 3O 4 nanoparticles were prepared by liquid precipitation and characterized by X-ray diffraction (XRD). Polyacrylic acid (PAA) film was coated on the magnetic particles using plasma coating technique. Transmission electron microscope (TEM) observation and infrared spectrum measurement indicate that the particle surface is well coated with PAA, and the film thickness is around 1 nm. Practical paper factory wastewater treatment using the modified magnetic seeds in a superconducting magnet (SCM) was carried out. The results show that the maximum removal rate of chemical oxygen demand (COD) by SCM method can reach 76%.

A facile synthesis of poly(aniline-co-o-bromoaniline) copolymer: Characterization and application as semiconducting material

NASA Astrophysics Data System (ADS)

Mahudeswaran, A.; Vivekanandan, J.; Vijayanand, P. S.; Kojima, T.; Kato, S.

2016-01-01

Poly(aniline-co-o-bromoaniline) (p(an-co-o-BrAn)) copolymer has been synthesized using chemical oxidation method in the hydrochloric acid medium. Copolymerization of aniline with o-bromoaniline of different compositions, such as 1:1, 1:2, 2:1, 1:3 and 3:1 molar ratios were prepared. The synthesized copolymer is soluble in polar solvents like dimethyl sulphoxide (DMSO), dimethyl formamide (DMF), Tetrahydrofuran (THF) and 1-methyl 2-pyrrolidone (NMP). The copolymer is analyzed by various characterization techniques, such as FTIR, UV-Visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), conductivity, Differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). FTIR spectrum confirms the characteristic peaks of the copolymer containing benzenoid and quinoid ring stretching. UV spectrum reveals the formation of π-π∗ transition and n-π∗ transition between the energy levels. XRD peaks reveal that the copolymer possesses amorphous nature. Morphological study reveals that the agglomerated particles form globular structure and size of the each particle is about 100 nm. The electrical conductivity of the copolymers is found in the range of 10-5Scm-1. These organic semiconductor materials can be used to fabricate thinner and cheaper environmental friendly optoelectronic devices that will replace the conventional inorganic semiconductors.

Hydrothermal Growth of Vertically Aligned ZnO Nanorods Using a Biocomposite Seed Layer of ZnO Nanoparticles.

PubMed

Ibupoto, Zafar Hussain; Khun, Kimleang; Eriksson, Martin; AlSalhi, Mohammad; Atif, Muhammad; Ansari, Anees; Willander, Magnus

2013-08-19

Well aligned ZnO nanorods have been prepared by a low temperature aqueous chemical growth method, using a biocomposite seed layer of ZnO nanoparticles prepared in starch and cellulose bio polymers. The effect of different concentrations of biocomposite seed layer on the alignment of ZnO nanorods has been investigated. ZnO nanorods grown on a gold-coated glass substrate have been characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. These techniques have shown that the ZnO nanorods are well aligned and perpendicular to the substrate, and grown with a high density and uniformity on the substrate. Moreover, ZnO nanorods can be grown with an orientation along the c -axis of the substrate and exhibit a wurtzite crystal structure with a dominant (002) peak in an XRD spectrum and possessed a high crystal quality. A photoluminescence (PL) spectroscopy study of the ZnO nanorods has revealed a conventional near band edge ultraviolet emission, along with emission in the visible part of the electromagnetic spectrum due to defect emission. This study provides an alternative method for the fabrication of well aligned ZnO nanorods. This method can be helpful in improving the performance of devices where alignment plays a significant role.

Hydrothermal Growth of Vertically Aligned ZnO Nanorods Using a Biocomposite Seed Layer of ZnO Nanoparticles

PubMed Central

Ibupoto, Zafar Hussain; Khun, Kimleang; Eriksson, Martin; AlSalhi, Mohammad; Atif, Muhammad; Ansari, Anees; Willander, Magnus

2013-01-01

Well aligned ZnO nanorods have been prepared by a low temperature aqueous chemical growth method, using a biocomposite seed layer of ZnO nanoparticles prepared in starch and cellulose bio polymers. The effect of different concentrations of biocomposite seed layer on the alignment of ZnO nanorods has been investigated. ZnO nanorods grown on a gold-coated glass substrate have been characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. These techniques have shown that the ZnO nanorods are well aligned and perpendicular to the substrate, and grown with a high density and uniformity on the substrate. Moreover, ZnO nanorods can be grown with an orientation along the c-axis of the substrate and exhibit a wurtzite crystal structure with a dominant (002) peak in an XRD spectrum and possessed a high crystal quality. A photoluminescence (PL) spectroscopy study of the ZnO nanorods has revealed a conventional near band edge ultraviolet emission, along with emission in the visible part of the electromagnetic spectrum due to defect emission. This study provides an alternative method for the fabrication of well aligned ZnO nanorods. This method can be helpful in improving the performance of devices where alignment plays a significant role. PMID:28811454

Biogenic silver nanoparticles: efficient and effective antifungal agents

NASA Astrophysics Data System (ADS)

Netala, Vasudeva Reddy; Kotakadi, Venkata Subbaiah; Domdi, Latha; Gaddam, Susmila Aparna; Bobbu, Pushpalatha; Venkata, Sucharitha K.; Ghosh, Sukhendu Bikash; Tartte, Vijaya

2016-04-01

Biogenic synthesis of silver nanoparticles (AgNPs) by exploiting various plant materials is an emerging field and considered green nanotechnology as it involves simple, cost effective and ecofriendly procedure. In the present study AgNPs were successfully synthesized using aqueous callus extract of Gymnema sylvestre. The aqueous callus extract treated with 1nM silver nitrate solution resulted in the formation of AgNPs and the surface plasmon resonance (SPR) of the formed AgNPs showed a peak at 437 nm in the UV Visible spectrum. The synthesized AgNPs were characterized using Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and X-ray diffraction spectroscopy (XRD). FTIR spectra showed the peaks at 3333, 2928, 2361, 1600, 1357 and 1028 cm-1 which revealed the role of different functional groups possibly involved in the synthesis and stabilization of AgNPs. TEM micrograph clearly revealed the size of the AgNPs to be in the range of 3-30 nm with spherical shape and poly-dispersed nature; it is further confirmed by Particle size analysis that the stability of AgNPs is due its high negative Zeta potential (-36.1 mV). XRD pattern revealed the crystal nature of the AgNPs by showing the braggs peaks corresponding to (111), (200), (220) and (311) planes of face-centered cubic crystal phase of silver. Selected area electron diffraction pattern showed diffraction rings and confirmed the crystalline nature of synthesized AgNPs. The synthesized AgNPs exhibited effective antifungal activity against Candida albicans, Candida nonalbicans and Candida tropicalis.

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.

Alternating current response studies on nickel ferrite-niobium composite at room temperature

NASA Astrophysics Data System (ADS)

Reddy, L. P. Babu; Rajprakash, H. G.; Chethan, B.; Vijayakumari, S. C.; Ravikiran, Y. T.

2018-05-01

In the present research NDNF -Niobium Pentaxide doped Nickel Ferrite [NiFe2O4-Nb2O5-50%] composite was prepared by Mechano-Chemical mixing of NiFe2O4 [NF] with Nb2O5. NF and the NDNF were structurally characterized by four transform infrared spectroscopy [FTIR] and X-ray diffraction [XRD] techniques. The presence of characteristic absorption bands of NF and Nb2O5 in the FTIR spectrum of NDNF with small shift confirmed interfacial interaction of NF with Nb2O5. XRD studies also confirm interfacial interaction between NF and Nb2O5 in the composite and crystalline nature with an average crystallite size of 30nm. The Alternating Current (AC) response parameters of NF and the NDNF were comparatively studied in the frequency range 100Hz-1MHz at room temperature. Increase in AC conductivity of the NDNF has compared to NF was observed and discussed based on the electron hole exchange mechanism.

Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

Study on structural, morphological, optical and thermal properties of guanidine carbonate doped nickel sulfate hexahydrate crystal.

PubMed

Silambarasan, A; Rajesh, P; Ramasamy, P

2015-01-05

The single crystal of guanidine carbonate doped nickel sulfate hexahydrate was grown from solution for ultraviolet filters. The single crystal XRD confirms that the grown single crystal belongs to the tetragonal system with the space group of P4₁2₁2. The crystallinity of the grown crystal was estimated by powder X-ray diffraction studies. The optical transmission and thermal stability of as-grown guanidine carbonate doped nickel sulfate single crystals have been studied. The optical transmission spectrum demonstrates the characteristics of ultraviolet filters. The TG/DTA studies confirm the thermal properties of grown crystals. Thermo-gravimetric analysis showed that the dehydration temperature of the guanidine carbonate doped nickel sulfate crystal is about 100 °C, which is much higher than that of pure nickel sulfate hexahydrate (NSH) crystals which is 72 °C. The growth behaviors and dislocation density were detected under the high resolution XRD and etching studies respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Time dependent rise and decay of photocurrent in zinc oxide nanoparticles in ambient and vacuum medium

NASA Astrophysics Data System (ADS)

C, Rajkumar; Srivastava, Rajneesh K.

2018-05-01

Zinc oxide (ZnO) nanoparticle has been synthesized by cost effective Co-precipitation method and studied its photo-response activity. The synthesized ZnO nanomaterial was characterized by using various analytical techniques such as x-ray diffraction (XRD), UV–visible spectroscopy, FTIR spectroscopy, photoluminescence (PL) spectroscopy, and Scanning Electron Microscopy (SEM). From the XRD results, it is confirmed that synthesized ZnO nanomaterial possess hexagonal wurtzite phase structure with an average crystallite size of ∼16–17 nm. The UV-Visible absorption spectrum shows that it has blue shift compared to their bulk counterparts. Photoluminescence spectra of ZnO nanoparticles have a strong violet band at 423 nm and three weak bands at 485 nm (blue), 506 nm (green), and 529 nm (green). The presence of hydroxyl group was confirmed by FTIR. The photo-response analysis was studied by the time-dependent rise and decay photocurrent of ZnO nanoparticle was tested in the air as well as vacuum medium.

Identification of montgomeryite mineral [Ca4MgAl4(PO4)6·(OH)4·12H2O] found in the Jenolan Caves—Australia

NASA Astrophysics Data System (ADS)

Frost, Ray L.; Xi, Yunfei; Palmer, Sara J.; Pogson, Ross E.

In this paper, we report on many phosphate containing natural minerals found in the Jenolan Caves - Australia. Such minerals are formed by the reaction of bat guano and clays from the caves. Among these cave minerals is the montgomeryite mineral [Ca4MgAl4(PO4)6·(OH)4·12H2O]. The presence of montgomeryite in deposits of the Jenolan Caves - Australia has been identified by X-ray diffraction (XRD). Raman spectroscopy complimented with infrared spectroscopy has been used to characterise the crystal structure of montgomeryite. The Raman spectrum of a standard montgomeryite mineral is identical to that of the Jenolan Caves sample. Bands are assigned to H2PO4-, OH and NH stretching vibrations. By using a combination of XRD and Raman spectroscopy, the existence of montgomeryite in the Jenolan Caves - Australia has been proven. A mechanism for the formation of montgomeryite is proposed.

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.

Shock induced reaction of Ni/Al nanopowder mixture.

PubMed

Meng, C M; Wei, J J; Chen, Q Y

2012-11-01

Nanopowder Ni/Al mixture (mixed in Al:Ni = 2:1 stoichiometry) was shock compressed by employing single and two-stage light gas gun. The particle size of Al and Ni are 100-200 nm and 50-70 nm respectively, morphologies of Al and Ni are sphere like either. Recovered product was characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) analysis. According to the XRD spectrum, the mixed powder undergo complete reaction under shock compression, reaction product consist of Ni2Al3, NiAl and corundum structure Al2O3 compound. Grain size of Ni-Al compound is less than 100 nm. With the shock pressure increasing, the ratio of Ni2Al3 decreased obviously. The corundum crystal size is 400-500 nm according to the SEM observation. The results of shock recovery experiments and analysis show that the threshold pressure for reaction of nano size powder Ni/Al mixture is much less than that of micro size powder.

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.

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.

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

PubMed

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

2014-09-01

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

Synthesis, growth, structural, optical, spectral, thermal and mechanical studies of 4-methoxy 4-nitrostilbene (MONS): a new organic nonlinear optical single crystal.

PubMed

Dinakaran, Paul M; Bhagavannarayana, G; Kalainathan, S

2012-11-01

4-Methoxy 4-nitrostilbene (MONS), a new organic nonlinear optical material has been synthesized. Based on the solubility data good quality single crystal with dimensions up to 38×11×3 mm(3) has been grown by slow evaporation method using ethyl methyl ketone (MEK) as a solvent. Powder XRD confirms the crystalline property and also the diffraction planes have been indexed. The lattice parameters for the grown MONS crystals were determined by using single crystal X-ray diffraction analysis and it reveals that the crystal lattice system is triclinic. The crystalline perfection of the grown crystals has been analysed by high resolution X-ray diffraction (HRXRD) rocking curve measurements. Fourier transform infrared (FTIR) spectrum for powdered MONS sample confirms the functional groups present in the grown crystal. The UV-vis absorption spectrum has been recorded in the range of 190-1100 nm and the cut off wavelength 499 nm has been determined. The optical constants of MONS have been determined through UV-vis-NIR spectroscopy. The MONS crystals were further subjected to other characterizations. i.e., (1)H NMR, TG/DTA, photoluminescence and microhardness test. The Kurtz and Perry powder technique confirms the NLO property of the grown crystal and the SHG efficiency of MONS was found to be 1.55× greater than that of KDP crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

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

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

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

EPR and optical investigations of LaMgAl{sub 11}O{sub 19}:Cr{sup 3+} phosphor

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

Singh, Vijay, E-mail: vijayjiin2006@yahoo.com; Sivaramaiah, G.; Rao, J.L.

2014-12-15

Graphical abstract: The EPR spectrum of as-prepared LaMgAl{sub 11}O{sub 19}:Cr{sup 3+} phosphor at 110 K. - Highlights: • Using the combustion synthesis, LaMgAl{sub 11}O{sub 19}:Cr{sup 3+} phosphor has been prepared in a few minutes. • Optical investigation indicates that Cr{sup 3+} ions are present in octahedral symmetry. • The EPR signals indicate that exchange coupled Cr{sup 3+}–Cr{sup 3+} ion pairs in weakly distorted sites. - Abstract: The LaMgAl{sub 11}O{sub 19}:Cr{sup 3+} phosphor has been prepared by a low-temperature combustion synthesis method. As-prepared combustion synthesized powder was characterized using powder X-ray diffraction (XRD), diffuse reflectance (DRS), electron paramagnetic resonance (EPR) andmore » photoluminescence (PL) studies. The X-ray diffraction pattern reveals crystalline hexagonal phases. The UV–vis diffuse reflectance spectrum exhibits three broad bands characteristic of Cr{sup 3+} ions in octahedral symmetry. The EPR spectrum exhibits several resonance signals. The signals with the effective g values at g = 4.84, 3.64 and 2.26 have been attributed to the isolated Cr{sup 3+} ions. The signal with the effective g value at g = 1.94 has been attributed to exchange coupled Cr{sup 3+}–Cr{sup 3+} ion pairs. The PL studies exhibit several bands characteristic of Cr{sup 3+} ions in octahedral symmetry.« less

On thermal conditions and properties of thallium bromide single crystals grown by the Electro Dynamic Gradient method

NASA Astrophysics Data System (ADS)

Zheng, Zhiping; Yu, Yongtao; Gong, Shuping; Fu, Qiuyun; Zhou, Dongxiang

2013-05-01

The Electro Dynamic Gradient (EDG) method has been proved to be a feasible way to grow TlBr crystals in our previous work. In this research, the influence of thermal conditions such as cooling rate during growth process on the crystal performance was investigated. Crystals of approximately 12 mm diameter were obtained by the EDG method at different cooling rates during the growth process, and the quality of the crystals was routinely evaluated by X-ray diffraction (XRD), infrared (IR) and ultraviolet (UV) transmission, I-V measurement and energy response spectrum. The results proved that thermal conditions during growth had a profound influence on the characteristics of the crystals.

ZnO nanoparticles based fiber optic gas sensor

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

Narasimman, S.; Sivacoumar, R.; Alex, Z. C.

In this work, ZnO nanoparticles were synthesized by simple aqueous chemical route method. The synthesized ZnO nanoparticles were characterized by X-ray diffraction and scanning electron microscope. The sensitivity of the nanoparticles was studied for different gases like acetone, ammonia and ethanol in terms of variation in spectral light intensity. The XRD and SEM analysis confirms the formation of hexagonal wurtzite structure with the grain size of 11.2 nm. The small cladding region of the optical fiber was replaced with the synthesized nanoparticles. The light spectrum was recorded for different gas concentrations. The synthesized nanoparticles showed high sensitivity towards ammonia in lowmore » ppm level and acetone in high ppm level.« less

Crystal growth, electronic structure and optical properties of Sr2Mg(BO3)2

NASA Astrophysics Data System (ADS)

Lv, Xianshun; Wei, Lei; Wang, Xuping; Xu, Jianhua; Yu, Huajian; Hu, Yanyan; Zhang, Huadi; Zhang, Cong; Wang, Jiyang; Li, Qinggang

2018-02-01

Single crystals of Sr2Mg(BO3)2 (SMBO) were grown by Kyropoulos method. X-ray powder diffraction (XRD) analysis, transmission spectrum, thermal properties, band structure, density of states and charge distribution as well as Raman spectra of SMBO were described. The as-grown SMBO crystals show wide transparency range with UV cut-off below 180 nm. A direct band gap of 4.66 eV was obtained from the calculated electronic structure results. The calculated band structure and density of states results indicated the top valence band is determined by O 2p states whereas the low conduction band mainly consists of Sr 5s states. Twelve Raman peaks were observed in the experimental spectrum, fewer than the number predicted by the site group analysis. Raman peaks of SMBO were assigned combining first-principle calculation and site group analysis results. The strongest peak at 917 cm-1 in the experimental spectrum is assigned to symmetric stretching mode A1‧(ν1) of free BO3 units. SMBO is a potential Raman crystal which can be used in deep UV laser frequency conversion.

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.

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.

Exfoliation of Hexagonal Boron Nitride via Ferric Chloride Intercalation

NASA Technical Reports Server (NTRS)

Hung, Ching-cheh; Hurst, Janet; Santiago, Diana; Rogers, Richard B.

2014-01-01

Sodium fluoride (NaF) was used as an activation agent to successfully intercalate ferric chloride (FeCl3) into hexagonal boron nitride (hBN). This reaction caused the hBN mass to increase by approx.100 percent, the lattice parameter c to decrease from 6.6585 to between 6.6565 and 6.6569 ?, the x-ray diffraction (XRD) (002) peak to widen from 0.01deg to 0.05deg of the full width half maximum value, the Fourier transform infrared (FTIR) spectrum's broad band (1277/cm peak) to change shape, and new FTIR bands to emerge at 3700 to 2700 and 1600/cm. This indicates hBN's structural and chemical properties are significantly changed. The intercalated product was hygroscopic and interacted with moisture in the air to cause further structural and chemical changes (from XRD and FTIR). During a 24-h hold at room temperature in air with 100 percent relative humidity, the mass increased another 141 percent. The intercalated product, hydrated or not, can be heated to 750 C in air to cause exfoliation. Exfoliation becomes significant after two intercalation-air heating cycles, when 20-nm nanosheets are commonly found. Structural and chemical changes indicated by XRD and FTIR data were nearly reversed after the product was placed in hydrochloric acid (HCl), resulting in purified, exfoliated, thin hBN products.

Synthesis and characterization of Sn/zeolite and catalytic activity test in the esterification reaction of sludge oil

NASA Astrophysics Data System (ADS)

Alimuddin, Andi Hairil; Usman, Thamrin; Wahyuni, Nelly; Rudiyansyah, Prawatya, Yopa Eka; Astar, Ismail; Yustira, Yudi

2017-03-01

Synthesis of Sn-Zeolite has been made to use for esterification reaction of free fatty acids in sludge oil. Catalyst characterization was accomplished using X-Ray Diffraction (XRD), X-Ray Flourecence (XRF), and Fourier Transform Infra Red (FTIR). Catalyst Sn/zeolite was synthesized by impregnated Sn of SnCl2 into the zeolite. The amount of Sn impregnated base on the value of cation exchange capacity (CEC) of zeolites. Esterification reaction of fatty acids from sludge oil using Sn/Zeolite catalyst was did by variated the reaction time. XRD analysis results showed that the catalyst Sn/zeolite was dominated by modernit and quartz. XRF analysis results was increasing amount of Sn metal and the Si/Al ratio on Sn/zeolite catalyst along with addition of Sn metal. FTIR analysis results showed that the catalyst synthesized had Bronsted acid side (the spectrum 1639.4; 1656.7; 1654.8 cm-1) and the Lewis acid (spectrum 1400.2 and 1402.2 cm-1). The results showed that the optimum conditions of esterification reaction in 4 hours reaction time, 5% concentration of the catalyst, and molar ratio was about 1:10 with a conversion percentage of products reached 96.00%, which can be achieved with a ratio was about 4:1 between Sn and zeolite on Sn/zeolite catalyst.

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

PubMed

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

2015-12-01

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

Documenting mudstone heterogeneity by use of principal component analysis of X-ray diffraction and portable X-ray fluorescence data: A case study in the Triassic Shublik Formation, Alaska North Slope

USGS Publications Warehouse

Boehlke, Adam; Whidden, Katherine J.; Benzel, William M.

2017-01-01

Determining the chemical and mineralogical variability within fine-grained mudrocks poses analytical challenges but is potentially useful for documenting subtle stratigraphic differences in physicochemical environments that may influence petroleum reservoir properties and behavior. In this study, we investigate the utility of combining principal component analysis (PCA) of X-ray diffraction (XRD) data and portable X-ray fluorescence (pXRF) data to identify simplifying relationships within a large number of samples and subsequently evaluate a subset that encompasses the full spectrum or range of mineral and chemical variability within a vertical section. Samples were collected and analyzed from a vertical core of the Shublik Formation, a heterogeneous, phosphate-rich, calcareous mudstone-to-marl unit deposited in the Arctic Alaska Basin (AAB) during the Middle and Late Triassic. The Shublik is a major petroleum source rock in the Alaskan North Slope, and is considered a prime target for continuous self-sourced resource plays.

Powder-XRD and (14) N magic angle-spinning solid-state NMR spectroscopy of some metal nitrides.

PubMed

Kempgens, Pierre; Britton, Jonathan

2016-05-01

Some metal nitrides (TiN, ZrN, InN, GaN, Ca3 N2 , Mg3 N2 , and Ge3 N4 ) have been studied by powder X-ray diffraction (XRD) and (14) N magic angle-spinning (MAS) solid-state NMR spectroscopy. For Ca3 N2 , Mg3 N2 , and Ge3 N4 , no (14) N NMR signal was observed. Low speed (νr  = 2 kHz for TiN, ZrN, and GaN; νr  = 1 kHz for InN) and 'high speed' (νr  = 15 kHz for TiN; νr  = 5 kHz for ZrN; νr  = 10 kHz for InN and GaN) MAS NMR experiments were performed. For TiN, ZrN, InN, and GaN, powder-XRD was used to identify the phases present in each sample. The number of peaks observed for each sample in their (14) N MAS solid-state NMR spectrum matches perfectly well with the number of nitrogen-containing phases identified by powder-XRD. The (14) N MAS solid-state NMR spectra are symmetric and dominated by the quadrupolar interaction. The envelopes of the spinning sidebands manifold are Lorentzian, and it is concluded that there is a distribution of the quadrupolar coupling constants Qcc 's arising from structural defects in the compounds studied. Copyright © 2015 John Wiley & Sons, Ltd.

In-situ XRD vs ex-situ vacuum annealing of tantalum oxynitride thin films: Assessments on the structural evolution

NASA Astrophysics Data System (ADS)

Cunha, L.; Apreutesei, M.; Moura, C.; Alves, E.; Barradas, N. P.; Cristea, D.

2018-04-01

The purpose of this work is to discuss the main structural characteristics of a group of tantalum oxynitride (TaNxOy) thin films, with different compositions, prepared by magnetron sputtering, and to interpret and compare the structural changes, by X-ray diffraction (XRD), when the samples are vacuum annealed under two different conditions: i) annealing, followed by ex-situ XRD: one sample of each deposition run was annealed at a different temperature, until a maximum of 800 °C, and the XRD patterns were obtained, at room temperature, after each annealing process; ii) annealing with in-situ XRD: the diffraction patterns are obtained, at certain temperatures, during the annealing process, using always the same sample. In-situ XRD annealing could be an interesting process to perform annealing, and analysing the evolution of the structure with the temperature, when compared to the classical process. A higher structural stability was observed in some of the samples, particularly on those with highest oxygen content, but also on the sample with non-metal (O + N) to metal (Ta) ratio around 0.5.

Effect of iron doping on structural and microstructural properties of nanocrystalline ZnSnO3 thin films prepared by spray pyrolysis techniques

NASA Astrophysics Data System (ADS)

Pathan, Idris G.; Suryawanshi, Dinesh N.; Bari, Anil R.; Patil, Lalchand A.

2018-05-01

This work presents the effect of iron doping having different volume ratios (1 ml, 2.5 ml and 5 ml) on the structural, microstructural and electrical properties of zinc stannate thin films, prepared by spray pyrolysis method. These properties were characterized with X-ray diffraction (XRD) and Transmission Electron Microscope (TEM). In our study, XRD pattern indicates that ZnSnO3 has a perovskite phase with face exposed hexahedron structure. The electron diffraction fringes observed are in consistent with the peak observed in XRD patterns. Moreover the sensor reported in our study is cost-effective, user friendly and easy to fabricate.

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

Pole Figure Explorer v. 1.8

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

Van Benthem, Mark H.

2016-05-04

This software is employed for 3D visualization of X-ray diffraction (XRD) data with functionality for slicing, reorienting, isolating and plotting of 2D color contour maps and 3D renderings of large datasets. The program makes use of the multidimensionality of textured XRD data where diffracted intensity is not constant over a given set of angular positions (as dictated by the three defined dimensional angles of phi, chi, and two-theta). Datasets are rendered in 3D with intensity as a scaler which is represented as a rainbow color scale. A GUI interface and scrolling tools along with interactive function via the mouse allowmore » for fast manipulation of these large datasets so as to perform detailed analysis of diffraction results with full dimensionality of the diffraction space.« less

Green synthesis, characterization and catalytic degradation studies of gold nanoparticles against congo red and methyl orange.

PubMed

Umamaheswari, C; Lakshmanan, A; Nagarajan, N S

2018-01-01

The present study reports, novel and greener method for synthesis of gold nanoparticles (AuNPs) using 5,7-dihydroxy-6-metoxy-3 ' ,4 ' methylenedioxyisoflavone (Dalspinin), isolated from the roots of Dalbergia coromandeliana was carried out for the first time. The synthesized gold nanoparticles were characterized by UV-Vis spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The observed surface plasmon resonance (SPR) at 532nm in the UV-Vis absorption spectrum indicates the formation of gold nanoparticles. The powder XRD and SAED pattern for synthesized gold nanoparticles confirms crystalline nature. The HR-TEM images showed that the AuNPs formed were small in size, highly monodispersed and spherical in shape. The average particle sizes of the AuNPs are found to be ~10.5nm. The prepared AuNPs were found to be stable for more than 5months without any aggregation. The catalytic degradation studies of the synthesized AuNPs towards degradation of congo red and methyl orange, showed good catalytic in the complete degradation of both the dyes. The reduction catalyzed by gold nanoparticles followed the pseudo-first order kinetics, with a rate constant of 4.5×10 -3 s -1 (R 2 =0.9959) and 1.7×10 -3 s -1 (R 2 =0.9918) for congo red (CR) and methyl orange (MO), respectively. Copyright © 2017. Published by Elsevier B.V.

Synthesis of nanocrystalline Gd2Ti2O7 by combustion process and its structural, optical and dielectric properties

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Wariar, P. R. S.

2017-07-01

Nanosized pyrochlore material Gadolinium Titanate (Gd2Ti2O7) powder was prepared by modified single step auto-ignition combustion process. The phase formation has been investigated using X-Ray diffraction analysis (XRD). The crystalline pyrochlore phase is further confirmed by the presence of metal-oxygen bonds in the FT-IR spectra. XRD analysis revealed that Gd2Ti2O7 has a cubic structure with Fd3m space group. The combustion powder was sintered to high density (97% of theoretical density) at ˜13000 C for 4h and the surface morphology was examined by Scanning Electron Microscopy (SEM). The optical band gap of Gd2Ti2O7 determined from the absorption spectrum is found to be 4.2 eV, which corresponds to direct allowed transitions. The dielectric measurements were carried out using LCR meter in the radio frequency region at room temperature. The sintered Gd2Ti2O7 has a dielectric constant (Ɛr) = 40 and dielectric loss (tan δ) = 0.01 at 1MHz.

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

NASA Astrophysics Data System (ADS)

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

2011-03-01

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

Structural versus electrical properties of an organic-inorganic hybrid material based on sulfate

NASA Astrophysics Data System (ADS)

Ben Rached, Asma; Guionneau, Philippe; Lebraud, Eric; Mhiri, Tahar; Elaoud, Zakaria

2017-01-01

A new organo-sulfate compound is obtained by slow evaporation at room temperature and is characterized by powder and single-crystal X-ray diffraction (XRD) at variable temperatures. The benzylammonium monohydrogenosulfate of formula C6H5CH2NH3+. HSO4-, denoted (BAS), crystallizes in the monoclinic system P21/c space group with the following parameters at room temperature: a=5.623(5)Å, b=20.239(5) Å, c=8.188(5)Å, β=94.104(5)°. The crystal structure consists of infinite parallel two-dimensional planes built by HSO4- anions and C6H5CH2NH3+ cations interconnected by strong O-H….. O and N-H….. O hydrogen bonds. A phase transition is detected at 350 K by differential scanning calorimetry (DSC) and confirmed by powder XRD. Conductivity measurements using the impedance spectroscopy technique allow to determine the conductivity relaxation parameters associated with the H+ conduction from an analysis of the M"/M"max spectrum measured in a wide temperature range. Transport properties of this material appear to be due to an H+ ion hopping mechanism.

One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

NASA Astrophysics Data System (ADS)

Pujar, Malatesh S.; Hunagund, Shirajahammad M.; Desai, Vani R.; Patil, Shivaprasadgouda; Sidarai, Ashok H.

2018-04-01

We report the simple Co-precipitation method for the synthesis of Cerium oxide (CeO2) nanoparticles (NPs) in an ambient temperature. We have taken the Cerium (III) nitrate hexahydrate (Ce(NO3)3.6H2O) and Sodium hydroxide (NaOH) as the precursors. The obtained NPs were analyzed using the UV-Vis spectrophotometer, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The obtained results signify that UV-Vis spectrum exhibited a well-defined absorption peak at 274 nm and the estimated energy gap (Eg) is 4.05 eV. The FT-IR analysis provides the supporting evidence for the presence of bonding of O-H, nitrates, alcohols and O-Ce-O vibrations. The XRD result reveals that the synthesized CeO2 NPs was crystallite with cubic phase structure and the estimated average crystallite size of CeO2 NPs using Scherer's and W-H method was significantly different due to their assumptions. Further, it is purposed to study their photocatalytic biological activities.

The new 3-(tert-butyl)-1-(2-nitrophenyl)-1H-pyrazol-5-amine: Experimental and computational studies

NASA Astrophysics Data System (ADS)

Cuenú, Fernando; Muñoz-Patiño, Natalia; Torres, John Eduard; Abonia, Rodrigo; Toscano, Rubén A.; Cobo, J.

2017-11-01

The molecular and supramolecular structure of the title compound, 3-(tertbutyl)-1-(2-nitrophenyl)-1H-pyrazol-5-amine (2NPz) from the single crystal X-ray diffraction (SC-XRD) and spectroscopic data analysis is reported. The computational analysis of the structure, geometry optimization, vibrational frequencies, nuclear magnetic resonance and UV-Vis is also described and compared with experimental data. Satisfactory theoretical aspects were made for the molecule using density functional theory (DFT), with B3LYP and B3PW91 functionals, and Hartree-Fock (HF), with 6-311++G(d,p) basis set, using GAUSSIAN 09 program package without any constraint on the geometry. With VEDA 4 software, vibrational frequencies were assigned in terms of the potential energy distribution while, with the GaussSum software, the percentage contribution of the frontier orbitals at each transition of the electronic absorption spectrum was established. The obtained results indicated that optimized geometry could well reflect the molecular structural parameters from SC-XRD. Theoretical data obtained for the vibrational analysis and NMR spectra are consistent with experimental data.

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

Yudoyono, Gatut, E-mail: gyudoyono@physics.its.ac.id; Zharvan, Vicran; Ichzan, Nur

Titanium dioxide (titania) nanoparticle were synthesized by coprecipitation process of titanium trichloride (TiCl{sub 3}) in aqueous medium, with NH{sub 4}OH as pH regulator. The pH solution was varied during the synthesis process between pH 3-8.4, and all samples were calcined temperature at 400°C for 3 hours. Characteristics and properties of the TiO{sub 2} powder were investigated using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM). XRD results show that the single-phase rutile formed when the pH is less than 5, anatase single phase formed began pH 8, and the pH of the solution between 5-8 formed mixed phase rutile-anatase-brookite, rutile-brookite ormore » anatase-brookite. Methylene Blue (MB) photodegradation test were performed in order to evaluate photocatalytic activity. Nanoparticles TiO{sub 2} rutile, anatase phase, and mixed phase rutile-brookite, anatase-brookite used to test the photocatalytic activity by measuring the absorbance spectrum photodegradation using UV-Vis spectrometer. The test results showed that the mixture phase of rutile-brookite provide the greatest photodegradation than other phases.« less

Study on the removal of iron impurities in methanesulfonic acid tin plating bath

NASA Astrophysics Data System (ADS)

Hou-li, LIU; Jian-Jun, CHEN; Hong-Liang, PAN

2018-03-01

This thesis investigated the the influence of sodium sulfite as reducing agent on the recovery rate of tin ion. The approach is that HZ016 type cation exchange resin was used to adsorb Sn2+ and Fe2+ in electroplated tin solution first. After adsorption, the resin was removed by sulfuric acid, which was added with NaOH to adjust pH value to form precipitation and separate tin. X-ray diffraction (XRD) and energy spectrum (EDS) method were used to analyze the composition of the precipitates adjusted by pH. The results show that when the mass ratio of resin to bath is 1:2, the adsorption efficiency of resin reaches 98.3% and 97.1% respectively, and the elution efficiency of tin and iron reaches 95.1% and 94% respectively when the mass ratio of resin to eluent sulfuric acid is 1:4. Sodium sulfite was added to increase the efficiency of tin recovery by 8.1%. EDS and XRD atlas showed that after pH regulation, the main composition of the filtration precipitation was the hydroxides of tin.

Molten salt synthesis and luminescent properties of YVO4:Ln (Ln = Eu3+, Dy3+) nanophosphors.

PubMed

Liu, Chenglu; Wang, Fang; Jia, Peiyun; Lin, Jun; Zhou, Zhiqiang

2012-01-01

Eu3+ and Dy(3+)-doped YVO4 nanocrystallites were successfully prepared at 400 degrees C in equal moles of NaNO3 and KNO3 molten salts. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, transmission electronic microscopy (TEM), photoluminescence (PL) spectrum and lifetime were used to characterize the nanocrystallites. XRD results demonstrate that NaOH concentration and annealing temperature play important roles in phase purity and crystallinity of the nanocrystallites, the optimum NaOH concentration and annealing temperature being 6:40 and 400 degrees C respectively. TEM micrographs show the nanocrystallites are well crystallized with a cubic morphology in an average grain size of about 18 nm. Upon excitation of the vanadate group at 314 nm, YVO4:Eu3+ and YVO4:Dy3+ nanocrystallites exhibit the characteristic emission of Eu3+ and Dy3+, which indicates that there is an energy transfer from the vanadate group to the rare earth ions. Moreover, the structure and luminescent properties of the nanocrystallites were compared with their bulk counterparts with same composition in detail.

Study of benzotriazole as corrosion inhibitors of carbon steel in chloride solution containing hydrogen sulfide using electrochemical impedance spectroscopy (EIS)

NASA Astrophysics Data System (ADS)

Solehudin, Agus; Nurdin, Isdiriayani

2014-03-01

Corrosion and inhibition studies on API 5LX65 carbon steel in chloride solution containing various concentrations of benzotriazole has been conducted at temperature of 70°C using Electrochemical Impedance Spectroscopy (EIS). Corroded carbon steel surface with and without inhibitor have been observed using X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Energy Dispersive Spectroscopy (EDS). The objectives of this research are to study the performance of benzotriazole as corrosion inhibitors. The experimental results of carbon steel corrosion in 3.5% NaCl solution containing 500 mg/l H2S at different BTAH concentrations showed that corrosion rate of carbon steel decreases with increasing of BTAH concentrations from 0 to 10 mmol/l. The inhibition efficiency of BTAH was found to be affected by its concentration. The optimum efficiency obtained of BTAH is 93% at concentration of 5 mmol/l. The result of XRD and EDS analysis reveal the iron sulfide (FeS) formation on corroded carbon steel surface without inhibitor. The EDS spectrum show the Nitrogen (N) bond on carbon steel surface inhibited by BTAH.

Accessibility of Enzymatically Delignified Bambusa bambos for Efficient Hydrolysis at Minimum Cellulase Loading: An Optimization Study.

PubMed

Kuila, Arindam; Mukhopadhyay, Mainak; Tuli, D K; Banerjee, Rintu

2011-01-01

In the present investigation, Bambusa bambos was used for optimization of enzymatic pretreatment and saccharification. Maximum enzymatic delignification achieved was 84%, after 8 h of incubation time. Highest reducing sugar yield from enzyme-pretreated Bambusa bambos was 818.01 mg/g dry substrate after 8 h of incubation time at a low cellulase loading (endoglucanase, β-glucosidase, exoglucanase, and xylanase were 1.63 IU/mL, 1.28 IU/mL, 0.08 IU/mL, and 47.93 IU/mL, respectively). Enzyme-treated substrate of Bambusa bambos was characterized by analytical techniques such as Fourier transformed infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The FTIR spectrum showed that the absorption peaks of several functional groups were decreased after enzymatic pretreatment. XRD analysis indicated that cellulose crystallinity of enzyme-treated samples was increased due to the removal of amorphous lignin and hemicelluloses. SEM image showed that surface structure of Bambusa bambos was distorted after enzymatic pretreatment.

Influence of the synthesis parameters on the properties of amidoxime grafted sepiolite nanocomposites

NASA Astrophysics Data System (ADS)

Taimur, Shaista; Yasin, Tariq

2017-11-01

Novel polyacrylonitrile (PAN) grafted sepiolite nanocomposites were synthesized via emulsion polymerization. The influence of synthesis parameters on the degree of grafting was studied by varying the concentrations of monomer, initiator and surfactant. The nitrile groups of PAN were chemically modified into amidoxime. Both the grafting and amidoxime percentages were determined gravimetrically and maximum grafting of 373% was achieved at 5% acrylonitrile, 1% surfactant and 0.1% initiator concentrations. The presence of vibration at 2242 cm-1 in Fourier transform infrared (FT-IR) spectrum and x-ray diffraction (XRD) reflection at 2θ = 16.9° (010) confirmed the grafting of PAN chains onto modified sepiolite. XRD patterns also indicated a decrease in crystallinity of sepiolite and appearance of new amorphous region in grafted nanocomposites. The morphological changes of sepiolite during silanization and grafting of PAN is also confirmed by field emission scanning electron microscope (FESEM). Transmission electron microscope (TEM) images clearly showed the shortening of fibers after silanization of sepiolite and the same were involved in heterogeneous nucleation in micelles. These developed amidoxime grafted sepiolite nanocomposites can be used as adsorbent for the metal recovery.

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.

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.;

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

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.

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.

Wet chemical synthesis and luminescence in Ca5(PO4)3M:Eu2+ (M = Br, I) phosphors for solid state lighting

NASA Astrophysics Data System (ADS)

Mungmode, C. D.; Gahane, D. H.; Moharil, S. V.

2018-05-01

A simple wet chemical synthesis of Eu2+ activated Ca5(PO4)3Br and Ca5(PO4)3I phosphors and their photoluminescence is reported. Formation of Ca5(PO4)3Br is confirmed by X-ray diffraction (XRD). Synthesized phosphors are analyzed for photoluminescence (PL) spectrum. A bright blue emission is observed when phosphors are excited by near Ultra Violet (nUV) radiations. Photoluminescence emission spectrum for (Ca0.985Eu0.015)5(PO4)3Br is centered at 457 nm and for (Ca0.985Eu0.015)5(PO4)3 I it peaks at 455 nm when excited by 365 nm near UV radiation. Eu2+ luminescence in Ca5(PO4)3Br is reported for the first time. The phosphors can be efficiently excited by nUV radiations. This shows that phosphors may be used as blue phosphor in pcLED for Solid State Lighting.

Biosynthesis of silver nanoparticles using Plectranthus amboinicus leaf extract and its antimicrobial activity

NASA Astrophysics Data System (ADS)

Ajitha, B.; Ashok Kumar Reddy, Y.; Sreedhara Reddy, P.

2014-07-01

This study reports the simple green synthesis method for the preparation of silver nanoparticles (Ag NPs) using Plectranthus amboinicus leaf extract. The pathway of nanoparticles formation is by means of reduction of AgNO3 by leaf extract, which acts as both reducing and capping agents. Synthesized Ag NPs were subjected to different characterizations for studying the structural, chemical, morphological, optical and antimicrobial properties. The bright circular fringes in SAED pattern and diffraction peaks in XRD profile reveals high crystalline nature of biosynthesized Ag NPs. Morphological studies shows the formation of nearly spherical nanoparticles. FTIR spectrum confirms the existence of various functional groups of biomolecules capping the nanoparticles. UV-visible spectrum displays single SPR band at 428 nm indicating the absence of anisotropic particles. The synthesized Ag NPs exhibited better antimicrobial property towards gram negative Escherichia coli and towards tested Penicillium spp. than other tested microorganisms using disc diffusion method. Finally it has proven that the synthesized bio-inspired Ag NPs have potent antimicrobial effect.

Luminescence Characteristics of ZnGa2O4 Thick Film Doped with Mn2+ and Cr3+ at Various Sintering Temperatures

NASA Astrophysics Data System (ADS)

Cha, Jae Hyeok; Kim, Kyung Hwan; Park, Yong Seo; Kwon, Sang Jik; Choi, Hyung Wook

2007-10-01

ZnGa2O4 phosphor separately doped with Mn2+ and Cr3+ was synthesized by solid-state reaction, and thick films were deposited by screen printing. The X-ray diffraction (XRD) patterns of ZnGa2O4 phosphor thick films show a (311) main peak and a spinal phase. Uniform distribution and filled morphology of the doped ZnGa2O4 phosphor thick films were formed at the sintering temperature of 1100 °C. The CL spectrum of Mn2+-doped ZnGa2O4 shows the main peak of 512 nm green emission with the 4T1→6A1 transition of Mn2+ ions and the CL spectrum of Cr3+-doped ZnGa2O4 shows the main peak of 716 nm red emission with the 2E→4A2 transition of Cr3+ ions.

Effect of annealing on morphology and photoluminescence of beta-Ga2O3 nanostructures.

PubMed

Zhang, Shiying; Zhuang, Huizhao; Xue, Chengshan; Li, Baoli

2008-07-01

A novel method was applied to prepare one-dimensional beta-Ga2O3 nanostructure films. In this method, beta-Ga2O3 nanostructures have been successfully synthesized on Si(111) substrates through annealing sputtered Ga22O3/Mo films for differernt time under flowing ammonia. The as-synthesized beta-Ga2O3 nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and photoluminescence (PL) spectrum. The results show that the formed nanostructures are single-crystalline Ga2O3 with monoclinic structure. The annealing time of the samples has an evident influence on the morphology and optical property of the nanostructured beta-Ga2O3 synthesized. The representative photoluminescence spectrum at room temperature exhibits a strong and broad emission band centered at 411.5 nm and a relatively weak emission peak located at 437.6 nm. The growth mechanism of the beta-Ga2O3 nanostructured materials is also discussed briefly.

Synthesis, structure and characterization of a hybrid centrosymmetric material (4-dimethylaminopyridinium nitrate gallic acid monohydrate) well-designed for non-linear optics

NASA Astrophysics Data System (ADS)

Ennaceur, Nasreddine; Jalel, Boutheina; Henchiri, Rokaya; Cordier, Marie; Ledoux-Rak, Isabelle

2018-01-01

Hybrid material: 4-Dimethylaminopyridinium nitrate gallic acid monohydrate abbreviated DNGA monohydrate has been successfully synthesized by slow evaporation method at room temperature. X-ray diffraction (XRD) on a single crystal showed that the latter was crystallized in P-1 space group. Likewise, thermal analyses demonstrated the stability of our crystal up to 80 °C. Besides, the analysis of the infrared spectrum (FTIR), allowed us to confirm the presence of the different groups present in the structure. Furthermore, by studying the UV-Visible spectrum, the transparency of our crystal was proven. Despite the fact that of having a centrosymmetric structure, the nonlinear optical properties of our single crystal, which was tested by Kurtz-Perry technique, proved that its second harmonic generation efficiency was 1.22 times more than that of KDP (potassium dihydrogen phosphate) single crystal. This nonlinear optical behavior of the studied compound was also determined through the calculations of polarizability and first hyperpolarizability values.

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 and Characterization of a New Co-Crystal Explosive with High Energy and Good Sensitivity

NASA Astrophysics Data System (ADS)

Gao, Han; Jiang, Wei; Liu, Jie; Hao, Gazi; Xiao, Lei; Ke, Xiang; Chen, Teng

2017-10-01

A new energetic co-crystal consisting of one of the most powerful explosive molecules 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) and the military explosive cyclotrimethylenetrinitramine (RDX) was prepared with a simple solvent evaporation method. Scanning electron microscopy (SEM) revealed the morphology of the bar-shaped product, which differed greatly from the morphology of the individual components. Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction spectrum (XRD), and differential scanning calorimetry (DSC) proved the formation of the co-crystal at the molecular level. The result of mechanical sensitivity test indicated the sensitivity was effectively reduced compared to raw CL-20. Finally, a possible crystallization mechanism was discussed.

Effects of Ni(2+) on aluminum hydroxide scale formation and transformation on a simulated drinking water distribution system.

