A novel orange-red emitting NaCaVO{sub 4}:Sm{sup 3+} phosphor for solid state lighting

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

Biswas, Pankaj, E-mail: pankaj79biswas@gmail.com; Kumar, Vinay, E-mail: vinaykdhiman@yahoo.com; Ntwaeaborwa, O. M.

2016-05-06

The samarium doped NaCaVO{sub 4} phosphor was synthesized by the combustion method. The X-ray powder diffraction (XRD) analysis confirmed that the phosphor powder crystallized as orthorhombic structure belonging to space group Cmcm. From Williamson-Hall analysis the grain size and microstrain in the powder was estimated. The Fourier- transform infrared (FT-IR) studies further validated the formation of vanadate phase of the phosphor. Photoluminescence (PL) study revealed that the phosphor could be efficiently excited by UV-VIS from 200 nm to 500 nm. The 565 nm, 602 nm, 648 nm and 713 nm emissions were ascribed to {sup 4}G{sub 5/2} to {sup 6}H{submore » J} (J = 5/2, 7/2, 9/2 and 11/2) transitions of the Sm{sup 3+} ion. The present material may be explored as a novel phosphor to be excited by UV light emitting diodes (LEDs) chips for solid-state lighting and display applications.« less

Room temperature luminescence and ferromagnetism of AlN:Fe

NASA Astrophysics Data System (ADS)

Li, H.; Cai, G. M.; Wang, W. J.

2016-06-01

AlN:Fe polycrystalline powders were synthesized by a modified solid state reaction (MSSR) method. Powder X-ray diffraction and transmission electron microscopy results reveal the single phase nature of the doped samples. In the doped AlN samples, Fe is in Fe2+ state. Room temperature ferromagnetic behavior is observed in AlN:Fe samples. Two photoluminescence peaks located at about 592 nm (2.09 eV) and 598 nm (2.07 eV) are observed in AlN:Fe samples. Our results suggest that AlN:Fe