PubMed

Wang, Wendong; Song, Shan; Zhang, Xiaoni; Mitchell Spear, J; Wang, Xiaochang; Wang, Wen; Ding, Zhenzhen; Qiao, Zixia

2014-07-01

Observations of aluminum containing sediments/scales formed within the distribution pipes have been reported for several decades. In this study, the effect of Ni(2+) on the formation and transformation processes of aluminum hydroxide sediment in a simulated drinking water distribution system were investigated using X-ray diffraction spectrum (XRD), Fourier transform infrared spectrum (FT-IR), scanning electron microscope (SEM), and thermodynamic calculation methods. It was determined that the existence of Ni(2+) had notable effects on the formation of bayerite. In the system without Ni(2+) addition, there was no X-ray diffraction signal observed after 400 d of aging. The presence of Ni(2+), however, even when present in small amounts (Ni/Al=1:100) the formation of bayerite would occur in as little as 3d at pH 8.5. As the molar ratio of Ni/Al increase from 1:100 to 1:10, the amount of bayerite formed on the pipeline increased further; meanwhile, the specific area of the pipe scale decreased from 160 to 122 m(2)g(-1). In the system with Ni/Al molar ratio at 1:3, the diffraction spectrum strength of bayerite became weaker, and disappeared when Ni/Al molar ratios increased above 1:1. At these highs Ni/Al molar ratios, Ni5Al4O11⋅18H2O was determined to be the major component of the pipe scale. Further study indicated that the presence of Ni(2+) promoted the formation of bayerite and Ni5Al4O11⋅18H2O under basic conditions. At lower pH (6.5) however, the existence of Ni(2+) had little effect on the formation of bayerite and Ni5Al4O11⋅18H2O, rather the adsorption of amorphous Al(OH)3 for Ni(2+) promoted the formation of crystal Ni(OH)2. Copyright © 2013 Elsevier Ltd. All rights reserved.

Modeling and measurements of XRD spectra of extended solids under high pressure

NASA Astrophysics Data System (ADS)

Batyrev, I. G.; Coleman, S. P.; Stavrou, E.; Zaug, J. M.; Ciezak-Jenkins, J. A.

2017-06-01

We present results of evolutionary simulations based on density functional calculations of various extended solids: N-Si and N-H using variable and fixed concentration methods of USPEX. Predicted from the evolutionary simulations structures were analyzed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction spectra. Stability of the predicted system was estimated from convex-hull plots. X-ray diffraction spectra were calculated using a virtual diffraction algorithm which computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculations of thousands of XRD spectra were used to search for a structure of extended solids at certain pressures with best fits to experimental data according to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Comparison of Raman and IR spectra calculated for best fitted structures with available experimental data shows reasonable agreement for certain vibration modes. Part of this work was performed by LLNL, Contract DE-AC52-07NA27344. We thank the Joint DoD / DOE Munitions Technology Development Program, the HE C-II research program at LLNL and Advanced Light Source, supported by BES DOE, Contract No. DE-AC02-05CH112.

[Preparation of large area Al-ZnO thin film by DC magnetron sputtering].

PubMed

Jiao, Fei; Liao, Cheng; Han, Jun-Feng; Zhou, Zhen

2009-03-01

Solar cells of p-CIS/n-buffer/ZnO type, where CIS is (CuInS2, CuInSe2 or intermediates, are thin-film-based devices for the future high-efficiency and low-cost photovoltaic devices. As important thin film, the properties of Al-doped ZnO (AZO) directly affect the parameter of the cell, especially for large volume. In the present paper, AZO semiconductor transparent thin film on soda-lime glass was fabricated using cylindrical zinc-aluminum target, which can not only lower the cost of the target but also make the preparation of large area AZO thin film more easily. Using the DC magnet sputtering techniques and rolling target, high utilization efficiency of target was achieved and large area uniform and directional film was realized. An introduction to DC magnet sputtering techniques for large area film fabrication is given. With different measurement methods, such as X-ray diffraction (XRD) and scan electron microscope (SEM), we analyzed large size film's structure, appearance, and electrical and optical characteristics. The XRD spectrum indicated that the AZO film shows well zinc-blende structure with a preferred (002) growth and the c-axis is oriented normal to the substrate plane. The lattice constant is 5.603 9 nm and the mismatch with CdS thin film is only 2 percent. It absolutely satisfied the demand of the GIGS solar cell. The cross-section of the AZO thin film indicates the columnar structure and the surface morphology shows that the crystal size is about 50 nm that is consistent with the result of XRD spectrum. By the optical transmission curve, not only the high transmission rate over 85 percent in the visible spectrum between 400 nm and 700 nm was showed but also the band gap 3.1 eV was estimated. And all these parameters can meet the demand of the large area module of GIGS solar cell. The result is that using alloy target and Ar gas, and controlling the appropriate pressure of oxygen, we can get directional, condensed, uniform, high transmitting rate, low resistance and large size (300 mm x 300 mm) AZO film.

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

Sharma, Rabindar K.; Reddy, G. B.

In this work, we have successfully developed plasma assisted paste sublimation route to deposit vertically aligned MoO{sub 3} nanoflakes (NFs) on nickel coated glass substrate in oxygen plasma ambience with the assistant of Ni thin layer as a catalyst. In our case, sublimation source (Mo strip surface) is resistively heated by flowing current across it. The structural, morphological, and optical properties of NFs have been investigated systematically using x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) with selected area electron diffraction (SAED), High resolution transmission electron microscopy (HRTEM), micro-Raman spectroscopy, and Photoluminescence (PL) spectroscopy. Studies reveal thatmore » the presence of oxygen plasma and the nickel thin layer are very essential for the growth of vertically aligned NFs. The observed results divulge that α-MoO{sub 3} NFs are deposited uniformly on large scale with very high aspect (height/thickness) ratio more than 30 and well aligned along [0 k 0] crystallographic direction where k is even (2, 4, 6). Raman spectrum shows a significant size effect on the vibrational property of MoO{sub 3} nanoflakes. The PL spectrum of MoO{sub 3} NFs was recorded at room temperature and four prominent peaks at 365 nm, 395 nm, 452 nm, and 465 nm corresponding to UV-visible region were observed. In this paper, a three step growth strategy for the formation of MoO{sub 3} NFs has been proposed in detail.« less

Crystal growth, characterization and theoretical studies of 4-aminopyridinium picrate

NASA Astrophysics Data System (ADS)

Aditya Prasad, A.; Muthu, K.; Rajasekar, M.; Meenatchi, V.; Meenakshisundaram, S. P.

2015-01-01

Single crystals of 4-aminopyridinium picrate (APP) were grown by slow evaporation of a mixed solvent system methanol-acetone (1:1, v/v) containing equimolar quantities of 4-aminopyridine and picric acid. Structure is elucidated by single crystal XRD analysis and the crystal belongs to monoclinic system with four molecules in the unit cell (space group P21/c) and the cell parameter values are, a = 8.513 Å (±0.015), b = 11.33 Å (±0.02), c = 14.33 Å (±0.03) and β = 104.15° (±0.019), V = 1340 A3 (±6) with refined R factors R1 = 0.0053 and wR2 = 0.0126. The electron density mapping is interpreted to find coordinates for each atom in the crystallized molecules. The various functional groups present in the molecule are confirmed by FT-IR analysis. UV-visible spectral analysis was used to determine the band gap energy of 4-aminopyridinium picrate. Powder X-ray diffraction pattern reveals the crystallinity of the as-grown crystal and it closely resembles the simulated XRD from the single crystal XRD analysis. Scanning electron microscopy reveals the surface morphology of the grown crystal. Optimized geometry is derived by Hartree-Fock theory calculations and the first-order molecular hyperpolarizability (β), theoretically calculated bond length, bond angles and excited state energy from theoretical UV-vis spectrum were estimated.

Structural characterization of Er(3+),Yb(3+)-doped Gd2O3 phosphor, synthesized using the solid-state reaction method, and its luminescence behavior.

PubMed

Tamrakar, Raunak Kumar; Bisen, D P; Brahme, Nameeta

2016-02-01

We report the synthesis and structural characterization of Er(3+),Yb(3+)-doped Gd2O3 phosphor. The sample was prepared using the conventional solid-state reaction method, which is the most suitable method for large-scale production. The prepared phosphor sample was characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), thermoluminescence (TL), photoluminescence (PL) and CIE techniques. For PL studies, the excitation and emission spectra of Gd2O3 phosphor doped with Er(3+) and Yb(3+) were recorded. The excitation spectrum was recorded at a wavelength of 551 nm and showed an intense peak at 276 nm. The emission spectrum was recorded at 276 nm excitation and showed peaks in all blue, green and red regions, which indicate that the prepared phosphor may act as a single host for white light-emitting diode (WLED) applications, as verified by International de I'Eclairage (CIE) techniques. From the XRD data, the calculated average crystallite size of Er(3+) and Yb(3+) -doped Gd2O3 phosphor is ~ 38 nm. A TL study was carried out for the phosphor using UV irradiation. The TL glow curve was recorded for UV, beta and gamma irradiations, and the kinetic parameters were also calculated. In addition, the trap parameters of the prepared phosphor were also studied using computerized glow curve deconvolution (CGCD). Copyright © 2015 John Wiley & Sons, Ltd.

The Effect of Rare Earth Dopants in Crystal Structure of Bi-2212 Superconductor

NASA Astrophysics Data System (ADS)

Suharta, W. G.; Widagda, IGA.; Putra, K.; Suyanto, H.

2017-03-01

Bi2Sr2CaCu2O8+∂ samples have been successfully synthesized by doping rare earth (RE) variations using wet-mixing method. Samples calcined at 600°C for 3 hours and sintered at 850°C for 10 hours. The purpose of research is to determine the effect of the RE dopant on the microscopic structure of BSCRECO superconductors. Therefore, the research was conducted characterization by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope (SEM). Measurements with XRD could be carried out and crystal system of Bi2Sr2CaCu2O8+∂ with rare earth (RE) dopants could be determined clearly. Generally, crystallization has occurred very well demonstrated by the diffraction peaks are sharp, which is dominated by the emergence of Bi-2212 phase. Search match results of XRD spectrum showed Bi2Sr2CuOx (2201) and Ca2CuO3 (21) as an impurity phase with small intensity. Also, that is showing volume fraction from 85 to 92% and orthorombic value for all samples from 5 to 7%. The effect of RE dopants resulted a shift angle 2θ and changes in the volume of the unit cells of each sample. The value of the unit cell volume of the largest to smallest is BS(CN)CO, BS(CNG)CO, BS(CNEG)CO, BS(CNE)CO, BS(CG)CO, BS(CEG)CO and BS(CE)CO. Measurement with FTIR showed the bending vibration absorption by CO3 2- in the wavelength range between 1500 and 1520 cm-1, vibration of M-O between 420 and 650 cm-1, the complex formation of BSCCO in the wavelength range between 1690 and 1700 cm-1. Measurement with SEM showed rod shape with particle size in hundreds nanometer.

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.

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.

Metastable and equilibrium phase formation in sputter-deposited Ti/Al multilayer thin films

NASA Astrophysics Data System (ADS)

Lucadamo, G.; Barmak, K.; Lavoie, C.; Cabral, C., Jr.; Michaelsen, C.

2002-06-01

The sequence and kinetics of metastable and equilibrium phase formation in sputter deposited multilayer thin films was investigated by combining in situ synchrotron x-ray diffraction (XRD) with ex situ electron diffraction and differential scanning calorimetry (DSC). The sequence included both cubic and tetragonal modifications of the equilibrium TiAl3 crystal structure. Values for the formation activation energies of the various phases in the sequence were determined using the XRD and DSC data obtained here, as well as activation energy data reported in the literature.

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.

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.

Structural properties and electrochemistry of α-LiFeO2

NASA Astrophysics Data System (ADS)

Abdel-Ghany, A. E.; Mauger, A.; Groult, H.; Zaghib, K.; Julien, C. M.

2012-01-01

In this work, we study the physico-chemistry and electrochemistry of lithium ferrite synthesized by solid-state reaction. Characterization included X-ray diffraction (XRD), scanning electronic microscopy (SEM), Raman scattering (RS), Fourier transform infrared spectroscopy (FTIR), and SQUID magnetometry. XRD peaks gradually sharpen with increasing firing temperature; all the diffraction peaks can be indexed to the cubic α-LiFeO2 phase (Fm3m space group) with the refined cell parameter a = 4.155 Å. RS and FTIR spectra show the vibrational modes due to covalent Fe-O bonds and the Li-cage mode at low-frequency. The electrochemical properties of Li/LiFeO2 are revisited along with the post-mortem analysis of the positive electrode material using XRD and Raman experiments.

Ostwald ripening and interparticle-diffraction effects for illite crystals

USGS Publications Warehouse

Eberl, D.D.; Srodon, J.

1988-01-01

The Warren-Averbach method, an X-ray diffraction (XRD) method used to measure mean particle thickness and particle-thickness distribution, is used to restudy sericite from the Silverton caldera. Apparent particle-thickness distributions indicate that the clays may have undergone Ostwald ripening and that this process has modified the K-Ar ages of the samples. The mechanism of Ostwald ripening can account for many of the features found for the hydrothermal alteration of illite. Expandabilities measured by the XRD peak-position method for illite/smectites (I/S) from various locations are smaller than expandabilities measured by transmission electron microscopy (TEM) and by the Warren-Averbach (W-A) method. This disparity is interpreted as being related to the presence of nonswelling basal surfaces that form the ends of stacks of illite particles (short-stack effect), stacks that, according to the theory of interparticle diffraction, diffract as coherent X-ray scattering domains. -from Authors

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.

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.

Structure and optical properties of 2D layered MoS2 crystals implemented with novel friction induced crystal growth

NASA Astrophysics Data System (ADS)

Tanabe, Tadao; Ito, Takafumi; Oyama, Yutaka

2018-03-01

We used X-ray diffraction, and Raman and photoluminescence (PL) spectroscopies to examine the structure and optical properties of molybdenum disulfide (MoS2) crystals grown by friction at the interface between two materials. MoS2 is produced chemically from molybdenum dithiocarbamates (MoDTC) in synthetic oil under sliding friction conditions. The X-ray diffraction (XRD) patterns indicate that the structure of the MoS2 is layered with the c-axis perpendicular to the surface. The MoS2 layer was formed on stainless steel and germanium by friction at the interface between these materials and high carbon chromium bearing steel. The number of layers is estimated to be N (N > 6) from the distance between the Raman frequencies of the E12g and A1g modes. For MoS2 grown on stainless steel, exciton peak is observed in the PL spectrum at room temperature. These results show that this friction induced crystal growth method is viable for synthesizing atomic layers of MoS2 at solid surfaces.

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.

Structural characterization of titania by X-ray diffraction, photoacoustic, Raman spectroscopy and electron paramagnetic resonance spectroscopy.

PubMed

Kadam, R M; Rajeswari, B; Sengupta, Arijit; Achary, S N; Kshirsagar, R J; Natarajan, V

2015-02-25

A titania mineral (obtained from East coast, Orissa, India) was investigated by X-ray diffraction (XRD), photoacoustic spectroscopy (PAS), Raman and Electron Paramagnetic Resonance (EPR) studies. XRD studies indicated the presence of rutile (91%) and anatase (9%) phases in the mineral. Raman investigation supported this information. Both rutile and anatase phases have tetragonal structure (rutile: space group P4(2)/mnm, a=4.5946(1) Å, c=2.9597(1) Å, V=62.48(1) (Å)(3), Z=2; anatase: space group I4(1)/amd, 3.7848(2) Å, 9.5098(11) Å, V=136.22(2) (Å)(3), Z=4). The deconvoluted PAS spectrum showed nine peaks around 335, 370, 415,485, 555, 605, 659, 690,730 and 785 nm and according to the ligand field theory, these peaks were attributed to the presence of V(4+), Cr(3+), Mn(4+) and Fe(3+) species. EPR studies revealed the presence of transition metal ions V(4+)(d(1)), Cr(3+)(d(3)), Mn(4+)(d(3)) and Fe(3+)(d(5)) at Ti(4+) sites. The EPR spectra are characterized by very large crystal filed splitting (D term) and orthorhombic distortion term (E term) for multiple electron system (s>1) suggesting that the transition metal ions substitute the Ti(4+) in the lattice which is situated in distorted octahedral coordination of oxygen. The possible reasons for observation of unusually large D and E term in the EPR spectra of transition metal ions (S=3/2 and 5/2) are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Development and characterization of Mn2+-doped MgO nanoparticles by solution combustion synthesis

NASA Astrophysics Data System (ADS)

Basha, Md. Hussain; Gopal, N. O.; Rao, J. L.; Nagabhushana, H.; Nagabhushana, B. M.; Chakradhar, R. P. S.

2015-06-01

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å3. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn2+ ions with S=I=5/2.The observed g value and the hyperfine value reveal the ionic bonding between Mn2+ and its surroundings.

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

NASA Astrophysics Data System (ADS)

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

2014-12-01

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

Structural, optical and magnetic behaviour of nanocrystalline Volborthite

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

Arvind, Hemant K., E-mail: hemantarvind@gmail.com; Kumar, Sudhish, E-mail: skmlsu@gmail.com; Kalal, Sangeeta

2016-05-06

Nanocrystalline sample of Volborthite (Copper Pyrovanadate: Cu{sub 3}V{sub 2} (OH){sub 2}O{sub 7}.2H{sub 2}O) has been synthesized using wet chemical route and characterized by XRD, SEM, FTIR, UV-Vis-NIR spectroscopic and magnetization measurements. Room temperature X-ray diffraction analysis confirms the single phase monoclinic structure and nanocrystalline nature of Volborthite. The UV-Visible optical absorption spectrum displays two broad absorption peaks in the range of 200-350 nm and 400-1000 nm. The direct band gap is found to be E{sub g}= ∼2.74 eV. Bulk Volborthite was reported to be a natural frustrated antiferromagnet, however our nanocrystalline Volborthite display week ferromagnetic hysteresis loop with very small coercivity andmore » retentivity at room temperature.« less

Fabrication and characterization of nickel oxide nanoparticles/silicon NiO NPS/Si

NASA Astrophysics Data System (ADS)

Shuihab, Aliyah; Khalf, Surour

2018-05-01

In this study, (NiO) thin film which prepared by chemical method and deposited by drop casting technique on glass. The structural, optical and chemical analyses have been investigated. X-ray diffraction (XRD) measurements relieve that the (NiO) thin film was polycrystalline, cubic structure and there is no trace of the other material. UV-Vis measurements reveal that the energy gap of (NiO) thin film was found 1.8 eV. The Fourier Transform Infrared Spectroscopy (FTIR) spectrum of (NiO) thin film shows NiO nanoparticles had its IR peak of Ni-O stretching vibration and shifted to blue direction. Due to their quantum size effect and spherical nanostructures, the FTIR absorption of NiO nanoparticles is blue-shifted compared to that of the bulk form.

Influence of gamma irradiation on the surface morphology, XRD and thermophysical properties of silicide hexoboride

NASA Astrophysics Data System (ADS)

Mirzayev, Matlab N.; Mehdiyeva, Ravan N.; Garibov, Ramin G.; Ismayilova, Narmin A.; Jabarov, Sakin H.

2018-05-01

In this study, compounds of B6Si were irradiated using a 60Co gamma source that have an energy line of 1.25 MeV at the absorbed dose rates from 14.6 kGy to 194.4 kGy. Surface morphology images of the sample obtained by Scanning Electron Microscope (SEM) show that the crystal structure at a high absorbed doses (D ≥ 145.8kGy) starts to be destroyed. X-ray diffraction studies revealed that with increasing radiation absorption dose, the spectrum intensity of the sample was decreased 1.96 times compared with the initial value. Thermal properties were studied by Differential scanning calorimetry (DSC) method in the temperature range of 30-1000∘C.

Spectral downshifting in MBO3:Nd3+ (M=Y, La) phosphor

NASA Astrophysics Data System (ADS)

Omanwar, S. K.; Sawala, N. S.

2017-11-01

The spectral downshifting (DS) from ultra-violet (UV)/visible (VIS) light to near infra-red (NIR) radiation in Nd3+ doped YBO3 and LaBO3 phosphors is reported. The prepared materials were characterized by X-ray powder diffraction (XRD) and photoluminescence (PL) properties along with time-decay curves were studied which confirmed the spectral DS from VIS to NIR radiation. This can be employed to overcome the spectral mismatch of crystalline silicon (c-Si) solar cell with solar spectrum. The prepared Nd3+ doped as prepared phosphors provide NIR emission (1052 nm) at excitation of 586 nm where response of c-Si solar cell was optimum. Thus spectral modification by mentioned phosphor can be utilized to improve solar cells performance. Hence these phosphors have potential application for photovoltaic (PV) technology.

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

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...

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.

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.

Application of graphene oxide-poly (vinyl alcohol) polymer nanocomposite for memory devices

NASA Astrophysics Data System (ADS)

Kaushal, Jyoti; Kaur, Ravneet; Sharma, Jadab; Tripathi, S. K.

2018-05-01

Significant attention has been gained by polymer nanocomposites because of their possible demands in future electronic memory devices. In the present work, device based on Graphene Oxide (GO) and polyvinyl alcohol (PVA) has been made and examined for the memory device application. The prepared Graphene oxide (GO) and GO-PVA nanocomposite (NC) has been characterized by X-ray Diffraction (XRD). GO nanosheets show the diffraction peak at 2θ = 11.60° and the interlayer spacing of 0.761 nm. The XRD of GO-PVA NC shows the diffraction peak at 2θ =18.56°. The fabricated device shows bipolar switching behavior having ON/OFF current ratio ˜102. The Write-Read-Erase-Read (WRER) cycles test shows that the Al/GO-PVA/Ag device has good stability and repeatability.

Structural, Optical, and Electronic Characterization of Fe-Doped Alumina Nanoparticles

NASA Astrophysics Data System (ADS)

Heiba, Zein K.; Mohamed, Mohamed Bakr; Wahba, Adel Maher; Imam, N. G.

2018-01-01

The effects of iron doping on the structural, optical, and electronic properties of doped alumina have been studied. Single-phase iron-doped alumina Al2- x Fe x O3 ( x = 0.00 to 0.30) nanoparticles were synthesized via citrate-precursor method. Formation of single-phase hexagonal corundum structure with no other separate phases was demonstrated by x-ray diffraction (XRD) analysis and Fourier-transform infrared spectroscopy. The effects of iron doping on the α-Al2O3 structural parameters, viz. atomic coordinates, lattice parameters, crystallite size, and microstrain, were estimated from XRD data by applying the Rietveld profile fitting method. Transmission electron microscopy further confirmed the nanosize nature of the prepared samples with size ranging from 12 nm to 83 nm. The electronic band structure was investigated using density functional theory calculations to explain the decrease in the energy gap of Al2- x Fe x O3 as the amount of Fe was increased. The colored emission peaks in the visible region (blue, red, violet) of the electromagnetic spectrum obtained for the Fe-doped α-Al2O3 nanoparticles suggest their potential application as ceramic nanopigments.

Impact of copper substitution on the structural, ferroelectric and magnetic properties of tungsten bronze ceramics

NASA Astrophysics Data System (ADS)

Jindal, Shilpi; Devi, Sheela; Batoo, Khalid Mujasam; Kumar, Gagan; Vasishth, Ajay

2018-05-01

The copper substituted tungsten bronze ceramics with generic formula Ba5CaCuXTi2-xNb8O30(x = 0.0, 0.02, 0.04, 0.06 and 0.08) were successfully synthesized for the first time by solid state reaction method. X-ray diffraction (XRD), Scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX) were utilized to examine the different structural parameters and elemental compositions. XRD study depicted the single phase tetragonal structure having space group P4bm. The crystallite size was observed to be in the range 14.4-30.23 nm. The coexistent of ferroelectricity and magnetism was established by P-E and M-H measurements. The P-E loop study indicated an increase in the coercive field (11.805-23.736 kVcm-1) while the M-H study depicted adecrease in the magnetization (7.65 × 10-4-5.32 × 10-4 emu/g) with the incorporation of Cu2+ ions. Raman spectrum depicted that there is shift in the position of Raman modes with the substitution of copper which revealed one-mode behavior in the synthesized ceramics.

Structure and Luminescence Properties of New Green-Emitting Phosphor BaAl12O19:Tb

NASA Astrophysics Data System (ADS)

Xiao, Linjiu; He, Mingrui; Tian, Yanwen; Chen, Yongjie; Karaki, Tomoaki; Zhang, Liqing; Wang, Ning

2007-09-01

New green-emitting BaAl12O19:Tb phosphors were prepared by using the sol-gel method, and their structure and luminescence property were characterized by X-ray diffraction (XRD) analysis and fluorescence spectrometry. The results of XRD analysis revealed that a Ba1-xAl12O19:Tbx crystal structure was obtained at 1300 °C and Tb3+ ions substituted Ba2+ ions into the BaAl12O19 phase in the ion range x=0.005--0.05. The excitation peak of BaAl12O19:Tb was a wide band at approximately 240 nm, originating from the 4 f8-4 f75d1 transition of Tb3+. The emission spectrum consisted of eight emission peaks, originating from the 5D3-7Fi (i=6,5,4,3) and 5D4-7Fj ( j=6,5,4,3) transitions of Tb3+. The emission intensity of BaAl12O19:Tb phosphors at 543 nm was strongest when the phosphors were crystallized at 1300 °C for 2 h, and the content of Tb3+ was 2 mol %.

Ferroelectricity of strained SrTiO3 in lithium tetraborate glass-nanocomposite and glass-ceramic

NASA Astrophysics Data System (ADS)

Abdel-Khalek, E. K.; Mohamed, E. A.; Kashif, I.

2018-02-01

Glass-nanocomposite (GNCs) sample of the composition [90Li2B4O7-10SrTiO3] (mol %) was prepared by conventional melt quenching technique. The glassy phase and the amorphous nature of the GNCs sample were identified by Differential thermal analysis (DTA) and X-ray diffraction (XRD) studies, respectively. DTA of the GNCs exhibits sharp and broad exothermic peaks which represent the crystallization of Li2B4O7 and SrTiO3, respectively. The tetragonal Li2B4O7 and tetragonal SrTiO3 crystalline phases in glass-ceramic (GC) were identified by XRD and scanning electron microscopic (SEM). The strain tetragonal SrTiO3 phase in GNCs and GC has been confirmed by SEM. The values of crystallization activation energies (Ec1 and Ec2) for the first and second exothermic peaks are equal to 174 and 1452 kJ/mol, respectively. The Ti3+ ions in tetragonal distorted octahedral sites in GNCs were identified by optical transmission spectrum. GNCs and GC samples exhibit broad dielectric anomalies at 303 and 319 K because of strained SrTiO3 ferroelectric, respectively.

Low-cost and eco-friendly green synthesis of silver nanoparticles using Prunus japonica (Rosaceae) leaf extract and their antibacterial, antioxidant properties.

PubMed

Saravanakumar, Arthanari; Peng, Mei Mei; Ganesh, Mani; Jayaprakash, Jayabalan; Mohankumar, Murugan; Jang, Hyun Tae

2017-09-01

Low cost and eco-friendly green synthesis of silver nanoparticles (AgNPs) from silver nitrate (AgNO 3 ) using Prunus japonica leaves extract as reducing agent by a simple method at room temperature. The biosynthesized nanoparticles (NPs) were characterized by UV-Vis, tunneling electron microscopy (HR-TEM), scanning electron microscopy (SEM) coupled with X-ray energy dispersive spectrophotometer (EDAX), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). In UV-Vis spectroscopy results, the λ max was observed at 441 nm. The AgNPs synthesized were spherical, hexagonal, and irregular in shapes. The EDAX and XRD spectrum confirmed the presence of silver ions and crystalline nature of synthesized AgNPs. FTIR showed the functional groups such as C = O, N-H and C-N groups involved in the reduction of Ag +  to Ag. 2, 2-Diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay was performed and it showed the percentage inhibition in concentration-dependent manner. The synthesized AgNPs showed antibacterial activity against Escherichia coli, Proteus vulgaris, Staphylococcus aureus and Bacillus cereus to different extents and the higher activity was observed in Proteus vulgaris.

Study of benzotriazole as corrosion inhibitors of carbon steel in chloride solution containing hydrogen sulfide using electrochemical impedance spectroscopy (EIS)

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

Solehudin, Agus, E-mail: asolehudin@upi.edu; Nurdin, Isdiriayani

2014-03-24

Corrosion and inhibition studies on API 5LX65 carbon steel in chloride solution containing various concentrations of benzotriazole has been conducted at temperature of 70°C using Electrochemical Impedance Spectroscopy (EIS). Corroded carbon steel surface with and without inhibitor have been observed using X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Energy Dispersive Spectroscopy (EDS). The objectives of this research are to study the performance of benzotriazole as corrosion inhibitors. The experimental results of carbon steel corrosion in 3.5% NaCl solution containing 500 mg/l H{sub 2}S at different BTAH concentrations showed that corrosion rate of carbon steel decreases with increasing of BTAHmore » concentrations from 0 to 10 mmol/l. The inhibition efficiency of BTAH was found to be affected by its concentration. The optimum efficiency obtained of BTAH is 93% at concentration of 5 mmol/l. The result of XRD and EDS analysis reveal the iron sulfide (FeS) formation on corroded carbon steel surface without inhibitor. The EDS spectrum show the Nitrogen (N) bond on carbon steel surface inhibited by BTAH.« less

Biosynthesis and characterization of ZnO nanoparticles using the aqueous leaf extract of Imperata cylindrica L.

NASA Astrophysics Data System (ADS)

Saputra, I. S.; Yulizar, Y.

2017-04-01

ZnO nanoparticles (ZnO NPs) were biosynthesized.The growth was observed by a sol-gel method. ZnO were successfully formed through the reaction of zinc nitrate tetrahydrate Zn(NO3)2.4H2O precursor with aqueous leaf extract of Imperata cylindrica L (ICL). The structural and optical properties of ZnO were investigated. The as-synthesized products were characterized by UV-Visible (UV-Vis), UV diffuse reflectance spectroscopy (UV-DRS), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS). UV-Vis absorption data showed hydrolysis and characteristic of absorption peak at 300 nm of Zn(OH)2. UV-DRS confirmed that ZnO NPs has the indirect band gap at 3.13 eV. FTIR spectrum revealed the functional groups and indicated the presence of protein as the capping and stabilizing agent on the ZnO surface. Powder XRD studies indicated the formation of pure wurtzite hexagonal structure with particle size of 11.9 nm. The detailed morphological and structural characterizations revealed that the synthesized products were hexagonal nanochip.

Nanostructured CdO-NiO composite for multifunctional applications

NASA Astrophysics Data System (ADS)

Karthik, K.; Dhanuskodi, S.; Gobinath, C.; Prabukumar, S.; Sivaramakrishnan, S.

2018-01-01

In this study, CdO, NiO, and CdO-NiO nanocomposites (NCs) were synthesized and investigated by X-ray diffraction (XRD), scanning electron microscopy, and Fourier transform-infrared spectroscopy. XRD detected cubic structures with average crystallite sizes of 45 nm for CdO, 25 nm for NiO, and 30 nm for CdO-NiO. The band gap was estimated based on the ultraviolet-visible spectra. The near band edge emission was determined according to the luminescence spectrum. The antibacterial activities were tested against seven foodborne pathogens and the zones of inhibition with the Gram-negative bacterium Bacillus subtilis measured as 30 mm with CdO, 20 mm NiO, and 27 mm with CdO-NiO. The death of the bacterial cells was confirmed by confocal laser scanning microscope analysis. Cytotoxicity assays indicated the non-toxic effects of the NCs on normal healthy red blood cells. Furthermore, the in vitro cytotoxic effects of the CdO, NiO, and CdO-NiO NCs were examined using the human MCF-7 breast cancer cell line based on 3-[4,5-dimethylthiazol-2-yl]2,5-diphenyltetrazolium bromide assays with normal mouse embryonic fibroblasts (NH3T3) under identical conditions.

Effect of Cr doping on the structural, morphological, optical and electrical properties of indium tin oxide films

NASA Astrophysics Data System (ADS)

Mirzaee, Majid; Dolati, Abolghasem

2015-03-01

We report on the preparation and characterization of high-purity chromium (0.5-2.5 at.%)-doped indium tin oxide (ITO, In:Sn = 90:10) films deposited by sol-gel-mediated dip coating. The effects of different Cr-doping contents on structural, morphological, optical and electrical properties of the films were characterized by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV-Vis spectroscopy and four-point probe methods. XRD showed high phase purity cubic In2O3 and indicated a contraction of the lattice with Cr doping. FESEM micrographs show that grain size decreased with increasing the Cr-doping content. A method to determine chromium species in the sample was developed through the decomposition of the Cr 2 p XPS spectrum in Cr6+ and Cr3+ standard spectra. Optical and electrical studies revealed that optimum opto-electronic properties, including minimum sheet resistance of 4,300 Ω/Sq and an average optical transmittance of 85 % in the visible region with a band gap of 3.421 eV, were achieved for the films doped with Cr-doping content of 2 at.%.

Crystallized InBiS3 thin films with enhanced optoelectronic properties

NASA Astrophysics Data System (ADS)

Ali, N.; Hussain, Arshad; Ahmed, R.; Omar, M. Firdaus Bin; Sultan, M.; Fu, Yong Qing

2018-04-01

In this paper, a one-step thermal evaporation approach was used for fabrication of indium bismuth sulphide thin films, and the synergetic effects of co-evaporation of two sources (indium granules and Bi2S3 powders) were investigated using different characterization techniques. X-ray diffraction (XRD) analysis confirmed the crystalline orthorhombic structure for the post-annealed samples. Surface roughness and crystal size of the obtained film samples were increased with increasing annealing temperatures. Analysis using X-ray photoelectron spectroscopy showed the formation of the InBiS3 structure for the obtained films, which is also confirmed by the XRD results. The optical absorption coefficient value of the annealed samples was found to be in the order of 105 cm-1 in the visible region of the solar spectrum. The optical band gap energy and electrical resistivity of the fabricated samples were observed to decrease (from 2.2 to 1.3 eV, and from 0.3 to 0.01 Ω-cm, respectively) with increasing annealing temperatures (from 200 to 350 °C), indicating the suitability of the prepared InBiS3 thin films for solar cell applications.

Optical and superparamagnetic behavior of ZnFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Lal, Ganesh; Punia, Khushboo; Dolia, S. N.; Kumar, Sudhish

2018-05-01

Nanoparticles of zinc ferrite have been synthesized using a low temperature citrate sol-gel route and characterized by powder X-ray diffraction (XRD), Raman & UV-Vis-NIR spectroscopic and SQUID magnetometry measurements. Analysis of XRD pattern and Raman spectrum confirmed that the synthesized ZnFe2O4 sample crystallizes in single phase fcc spinel ferrite structure and the average particle size of nanoparticles is estimated to 24nm. Optical absorption study shows that maximum photo absorption take place in the visible band and peaking in UV band at 206nm and the band gap energy is estimated to Eg = 2.1eV. Zero Field Cooled (ZFC) and Field Cooled (FC) modes of magnetization down to 5K and in fields up to 20kOe shows that ZnFe2O4 nanoparticles exhibits superparamagnetism with high magneto-crystalline anisotropy and high magnetization. Small difference of 9K between the separation temperature TS=˜30K and blocking temperature TB= 21K are suggestive of the formation of ferromagnetic clusters and a narrow particle size distribution of the nanoparticles in superparamagnetic ZnFe2O4 nanoparticles.

Thermal behaviour and microanalysis of coal subbituminus

NASA Astrophysics Data System (ADS)

Heriyanti; Prendika, W.; Ashyar, R.; Sutrisno

2018-04-01

Differential scanning calorimetry (DSC) and X-ray powder diffraction (XRD) is used to study the thermal behaviour of sub-bituminous coal. The DSC experiment was performed in air atmosphere up to 125 °C at a heating rate of 25 °C min1. The DSC curve showed that the distinct transitional stages in the coal samples studied. Thermal heating temperature intervals, peak and dissociation energy of the coal samples were also determined. The XRD analysis was used to evaluate the diffraction pattern and crystal structure of the compounds in the coal sample at various temperatures (25-350 °C). The XRD analysis of various temperatures obtained compounds from the coal sample, dominated by quartz (SiO2) and corundum (Al2O3). The increase in temperature of the thermal treatment showed a better crystal formation.

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.

Structural, optical and magnetic investigation of Gd implanted CeO2 nanocrystals

NASA Astrophysics Data System (ADS)

Kaviyarasu, K.; Murmu, P. P.; Kennedy, J.; Thema, F. T.; Letsholathebe, Douglas; Kotsedi, L.; Maaza, M.

2017-10-01

Gadolinium implanted cerium oxide (Gd-CeO2) nanocomposites is an important candidate which have unique hexagonal structure and high K- dielectric constant. Gd-CeO2 nanoparticles were synthesized using hydrothermal method. X-ray diffraction (XRD) results showed that the peaks are consistent with pure phase cubic structure the XRD pattern also confirmed crystallinity and phase purity of the sample. Nanocrystals sizes were found to be up to 25 nm as revealed by XRD and SEM. It is suggested that Gd gives an affirmative effect on the ion influence behavior of Gd-CeO2. XRD patterns showed formation of new phases and SEM micrographs revealed hexagonal structure. Photoluminescence measurement (PL) reveals the systematic shift of the emission band towards lower wavelength thereby ascertaining the quantum confinement effect (QCE). The PL spectrum has wider broad peak ranging from 390 nm to 770 nm and a sharp one centered on at 451.30 nm which is in tune with Gd ions. In the Raman spectra showed intense band observed between 460 cm-1 and 470 cm-1 which is attributed to oxygen ions into CeO2. Room temperature ferromagnetism was observed in un-doped and Gd implanted and annealed CeO2 nanocrystals. In the recent studies, ceria based materials have been considered as one of the most promising electrolytes for reduced temperature SOFC (solid oxide fuel cell) system due to their high ionic conductivities allowing its use in stainless steel supported fuel cells. CeO2 having an optical bandgap 3.3 eV and n-type carrier density which make it a promising candidate for various technological application such as buffer layer on silicon on insulator devices.

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.

Biomimetics of silver nanoparticles by white rot fungus, Phaenerochaete chrysosporium.

PubMed

Vigneshwaran, Nadanathangam; Kathe, Arati A; Varadarajan, P V; Nachane, Rajan P; Balasubramanya, R H

2006-11-01

Extracellular synthesis of silver nanoparticles by a white rot fungus, Phaenerochaete chrysosporium is reported in this paper. Incubation of P. chrysosporium mycelium with silver nitrate solution produced silver nanoparticles in 24h. These silver nanoparticles were characterized by means of UV-vis spectroscopy, X-ray diffraction analysis, scanning electron microscopy, transmission electron microscopy, and photoluminescence spectroscopy. The synthesized silver nanoparticles absorbed maximum at 470 nm in the visible region. XRD spectrum of the silver nanoparticles confirmed the formation of metallic silver. The SEM characterization of the fungus reacted on the Ag+ indicated that the protein might be responsible for the stabilization of silver nanoparticles. This result was further supported by the TEM examination. Though shape variation was noticed, majority of the nanoparticles were found to be of pyramidal shape as seen under TEM. Photoluminescence spectrum showed a broad emission peak of silver nanoparticles at 423 nm when excited at 350 nm. Apart from eco-friendliness, fungus as bio-manufacturing unit will give us an added advantage in ease of handling when compared to other classes of microorganisms.

Surface enhanced Raman spectral studies of 2-bromo-1,4-naphthoquinone.

PubMed

Geetha, K; Umadevi, M; Sathe, G V; Vanelle, P; Terme, T; Khoumeri, O

2015-03-05

Silver nanoparticles have been synthesized by a simple and inexpensive solution combustion method with urea as fuel. The structural and morphology of the silver nanoparticles were investigated through X-ray powder diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersion Spectra (EDS) techniques. Structural and morphological results confirmed the nanocrystalline nature of the silver nanoparticles. Density Functional Theory (DFT) calculations were also performed to study the ground and excited state behavior of 2-bromo-1,4-naphthoquinone (2-BrNQ) and 2-BrNQ on silver nanoparticles. Surface-Enhanced Raman Scattering (SERS) spectra of 2-BrNQ adsorbed on silver nanoparticles were investigated. The CO, CH in-plane bending and CBr stretching modes were enhanced in SERS spectrum with respect to normal Raman spectrum. The spectral analysis reveals that the 2-BrNQ adsorbed 'stand-on' orientation on the silver surface. Density Functional Theory (DFT) calculations are also performed to study the vibrational features of 2-BrNQ molecule and 2-BrNQ molecule on silver surface. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and Use of [Cd(Detu)2(OOCCH3)2]·H2O as Single Molecule Precursor for Cds Nanoparticles

PubMed Central

Ajibade, Peter A.

2013-01-01

Substituted thiourea ligands are of interest because they possess various donor sites for metal ions and their application in separation of metal ions and as antimicrobial agents. The coordination of the sulfur donor atom led to interest in them as precursor for semiconductor nanoparticles. In this study, cadmium(II) complex of diethylthiourea was synthesized and characterized by elemental analysis, FTIR, and X-ray crystallography. Single crystal X-ray structure of the complex showed that the octahedral geometry around the Cd ion consists of two molecules of diethylthiourea acting as monodentate ligands and two chelating acetate ions. The thermal decomposition of the compound showed that it decomposed to give CdS. The compound was thermolysed in hexadecylamine (HDA) to prepare HDA-capped CdS nanoparticles. The absorption spectrum showed blue shifts in its absorption band edges which clearly indicated quantum confinement effect, and the emission spectrum showed characteristic band edge luminescence. The broad diffraction peaks of the XRD pattern showed the materials to be of the nanometric size. PMID:24294141

Biosynthesis of silver nanoparticles using Plectranthus amboinicus leaf extract and its antimicrobial activity.

PubMed

Ajitha, B; Ashok Kumar Reddy, Y; Sreedhara Reddy, P

2014-07-15

This study reports the simple green synthesis method for the preparation of silver nanoparticles (Ag NPs) using Plectranthus amboinicus leaf extract. The pathway of nanoparticles formation is by means of reduction of AgNO3 by leaf extract, which acts as both reducing and capping agents. Synthesized Ag NPs were subjected to different characterizations for studying the structural, chemical, morphological, optical and antimicrobial properties. The bright circular fringes in SAED pattern and diffraction peaks in XRD profile reveals high crystalline nature of biosynthesized Ag NPs. Morphological studies shows the formation of nearly spherical nanoparticles. FTIR spectrum confirms the existence of various functional groups of biomolecules capping the nanoparticles. UV-visible spectrum displays single SPR band at 428 nm indicating the absence of anisotropic particles. The synthesized Ag NPs exhibited better antimicrobial property towards gram negative Escherichia coli and towards tested Penicillium spp. than other tested microorganisms using disc diffusion method. Finally it has proven that the synthesized bio-inspired Ag NPs have potent antimicrobial effect. Copyright © 2014 Elsevier B.V. All rights reserved.

The Effect of Compaction Force on the Transition to Hydrate of Anhydrous Aripiprazole.

PubMed

Togo, Taichiro; Taniguchi, Toshiya; Nakata, Yoshitaka

2018-01-01

Aripiprazole (APZ) is used to treat schizophrenia and is administered as a tablet containing the anhydrous form of APZ. In this study, the effect of compaction force on the crystal form transition was investigated. The crystalline state was observed by X-ray diffraction (XRD). APZ Anhydrous Form II was compacted into tablets. The XRD intensity of anhydrous APZ became lower with higher compressive force. The degree of crystallinity decreased with the compaction force. The powder and the compacted tablets of anhydrous APZ were stored for one week under 60°C and 75% relative humidity. The powder showed no crystal form transition after storage. For the tablets, however, XRD peaks of APZ hydrate were observed after storage. The tablets compacted with higher force showed the higher XRD diffraction intensity of hydrate form. We concluded that the crystallinity reduction of APZ Anhydrous Form II by compaction caused and accelerated the transition to hydrate under high temperature and humidity conditions. In order to manufacture crystallographically stable tablets containing anhydrous APZ, it is important to prevent this crystallinity reduction during compaction.

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.

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.

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.

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.

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.

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.

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.

Sand sources and transport pathways for the San Francisco Bay coastal system, based on X-ray diffraction mineralogy

USGS Publications Warehouse

Hein, James R.; Mizell, Kira; Barnard, Patrick L.; Barnard, P.L.; Jaffee, B.E.; Schoellhamer, D.H.

2013-01-01

The mineralogical compositions of 119 samples collected from throughout the San Francisco Bay coastal system, including bayfloor and seafloor, area beaches, cliff outcrops, and major drainages, were determined using X-ray diffraction (XRD). Comparison of the mineral concentrations and application of statistical cluster analysis of XRD spectra allowed for the determination of provenances and transport pathways. The use of XRD mineral identifications provides semi-quantitative compositions needed for comparisons of beach and offshore sands with potential cliff and river sources, but the innovative cluster analysis of XRD diffraction spectra provides a unique visualization of how groups of samples within the San Francisco Bay coastal system are related so that sand-sized sediment transport pathways can be inferred. The main vector for sediment transport as defined by the XRD analysis is from San Francisco Bay to the outer coast, where the sand then accumulates on the ebb tidal delta and also moves alongshore. This mineralogical link defines a critical pathway because large volumes of sediment have been removed from the Bay over the last century via channel dredging, aggregate mining, and borrow pit mining, with comparable volumes of erosion from the ebb tidal delta over the same period, in addition to high rates of shoreline retreat along the adjacent, open-coast beaches. Therefore, while previously only a temporal relationship was established, the transport pathway defined by mineralogical and geochemical tracers support the link between anthropogenic activities in the Bay and widespread erosion outside the Bay. The XRD results also establish the regional and local importance of sediment derived from cliff erosion, as well as both proximal and distal fluvial sources. This research is an important contribution to a broader provenance study aimed at identifying the driving forces for widespread geomorphic change in a heavily urbanized coastal-estuarine system.

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

NASA Astrophysics Data System (ADS)

Du, Xiaoqing; Ye, Xiaoqiu; Ren, Qingbo

2017-12-01

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

Preparation of Composite Coating on AZ91D Magnesium Alloy by Silica Sol-Micro Oxidation

NASA Astrophysics Data System (ADS)

Shao, Zhongcai; Zhang, Feifei; Zhao, Ruiqiang; Shen, Xiaoyi

2016-03-01

Composite coating was prepared on AZ91D magnesium alloy with a new method which combined silica sol with micro-arc oxidation (MAO). The MAO coating was prepared on the basis of MAO solution, and then coated by sol-gel process. The composite coating was obtained after second MAO treatment. Scanning electron microscopy coupled with X-ray diffraction (XRD), energy spectrum analysis and electrochemical testing was applied to characterize the properties of MAO coating and composite coating. The experimental test results indicated that the Si element derived from SiO2 gel particle embedded into the MAO coating by second MAO treatment. The surface of composite coating became dense and the holes were smaller with silica sol sealing process. The corrosion resistance of composite coating was improved than the MAO coating.

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

PubMed

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

2016-11-07

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

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

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

DTIC Science & Technology

2010-12-01

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

Micro-X-ray diffraction assessment of shock stage in enstatite chondrites

NASA Astrophysics Data System (ADS)

Izawa, Matthew R. M.; Flemming, Roberta L.; Banerjee, Neil R.; McCausland, Philip J. A.

2011-05-01

A new method for assessing the shock stage of enstatite chondrites has been developed, using in situ micro-X-ray diffraction (μXRD) to measure the full width at half maximum (FWHMχ) of peak intensity distributed along the direction of the Debye rings, or chi angle (χ), corresponding to individual lattice reflections in two-dimensional XRD patterns. This μXRD technique differs from previous XRD shock characterization methods: it does not require single crystals or powders. In situ μXRD has been applied to polished thin sections and whole-rock meteorite samples. Three frequently observed orthoenstatite reflections were measured: (020), (610), and (131); these were selected as they did not overlap with diffraction lines from other phases. Enstatite chondrites are commonly fine grained, stained or darkened by weathering, shock-induced oxidation, and metal/sulfide inclusions; furthermore, most E chondrites have little olivine or plagioclase. These characteristics inhibit transmitted-light petrography, nevertheless, shock stages have been assigned MacAlpine Hills (MAC) 02837 (EL3) S3, Pecora Escarpment (PCA) 91020 (EL3) S5, MAC 02747 (EL4) S4, Thiel Mountains (TIL) 91714 (EL5) S2, Allan Hills (ALHA) 81021 (EL6) S2, Elephant Moraine (EET) 87746 (EH3) S3, Meteorite Hills (MET) 00783 (EH4) S4, EET 96135 (EH4-5) S2, Lewis Cliff (LEW) 88180 (EH5) S2, Queen Alexandra Range (QUE) 94204 (EH7) S2, LaPaz Icefield (LAP) 02225 (EH impact melt) S1; for the six with published shock stages, there is agreement with the published classification. FWHMχ plotted against petrographic shock stage demonstrates positive linear correlation. FWHMχ ranges corresponding to shock stages were assigned as follows: S1 < 0.7°, S2 = 0.7-1.2°, S3 = 1.2-2.3°, S4 = 2.3-3.5°, S5 > 3.5°, S6—not measured. Slabs of Abee (EH impact-melt breccia), and Northwest Africa (NWA) 2212 (EL6) were examined using μXRD alone; FWHMχ values place both in the S2 range, consistent with literature values. Micro-XRD analysis may be applicable to other shocked orthopyroxene-bearing rocks.

Application of Chlorophyll as Sensitizer for ZnS Photoanode in a Dye-Sensitized Solar Cell (DSSC)

NASA Astrophysics Data System (ADS)

Panda, B. B.; Mahapatra, P. K.; Ghosh, M. K.

2018-03-01

Zinc sulphide thin films have been synthesized by the electrodeposition method onto stainless steel substrate followed by dipping in acetone solution of chlorophyll in different time intervals to form photosensitised thin films. The photoelectrochemical parameters of the films have been studied using the photoelectrochemical cell having the cell configuration as follows {{photoelectrode/NaOH}}({1{{M}}} ) + {{S}}({1{{M}}} ) + {{N}}{{{a}}_2}{{S}}({1{{M}}} ){{/C}} ({{{graphite}}} ) . The photoelectrochemical characterization of the semiconductor film and dye-sensitised films has been carried out by measuring current-voltage (I-V) in the dark, power output and photoresponse. The study proves that the conductivity of both ZnS film and dye-sensitised ZnS films are n-type. The power output curves illustrate that open circuit voltage (V oc) and short circuit current (I sc) increase from 0.210 V to 0.312 V and from 0.297 mA to 0.533 mA, respectively. The fill factor initially decreases from 0.299 to 0.213 and then increases to 0.297 irregularly whereas efficiency increases from 0.047% to 0.123%. The UV-Vis absorbance spectrum of chlorophyll in acetone shows the presence of chlorophyll. The structural morphology of the ZnS thin films has also been analysed by using x-ray diffraction technique (XRD) and a scanning electron microscope (SEM). The XRD pattern shows the formation of nanocrystalline ZnS thin films of size 65 nm and the SEM images confirm the formation of fibrous film of ZnS. The energy diffraction analysis of x-ray confirms the formation of ZnS thin films.

Angle-resolved diffraction grating biosensor based on porous silicon

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

Lv, Changwu; Li, Peng; Jia, Zhenhong, E-mail: jzhh@xju.edu.cn

2016-03-07

In this study, an optical biosensor based on a porous silicon composite structure was fabricated using a simple method. This structure consists of a thin, porous silicon surface diffraction grating and a one-dimensional porous silicon photonic crystal. An angle-resolved diffraction efficiency spectrum was obtained by measuring the diffraction efficiency at a range of incident angles. The angle-resolved diffraction efficiency of the 2nd and 3rd orders was studied experimentally and theoretically. The device was sensitive to the change of refractive index in the presence of a biomolecule indicated by the shift of the diffraction efficiency spectrum. The sensitivity of this sensormore » was investigated through use of an 8 base pair antifreeze protein DNA hybridization. The shifts of the angle-resolved diffraction efficiency spectrum showed a relationship with the change of the refractive index, and the detection limit of the biosensor reached 41.7 nM. This optical device is highly sensitive, inexpensive, and simple to fabricate. Using shifts in diffraction efficiency spectrum to detect biological molecules has not yet been explored, so this study establishes a foundation for future work.« less

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...

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.

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.

Growth of high quality and large-sized Rb 0.3MoO 3 single crystals by molten salt electrolysis method

NASA Astrophysics Data System (ADS)

Wang, Junfeng; Xiong, Rui; Yi, Fan; Yin, Di; Ke, Manzhu; Li, Changzhen; Liu, Zhengyou; Shi, Jing

2005-05-01

High quality and large-sized Rb 0.3MoO 3 single crystals were synthesized by molten salt electrolysis method. X-ray diffraction (XRD) patterns and rocking curves, as well as the white beam Laue diffraction of X-ray images show the crystals grown by this method have high quality. The lattice constants evaluated from XRD patterns are a0=1.87 nm, b0=0.75 nm, c0=1.00 nm, β=118.83∘. The in situ selected area electron diffraction (SAED) patterns along the [101¯], [11¯1¯] and [103¯] zone axes at room temperature indicate that the Rb 0.3MoO 3 crystal possess perfect C-centered symmetry. Temperature dependence of the resistivity shows this compound undergoes a metal to semiconductor transition at 183 K.

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.

Structural and optical properties of lithium sodium borate glasses doped with Sm3+ ions

NASA Astrophysics Data System (ADS)

Dawaud, R. S. E. S.; Hashim, S.; Alajerami, Y. S. M.; Mhareb, M. H. A.; Maqableh, M. M.; Tamchek, N.

2014-07-01

Absorption and emission spectra of Sm3+ doped lithium sodium borate (LNB) have been reported. The samples were prepared by the melt-quenching technique and characterized by X-ray diffraction (XRD), diffraction thermal analysis (DTA), Fourier transforms infrared (FTIR) spectroscopy and field emission scanning electron microscopy (FESEM). From the thermo-grams spectrum, glass transition (Tg), crystallization (Tc) and melting temperatures (Tm) have been evaluated. Direct and indirect optical band gaps have been calculated based on the glasses UV absorption spectra. These glasses have shown strong nine absorption bands with hypersensitive transition at 1221 nm (6H5/2→4H3/2) and five emission bands for the transition at 4I7/2→6H13/2 (green color), 4I7/2→6H7/2 (orange color), 4I7/2→6H9/2 (orange color), 4I7/2→6H11/2 (red color) and 4I7/2→6H13/2 (red color) with performing an excitation of 400 nm. The oscillator strengths, refractive index, ions concentration, polaron radius and other parameters have been calculated for each dopant.

Green synthesis of Silver and Gold Nanoparticles for Enhanced catalytic and bactericidal activity

NASA Astrophysics Data System (ADS)

Naraginti, S.; Tiwari, N.; Sivakumar, A.

2017-11-01

A rapid one step green synthetic method using kiwi fruit extract was employed for preparation of silver and gold nanoparticles. The synthesized nanoparticles were successfully used as green catalysts for the reduction of 4-nitrophenol (4-NP) and methylene blue (MB). They also exhibited excellent antimicrobial activity against clinically isolated Pseudomonas aeruginosa (P.aeruginosa) and Staphylococcus aureus (S.aureus). It was noticed that with increase in concentration of the aqueous silver and gold solutions, particle size of the Ag and Au NPS showed increase as evidenced from UV-Visible spectroscopy and TEM micrograph. The method employed for the synthesis required only a few minutes for more than 90% formation of nanoparticles when the temperature was raised to 80°C. It was also noticed that the catalytic activity of nanoparticles depends upon the size of the particles. These nanoparticles were observed to be crystalline from the clear lattice fringes in the transmission electron microscopic (TEM) images, bright circular spots in the selected area electron diffraction (SAED) pattern and peaks in the X-ray diffraction (XRD) pattern. The Fourier-transform infrared (FTIR) spectrum indicated the presence of different functional groups in the biomolecule capping the nanoparticles.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Zn(II)-PEG 300 globules as soft template for the synthesis of hexagonal ZnO micronuts by the hydrothermal reaction method.

PubMed

Shi, Xixi; Pan, Lingling; Chen, Shuoping; Xiao, Yong; Liu, Qiaoyun; Yuan, Liangjie; Sun, Jutang; Cai, Lintao

2009-05-19

Hexagonal ZnO micronuts (HZMNs) have been successfully synthesized with the assistance of poly(ethylene glycol) (PEG) 300 via a hydrothermal method. The structure and morphology of the HZMNs were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). An individual ZnO micronut is revealed as twinned crystals. Time-dependent investigation shows that the growth of HZMNs involves a dissolution-recrystallization process followed by Ostwald ripening, in which is the first formed solid ZnO particles dissolve and transform to HZMNs with hollow structure. PEG 300 has been found to play a crucial role in the growth of this unique hollow structure. TEM observations show that the PEG chains aggregate to globules in water, which then have interaction with the dissolved zinc species to form the globules in a coiled state under hydrothermal conditions. These Zn(II)-PEG 300 globules act as soft template for the growth of HZMNs, and the possible growth mechanism is proposed. The room-temperature photoluminescence (PL) spectrum shows red emission around 612 nm with a full width at half-maximum (fwhm) only about 13 nm.

Enhancement of efficiency by embedding ZnS and Mn-doped ZnS nanoparticles in P3HT:PCBM hybrid solid state solar cells

NASA Astrophysics Data System (ADS)

Jabeen, Uzma; Adhikari, Tham; Shah, Syed Mujtaba; Nunzi, Jean-Michel; Badshah, Amin; Ahmad, Iqbal

2017-06-01

Zinc sulphide (ZnS) and Mn-doped ZnS nanoparticles were synthesized by wet chemical method. The synthesized nanoparticles were characterized by UV-visible, fluorescence, X-ray diffraction (XRD), fourier transform infra-red (FTIR) spectrometer, field emission scanning electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). Scanning electron microscope (SEM) was used to find particle size while chemical composition of the synthesized materials was investigated by EDAX. UV-visible absorption spectrum of Mn-doped ZnS was slightly shifted to lower wavelength with respect to the un-doped zinc sulphide with decrease in the size of nanoparticles. Consequently, the band gap was tuned from 3.04 to 3.13 eV. The photoluminescence (PL) emission positioned at 597 nm was ascribed to 4T1 → 6A1 transition within the 3d shell of Mn2+. X-ray diffraction (XRD) analysis revealed that the synthesized nanomaterials existed in cubic crystalline state. The effect of embedding un-doped and doped ZnS nanoparticles in the active layer and changing the ratio of PCBM ([6, 6]-phenyl-C61-butyric acid methyl ester) to nanoparticles on the performance of hybrid solar cell was studied. The device with active layer consisting of poly(3-hexylthiophene) (P3HT), [6, 6]-phenyl-C61-butyric acid methyl ester (PCBM), and un-doped ZnS nanoparticles combined in the ratio of (1:0.5:0.5) attained an efficiency of 2.42% which was found 71% higher than the reference device under the same conditions but not containing nanoparticles. Replacing ZnS nanoparticles with Mn-doped ZnS had a little effect on the enhancement of efficiency. The packing behavior and morphology of blend of nanoparticles with P3HT:PCBM were examined using atomic force microscope (AFM) and XRD. Contribution to the topical issue "Materials for Energy harvesting, conversion and storage II (ICOME 2016)", edited by Jean-Michel Nunzi, Rachid Bennacer and Mohammed El Ganaoui

Structure of chitosan thermosensitive gels containing graphene oxide

NASA Astrophysics Data System (ADS)

Tylman, Michał; Pieklarz, Katarzyna; Owczarz, Piotr; Maniukiewicz, Waldemar; Modrzejewska, Zofia

2018-06-01

The supramolecular hydrogels of chitosan and graphene oxide (GO) have been prepared at temperature of the human body, by controlling the concentration of GO and ratio of chitosan to GO. During the preparation of gels the sodium β-glycerophosphate (Na-β-GP) was used as a neutralizing agent. The structure of obtained gels was determined on the basis of FTIR spectra and XRD diffraction patterns. The results of structural studies have been referenced to gels without graphene oxide. It was found that the gels crystalline structure after the addition of GO does not change. The XRD diffraction patterns are characterized by a number of peaks associated with precipitated NaCl during drying and presence of sodium β-glycerophosphate.

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.

Ion beam modification of the structure and properties of hexagonal boron nitride: An infrared and X-ray diffraction study

NASA Astrophysics Data System (ADS)

Aradi, E.; Naidoo, S. R.; Billing, D. G.; Wamwangi, D.; Motochi, I.; Derry, T. E.

2014-07-01

The vibrational mode for the cubic symmetry of boron nitride (BN) has been produced by boron ion implantation of hexagonal boron nitride (h-BN). The optimum fluence at 150 keV was found to be 5 × 1014 ions/cm2. The presence of the c-BN phase was inferred using glancing incidence XRD (GIXRD) and Fourier Transform Infrared Spectroscopy (FTIR). After implantation, Fourier Transform Infrared Spectroscopy indicated a peak at 1092 cm-1 which corresponds to the vibrational mode for nanocrystalline BN (nc-BN). The glancing angle XRD pattern after implantation exhibited c-BN diffraction peaks relative to the implantation depth of 0.4 μm.

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...

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.

Synthesis and photoluminescent and nonlinear optical properties of manganese doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Nazerdeylami, Somayeh; Saievar-Iranizad, Esmaiel; Dehghani, Zahra; Molaei, Mehdi

2011-01-01

In this work we synthesized ZnS:Mn 2+ nanoparticles by chemical method using PVP (polyvinylpyrrolidone) as a capping agent in aqueous solution. The structure and optical properties of the resultant product were characterized using UV-vis optical spectroscopy, X-ray diffraction (XRD), photoluminescence (PL) and z-scan techniques. UV-vis spectra for all samples showed an excitonic peak at around 292 nm, indicating that concentration of Mn 2+ ions does not alter the band gap of nanoparticles. XRD patterns showed that the ZnS:Mn 2+ nanoparticles have zinc blende structure with the average crystalline sizes of about 2 nm. The room temperature photoluminescence (PL) spectrum of ZnS:Mn 2+ exhibited an orange-red emission at 594 nm due to the 4T 1- 6A 1 transition in Mn 2+. The PL intensity increased with increase in the Mn 2+ ion concentration. The second-order nonlinear optical properties of nanoparticles were studied using a continuous-wave (CW) He-Ne laser by z-scan technique. The nonlinear refractive indices of nanoparticles were in the order of 10 -8 cm 2/W with negative sign and the nonlinear absorption indices of these nanoparticles were obtained to be about 10 -3 cm/W with positive sign.

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

Khader, S. Abdul, E-mail: khadersku@gmail.com; Parveez, Asiya; Sankarappa, T., E-mail: sankarappa@rediffmail.com

The Magneto-electric composites (x) Ni{sub 0.7}Co{sub 0.1}Cu{sub 0.2}Fe{sub 2}O{sub 4} + (1-x) BaTiO{sub 3} (x=10%, 20% and 30%) were synthesized by sintering mixtures of highly ferroelectric BaTiO{sub 3} (BT) and highly magneto-strictive component Ni{sub 0.7}Co{sub 0.1}Cu{sub 0.2}Fe{sub 2}O{sub 4} (NCCF). The presences of constituent phases in magneto-electric composites were probed by X-ray diffraction (XRD) studies. The peaks observed in the XRD spectrum indicated spinel cubic structure for NCCF ferrite phase and tetragonal perovskite structure for BT and, both spinel and pervoskite structures for synthesized ME composites. Surface morphology of the samples has been investigated using Field Emission Scanning Electron Microscopemore » (FESEM). Frequency and composition dependent dielectric properties of synthesized composites were measured from 100 Hz to 1 MHz at room temperature using Hioki LCR Hi-TESTER. The dielectric dispersion is observed at lower frequencies for the synthesized ME composites. The hysteresis behavior was studied to understand the magnetic ordering in the synthesized composites using a Vibrating Sample Magnetometer (VSM). It is observed that the values of saturation magnetization increases along with the ferrite content.« less

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

Khader, S. Abdul, E-mail: khadersku@gmail.com; Sankarappa, T., E-mail: sankarappa@rediffmail.com; Giridharan, N. V.

The Magneto-electric composites (x) Mg{sub 0.2}Cu{sub 0.3}Zn{sub 0.5}Fe{sub 2}O{sub 4} + (1-x) Ba{sub 0.8}Zr{sub 0.2}TiO{sub 3} (x=15%,30%,45%) were synthesized by sintering mixtures of highly ferroelectric Ba{sub 0.8}Zr{sub 0.2}TiO{sub 3} (BZT) and highly magneto-strictive component Mg{sub 0.2}Cu{sub 0.3}Zn{sub 0.5}Fe{sub 2}O{sub 4} (MCZF). The presences of two phases in magneto-electric composites were probed by X-ray diffraction (XRD) studies. The peaks observed in the XRD spectrum indicated spinel cubic structure for MCZF ferrite and tetragonal perovskite structure for BZT and, both spinel and pervoskite structures for synthesized composites. Surface morphology of the samples has been investigated using Field Emission Scanning Electron Microscope (FESEM).more » Frequency dependent dielectric properties of synthesized composites were measured from 100 Hz to 1 MHz at RT using HIOKI LCR HI-TESTER. The dielectric dispersion is observed at lower frequencies for the synthesized ME composites. The magnetic properties of synthesized composites were analyzed using a Vibrating Sample Magnetometer (VSM). It is observed that the values of saturation magnetization increases along with the ferrite content.« less

Green synthesis of silver nanoparticles using methanolic root extracts of Diospyros paniculata and their antimicrobial activities.

PubMed

Rao, N Hanumanta; N, Lakshmidevi; Pammi, S V N; Kollu, Pratap; S, Ganapaty; P, Lakshmi

2016-05-01

Since the discovery and subsequent widespread use of antibiotics, a variety of bacterial species of human and animal origin have developed numerous mechanisms that render bacteria resistant to some, and in certain cases to nearly all antibiotics, thereby limiting the treatment options and compromising effective therapy. In the present study, the green synthesis of nanoparticles is carried out by the reduction of silver acetate in the presence of crude methanolic root extracts of Diospyros paniculata, a member of family Ebenaceae. The UV-Vis absorption spectrum of the biologically reduced reaction mixture showed the surface plasmon peak at 428 nm, a characteristic peak of silver nanoparticles. X-ray diffraction (XRD) analysis confirmed the face-centered cubic crystalline structure of metallic silver. The average diameter of Ag NPs is about 17 nm from Transmission Electron Microscopy (TEM) which is in good agreement with the average crystallite size (19 nm) calculated from XRD analysis. Further the study has been extended to the antimicrobial activity against test pathogenic Gram (+), Gram (-) bacterial and fungal strains. The biologically synthesized silver nanoparticles showed promising activity against all the tested pathogenic strains and the activity has been enhanced with the increased dose levels. Copyright © 2016 Elsevier B.V. All rights reserved.

Green way genesis of silver nanoparticles using multiple fruit peels waste and its antimicrobial, anti-oxidant and anti-tumor cell line studies

NASA Astrophysics Data System (ADS)

Naganathan, Kiruthika; Thirunavukkarasu, Somanathan

2017-04-01

Green synthesis of silver nanoparticles (SNP) opens a new path to kill and prevent various infectious diseases and also tumor. In this study, we have synthesized silver nanoparticles using multiple fruit peel waste (pomegranate, orange, banana and apple (POBA)). The primarily nanoparticles formation has been confirmed by the color change. The synthesized SNP were analyzed by various physicochemical techniques such as UV- Visible spectroscopy, x-ray diffraction (XRD), fourier transform infra red (FT-IR) spectroscopy and transmission electron microscope (TEM). The formation of SNP was confirmed by its absorbance peak observed at 430 nm in UV-Visible spectrum. Further, the obtained SNP were identified by XRD and TEM, respectively to know the crystalline nature and size and shape of the particles. The activities of SNP were checked with human pathogens (Salmonella, E.coli and Pseudomonas), plant pathogen (Fusarium) and marine pathogen (Aeromonas hydrophila) and also studied the scavenging effect and anticancer properties against MCF-7 cell lines. This studies proves that the SNP prepared from fruit waste peel extract approach appears extremely fast, cost efficient, eco-friendly and alternative for conventional methods of SNP synthesis to promote the usage of these nanoparticles in medicinal application.

Chamomile flower extract-directed CuO nanoparticle formation for its antioxidant and DNA cleavage properties.

PubMed

Duman, Fatih; Ocsoy, Ismail; Kup, Fatma Ozturk

2016-03-01

In this study, we report the synthesis of copper oxide nanoparticles (CuO NPs) using a medicinal plant (Matricaria chamomilla) flower extract as both reducing and capping agent and investigate their antioxidant activity and interaction with plasmid DNA (pBR322).The CuO NPs were characterized using Uv-Vis spectroscopy, FT-IR (Fourier transform infrared spectroscopy), DLS (dynamic light scattering), XRD (X-ray diffraction), EDX (energy-dispersive X-ray) spectroscopy and SEM (scanning electron microscopy). The CuO NPs exhibited nearly mono-distributed and spherical shapes with diameters of 140 nm size. UV-Vis absorption spectrum of CuO NPs gave a broad peak around 285 and 320 nm. The existence of functional groups on the surface of CuO NPs was characterized with FT-IR analysis. XRD pattern showed that the NPs are in the form of a face-centered cubic crystal. Zeta potential value was measured as -20 mV due to the presence of negatively charged functional groups in plant extract. Additionally, we demonstrated concentration-dependent antioxidant activity of CuO NPs and their interaction with plasmid DNA. We assumed that the CuO NPs both cleave and break DNA double helix structure. Copyright © 2015 Elsevier B.V. All rights reserved.

Structural, dielectric and magnetic studies of (x) Ni0.7Co0.1Cu0.2Fe2O4 + (1-x) BaTiO3 magnetoelectric composites

NASA Astrophysics Data System (ADS)

Khader, S. Abdul; Parveez, Asiya; Giridharan, N. V.; Sankarappa, T.

2016-05-01

The Magneto-electric composites (x) Ni0.7Co0.1Cu0.2Fe2O4 + (1-x) BaTiO3 (x=10%, 20% and 30%) were synthesized by sintering mixtures of highly ferroelectric BaTiO3 (BT) and highly magneto-strictive component Ni0.7Co0.1Cu0.2Fe2O4 (NCCF). The presences of constituent phases in magneto-electric composites were probed by X-ray diffraction (XRD) studies. The peaks observed in the XRD spectrum indicated spinel cubic structure for NCCF ferrite phase and tetragonal perovskite structure for BT and, both spinel and pervoskite structures for synthesized ME composites. Surface morphology of the samples has been investigated using Field Emission Scanning Electron Microscope (FESEM). Frequency and composition dependent dielectric properties of synthesized composites were measured from 100 Hz to 1 MHz at room temperature using Hioki LCR Hi-TESTER. The dielectric dispersion is observed at lower frequencies for the synthesized ME composites. The hysteresis behavior was studied to understand the magnetic ordering in the synthesized composites using a Vibrating Sample Magnetometer (VSM). It is observed that the values of saturation magnetization increases along with the ferrite content.

Structural, dielectric and magnetic studies of (x) Mg0.2Cu0.3Zn0.5Fe2O4 + (1-x) Ba0.8Zr0.2TiO3 magnetoelectric composites

NASA Astrophysics Data System (ADS)

Khader, S. Abdul; Giridharan, N. V.; Chaudhuri, Arka; Sankarappa, T.

2016-05-01

The Magneto-electric composites (x) Mg0.2Cu0.3Zn0.5Fe2O4 + (1-x) Ba0.8Zr0.2TiO3 (x=15%,30%,45%) were synthesized by sintering mixtures of highly ferroelectric Ba0.8Zr0.2TiO3 (BZT) and highly magneto-strictive component Mg0.2Cu0.3Zn0.5Fe2O4 (MCZF). The presences of two phases in magneto-electric composites were probed by X-ray diffraction (XRD) studies. The peaks observed in the XRD spectrum indicated spinel cubic structure for MCZF ferrite and tetragonal perovskite structure for BZT and, both spinel and pervoskite structures for synthesized composites. Surface morphology of the samples has been investigated using Field Emission Scanning Electron Microscope (FESEM). Frequency dependent dielectric properties of synthesized composites were measured from 100 Hz to 1 MHz at RT using HIOKI LCR HI-TESTER. The dielectric dispersion is observed at lower frequencies for the synthesized ME composites. The magnetic properties of synthesized composites were analyzed using a Vibrating Sample Magnetometer (VSM). It is observed that the values of saturation magnetization increases along with the ferrite content.

Structural, dielectric and ferroelectric studies of BZT doped Mg0.2Cu0.3Zn0.5Fe2O4 magnetoelectric composites

NASA Astrophysics Data System (ADS)

Khader, S. Abdul; Parveez, Asiya; Giridharan, N. V.; Sankarappa, T.

2018-05-01

The composites of ferrite-ferroelectric system (x) Mg0.2Cu0.3Zn0.5Fe2O4+ (1-x) Ba0.8Zr0.2TiO3 (x=15%, 30%, 45%) were synthesized by sintering mixtures of ferroelectric Ba0.8Zr0.2TiO3 (BZT) and ferrite component Mg0.2Cu0.3Zn0.5Fe2O4 (MCZF). The presences of two phases in magneto-electric composites were probed by X-ray diffraction (XRD) studies. The peaks observed in the XRD spectrum indicated spinel cubic structure for MCZF ferrite and tetragonal perovskite structure for BZT and, both spinel and pervoskite structures for synthesized composites. Surface morphology of the samples has been investigated using Field Emission Scanning Electron Microscope (FESEM). Frequency dependent dielectric properties of synthesized composites were measured from 100 Hz to 1 MHz at RT using HIOKI LCR HI-TESTER. The dielectric dispersion is observed at lower frequencies for the synthesized ME composites. The ferroelectric properties of synthesized composites were analyzed using a Precision ferroelectric tester. It is observed that the composites exhibited ferroelectric hysteresis with wide loops indicating lossy nature of composites.

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…

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

2016-02-17

N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« 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.

Magnetic properties of Co-ferrite-doped hydroxyapatite nanoparticles having a core/shell structure

NASA Astrophysics Data System (ADS)

Petchsang, N.; Pon-On, W.; Hodak, J. H.; Tang, I. M.

2009-07-01

The magnetic properties of Co-ferrite-doped hydroxyapatite (HAP) nanoparticles of composition Ca 10-3xFe 2xCo x(PO 4) 6(OH) 2 (where x=0, 0.1, 0.2, 0.3, 0.4 and 0.5% mole) are studied. Transmission electron microscope micrograms show that the 90 nm size nanoparticles annealed at 1250 °C have a core/shell structure. Their electron diffraction patterns show that the shell is composed of the hydroxyapatite and the core is composed of the Co-ferrite, CoFe 2O 4. Electron spin resonance measurements indicate that the Co 2+ ions are being substituted into the Ca(1) sites in HAP lattice. X-ray diffraction studies show the formation of impurity phases as higher amounts of the Fe 3+/Co 2+ ions which are substituted into the HAP host matrix. The presence of two sextets (one for the A-site Fe 3+ and the other for the B-site Fe 3+) in the Mössbauer spectrum for all the doped samples clearly indicates that the CoFe 2O 4.cores are in the ferromagnetic state. Evidence of the impurity phases is seen in the appearance of doublet patterns in the Mössbauer spectrums for the heavier-doped ( x=0.4 and 0.5) specimens. The decrease in the saturation magnetizations and other magnetic properties of the nanoparticles at the higher doping levels is consistent with some of the Fe 3+ and Co 2+ which being used to form the CoO and Fe 2O 3 impurity phase seen in the XRD patterns.

Synthesis and luminescent properties of Sm3+ doped zinc aluminate phosphor

NASA Astrophysics Data System (ADS)

Mahajan, Rubby; Kumar, Sandeep; Prakash, Ram; Kumar, Vinay

2018-05-01

Zinc Aluminate (ZnAl2O4) is a well-known wide band gap oxide that belongs to a class of mixed-metal oxides knows as spinels (AB2O4) where A and B are divalent and trivalent cations. Herein, the structural and photoluminescence properties of Sm3+ ion doped with ZnAl2O4 phosphors are reported. The nanophosphors were synthesized via solution combustion synthesis route at temperature 570 °C. The synthesized samples were characterized by X-ray powder diffraction (XRD), Photoluminescence (PL) spectroscopy, and Ultraviolet-visible spectroscopy. The XRD pattern confirms the cubic phase of phosphor. The calculated lattice parameter were found as a = b = c = 8.0517Å and V = 521.85Å3. The crystallite size of the phosphor was calculated using the Debye-Scherrer formula and found to be ˜19 nm. The emission spectrum at excitation wavelength of 401 nm gave the emission peaks at 563 nm, 601 nm, 648 nm, 697 nm corresponding to the transitions 4G5/2→ 6H5/2, 4G5/2→6H7/2, 4G5/2→6H9/2, 4G5/2 → 6H11/2 of Sm3+ ions, respectively. The diffuse reflectance spectrum was used to calculate the band gap of material and found to be 5.12 eV. The CIE coordinates were found to be (x = 0.56, y = 0.40) that falls in the orange red region of the color gamut. The present phosphor may have potential applications as phosphor for near UV WLED for solid state lighting.

Rapid Extracellular Biosynthesis of Silver Nanoparticles by Cunninghamella phaeospora Culture Supernatant

PubMed Central

Ghareib, Mohamed; Tahon, Medhat Abu; Saif, Mona Mostafa; El-Sayed Abdallah, Wafaa

2016-01-01

The development of green approaches for the biosynthesis of silver nanoparticles (AgNPs) is of prime significance in the field of nanotechnology research. A fast and eco-friendly protocol for the biosynthesis of extracellular AgNPs using culture supernatant (CS) from the fungus Cunninghamella phaeospora was studied in this work. This CS was proved as a potential new source for the extracellular biosynthesis of AgNPs. The AgNPs were formed at 100 oC and pH 9 within four min of contact between CS and 1mM silver nitrate (AgNO3) solution. Nitrate reductase (NR) was confirmed to play a pivotal role in the biosynthesis of AgNPs. The enzyme expressed its highest activity at 80 oC and pH 9. At 100 oC the enzyme retained 70% of its original activity for one hour. The half-life (T1/2) of the enzyme activity was calculated to be 1.55 h confirming its thermostability. The produced AgNPs were characterized by UV-Vis spectroscopy, high resolution-transmission electron microscope (HR-TEM) and x-ray diffraction (XRD). These NPs showed an absorption peak at 415 nm in UV-Vis spectrum corresponding to the plasmon resonance of AgNPs. Transmission electron micrographs revealed the production of monodispersed spherical NPs with average particle size 14 nm. XRD spectrum of the NPs confirmed the formation of metallic crystalline silver. It was also suggested that the aromatic amino acids play a role in the biosynthesis process. The current research provided an insight on the green biosynthesis of AgNPs including some mechanistic aspects using a new mycogenic source. PMID:28243290

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.

Ultrafast visualization of crystallization and grain growth in shock-compressed SiO2

PubMed Central

Gleason, A. E.; Bolme, C. A.; Lee, H. J.; Nagler, B.; Galtier, E.; Milathianaki, D.; Hawreliak, J.; Kraus, R. G.; Eggert, J. H.; Fratanduono, D. E.; Collins, G. W.; Sandberg, R.; Yang, W.; Mao, W. L.

2015-01-01

Pressure- and temperature-induced phase transitions have been studied for more than a century but very little is known about the non-equilibrium processes by which the atoms rearrange. Shock compression generates a nearly instantaneous propagating high-pressure/temperature condition while in situ X-ray diffraction (XRD) probes the time-dependent atomic arrangement. Here we present in situ pump–probe XRD measurements on shock-compressed fused silica, revealing an amorphous to crystalline high-pressure stishovite phase transition. Using the size broadening of the diffraction peaks, the growth of nanocrystalline stishovite grains is resolved on the nanosecond timescale just after shock compression. At applied pressures above 18 GPa the nuclueation of stishovite appears to be kinetically limited to 1.4±0.4 ns. The functional form of this grain growth suggests homogeneous nucleation and attachment as the growth mechanism. These are the first observations of crystalline grain growth in the shock front between low- and high-pressure states via XRD. PMID:26337754

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.

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.

Role of Ga particulates on the structure and optical properties of Y3(Al,Ga)5O12:Tb thin films prepared by PLD

NASA Astrophysics Data System (ADS)

Yousif, A.; Duvenhage, M. M.; Ntwaeaborwa, O. M.; Swart, H. C.

2018-04-01

Y3(Al,Ga)5O12:Tb thin films (70 nm) have been prepared by pulsed laser deposition on a Si (100) substrate at the substrate temperature of 300 °C. The effect of annealing time on the structural, morphological and luminescence properties of Y3(Al,Ga)5O12:Tb thin films at 800 °C were studied. The crystal structure of the samples was studied by X- ray diffraction (XRD) and showed shifts in the peak positions to lower diffraction angles for the annealed film compared to the XRD peak positions of the commercial Y3(Al,Ga)5O12:Tb powder. A new excitation band different from the original Y3(Al,Ga)5O12:Tb powder was also observed for the annealed films. The shift in the XRD pattern and the new excitation band for the annealed film suggested that the films were enriched with Ga after annealing.

Ultrafast visualization of crystallization and grain growth in shock-compressed SiO 2

DOE PAGES

Gleason, A. E.; Bolme, C. A.; Lee, H. J.; ...

2015-09-04

Pressure- and temperature-induced phase transitions have been studied for more than a century but very little is known about the non-equilibrium processes by which the atoms rearrange. Shock compression generates a nearly instantaneous propagating high-pressure/temperature condition while in situ X-ray diffraction (XRD) probes the time-dependent atomic arrangement. Here we present in situ pump–probe XRD measurements on shock-compressed fused silica, revealing an amorphous to crystalline high-pressure stishovite phase transition. Using the size broadening of the diffraction peaks, the growth of nanocrystalline stishovite grains is resolved on the nanosecond timescale just after shock compression. At applied pressures above 18 GPa the nuclueationmore » of stishovite appears to be kinetically limited to 1.4 ± 0.4 ns. The functional form of this grain growth suggests homogeneous nucleation and attachment as the growth mechanism. As a result, these are the first observations of crystalline grain growth in the shock front between low- and high-pressure states via XRD.« less

Computer Simulations to Study Diffraction Effects of Stacking Faults in Beta-SiC: II. Experimental Verification. 2; Experimental Verification

NASA Technical Reports Server (NTRS)

Pujar, Vijay V.; Cawley, James D.; Levine, S. (Technical Monitor)

2000-01-01

Earlier results from computer simulation studies suggest a correlation between the spatial distribution of stacking errors in the Beta-SiC structure and features observed in X-ray diffraction patterns of the material. Reported here are experimental results obtained from two types of nominally Beta-SiC specimens, which yield distinct XRD data. These samples were analyzed using high resolution transmission electron microscopy (HRTEM) and the stacking error distribution was directly determined. The HRTEM results compare well to those deduced by matching the XRD data with simulated spectra, confirming the hypothesis that the XRD data is indicative not only of the presence and density of stacking errors, but also that it can yield information regarding their distribution. In addition, the stacking error population in both specimens is related to their synthesis conditions and it appears that it is similar to the relation developed by others to explain the formation of the corresponding polytypes.

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.

Water-repellent coatings prepared by modification of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Chakradhar, R. P. S.; Dinesh Kumar, V.

Superhydrophobic coatings with a static water contact angle (WCA) > 150° were prepared by modifying ZnO nanoparticles with stearic acid (ZnO@SA). ZnO nanoparticles of size ˜14 nm were prepared by solution combustion method. X-ray diffraction (XRD) studies reveal that as prepared ZnO has hexagonal wurtzite structure whereas the modified coatings convert to zinc stearate. Field emission scanning electron micrographs (FE-SEM) show the dual morphology of the coatings exhibiting both particles and flakes. The flakes are highly fluffy in nature with voids and nanopores. Fourier transformed infrared (FTIR) spectrum shows the stearate ion co-ordinates with Zn2+ in the bidentate form. The surface properties such as surface free energy (γp) and work of adhesion (W) of the unmodified and modified ZnO coatings have been evaluated. The electron paramagnetic resonance (EPR) spectroscopy reveals that surface defects play a major role in the wetting behavior.

Preparation of chitosan-ferulic acid conjugate: Structure characterization and in the application of pharmaceuticals.

PubMed

Li, Chen; Li, Jian-Bin

2017-12-01

A novel drug delivery system based on chitosan derivatives was prepared by introducting ferulic acid to chitosan adopting a free radical-induced grafting procedure. This paper used an ascorbic acid/hydrogen peroxide redox pair as radical initiator. The chitosan derivative was characterized by Fourier transformed infrared (FTIR), Ultraviolet-visible spectrum (UV), Differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Electron microscopic scanning (SEM). What is more, preparing microcapsules with the chitosan conjugate as wall material, the drug release propertie of chitosan conjugates were compared with that of a blank chitosan, which treated in the same conditions but in the absence of ferulic acid. The study clearly demonstrates that free radical-induced grafting procedure was an effective reaction methods and chitosan-ferulic acid is a potential functionalized carrier material for drug delivery. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of hollow ZnO microspheres by an integrated autoclave and pyrolysis process.

PubMed

Duan, Jinxia; Huang, Xintang; Wang, Enke; Ai, Hanhua

2006-03-28

Hollow zinc oxide microspheres have been synthesized from a micro ZnBr2·2H2O precursor obtained by an autoclave process in bromoform steam at 220 °C /2.5 MPa. Field-emission scanning electron microscropy (FE-SEM) and transmission electron microscopy (TEM) show that the products are about 1.0 µm single crystal spherical particles with hollow interiors, partly open surfaces and walls self-assembled by ZnO nanoparticles. X-ray diffraction (XRD) analysis shows that the as-prepared ZnO hollow spheres are of a hexagonal phase structure. A possible formation mechanism is suggested on the basis of the shape evolution of ZnO nanostructures observed by SEM and TEM. The room-temperature photoluminescence (PL) spectrum shows UV emission around 386 nm and weak green emission peaks indicating that there are few defects in the single crystal grains of the ZnO microspheres.

A Novel High-Density Phase and Amorphization of Nitrogen-Rich 1H-Tetrazole (CH2N4) under High Pressure

PubMed Central

Li, Wenbo; Huang, Xiaoli; Bao, Kuo; Zhao, Zhonglong; Huang, Yanping; Wang, Lu; Wu, Gang; Zhou, Bo; Duan, Defang; Li, Fangfei; Zhou, Qiang; Liu, Bingbing; Cui, Tian

2017-01-01

The high-pressure behaviors of nitrogen-rich 1H-tetrazole (CH2N4) have been investigated by in situ synchrotron X-ray diffraction (XRD) and Raman scattering up to 75 GPa. A first crystalline-to-crystalline phase transition is observed and identified above ~3 GPa with a large volume collapse (∼18% at 4.4 GPa) from phase I to phase II. The new phase II forms a dimer-like structure, belonging to P1 space group. Then, a crystalline-to-amorphous phase transition takes place over a large pressure range of 13.8 to 50 GPa, which is accompanied by an interphase region approaching paracrystalline state. When decompression from 75 GPa to ambient conditions, the final product keeps an irreversible amorphous state. Our ultraviolet (UV) absorption spectrum suggests the final product exhibits an increase in molecular conjugation. PMID:28218236

Characterization of konjac glucomannan-gelatin IPN physical hydrogel scaffold

NASA Astrophysics Data System (ADS)

Chen, Xiliang; Chen, Qinghua; Yan, Tingting; Liu, Jinkun

2017-06-01

A novel IPN hydrogel scaffold is prepared by freeze-drying method, in which konjac galactomannan (KGM) and gelatin are physically crosslinked respectively. This scaffold is thermostable, and the structure of this scaffold is analysed by scanning electron microscope, Fourier transform infrared spectrum, and X-ray diffraction method. The FT-IR results show that hydrogen bonds are formed between KGM and gelatin molecules, which hinder the formation of their respective crosslinking. This is consistent with the XRD results that the crystallinity gets lower in the IPN gels compared with pure gelatin and KGM gels. The morphologies of freeze-dried hydrogels are observed by SEM and the mechanical properties of the scaffolds are tested to analyse the relationship between the structures and properties. Although this novel IPN hydrogel is physical gel, it shows rubber-like performance as chemical gels. And it is nontoxic, so it can be used as the scaffold for cartilage tissue engineering that embedded in human bodies.

Green synthesis of nanosilver as a sensor for detection of hydrogen peroxide in water.

PubMed

Shukla, Vineet K; Yadav, Raghvendra S; Yadav, Poonam; Pandey, Avinash C

2012-04-30

Present "green" synthesis is an efficient, easy-going, fast, renewable, inexpensive, eco-friendly and non-toxic approach for nanosilver formation, which offers numerous benefits over physiochemical approaches. The X-ray diffraction (XRD) pattern suggests the formation and crystallinity of nanosilver. The average particle size of silver nanoparticles was 8.25±1.37 nm as confirmed by transmission electron microscopy (TEM). The UV-vis absorption spectrum shows a characteristic absorption peak of silver nanoparticles at 410 nm. FTIR confirms Azadirachtin as reducing and stabilizing agent for nanosilver formation. In addition, the nanosilver modified electrode (Ag/GC) exhibited an excellent electro-catalytic activity toward the reduction of hydrogen peroxide (H(2)O(2)). The produced nanosilver is stable and comparable in size. These silver nanoparticles show potential applications in the field of sensors, catalysis, fuel cells and nanodevices. Copyright © 2012 Elsevier B.V. All rights reserved.

Fabrication of Ta nanoparticles induced by nanosecond laser ablation in ethanol: the study of laser fluence effects

NASA Astrophysics Data System (ADS)

Azadi Kenari, Fariba; Moniri, Samira; Hantehzadeh, Mohammad Reza; Dorranian, Davoud; Ghoranneviss, Mahmood

2018-05-01

Tantalum nanoparticles (Ta NPs) were synthesized in ethanol solution by ablation with a 1064 nm Nd:YAG laser. Prepared NPs were investigated by UV-visible absorption spectroscopy, Transmission electron microscopy, X-ray diffraction and Photoluminescence measurement. The average sizes of NPs were calculated to be in the range of 12-18 nm. From the UV-visible studies, the plasmon peak position of Ta NPs was observed in the spectral range of 206-208 nm. The XRD spectra clearly showed the crystalline structure of NPs and various peaks of Ta and Ta2O5. Moreover, the UV region in the PL spectrum included the free exciton and the bound exciton emission correlated with the defect concentration. In fact, the laser ablation in the organic and inorganic solvents is a strong technique to obtain some NPs with particular structures, which are impossible to produce by conventional methods.

Growth and field emission properties of globe-like diamond microcrystalline-aggregate

NASA Astrophysics Data System (ADS)

Gao, Jin-hai; Zhang, Lan; Zhao, Limin; Hao, Haoshan

2009-02-01

The globe-like diamond microcrystalline-aggregates were fabricated by microwave plasma chemical vapor deposition (MPCVD) method. The ceramic with a Ti mental layer was used as substrate. The fabricated diamond was evaluated by Raman scattering spectroscopy, X-ray diffraction spectrum (XRD), and scanning electron microscope (SEM). The field emission properties were tested by using a diode structure in a vacuum. A phosphor-coated indium tin oxide (ITO) anode was used for observing and characterizing the field emission. It was found that the globe-like diamond microcrystalline-aggregates exhibited good electron emission properties. The turn-on field was only 0.55 V/μm, and emission current density as high as 11 mA/cm 2 was obtained under an applied field of 2.9 V/μm for the first operation. The growth mechanism and field emission properties of the globe-like diamond microcrystalline-aggregates are discussed relating to microstructure and electrical conductivity.

A Novel High-Density Phase and Amorphization of Nitrogen-Rich 1H-Tetrazole (CH2N4) under High Pressure.

PubMed

Li, Wenbo; Huang, Xiaoli; Bao, Kuo; Zhao, Zhonglong; Huang, Yanping; Wang, Lu; Wu, Gang; Zhou, Bo; Duan, Defang; Li, Fangfei; Zhou, Qiang; Liu, Bingbing; Cui, Tian

2017-02-20

The high-pressure behaviors of nitrogen-rich 1H-tetrazole (CH 2 N 4 ) have been investigated by in situ synchrotron X-ray diffraction (XRD) and Raman scattering up to 75 GPa. A first crystalline-to-crystalline phase transition is observed and identified above ~3 GPa with a large volume collapse (∼18% at 4.4 GPa) from phase I to phase II. The new phase II forms a dimer-like structure, belonging to P1 space group. Then, a crystalline-to-amorphous phase transition takes place over a large pressure range of 13.8 to 50 GPa, which is accompanied by an interphase region approaching paracrystalline state. When decompression from 75 GPa to ambient conditions, the final product keeps an irreversible amorphous state. Our ultraviolet (UV) absorption spectrum suggests the final product exhibits an increase in molecular conjugation.

Effect of fluorine doped TiO2 on the property of perovskite solar cell

NASA Astrophysics Data System (ADS)

Zhang, X. Q.; Wu, Y. P.; Huang, Y.; Zhou, Z. H.; Shen, S.

2017-03-01

Anatase TiO2 nanoparticles with different amounts of fluorine doping were synthesized by a hydrothermal method using hydrogen titanate nanotubes as a precursor and applied as mesoporous layer for preparing perovskite solar cell. The morphology and structures were characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD), meanwhile, the properties and performances were tested by photoluminescence spectrum (PL) and current density and voltage (J-V) curve. It was found that doping fluorine into TiO2 made the photoelectric conversion efficiency (PCE) of perovskite solar cell (PSC) to be improved. The best PCE of PSC based on a F-doped TiO2 was 13.06% and increased by 51% compared to an un-doped TiO2. The study provided a direction for the exploration of high performance electron transport layer of perovskite solar cell.

A New Look at the Structural and Magnetic Properties of Potassium Neptunate K2NpO4 Combining XRD, XANES Spectroscopy, and Low-Temperature Heat Capacity.

PubMed

Smith, Anna L; Colineau, Eric; Griveau, Jean-Christophe; Popa, Karin; Kauric, Guilhem; Martin, Philippe; Scheinost, Andreas C; Cheetham, Anthony K; Konings, Rudy J M

2017-05-15

The physicochemical properties of the potassium neptunate K 2 NpO 4 have been investigated in this work using X-ray diffraction, X-ray absorption near edge structure (XANES) spectroscopy at the Np-L 3 edge, and low-temperature heat capacity measurements. A Rietveld refinement of the crystal structure is reported for the first time. The Np(VI) valence state has been confirmed by the XANES data, and the absorption edge threshold of the XANES spectrum has been correlated to the Mössbauer isomer shift value reported in the literature. The standard entropy and heat capacity of K 2 NpO 4 have been derived at 298.15 K from the low-temperature heat capacity data. The latter suggest the existence of a magnetic ordering transition around 25.9 K, most probably of the ferromagnetic type.

Deposition and characterization of ZnSe nanocrystalline thin films

NASA Astrophysics Data System (ADS)

Temel, Sinan; Gökmen, F. Özge; Yaman, Elif; Nebi, Murat

2018-02-01

ZnSe nanocrystalline thin films were deposited at different deposition times by using the Chemical Bath Deposition (CBD) technique. Effects of deposition time on structural, morphological and optical properties of the obtained thin films were characterized. X-ray diffraction (XRD) analysis was used to study the structural properties of ZnSe nanocrystalline thin films. It was found that ZnSe thin films have a cubic structure with a preferentially orientation of (111). The calculated average grain size value was about 28-30 nm. The surface morphology of these films was studied by the Field Emission Scanning Electron Microscope (FESEM). The surfaces of the thin films were occurred from small stacks and nano-sized particles. The band gap values of the ZnSe nanocrystalline thin films were determined by UV-Visible absorption spectrum and the band gap values were found to be between 2.65-2.86 eV.

Preparation and characterization of graphene/CdS nanocomposites

NASA Astrophysics Data System (ADS)

Wu, Jili; Bai, Song; Shen, Xiaoping; Jiang, Lei

2010-11-01

Graphene-based nanocomposites are emerging as a new class of materials that hold promise for many applications. In this paper, we present a facile approach for the preparation of graphene/CdS nanocomposites through simple reflux processes, in which thiourea (CS(NH 2) 2) and thioacetamide (C 2H 5NS) act as a sulphide source, respectively. The samples were characterized by the X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectrum (FT-IR), ultraviolet-visible (UV-vis) spectroscopy and thermogravimetry analysis. It was shown that in the nanocomposites, the CdS nanoparticles were densely and uniformly deposited on the graphene sheets, and the sulphide source used has a great influence on the morphology, structure and property of the graphene/CdS nanocomposites. The good distribution of CdS nanoparticles on graphene sheets guarantees the efficient optoelectronic properties of graphene/CdS and would be promising for practical applications in future nanotechnology.

Green synthesis of colloidal copper oxide nanoparticles using Carica papaya and its application in photocatalytic dye degradation

NASA Astrophysics Data System (ADS)

Sankar, Renu; Manikandan, Perumal; Malarvizhi, Viswanathan; Fathima, Tajudeennasrin; Shivashangari, Kanchi Subramanian; Ravikumar, Vilwanathan

2014-03-01

Copper oxide (CuO) nanoparticles were synthesized by treating 5 mM cupric sulphate with Carica papaya leaves extract. The kinetics of the reaction was studied using UV-visible spectrophotometry. An intense surface Plasmon resonance between 250-300 nm in the UV-vis spectrum clearly reveals the formation of copper oxide nanoparticles. The results of scanning electron microscopy (SEM) and dynamic light scattering (DLS) exhibited that the green synthesized copper oxide nanoparticles are rod in shape and having a mean particle size of 140 nm, further negative zeta potential disclose its stability at -28.9 mV. The Fourier-transform infrared (FTIR) spectroscopy results examined the occurrence of bioactive functional groups required for the reduction of copper ions. X-ray diffraction (XRD) spectra confirmed the copper oxide nanoparticles crystalline nature. Furthermore, colloidal copper oxide nanoparticles effectively degrade the Coomassie brilliant blue R-250 dye beneath the sunlight.

Stabilization and enhanced energy gap by Mg doping in ɛ-phase Ga2O3 thin films

NASA Astrophysics Data System (ADS)

Bi, Xiaoyu; Wu, Zhenping; Huang, Yuanqi; Tang, Weihua

2018-02-01

Mg-doped Ga2O3 thin films with different doping concentrations were deposited on sapphire substrates using laser molecular beam epitaxy (L-MBE) technique. X-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS) and ultraviolet-visible (UV-vis) absorption spectrum were used to characterize the crystal structure and optical properties of the as-grown films. Compared to pure Ga2O3 thin film, the Mg-doped thin films have transformed from the most stable β-phase into ɛ-phase. The absorption edge shifted to about 205 nm and the optical bandgap increased to ˜ 6 eV. These properties reveal that Mg-doped Ga2O3 films may have potential applications in the field of deep ultraviolet optoelectronic devices, such as deep ultraviolet photodetectors, short wavelength light emitting devices and so on.

Development and characterization of Mn{sup 2+}-doped MgO nanoparticles by solution combustion synthesis

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

Basha, Md. Hussain; Gopal, N. O., E-mail: nogopal@yahoo.com; Rao, J. L.

2015-06-24

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å{sup 3}. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn{sup 2+} ions with S=I=5/2.The observedmore » g value and the hyperfine value reveal the ionic bonding between Mn{sup 2+} and its surroundings.« less

Biosynthesis of palladium nanoparticles using Saccharomyces cerevisiae extract and its photocatalytic degradation behaviour

NASA Astrophysics Data System (ADS)

Sriramulu, Mohana; Sumathi, Shanmugam

2018-06-01

In this article, we have discussed the biosynthesis of palladium nanoparticles (PdNPs) using aqueous Saccharomyces cerevisiae extract and its photocatalytic application. The biosynthesised PdNPs were characterised by UV-Vis spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX) and Atomic force microscopy (AFM). The formation of PdNPs was confirmed from the disappearance of the peak at 405 nm in the UV-Vis spectrum. Agglomerated and hexagonal shaped PdNPs were noted by SEM. FTIR was performed to identify the biomolecules responsible for the synthesis of PdNPs. Bioactive compounds in the yeast extract acted as secondary metabolites which facilitated the formation of PdNPs. The yeast synthesised PdNPs degraded 98% of direct blue 71 dye photochemically within 60 min under UV light.

Characterization of potassium bromide crystals grown in the aqueous solution of picric acid

NASA Astrophysics Data System (ADS)

Maheswari, J. Uma; Krishnan, C.; Kalyanaraman, S.; Selvarajan, P.

2016-12-01

Potassium bromide crystals were grown in the aqueous solution of picric acid by slow evaporation technique at room temperature. X-ray Diffraction (XRD) analysis ensures that the grown sample is in Fm3m space group and FCC structure. Energy Dispersive X-ray Spectroscopy (EDX) reveals the presence of elements in the title compound. UV-Vis-NIR spectrum reveals that the grown sample is a promising nonlinear optical (NLO) material. FTIR analysis confirms the functional groups present in the sample. The thermogravimetric (TG) and differential thermogravimetric (DTA) analyses ensure that the sample material is thermally stable up to 160 °C. The second harmonic efficiency of the sample is 1.3 times greater than that of standard KDP. The mechanical strength of the grown sample is estimated by Vickers microhardness tester. The electrical properties were investigated by impedance analysis and the results of various studies of the grown crystals are discussed.

Facile green synthesis of variable metallic gold nanoparticle using Padina gymnospora, a brown marine macroalga

NASA Astrophysics Data System (ADS)

Singh, M.; Kalaivani, R.; Manikandan, S.; Sangeetha, N.; Kumaraguru, A. K.

2013-04-01

The process of development of reliable and eco-friendly metallic nanoparticles is an important step in the field of nanotechnology. To achieve this, use of natural sources like biological systems becomes essential. In the present work, extracellular biosynthesis of gold nanoparticles using Padina gymnospora has been attempted and achieved rapid formation of gold nanoparticles in a short duration. The UV-vis spectrum of the aqueous medium containing gold ion showed peak at 527 nm corresponding to the plasmon absorbance of gold nanoparticles. Scanning electron microscopy showed the formation of well-dispersed gold nanoparticles. FTIR spectra of brown alga confirmed that hydroxyl groups present in the algal polysaccharides were involved in the gold bioreduction. AFM analysis showed the results of particle sizes (53-67 nm) and average height of the particle roughness (60.0 nm). X-ray diffraction (XRD) spectrum of the gold nanoparticles exhibited Bragg reflections corresponding to gold nanoparticles. This environment-friendly method of biological gold nanoparticle synthesis can be applied potentially in various products that directly come in contact with the human body, such as cosmetics, and foods and consumer goods, besides medical applications.

Morphology, structure and optical properties of hydrothermally synthesized CeO2/CdS nanocomposites

NASA Astrophysics Data System (ADS)

Mohanty, Biswajyoti; Nayak, J.

2018-04-01

CeO2/CdS nanocomposites were synthesized using a two-step hydrothermal technique. The effects of precursor concentration on the optical and structural properties of the CeO2/CdS nanoparticles were systematically studied. The morphology, composition and the structure of the CeO2/CdS nanocomposite powder were studied by scanning electron microscopy (SEM), energy dispersive X-ray spectrum analysis (EDXA) and X-ray diffraction (XRD), respectively. The optical properties of CeO2/CdS nanocomposites were studied by UV-vis absorption and photoluminescence (PL) spectroscopy. The optical band gaps of the CeO2/CdS nanopowders ranged from 2.34 eV to 2.39 eV as estimated from the UV-vis absorption. In the room temperature photoluminescence spectrum of CeO2/CdS nanopowder, a strong blue emission band was observed at 400 nm. Since the powder shows strong visible luminescence, it may be used as a blue phosphor in future. The original article published with this DOI was submitted in error. The correct article was inadvertently left out of the original submission. This has been rectified and the correct article was published online on 16 April 2018.

Oxygen vacancy effect on photoluminescence of KNb3O8 nanosheets

NASA Astrophysics Data System (ADS)

Li, Rui; Liu, Liying; Ming, Bangming; Ji, Yuhang; Wang, Ruzhi

2018-05-01

Fungus-like potassium niobate (KNb3O8) nanosheets have been synthesized on indium-doped tin oxide (ITO) glass substrates by a simple and environmental friendly two-step hydrothermal process. The prepared samples have been characterized by using X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), High Resolution Transmission Electron Microscope (HRTEM), Fourier Transform Infra-Red Spectroscopy (FTIR), Raman Spectroscopy and X-ray Photoelectron Spectroscopy (XPS). Furthermore, the photoluminescence (PL) of KNb3O8 nanosheets have been systematically studied. The results showed that the PL spectrum is between 300 and 645 nm with a 325 nm light excitation, which is divided into some sub-peaks. It is different from the perfect KNb3O8 nanosheets whose PL emission peaks located at near 433 nm. It should be originated from the effect of the oxygen (O) vacancies in the KNb3O8 nanosheets, which the PLs peaks can be found at about 490 nm and 530 nm by different position of O vacancy. The experimental results are in accordance with the first-principles calculations. Our results may present a feasible clue to estimate the defect position in KNb3O8 by the shape analysis of its spectrum of PLs.

Rapid synthesis of barium titanate microcubes using composite-hydroxides-mediated avenue

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

He, Xi; Ouyang, Jing, E-mail: jingouyang@csu.edu.cn; Jin, Jiao

2014-04-01

Highlights: • Barium titanate oxides microcubes can be synthesized within 1 min. • Composite-hydroxides-mediated strategy provided a possible large scale production. • BST obtained in the strategy showed fairly good crystallinity and tetragonality. - Abstract: This paper reports the rapid synthesis of barium titanate (BaTiO{sub 3}, BTO) microcubes via composite-hydroxides-mediated reaction within 1 min. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectrum (EDS) results confirmed both cubic and tetragonal lattices in the sample and the uniform microcubes with an average size of 1 μm. Ultraviolet–visible (UV–vis) spectrum indicated that the band gap of the BTO powder wasmore » 3.05 eV. Ferroelectric polarization vs. electric field (P–E) tests showed that the ferroelectric domains had formed in the as-synthesized BTO microcubes and sintered ceramics. BTO ceramics sintered at 1100 °C for 3 h showed fairly good tetragonality and possessed a maximum polarization of 0.21 μC/cm{sup 2}, indicating that the sintering temperature for the BTO powders prepared via this method was relatively low. The process and equipment reported herein provided a potential method for the rapid synthesis of titanate based perovskites.« less

Matching characteristics of different buffer layers with VO2 thin films

NASA Astrophysics Data System (ADS)

Yang, Kai; Zhang, Dongping; Liu, Yi; Guan, Tianrui; Qin, Xiaonan; Zhong, Aihua; Cai, Xingmin; Fan, Ping; Lv, Weizhong

2016-10-01

VO2 thin films were fabricated by reactive DC magnetron sputtering on different buffer layers of MgF2, Al2O3 and TiO2, respectively. The crystallinity and orientation relationship, thickness of VO2 thin films, atoms vibrational modes, optical and electrical property, surface morphology of films were characterized by X-ray diffraction, Raman scattering microscopy, step profiler, spectrophotometer, four-probe technique, and scanning electron microscopy, respectively. XRD results investigated that the films have preferential crystalline planes VO2 (011). The crystallinity of VO2 films grown on TiO2 buffer layers are superior to VO2 directly deposited on soda-lime glass. The Raman bands of the VO2 films correspond to an Ag symmetry mode of VO2 (M). The sample prepared on 100nm TiO2 buffer layer appears nanorods structure, and exhibits remarkable solar energy modulation ability as high as 5.82% in full spectrum and 23% in near infrared spectrum. Cross-sectional SEM image of the thin films samples indicate that MgF2 buffer layer has clear interface with VO2 layer. But there are serious interdiffusion phenomenons between Al2O3, TiO2 buffer layer with VO2 layer.

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…

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

Influence of the dopant concentration on structural, optical and photovoltaic properties of Cu-doped ZnS nanocrystals based bulk heterojunction hybrid solar cells

NASA Astrophysics Data System (ADS)

Jabeen, Uzma; Adhikari, Tham; Shah, Syed Mujtaba; Pathak, Dinesh; Wagner, Tomas; Nunzi, Jean-Michel

2017-06-01

Zinc sulphide (ZnS) and Cu-doped ZnS nanoparticles were synthesized by the wet chemical method. The nanoparticles were characterized by UV-visible, fluorescence, fourier transform infra-red (FTIR) spectrometry, X-ray diffraction (XRD), X-ray photoelectron spectrometry (XPS), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM). Scanning electron microscopy supplemented with EDAX was employed to observe the morphology and chemical composition of the un-doped and doped samples. A significant blue shift of the absorption band with respect to the un-doped zinc sulphide was sighted by increasing the Cu concentration in the doped sample with decreasing the size of nanoparticles. Consequently, the band gap was tuned from 3.13 to 3.49 eV due to quantum confinement. The green emission arises from the recombination between the shallow donor level (sulfur vacancy) and the t2 level of Cu2+. However, the fluorescence emission spectrum of the undoped ZnS nanoparticles was deconvoluted into two bands, which are centered at 419 and 468 nm. XRD analysis showed that the nanomaterials were in cubic crystalline state. XRD peaks show that there were no massive crystalline distortions in the crystal lattice when the Cu concentration (0.05-0.1 M) was increased in the ZnS lattice. However, in the case of Cu-doped samples (0.15-0.2 M), the XRD pattern showed an additional peak at 37° due to incomplete substitution occurring during the experimental reaction step. A comparative study of surfaces of undoped and Cu-doped ZnS nanoparticles were investigated using X-ray photoelectron spectroscopy (XPS). The synthesized nanomaterial in combination with poly(3-hexylthiophene) (P3HT) was used in the fabrication of solar cells. The devices with ZnS nanoparticles showed an efficiency of 0.31%. The overall power conversion efficiency of the solar cells at 0.1 M Cu content in doped ZnS nanoparticles was found to be 1.6 times higher than the reference device (P3HT:ZnS). Furthermore, atomic force microscopy and X-ray diffraction techniques were employed to study morphology and packing behavior of blends of nanocrystals and polymer respectively. Contribution to the topical issue "Materials for Energy harvesting, conversion and storage II (ICOME 2016)", edited by Jean-Michel Nunzi, Rachid Bennacer and Mohammed El Ganaoui

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.

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.

Statistical Nature of Atomic Disorder in Irradiated Crystals.

PubMed

Boulle, A; Debelle, A

2016-06-17

Atomic disorder in irradiated materials is investigated by means of x-ray diffraction, using cubic SiC single crystals as a model material. It is shown that, besides the determination of depth-resolved strain and damage profiles, x-ray diffraction can be efficiently used to determine the probability density function (PDF) of the atomic displacements within the crystal. This task is achieved by analyzing the diffraction-order dependence of the damage profiles. We thereby demonstrate that atomic displacements undergo Lévy flights, with a displacement PDF exhibiting heavy tails [with a tail index in the γ=0.73-0.37 range, i.e., far from the commonly assumed Gaussian case (γ=2)]. It is further demonstrated that these heavy tails are crucial to account for the amorphization kinetics in SiC. From the retrieved displacement PDFs we introduce a dimensionless parameter f_{D}^{XRD} to quantify the disordering. f_{D}^{XRD} is found to be consistent with both independent measurements using ion channeling and with molecular dynamics calculations.

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

PubMed

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

2012-04-01

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

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,

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

System and technique for characterizing fluids using ultrasonic diffraction grating spectroscopy

DOEpatents

Greenwood, Margaret S [Richland, WA

2008-07-08

A system for determining property of multiphase fluids based on ultrasonic diffraction grating spectroscopy includes a diffraction grating on a solid in contact with the fluid. An interrogation device delivers ultrasound through the solid and a captures a reflection spectrum from the diffraction grating. The reflection spectrum exhibits peaks whose relative size depends on the properties of the various phases of the multiphase fluid. For example, for particles in a liquid, the peaks exhibit dependence on the particle size and the particle volume fraction. Where the exact relationship is know know a priori, data from different peaks of the same reflection spectrum or data from the peaks of different spectra obtained from different diffraction gratings can be used to resolve the size and volume fraction.

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.

Identification of a deleterious phase in photocatalyst based on Cd1 - xZnxS/Zn(OH)2 by simulated XRD patterns.

PubMed

Cherepanova, Svetlana; Markovskaya, Dina; Kozlova, Ekaterina

2017-06-01

The X-ray diffraction (XRD) pattern of a deleterious phase in the photocatalyst based on Cd 1 - x Zn x S/Zn(OH) 2 contains two relatively intense asymmetric peaks with d-spacings of 2.72 and 1.56 Å. Very small diffraction peaks with interplanar distances of (d) ≃ 8.01, 5.40, 4.09, 3.15, 2.49 and 1.35 Å are characteristic of this phase but not always observed. To identify this phase, the XRD patterns for sheet-like hydroxide β-Zn(OH) 2 and sheet-like hydrozincite Zn 5 (CO 3 ) 2 (OH) 6 as well as for turbostratic hydrozincite were simulated. It is shown that the XRD pattern calculated on the basis of the last model gives the best correspondence with experimental data. Distances between layers in the turbostratically disordered hydrozincite fluctuate around d ≃ 8.01 Å. This average layer-to-layer distance is significantly higher than the interlayer distance 6.77 Å in the ordered Zn 5 (CO 3 ) 2 (OH) 6 probably due to a deficiency of CO 3 2- anions, excess OH - and the presence of water molecules in the interlayers. It is shown by variable-temperature XRD and thermogravimetric analysis (TGA) that the nanocrystalline turbostratic nonstoichiometric hydrozincite-like phase is quite thermostable. It decomposes into ZnO in air above 473 K.

In situ 2D diffraction as a tool to characterize ferroelectric and piezoelectric thin films

NASA Astrophysics Data System (ADS)

Khamidy, N. I.; Kovacova, V.; Bernasconi, A.; Le Rhun, G.; Vaxelaire, N.

2017-08-01

In this paper the application of 2D x-ray diffraction (XRD2) as a technique to characterize in situ during electrical cycling the properties of a ferroelectric and piezoelectric thin film is discussed. XRD2 is one type of XRD on which a 2D detector is used instead of a point detector. This technique enables simultaneous recording of many sample information in a much shorter time compared to conventional XRD. The discussion is focused especially on the data processing technique of the huge data acquired. The methodology to calculate an effective piezoelectric coefficient, analyze the phase and texture, and estimate the domain size and shape is described in this paper. This methodology is then applied to a lead zirconate titanate (PZT) thin film at the morphotropic phase boundary (MPB) composition (i.e. Pb[Zr0.52Ti0.48]O3) with a preferred orientation of (1 0 0). The in situ XRD2 characterization was conducted in the European synchrotron radiation facility (ESRF) in Grenoble, France. Since a high-energy beam with vertical resolution as small as 100 nm was used, a cross-sectional scan of the sample was performed over the entire thickness of the film. From these experimental results, a better understanding on the piezoelectricity phenomena in PZT thin film at MPB composition were achieved, providing original feedback between the elaboration processes and functional properties of the film.

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

NASA Astrophysics Data System (ADS)

Takahasi, Masamitu

2018-05-01

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

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 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.

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.

A study of angular spectrum and limited diffraction beams for calculation of field of array transducers

NASA Astrophysics Data System (ADS)

Cheng, Jiqi; Lu, Jian-Yu

2002-05-01

Angular spectrum is one of the most powerful tools for field calculation. It is based on linear system theory and the Fourier transform and is used for the calculation of propagating sound fields at different distances. In this report, the generalization and interpretation of the angular spectrum and its intrinsic relationship with limited diffraction beams are studied. With an angular spectrum, the field at the surface of a transducer is decomposed into limited diffractions beams. For an array transducer, a linear relationship between the quantized fields at the surface of elements of the array and the propagating field at any point in space can be established. For an annular array, the field is decomposed into limited diffraction Bessel beams [P. D. Fox and S. Holm, IEEE Trans. Ultrason. Ferroelectr. Freq. Control 49, 85-93 (2002)], while for a two-dimensional (2-D) array the field is decomposed into limited diffraction array beams [J-y. Lu and J. Cheng, J. Acoust. Soc. Am. 109, 2397-2398 (2001)]. The angular spectrum reveals the intrinsic link between these decompositions. [Work supported in part by Grant 5RO1 HL60301 from NIH.

Thermoluminescence, ESR and x-ray diffraction studies of CaSO4 : Dy phosphor subjected to post preparation high temperature thermal treatment

NASA Astrophysics Data System (ADS)

Bakshi, A. K.; Patwe, S. J.; Bhide, M. K.; Sanyal, B.; Natarajan, V.; Tyagi, A. K.; Kher, R. K.

2008-01-01

Thermoluminescence (TL), electron spin resonance (ESR) and x ray diffraction studies of CaSO4 : Dy phosphor subjected to post preparation high temperature treatment were carried out. Analysis of the TL glow curve indicated that the dosimetric glow peak at 240 °C reduces, whereas the low temperature satellite peak increases with the increase in the annealing temperature in the range 650-1000 °C. The influence of the annealing atmosphere on the TL glow curve structure was also observed. Reduction of the photoluminescence intensity of the annealed phosphor indicated that the environment of Dy3+ ions might have undergone some change due to high temperature treatment. Reduction in the ESR signal intensity corresponding to O_{3}^{-} and SO_{3}^{-} radicals was observed initially with the increase in the annealing temperaure; subsequently their intensity increased with temperature. Signals due to the SO_{4}^{-} radical vanished, when the phosphor was annealed beyond 800 °C. A signal corresponding to SH2- radicals was also observed in the ESR spectra for samples subjected to annealing in the temperature regime 800-1000 °C. XRD of the in situ annealed phosphor showed a change in the unit cell parameters. An endothermic peak at 860 °C in the DTA spectrum was observed.

Characterization and electron-energy-loss spectroscopy on NiV and NiMo superlattices

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

Mahmood, S.H.

1986-01-01

NiV superlattices with periods (A) ranging from 15 to 80 A, and NiMo superlattices with from 14 to 110 A were studied using X-ray Diffraction (XRD), Electron Diffraction (ED), Energy-Dispersive X-Ray (EDX) microanalysis, and Electron Energy Loss Spectroscopy (EELS). Both of these systems have sharp superlattice-to-amorphous (S-A) transitions at about empty set = 17A. Superlattices with empty set around the S-A boundary were found to have large local variations in the in-plane grain sizes. Except for a few isolated regions, the chemical composition of the samples were found to be uniform. In samples prepared at Argonne National Laboratory (ANL), mostmore » places studied with EELS showed changes in the EELS spectrum with decreasing empty set. An observed growth in a plasmon peak at approx. 10ev in both NiV and NiMo as empty set decreased down to 19 A is attributed to excitation of interface plasmons. Consistent with this attribution, the peak height shrank in the amorphous samples. The width of this peak is consistent with the theory. The sift in this peak down to 9 ev with decreasing empty set in NiMo is not understood.« less

A novel green synthesis of Fe3O4-Ag core shell recyclable nanoparticles using Vitis vinifera stem extract and its enhanced antibacterial performance

NASA Astrophysics Data System (ADS)

Venkateswarlu, Sada; Natesh Kumar, B.; Prathima, B.; Anitha, K.; Jyothi, N. V. V.

2015-01-01

We described a novel and eco-friendly method for preparing Fe3O4-Ag core shell nanoparticles (CSNPs) with high magnetism and potent antibacterial activity. The Fe3O4-Ag CSNPs were obtained using waste material of Vitis vinifera (grape) stem extract as the green solvent, reducing and capping agent. The result recorded from X-ray powder diffraction (XRD), UV-vis spectrum, energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR) supports the biosynthesis and characterization of Fe3O4-Ag CSNPs. From transmission electron microscopy (TEM) the size of the Fe3O4-Ag nanoparticles was measured below 50 nm; high-resolution TEM (HRTEM) indicates the core shell structure; and selected area electron diffraction (SAED) has revealed polycrystalline nature. Vibrating sample magnetometer (VSM) shows the ferromagnetic nature of Fe3O4-Ag CSNPs at room temperature with saturation magnetization of 15.74 emu/g. Further, these biogenic nanoparticles were highly hazardous to microorganisms. The antibacterial activity of biogenic Fe3O4-Ag CSNPs showed potent inhibitory activity against both Gram-positive and Gram-negative pathogens. These nanoparticles may also be reusable because of its excellent ferromagnetic property.

XRD measurement of mean thickness, thickness distribution and strain for illite and illite-smectite crystallites by the Bertaut-Warren-Averbach technique

USGS Publications Warehouse

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

1998-01-01

A modified version of the Bertaut-Warren-Averbach (BWA) technique (Bertaut 1949, 1950; Warren and Averbach 1950) has been developed to measure coherent scattering domain (CSD) sizes and strains in minerals by analysis of X-ray diffraction (XRD) data. This method is used to measure CSD thickness distributions for calculated and experimental XRD patterns of illites and illite-smectites (I-S). The method almost exactly recovers CSD thickness distributions for calculated illite XRD patterns. Natural I-S samples contain swelling layers that lead to nonperiodic structures in the c* direction and to XRD peaks that are broadened and made asymmetric by mixed layering. Therefore, these peaks cannot be analyzed by the BWA method. These difficulties are overcome by K-saturation and heating prior to X-ray analysis in order to form 10-Å periodic structures. BWA analysis yields the thickness distribution of mixed-layer crystals (coherently diffracting stacks of fundamental illite particles). For most I-S samples, CSD thickness distributions can be approximated by lognormal functions. Mixed-layer crystal mean thickness and expandability then can be used to calculate fundamental illite particle mean thickness. Analyses of the dehydrated, K-saturated samples indicate that basal XRD reflections are broadened by symmetrical strain that may be related to local variations in smectite interlayers caused by dehydration, and that the standard deviation of the strain increases regularly with expandability. The 001 and 002 reflections are affected only slightly by this strain and therefore are suited for CSD thickness analysis. Mean mixed-layer crystal thicknesses for dehydrated I-S measured by the BWA method are very close to those measured by an integral peak width method.

Synthesis and structural properties of Ba(1-x)LaxTiO3 perovskite nanoparticles fabricated by solvothermal synthesis route

NASA Astrophysics Data System (ADS)

Puli, Venkata Sreenivas; Adireddy, Shiva; Elupula, Ravinder; Molugu, Sudheer; Shipman, Josh; Chrisey, Douglas B.

2017-05-01

We report the successful synthesis and structural characterization of barium lanthanum titanate Ba(1-x)LaxTiO3 (x=0.003,0.006,0.010) nanoparticles. The colloidal nanoparticles were prepared with high yield by a solvothermal method at temperatures as low as 150°C for 24h. The as-prepared nanopowders were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. The XRD studies revealed pseudo-cubic crystalline structure, with no impurity phases at room temperature. However ferroelectric tetragonal modes were clearly observed using Raman spectroscopy measurements. From TEM measurements, uniformly sized BLT nanoparticles were observed. Selected area diffraction TEM images revealed polycrystalline perovskite ring patterns, identified as corresponding to the tetragonal phase.

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

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

NASA Astrophysics Data System (ADS)

Constantinescu, Serban Grigore; Udubasa, Sorin S.; Udubasa, Gheorghe; Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel

2012-03-01

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

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.

Novel synthesis and structural analysis of zinc oxide nanoparticles for the non enzymatic glucose biosensor.

PubMed

Dayakar, T; Venkateswara Rao, K; Bikshalu, K; Rajendar, V; Park, Si-Hyun

2017-06-01

A non-enzymatic glucose biosensor was developed by utilizing the zinc oxide nanoparticles (ZnO NPs) synthesized by a novel green method using the leaf extract of Ocimum tenuiflorum. The structural, optical and morphological properties of ZnO NPs characterized by means of X-ray diffraction (XRD), ultraviolet-visible (UV-vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy-dispersive X-ray (EDAX) spectroscopy, and transmission electron microscopy (TEM). The XRD analysis revealed that the ZnO NPs were crystalline and had a hexagonal wurtzite structure. The crystallite size measured by XRD was the same as that measured using SEM and TEM. The UV-vis absorption spectrum estimates the band gap of ZnO NPs present in the range of 2.82 to 3.45eV. The reduction and formation of ZnO NPs mainly due to the involvement of leaf extract bio-molecular compounds analyzed from the FTIR spectra. The SEM result confirms the morphology of the NPs responsible from the various concentration of leaf extract in the synthesis process. HRTEM analysis depicts the spherical structure of ZnO NPs. The synthesized NPs have the average size ranges from 10 to 20nm. The fabricated GCE/ZnO glucose sensor represents superior electro catalytic activity that has been observed for ZnO NPs with a reproducible sensitivity of 631.30μAmM -1 cm -2 , correlation coefficient of R=0.998, linear dynamic range from 1-8.6mM, low detection limit of 0.043μM (S/N=3) and response time<4s. Copyright © 2017 Elsevier B.V. All rights reserved.

Identification of Uranium Minerals in Natural U-Bearing Rocks Using Infrared Reflectance Spectroscopy.

PubMed

Beiswenger, Toya N; Gallagher, Neal B; Myers, Tanya L; Szecsody, James E; Tonkyn, Russell G; Su, Yin-Fong; Sweet, Lucas E; Lewallen, Tricia A; Johnson, Timothy J

2018-02-01

The identification of minerals, including uranium-bearing species, is often a labor-intensive process using X-ray diffraction (XRD), fluorescence, or other solid-phase or wet chemical techniques. While handheld XRD and fluorescence instruments can aid in field applications, handheld infrared (IR) reflectance spectrometers can now also be used in industrial or field environments, with rapid, nondestructive identification possible via analysis of the solid's reflectance spectrum providing information not found in other techniques. In this paper, we report the use of laboratory methods that measure the IR hemispherical reflectance of solids using an integrating sphere and have applied it to the identification of mineral mixtures (i.e., rocks), with widely varying percentages of uranium mineral content. We then apply classical least squares (CLS) and multivariate curve resolution (MCR) methods to better discriminate the minerals (along with two pure uranium chemicals U 3 O 8 and UO 2 ) against many common natural and anthropogenic background materials (e.g., silica sand, asphalt, calcite, K-feldspar) with good success. Ground truth as to mineral content was attained primarily by XRD. Identification is facile and specific, both for samples that are pure or are partially composed of uranium (e.g., boltwoodite, tyuyamunite, etc.) or non-uranium minerals. The characteristic IR bands generate unique (or class-specific) bands, typically arising from similar chemical moieties or functional groups in the minerals: uranyls, phosphates, silicates, etc. In some cases, the chemical groups that provide spectral discrimination in the longwave IR reflectance by generating upward-going (reststrahlen) bands can provide discrimination in the midwave and shortwave IR via downward-going absorption features, i.e., weaker overtone or combination bands arising from the same chemical moieties.

Facile green synthesis of silver nanoparticles using seed aqueous extract of Pistacia atlantica and its antibacterial activity

NASA Astrophysics Data System (ADS)

Sadeghi, Babak; Rostami, Amir; Momeni, S. S.

2015-01-01

In the present work, we describe the synthesis of silver nanoparticles (Ag-NPs) using seed aqueous extract of Pistacia atlantica (PA) and its antibacterial activity. UV-visible spectroscopy, X-ray diffraction (XRD), Fourier transform infra red spectroscopy (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray energy dispersive spectrophotometer (EDAX) were performed to ascertain the formation of Ag-NPs. It was observed that the growths of Ag-NPs are stopped within 35 min of reaction time. The synthesized Ag-NPs were characterized by a peak at 446 nm in the UV-visible spectrum. XRD confirmed the crystalline nature of the nanoparticles of 27 nm size. The XRD peaks at 38°, 44°, 64° and 77° can be indexed to the (1 1 1), (2 0 0), (2 2 0) and (3 1 1) Bragg's reflections of cubic structure of metallic silver, respectively. The FTIR result clearly showed that the extracts containing OH as a functional group act in capping the nanoparticles synthesis. Antibacterial activities of Ag-NPs were tested against the growth of Gram-positive (S. aureus) using SEM. The inhibition was observed in the Ag-NPs against S. aureus. The results suggest that the synthesized Ag-NPs act as an effective antibacterial agent. It is confirmed that Ag-NPs are capable of rendering high antibacterial efficacy and hence has a great potential in the preparation of used drugs against bacterial diseases. The scanning electron microscopy (SEM), indicated that, the most strains of S. aureus was damaged and extensively disappeared by addition of Ag-NPs. The results confirmed that the (PA) is a very good eco friendly and nontoxic source for the synthesis of Ag-NPs as compared to the conventional chemical/physical methods.

Facile green synthesis of silver nanoparticles using seed aqueous extract of Pistacia atlantica and its antibacterial activity.

PubMed

Sadeghi, Babak; Rostami, Amir; Momeni, S S

2015-01-05

In the present work, we describe the synthesis of silver nanoparticles (Ag-NPs) using seed aqueous extract of Pistacia atlantica (PA) and its antibacterial activity. UV-visible spectroscopy, X-ray diffraction (XRD), Fourier transform infra red spectroscopy (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray energy dispersive spectrophotometer (EDAX) were performed to ascertain the formation of Ag-NPs. It was observed that the growths of Ag-NPs are stopped within 35 min of reaction time. The synthesized Ag-NPs were characterized by a peak at 446 nm in the UV-visible spectrum. XRD confirmed the crystalline nature of the nanoparticles of 27 nm size. The XRD peaks at 38°, 44°, 64° and 77° can be indexed to the (111), (200), (220) and (311) Bragg's reflections of cubic structure of metallic silver, respectively. The FTIR result clearly showed that the extracts containing OH as a functional group act in capping the nanoparticles synthesis. Antibacterial activities of Ag-NPs were tested against the growth of Gram-positive (S. aureus) using SEM. The inhibition was observed in the Ag-NPs against S. aureus. The results suggest that the synthesized Ag-NPs act as an effective antibacterial agent. It is confirmed that Ag-NPs are capable of rendering high antibacterial efficacy and hence has a great potential in the preparation of used drugs against bacterial diseases. The scanning electron microscopy (SEM), indicated that, the most strains of S. aureus was damaged and extensively disappeared by addition of Ag-NPs. The results confirmed that the (PA) is a very good eco friendly and nontoxic source for the synthesis of Ag-NPs as compared to the conventional chemical/physical methods. Copyright © 2014 Elsevier B.V. All rights reserved.

Enhanced synergism of antibiotics with zinc oxide nanoparticles against extended spectrum β-lactamase producers implicated in urinary tract infections

NASA Astrophysics Data System (ADS)

Bhande, Rashmi M.; Khobragade, C. N.; Mane, R. S.; Bhande, S.

2013-01-01

In this study, enhanced synergistic bioactivity of zinc oxide nanoparticles (ZnO NPs) with β-lactam antibiotics were evaluated against a panel of clinically isolated extended spectrum β-lactamase producers implicated in urinary tract infections. Chemically synthesized zinc oxide nanoparticles (15 nm) were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmittance electron microscopy (HR-TEM), selective area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS), and UV-Visible spectrophotometry techniques. The antimicrobial potency (10 ± 0.66, 12, 11.33 ± 1.10, and 0.7 ± 0.66 mm inhibiting zone) and minimum inhibitory concentrations (80, 60, 30, 50 μg/ml) of ZnO NPs were tested separately whereas time-kill and membrane leakage assays were evaluated in combination with ZnO NPs+ cefotaxime, ampicillin, ceftriaxone, cefepime against the β-lactamase producer strains of E. coli, K. pneumoniae, S. paucimobilis, and P. aeruginosa, respectively. Time-kill curve dynamics of ZnO NPs with β-lactam antibiotics revealed enhanced bactericidal activity (50, 85, 58, 50 % fold inhibition) by delaying the exponential and stationary phases of all isolates when tested separately. Posttime-kill effect was studied on cell membrane by assaying leakage of reducing sugars (130.2, 124.7, 137, and 115.8 μg/bacterial dry weight of 1 mg (μg/mg) and proteins (15, 10, 16, 18 μg/mg). These assays revealed that membrane leakage was due to synergism of ZnO NPs+ β-lactam antibiotics which successfully damage cell membrane thereby leading to death of all ESBL producers. The results demonstrate the utilization of ZnO NPs as a potentiator of β-lactam antibiotics and suggest the possibility to use nanoparticles in a combination therapy to treat UTI.

Detecting Nanophase Weathering Products with CheMin: Reference Intensity Ratios of Allophane, Aluminosilicate Gel, and Ferrihydrite

NASA Technical Reports Server (NTRS)

Rampe, E. B.; Bish, D. L.; Chipera, S. J.; Morris, R. V.; Achilles, C. N.; Ming, D W.; Blake, D. F.; Anderson, R. C.; Bristow, T. F.; Crisp, A.;

[Study on the relationship between structure and spectroscopy of two compounds containing 2,2'-bipy and [MoO3] cluster skeletons].

PubMed

Zhang, Zi-Ming; Chen, Yi-Ping; You, Zhu-Chai; Su, Liu-Qin; Wang, Hao; Sun, Yan-Qiong

2013-11-01

Two compounds of molybdate with 2, 2'-bipy and [MoO3]: [(2, 2'-bipy)2 (MoO3)3]n (I) and [(2, 2'-bipy) (MoO3)]n (II) were successfully synthesized by hydrothermal synthesis method with programmable temperature control. In order to clarify the relationship between the structure and spectroscopy of these two compounds, both of them were characterized by means of X-ray powder diffraction (XRD), Fourier transform infrared spectra(FTIR), thermal perturbation 2D-IR correlation spectrum (2D-IR COS), thermogravimetric analysis(TGA), scanning electron microscopy(SEM), High temperature infrared analysis, UV-Vis DRS adsorption spectra and solid fluorescence spectrum to investigate the relationship between structure and properties of the title compounds. The powder XRD patterns of the complexes are well matched with the simulation based on single-crystal analysis, which indicate that compound I and II are in a pure phase. The characteristics of vibration frequency of FTIR and thermal perturbation relative spectral response of 2D-IR peak is consistent with thecompound I and II structure analysis. The synchronous and asynchronous correlation 2D-IR spectra of compounds also identified the compounds I and II molybdenum-oxygen cluster skeletons sequencing of vibration intensity change with temperature consistent with the high temperature infrared analysis. Through the TGA and high temperature infrared analysis it was found that the decomposition temperature was more than 300 degrees C and maximum weight losses rates above 800 degrees C, which suggest that they have good thermal stability. According to the UV-Vis DRS spectrum of the compound I and II there exists a wide ultraviolet absorption band in a range of 225 to 350 nm. The compound I and II steady-state fluorescence spectrum under the excitation of 277 and 295 nm respectively revealed compound I and II have the strongest emission peak at 460 and 480 nm respectively. This paper illustrates the coordination situation of these two compounds, and reveals the inherent law of valence electrons in molecule energy level transition. In the meantime it was verified that the weak interaction not only plays a role of stability in the frame of the structure of the complexes, but also plays an important role in heat resistance.

A facile biomimetic preparation of highly stabilized silver nanoparticles derived from seed extract of Vigna radiata and evaluation of their antibacterial activity

NASA Astrophysics Data System (ADS)

Choudhary, Manoj Kumar; Kataria, Jyoti; Cameotra, Swaranjit Singh; Singh, Jagdish

2016-01-01

The significant antibacterial activity of silver nanoparticles draws the major attention toward the present nanobiotechnology. Also, the use of plant material for the synthesis of metal nanoparticles is considered as a green technology. In this context, a non-toxic, eco-friendly, and cost-effective method has been developed for the synthesis of silver nanoparticles using seed extract of mung beans ( Vigna radiata). The synthesized nanoparticles have been characterized by UV-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), atomic absorption spectroscopy (AAS), and X-ray diffraction (XRD). The UV-visible spectrum showed an absorption peak at around 440 nm. The different types of phytochemicals present in the seed extract synergistically reduce the Ag metal ions, as each phytochemical is unique in terms of its structure and antioxidant function. The colloidal silver nanoparticles were observed to be highly stable, even after 5 months. XRD analysis showed that the silver nanoparticles are crystalline in nature with face-centered cubic geometry and the TEM micrographs showed spherical particles with an average size of 18 nm. Further, the antibacterial activity of silver nanoparticles was evaluated by well-diffusion method and it was observed that the biogenic silver nanoparticles have an effective antibacterial activity against Escherichia coli and Staphylococcus aureus. The outcome of this study could be useful for nanotechnology-based biomedical applications.

Impact of annealing on physical properties of e-beam evaporated polycrystalline CdO thin films for optoelectronic applications

NASA Astrophysics Data System (ADS)

Purohit, Anuradha; Chander, S.; Dhaka, M. S.

2017-04-01

An impact of annealing on the physical properties of polycrystalline CdO thin films is carried out in this study. CdO thin films of thickness 650 nm were fabricated on glass and indium tin oxide (ITO) substrates employing e-beam evaporation technique. The pristine thin films were annealed in air atmosphere at 250 °C, 400 °C and 550 °C for one hour followed by investigation of structural, optical, electrical and morphological properties along with elemental composition using X-ray diffraction (XRD), UV-Vis spectrophotometer, Fourier transform infrared (FTIR) spectrometer, source meter, scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS), respectively. XRD patterns confirmed the polycrystalline nature and cubic structure (with space group Fm 3 bar m) of the films. The crystallographic parameters are calculated and found to be influenced by the post-air annealing treatment. The optical study shows that direct band gap is ranging from 1.98 eV to 2.18 eV and found to be decreased with post-annealing. The refractive index and optical conductivity are also increased with annealing temperature. The current-voltage characteristics show ohmic behaviour of the annealed films. The surface morphology is observed to be improved with annealing and grain-size is increased as well as EDS spectrum confirmed the presence of cadmium (Cd) and oxygen (O) in the deposited films.

[Effects of magnetron sputtered ZrN on the bonding strength of titanium porcelain].

PubMed

Zhou, Shu; Zhang, Wen-yan; Guang, Han-bing; Xia, Yang; Zhang, Fei-min

2009-04-01

To investigate the effect of magnetron sputtered ZrN on the bonding strength between a low-fusing porcelain (Ti/Vita titankeramik system) and commercially pure cast titanium. Sixteen specimens were randomly assigned to test group and control group (n=8). The control group received no surface treated. Magnetron sputtered ZrN film was deposited on the surface of specimens in the test group. Then the sixteen titanium-porcelain specimens were prepared in a rectangular shape and went through three-point bending test on a universal test machine. The bond strength of Ti/porcelain was recorded. The phase composition of the specimens was analyzed using X-ray diffraction (XRD). The interface at titanium and porcelain and the titanium surface after debonding were observed with a scanning electron microscopy (SEM) and analyzed using energy depressive spectrum (EDS). New phase of ZrN was found with XRD in the test group. Statistical analysis showed higher bond strength following ZrN surface treatment in the test group [(45.991+/-0.648) MPa] than that in the control group [(29.483+/-1.007) MPa] (P=0.000). Bonded ceramic could be observed in test group, the amount of bonded ceramic was more than that in the control group. No obvious bonded ceramic in control group was found. Magnetron sputtered ZrN can improve bond strength of Ti/Vita titankeramik system significantly.

Green synthesis, characterization and antibacterial efficacy of palladium nanoparticles synthesized using Filicium decipiens leaf extract

NASA Astrophysics Data System (ADS)

Sharmila, G.; Farzana Fathima, M.; Haries, S.; Geetha, S.; Manoj Kumar, N.; Muthukumaran, C.

2017-06-01

Synthesis of metal nanoparticles through green chemistry route is an emerging eco-friendly approach in the present days. An eco-friendly, biogenic synthesis of palladium nanoparticles (PdNPs) using Filicium decipiens leaf extract was reported in the present study. The synthesized PdNPs were characterized by UV-visible spectroscopy, Transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The PdNPs formation was confirmed by UV-visible spectrophotometer and spherical shaped PdNPs with size range of 2-22 nm was observed in TEM analysis. Energy dispersive X-ray spectroscopy (EDS) analysis confirmed the presence of palladium in the synthesized nanoparticles. The crystalline nature of PdNPs was confirmed by XRD pattern and compared with the standard. The phytochemicals and proteins were identified by their functional groups in FT-IR spectrum and revealed the amide, amine groups present in F. decipiens may have involved in the bio-reduction reaction for PdNPs synthesis. Prepared PdNPs showed potential antibacterial activity against both Gram-positive and Gram-negative bacteria. F. decipiens leaf extract based PdNPs showed high bactericidal activity against Escherichia coli, Pseudomonas aeruginosa as compared to Staphylococcus aureus and Bacillus subtilis Results showed that phytochemicals rich F. decipiens leaf extract may be utilized as an effective non-toxic reducing agent for PdNPs synthesis and prepared PdNPs may useful in biomedical applications.

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.

Temperature dependent dielectric relaxation and ac-conductivity of alkali niobate ceramics studied by impedance spectroscopy

NASA Astrophysics Data System (ADS)

Yadav, Abhinav; Mantry, Snigdha Paramita; Fahad, Mohd.; Sarun, P. M.

2018-05-01

Sodium niobate (NaNbO3) ceramics is prepared by conventional solid state reaction method at sintering temperature 1150 °C for 4 h. The structural information of the material has been investigated by X-ray diffraction (XRD) and Field emission scanning electron microscopy (FE-SEM). The XRD analysis of NaNbO3 ceramics shows an orthorhombic structure. The FE-SEM micrograph of NaNbO3 ceramics exhibit grains with grain sizes ranging between 1 μm to 5 μm. The surface coverage and average grain size of NaNbO3 ceramics are found to be 97.6 % and 2.5 μm, respectively. Frequency dependent electrical properties of NaNbO3 is investigated from room temperature to 500 °C in wide frequency range (100 Hz-5 MHz). Dielectric constant, ac-conductivity, impedance, modulus and Nyquist analysis are performed. The observed dielectric constant (1 kHz) at transition temperature (400 °C) are 975. From conductivity analysis, the estimated activation energy of NaNbO3 ceramics is 0.58 eV at 10 kHz. The result of Nyquist plot shows that the electrical behavior of NaNbO3 ceramics is contributed by grain and grain boundary responses. The impedance and modulus spectrum asserts that the negative temperature coefficient of resistance (NTCR) behavior and non-Debye type relaxation in NaNbO3.

Crucial role of molecular planarity on the second order nonlinear optical property of pyridine based chalcone single crystals

NASA Astrophysics Data System (ADS)

Menezes, Anthoni Praveen; Jayarama, A.; Ng, Seik Weng

2015-05-01

An efficient nonlinear optical material 2E-3-(4-bromophenyl)-1-(pyridin-3-yl) prop-2-en-1-one (BPP) was synthesized and single crystals were grown using slow evaporation solution growth technique at room temperature. Grown crystal had prismatic morphology and its structure was confirmed by various spectroscopic studies, elemental analysis, and single crystal X-ray diffraction (XRD) technique. The single crystal XRD of the crystal showed that BPP crystallizes in monoclinic system with noncentrosymmetric space group P21 and the cell parameters are a = 5.6428(7) Å, b = 3.8637(6) Å, c = 26.411(2) Å, β = 97.568(11) deg and v = 575.82(12) Å3. The UV-Visible spectrum reveals that the crystal is optically transparent and has high optical energy band gap of 3.1 eV. The powder second harmonic generation efficiency (SHG) of BPP is 6.8 times that of KDP. From thermal analysis it is found that the crystal melts at 139 °C and decomposes at 264 °C. High optical transparency down to blue region, higher powder SHG efficiency and better thermal stability than that of urea makes this chalcone derivative a promising candidate for SHG applications. Furthermore, effect of molecular planarity on SHG efficiency and role of pyridine ring adjacent to carbonyl group in forming noncentrosymmetric crystal systems of chalcone family is also discussed.

Role of manganese dioxide in the recovery of oxide-sulphide zinc ore.

PubMed

Yang, Kun; Zhang, Libo; Zhu, Xingcai; Peng, Jinhui; Li, Shiwei; Ma, Aiyuan; Li, Haoyu; Zhu, Fei

2018-02-05

In this article, the role of MnO 2 in the recovery of oxide-sulphide zinc ore discussed. Through adopting various modern analysis techniques (such as X-ray diffraction pattern, X-ray photoelectron spectroscopy, scanning electron microscope, energy dispersive X-ray analysis, and fourier transform infrared spectroscopy), the function and mechanism of MnO 2 during the phase transformation process is found out. Thermodynamic mechanisms involved in the phase transformation process with or without addition of manganese dioxide investigated by exploiting the Equilib module of FactSage. What's more, XRD patterns, XPS spectra and SEM-EDAX analyses of zinc calcines verify well the calculations of FactSage. Results reveal that the addition of MnO 2 will produce an aggregation of ZnMn 2 O 4 , a valuable energy material, while roasting on its own, results in generating undesirable Zn 2 SiO 4 , the oxidation degree being relatively low. Moreover, XRD pattern of zinc calcine and FT-IR spectrum of yellow product collected in the calcination process prove that the sulphur-fixing value of the additive MnO 2 , which can promote transforming to the elemental sulphur. The volatile S can be collected through a simple guiding device. In this process, the emission of SO 2 effectively avoids, thus MnO 2 deems as a potential additive in the recovery of oxide-sulphide zinc ore. Copyright © 2017. Published by Elsevier B.V.

Studies on the synthesis, spectral, optical and thermal properties of l-Valine Zinc Sulphate: an organic inorganic hybrid nonlinear optical crystal.

PubMed

Puhal Raj, A; Ramachandra Raja, C

2012-11-01

Nonlinear optical (NLO) organic inorganic hybrid l-Valine Zinc Sulphate (LVZS) was synthesized and single crystals were obtained from saturated aqueous solution by slow evaporation method at 36°C using a constant temperature bath (CTB) with an accuracy of ±0.01°C. This crystal is reported with its characterization by single crystal and powder XRD, FTIR, UV-Vis-NIR, TG/DTA analysis and SHG test. Single crystal XRD study reveals that LVZS crystallizes in monoclinic system with the lattice constants a=9.969(3) Å, b=7.238(3) Å, c=24.334(9) Å and cell volume is 1736.00Å(3). Sharp peaks observed in powder X-ray diffraction studies confirm the high degree of crystallinity of grown crystal. The incorporation of sulphate ion with l-valine is confirmed by FTIR spectrum in LVZS crystal(.) A remarkable increase in optical transparency has been observed in LVZS when compared to l-valine and zinc sulphate heptahydrate Thermal properties of LVZS have been reported by using TG/DTA analysis. Kurtz powder second harmonic generation (SHG) test confirms NLO property of the crystal and SHG efficiency of LVZS was found to be 1.34 times more than pure l-valine. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis and controlled release properties of 2,4-dichlorophenoxy acetate–zinc layered hydroxide nanohybrid

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

Bashi, Abbas M., E-mail: abbasmatrood@yahoo.com; Hussein, Mohd Zobir; Zainal, Zulkarnain

2013-07-15

Direct reaction of ZnO with 2,4-dichlorophenoxyacetic acid (24D) solutions of different concentrations allows obtaining new organic–inorganic nanohybrid materials formed by intercalation of 24D into interlayers of zinc layered hydroxide (ZLH). XRD patterns show a progressive evolution of the structure as 24D concentration increases. The nanohybrid obtained at higher 24D concentration (24D–ZLH(0.4)) reveals a well ordered layered structure with two different basal spacings at 25.2 Å and 24 Å. The FTIR spectrum showing the vibrations bands of the functional groups of 24D and of the ZLH confirms the intercalation. SEM images are in agreement with the structural evolution observed by XRDmore » and reveal the ribbon morphology of the nanohybrids. The release studies of 24D showed a rapid release of 94% for the first 100 min governed by the pseudo-second order kinetic model. - Graphical abstract: The phenomenon indicates that the optical energy gap is enlarged with the increase of molar concentrations in 2,4-dichlorophenoxy acetate anion content into ZnO to create a ZLH–24D nanohybrid. - Highlights: • Nanohybrid was synthesized from 2,4-dichlorophenoxy acetate with-Zinc LHD, using wet chemistry. • Characterized using SEM, TEM, EDX, FTIR, XRD and TGA. • Ribbon-shaped 24D–Zn-layered hydroxide nanoparticles with (003) diffractions of 2.5 nm phase were synthesized.« less

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

Effect of solvent on the synthesis of SnO{sub 2} nanoparticles

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

Kumar, Virender; Singh, Karamjit; Singh, Kulwinder

Tin oxide (SnO{sub 2}) nanoparticles have been synthesized by co-precipitation method. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD) and Ultraviolet-Visible spectroscopy (UV-VIS). XRD analysis confirmed the formation of single phase of SnO{sub 2} nanoparticles. It has been found that solvents played important role in controlling the crystallite size of SnO{sub 2} nanoparticles. The XRD analysis showed well crystallized tetragonal SnO{sub 2} nanoparticles. The crystallite size of SnO{sub 2} nanoparticles varies with the solvent. Tauc plot showed that optical band gap was also tailored by controlling the solvent during synthesis.

High temperature XRD of Cu2.1Zn0.9SnSe4

NASA Astrophysics Data System (ADS)

Chetty, Raju; Mallik, Ramesh Chandra

2014-04-01

Quaternary compound with chemical composition Cu2.1Zn0.9SnSe4 is prepared by solid state synthesis. High temperature XRD (X-Ray Diffraction) of this compound is used in studying the effect of temperature on lattice parameters and thermal expansion coefficients. Thermal expansion coefficient is one of the important quantities in evaluating the Grüneisen parameter which further useful in determining the lattice thermal conductivity of the material. The high temperature XRD of the material revealed that the lattice parameters as well as thermal expansion coefficients of the material increased with increase in temperature which confirms the presence of anharmonicty.

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.

Organic Photonics: Toward a New Generation of Thin Film Photovoltaics and Lasers

DTIC Science & Technology

2011-03-07

plane. 39 Both electron and x - ray diffraction confirm the existence of crystalline domains of CuPc and C60. Crystalline domain sizes range from 5...nanocrystalline domains indicated by white curves that locate the domain boundaries. Scale bar=5 nm. b, X - ray diffraction pattern of an OVPD grown A... ray diffraction (XRD) and atomic force microscopy (AFM), as shown in Fig. 8. A cross-sectional TEM image of [CuPc(6.1nm)/C60(6.1nm)]10 is shown in

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

Shivananda, C. S.; Rao, B. Lakshmeesha; Madhukumar, R.

In this work silk fibroin/pullulan blend films have been prepared by solution casting method. The blend films were examined for structural, and thermal properties using X-ray diffraction (XRD), thermogravimatric (TGA) and differential scanning calorimetry (DSC) analysis. The XRD results indicate that with the introduction of pullulan, the interaction between SF and pullulan in the blend films induced the conformation transition of SF films and amorphous phase increases with increasing pullulan ratio. The thermal properties of the blend films were improved significantly in the blend films.

Electric-field responsive contrast agent based on liquid crystals and magnetic nanoparticles

NASA Astrophysics Data System (ADS)

Mair, Lamar O.; Martinez-Miranda, Luz J.; Kurihara, Lynn K.; Nacev, Aleksandar; Hilaman, Ryan; Chowdhury, Sagar; Jafari, Sahar; Ijanaten, Said; da Silva, Claudian; Baker-McKee, James; Stepanov, Pavel Y.; Weinberg, Irving N.

2018-05-01

The properties of liquid crystal-magnetic nanoparticle composites have potential for sensing in the body. We study the response of a liquid crystal-magnetic nanoparticle (LC-MNP) composite to applied potentials of hundreds of volts per meter. Measuring samples using X-ray diffraction (XRD) and imaging composites using magnetic resonance imaging (MRI), we demonstrate that electric potentials applied across centimeter scale LC-MNP composite samples can be detected using XRD and MRI techniques.

Compression Freezing Kinetics of Water to Ice VII

DOE PAGES

Gleason, A. E.; Bolme, C. A.; Galtier, E.; ...

2017-07-11

Time-resolved x-ray diffraction (XRD) of compressed liquid water shows transformation to ice VII in 6 nsec, revealing crystallization rather than amorphous solidification during compression freezing. Application of classical nucleation theory indicates heterogeneous nucleation and one-dimensional (e.g., needlelike) growth. In conclusion, these first XRD data demonstrate rapid growth kinetics of ice VII with implications for fundamental physics of diffusion-mediated crystallization and thermodynamic modeling of collision or impact events on ice-rich planetary bodies.

Coupling Graphene Sheets with Magnetic Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

sheets obtained from three different synthetic methods: (i) electrochemical exfoliation of highly oriented pyrolytic graphite ( HOPG ) [8], (ii...Figure 8d, the characteristic lattice fringes of ɤ-Fe2O3 nanoparticles in graphene sheet is shown. Typical X-ray diffraction ( XRD ) patterns of the HOPG ...pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG , exfoliated graphene, PyDop1

Compression Freezing Kinetics of Water to Ice VII

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

Gleason, A. E.; Bolme, C. A.; Galtier, E.

Time-resolved x-ray diffraction (XRD) of compressed liquid water shows transformation to ice VII in 6 nsec, revealing crystallization rather than amorphous solidification during compression freezing. Application of classical nucleation theory indicates heterogeneous nucleation and one-dimensional (e.g., needlelike) growth. In conclusion, these first XRD data demonstrate rapid growth kinetics of ice VII with implications for fundamental physics of diffusion-mediated crystallization and thermodynamic modeling of collision or impact events on ice-rich planetary bodies.

Understanding Two Different Structures in the Dark Stable State of the Oxygen‐Evolving Complex of Photosystem II: Applicability of the Jahn–Teller Deformation Formula

PubMed Central

Shoji, Mitsuo; Isobe, Hiroshi; Tanaka, Ayako; Fukushima, Yoshimasa; Kawakami, Keisuke; Umena, Yasufumi; Kamiya, Nobuo; Nakajima, Takahito

2017-01-01

Abstract Tanaka et al. (J. Am. Chem. Soc., 2017, 139, 1718) recently reported the three‐dimensional (3D) structure of the oxygen evolving complex (OEC) of photosystem II (PSII) by X‐ray diffraction (XRD) using extremely low X‐ray doses of 0.03 and 0.12 MGy. They observed two different 3D structures of the CaMn4O5 cluster with different hydrogen‐bonding interactions in the S1 state of OEC keeping the surrounding polypeptide frameworks of PSII the same. Our Jahn–Teller (JT) deformation formula based on large‐scale quantum mechanics/molecular mechanics (QM/MM) was applied for these low‐dose XRD structures, elucidating important roles of JT effects of the MnIII ion for subtle geometric distortions of the CaMn4O5 cluster in OEC of PSII. The JT deformation formula revealed the similarity between the low‐dose XRD and damage‐free serial femtosecond X‐ray diffraction (SFX) structures of the CaMn4O5 cluster in the dark stable state. The extremely low‐dose XRD structures were not damaged by X‐ray irradiation. Implications of the present results are discussed in relation to recent SFX results and a blue print for the design of artificial photocatalysts for water oxidation. PMID:29577075

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

PubMed

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

2013-12-01

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

Evolution of the substructure of a novel 12% Cr steel under creep conditions

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

Yadav, Surya Deo, E-mail: surya.yadav@tugraz.at; Kalácska, Szilvia, E-mail: kalacska@metal.elte.hu; Dománková, Mária, E-mail: maria.domankova@stuba.sk

2016-05-15

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used tomore » the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.« less

Raman spectroscopy of synthetic and natural iowaite.

PubMed

Frost, Ray L; Adebajo, Moses O; Erickson, Kristy L

2005-02-01

The chemistry of a magnesium based hydrotalcite known as iowaite Mg6Fe2Cl2(OH)16.4H2O has been studied using Raman spectroscopy. Iowaite has chloride as the counter anion in the interlayer. The formula of synthetic iowaite was found to be Mg5.78Fe2.09(Cl,(CO3)0.5)(OH)16.4H2O. Oxidation of natural iowaite results in the formation of Mg4FeO(Cl,CO3) (OH)8.4H2O. X-ray diffraction (XRD) shows that the iowaite is a layered structure with a d(001) spacing of 8.0 angtsroms. For synthetic iowaite three Raman bands at 1376, 1194 and 1084 cm(-1) are attributed to CO3 stretching vibrations. These bands are not observed for the natural iowaite but are observed when the natural iowaite is exposed to air. The Raman spectrum of natural iowaite shows three bands at 708, 690 and 620 cm(-1) and upon exposure to air, two broad bands are found at 710 and 648 cm(-1). The Raman spectrum of synthetic iowaite has a very broad band at 712 cm(-1). The Raman spectrum of natural iowaite shows an intense band at 527 cm(-1). The air oxidized iowaite shows two bands at 547 and 484 cm(-1) attributed to the (CO3)(2-)nu2 bending mode. Raman spectroscopy has proven most useful for the study of the chemistry of iowaite and chemical changes induced in natural iowaite upon exposure to air.

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

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

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

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.

Supercritical carbon dioxide treatment as a method for polymorph preparation of deoxycholic acid.

PubMed

Tozuka, Yuichi; Kawada, Dai; Oguchi, Toshio; Yamamoto, Keiji

2003-09-16

A new polymorph of deoxycholic acid (DCA) was formed by using a supercritical carbon dioxide treatment. Deoxycholic acid crystals were stored in a pressure vessel purged with carbon dioxide at 12MPa, 60 degrees C for definite intervals. After storage for 1h in supercritical carbon dioxide (SC-CO2), new X-ray diffraction (XRD) peaks, not found in the bulk DCA crystal, were observed at 2theta = 7.4 degrees, 9.7 degrees and 14.0 degrees. The intensities of the new diffraction peaks increased with an increase in storage time, whereas the intensities of the diffraction peaks due to bulk DCA crystal decreased. On the DSC curves, the crystals obtained showed an exothermic peak at around 155 degrees C followed by the melting peak of bulk DCA crystal at 175 degrees C. By the temperature-controlled powder XRD measurement, the crystals obtained were found to be a metastable form of DCA. The polymorphs of DCA have not been reported; therefore, the SC-CO2 treatment would be a peculiar method to obtain a DCA polymorph.

Electrochemical reactions in fluoride-ion batteries: mechanistic insights from pair distribution function analysis

DOE PAGES

Grenier, Antonin; Porras-Gutierrez, Ana-Gabriela; Groult, Henri; ...

2017-07-05

Detailed analysis of electrochemical reactions occurring in rechargeable Fluoride-Ion Batteries (FIBs) is provided by means of synchrotron X-ray diffraction (XRD) and Pair Distribution Function (PDF) analysis.

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

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

NASA Astrophysics Data System (ADS)

Stan, Manuela; Popa, Adriana; Toloman, Dana; Silipas, Teofil-Danut; Vodnar, Dan Cristian; Katona, Gabriel

2015-12-01

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn2+ ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes and oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs.

Phase Compositions of Self Reinforcement Al2O3/CaAl12O19 Composite using X-ray Diffraction Data and Rietveld Technique

NASA Astrophysics Data System (ADS)

Asmi, D.; Low, I. M.; O'Connor, B.

2008-03-01

The analysis of x-ray diffraction (XRD) patterns by the Rietveld technique was tested to the quantitatively phase compositions of self reinforcement Al2O3/CaAl12O19 composite. Room-temperature XRD patterns revealed that α-Al2O3 was the only phase presence in the CA0 sample, whereas the α-Al2O3 and CaAl12O19 phases were found for CA5, CA15, CA30, and CA50 samples. The peak intensity of CA6 in the self reinforcement Al2O3/CaAl12O19 composites increased in proportion with increase in CaAl12O19 content in contrast to α-Al2O3. The diffraction patterns for CA100 sample shows minor traces of α-Al2O3 even in relatively low peak intensity. It is suggesting that the in-situ reaction sintering of raw materials were not react completely to form 100 wt% CaAl12O19 at temperature 1650 °C. Quantitative phase compositions of self reinforcement Al2O3/CaAl12O19 composites by Rietveld analysis with XRD data has been well demonstrated. The results showed that the GOF values are relatively low and the fluctuation in the difference plots shows a reasonable fit between the observed and the calculated plot.

Kinetics and structural changes of Li-rich layered oxide 0.5Li2MnO3·0.5LiNi(0.292)Co(0.375)Mn(0.333)O2 material investigated by a novel technique combining in situ XRD and a multipotential step.

PubMed

Shen, Chong-Heng; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Wang, Qin; Su, Hang; Fu, Fang; Zheng, Xiao-Mei

2014-08-13

Li-rich layered oxide 0.5Li2MnO3·0.5LiNi0.292Co0.375Mn0.333O2 was prepared by an aqueous solution-evaporation route. X-ray powder diffraction (XRD) showed that the as-synthesized material was a solid solution consisting of layered α-NaFeO2-type LiMO2 (M = Ni, Co, Mn) and monoclinic Li2MnO3. The superlattice spots in the selected area electron diffraction pattern indicated the ordering of lithium ions with transition metal (TM) ions in TM layers in this Li-rich layered oxide. Electrochemical performance testing showed that the as-synthesized material could deliver an initial discharge capacity of 267.7 mAh/g, with a capacity retention of 88.5% after 33 cycles. A new combination technique, multipotential step in situ XRD (MPS in situ XRD) measurement, was applied for the first time to investigate the Li-rich layered oxide. Using this approach, the relationships between kinetics and structural variations can be obtained simutaneously. In situ XRD results showed that the c parameter decreased from 3.70 to 4.30 V and increased from 4.30 to 4.70 V, whereas the a parameter underwent a decrease above 4.30 V during the first charge process. Below 3.90 V during the first discharge process, a slight decrease in the c parameter was found along with an increase in the a parameter. During the first charge process, the value of the coefficient of diffusion for lithium ions (DLi+) decreased to its mininum at 4.55 V, which might be associated with Ni(2+) migration, as indicated by both Ni occupancy in 3b sites (Ni3b%) in the Li(+) layers and complicated chemical reactions. Remarkably, a lattice distortion might occur within the local domain in the host stucture during the first discharge process, indicated by a slight splitting of the (003) diffraction peak at 3.20 V.

Characterisation and luminescence studies of Tm and Na doped magnesium borate phosphors.

PubMed

Ekdal, E; Garcia Guinea, J; Karabulut, Y; Canimoglu, A; Harmansah, C; Jorge, A; Karali, T; Can, N

2015-09-01

In this study, structural and luminescence properties of magnesium borate of the form MgB4O7 doped with Tm and Na were investigated by X-ray diffraction (XRD), Raman spectroscopy and cathodoluminescence (CL). The morphologies of the synthetised compounds exhibit clustered granules and road-like materials. As doping trivalent ions into a host with divalent cations requires charge compensation, this effect is discussed. The CL spectra of undoped MgB4O7 shows a broad band emission centred around 350 nm which is postulated to be produced by self-trapped excitons and some other defects. From the CL emission spectrum, main emission bands centred at 360, 455, 475 nm due to the respective transitions of (1)D2→(3)H6,(1)D2→(3)F4 and (1)G4→(3)H6 suggest the presence of Tm(3+) ion in MgB4O7 lattice site. CL mechanism was proposed to explain the observed phenomena which are valuable in possibility of the developing new luminescent materials for different applications. In addition, the experimental Raman spectrum of doped and undoped MgB4O7 were reported and discussed. Copyright © 2015 Elsevier Ltd. All rights reserved.

A photoelectrochemical immunosensor for detection of α-fetoprotein based on Au-ZnO flower-rod heterostructures

NASA Astrophysics Data System (ADS)

Han, Zhizhong; Luo, Min; Chen, Li; Chen, Jinghua; Li, Chunyan

2017-04-01

In this work, a novel label free photoelectrochemical (PEC) immunosensor has been developed for the detection of α-fetoprotein (AFP). The immunosensor was based on Au-ZnO flower-rods (FRs) heterostructure, where Au nanoparticles (NPs) were firstly electrodeposited by cyclic voltammetry methods. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Mott-Schottky plot (MS), UV-vis diffuse reflectance spectrum and fluorescence emission spectrum were used for the characterizations of Au-ZnO FRs. The results demonstrated that Au NPs not only obviously enhanced the visible light absorption of ZnO FRs due to surface plasmon resonance (SPR) but also improved the separation of photo-generated electron-hole pairs. Therefore, the photocurrent of Au-ZnO FRs was increased under simulated sunlight. The photocurrent was reduced after the specific antibody-antigen immune reaction. And the photocurrent decrement was linear with the logarithm of AFP antigen concentration in the range from 0.005 ng mL-1 to 50 ng mL-1 with a low detection limit of 0.56 pg mL-1 (S/N = 3). The PEC immunosensor also exhibited high anti-interference property and acceptable stability. This work would provide a promising photoelectrochemical strategy for the detection of other proteins in clinical diagnosis.

Utilization of visible to NIR light energy by Yb+3, Er+3 and Tm+3 doped BiVO4 for the photocatalytic degradation of methylene blue

NASA Astrophysics Data System (ADS)

Regmi, Chhabilal; Kshetri, Yuwaraj K.; Ray, Schindra Kumar; Pandey, Ramesh Prasad; Lee, Soo Wohn

2017-01-01

Lanthanide-doped BiVO4 semiconductors with efficient photocatalytic activities over a broad range of the solar light spectrum have been synthesized by the microwave hydrothermal method using ethylenediaminetetraacetic acid (EDTA). The structural, morphological, and optical properties of the as-synthesized samples were evaluated by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray powder diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, UV-vis diffuse reflectance spectroscopy (DRS), and photoluminescence spectroscopy (PL). The chemical compositions were analyzed by X-ray photoelectron spectroscopy (XPS). The toxicity of the samples was measured using Mus musculus skin melanoma cells (B16-F10 (ATCC® CRL-6475™)) and were found to be nontoxic for human cells. The photocatalytic efficiency of the prepared samples was evaluated by methylene blue (MB) degradation. The best photocatalytic activity was shown by BiVO4 with 6:3:3 mol percentage of Yb+3:Er+3:Tm+3 in all solar light spectrum. The synthesized samples possess low band gap energy and a hollow structure suitable for the better photocatalytic activity. The observed NIR photoactivity supports that the upconversion mechanism is involved in the overall photocatalytic process. Therefore, this approach provides a better alternative upconversion material for integral solar light absorption.

The characteristics of steel slag and the effect of its application as a soil additive on the removal of nitrate from aqueous solution.

PubMed

Liyun, Yang; Ping, Xu; Maomao, Yang; Hao, Bai

2017-02-01

This study examined the characteristics of nitrate removal from aqueous solution by steel slag and the feasibility of using steel slag as a soil additive to remove nitrate. Steel slag adsorbents were characterized by X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM) and infrared spectrum (IR spectrum). Adsorption isotherms and kinetics were also analysed. Various parameters were measured in a series of batch experiments, including the sorbent dose, grain size of steel slag, reaction time, initial concentration of nitrate nitrogen, relationship between Al, Fe and Si ions leached from the steel slag and residual nitrate in the aqueous solution. The nitrate adsorbing capacity increased with increasing amounts of steel slag. In addition, decreasing the grain diameter of steel slag also enhanced the adsorption efficiency. Nitrate removal from the aqueous solution was primarily related to Al, Fe, Si and Mn leached from the steel slag. The experimental data conformed to second-order kinetics and the Freundlich isothermal adsorption equation, indicating that the adsorption of nitrate by steel slag is chemisorption under the action of monolayer adsorption. Finally, it was determined that using steel slag as a soil additive to remove nitrate is a feasible strategy.

High-Temperature, Perhaps Silicic, Volcanism on Mars Evidenced by Tridymite Detection in High-SiO2 Sedimentary Rock at Gale Crater, Mars

NASA Technical Reports Server (NTRS)

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

Growth and characterization of Na2Mo2O7 crystal scintillators for rare event searches

NASA Astrophysics Data System (ADS)

Pandey, Indra Raj; Kim, H. J.; Kim, Y. D.

2017-12-01

Disodium dimolybdate (Na2Mo2O7) crystals were grown using the Czochralski technique. The thermal characteristics of the compound were analyzed using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) measurements. The crystal structure of the grown sample was confirmed using X-ray diffraction (XRD). Luminescence properties were measured at room and low temperatures, using a light emitting diode (LED) source. Very weak luminescence was observed at room temperature; however, the luminescence intensity was enhanced at low temperatures. The crystal's transmittance spectrum was measured for estimating its optical quality and energy band gap. The grown crystal exhibited a luminescence light yield of 55% compared with CaMoO4 crystals at 10 K, when excited by a 280-nm-wavelength LED source, but does not have the drawbacks of radioactive Ca isotopes. These results suggest that at cryogenic temperatures, Na2Mo2O7 crystal scintillators are promising for the detection of dark matter and neutrinoless double beta decay of 100Mo.

Synthesis and characterization of structural, morphological and photosensor properties of Cu0.1Zn0.9S thin film prepared by a facile chemical method

NASA Astrophysics Data System (ADS)

Gubari, Ghamdan M. M.; Ibrahim Mohammed S., M.; Huse, Nanasaheb P.; Dive, Avinash S.; Sharma, Ramphal

2018-05-01

The Cu0.1Zn0.9S thin film was grown by facile chemical bath deposition (CBD) method on glass substrates at 60°C. The structural, morphological, photosensor properties of the as-grown thin film has been investigated. The structural and phase confirmation of the as-grown thin film was carried out by X-ray diffraction (XRD) technique and Raman spectroscopy. The FE-SEM images showed that the thin films are well covered with material on an entire glass substrate. From the optical absorption spectrum, the direct band gap energy for the Cu0.1Zn0.9S thin film was found to be ˜3.16 eV at room temperature. The electrical properties were measured at room temperature in the voltage range ±2.5 V, showed a drastic enhancement in current under light illumination with the highest photosensitivity of ˜72 % for 260 W.

Mangifera Indica leaf-assisted biosynthesis of well-dispersed silver nanoparticles

NASA Astrophysics Data System (ADS)

Philip, Daizy

2011-01-01

The use of various parts of plants for the synthesis of nanoparticles is considered as a green technology as it does not involve any harmful chemicals. The present study reports a facile and rapid biosynthesis of well-dispersed silver nanoparticles. The method developed is environmentally friendly and allows the reduction to be accelerated by changing the temperature and pH of the reaction mixture consisting of aqueous AgNO 3 and Mangifera Indica leaf extract. At a pH of 8, the colloid consists of well-dispersed triangular, hexagonal and nearly spherical nanoparticles having size ˜20 nm. The UV-vis spectrum of silver nanoparticles gave surface plasmon resonance (SPR) at 439 nm. The synthesized nanocrystals were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Water soluble organics present in the leaf are responsible for the reduction of silver ions. This green method provides faster synthesis comparable to chemical methods and can be used in areas such as cosmetics, foods and medical applications.

Influence of Oxygen ions irradiation on Polyaniline/Single Walled Carbon Nanotubes nanocomposite

NASA Astrophysics Data System (ADS)

Patil, Harshada K.; Deshmukh, Megha A.; Gaikwad, Sumedh D.; Bodkhe, Gajanan A.; Asokan, K.; Yasuzawa, Mikito; Koinkar, Pankaj; Shirsat, Mahendara D.

2017-01-01

Influence of Oxygen ions (100 MeV) irradiation on Polyaniline (PANI)/Single Walled Carbon Nanotubes (SWNTs) nanocomposite was studied in the present investigation. PANI/SWNTs nanocomposite was synthesized by electrochemical Cyclic Voltammetry technique. Nanocomposite was exposed under SHI irradiation of Oxygen (100 MeV) ions for three different fluences such as 1×1010 ions/cm2, 5×1010 ions/cm2 and 1×1011 ions/cm2. The SHI irradiated PANI/SWNTs nanocomposite was investigated by using morphological (AFM), structural (XRD) and spectroscopy (FTIR) characterization. AFM study exhibits effects of SHI irradiation on morphology of the nanocomposite and root mean square roughness of the nanocomposite is observed to be decreased as fluence was increased. The FTIR absorption spectrum exhibits formation of new functional sites with the increase in intensity of absorption peaks, due to SHI irradiation. X-Ray Diffraction studies show a gradual decrease in the crystalline nature of the nanocomposite upon irradiation.

Biosynthesis, characterization and cytotoxic effect of plant mediated silver nanoparticles using Morinda citrifolia root extract.

PubMed

Suman, T Y; Radhika Rajasree, S R; Kanchana, A; Elizabeth, S Beena

2013-06-01

Silver has been used since time to control bodily infection, prevent food spoilage and heal wounds by preventing infection. The present study aims at an environmental friendly method of synthesizing silver nanoparticles, from the root of Morinda citrifolia; without involving chemical agents associated with environmental toxicity. The obtained nanoparticles were characterized by UV-vis absorption spectroscopy with an intense surface plasmon resonance band at 413 nm clearly reveals the formation of silver nanoparticles. Fourier transmission infra red spectroscopy (FTIR) showed nanopartilces were capped with plant compounds. Field emission-scanning electron microscopy (FE-SEM) and Transmission electron microscopy (TEM) showed that the spherical nature of the silver nanoparticles with a size of 30-55 nm. The X-ray diffraction spectrum XRD pattern clearly indicates that the silver nanoparticles formed in the present synthesis were crystalline in nature. In addition these biologically synthesized nanoparticles were also proved to exhibit excellent cytotoxic effect on HeLa cell. Copyright © 2013 Elsevier B.V. All rights reserved.

Trimethylamine Sensors Based on Au-Modified Hierarchical Porous Single-Crystalline ZnO Nanosheets.

PubMed

Meng, Fanli; Zheng, Hanxiong; Sun, Yufeng; Li, Minqiang; Liu, Jinhuai

2017-06-22

It is of great significance for dynamic monitoring of foods in storage or during the transportation process through on-line detecting trimethylamine (TMA). Here, TMA were sensitively detected by Au-modified hierarchical porous single-crystalline ZnO nanosheets (HPSCZNs)-based sensors. The HPSCZNs were synthesized through a one-pot wet-chemical method followed by an annealing treatment. Polyethyleneimine (PEI) was used to modify the surface of the HPSCZNs, and then the PEI-modified samples were mixed with Au nanoparticles (NPs) sol solution. Electrostatic interactions drive Au nanoparticles loading onto the surface of the HPSCZNs. The Au-modified HPSCZNs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive spectrum (EDS), respectively. The results show that Au-modified HPSCZNs-based sensors exhibit a high response to TMA. The linear range is from 10 to 300 ppb; while the detection limit is 10 ppb, which is the lowest value to our knowledge.

Green synthesis of colloidal copper oxide nanoparticles using Carica papaya and its application in photocatalytic dye degradation.

PubMed

Sankar, Renu; Manikandan, Perumal; Malarvizhi, Viswanathan; Fathima, Tajudeennasrin; Shivashangari, Kanchi Subramanian; Ravikumar, Vilwanathan

2014-01-01

Copper oxide (CuO) nanoparticles were synthesized by treating 5 mM cupric sulphate with Carica papaya leaves extract. The kinetics of the reaction was studied using UV-visible spectrophotometry. An intense surface Plasmon resonance between 250-300 nm in the UV-vis spectrum clearly reveals the formation of copper oxide nanoparticles. The results of scanning electron microscopy (SEM) and dynamic light scattering (DLS) exhibited that the green synthesized copper oxide nanoparticles are rod in shape and having a mean particle size of 140 nm, further negative zeta potential disclose its stability at -28.9 mV. The Fourier-transform infrared (FTIR) spectroscopy results examined the occurrence of bioactive functional groups required for the reduction of copper ions. X-ray diffraction (XRD) spectra confirmed the copper oxide nanoparticles crystalline nature. Furthermore, colloidal copper oxide nanoparticles effectively degrade the Coomassie brilliant blue R-250 dye beneath the sunlight. Copyright © 2013 Elsevier B.V. All rights reserved.

Highly branched RuO2 Nanorods on Electrospun TiO2 Nanofibers toward Electrochemical Catalysts

NASA Astrophysics Data System (ADS)

Cho, Yukyung; Kim, Su-Jin; Lee, Nam-Suk; Kim, Myung Hwa; Lee, Youngmi

2014-03-01

We report a facile growth route to synthesize hierarchically grown single crystalline metallic RuO2 nanorods on electrospun TiO2 nanofibers via a combination of a simple vapour phase transport process with an electrospinning process. This synthetic strategy could be very useful to design a variety of highly branched network architectures of the functional hetero-nanostructures for electrochemical applications. Particularly, Ruthenium oxide (RuO2) 1-dimensional nanostructures can be used as the effective catalysts or electrochemical electrode materials. Thus, we first synthesize TiO2 nanofibers from mixture of titanium isopropoxide precursor and polymer and then ruthenium hydroxide precursor on TiO2 nanofibers are transformed into RuO2 nanorods by thermal treatment at 250oC in air. The crystalline structures of products are confirmed using scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) spectrum, Raman spectroscopy, and high resolution electron microscopy (HRTEM). The fundamental electrochemical performances are examined using cyclic voltammetry (CV).

Preparation, crystal structure and enhanced bipolar response of 0.90BLNT-0.10BCT lead-free piezoceramics

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

Pal, Vijayeta, E-mail: vijayetapal@yahoo.in; Dwivedi, R. K.; Kumar, A.

2016-05-06

In the present work, a solid solution of lead free 0.90[(Bi{sub 0.96}La{sub 0.04}){sub 0.5}Na{sub 0.5}TiO{sub 3}]-0.10(Ba{sub 0.90}Ca{sub 0.10}TiO{sub 3}] (abbreviated as 0.90BLNT-0.10BCT) piezoceramics has been synthesized by semi-wet technique. X-ray diffraction pattern confirms the phase formation. Rietveld refinement of XRD data demonstrates the coexistence of rhombhohedral (R3c) + tetragonal (P4mm) phase at room temperature. Raman spectrum is also support the above analysis. A large enhancement in bipolar strain of 0.12 % and calculated normalized strain, d*{sub 33} (defined as S{sub max}/E{sub max}) ~ 265 pm/V at 40kV/cm has been observed for this composition as compared to pure BLNT specimen, whichmore » make possible it as a potential lead-free candidates for piezoelectric applications.« less

Synthesis of quaternary chalcogenide CZTS nanoparticles by a hydrothermal route

NASA Astrophysics Data System (ADS)

Das, S.; Sa, K.; Mahakul, P. C.; Raiguru, J.; Alam, I.; Subramanyam, BVRS; Mahanandia, P.

2018-03-01

Cu2ZnSnS4 (CZTS) has emerged as a potential absorber towards inorganic photovoltaic device application for its outstanding properties like non toxicity, earth abundancy nature, optimal band gap matched with solar spectrum (1.45- 1.65eV), high absorption coefficient (104cm‑1). Here, a low cost, environment friendly facile hydrothermal route to synthesize phase pure CZTS nanoparticles using Cu (II), Zn (II), Sn (II) inorganic metal salts and thiourea as Sulphur source in distilled water solution as precursor is reported. The as synthesized samples characterized by X-Ray diffraction (XRD) and RAMAN confirmed structure and phase of CZTS nanocrystals. The morphology of the prepared CZTS have been characterized by scanning electron microscopy (SEM). The particle size is found in the range 4-5 nm with crystalline nature have been characterized by transmission electron microscope (TEM). The optical band gap of the as prepared samples is calculated to be 1.65eV from UV-Visible analysis which proves it can be used towards photovoltaic applications.

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

PubMed

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

2018-02-15

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

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

Physiochemical, Optical and Biological Activity of Chitosan-Chromone Derivative for Biomedical Applications

PubMed Central

Kumar, Santosh; Koh, Joonseok

2012-01-01

This paper describes the physiochemical, optical and biological activity of chitosan-chromone derivative. The chitosan-chromone derivative gels were prepared by reacting chitosan with chromone-3-carbaldehyde, followed by solvent exchange, filtration and drying by evaporation. The identity of Schiff base was confirmed by UV-Vis absorption spectroscopy and Fourier-transform infrared (FTIR) spectroscopy. The chitosan-chromone derivative was evaluated by X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), photoluminescence (PL) and circular dichroism (CD). The CD spectrum showed the chitosan-chromone derivative had a secondary helical structure. Microbiological screening results demonstrated the chitosan-chromone derivative had antimicrobial activity against Escherichia coli bacteria. The chitosan-chromone derivative did not have any adverse effect on the cellular proliferation of mouse embryonic fibroblasts (MEF) and did not lead to cellular toxicity in MEFs. These results suggest that the chitosan-chromone derivative gels may open a new perspective in biomedical applications. PMID:22754352

Synthesis and Photoluminescence of Single-Crystalline Fe(III)-Doped CdS Nanobelts.

PubMed

Kamran, Muhammad Arshad; Zou, Bingsuo; Majid, A; Alharbil, Thamer; Saeed, M A; Abdullah, Ali; Javed, Qurat-ul-ain

2016-04-01

In this paper, we report the synthesis and optical properties of Fe(III) doped CdS nanobelts (NBs) via simple Chemical Vapor Deposition (CVD) technique to explore their potential in nano-optics. The energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) analysis manifested the presence of Fe(III) ions in the NBs subsequently confirmed by the peak shifting to lower phonon energies as recorded by Raman spectra and shorter lifetime in ns. Photoluminescence (PL) spectrum investigations of the single Fe(III)-doped CdS NBs depicted an additional PL peak centered at 573 nm (orange emission) in addition to the bandedge(BE) emission. The redshift and decrease in the BE intensity of the PL peaks, as compared to the bulk CdS, confirmed the quenching of spectra upon Fe doping. The synthesis and orange emission for Fe-doped CdS NBs have been observed for the first time and point out their potential in nanoscale devices.

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

NASA Astrophysics Data System (ADS)

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

2011-05-01

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

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.

The effect of reaction temperature on the particle size of bismuth oxide nanoparticles synthesized via hydrothermal method

NASA Astrophysics Data System (ADS)

Zulkifli, Zulfa Aiza; Razak, Khairunisak Abdul; Rahman, Wan Nordiana Wan Abdul

2018-05-01

Bismuth oxide (Bi2O3) nanoparticles have been synthesized at different temperatures from 70 to 120˚C without any subsequent heat treatment using hydrothermal method. The particle size, and crystal structure of as-synthesized particles were investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), Energy-dispersive X-ray spectroscopy (EDX) and Fourier transform Infra-Red (FTIR). The nanoparticles are of a pure moniclinic Bi2O3 phase with rods shape. The average size of nanoparticles increases with the increase of reaction temperature. It was clear that longer reaction temperature allows precipitation completely occured and form larger nanoparticles (NPs). The crystallinity of Bi2O3 also are of high purity even at lower reaction temperature. The FTIR spectrum showed the absorption band at 845 cm-1 which is attributed to Bi-O-Bi bond, and the strong absorption band recorded at 424 cm-1 that is due to the stretching mode of Bi-O.

Infrared and infrared emission spectroscopic study of typical Chinese kaolinite and halloysite.

PubMed

Cheng, Hongfei; Frost, Ray L; Yang, Jing; Liu, Qinfu; He, Junkai

2010-12-01

The structure and thermal stability between typical Chinese kaolinite and halloysite were analysed by X-ray diffraction (XRD), infrared spectroscopy, infrared emission spectroscopy (IES) and Raman spectroscopy. Infrared emission spectroscopy over the temperature range of 300-700°C has been used to characterise the thermal decomposition of both kaolinite and halloysite. Halloysite is characterised by two bands in the water bending region at 1629 and 1648 cm(-1), attributed to structural water and coordinated water in the interlayer. Well defined hydroxyl stretching bands at around 3695, 3679, 3652 and 3625 cm(-1) are observed for both kaolinite and halloysite. The 550°C infrared emission spectrum of halloysite is similar to that of kaolinite in 650-1350 cm(-1) spectral region. The infrared emission spectra of halloysite were found to be considerably different to that of kaolinite at lower temperatures. These differences are attributed to the fundamental difference in the structure of the two minerals. Copyright © 2010 Elsevier B.V. All rights reserved.

Trimethylamine Sensors Based on Au-Modified Hierarchical Porous Single-Crystalline ZnO Nanosheets

PubMed Central

Zheng, Hanxiong; Sun, Yufeng; Li, Minqiang; Liu, Jinhuai

2017-01-01

It is of great significance for dynamic monitoring of foods in storage or during the transportation process through on-line detecting trimethylamine (TMA). Here, TMA were sensitively detected by Au-modified hierarchical porous single-crystalline ZnO nanosheets (HPSCZNs)-based sensors. The HPSCZNs were synthesized through a one-pot wet-chemical method followed by an annealing treatment. Polyethyleneimine (PEI) was used to modify the surface of the HPSCZNs, and then the PEI-modified samples were mixed with Au nanoparticles (NPs) sol solution. Electrostatic interactions drive Au nanoparticles loading onto the surface of the HPSCZNs. The Au-modified HPSCZNs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive spectrum (EDS), respectively. The results show that Au-modified HPSCZNs-based sensors exhibit a high response to TMA. The linear range is from 10 to 300 ppb; while the detection limit is 10 ppb, which is the lowest value to our knowledge. PMID:28640226

Spectroscopic investigations on the orientation of 1,4-dibromonaphthalene on silver nanoparticles.

PubMed

Geetha, K; Umadevi, M; Sathe, G V; Erenler, R

2013-12-01

Silver nanoparticles (Ag NPs) have been prepared by solution combustion method with glycine as fuel. Silver nanoparticles were characterized by X-Ray Diffraction (XRD), High Resolution Transmission Electron Microscopy (HRTEM) and UV-visible spectroscopy. The prepared silver nanoparticles exhibit cubic crystalline structure with grain size of 59 nm. HRTEM image shows that the silver nanoparticles have strain and four-fold symmetry formed by twinning in the crystal structure. The optical adsorption spectrum shows that the surface plasmon resonance peak of silver is observed at 380 nm. The orientation of 1,4-dibromonaphthlaene (1,4-DBrN) on silver nanoparticles has been inferred from nRs and SERS spectral features. The absence of a C-H stretching vibrations, the observed high intense C-H out-of-plane bending modes and high intense C-Br stretching vibration suggest that the 1,4-DBrN molecule may be adsorbed in a 'stand-on' orientation to the surface. Copyright © 2013 Elsevier B.V. All rights reserved.

Elucidation of reaction mechanism involved in the formation of LaNiO3 from XRD and TG analysis

NASA Astrophysics Data System (ADS)

Dharmadhikari, Dipti V.; Athawale, Anjali A.

2013-06-01

The present work is focused on the synthesis and elucidation of reaction mechanism involved in the formation of LaNiO3 with the help of X-ray diffraction (XRD) and thermogravimetric (TG) analysis. LaNiO3 was synthesized by hydrothermal method by heating at 160°C under autogenous pressure for 6h. Pure phase product was obtained after calcining the hydrothermally activated product for 6h at 700°C. The various phases of the product obtained after hydrothermal treatment and calcination followed by the formation of pure phase nanocrystalline lanthanum nickel oxide could be determined from XRD analysis of the samples. The reaction mechanism and phase formation temperature has been interpreted by thermogravimetric analysis of the hydrothermally synthesized product and XRD analysis.

High temperature XRD of Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4}

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

Chetty, Raju, E-mail: rcmallik@physics.iisc.ernet.in; Mallik, Ramesh Chandra, E-mail: rcmallik@physics.iisc.ernet.in

2014-04-24

Quaternary compound with chemical composition Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4} is prepared by solid state synthesis. High temperature XRD (X-Ray Diffraction) of this compound is used in studying the effect of temperature on lattice parameters and thermal expansion coefficients. Thermal expansion coefficient is one of the important quantities in evaluating the Grüneisen parameter which further useful in determining the lattice thermal conductivity of the material. The high temperature XRD of the material revealed that the lattice parameters as well as thermal expansion coefficients of the material increased with increase in temperature which confirms the presence of anharmonicty.

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.

Cooperative use of VCD and XRD for the determination of tetrahydrobenzoisoquinolines absolute configuration: a reliable proof of memory of chirality and retention of configuration in enediyne rearrangements.

PubMed

Mondal, Shovan; Naubron, Jean-Valère; Campolo, Damien; Giorgi, Michel; Bertrand, Michéle P; Nechab, Malek

2013-12-01

The absolute configurations (AC) of azaheterocylic compounds resulting from the cascade rearrangement of enediynes involving only light atoms were unambiguously assigned by the joint use of vibrational circular dichroism (VCD) and copper radiation single crystal X-ray diffraction (XRD). These AC determinations proved that the rearrangements of enediynes proceeded with memory of chirality and retention of configuration. © 2013 Wiley Periodicals, Inc.

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

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Tong, Guoquan

2015-10-01

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

Classification of crystal structure using a convolutional neural network

PubMed Central

Park, Woon Bae; Chung, Jiyong; Sohn, Keemin; Pyo, Myoungho

2017-01-01

A deep machine-learning technique based on a convolutional neural network (CNN) is introduced. It has been used for the classification of powder X-ray diffraction (XRD) patterns in terms of crystal system, extinction group and space group. About 150 000 powder XRD patterns were collected and used as input for the CNN with no handcrafted engineering involved, and thereby an appropriate CNN architecture was obtained that allowed determination of the crystal system, extinction group and space group. In sharp contrast with the traditional use of powder XRD pattern analysis, the CNN never treats powder XRD patterns as a deconvoluted and discrete peak position or as intensity data, but instead the XRD patterns are regarded as nothing but a pattern similar to a picture. The CNN interprets features that humans cannot recognize in a powder XRD pattern. As a result, accuracy levels of 81.14, 83.83 and 94.99% were achieved for the space-group, extinction-group and crystal-system classifications, respectively. The well trained CNN was then used for symmetry identification of unknown novel inorganic compounds. PMID:28875035

Classification of crystal structure using a convolutional neural network.

PubMed

Park, Woon Bae; Chung, Jiyong; Jung, Jaeyoung; Sohn, Keemin; Singh, Satendra Pal; Pyo, Myoungho; Shin, Namsoo; Sohn, Kee-Sun

2017-07-01

A deep machine-learning technique based on a convolutional neural network (CNN) is introduced. It has been used for the classification of powder X-ray diffraction (XRD) patterns in terms of crystal system, extinction group and space group. About 150 000 powder XRD patterns were collected and used as input for the CNN with no handcrafted engineering involved, and thereby an appropriate CNN architecture was obtained that allowed determination of the crystal system, extinction group and space group. In sharp contrast with the traditional use of powder XRD pattern analysis, the CNN never treats powder XRD patterns as a deconvoluted and discrete peak position or as intensity data, but instead the XRD patterns are regarded as nothing but a pattern similar to a picture. The CNN interprets features that humans cannot recognize in a powder XRD pattern. As a result, accuracy levels of 81.14, 83.83 and 94.99% were achieved for the space-group, extinction-group and crystal-system classifications, respectively. The well trained CNN was then used for symmetry identification of unknown novel inorganic compounds.

Tensile stress effect on epitaxial BiFeO 3 thin film grown on KTaO 3

DOE PAGES

Bae, In-Tae; Ichinose, Tomohiro; Han, Myung-Geun; ...

2018-01-17

Comprehensive crystal structural study is performed for BiFeO 3 (BFO) film grown on KTaO 3 (KTO) substrate using transmission electron microscopy (TEM) and x-ray diffraction (XRD). Nano beam electron diffraction (NBED) combined with structure factor calculation and high resolution TEM images clearly reveal that the crystal structure within BFO thin film is rhombohedral BFO, i.e., bulk BFO phase. Epitaxial relationship found by NBED indicates the BFO film grows in a manner that minimizes lattice mismatch with KTO. It further suggests BFO film is under slight biaxial tensile stress (~0.35%) along in-plane direction. XRD reveals BFO lattice is under compressive stressmore » (~1.6%), along out-of-plane direction as a result of the biaxial tensile stress applied along in-plane direction. This leads to Poisson’s ratio of ~0.68. In addition, we demonstrate (1) why hexagonal notation rather than pseudocubic one is required for accurate BFO phase evaluation and (2) a new XRD method that shows how rhombohedral BFO can readily be identified among other phases by measuring a rhombohedral specific Bragg’s peak.« less

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.

XRD and FTIR structural investigation of gadolinium-zinc-borate glass ceramics

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

Borodi, G.; Pascuta, P.; Dan, V.

2013-11-13

X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy measurements have been employed to investigate the (Gd{sub 2}O{sub 3}){sub x}⋅(B{sub 2}O{sub 3}){sub (60−x)}⋅(ZnO){sub 40} glass ceramics system, with 0 ≤ x ≤ 15 mol%. After heat treatment applied at 860 °C for 2 h, some structural changes were observed and new crystalline phases appeared in the structure of the samples. In these glass ceramics four crystalline phases were identified using powder diffraction files (PDF 2), namely ZnB{sub 4}O{sub 7}, Zn{sub 4}O(B{sub 6}O{sub 12}), Zn{sub 3}(BO{sub 3}){sub 2} and GdBO{sub 3}. From the XRD data, the average unit-cell parameter and themore » quantitative ratio of the crystallographic phases in the studied samples were evaluated. FTIR data revealed that the BO{sub 3}, BO{sub 4} and ZnO{sub 4} are the main structural units of these glass ceramics network. The compositional dependence of the different structural units which appear in the studied samples was followed.« less

Tensile stress effect on epitaxial BiFeO 3 thin film grown on KTaO 3

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

Bae, In-Tae; Ichinose, Tomohiro; Han, Myung-Geun

Comprehensive crystal structural study is performed for BiFeO 3 (BFO) film grown on KTaO 3 (KTO) substrate using transmission electron microscopy (TEM) and x-ray diffraction (XRD). Nano beam electron diffraction (NBED) combined with structure factor calculation and high resolution TEM images clearly reveal that the crystal structure within BFO thin film is rhombohedral BFO, i.e., bulk BFO phase. Epitaxial relationship found by NBED indicates the BFO film grows in a manner that minimizes lattice mismatch with KTO. It further suggests BFO film is under slight biaxial tensile stress (~0.35%) along in-plane direction. XRD reveals BFO lattice is under compressive stressmore » (~1.6%), along out-of-plane direction as a result of the biaxial tensile stress applied along in-plane direction. This leads to Poisson’s ratio of ~0.68. In addition, we demonstrate (1) why hexagonal notation rather than pseudocubic one is required for accurate BFO phase evaluation and (2) a new XRD method that shows how rhombohedral BFO can readily be identified among other phases by measuring a rhombohedral specific Bragg’s peak.« 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.

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.

Residual stresses in continuous graphite fiber Al metal matrix composites

NASA Technical Reports Server (NTRS)

Park, Hun Sub; Zong, Gui Sheng; Marcus, Harris L.

1988-01-01

The residual stresses in graphite fiber reinforced aluminum (Gr/Al) composites with various thermal histories are measured using X-ray diffraction (XRD) methods. The XRD stress analysis is based on the determination of lattice strains by precise measurements of the interplanar spacings in different directions of the sample. The sample is a plate consisting of two-ply P 100 Gr/Al 6061 precursor wires and Al 6061 overlayers. Prior to XRD measurement, the 6061 overlayers are electrochemically removed. In order to calibrate the relationship between stress magnitude and lattice spacing shift, samples of Al 6061 are loaded at varying stress levels in a three-point bend fixture, while the stresses are simultaneously determined by XRD and surface-attached strain gages. The stresses determined by XRD closely match those determined by the strain gages. Using these calibrations, the longitudinal residual stresses of P 100 Gr/Al 6061 composites are measured for various heat treatments, and the results are presented.

Collimation testing using slit Fresnel diffraction

NASA Astrophysics Data System (ADS)

Luo, Xiaohe; Hui, Mei; Wang, Shanshan; Hou, Yinlong; Zhou, Siyu; Zhu, Qiudong

2018-03-01

A simple collimation testing method based on slit Fresnel diffraction is proposed. The method needs only a CMOS and a slit with no requirement in dimensional accuracy. The light beam to be tested diffracts across the slit and forms a Fresnel diffraction pattern received by CMOS. After analysis, the defocusing amount and the distance between the primary peak point and secondary peak point of diffraction pattern fulfill an expression relationship and then the defocusing amount can be deduced from the expression. The method is applied to both the coherent beam and partially coherent beam, and these two beams are emitted from a laser and light-emitting diode (LED) with a spectrum width of about 50 nm in this paper. Simulations show that the wide spectrum of LED has the effect of smooth filtering to provide higher accuracy. Experiments show that the LED with a spectrum width of about 50 nm has a lower limitation error than the laser and can achieve up to 58.1601 μm with focal length 200 mm and slit width 15 mm.

A quantitative X-ray diffraction inventory of the tephra and volcanic glass inputs into the Holocene marine sediment archives off Iceland: A contribution to V.A.S.T.

USGS Publications Warehouse

Andrews, John T.; Kristjansdottir, Greta B.; Eberl, Dennis D.; Jennings, Anne E.

2013-01-01

This paper re-evaluates how well quantitative x-ray diffraction (qXRD) can be used as an exploratory method of the weight percentage (wt%) of volcaniclastic sediment, and to identify tephra events in marine cores. In the widely used RockJock v6 software programme, qXRD tephra and glass standards include the rhyodacite White River tephra (Alaska), a rhyolitic tephra (Hekla-4) and the basaltic Saksunarvatn tephra. Experiments of adding known wt% of tephra to felsic bedrock samples indicated that additions ≥10 wt% are accurately detected, but reliable estimates of lesser amounts are masked by amorphous material produced by milling. Volcaniclastic inputs range between 20 and 50 wt%. Primary tephra events are identified as peaks in residual qXRD glass wt% from fourth-order polynomial fits. In cores where tephras have been identified by shard counts in the > 150 µm fraction, there is a positive correlation (validation) with peaks in the wt% glass estimated by qXRD. Geochemistry of tephra shards confirms the presence of several Hekla-sourced tephras in cores B997-317PC1 and -319PC2 on the northern Iceland shelf. In core B997-338 (north-west Iceland), there are two rhyolitic tephras separated by ca. 100 cm with uncorrected radiocarbon dates on articulated shells of around 13 000 yr B.P. These tephras may be correlatives of the Borrobol and Penifiler tephras found in Scotland. The number of Holocene tephra events per 1000 yr was estimated from qXRD on 16 cores and showed a bimodal distribution with an increased number of events in both the late and early Holocene.

Revisiting the hydration structure of aqueous Na +

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

Galib, M.; Baer, M. D.; Skinner, L. B.

In this paper, a combination of theory, X-ray diffraction (XRD) and extended x-ray absorption fine structure (EXAFS) are used to probe the hydration structure of aqueous Na +. The high spatial resolution of the XRD measurements corresponds to Qmax = 24 Å –1 while the first-reported Na K-edge EXAFS measurements have a spatial resolution corresponding to 2k = Qmax = 16 Å –1. Both provide an accurate measure of the shape and position of the first peak in the Na–O pair distribution function, g NaO(r). The measured Na–O distances of 2.384 ± 0.003 Å (XRD) and 2.37 ± 0.024 Åmore » (EXAFS) are in excellent agreement. These measurements show a much shorter Na–O distance than generally reported in the experimental literature (Na–O avg ~ 2.44 Å) although the current measurements are in agreement with recent neutron diffraction measurements. The measured Na–O coordination number from XRD is 5.5 ± 0.3. The measured structure is compared with both classical and first-principles density functional theory (DFT) simulations. Both of the DFT-based methods, revPBE and BLYP, predict a Na–O distance that is too long by about 0.05 Å with respect to the experimental data (EXAFS and XRD). The inclusion of dispersion interactions (–D3 and –D2) significantly worsens the agreement with experiment by further increasing the Na–O distance by 0.07 Å. In contrast, the use of a classical Na–O Lennard-Jones potential with SPC/E water accurately predicts the Na–O distance as 2.39 Å although the Na–O peak is over-structured with respect to experiment.« less

Revisiting the hydration structure of aqueous Na +

DOE PAGES

Galib, M.; Baer, M. D.; Skinner, L. B.; ...

2017-02-27

In this paper, a combination of theory, X-ray diffraction (XRD) and extended x-ray absorption fine structure (EXAFS) are used to probe the hydration structure of aqueous Na +. The high spatial resolution of the XRD measurements corresponds to Qmax = 24 Å –1 while the first-reported Na K-edge EXAFS measurements have a spatial resolution corresponding to 2k = Qmax = 16 Å –1. Both provide an accurate measure of the shape and position of the first peak in the Na–O pair distribution function, g NaO(r). The measured Na–O distances of 2.384 ± 0.003 Å (XRD) and 2.37 ± 0.024 Åmore » (EXAFS) are in excellent agreement. These measurements show a much shorter Na–O distance than generally reported in the experimental literature (Na–O avg ~ 2.44 Å) although the current measurements are in agreement with recent neutron diffraction measurements. The measured Na–O coordination number from XRD is 5.5 ± 0.3. The measured structure is compared with both classical and first-principles density functional theory (DFT) simulations. Both of the DFT-based methods, revPBE and BLYP, predict a Na–O distance that is too long by about 0.05 Å with respect to the experimental data (EXAFS and XRD). The inclusion of dispersion interactions (–D3 and –D2) significantly worsens the agreement with experiment by further increasing the Na–O distance by 0.07 Å. In contrast, the use of a classical Na–O Lennard-Jones potential with SPC/E water accurately predicts the Na–O distance as 2.39 Å although the Na–O peak is over-structured with respect to experiment.« less

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

Zhang, Baozhuo; Young, Marcus L.

Many technological applications of austenitic shape memory alloys (SMAs) involve cyclical mechanical loading and unloading in order to take advantage of pseudoelasticity. In this paper, we investigated the effect of mechanical bending of pseudoelastic NiTi SMA wires using high-energy synchrotron radiation X-ray diffraction (SR-XRD). Differential scanning calorimetry was performed to identify the phase transformation temperatures. Scanning electron microscopy images show that micro-cracks in compressive regions of the wire propagate with increasing bend angle, while tensile regions tend not to exhibit crack propagation. SR-XRD patterns were analyzed to study the phase transformation and investigate micromechanical properties. By observing the various diffraction peaks such as the austenite (200) and the martensite (more » $${\\bar 1}12$$), ($${\\bar 1}03$$), ($${\\bar 1}11$$), and (101) planes, intensities and residual strain values exhibit strong anisotropy, depending upon whether the sample is in compression or tension during bending.« less

Study of Initial Stages of Ball-Milling of Cu Powder Using X-ray Diffraction

NASA Astrophysics Data System (ADS)

Gayathri, N.; Mukherjee, Paramita

2018-04-01

The initial stage of size refinement of Cu powder is studied using detailed X-ray diffraction (XRD) analysis to understand the mechanism of formation of nanomaterials during the ball-milling process. The study was restricted to samples obtained for milling time up to 240 min to understand the deformation mechanism at the early stages of ball milling. Various model based approaches for the analysis of the XRD were used to study the evolution of the microstructural parameters such as domain size and microstrain along the different crystallographic planes. It was seen that the domain size saturates at a low value along the (311) plane whereas the size along the (220) and (200) plane is still higher. The r.m.s microstrain showed a non-monotonic change along the different crystallographic directions up to the milling time of 240 min.

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

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

Stan, Manuela, E-mail: manuela.stan@itim-cj.ro; Popa, Adriana; Toloman, Dana

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn{sup 2+} ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes andmore » oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs.« less

Body-centered orthorhombic C 16 : A novel topological node-line semimetal

DOE PAGES

Wang, Jian -Tao; Weng, Hongming; Nie, Simin; ...

2016-05-11

We identify by ab initio calculations a novel topological semimetal carbon phase in all-sp 2 bonding networks with a 16-atom body-centered orthorhombic unit cell, termed bco-C 16. Total-energy calculations show that bco-C 16 is comparable to solid fcc-C 60 in energetic stability, and phonon and molecular dynamics simulations confirm its dynamical stability. This all-sp 2 carbon allotrope can be regarded as a three-dimensional modification of graphite, and its simulated x-ray diffraction (XRD) pattern matches well a previously unexplained diffraction peak in measured XRD spectra of detonation and chimney soot, indicating its presence in the specimen. Electronic band structure calculations revealmore » that bco-C 16 is a topological node-line semimetal with a single nodal ring. Lastly, these findings establish a novel carbon phase with intriguing structural and electronic properties of fundamental significance and practical interest.« less

Characterization of cubic ceria?zirconia powders by X-ray diffraction and vibrational and electronic spectroscopy

NASA Astrophysics Data System (ADS)

Sánchez Escribano, Vicente; Fernández López, Enrique; Panizza, Marta; Resini, Carlo; Gallardo Amores, José Manuel; Busca, Guido

2003-10-01

The X-ray diffraction (XRD) patterns and the Infrared, Raman and UV-visible spectra of CeO 2ZrO 2 powders prepared by co-precipitation are presented. Raman spectra provide evidence for the largely predominant cubic structure of the powders with CeO 2 molar composition higher than 25%. Also skeletal IR spectra allow to distinguish cubic from tetragonal phases which are instead not easily distinguished on the basis of the XRD patterns. All mixed oxides including pure ceria are strong UV absorbers although also absorb in the violet visible region. By carefully selecting their composition and treatment temperature, the onset of the radiation that they cut off can be chosen in the 425-475 nm interval. Although they are likely metastable, the cubic phases are still pure even after heating at 1173 K for 4 h.

A photodiode based on PbS nanocrystallites for FYTRONIX solar panel automatic tracking controller

NASA Astrophysics Data System (ADS)

Wageh, S.; Farooq, W. A.; Tataroğlu, A.; Dere, A.; Al-Sehemi, Abdullah G.; Al-Ghamdi, Ahmed A.; Yakuphanoglu, F.

2017-12-01

The structural, optical and photoelectrical properties of the fabricated Al/PbS/p-Si/Al photodiode based on PbS nanocrystallites were investigated. The PbS nanocrystallites were characterized by X-ray diffraction (XRD), UV-VIS-NIR, Infrared and Raman spectroscopy. The XRD diffraction peaks show that the prepared PbS nanostructure is in high crystalline state. Various electrical parameters of the prepared photodiode were analyzed from the electrical characteristics based on I-V and C-V-G. The photodiode has a high rectification ratio of 5.85×104 at dark and ±4 V. Moreover, The photocurrent results indicate a strong photovoltaic behavior. The frequency dependence of capacitance and conductance characteristics was attributed to depletion region behavior of the photodiode. The diode was used to control solar panel power automatic tracking controller in dual axis. The fabricated photodiode works as a photosensor to control Solar tracking systems.

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

NASA Astrophysics Data System (ADS)

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

2016-01-01

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

Sodium storage mechanisms of bismuth in sodium ion batteries: An operando X-ray diffraction study

NASA Astrophysics Data System (ADS)

Gao, Hui; Ma, Wensheng; Yang, Wanfeng; Wang, Jiawei; Niu, Jiazheng; Luo, Fakui; Peng, Zhangquan; Zhang, Zhonghua

2018-03-01

Understanding the sodium (Na) chemistry is crucial for development of high-performance sodium ion batteries (SIBs). Nanostructured bismuth (Bi) has shown great potentials as an anode in SIBs, however, the Na storage mechanisms of Bi are still unclear. Herein, the operando X-ray diffraction (XRD) technique was utilized to probe the Na storage mechanisms of three Bi anodes (sputtered Bi film, nanoporous Bi and commercial Bi). Despite different morphologies and sizes, all the Bi anodes follow the same two-step reversible alloying/dealloying mechanisms (Bi ↔ NaBi ↔ Na3Bi) during the discharge/charge processes, associated with two voltage plateaus. As for the intercalation/deintercalation mechanism proposed for nanostructured Bi anodes in SIBs, we rationalize the reason why only the Bi phase is detected in the discharged/charged samples under ex-situ XRD conditions through addressing the stability issue of the Na-Bi system (NaBi and Na3Bi).

Disruption of crystalline structure of Sn3.5Ag induced by electric current

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

Huang, Han-Chie; Lin, Kwang-Lung, E-mail: matkllin@mail.ncku.edu.tw; Wu, Albert T.

2016-03-21

This study presented the disruption of the Sn and Ag{sub 3}Sn lattice structures of Sn3.5Ag solder induced by electric current at 5–7 × 10{sup 3} A/cm{sup 2} with a high resolution transmission electron microscope investigation and electron diffraction analysis. The electric current stressing induced a high degree of strain on the alloy, as estimated from the X-ray diffraction (XRD) peak shift of the current stressed specimen. The XRD peak intensity of the Sn matrix and the Ag{sub 3}Sn intermetallic compound diminished to nearly undetectable after 2 h of current stressing. The electric current stressing gave rise to a high dislocation density ofmore » up to 10{sup 17}/m{sup 2}. The grain morphology of the Sn matrix became invisible after prolonged current stressing as a result of the coalescence of dislocations.« less

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.

Hepatoprotective effect of engineered silver nanoparticles coated bioactive compounds against diethylnitrosamine induced hepatocarcinogenesis in experimental mice.

PubMed

Prasannaraj, Govindaraj; Venkatachalam, Perumal

2017-02-01

Nanoparticle based drug delivery can rapidly improves the therapeutic potential of anti-cancer agents. The present study focused to evaluate the hepatoprotective activity of silver nanoparticles (AgNPs) synthesized using aqueous extracts of Andrographis paniculata leaves (ApAgNPs) and Semecarpus anacardium nuts (SaAgNPs) against diethylnitrosamine (DEN) induced liver cancer in mice model. The physico-chemical properties of synthesized AgNPs were characterized by Fourier transform infrared (FTIR) spectroscopy, Transmission Electron Microscopy (TEM), Selected Area Electron Diffraction (SAED), X-ray Diffraction (XRD), Energy Dispersive X-ray (EDX) spectrum, Zeta potential and Dynamic Light Scattering (DLS) analysis. The surface plasmon resonance (SPR) absorption spectrum revealed a strong peak at 420nm for both SaAgNPs and ApAgNPs. FTIR results exhibited the presence of possible functional groups in the synthesized AgNPs. TEM analysis determined the hexagonal, and spherical shape of the synthesized silver nanoparticles. The XRD and SAED pattern confirmed the crystalline nature and crystalline size of the AgNPs. EDX result clearly showed strong silver signals in the range between 2 and 4keV. Zeta potential measurements indicated a sharp peak at -3.93 and -13.8mV for ApAgNPs and SaAgNPs, respectively. DLS measurement expressed the particle size distribution was 70 and 60nm for ApAgNPs and SaAgNPs, respectively. DEN (20mg/kg b.wt.) was subjected to induce liver cancer in mice for 8weeks and treated with biosynthesized silver nanoparticles. Interestingly, ApAgNPs and SaAgNPs treated DEN induced animal groups show a decreased level of aspartate amino transferase (AST), alanine amino transferase (ALT), serum glutamate oxaloacetate transaminase (SGOT), serum glutamate pyruvate transaminase (SGPT) activity and elevated level of catalase (CAT), glutathione peroxidase (GPx), glutathione S-transferase (GST) and superoxide dismutase (SOD) activity over untreated DEN control animals group. Histopathological investigation reveals decreased fat accumulation, appearance of binucleated cells in nanoparticle treated animals and showed mere normal cells induced by DEN. Argyrophilic nucleolar organiser region (AgNORs) had a significant decrease in number of acidic proteins and mast cells assay showed decrease of metachromatic cells in nanoparticles treated animal groups over control. Present results strongly suggest that biomolecule coated silver nanoparticles exposure showed potential hepatoprotective effect against DEN induced liver cancer and could be used as an effective anticancer nanodrug. Copyright © 2017. Published by Elsevier B.V.

Growth and characterization of an organic single crystal: 2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide

NASA Astrophysics Data System (ADS)

Senthil, K.; Kalainathan, S.; Ruban Kumar, A.

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. 1H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker’s hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal.

Growth and characterization of an organic single crystal: 2-[2-(4-diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide.

PubMed

Senthil, K; Kalainathan, S; Ruban Kumar, A

2014-05-05

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. (1)H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker's hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal. Copyright © 2014 Elsevier B.V. All rights reserved.

XRD and mineralogical analysis of gypsum dunes at White Sands National Monument, New Mexico and applications to gypsum detection on Mars

NASA Astrophysics Data System (ADS)

Lafuente, B.; Bishop, J. L.; Fenton, L. K.; King, S. J.; Blake, D.; Sarrazin, P.; Downs, R.; Horgan, B. H.

2013-12-01

A field portable X-ray Diffraction (XRD) instrument was used at White Sands National Monument to perform in-situ measurements followed by laboratory analyses of the gypsum-rich dunes and to determine its modal mineralogy. The field instrument is a Terra XRD (Olympus NDT) based on the technology of the CheMin (Chemistry and Mineralogy) instrument onboard the Mars Science Laboratory (MSL) rover Curiosity which is providing the mineralogical and chemical composition of scooped soil samples and drilled rock powders collected at Gale Crater [1]. Using Terra at White Sands will contribute to 'ground truth' for gypsum-bearing environments on Mars. Together with data provided by VNIR spectra [2], this study clarifies our understanding of the origin and history of gypsum-rich sand dunes discovered near the northern polar region of Mars [3]. The results obtained from the field analyses performed by XRD and VNIR spectroscopy in four dunes at White Sands revealed the presence of quartz and dolomite. Their relative abundance has been estimated using the Reference Intensity Ratio (RIR) method. For this study, particulate samples of pure natural gypsum, quartz and dolomite were used to prepare calibration mixtures of gypsum-quartz and gypsum-dolomite with the 90-150μm size fractions. All single phases and mixtures were analyzed by XRD and RIR factors were calculated. Using this method, the relative abundance of quartz and dolomite has been estimated from the data collected in the field. Quartz appears to be present in low amounts (2-5 wt.%) while dolomite is present at percentages up to 80 wt.%. Samples from four dunes were collected and prepared for subsequent XRD analysis in the lab to estimate their composition and illustrate the changes in mineralogy with respect to location and grain size. Gypsum-dolomite mixtures: The dolomite XRD pattern is dominated by an intense diffraction peak at 2θ≈36 deg. which overlaps a peak of gypsum, This makes low concentrations of dolomite difficult to quantify in mixtures with high concentration of gypsum. Dolomite has been detected in some locations at dune 3 as high as 80 wt.%. Gypsum-quartz mixtures: The intensity of the main diffraction peak of quartz at 2θ≈31 deg. decreases progressively with the decrease of the amount of quartz in the mixtures. Samples from dune 1 and 2 show quartz abundance at 5.6 and 2.6 wt.% respectively . [1] Blake et al. Space Sci. Rev. (2012). doi:10.1007/s11214-012-9905-1. [2] King et al. (2013) AGU, submitted. [3] Langevin et al. (2005). Science 307, 1584-1586.

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.

Controlling the Optical and Magnetic Properties of Nanostructured Cuprous Oxide Synthesized from Waste Electric Cables

NASA Astrophysics Data System (ADS)

Abdelbasir, S. M.; El-Sheikh, S. M.; Rashad, M. M.; Rayan, D. A.

2018-03-01

Cuprous oxide Cu2O nanopowders were purposefully synthesised from waste electric cables (WECs) via a simple precipitation route at room temperature using lactose as a reducing agent. In this regard, dimethyl sulfoxide (DMSO) was first applied as an organic solvent for the dissolution of the cable insulating materials. Several parameters were investigated during dissolution of WECs such as dissolution temperature, time and solid/liquid ratio to determine the dissolution percentage of the insulating materials in DMSO. The morphology and the optical properties of the formed Cu2O particles were investigated using X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), Fourier-transform infrared spectroscopy and UV-visible-near IR spectrophotometer. XRD data confirmed the presence of single crystalline phase of Cu2O nanoparticles. FE-SEM and TEM images revealed spherical, cubic and octahedral shapes with the various particle sizes ranged from 16 to 57 nm depending on the synthesis conditions. A possible mechanism explaining the Cu2O nanostructures formation was proposed. The band gap energies of the Cu2O nanostructures were estimated and the values were located between 1.5 and 2.08 eV. Photoluminescence spectroscopy analysis clearly showed a noticeably blue-shifted emission for the synthesized samples compared to spectrum of the bulk. Eventually, magnetic properties of the synthesized nanoparticles have been measured by vibrating sample magnetometer and the attained results implied that the synthesized particles are weakly ferromagnetic in nature at normal temperature.

Oxygen partial pressure effects on the RF sputtered p-type NiO hydrogen gas sensors

NASA Astrophysics Data System (ADS)

Turgut, Erdal; Çoban, Ömer; Sarıtaş, Sevda; Tüzemen, Sebahattin; Yıldırım, Muhammet; Gür, Emre

2018-03-01

NiO thin films were grown by Radio Frequency (RF) Magnetron Sputtering method under different oxygen partial pressures, which are 0.6 mTorr, 1.3 mTorr and 2.0 mTorr. The effects of oxygen partial pressures on the thin films were analyzed through Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS) and Hall measurements. The change in the surface morphology of the thin films has been observed with the SEM and AFM measurements. While nano-pyramids have been obtained on the thin film grown at the lowest oxygen partial pressure, the spherical granules lower than 60 nm in size has been observed for the samples grown at higher oxygen partial pressures. The shift in the dominant XRD peak is realized to the lower two theta angle with increasing the oxygen partial pressures. XPS measurements showed that the Ni2p peak involves satellite peaks and two oxidation states of Ni, Ni2+ and Ni3+, have been existed together with the corresponding splitting in O1s spectrum. P-type conductivity of the grown NiO thin films are confirmed by the Hall measurements with concentrations on the order of 1013 holes/cm-3. Gas sensor measurements revealed minimum of 10% response to the 10 ppm H2 level. Enhanced responsivity of the gas sensor devices of NiO thin films is shown as the oxygen partial pressure increases.

Modification of optical and electrical properties of zinc oxide-coated porous silicon nanostructures induced by swift heavy ion

PubMed Central

2012-01-01

Morphological and optical characteristics of radio frequency-sputtered zinc aluminum oxide over porous silicon (PS) substrates were studied before and after irradiating composite films with 130 MeV of nickel ions at different fluences varying from 1 × 1012 to 3 × 1013 ions/cm2. The effect of irradiation on the composite structure was investigated by scanning electron microscopy, X-ray diffraction (XRD), photoluminescence (PL), and cathodoluminescence spectroscopy. Current–voltage characteristics of ZnO-PS heterojunctions were also measured. As compared to the granular crystallites of zinc oxide layer, Al-doped zinc oxide (ZnO) layer showed a flaky structure. The PL spectrum of the pristine composite structure consists of the emission from the ZnO layer as well as the near-infrared emission from the PS substrate. Due to an increase in the number of deep-level defects, possibly oxygen vacancies after swift ion irradiation, PS-Al-doped ZnO nanocomposites formed with high-porosity PS are shown to demonstrate a broadening in the PL emission band, leading to the white light emission. The broadening effect is found to increase with an increase in the ion fluence and porosity. XRD study revealed the relative resistance of the film against the irradiation, i.e., the irradiation of the structure failed to completely amorphize the structure, suggesting its possible application in optoelectronics and sensing applications under harsh radiation conditions. PMID:22748164

Dielectric and magnetic studies of Cr+3 doped nickel ferrite by combustion method

NASA Astrophysics Data System (ADS)

Parveez, Asiya; Shekhawat, M. S.; Sindhu, S.; Srikanth, C.; Nayeem, Firdous; Mohd. Shariff, S.; Sinha, R. R.; Chaudhuri, Arka; Khader, S. Abdul

2018-05-01

Cr+3 doped nickel ferrite nanoparticles having the basic composition NiCrxFe2-xO4 (x=0, 0.1, 0.15, 0.2, 1) were prepared using auto combustion method. Structural, dielectric, a.c conductivity and magnetic properties of these samples, which are sintered at 800°C were studied. The structures of the synthesized samples were probed by X-ray diffraction (XRD) studies. The peaks observed in the XRD spectrum indicated single phase spinel cubic structure for the synthesized samples. Surface morphology of the samples has been investigated using Field Emission Scanning Electron Microscope (FESEM). The dielectric constant (ɛ') and dielectric loss factor (ɛ″) of nanocrystalline nickel ferrites were investigated as a function of frequency and Cr+3 concentration at room temperature over the frequency range 100 Hz to 1 MHz using Hioki make LCR Hi-Tester 3250. The dependence of ɛ' and ɛ″ with the frequency of the alternating applied electric field is in accordance with the Maxwell-Wagner type interfacial polarization, which is in agreement with the Koop's theory. The electrical conductivity (σac) deduced from the measured dielectric data has been thoroughly analyzed and found that the conduction mechanism in NiCrxFe2-xO4 nanoferrites are in conformity with the electron hopping model. The magnetic properties of Cr+3 doped nano-nickel ferrite were analyzed using a Vibrating Sample Magnetometer (VSM). It is observed that the values of saturation magnetization decreases along with the increase in chromium content.

Aloe vera extract functionalized zinc oxide nanoparticles as nanoantibiotics against multi-drug resistant clinical bacterial isolates.

PubMed

Ali, Khursheed; Dwivedi, Sourabh; Azam, Ameer; Saquib, Quaiser; Al-Said, Mansour S; Alkhedhairy, Abdulaziz A; Musarrat, Javed

2016-06-15

ZnO nanoparticles (ZnONPs) were synthesised through a simple and efficient biogenic synthesis approach, exploiting the reducing and capping potential of Aloe barbadensis Miller (A. vera) leaf extract (ALE). ALE-capped ZnO nanoparticles (ALE-ZnONPs) were characterized using UV-Vis spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) analyses. XRD analysis provided the average size of ZnONPs as 15 nm. FTIR spectral analysis suggested the role of phenolic compounds, terpenoids and proteins present in ALE, in nucleation and stability of ZnONPs. Flow cytometry and atomic absorption spectrophotometry (AAS) data analyses revealed the surface binding and internalization of ZnONPs in Gram +ve (Staphylococcus aureus) and Gram -ve (Escherichia coli) cells, respectively. Significant antibacterial activity of ALE-ZnONPs was observed against extended spectrum beta lactamases (ESBL) positive E. coli, Pseudomonas aeruginosa, and methicillin resistant S. aureus (MRSA) clinical isolates exhibiting the MIC and MBC values of 2200, 2400 μg/ml and 2300, 2700 μg/ml, respectively. Substantial inhibitory effects of ALE-ZnONPs on bacterial growth kinetics, exopolysaccharides and biofilm formation, unequivocally suggested the antibiotic and anti-biofilm potential. Overall, the results elucidated a rapid, environmentally benign, cost-effective, and convenient method for ALE-ZnONPs synthesis, for possible applications as nanoantibiotics or drug carriers. Copyright © 2016 Elsevier Inc. All rights reserved.

Impedance spectroscopy of the oxide films formed during high temperature oxidation of a cobalt-plated ferritic alloy

NASA Astrophysics Data System (ADS)

Velraj, S.; Zhu, J. H.; Painter, A. S.; Du, S. W.; Li, Y. T.

2014-02-01

Impedance spectroscopy was used to evaluate the oxide films formed on cobalt-coated Crofer 22 APU ferritic stainless steel after thermal oxidation at 800 °C in air for different times (i.e. 2, 50, 100 and 500 h). Impedance spectra of the oxide films exhibited two or three semicircles depending on the oxidation time, which correspond to the presence of two or three individual oxide layers. Coupled with scanning electron microscopy/energy-dispersive spectroscopy (SEM/EDS) and X-ray diffraction (XRD), the individual oxide layer corresponding to each semicircle was determined unambiguously. Impedance spectrum analysis of the oxide films formed on the sample after thermal exposure at 800 °C in air for 2 h led to the identification of the low-frequency and high-frequency semicircles as being from Cr2O3 and Co3O4, respectively. SEM/EDS and XRD analysis of the 500-h sample clearly revealed the presence of three oxide layers, analyzed to be Co3-xCrxO4, CoCr2O4, and Cr2O3. Although the SEM images of the 50-h and 100-h samples did not clearly show the CoCr2O4 layer, impedance plots implied their presence. The oxide scales were assigned to their respective semicircles and the electrical properties of Co3-xCrxO4, CoCr2O4 and Cr2O3 were determined from the impedance data.

Structural refinement, band-gap analysis and optical properties of GdAlO3 nanophosphors influenced by Dy3+ ion concentrations for white light emitting device applications

NASA Astrophysics Data System (ADS)

Jisha, P. K.; Naik, Ramachandra; Prashantha, S. C.; Nagaswarupa, H. P.; Nagabhushana, H.; Basavaraj, R. B.; Sharma, S. C.; Prasad, Daruka

2016-04-01

Nanosized GdAlO3 phosphors activated with Dy3+ were prepared by a combustion method. Synthesized phosphors were calcined at 1000 °C for 3 h in order to achieve crystallinity. Powder x-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis was used to characterize the prepared product. The orthorhombic phase was observed in the XRD pattern. The particle size of the samples was calculated as around 25 nm. The SEM images show an irregular shape of the prepared nanophosphor. Functional groups of the phosphors were examined by Fourier transform infrared (FTIR) spectroscopy. Photoluminescence (PL) properties of Dy3+ doped GdAlO3 for near-ultraviolet excitation (352 nm) were studied in order to investigate the possibility of its use in white light emitting device applications. Judd-Ofelt intensity parameters, radiative transition rate (A T) and radiative lifetimes (τ rad) were evaluated from the emission spectrum by adopting a standard procedure. The Commission International de l’Eclairage (CIE) color coordinates and correlated color temperature (CCT) are studied for the optimized phosphor. It is found that the color coordinates of Dy3+ doped GdAlO3 powders fall in the white region of the CIE diagram, and the average CCT value was found to be about 6276 K. Therefore, the present phosphor is highly useful for display applications.

Microstructure and Electrical Properties of Antimony Telluride Thin Films Deposited by RF Magnetron Sputtering on Flexible Substrate Using Different Sputtering Pressures

NASA Astrophysics Data System (ADS)

Khumtong, T.; Sukwisute, P.; Sakulkalavek, A.; Sakdanuphab, R.

2017-05-01

The microstructural, electrical, and thermoelectric properties of antimony telluride (Sb2Te3) thin films have been investigated for thermoelectric applications. Sb2Te3 thin films were deposited on flexible substrate (polyimide) by radiofrequency (RF) magnetron sputtering from a Sb2Te3 target using different sputtering pressures in the range from 4 × 10-3 mbar to 1.2 × 10-2 mbar. The crystal structure, [Sb]:[Te] ratio, and electrical and thermoelectric properties of the films were analyzed by grazing-incidence x-ray diffraction (XRD) analysis, energy-dispersive x-ray spectroscopy (EDS), and Hall effect and Seebeck measurements, respectively. The XRD spectra of the films demonstrated polycrystalline structure with preferred orientation of (015), (110), and (1010). A high-intensity spectrum was found for the film deposited at lower sputtering pressure. EDS analysis of the films revealed the effects of the sputtering pressure on the [Sb]:[Te] atomic ratio, with nearly stoichiometric films being obtained at higher sputtering pressure. The stoichiometric Sb2Te3 films showed p-type characteristics with electrical conductivity, carrier concentration, and mobility of 35.7 S cm-1, 6.38 × 1019 cm-3, and 3.67 cm2 V-1 s-1, respectively. The maximum power factor of 1.07 × 10-4 W m-1 K-2 was achieved for the film deposited at sputtering pressure of 1.0 × 10-2 mbar.

Purification, characterization and antioxidant properties of a novel polysaccharide extracted from Sorghum bicolor (L.) seeds in sausage.

PubMed

Ben Slima, Sirine; Ktari, Naourez; Trabelsi, Imen; Moussa, Hafedh; Makni, Iskandar; Ben Salah, Riadh

2018-01-01

A novel polysaccharide named Sorghum Water-Soluble Polysaccharide (SWSP) was purified from Sorghum bicolor (L.) seeds. It was structurally characterized by high performance liquid chromatography (HPLC), thin layer chromatography (TLC), Fourier transform-infrared spectroscopy analysis (FT-IR), X-ray diffraction (XRD) and mass spectroscopy (MS). HPLC and TLC showed that SWSP is a glucose polymer. The FT-IR spectrum proved the polysaccharide characteristic band of SWSP. XRD and microscopy analyses revealed that SWSP is a semi-crystalline polymer. Functional properties of SWSP were determined based on Water Holding Capacity (WHC), Oil Holding Capacity (OHC) and emulsification properties. SWSP showed good WHC and OHC, recorded at 3.01±0.03 and 1.02±0.03g/g, respectively and exhibited excellent emulsion properties even after 168h (61.5±0.02%). The effect of SWSP on oxidative stability of sausage during storage up to 12days at 4°C was investigated. Results showed a high rate (P<0.05) of oxymyoglobin and low lipid oxidation. The antioxidant activities of SWSP were also studied in vitro. Results demonstrated that the polysaccharides exhibited interesting 1,1-diphenyl-2-picrylhydrazyl (DPPH), ABTS radical scavenging, and ß-carotene bleaching inhibition activities. Overall, this natural polysaccharide was proved to enhance the oxidation stability of sausages, since it can efficiently substitute synthetic antioxidants in meat industry. Copyright © 2017 Elsevier B.V. All rights reserved.

Biosynthesis of Stable Antioxidant ZnO Nanoparticles by Pseudomonas aeruginosa Rhamnolipids

PubMed Central

Singh, Brahma Nand; Rawat, Ajay Kumar Singh; Khan, Wasi; Naqvi, Alim H.; Singh, Braj Raj

2014-01-01

During the last several years, various chemical methods have been used for synthesis of a variety of metal nanoparticles. Most of these methods pose severe environmental problems and biological risks; therefore the present study reports a biological route for synthesis of zinc oxide nanoparticles using Pseudomonas aeruginosa rhamnolipids (RLs) (denoted as RL@ZnO) and their antioxidant property. Formation of stable RL@ZnO nanoparticles gave mostly spherical particles with a particle size ranging from 35 to 80 nm. The RL@ZnO nanoparticles were characterized by UV-visible (UV–vis) spectroscopy, scanning electron microscopy, transmission electron microscopy, dynamic light scattering, Fourier transform infrared spectroscopy, X-ray diffraction (XRD), and thermal gravimetric analysis. The UV–vis spectra presented a characteristic absorbance peak at ∼360 nm for synthesized RL@ZnO nanoparticles. The XRD spectrum showed that RL@ZnO nanoparticles are crystalline in nature and have typical wurtzite type polycrystals. Antioxidant potential of RL@ZnO nanoparticles was assessed through 2,2–diphenyl-1-picrylhydrazyl (DPPH), hydroxyl, and superoxide anion free radicals with varying concentration and time of the storage up to 15 months, while it was found to decline in bare ZnO nanoparticles. Similarly, the inhibitory effects on β-carotene oxidation and lipid peroxidation were also observed. These results elucidate the significance of P. aeruginosa RL as effective stabilizing agents to develop surface protective ZnO nanoparticles, which can be used as promising antioxidants in biological system. PMID:25187953

Green synthesis of gold nanoparticles using Trigonella foenum-graecum and its size-dependent catalytic activity

NASA Astrophysics Data System (ADS)

Aswathy Aromal, S.; Philip, Daizy

2012-11-01

The development of new synthesis methods for monodispersed nanocrystals using cheap and nontoxic chemicals, environmentally benign solvents and renewable materials remains a challenge to the scientific community. Most of the current methods involve known protocols which may be potentially harmful to either environment or human health. Recent research has been focused on green synthesis methods to produce new nanomaterials, ecofriendly and safer with sustainable commercial viability. The present work reports the green synthesis of gold nanoparticles using the aqueous extract of fenugreek (Trigonella foenum-graecum) as reducing and protecting agent. The pathway is based on the reduction of AuCl4- by the extract of fenugreek. This method is simple, efficient, economic and nontoxic. Gold nanoparticles having different sizes in the range from 15 to 25 nm could be obtained by controlling the synthesis parameters. The nanoparticles have been characterized by UV-Visible spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and FTIR analysis. The high crystallinity of nanoparticles is evident from clear lattice fringes in the HRTEM images, bright circular spots in the SAED pattern and peaks in the XRD pattern. FTIR spectrum indicates the presence of different functional groups present in the biomolecule capping the nanoparticles. The synthesized gold nanoparticles show good catalytic activity for the reduction of 4-nitrophenol to 4-aminophenol by excess NaBH4. The catalytic activity is found to be size-dependent, the smaller nanoparticles showing faster activity.

DISTRIBUTION SYSTEM SOLIDS - A RESEARCH APPROACH

EPA Science Inventory

The U.S. EPA's AWBERC research facility is equipped with capabilities to analyze a variety of solids in support many Laboratory-wide research studies. Techniques available on site include X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microsco...

Spectral characteristics of multimode semiconductor lasers with a high-order surface diffraction grating

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

Zolotarev, V V; Leshko, A Yu; Pikhtin, N A

2014-10-31

We have studied the spectral characteristics of multimode semiconductor lasers with high-order surface diffraction gratings based on asymmetric separate-confinement heterostructures grown by metalorganic vapour phase epitaxy (λ = 1070 nm). Experimental data demonstrate that, in the temperature range ±50 °C, the laser emission spectrum is ∼5 Å in width and contains a fine structure of longitudinal and transverse modes. A high-order (m = 15) surface diffraction grating is shown to ensure a temperature stability of the lasing spectrum dλ/dT = 0.9 Å K{sup -1} in this temperature range. From analysis of the fine structure of the lasing spectrum, we havemore » evaluated the mode spacing and, thus, experimentally determined the effective length of the Bragg diffraction grating, which was ∼400 μm in our samples. (lasers)« less

Characterization of crystallographic properties of thin films using X-ray diffraction

NASA Astrophysics Data System (ADS)

Zoo, Yeongseok

2007-12-01

Silver (Ag) has been recognized as one of promising candidates in Ultra-Large Scale Integrated (ULSI) applications in that it has the lowest bulk electrical resistivity of all pure metals and higher electromigration resistance than other interconnect materials. However, low thermal stability on Silicon Dioxide (Si02) at high temperatures (e.g., agglomeration) is considered a drawback for the Ag metallization scheme. Moreover, if a thin film is attached on a substrate, its properties may differ significantly from that of the bulk, since the properties of thin films can be significantly affected by the substrate. In this study, the Coefficient of Thermal Expansion (CTE) and texture evolution of Ag thin films on different substrates were characterized using various analytical techniques. The experimental results showed that the CTE of the Ag thin film was significantly affected by underlying substrate and the surface roughness of substrate. To investigate the alloying effect for Ag meatallization, small amounts of Copper (Cu) were added and characterized using theta-2theta X-ray Diffraction (XRD) scan and pole figure analysis. These XRD techniques are useful for investigating the primary texture of a metal film, (111) in this study, which (111) is the notation of a specific plane in the orthogonal coordinate system. They revealed that the (111) textures of Ag and Ag(Cu) thin films were enhanced with increasing temperature. Comparison of texture profiles between Ag and Ag(Cu) thin films showed that Cu additions enhanced (111) texture in Ag thin films. Accordingly, the texture enhancement in Ag thin films by Cu addition was discussed. Strained Silicon-On-Insulator (SSOI) is being considered as a potential substrate for Complementary Metal-Oxide-Semiconductor (CMOS) technology since the induced strain results in a significant improvement in device performance. High resolution X-ray diffraction (XRD) techniques were used to characterize the perpendicular and parallel strains in SSOI layers. XRD diffraction profiles generated from the crystalline SSOI layer provided a direct measurement of the layer's strain components. In addition, it has demonstrated that the rotational misalignment between the layer and the substrate can be incorporated within the biaxial strain equations for epitaxial layers. Based on these results, the strain behavior of the SSOI layer and the relation between strained Si and SiO2 layers are discussed for annealed samples.

In-field X-ray and neutron diffraction studies of re-entrant charge-ordering and field induced metastability in La0.175Pr0.45Ca0.375MnO3-δ

NASA Astrophysics Data System (ADS)

Sharma, Shivani; Shahee, Aga; Yadav, Poonam; da Silva, Ivan; Lalla, N. P.

2017-11-01

Low-temperature high-magnetic field (2 K, 8 T) (LTHM) powder X-ray diffraction (XRD) and time of flight powder neutron diffraction (NPD), low-temperature transmission electron microscopic (TEM), and resistivity and magnetization measurements have been carried out to investigate the re-entrant charge ordering (CO), field induced structural phase transitions, and metastability in phase-separated La0.175Pr0.45Ca0.375MnO3-δ (LPCMO). Low-temperature TEM and XRD studies reveal that on cooling under zero-field, paramagnetic Pnma phase transforms to P21/m CO antiferromagnetic (AFM) insulating phase below ˜233 K. Unlike reported literature, no structural signature of CO AFM P21/m to ferromagnetic (FM) Pnma phase-transition during cooling down to 2 K under zero-field was observed. However, the CO phase was found to undergo a re-entrant transition at ˜40 K. Neutron diffraction studies revealed a pseudo CE type spin arrangement of the observed CO phase. The low-temperature resistance, while cooled under zero-field, shows insulator to metal like transition below ˜105 K with minima at ˜25 K. On application of field, the CO P21/m phase was found to undergo field-induced transition to FM Pnma phase, which shows irreversibility on field removal below ˜40 K. Zero-field warming XRD and NPD studies reveal that field-induced FM Pnma phase is a metastable phase, which arise due to the arrest of kinetics of the first-order phase transition of FM Pnma to CO-AFM P21/m phase, below 40 K. Thus, a strong magneto-structural coupling is observed for this system. A field-temperature (H-T) phase-diagram has been constructed based on the LTHM-XRD, which matches very nicely with the reported H-T phase-diagram constructed based on magnetic measurements. Due to the occurrence of gradual growth of the re-entrant CO phase and the absence of a clear structural signature of phase-separation of CO-AFM P21/m and FM Pnma phases, the H-T minima in the phase-diagram of the present LPCMO sample has been attributed to the strengthening of AFM interaction during re-entrant CO transition and not to glass like "dynamic to frozen" transition.

Thermoluminescence and X-ray diffraction studies on sliced ancient porcelain samples

NASA Astrophysics Data System (ADS)

Leung, P. L.; Yang, B.

1999-09-01

The thermal activation characteristics (TACs) of the sensitivity of the '110°C' peak in 14 sliced ancient Chinese porcelain samples are studied. Comparing with the TACs of natural quartz and synthetic mullite, the relation between the TACs and the composition of the sample is discussed with reference to the X-ray diffraction (XRD) spectra. It is suggested that in some cases, contribution of the porcelain components other than quartz to the TACs is not negligible.

Test and Delivery of the Chemin Mineralogical Instrument for Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Blake, D. F.; Vaniman, D.; Anderson, R.; Bish, D.; Chipera, S.; Chemtob, S.; Crisp, J.; DesMarais, D. J.; Downs, R.; Feldman, S.;

Deposition of dual-layer coating on Ti6Al4V

NASA Astrophysics Data System (ADS)

Hussain Din, Sajad; Shah, M. A.; Sheikh, N. A.

2017-03-01

Dual-layer diamond coatings were deposited on titanium alloy (Ti6Al4V) using a hot filament chemical vapour deposition technique with the anticipation of studying the structural and morphology properties of the alloy. The coated diamond films were characterized using scanning electron microscope, x-ray diffraction (XRD), and Raman spectroscopy. The XRD studies reveal that the deposited films are highly crystalline in nature, whereas morphological studies show that the films have a cauliflower structure. XRD analysis was used to calculate the structural parameters of the Ti6Al4V and CVD-coated Ti6Al4V. Raman spectroscopy was used to determine the nature and magnitude of the residual stress of the coatings.

Synthesis and characterization of nanostructured titanium carbide for fuel cell applications

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

Singh, Paviter; Singh, Harwinder; Singh, Bikramjeet

2016-04-13

Titanium carbide (TiC) nanoparticles have been successfully synthesized by carbo-thermic reaction of titanium and acetone at 800 °C. This method is relatively low temperature synthesis route. It can be used for large scale production of TiC. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analyzer (DTA) techniques. XRD analysis confirmed the formation of single phase TiC. XRD analysis confirmed that the particles are spherical in shape with an average particle size of 13 nm. DTA analysis shows that the phase is stable upto 900 °C and the material can be used formore » high temperature applications.« less

Role of low-temperature AlGaN interlayers in thick GaN on silicon by metalorganic vapor phase epitaxy

NASA Astrophysics Data System (ADS)

Fritze, S.; Drechsel, P.; Stauss, P.; Rode, P.; Markurt, T.; Schulz, T.; Albrecht, M.; Bläsing, J.; Dadgar, A.; Krost, A.

2012-06-01

Thin AlGaN interlayers have been grown into a thick GaN stack on Si substrates to compensate tensile thermal stress and significantly improve the structural perfection of the GaN. In particular, thicker interlayers reduce the density in a-type dislocations as concluded from x-ray diffraction (XRD) measurements. Beyond an interlayer thickness of 28 nm plastic substrate deformation occurs. For a thick GaN stack, the first two interlayers serve as strain engineering layers to obtain a crack-free GaN structure, while a third strongly reduces the XRD ω-(0002)-FWHM. The vertical strain and quality profile determined by several XRD methods demonstrates the individual impact of each interlayer.

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.

Study of structural and magnetic properties of cobalt ferrite nanoparticles sintered at different temperature

NASA Astrophysics Data System (ADS)

Kumari, Mukesh; Bhatnagar, Mukesh Chander

2018-05-01

Cobalt ferrite (CFO) has been synthesized in the form of nanoparticles (NPs) through sol-gel auto-combustion method. The prepared NPs of CFO were sintered for four hours at various temperatures from 300°C to 900°C. The physical properties of the sintered samples have been optimized using X-ray diffraction (XRD), Raman spectroscopy and physical properties measurement system (PPMS). The XRD and Raman studies have confirmed the cubic spinel phase formation of CFO NPs. XRD results showed that as we increase the sintering temperature the crystallite size of particles increases. Whereas the magnetic studies revealed that the saturation magnetization (MS) increases while the coercivity (HC) of nanoparticles decreases with increase of sintering temperature.

Single phase Pb0.7Bi0.3Fe0.65Nb0.35O3 multiferroic: Neutron diffraction, impedance and modulus studies

NASA Astrophysics Data System (ADS)

Dadami, Sunanda T.; Matteppanvar, Shidaling; Shivaraja, I.; Rayaprol, Sudhindra; Deshpande, S. K.; Angadi, Basavaraj

2018-04-01

The Pb0.7Bi0.3Fe0.65Nb0.35O3 (PBFNO) multiferroic solid solution was synthesized by using single step solid state reaction method. Single phase formation was confirmed through room temperature (RT) X Ray Diffraction (XRD) and Neutron Diffraction (ND). Rietveld refinement was used to perform the structural analysis using FullProf Suite program. RT XRD and ND patterns well fitted with monoclinic structure (Cm space group) and cell parameters from the ND data are found to be a = 5.6474(4) Å, b = 5.6415(3) Å, c = 3.9992(3) Å and β = 89.95(2)°. ND data at RT exhibits G-type antiferromagnetic structure. The electrical properties (impedance and modulus) of PBFNO were studied as a function of frequency (100 Hz - 5 MHz) and temperature (133 K - 293 K) by Impedance spectroscopy technique. Impedance and modulus spectroscopy studies confirm the contribution to the conductivity is from grains only and the relaxation is of non-Debye type. The PBFNO sample exhibits negative temperature coefficient of resistance (NTCR) behaviour. PBFNO is found be a potential candidate for RT applications.

Effect of different conventional melt quenching technique on purity of lithium niobate (LiNbO3) nano crystal phase formed in lithium borate glass

NASA Astrophysics Data System (ADS)

Kashif, Ismail; Soliman, Ashia A.; Sakr, Elham M.; Ratep, Asmaa

2012-01-01

The glass system (45Li2O + 45B2O3 + 10Nb2O5) was fabricated by the conventional melt quenching technique poured in water, at air, between two hot plates and droplets at the cooled surface. The glass and glass ceramics were studied by differential thermal analysis (DTA) and X-ray diffraction (XRD). The as quenched samples poured in water and between two hot plates were amorphous. The samples poured at air and on cooled surface were crystalline as established via X-ray powder diffraction (XRD) studies. Differential thermal analysis was measured. The glass transition temperature (Tg) and the crystallization temperatures were calculated. Lithium niobate (LiNbO3) was the main phase in glass ceramic poured at air, droplets at the cooled surface and the heat treated glass sample at 500, 540 and 580 °C in addition to traces from LiNb3O8. Crystallite size of the main phases determined from the X-ray diffraction peaks is in the range of <100 nm. The fraction of crystalline (LiNbO3) phase decreases with increase in the heat treatment temperature.

Developing high-transmittance heterojunction diodes based on NiO/TZO bilayer thin films

PubMed Central

2013-01-01

In this study, radio frequency magnetron sputtering was used to deposit nickel oxide thin films (NiO, deposition power of 100 W) and titanium-doped zinc oxide thin films (TZO, varying deposition powers) on glass substrates to form p(NiO)-n(TZO) heterojunction diodes with high transmittance. The structural, optical, and electrical properties of the TZO and NiO thin films and NiO/TZO heterojunction devices were investigated with scanning electron microscopy, X-ray diffraction (XRD) patterns, UV-visible spectroscopy, Hall effect analysis, and current-voltage (I-V) analysis. XRD analysis showed that only the (111) diffraction peak of NiO and the (002) and (004) diffraction peaks of TZO were observable in the NiO/TZO heterojunction devices, indicating that the TZO thin films showed a good c-axis orientation perpendicular to the glass substrates. When the sputtering deposition power for the TZO thin films was 100, 125, and 150 W, the I-V characteristics confirmed that a p-n junction characteristic was successfully formed in the NiO/TZO heterojunction devices. We show that the NiO/TZO heterojunction diode was dominated by the space-charge limited current theory. PMID:23634999

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

Surface modified α-glycine - EuF3: Gd nanoparticles for upconversion luminescence

NASA Astrophysics Data System (ADS)

Mahajan, Manoj P.; Khandpekar, M. M.

2018-04-01

Gadolinium doped EuF3 nanoparticles have been synthesized in the presence of α-glycine via chloride route with subsequent microwave drying. The XRD profile shows hexagonal phase structure with lattice parameters a = b = 6.920 A° and c = 7.085 A° (JCPDS No. 32-0373) with Debye-Scherer particle size of 51 nm. The SEM shows chipped morphology and TEM images exhibit shallow toroid like hexagonal - rounded nanostructures (30 - 50 nm) and their subsequent spontaneous transformation in to hyperboloid shaped nanostructures (200 - 600 nm) possibly with extension of the reaction time. SAED pattern confirms crystalline nature of nanoparticles and the planes are in agreement with XRD Peaks. Comparative FTTR and Raman spectrum shows presence of various functional groups confirming the capping of the glycine on EuF3:Gd core. A TGA/DTA spectrum shows decomposition in two stages. The photoluminescence spectrum shows up conversion luminescence at wavelength 653 nm (red).

Structural and thermal properties of silk fibroin - Silver nanoparticles composite films

NASA Astrophysics Data System (ADS)

Shivananda, C. S.; Rao B, B. Lakshmeesha; Shetty, G. Rajesh; Sangappa, Y.

2018-05-01

In this work, silk fibroin-silver nanoparticles (SF-AgNPs) composite films have been prepared by simple solution casting method. The composite films were examined for structural and thermal properties using X-ray diffraction (XRD), thermogravimatric (TGA) and differential scanning calorimetry (DSC) analysis. The XRD results showed that with the introduction of AgNPs in the silk fibroin matrix the amorphous nature of the silk fibroin decreases with increasing nanoparticles concentration. The silk fibroin films possess good thermal stability with the presence of AgNPs.

Structural, thermal, optical, and photoacoustic study of nanocrystalline Bi{sub 2}Te{sub 3} produced by mechanical alloying

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

Souza, S. M.; Triches, D. M.; Poffo, C. M.

2011-01-01

Nanocrystalline Bi{sub 2}Te{sub 3} was produced by mechanical alloying and its properties were investigated by differential scanning calorimetry (DSC) x-ray diffraction (XRD), Raman spectroscopy (RS), and photoacoustic spectroscopy (PAS). Combining the XRD and RS results, the volume fraction of the interfacial component in as-milled and annealed samples was estimated. The PAS results suggest that the contribution of the interfacial component to the thermal diffusivity of nanostructured Bi{sub 2}Te{sub 3} is very significant.

Spectral studies of 2-pyrazoline derivatives: structural elucidation through single crystal XRD and DFT calculations.

PubMed

Chinnaraja, D; Rajalakshmi, R; Srinivasan, T; Velmurugan, D; Jayabharathi, J

2014-04-24

A series of biologically active N-thiocarbamoyl pyrazoline derivatives have been synthesized using anhydrous potassium carbonate as the catalyst. All the synthesized compounds were characterized by FT-IR, (1)H NMR, (13)C NMR spectral studies, LCMS, CHN Analysis and X-ray diffraction analysis (compound 7). In order to supplement the XRD parameters, molecular modelling was carried out by Gaussian 03W. From the optimized structure, the energy, dipolemoment and HOMO-LUMO energies of all the systems were calculated. Copyright © 2014 Elsevier B.V. All rights reserved.

Coupling Graphene Sheets with Iron Oxide Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

of highly oriented pyrolytic graphite ( HOPG ) flake. Two electrode system containing platinum as counter electrode and HOPG as working electrode is... XRD ) patterns of the HOPG , exfoliated graphene, PyDop1-ɤ-Fe2O3 and PyDop1-ɤ-Fe2O3-graphene are given in Figure 1e. HOPG show a very sharp diffraction...atoms arranged in hexagonal pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG

Structural and optical properties of electrospun MoO3 nanowires

NASA Astrophysics Data System (ADS)

Das, Arnab Kumar; Modak, Rajkumar; Srinivasan, Ananthakrishnan

2018-05-01

Nanofibers of polyvinyl alcohol (PVA) containing ammonium molybdate were prepared by a combination of sol-gel and electrospinning techniques. Heat treatment of the as-spun composite nanofibers at 500 °C yielded MoO3 nanowires with a diameter of ˜180 nm. The product was characterized by X-ray diffraction (XRD), scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. XRD and Raman spectra of the heat nanowires clearly show the formation of orthorhombic single phase MoO3 structure without any impurity phases.

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.

Solid state vibrational spectroscopy of anhydrous lithium hexafluorophosphate (LiPF6)

NASA Astrophysics Data System (ADS)

Kock, L. D.; Lekgoathi, M. D. S.; Crouse, P. L.; Vilakazi, B. M.

2012-10-01

Raman and infrared studies of solid anhydrous lithium hexafluorophosphate (LiPF6) have been carried out. The studies were complemented by X-ray powder diffraction (XRD) and Thermogravimetric (TG) analysis techniques. The results indicate that when solid LiPF6 is studied in a strictly anhydrous environment, more consistent thermal stability data can be obtained. TG analysis, using a scan rate of 10 °C min-1, indicate the onset of thermal decomposition of the anhydrous LiPF6 occurring at about 134.84 °C while the partially hydrolysed compound starts at 114.46 °C. The Raman spectra of anhydrous MPF6 (M = Li+, Na+ and K+) are best interpreted in terms of a cubic space group Fm3m(Ohs), (ZB = 1), giving rise to 21 vibrational modes (A1g(R)+Eg(R)+T1g+T2g(R)+3T1u(1R)+T2u) and as such, LiPF6 may be considered isostructural with NaPF6 and KPF6. Crystal symmetry distortions in the anhydrous LiPF6 give rise additional bands in the Raman spectrum due to T1u infrared active modes and the ν1 (A1g) Raman band appears in the infrared spectrum in violation of the mutual exclusion selection rule for centro-symmetric sites. When these observations are considered, the Raman spectrum of LiPF6 is similar to those of NaPF6 and KPF6, with observations of the expected shifts due to cation size and/or electronegativity effects.

High-pressure phase transition in silicon carbide under shock loading using ultrafast x-ray diffraction

NASA Astrophysics Data System (ADS)

Tracy, S. J.; Smith, R. F.; Wicks, J. K.; Fratanduono, D. E.; Gleason, A. E.; Bolme, C.; Speziale, S.; Appel, K.; Prakapenka, V. B.; Fernandez Panella, A.; Lee, H. J.; MacKinnon, A.; Eggert, J.; Duffy, T. S.

2017-12-01

The behavior of silicon carbide (SiC) under shock loading was investigated through a series of time-resolved pump-probe x-ray diffraction (XRD) measurements. SiC is found at impact sites and has been put forward as a possible constituent in the proposed class of extra-solar planets known as carbon planets. Previous studies have used wave profile measurements to identify a phase transition under shock loading near 1 Mbar, but crystal structure information was not obtained. We have carried out an in situ XRD study of shock-compressed SiC using the Matter in Extreme Conditions instrument of the Linac Coherent Light Source. The femtosecond time resolution of the x-ray free electron laser allows for the determination of time-dependent atomic arrangements during shock loading and release. Two high-powered lasers were used to generate ablation-driven compression waves in the samples. Time scans were performed using the same drive conditions and nominally identical targets. For each shot in a scan, XRD data was collected at a different probe time after the shock had entered the SiC. Probe times extended up to 40 ns after release. Scans were carried out for peak pressures of 120 and 185 GPa. Our results demonstrate that SiC transforms directly from the ambient tetrahedrally-coordinated phase to the octahedral B1 structure on the nanosecond timescale of laser-drive experiments and reverts to the tetrahedrally coordinated ambient phase within nanoseconds of release. The data collected at 120 GPa exhibit diffraction peaks from both compressed ambient phase and transformed B1 phase, while the data at 185 GPa show a complete transformation to the B1 phase. Densities determined from XRD peaks are in agreement with an extrapolation of previous continuum data as well as theoretical predictions. Additionally, a high degree of texture was retained in both the high-pressure phase as well as on back transformation. Two-dimensional fits to the XRD data reveal details of the orientational relationships between the low- and high-pressure phases that can be interpreted to provide information about transformation pathways between tetrahedral and octahedral coordination structures. We acknowledge support for this work from SLAC National Accelerator Laboratory, Lawrence Livermore National Laboratory, and Los Alamos National Laboratory.

Two-dimensional X-ray diffraction and transmission electron microscopy study on the effect of magnetron sputtering atmosphere on GaN/SiC interface and gallium nitride thin film crystal structure

NASA Astrophysics Data System (ADS)

Shen, Huaxiang; Zhu, Guo-Zhen; Botton, Gianluigi A.; Kitai, Adrian

2015-03-01

The growth mechanisms of high quality GaN thin films on 6H-SiC by sputtering were investigated by X-ray diffraction (XRD) and scanning transmission electron microscopy (STEM). The XRD θ-2θ scans show that high quality ( 0002 ) oriented GaN was deposited on 6H-SiC by reactive magnetron sputtering. Pole figures obtained by 2D-XRD clarify that GaN thin films are dominated by ( 0002 ) oriented wurtzite GaN and { 111 } oriented zinc-blende GaN. A thin amorphous silicon oxide layer on SiC surfaces observed by STEM plays a critical role in terms of the orientation information transfer from the substrate to the GaN epilayer. The addition of H2 into Ar and/or N2 during sputtering can reduce the thickness of the amorphous layer. Moreover, adding 5% H2 into Ar can facilitate a phase transformation from amorphous to crystalline in the silicon oxide layer and eliminate the unwanted { 3 3 ¯ 02 } orientation in the GaN thin film. Fiber texture GaN thin films can be grown by adding 10% H2 into N2 due to the complex reaction between H2 and N2.

X-ray diffraction investigation of amorphous calcium phosphate and hydroxyapatite under ultra-high hydrostatic pressure

NASA Astrophysics Data System (ADS)

Lam, Elisa; Gu, Qinfen; Swedlund, Peter J.; Marchesseau, Sylvie; Hemar, Yacine

2015-11-01

The changes in the crystal structures of synthetically prepared amorphous calcium phosphate (ACP) and hydroxyapatite (HAP) in water (1:1 mass ratio) were studied by synchrotron X-ray diffraction (XRD) under ultra-high hydrostatic pressures as high as 2.34 GPa for ACP and 4 GPa for HAP. At ambient pressure, the XRD patterns of the ACP and HAP samples in capillary tubes and their environmental scanning electron micrographs indicated amorphous and crystalline characteristics for ACP and HAP, respectively. At pressures greater than 0.25 GPa, an additional broad peak was observed in the XRD pattern of the ACP phase, indicating a partial phase transition from an amorphous phase to a new high-pressure amorphous phase. The peak areas and positions of the ACP phase, as obtained through fitting of the experimental data, indicated that the ACP exhibited increased pseudo-crystalline behavior at pressures greater than 0.96 GPa. Conversely, no structural changes were observed for the HAP phase up to the highest applied pressure of 4 GPa. For HAP, a unit-cell reduction during compression was evidenced by a reduction in both refined lattice parameters a and c. Both ACP and HAP reverted to their original structures when the pressure was fully released to ambient pressure.

Effect of aging temperature on formation of sol-gel derived fluor-hydroxyapatite nanoparticles.

PubMed

Joughehdoust, S; Behnamghader, A; Jahandideh, R; Manafi, S

2010-04-01

Synthetic hydroxyapatite (HA) has been recognized as one of the most important bone substitute materials in orthopaedics and dentistry over past few decades because of its chemical and biological similarity to the mineral phase of human bone. One solution for reduction the solubility of HA in biological environments is replacing F- by OH in HA structure and forming fluor-hydroxyapatite (FHA) solid solution. In this paper, FHA nanoparticles were successfully synthesized by a sol-gel method. Also, the influence of aging temperature on formation of FHA powder was studied. Equimolar solutions of calcium nitrate tetrahydrate, triethyl phosphite and ammonium fluoride in ethanol were used as Ca, P and F precursors. After aging at different temperatures, the synthesized powders were heat treated at 550 degrees C. The powders were investigated with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), selected area electron diffraction pattern (SAED), energy dispersive analysis of X-ray (EDAX) and zetasizer measurement. The results of XRD proved the presence of fluorapatite (FA) and HA in all samples. In addition, the formation of FHA was confirmed by FT-IR results. XRD studies also showed that the crystallites were in nanometric scale. At the same time, this result was in good agreement with the result of zetasizer analysis.

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

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

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

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

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

Structural and spectroscopic study of mechanically synthesized SnO2 nanostructures

NASA Astrophysics Data System (ADS)

Vij, Ankush; Kumar, Ravi

2016-05-01

We report the single step synthesis of SnO2 nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO2 nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A1g Raman mode towards lower wave number, which is correlated with the nanostructure formation.

Analysis of x-ray diffraction pattern and complex plane impedance plot of polypyrrole/titanium dioxide nanocomposite: A simulation study

NASA Astrophysics Data System (ADS)

Ravikiran, Y. T.; Vijaya Kumari, S. C.

2013-06-01

To innovate the properties of Polypyrrole/Titanium dioxide (PPy/TiO2) nanocomposite further, it has been synthesized by chemical polymerization technique. The nanostructure and monoclinic phase of the prepared composite have been confirmed by simulating the X-ray diffraction pattern (XRD). Also, complex plane impedance plot of the composite has been simulated to find equivalent resistance capacitance circuit (RC circuit) and numerical values of R and C have been predicted.

[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.

Semi-insulating GaN Substrates for High-frequency Device Fabrication

DTIC Science & Technology

2008-06-18

of the undoped and iron-doped samples were probed by X-ray diffraction (XRD) measurements using a Philips X’pert MRD triple axis diffracted beam system...diode laser. The light emitted by the samples was dispersed by a Princeton/Acton Trivista 557 triple spectrometer fit with an LN2 cool OMA V InGaAs... point out that the relative intensity of all these bands decreases with increasing of the iron doping. This observation is consistent with the change in

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

Synthesis of Silver and Gold Nanoparticles Using Antioxidants from Blackberry, Blueberry, Pomegranate, and Turmeric Extracts

EPA Science Inventory

Greener synthesis of Ag and Au nanoparticles is described using antioxidants from blackberry, blueberry, pomegranate, and turmeric extracts. The synthesized particles were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HR...

Phosphate Remediation and Recovery using Iron Oxide-based Adsorbents

EPA Science Inventory

E33-modified sorbents for the removal of phosphate from lake water was investigated in this study. E33-modified sorbents were synthesized by coating with manganese and nanoparticles. Characterization was done by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-...

Effects of Plastizers on the Structure and Properties of Starch-Clay Nanocomposites

USDA-ARS?s Scientific Manuscript database

Biodegradable nanocomposites were successfully fabricated from corn starch and montmorillonite (MMT) nanoclays by melt extrusion processing. The structure and morphology of the nanocomposites were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM), and film propertie...

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.

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.

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

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

PubMed

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

2017-04-01

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

XRD analysis of undoped and Fe doped TiO{sub 2} nanoparticles by Williamson Hall method

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

Bharti, Bandna; Barman, P. B.; Kumar, Rajesh, E-mail: rajesh.kumar@juit.ac.in

2015-08-28

Undoped and Fe doped titanium dioxide (TiO{sub 2}) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO{sub 2} and Fe doped TiO{sub 2} nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO{sub 2} with Fe doping was observed. The anatase phase of Fe-doped TiO{sub 2} nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size weremore » also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO{sub 2} and tensile strain for Fe-TiO{sub 2} nanoparticles annealed at 500°C.« less

Use of X-ray diffraction to quantify amorphous supplementary cementitious materials in anhydrous and hydrated blended cements

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

Snellings, R., E-mail: ruben.snellings@epfl.ch; Salze, A.; Scrivener, K.L., E-mail: karen.scrivener@epfl.ch

2014-10-15

The content of individual amorphous supplementary cementitious materials (SCMs) in anhydrous and hydrated blended cements was quantified by the PONKCS [1] X-ray diffraction (XRD) method. The analytical precision and accuracy of the method were assessed through comparison to a series of mixes of known phase composition and of increasing complexity. A 2σ precision smaller than 2–3 wt.% and an accuracy better than 2 wt.% were achieved for SCMs in mixes with quartz, anhydrous Portland cement, and hydrated Portland cement. The extent of reaction of SCMs in hydrating binders measured by XRD was 1) internally consistent as confirmed through the standardmore » addition method and 2) showed a linear correlation to the cumulative heat release as measured independently by isothermal conduction calorimetry. The advantages, limitations and applicability of the method are discussed with reference to existing methods that measure the degree of reaction of SCMs in blended cements.« 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.; 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

Enhanced model for determining the number of graphene layers and their distribution from X-ray diffraction data

PubMed Central

Ademi, Abdulakim; Grozdanov, Anita; Paunović, Perica; Dimitrov, Aleksandar T

2015-01-01

Summary A model consisting of an equation that includes graphene thickness distribution is used to calculate theoretical 002 X-ray diffraction (XRD) peak intensities. An analysis was performed upon graphene samples produced by two different electrochemical procedures: electrolysis in aqueous electrolyte and electrolysis in molten salts, both using a nonstationary current regime. Herein, the model is enhanced by a partitioning of the corresponding 2θ interval, resulting in significantly improved accuracy of the results. The model curves obtained exhibit excellent fitting to the XRD intensities curves of the studied graphene samples. The employed equation parameters make it possible to calculate the j-layer graphene region coverage of the graphene samples, and hence the number of graphene layers. The results of the thorough analysis are in agreement with the calculated number of graphene layers from Raman spectra C-peak position values and indicate that the graphene samples studied are few-layered. PMID:26665083

STM-electroluminescence from clustered C3N4 nanodomains synthesized via green chemistry process.

PubMed

Andrade, E P; Costa, B B A; Chaves, C R; de Paula, A M; Cury, L A; Malachias, A; Safar, G A M

2018-01-01

A Scanning Tunneling Microscopy/Spectroscopy (STM/STS) and synchrotron X-ray diffraction study on clustered C 3 N 4 nanoparticles (nanoflakes) is conducted on green-chemistry synthesized samples obtained from chitosan through high power sonication. Morphological aspects and the electronic characteristics are investigated. The observed bandgap of the nanoflakes reveals the presence of different phases in the material. Combining STM morphology, STS spectra and X-ray diffraction (XRD) results one finds that the most abundant phase is graphitic C 3 N 4 . A high density of defects is inferred from the XRD measurements. Additionally, STM-electroluminescence (STMEL) is detected in C 3 N 4 nanoflakes deposited on a gold substrate. The tunneling current creates photons that are three times more energetic than the tunneling electrons of the STM sample. We ponder about the two most probable models to explain the observed photon emission energy: either a nonlinear optical phenomenon or a localized state emission. Copyright © 2017 Elsevier B.V. All rights reserved.

Characterization of food additive-potato starch complexes by FTIR and X-ray diffraction.

PubMed

Dankar, Iman; Haddarah, Amira; Omar, Fawaz E L; Pujolà, Montserrat; Sepulcre, Francesc

2018-09-15

Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) techniques were used to study the effect of four food additives, agar, alginate, lecithin and glycerol, at three different concentrations, 0.5, 1 and 1.5%, on the molecular structure of potato puree prepared from commercial potato powder. Vibrational spectra revealed that the amylose-amylopectin skeleton present in the raw potato starch was missing in the potato powder but could be fully recovered upon water addition when the potato puree was prepared. FTIR peaks corresponding to water were clearly present in the potato powder, indicating the important structural role of water molecules in the recovery of the initial molecular conformation. None of the studied puree samples presented a crystalline structure or strong internal order. A comparison of the FTIR and XRD results revealed that the additives exerted some effects, mainly on the long-range order of the starch structure via interacting with and changing -OH and hydrogen bond interactions. Copyright © 2018 Elsevier Ltd. All rights reserved.

Structural and Electronic Properties Study of Colombian Aurifer Soils by Mössbauer Spectroscopy and X-ray Diffraction

NASA Astrophysics Data System (ADS)

Bustos Rodríguez, H.; Rojas Martínez, Y.; Oyola Lozano, D.; Pérez Alcázar, G. A.; Fajardo, M.; Mojica, J.; Molano, Y. J. C.

2005-02-01

In this work a study on gold mineral samples is reported, using optical microscopy, X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). The auriferous samples are from the El Diamante mine, located in Guachavez-Nariño (Colombia) and were prepared by means of polished thin sections. The petrography analysis registered the presence, in different percentages that depend on the sample, of pyrite, quartz, arsenopyirite, sphalerite, chalcopyrite and galena. The XRD analysis confirmed these findings through the calculated cell parameters. One typical Rietveld analysis showed the following weight percent of phases: 85.0% quartz, 14.5% pyrite and 0.5% sphalerite. In this sample, MS demonstrated the presence of two types of pyrite whose hyperfine parameters are δ 1 = 0.280 ± 0.002 mm/s and Δ 1 = 0.642 ± 0.002 mm/s, δ 2 = 0.379 ± 0.002 mm/s and Δ 2 = 0.613 ± 0.002 mm/s.

Structural and morphological study on ZnO:Al thin films grown using DC magnetron sputtering

NASA Astrophysics Data System (ADS)

Astuti, B.; Sugianto; Mahmudah, S. N.; Zannah, R.; Putra, N. M. D.; Marwoto, P.; Aryanto, D.; Wibowo, E.

2018-03-01

ZnO doped Al (ZnO:Al ) thin film was deposited on corning glass substrate using DC magnetron sputtering method. Depositon process of the ZnO:Al thin films was kept constant at plasma power, deposition temperature and deposition time are 40 watt, 400°C and 2 hours, respectivelly. Furthermore, for annealing process has been done on the variation of oxygen pressure are 0, 50, and 100 mTorr. X-ray diffraction (XRD), and SEM was used to characterize ZnO:Al thin film was obtained. Based on XRD characterization results of the ZnO:Al thin film shows that deposited thin film has a hexagonal structure with the dominant diffraction peak at according to the orientation of the (002) plane and (101). Finally, the crystal structure of the ZnO:Al thin films that improves with an increasing the oxygen pressure at annealing process up to 100 mTorr and its revealed by narrow FWHM value and also with dense crystal structure.

Facile synthesis of Co3O4 hexagonal plates by flux method

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Crystal Structure Variations of Sn Nanoparticles upon Heating

NASA Astrophysics Data System (ADS)

Mittal, Jagjiwan; Lin, Kwang-Lung

2018-04-01

Structural changes in Sn nanoparticles during heating below the melting point have been investigated using differential scanning calorimetry (DSC), x-ray diffraction (XRD) analysis, electron diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). DSC revealed that the heat required to melt the nanoparticles (28.43 J/g) was about half compared with Sn metal (52.80 J/g), which was attributed to the large surface energy contribution for the nanoparticles. ED and XRD analyses of the Sn nanoparticles revealed increased intensity for crystal planes having large interplaner distances compared with regular crystal planes with increasing heat treatment temperature (HTT). HRTEM revealed an increase in interlayer spacing at the surface and near joints between nanoparticles with the HTT, leading to an amorphous structure of nanoparticles at the surface at 220°C. These results highlight the changes that occur in the morphology and crystal structure of Sn nanoparticles at the surface and in the interior with increase of the heat treatment temperature.

Green synthesis of gold nanoparticles using aqueous extract of Dillenia indica

NASA Astrophysics Data System (ADS)

Sett, Arghya; Gadewar, Manoj; Sharma, Pragya; Deka, Manab; Bora, Utpal

2016-06-01

In this study, we report a novel method of gold nanoparticle (AuNP) synthesis using aqueous fruit extract of Dillenia indica. The phytochemicals present in the fruit extract act as an effective reducing and capping agent to synthesize AuNPs. The synthesized AuNPs were characterized by spectrophotometry, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. TEM studies revealed the particles of various sizes and mainly spherical in shape. Selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images confirmed the crystallinity of the particles. The XRD patterns showed peaks at (111), (200), (220) which exhibited preferential orientation of the AuNPs as face-centered cubic crystal. FTIR measurements confirmed the coating of phenolic compounds on the AuNPs indicating a possible role of biomolecules for the capping and efficient stabilization of the AuNPs. The synthesized AuNPs did not show any form of cytotoxicity in the normal fibroblast cell line L929.

Growth and characterization of hexamethylenetetramine crystals grown from solution

NASA Astrophysics Data System (ADS)

Babu, B.; Chandrasekaran, J.; Balaprabhakaran, S.

2014-06-01

Organic nonlinear optical single crystals of hexamethylenetetramine (HMT; 10 × 10 × 5 mm3) were prepared by crystallization from methanol solution. The grown crystals were subjected to various characterization techniques such as single crystal XRD, powder XRD, UV-Vis and electrical studies. Single crystal XRD analysis confirmed the crystalline structure of the grown crystals. Their crystalline nature was also confirmed by powder XRD technique. The optical transmittance property was identified from UV-Vis spectrum. Dielectric measurements were performed as a function of frequency at different temperatures. DC conductivity and photoconductivity studies were also carried out for the crystal. The powder second harmonic generation efficiency (SHG) of the crystal was measured using Nd:YAG laser and the efficiency was found to be two times greater than that of potassium dihydrogen phosphate (KDP).

Mineralogy of mine waste at the Vermont Asbestos Group mine, Belvidere Mountain, Vermont

USGS Publications Warehouse

Levitan, D.M.; Hammarstrom, J.M.; Gunter, M.E.; Seal, R.R.; Chou, I.-Ming; Piatak, N.M.

2009-01-01

Samples from the surfaces of waste piles at the Vermont Asbestos Group mine in northern Vermont were studied to determine their mineralogy, particularly the presence and morphology of amphiboles. Analyses included powder X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM), electron probe microanalysis (EPMA), and Raman spectroscopy. Minerals identified by XRD were serpentine-group minerals, magnetite, chlorite, quartz, olivine, pyroxene, and brucite; locally, mica and carbonates were also present. Raman spectroscopy distinguished antigorite and chrysotile, which could not be differentiated using XRD. Long-count, short-range XRD scans of the (110) amphibole peak showed trace amounts of amphibole in most samples. Examination of amphiboles in tailings by optical microscopy, SEM, and EPMA revealed non-fibrous amphiboles compositionally classified as edenite, magnesiohornblende, magnesiokatophorite, and pargasite. No fibrous amphibole was found in the tailings, although fibrous tremolite was identified in a sample of host rock. Knowledge of the mineralogy at the site may lead to better understanding of potential implications for human health and aid in designing a remediation plan.

Matching 4.7-Å XRD Spacing in Amelogenin Nanoribbons and Enamel Matrix

PubMed Central

Sanii, B.; Martinez-Avila, O.; Simpliciano, C.; Zuckermann, R.N.; Habelitz, S.

2014-01-01

The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. PMID:25048248

Facile synthesis of the Li-rich layered oxide Li1.23Ni0.09Co0.12Mn0.56O2 with superior lithium storage performance and new insights into structural transformation of the layered oxide material during charge-discharge cycle: in situ XRD characterization.

PubMed

Shen, Chong-Heng; Wang, Qin; Fu, Fang; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Su, Hang; Zheng, Xiao-Mei; Xu, Bin-Bin; Li, Jun-Tao; Sun, Shi-Gang

2014-04-23

In this work, the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 was synthesized through a facile route called aqueous solution-evaporation route that is simple and without waste water. The as-prepared Li1.23Ni0.09Co0.12Mn0.56O2 oxide was confirmed to be a layered LiMO2-Li2MnO3 solid solution through ex situ X-ray diffraction (ex situ XRD) and transmission electron microscopy (TEM). Electrochemical results showed that the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material can deliver a discharge capacity of 250.8 mAhg(-1) in the 1st cycle at 0.1 C and capacity retention of 86.0% in 81 cycles. In situ X-ray diffraction technique (in situ XRD) and ex situ TEM were applied to study structural changes of the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material during charge-discharge cycles. The study allowed observing experimentally, for the first time, the existence of β-MnO2 phase that is appeared near 4.54 V in the first charge process, and a phase transformation of the β-MnO2 to layered Li0.9MnO2 is occurred in the initial discharge process by evidence of in situ XRD pattrens and selected area electron diffraction (SAED) patterns at different states of the initial charge and discharge process. The results illustrated also that the variation of the in situ X-ray reflections during charge-discharge cycling are clearly related to the changes of lattice parameters of the as-prepared Li-rich oxide during the charge-discharge cycles.

Swinging Symmetry, Multiple Structural Phase Transitions, and Versatile Physical Properties in RECuGa3 (RE = La-Nd, Sm-Gd).

PubMed

Subbarao, Udumula; Rayaprol, Sudhindra; Dally, Rebecca; Graf, Michael J; Peter, Sebastian C

2016-01-19

The compounds RECuGa3 (RE = La-Nd, Sm-Gd) were synthesized by various techniques. Preliminary X-ray diffraction (XRD) analyses at room temperature suggested that the compounds crystallize in the tetragonal system with either the centrosymmetric space group I4/mmm (BaAl4 type) or the non-centrosymmetric space group I4mm (BaNiSn3 type). Detailed single-crystal XRD, neutron diffraction, and synchrotron XRD studies of selected compounds confirmed the non-centrosymmetric BaNiSn3 structure type at room temperature with space group I4mm. Temperature-dependent single-crystal XRD, powder XRD, and synchrotron beamline measurements showed a structural transition between centro- and non-centrosymmetry followed by a phase transition to the Rb5Hg19 type (space group I4/m) above 400 K and another transition to the Cu3Au structure type (space group Pm3̅m) above 700 K. Combined single-crystal and synchrotron powder XRD studies of PrCuGa3 at high temperatures revealed structural transitions at higher temperatures, highlighting the closeness of the BaNiSn3 structure to other structure types not known to the RECuGa3 family. The crystal structure of RECuGa3 is composed of eight capped hexagonal prism cages [RE4Cu4Ga12] occupying one rare-earth atom in each ring, which are shared through the edge of Cu and Ga atoms along the ab plane, resulting in a three-dimensional network. Resistivity and magnetization measurements demonstrated that all of these compounds undergo magnetic ordering at temperatures between 1.8 and 80 K, apart from the Pr and La compounds: the former remains paramagnetic down to 0.3 K, while superconductivity was observed in the La compound at T = 1 K. It is not clear whether this is intrinsic or due to filamentary Ga present in the sample. The divalent nature of Eu in EuCuGa3 was confirmed by magnetization measurements and X-ray absorption near edge spectroscopy and is further supported by the crystal structure analysis.

Creating poly(ethylene glycol) film on the surface of NiTi alloy by gamma irradiation

NASA Astrophysics Data System (ADS)

Yu, Hongyan; Yan, Jin; Ma, Huiling; Zeng, Xinmiao; Liu, Yang; Zhao, Xinqing

2015-07-01

NiTi alloy has been extensively utilized as biomaterials owing to its unique shape memory effect, superelasticity and biocompatibility. However, concern with the toxic and allergic responses of nickel potentially releasing from implants stimulated lots of researches of modification on NiTi alloy surface. Creating chemical bond attachment of bioorganic film on NiTi alloy surface could effectively inhibit Ni releasing and obtain bioactive functions for further application. In this work, to get a bioorganic surface, NiTi alloy was modified with poly(ethylene glycol) (PEG) film by gamma ray induced grafting or crosslinking. X-ray diffraction (XRD) spectrum, water contact angle geometer and X-ray photoelectron spectroscopy (XPS) techniques were used to characterize the NiTi surface. The results indicated that PEG was covalent bonded on NiTi alloy surface. Fluorescence microscope (FM) images for morphology of 1 day osteoblast culture on the PEG coated NiTi surface showed that PEG could improve cell proliferation on NiTi surface. Our work offers a way to introduce a bioorganic metal surface by gamma irradiation.

Preparation and modification of VO2 thin film on R-sapphire substrate by rapid thermal process

NASA Astrophysics Data System (ADS)

Zhu, Nai-Wei; Hu, Ming; Xia, Xiao-Xu; Wei, Xiao-Ying; Liang, Ji-Ran

2014-04-01

The VO2 thin film with high performance of metal-insulator transition (MIT) is prepared on R-sapphire substrate for the first time by magnetron sputtering with rapid thermal process (RTP). The electrical characteristic and THz transmittance of MIT in VO2 film are studied by four-point probe method and THz time domain spectrum (THz-TDS). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and search engine marketing (SEM) are employed to analyze the crystalline structure, valence state, surface morphology of the film. Results indicate that the properties of VO2 film which is oxidized from the metal vanadium film in oxygen atmosphere are improved with a follow-up RTP modification in nitrogen atmosphere. The crystallization and components of VO2 film are improved and the film becomes compact and uniform. A better phase transition performance is shown that the resistance changes nearly 3 orders of magnitude with a 2-°C hysteresis width and the THz transmittances are reduced by 64% and 60% in thermal and optical excitation respectively.

Optoelectronic and Electrochemical Properties of Vanadium Pentoxide Nanowires Synthesized by Vapor-Solid Process

PubMed Central

Pan, Ko-Ying; Wei, Da-Hua

2016-01-01

Substantial synthetic vanadium pentoxide (V2O5) nanowires were successfully produced by a vapor-solid (VS) method of thermal evaporation without using precursors as nucleation sites for single crystalline V2O5 nanowires with a (110) growth plane. The micromorphology and microstructure of V2O5 nanowires were analyzed by scanning electron microscope (SEM), energy-dispersive X-ray spectroscope (EDS), transmission electron microscope (TEM) and X-ray diffraction (XRD). The spiral growth mechanism of V2O5 nanowires in the VS process is proved by a TEM image. The photo-luminescence (PL) spectrum of V2O5 nanowires shows intrinsic (410 nm and 560 nm) and defect-related (710 nm) emissions, which are ascribable to the bound of inter-band transitions (V 3d conduction band to O 2p valence band). The electrical resistivity could be evaluated as 64.62 Ω·cm via four-point probe method. The potential differences between oxidation peak and reduction peak are 0.861 V and 0.470 V for the first and 10th cycle, respectively. PMID:28335268

Ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling

NASA Astrophysics Data System (ADS)

Bangi, Uzma K. H.; Park, Hyung-Ho; Han, Wooje; Prakshale, Vipul M.; Deshmukh, Lalasaheb P.

2017-05-01

The experimental results on the ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling have been reported in the present work. Lead oxide nanoflowers were prepared employing mixed ligands by subjecting the formed precipitate to ultrasonication and grinding/ball milling. The effect of ball milling as well as fine grinding in agate mortar on the microstructure and surface morphology of the lead oxide was studied. The characteristics of synthesized PbO were studied using X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and field emission scanning electron microscopy techniques. XRD results demonstrated the tetragonal phase of PbO with crystallite size of around 25 nm and strain of 3.6 × 10-3 calculated from Williamson-Hall plot. FESEM images manifested the formation of nanodiscs and nanoflowers with a diameter of around 300 nm and thickness of 50 nm. XPS spectra revealed the formation of PbO with photoelectron peak of Pb 4f and O 1 s lied at 137.68 and 529.96 eV. Moreover, FTIR spectrum exhibited Pb-O bond peak in the range of 400-530 cm-1.

Biogenic nano-scale silver particles by Tephrosia purpurea leaf extract and their inborn antimicrobial activity

NASA Astrophysics Data System (ADS)

Ajitha, B.; Ashok Kumar Reddy, Y.; Reddy, P. Sreedhara

2014-03-01

In this paper we report the green synthesis of silver nanoparticles (Ag NPs) using Tephrosia purpurea leaf extract. The biomolecules present in the leaf extract are responsible for the formation of Ag NPs and they found to play dual role of both reducing as well as capping agents. The high crystallinity of Ag NPs is evident from bright circular spot array of SAED pattern and diffraction peaks in XRD profile. The synthesized Ag NPs are found to be nearly spherical ones with size approximately ∼20 nm. FTIR spectrum evidences the presence of different functional groups of biomolecules participated in encapsulating Ag NPs and the possible mechanism of Ag NPs formation was also suggested. Appearance of yellow color and surface plasmon resonance (SPR) peak at 425 nm confirms the Ag NPs formation. PL spectra showed decrement in luminescence intensity at higher excitation wavelengths. Antimicrobial activity of Ag NPs showed better inhibitory activity towards Pseudomonas spp. and Penicillium spp. compared to other test pathogens using standard Kirby-Bauer disc diffusion assay.

Bark extract mediated green synthesis of silver nanoparticles: Evaluation of antimicrobial activity and antiproliferative response against osteosarcoma.

PubMed

Nayak, Debasis; Ashe, Sarbani; Rauta, Pradipta Ranjan; Kumari, Manisha; Nayak, Bismita

2016-01-01

In the current investigation we report the biosynthesis potentials of bark extracts of Ficus benghalensis and Azadirachta indica for production of silver nanoparticle without use of any external reducing or capping agent. The appearance of dark brown color indicated the complete nanoparticle synthesis which was further validated by absorbance peak by UV-vis spectroscopy. The morphology of the synthesized particles was characterized by Field emission- scanning electron microscopy (Fe-SEM) and atomic force microscopy (AFM). The X-ray diffraction (XRD) patterns clearly illustrated the crystalline phase of the synthesized nanoparticles. ATR-Fourier Transform Infrared (ATR-FTIR) spectroscopy was performed to identify the role of various functional groups in the nanoparticle synthesis. The synthesized nanoparticles showed promising antimicrobial activity against Gram negative (Escherichia coli, Pseudomonas aeruginosa and Vibrio cholerae) and Gram positive (Bacillus subtilis) bacteria. The synthesized nano Ag also showed antiproliferative activity against MG-63 osteosarcoma cell line in a dose dependent manner. Thus, these synthesized Ag nanoparticles can be used as a broad spectrum therapeutic agent against osteosarcoma and microorganisms. Copyright © 2015 Elsevier B.V. All rights reserved.

Facile Synthesis and Optical Properties of Small Selenium Nanocrystals and Nanorods

NASA Astrophysics Data System (ADS)

Jiang, Fengrui; Cai, Weiquan; Tan, Guolong

2017-06-01

Selenium is an important element for human's health, small size is very helpful for Se nanoparticles to be absorbed by human's body. Here, we present a facile approach to fabrication of small selenium nanoparticles (Nano-Se) as well as nanorods by dissolving sodium selenite (Na2SeO3) in glycerin and using glucose as the reduction agent. The as-prepared selenium nanoparticles have been characterized by X-ray diffraction (XRD), UV-Vis absorption spectroscopy and high resolution transmission electron microscope (HRTEM). The morphology of small Se nanoparticles and nanorods have been demonstrated in the TEM images. A small amount of 3-mercaptoproprionic acid (MPA) and glycerin play a key role on controlling the particle size and stabilize the dispersion of Nano-Se in the glycerin solution. In this way, we obtained very small and uniform Se nanoparticles; whose size ranges from 2 to 6 nm. This dimension is much smaller than the best value (>20 nm) ever reported in the literatures. Strong quantum confinement effect has been observed upon the size-dependent optical spectrum of these Se nanoparticles.

Facile Synthesis of Self-Assembled Flower-Like Mesoporous Zinc Oxide Nanoflakes for Energy Applications

NASA Astrophysics Data System (ADS)

Saranya, P. E.; Selladurai, S.

Flower-shaped self-assembled zinc oxide (ZnO) nanoflakes were successfully synthesized via a temperature-controlled hydrothermal method. The crystallinity and phase formation of the compound were determined from powder X-ray diffraction (PXRD) result. Surface morphology investigations reveal the self-assembled ZnO nanoflakes to form a spherical flower-like structure. In addition, the particle size was determined from high-resolution transmission electron microscope measurement as 18nm which is in accord with XRD and UV results. X-ray photo electron spectroscopy studies reveal the chemical composition and oxidation state of the ZnO nanoparticle. The specific surface area was calculated, and mesoporous nature was confirmed using Brunauer-Emmett-Teller analysis. Results support the superior interaction between the electrode and electrolyte ions through surface pores. Capacitive performance of the ZnO electrode material was determined using cyclic voltammetry and galvanostatic charge/discharge studies, and a maximum specific capacitance of 322F/g was obtained at 5mV/sec. Electrochemical impedance spectrum reveals the materials fast charge transfer kinetics.

Electrical and optical properties of sol-gel derived La modified PbTiO 3 thin films

NASA Astrophysics Data System (ADS)

Chopra, Sonalee; Sharma, Seema; Goel, T. C.; Mendiratta, R. G.

2004-09-01

Lanthanum modified lead titanate (Pb 1- xLa xTi 1- x/4 O 3) PLT x ( x=0.08 i.e. PLT8) sol-gel derived thin films have been prepared on indium tin oxide (ITO) coated glass and quartz substrates using lead acetate trihydrate, lanthanum acetate hydrate and titanium isopropoxide as precursors along with 2-methoxyethanol as solvent and acetic acid as catalyst by spin coating method. The microstructure and surface morphology of the films annealed at 650 °C have been studied by X-ray diffraction technique and atomic force microscope (AFM). XRD has shown a single phase with tetragonal structure and AFM images have confirmed a smooth and crack-free surface with low surface roughness. The dependence of leakage current on applied voltage show ohmic behavior at low field region with a space charge conduction mechanism at high fields. The wavelength dispersion curve of thin films obtained from the transmission spectrum of thin films show that the films have high optical transparency in the visible region.

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

Chondroitin sulfate template-mediated biomimetic synthesis of nano-flake hydroxyapatite

NASA Astrophysics Data System (ADS)

He, Dan; Xiao, Xiufeng; Liu, Fang; Liu, Rongfang

2008-11-01

By Ca(NO 3) 2·4H 2O and (NH 4) 3PO 4·3H 2O as reagents and chondroitin sulfate (ChS) as a template, nano-flake hydroxyapatite (HA) is synthesized using a biomimetic method according to the biomineralization theory. HA crystals obtained are characterized in crystalline phase, microstructure, chemical composition and morphology by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscopy (TEM) and elemental analysis respectively. UV-vis spectrum is adopted to investigate interactions between functional groups ChS and HA. The results show that HA crystal nucleation and growth take place in chemical interactions between HA crystals and ChS as a template. And elemental analysis indicates that obtained HA contains a small amount of ChS. Furthermore, ChS concentration significantly affects the morphology of HA crystals. Staple-fiber-like HA crystals can be obtained at a low concentration in ChS, and flake-like HA crystals synthesized at a high concentration (≥0.5 wt.%) of ChS as a template.

Investigation of the effect of alumina and compaction pressure on physical, electrical and tribological properties of Al-Fe-Cr-Al2O3 powder composites

NASA Astrophysics Data System (ADS)

Mohsin, Mohammad; Mohd, Aas; Suhaib, M.; Arif, Sajjad; Arif Siddiqui, M.

2017-10-01

In this experimental work, aluminium Al-20Fe-5Cr (in wt.%) matrix reinforced with varying wt.% Al2O3 (0, 10, 20 and 30) and compaction pressure (470, 550 and 600 MPa) were prepared by powder metallurgy technique. The characterization of composites were performed by scanning electron microscopy (SEM), x-ray diffraction (XRD), energy dispersive spectrum (EDS) and elemental mapping. Uniform distribution of Al2O3 in aluminium matrix were observed by elemental mapping. The composites showed an increase in density and hardness by increasing both alumina and compaction pressure. While, electrical conductivity decreased by the addition of alumina. The tribological study of the composites were performed on pin-on-disc apparatus at sliding conditions (applied load 40 N, sliding speed 1.5 m s-1, sliding distance 300 m). The tribological properties of the composites were improved by increasing alumina and compaction pressure. SEM analysis were also carried out to understand wear mechanism of the worn surfaces of various fabricated composites and aluminium matrix.

In2O3-ZnO heterostructure development in electrical and photoluminescence properties of In2O3 1-D nanostructures

NASA Astrophysics Data System (ADS)

Shariati, M.; Ghafouri, V.

2014-05-01

Indium Oxide quasi one-dimensional (1D) nanostructures known as nanowires and nanorods synthesis using the thermal evaporation method, has been articulated. To nucleate growth sites, substrate seeding promoted 1D nanostructures growth. The catalyst-mediated growth mechanism showed more favorable morphologies and physical properties in under vacuum conditions associated with bottom-up technique. Scanning electron microscopy (SEM) results showed that the Zn-doped 1D nanostructures had spherical caps. The X-ray diffraction (XRD) pattern and energy-dispersive X-ray (EDX) spectrum indicated that these caps intensively associated with ZnO. Therefore, it was reasonable that the vapor-liquid-solid mechanism (VLS) was responsible for the growth of the In2O3-ZnO heterostructure nanowires. This technique enhances optical and electrical properties in nanostructures. The photoluminescence (PL) analysis in Zn-doped In2O3 nanowires and nanorods shows that the intensity of the visible and UV-region emissions overwhelmingly increases and resistance measurement professes the improvement of linear conductance in VLS growth mechanism.

Novel chemical synthesis and characterization of copper pyrovanadate nanoparticles and its influence on the flame retardancy of polymeric nanocomposites

NASA Astrophysics Data System (ADS)

Ghiyasiyan-Arani, Maryam; Masjedi-Arani, Maryam; Ghanbari, Davood; Bagheri, Samira; Salavati-Niasari, Masoud

2016-05-01

In this work, copper pyrovanadate (Cu3V2O7(OH)2(H2O)2) nanoparticles have been synthesized by a simple and rapid chemical precipitation method. Different copper-organic complexes were used to control the size and morphology of products. The morphology and structure of the as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectrum, electron dispersive X-ray spectroscopy (EDX), thermal gravimetric analysis (TGA), differential thermal analysis (DTA) and photoluminescence (PL) spectroscopy. The influence of copper pyrovanadate nanostructures on the flame retardancy of the polystyrene, poly vinyl alcohol and cellulose acetate was studied. Dispersed nanoparticles play the role of a magnetic barrier layer, which slows down product volatilization and prevents the flame and oxygen from the sample during decomposition of the polymer. Cu3V2O7(OH)2(H2O)2 is converted to Cu3V2O8 with an endothermic reaction which simultaneously releases water and decrease the temperature of the flame region.

Synthesis process and photocatalytic properties of BiOBr nanosheets for gaseous benzene.

PubMed

Liu, Yu; Yin, Yongquan; Jia, Xueqing; Cui, Xiangyu; Tian, Canrui; Sang, Yuanhua; Liu, Hong

2016-09-01

A series of nano-BiOBr were prepared by an effective hydrothermal method in the presence of cetyltrimethyl ammonium bromide (CTAB) and ethanol at different calcination temperatures. The as-prepared nano-BiOBr samples were characterized by measuring the specific area (S BET), UV-Vis diffuse reflectance spectrum, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The results show that the calcination temperature has an important impact on the morphology and microstructure of BiOBr. The nano-BiOBr calcined at 120 °C showed excellent photocatalytic degradation properties for benzene, with photocatalytic degradation rate of 75 % for benzene under UV irradiation for 90 min, and removal efficiency of benzene was significantly enhanced by using nano-BiOBr catalyst compared to UV irradiation alone. BiOBr catalyst possessed good photocatalytic activity even after three consecutive photocatalytic reaction cycles, illustrating its excellent stability. The photocatalytic degradation of benzene followed the first-order kinetics, and the good catalytic capability of nano-BiOBr catalyst can be attributed to its crystalline, hierarchical nanostructure and nanosheet thickness.

Performance improvement of pentacosa-diynoic acid label dosimeter for radiation processing technology

NASA Astrophysics Data System (ADS)

Abdel-Fattah, A. A.; Soliman, Y. S.

2017-12-01

A radiation sensitive material, 10,12-pentacosa-diynoic acid (PCDA), was incorporated into polyvinyl butyral (PVB) films to develop indicators/dosimeters for blood and food irradiation. The present study aims to improve the dosimetric performance of these previously prepared dosimeters and to extend their shelf life by the combination of a radical scavenger, propyl gallate (PG), and a UV absorber, tinuvin-p (TP). The X-ray diffraction (XRD) patterns of the dosimeters were analysed and their dosimetric characteristics were investigated by specular reflectance in the visible spectrum range of 400-700 nm. Upon irradiation, the films turn blue exhibiting two main bands around 670 and 620 nm. Their dose-response functions were fitted by a double exponential growth, 5 parameters, equation. Irradiation temperature influences the dosimeter response at 670 nm without causing thermochromic transition up to 50 °C in poly-PCDA. The useful dose range is 5-4000 Gy depending on the wavelengths of analysis and PCDA content in the films. The overall uncertainty of dose measurement is less than 6% at 2σ.

Studies on growth, thermal, optical, vibrational properties and hyperpolarizability of a complex orthonitroaniline with picric acid

NASA Astrophysics Data System (ADS)

Anandhi, S.; Shyju, T. S.; Gopalakrishnan, R.

2010-11-01

The present article reports the growth of single crystals of a complex Orthonitroaniline with picric acid (2[C 6H 6N 2O 2]·C 6H 2(NO 2) 3OH) (ONAP) by solution growth (slow evaporation) method at room temperature. Single crystal XRD, UV-vis spectral analysis and TGA/DTA studies were carried out. FT-IR and Raman spectra were recorded to explore information of the functional groups. The high-resolution X-ray diffraction curve reveals the internal structural low angle boundaries. The PL spectrum of the title compound shows green emission. Dielectric behaviour was investigated at 33 and 70 °C. The dipole moment and first-order hyperpolarizability ( β) values were evaluated by using Gaussian 98 W software package with the help of B3LYP the density functional theory (DFT) method. The possible modes of vibrations are theoretically predicted by factor group analysis. The mechanical stability of the grown crystal was tested with Vicker's microhardness tester and the work hardening coefficient of the grown material was estimated.

Graft polymerization of guar gum with acryl amide irradiated by microwaves for colonic drug delivery.

PubMed

Shahid, Muhammad; Bukhari, Shazia Anwer; Gul, Yousra; Munir, Hira; Anjum, Fozia; Zuber, Mohammad; Jamil, Tahir; Zia, Khalid Mahmood

2013-11-01

This article is aimed to discuss the modification of guar gum through microwave irradiation by varying the time of irradiation. The characterization of the modified products was carried out using FTIR spectroscopic analysis. The FT-IR spectrum of the pure guar gum (GG) sample showed a broad peak at 3298 cm(-1) while the modified GG sample displayed a peak at 1541 cm(-1) which was absent in the crude sample. The X-ray diffraction (XRD) analysis confirmed the increase in crystallinity due to grafting of the sample with polyacrylamide (GG-g-PAM). Scanning electron microscope (SEM) images revealed that granular form of guar gum was changed into fibrillar structure after grafting. Thermo-gravimetric analysis of the modified samples was also carried out and discussed. The role of guar gum as a matrix for controlled release of drug triamcinolone was evaluated. The GG-acrylamide grafted samples presented a correlation between drug release and time of microwave exposure. The results revealed that such modified product has potential applications in colonic drug delivery system. Copyright © 2013 Elsevier B.V. All rights reserved.

Hot filament CVD of boron nitride films

DOEpatents

Rye, Robert R.

1992-01-01

Using a hot filament (.apprxeq.1400.degree. C.) to activate borazine (B.sub.3 N.sub.3 H.sub.6) molecules for subsequent reaction with a direct line-of-sight substrate, transparent boron ntiride films as thick as 25,000 angstroms are grown for a substrate temperature as low as 100.degree. C. The minimum temperature is determined by radiative heating from the adjacent hot filament. The low temperature BN films show no indication of crystallinity with X-ray diffraction (XRD). X-ray photoelectron spectra (XPS) show the films to have a B:N ratio of 0.97:1 with no other XPS detectable impurities above the 0.5% level. Both Raman and infrared (IR) spectroscopy are characteristic of h-BN with small amounts of hydrogen detected as N-H and B-H bands in the IR spectrum. An important feature of this method is the separation and localization of the thermal activation step at the hot filament from the surface reaction and film growth steps at the substrate surface. This allows both higher temperature thermal activation and lower temperature film growth.

Easy synthesis of bismuth iron oxide nanoparticles as photocatalyst for solar hydrogen generation from water

NASA Astrophysics Data System (ADS)

Deng, Jinyi

In this study, high purity bismuth iron oxide (BiFeO3/BFO) nanoparticles of size 50-80 nm have been successfully synthesized by a simple sol-gel method using urea and polyvinyl alcohol at low temperature. X-ray diffraction (XRD) measurement is used to optimize the synthetic process to get highly crystalline and pure phase material. Diffuse reflectance ultraviolet-visible (DRUV-Vis) spectrum indicates that the absorption cut-off wavelength of the nanoparticles is about 620 nm, corresponding to an energy band gap of 2.1 eV. Compared to BaTiO3, BFO has a better degradation of methyl orange under light radiation. Also, photocatalytic tests prove this material to be efficient towards water splitting under simulated solar light to generate hydrogen. The simple synthetic methodology adopted in this paper will be useful in developing low-cost semiconductor materials as effective photocatalysts for hydrogen generation. Photocatalytic tests followed by gas chromatography (GC) analyses show that BiFeO3 generates three times more hydrogen than commercial titania P25 catalyst under the same experimental conditions.

Structural characterization of precious-mean quasiperiodic Mo/V single-crystal superlattices grown by dual-target magnetron sputtering

NASA Astrophysics Data System (ADS)

Birch, J.; Severin, M.; Wahlström, U.; Yamamoto, Y.; Radnoczi, G.; Riklund, R.; Sundgren, J.-E.; Wallenberg, L. R.

1990-05-01

A class of quasiperiodic superlattice structures, which can be generated by the concurrent inflation rule A-->AmB and B-->A (where m=positive integer), has been studied both theoretically and experimentally. Given that the ratios between the thicknesses of the two superlattice building blocks, A and B, are chosen to be γ(m)=[m+(m2+4)1/2]/2 (known as the ``precious means''), then the x-ray- and electron-diffraction peak positions are analytically found to be located at the wave vectors q=2πΛ-1r[γ(m)]k, where r and k are integers and Λ is an average superlattice wavelength. The analytically obtained results have been compared to experimental results from single-crystalline Mo/V superlattice structures, generated with m=1, 2, and 3. The superlattices were grown by dual-target dc-magnetron sputtering on MgO(001) substrates kept at 700 °C. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) showed that the analytical model mentioned above predicts the peak positions of the experimental XRD and SAED spectra with a very high accuracy. Furthermore, numerical calculations of the diffraction intensities based on a kinematical model of diffraction showed good agreement with the experimental data for all three cases. In addition to a direct verification of the quasiperiodic modulation, both conventional and high-resolution cross-sectional transmission electron microscopy (XTEM) showed that the superlattices are of high crystalline quality with sharp interfaces. Based on lattice resolution images, the width of the interfaces was determined to be less than two (002) lattice-plane spacings (~=0.31 nm).

X-ray diffraction study of A- plane non-polar InN epilayer grown by MOCVD

NASA Astrophysics Data System (ADS)

Moret, Matthieu; Briot, Olivier; Gil, Bernard

2015-03-01

Strong polarisation-induced electric fields in C-plane oriented nitrides semiconductor layers reduce the performance of devices. Eliminating the polarization fields can be achieved by growing nitrides along non polar direction. We have grown non polar A-plane oriented InN on R-plane (1‾102) nitridated sapphire substrate by MOCVD. We have studied the structural anisotropy observed in these layers by analyzing High Resolution XRay Diffraction rocking curve (RC) experiments as a function of the in-plane beam orientation. A-plane InN epilayer have a unique epitaxial relationship on R-Plane sapphire and show a strong structural anisotropy. Full width at half maximum (FWHM) of the InN(11‾20) XRD RC values are contained between 44 and 81 Arcmin. FWHM is smaller when the diffraction occurs along the [0001] and the largest FWHM values, of the (11‾20) RC, are obtained when the diffraction occurs along the [1‾100] in-plane direction. Atomic Force Microscopy imaging revealed morphologies with well organized crystallites. The grains are structured along a unique crystallographic orientation of InN, leading to larger domains in this direction. This structural anisotropy can be, in first approximation, attributed to the difference in the domain sizes observed. XRD reciprocal space mappings (RSM) were performed in asymmetrical configuration on (13‾40) and (2‾202) diffraction plane. RSM are measured with a beam orientation corresponding to a maximal and a minimal width of the (11‾20) Rocking curves, respectively. A simple theoretical model is exposed to interpret the RSM. We concluded that the dominant contribution to the anisotropy is due to the scattering coherence length anisotropy present in our samples.

Investigation of photoluminescence and dielectric properties of pure and Fe doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmad, Arham S.

2018-05-01

The nanocrystallites of pure and Fe doped Nickel Oxide (NiO) were synthesized by the cost effective co-precipitation method using nickel nitrate as the initial precursor. The synthesized nickel oxide nanoparticles were characterized by X-Ray Diffraction (XRD), Photoluminiscence Spectroscopy (PL), LCR meter. The crystallite size of synthesized pure Nickel Oxide nanoparticles obtained by XRD using Debye Scherer's formula was found to be 21.8nm and the size decreases on increasing the dopant concentration. The optical properties were analyzed by PL and dielectric ones by using LCR meter.

Preparation of Cu-doped nickel oxide thin films and their properties

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

Gowthami, V.; Meenakshi, M.; Anandhan, N.

2014-04-24

Copper doped Nickel oxide film was preferred on glass substrate by simple nebulizer technique keeping the substrate temperature at 350°C and characterized by X-ray diffraction (XRD), Photoluminescence (PL) and Four probe resistivity measurements. XRD studies indicated cubic structure and the crystallites are preferentially oriented along the [111] direction. Interesting results have been obtained from the study of PL spectra. A peak corresponding to 376nm in the emission spectra for 0%, 5% and 10% copper doped samples. The samples show sharp and strong UV emission corresponding to the near band edge emission under excitation of 275nm.

Observation of martensitic transformation in Ni50Mn41Cu4Sn5 Heusler alloy prepared by mechanical alloying

NASA Astrophysics Data System (ADS)

Saini, Dinesh; Singh, Satyavir; Banerjee, M. K.; Sachdev, K.

2017-05-01

Mechanical alloying route has been employed for preparation of a single phase Ni50Mn41Cu4Sn5 (atomic %) Heusler alloy. Use of high energy planetary ball mill enables successful preparation of the same as authenticated by detailed X-ray diffraction (XRD) study. Microstructural study is carried out by optical and scanning electron microscopic techniques. XRD results reveal that increasing milling time leads to reduction in crystallite size and concurrent increase in lattice strain. Microstructural results indicate formation of self-assembled martensite twins.

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

Ren, Fang; Williams, Travis; Hattrick-Simpers, Jason

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.

Preparation and characterization of Fe50Co50 nanostructured alloy

NASA Astrophysics Data System (ADS)

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

2014-04-01

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

Structural and electrical study of ZrO{sub 2} nanoparticles modified with surfactants

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

Sidhu, Gaganpreet Kaur; Kumar, Rajesh, E-mail: rajeshbaboria@gmail.com; Tripathi, S. K.

2015-06-24

Zirconia ceramic is one of the most investigated materials for its outstanding mechanical properties and ionic conduction properties, due to its high oxygen ion conduction. In order to achieve novel properties of zirconia nanoparticles, nanoparticles of zirconia are modified by using two different surfactants (SDS and CTAB) were prepared by in-situ method using zirconia/surfactant dispersions. Zirconia nanoparticles with surfactant (SDS or CTAB) were synthesized by hydrothermal method. The structural and optical properties of Zirconia/surfactant nanoparticles were investigated comprehensively by X-Ray diffraction (XRD), and electrical measurements. XRD highlights the crystalline behavior of nanoparticles.

Multivariate analysis of DSC-XRD simultaneous measurement data: a study of multistage crystalline structure changes in a linear poly(ethylene imine) thin film.

PubMed

Kakuda, Hiroyuki; Okada, Tetsuo; Otsuka, Makoto; Katsumoto, Yukiteru; Hasegawa, Takeshi

2009-01-01

A multivariate analytical technique has been applied to the analysis of simultaneous measurement data from differential scanning calorimetry (DSC) and X-ray diffraction (XRD) in order to study thermal changes in crystalline structure of a linear poly(ethylene imine) (LPEI) film. A large number of XRD patterns generated from the simultaneous measurements were subjected to an augmented alternative least-squares (ALS) regression analysis, and the XRD patterns were readily decomposed into chemically independent XRD patterns and their thermal profiles were also obtained at the same time. The decomposed XRD patterns and the profiles were useful in discussing the minute peaks in the DSC. The analytical results revealed the following changes of polymorphisms in detail: An LPEI film prepared by casting an aqueous solution was composed of sesquihydrate and hemihydrate crystals. The sesquihydrate one was lost at an early stage of heating, and the film changed into an amorphous state. Once the sesquihydrate was lost by heating, it was not recovered even when it was cooled back to room temperature. When the sample was heated again, structural changes were found between the hemihydrate and the amorphous components. In this manner, the simultaneous DSC-XRD measurements combined with ALS analysis proved to be powerful for obtaining a better understanding of the thermally induced changes of the crystalline structure in a polymer film.

Aspherical-atom modeling of coordination compounds by single-crystal X-ray diffraction allows the correct metal atom to be identified.

PubMed

Dittrich, Birger; Wandtke, Claudia M; Meents, Alke; Pröpper, Kevin; Mondal, Kartik Chandra; Samuel, Prinson P; Amin Sk, Nurul; Singh, Amit Pratap; Roesky, Herbert W; Sidhu, Navdeep

2015-02-02

Single-crystal X-ray diffraction (XRD) is often considered the gold standard in analytical chemistry, as it allows element identification as well as determination of atom connectivity and the solid-state structure of completely unknown samples. Element assignment is based on the number of electrons of an atom, so that a distinction of neighboring heavier elements in the periodic table by XRD is often difficult. A computationally efficient procedure for aspherical-atom least-squares refinement of conventional diffraction data of organometallic compounds is proposed. The iterative procedure is conceptually similar to Hirshfeld-atom refinement (Acta Crystallogr. Sect. A- 2008, 64, 383-393; IUCrJ. 2014, 1,61-79), but it relies on tabulated invariom scattering factors (Acta Crystallogr. Sect. B- 2013, 69, 91-104) and the Hansen/Coppens multipole model; disordered structures can be handled as well. Five linear-coordinate 3d metal complexes, for which the wrong element is found if standard independent-atom model scattering factors are relied upon, are studied, and it is shown that only aspherical-atom scattering factors allow a reliable assignment. The influence of anomalous dispersion in identifying the correct element is investigated and discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Morphology and crystallinity of sisal nanocellulose after sonication

NASA Astrophysics Data System (ADS)

Sosiati, H.; Wijayanti, D. A.; Triyana, K.; Kamiel, B.

2017-09-01

Different preparation methods on the natural fibers resulted in different morphology. However, the relationships between type of natural fibers, preparation methods and the morphology of produced nanocellulose could not be exactly defined. The sisal nanocellulose was presently prepared by alkalization and bleaching followed by sonication to verify changes in the morphology and crystallinity of nanocellulose related to the formation mechanism. The extracted microcellulose was subjected to scanning electron microscopy (SEM) and x-ray diffraction (XRD) analysis. The isolated cellulose nanospheres were examined with respect to morphology by SEM and transmission electron microscopy (TEM) and, to crystallinity by electron diffraction analysis. Bleaching after alkalization made the microfibrils clearly separated from each other to the individual fiber whose width of the single fiber was ranging from 6 to 13 µm. The XRD crystallinity index (CI) of microcellulose gradually increased after the chemical treatments; 83.12% for raw sisal fiber, 88.57% for alkali treated fiber and 94.03% for bleached fibers. The ultrasonic agitation after bleaching that was carried out at 750 Watt, 20 kHz and amplitude of 39% for 2 h produces homogeneous cellulose nanospheres less than 50 nm in diameter with relatively low crystallinity. The electron diffraction analysis confirmed that the low crystallinity of produced nnocellulose is related to the effect of chemical treatment done before sonication.

Compositional and quantitative microtextural characterization of historic paintings by micro-X-ray diffraction and Raman microscopy.

PubMed

Romero-Pastor, Julia; Duran, Adrian; Rodríguez-Navarro, Alejandro Basilio; Van Grieken, René; Cardell, Carolina

2011-11-15

This work shows the benefits of characterizing historic paintings via compositional and microtextural data from micro-X-ray diffraction (μ-XRD) combined with molecular information acquired with Raman microscopy (RM) along depth profiles in paint stratigraphies. The novel approach was applied to identify inorganic and organic components from paintings placed at the 14th century Islamic University-Madrasah Yusufiyya-in Granada (Spain), the only Islamic University still standing from the time of Al-Andalus (Islamic Spain). The use of μ-XRD to obtain quantitative microtextural information of crystalline phases provided by two-dimensional diffraction patterns to recognize pigments nature and manufacture, and decay processes in complex paint cross sections, has not been reported yet. A simple Nasrid (14th century) palette made of gypsum, vermilion, and azurite mixed with glue was identified in polychromed stuccos. Here also a Christian intervention was found via the use of smalt, barite, hematite, Brunswick green and gold; oil was the binding media employed. On mural paintings and wood ceilings, more complex palettes dated to the 19th century were found, made of gypsum, anhydrite, barite, dolomite, calcite, lead white, hematite, minium, synthetic ultramarine blue, and black carbon. The identified binders were glue, egg yolk, and oil.

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

Mohamad, Khairul Anuar; Rusnan, Fara Naila; Seria, Dzulfahmi Mohd Husin

Investigation on the physical characterization and comparison of organic thin film based on a soluble 6,13-bis(triisopropylsilylethynyl) (TIPS) pentacene is reported. Oriented thin-films of pentacene have been successfully deposited by flow-coating method, in which the chloroform solution is sandwiched between a transparent substrate and a slide glass, followed by slow-drawing of the substrate with respect to the slide glass. Molecular orientation of flow-coated TIPS-pentacene is comparable to that of the thermal-evaporated pentacene thin film by the X-ray diffraction (XRD) results. XRD results showed that the morphology of flow-coated soluble pentacene is similar to that of the thermal-evaporated pentacene thin films inmore » series of (00l) diffraction peaks where the (001) diffraction peaks are strongest in the nominally out-of-plane intensity and interplanar spacing located at approximately 2θ = 5.33° (d-spacing, d{sub 001} = 16 Å). Following that, ITO/p-TIPS-pentacene/n-ZnO/Au vertical diode was fabricated. The diode exhibited almost linear characteristics at low voltage with nonlinear characteristics at higher voltage which similar to a pn junction behavior. The results indicated that the TIPS-pentacene semiconductor active thin films can be used as a hole injection layer for fabrication of a vertical organic transistor.« less

Thermal evaporation and condensation synthesis of metallic Zn layered polyhedral microparticles

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

Khan, Waheed S.; Cao, Chuanbao, E-mail: cbcao@bit.edu.cn; Usman, Zahid

2011-12-15

Highlights: Black-Right-Pointing-Pointer Zn polyhedral microparticles prepared by thermal evaporation and condensation route. Black-Right-Pointing-Pointer Vapour-solid process based growth model governs the formation of Zn microparticles. Black-Right-Pointing-Pointer A strong PL emission band is observed at 369 nm in UV region. Black-Right-Pointing-Pointer Radiative recombination of electrons in the s, p conduction band and the holes in the d bands causes this emission. -- Abstract: Metallic zinc layered polyhedral microparticles have been fabricated by thermal evaporation and condensation technique using zinc as precursor at 750 Degree-Sign C for 120 min and NH{sub 3} as a carrier gas. The zinc polyhedral microparticles with oblate sphericalmore » shape are observed to be 2-9 {mu}m in diameter along major axes and 1-7 {mu}m in thickness along minor axes. The structural, compositional and morphological characterizations were performed by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). A vapour-solid (VS) mechanism based growth model has been proposed for the formation of Zn microparticles. Room temperature photoluminescence (PL) emission spectrum of the product exhibited a strong emission band at 369 nm attributed to the radiative recombination of electrons in the s, p conduction band near Fermi surface and the holes in the d bands generated by the optical excitation.« less

X-ray diffraction study of the mineralogy of microinclusions in fibrous diamond

NASA Astrophysics Data System (ADS)

Smith, Evan; Kopylova, Maya; Dubrovinksy, Leonid

2010-05-01

Fibrous diamond, occurring both as cuboids and as coatings over non-fibrous diamond nuclei, is translucent due to the presence of millions of sub-micron-sized mineral and fluid inclusions. Diamond is strong and relatively inert, making it an excellent vessel to preserve trapped materials. These microinclusions represent direct samples of natural diamond-forming mantle fluids, and are critical for our understanding of diamond genesis. Traditionally, infrared spectroscopy, Raman spectroscopy, secondary ion mass spectrometry, electron microprobe, and FIB-TEM techniques have proven to be effective for the study of microinclusions in diamond. The abundance and random orientation of included minerals in fibrous diamond make them amenable to a powder-type X-ray diffraction (XRD) technique. This technique provides an accurate way to identify included minerals. It also has the advantage of analyzing thousands of inclusions simultaneously, rather than analyzing one inclusion at a time, as with common FIB-TEM techniques. XRD provides a bulk analysis, giving a superior measure of relative abundances of included minerals, as well as potentially accounting for small quantities of minerals that might otherwise be overlooked. We studied fibrous cuboid diamonds with microinclusions from the Democratic Republic of Congo (DRC) (23 samples), Brazil (4 samples), Jericho (1 sample), and Wawa conglomerates (9 samples). XRD analysis was performed at the Bayerisches Geoinstitut (BGI), University of Bayreuth, Germany. The unique XRD setup consists of a RIGAKU FR-D high-brilliance source, OSMIC Inc. Confocal Max-Flux optics, and a SMART APEX 4K CCD area detector. Preliminary XRD studies of microinclusions 8 fibrous diamonds from the DRC showed a prevalence of silicates with structural and coordinated H2O. Sheet silicates constituted 9 out of 13 detected minerals, with phlogopite-biotite micas being present in 4 out of 8 samples. Other detected minerals were 2 chlorite minerals, 2 clay phyllosilicates, serpentine, zircon, a hydrous carbonate and an unidentified zeolite. Many of these phases are deuteric, replacing high-T, high-P micas and carbonates that precipitate from the fluid in the diamond stability field. The ongoing XRD study will (1) elucidate the mineralogy of fluid inclusions in diamonds from Wawa, (2) compare XRD analyses to distinguish between diamonds with carbonatitic versus saline fluid compositions, and (3) reveal whether carbonates occur as crystalline phases or as dissolved or amorphous material in fibrous diamond.

Is Tridymite at Gale Crater Evidence for Silicic Volcanism on Mars?

NASA Technical Reports Server (NTRS)

Morris, Richard V.; Vaniman, David T.; Ming, Douglas W.; Graff, Trevor G.; Downs, Robert T.; Fendrich, Kim; Mertzman, Stanley A.

2016-01-01

The X-ray diffraction (XRD) instrument (CheMin) onboard the MSL rover Curiosity detected 17 wt% of the SiO2 polymorph tridymite (relative to bulk sample) for the Buckskin drill sample (73 wt% SiO2) obtained from sedimentary rock in the Murray formation at Gale Crater, Mars. Other detected crystalline materials are plagioclase, sanidine, cristobalite, cation-deficient magnetite, and anhydrite. XRD amorphous material constitutes approx. 60 wt% of bulk sample, and the position of its broad diffraction peak near approx. 26 deg. 2-theta is consistent with opal-A. Tridymite is a lowpressure, high-temperature mineral (approx. 870 to 1670 deg. C) whose XRD-identified occurrence on the Earth is usually associated with silicic (e.g., rhyolitic) volcanism. High SiO2 deposits have been detected at Gale crater by remote sensing from martian orbit and interpreted as opal-A on the basis H2O and Si-OH spectral features. Proposed opal-A formation pathways include precipitation of silica from lake waters and high-SiO2 residues of acid-sulfate leaching. Tridymite is nominally anhydrous and would not exhibit these spectral features. We have chemically and spectrally analyzed rhyolitic samples from New Mexico and Iwodake volcano (Japan). The glassy (by XRD) NM samples have H2O spectral features similar to opal-A. The Iwodake sample, which has been subjected to high-temperature acid sulfate leaching, also has H2O spectral features similar to opal-A. The Iwodake sample has approx. 98 wt% SiO2 and 1% wt% TiO2 (by XRF), tridymite (>80 wt.% of crystalline material without detectable quartz by XRD), and H2O and Si-OH spectral features. These results open the working hypothesis that the opal-A-like high-SiO2 deposits at Gale crater detected from martian orbit are products of alteration associated with silicic volcanism. The presence or absence of tridymite will depend on lava crystallization temperatures (NM) and post crystallization alteration temperatures (Iwodake).

In-plane x-ray diffraction for characterization of monolayer and few-layer transition metal dichalcogenide films

NASA Astrophysics Data System (ADS)

Chubarov, Mikhail; Choudhury, Tanushree H.; Zhang, Xiaotian; Redwing, Joan M.

2018-02-01

There is significant interest in the growth of single crystal monolayer and few-layer films of transition metal dichalcogenides (TMD) and other 2D materials for scientific exploration and potential applications in optics, electronics, sensing, catalysis and others. The characterization of these materials is crucial in determining the properties and hence the applications. The ultra-thin nature of 2D layers presents a challenge to the use of x-ray diffraction (XRD) analysis with conventional Bragg-Brentano geometry in analyzing the crystallinity and epitaxial orientation of 2D films. To circumvent this problem, we demonstrate the use of in-plane XRD employing lab scale equipment which uses a standard Cu x-ray tube for the analysis of the crystallinity of TMD monolayer and few-layer films. The applicability of this technique is demonstrated in several examples for WSe2 and WS2 films grown by chemical vapor deposition on single crystal substrates. In-plane XRD was used to determine the epitaxial relation of WSe2 grown on c-plane sapphire and on SiC with an epitaxial graphene interlayer. The evolution of the crystal structure orientation of WS2 films on sapphire as a function of growth temperature was also examined. Finally, the epitaxial relation of a WS2/WSe2 vertical heterostructure deposited on sapphire substrate was determined. We observed that WSe2 grows epitaxially on both substrates employed in this work under all conditions studied while WS2 exhibits various preferred orientations on sapphire substrate which are temperature dependent. In contrast to the sapphire substrate, WS2 deposited on WSe2 exhibits only one preferred orientation which may provide a route to better control the orientation and crystal quality of WS2. In the case of epitaxial graphene on SiC, no graphene-related peaks were observed in in-plane XRD while its presence was confirmed using Raman spectroscopy. This demonstrates the limitation of the in-plane XRD technique for characterizing low electron density materials.

Tunable-color luminescence via energy transfer in NaCa13/18Mg5/18PO4:A (A = Eu2+/Tb3+/Mn2+, Dy3+) phosphors for solid state lighting.

PubMed

Li, Kai; Fan, Jian; Mi, Xiaoyun; Zhang, Yang; Lian, Hongzhou; Shang, Mengmeng; Lin, Jun

2014-11-17

A series of NaCa13/18Mg5/18PO4(NCMPO):A (A = Eu(2+)/Tb(3+)/Mn(2+), Dy(3+)) phosphors have been prepared by the high-temperature solid-state reaction method. The X-ray diffraction (XRD) and Rietveld refinement, X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), cathodoluminescence (CL), decay lifetimes, and PL quantum yields (QYs) were utilized to characterize the phosphors. The pure crystalline phase of as-prepared samples has been demonstrated via XRD measurement and Rietveld refinements. XPS reveals that the Eu(2+)/Tb(3+)/Mn(2+) can be efficiently doped into the crystal lattice. NCMPO:Eu(2+)/Tb(3+)/Mn(2+) phosphors can be effectively excited under UV radiation, which show tunable color from purple-blue to red including white emission based on energy transfer from Eu(2+) to Tb(3+)/Mn(2+) ions. Under low-voltage electron beam bombardment, the NCMPO:A (A = Eu(2+)/Tb(3+)/Mn(2+), Dy(3+)) display their, respectively, characteristic emissions with different colors, and the CL spectrum of NCMPO:0.04Tb(3+) has the comparable intensity to the ZnO:Zn commercial product. In addition, the calculated CIE coordinate of NCMPO:0.04Tb(3+) (0.252, 0.432) is more saturated than it (0.195, 0.417). These results reveal that NCMPO:A (A = Eu(2+)/Tb(3+)/Mn(2+), Dy(3+)) may be potential candidate phosphors for WLEDs and FEDs.

Obtaining titanium dioxide nanoparticles with spherical shape and antimicrobial properties using M. citrifolia leaves extract by hydrothermal method.

PubMed

M, Sundrarajan; K, Bama; M, Bhavani; S, Jegatheeswaran; S, Ambika; A, Sangili; P, Nithya; R, Sumathi

2017-06-01

In this work, we synthesized titanium dioxide (TiO 2 ) nanoparticles using leaf extract of Morinda citrifolia (M. citrifolia) by the advanced hydrothermal method. The synthesized TiO 2 nanoparticles were characterized by X-ray diffraction (XRD), Fourier transmission infrared (FT-IR), Ultraviolet-visible diffuse reflectance (UV-Vis DRS), Ultraviolet-visible spectroscopy (UV-Vis), Raman spectroscopy, and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM with EDX) techniques. The XRD major peak at 27.3° corresponds to the (110) lattice plane of tetragonal rutile TiO 2 phase and average crystalline size of nanoparticles is 10nm. The FT-IR result confirmed that TiO 2 nanoparticles and the presences of very few amount of anthraquinone and phenolic compounds of the leaf extract. The obtained nanoparticles were also characterized by UV-Vis DRS absorption spectroscopy and an intense band at 423nm clearly reveals the formation of nanoparticles. SEM images with EDX spectra clearly reveal the size of the nanoparticles, between 15 and 19nm in excellent quasi-spherical shape, by virtue of stabilization (capping) agent. The presence of elements-titanium and oxygen was verified with EDX spectrum. Furthermore, the inhibitory activity of green synthesized TiO 2 nanoparticles was tested against human pathogens like Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, Candida albicans, and Aspergillus niger by the agar well-diffusion method. The TiO 2 nanoparticles exhibited superior antimicrobial activity against Gram-positive bacteria, demonstrating their antimicrobial value against pathogenic diseases. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of silver nanoparticles from stem bark of Cochlospermum religiosum (L.) Alston: an important medicinal plant and evaluation of their antimicrobial efficacy

NASA Astrophysics Data System (ADS)

Sasikala, A.; Linga Rao, M.; Savithramma, N.; Prasad, T. N. V. K. V.

2015-10-01

The use of different parts of plants for the synthesis of nanoparticles is considered as a green technology as it does not involve any harmful chemicals. Herein, we report on rapid biosynthesis of silver nanoparticles (SNPs) from aqueous stem bark extract of Cochlospermum religiosum a medicinal plant. The reduced silver nanoparticles were characterized by using UV-Visible spectroscopy (UV-Vis), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis, atomic force microscopy, and Fourier transform infrared (FT-IR). The UV-Visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 445 nm, XRD showed that the particles are crystalline in nature, with a face-centered cubic structure and the SEM images showed that the spherical-shaped silver nanoparticles were observed and the size range was found to be 20-35 nm. FT-IR spectroscopy analysis revealed that carbohydrate, polyphenols, and protein molecules were involved in the synthesis and capping of silver nanoparticles. These phytosynthesized SNPs were tested for their antimicrobial activity and it analyzed by measuring the inhibitory zone. Cochlospermum religiosum aqueous stem bark extract of SNPs showed highest toxicity to Staphylococcus followed by Pseudomonas, Escherichia coli and Bacillus and lowest toxicity towards Proteus. Whereas in fungal species highest inhibition zone against Aspergillus flavus followed by Rhizopus, Fusarium, and Curvularia, and minimum inhibition zone was observed against Aspergillus niger species. The outcome of this study could be useful for the development of value added products from indigenous medicinal plants of India for nanotechnology-based biomedical applications.

Effect of concentration and irradiation on the optical and structural properties of ZnO thin films deposited by spray pyrolysis techniques

NASA Astrophysics Data System (ADS)

Adeoye Victor, Babalola

2017-12-01

This study involves the preparation of ZnO thin films by spray pyrolysis and to investigate the effect of concentration of the film and irradiation on ZnO thin film deposited by spray pyrolysis method deposited at 350 ± 5 °C. The precursor for zinc oxide was produced from zinc acetate (Zn(CH3COO))2. The samples were annealed at 500 °C for 6 h and irradiated using 137Cs 90.998 mCi radiation. They were then characterised using ultra violet-visible spectrophotometry, X-ray Diffractometry (XRD) with Cu-Kα radiation to determine the structure of the film, Four-point probe for electrical properties and Rutherford Backscattering Spectrometry (RBS) were used for the composition of the film. XRD diffraction peaks observed for 0.05 M ZnO were (1 0 0), (0 0 2), (1 0 1) and (1 1 0) planes for the annealed and irradiated annealed ZnO films with no preferential orientation. The as-deposited films have low peaks belonging to (1 0 0), (0 0 2), (1 0 1), (1 1 0) plane and other peaks such as (1 1 2), (2 0 0) and (2 0 1). The results are explained with regard to the irradiation damage introduced to the samples. The as-deposited, annealed and irradiated-annealed films are highly transparent in the visible range of the electromagnetic spectrum with an average percent transmittance values of 85% and present a sharp ultraviolet cut-off at approximately 380 nm for the ZnO thin film.

Synthesis, characterization, and controlled release anticorrosion behavior of benzoate intercalated Zn-Al layered double hydroxides

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

Wang, Yi; Zhang, Dun, E-mail: zhangdun@qdio.ac.cn

2011-11-15

Graphical abstract: The benzoate anion released from Zn-Al LDHs provides a more effective long-term protection against corrosion of Q235 carbon steel in 3.5% NaCl solution. Highlights: {yields} A benzoate anion corrosion inhibitor intercalated Zn-Al layered double hydroxides (LDHs) has been assembled by coprecipitation method. {yields} The kinetic simulation indicates that the ion-exchange one is responsible for the release process and the diffusion through particle is the rate limiting step. {yields} A significant reduction of the corrosion rate is observed when the LDH nanohybrid is present in the corrosive media. -- Abstract: Corrosion inhibitor-inorganic clay composite including benzoate anion intercalated Zn-Almore » layered double hydroxides (LDHs) are assembled by coprecipitation. Powder X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectrum analyses indicate that the benzoate anion is successfully intercalated into the LDH interlayer and the benzene planes are vertically bilayer-positioned as a quasi-guest ion-pair form in the gallery space. Kinetic simulation for the release data, XRD and FT-IR analyses of samples recovered from the release medium indicate that ion-exchange is responsible for the release process and diffusion through the particle is also indicated to be the rate-limiting step. The anticorrosion capabilities of LDHs loaded with corrosion inhibitor toward Q235 carbon steel are analyzed by polarization curve and electrochemical impedance spectroscopy methods. Significant reduction of corrosion rate is observed when the LDH nanohybrid is present in the corrosive medium. This hybrid material may potentially be applied as a nanocontainer in self-healing coatings.« less

Enzyme-mediated formulation of stable elliptical silver nanoparticles tested against clinical pathogens and MDR bacteria and development of antimicrobial surgical thread.

PubMed

Thapa, Rupak; Bhagat, Chintan; Shrestha, Pragya; Awal, Suvash; Dudhagara, Pravin

2017-05-16

Silver nanoparticles (AgNPs) are believed to be emerging tool against various infectious diseases including multi-drug resistant (MDR) bacteria. In the present study, in vitro synthesis of AgNPs was optimized using 1:50 ratio of macerozyme (25 μg/μl) and 1 mM AgNO 3 incubated at 80 °C for 8 h. AgNPs were characterized by UV-Visible spectroscopy, dynamic light scattering (DLS), scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy (TEM) and X-ray diffraction (XRD). Characterization studies suggest the synthesis of elliptical, stable and crystalline AgNPs with an average size of 38.26 ± 0.4 nm calculated using TEM. The XRD pattern revealed the face-centered-cubic (fcc) form of metallic silver. Good shape integrity and dispersion of AgNPs after 1 year of incubation confirmed their stability. AgNPs were exibited the antimicrobial property against ten pathogenic bacteria, three molds and one yeast. The AgNPs also revealed remarkable antimicrobial activity against three MDR strains i.e. Extended spectrum beta-lactamase positive Escherichia coli, Staphylococcus aureus (MRSA) and Teicoplanin resistant Streptococcus Pneumoniae. The AgNPs coated surgical threads (suture) were revealed the remarkble antibacterial activity against three MDR strains. This is the first report to synthesize antimicrobial elliptical AgNPs using enzymes. The results suggest the possibilities to develop the nanoparticles coated antimicrobial medical fabric to combat against MDR infection.

Structural and spectroscopic study of mechanically synthesized SnO{sub 2} nanostructures

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

Vij, Ankush, E-mail: vij-anx@yahoo.com; Kumar, Ravi; Presently at Beant College of Engineering and Technology, Gurdaspur-143521

2016-05-23

We report the single step synthesis of SnO{sub 2} nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO{sub 2} nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A{sub 1g} Raman mode towards lower wave number, which is correlated with the nanostructure formation.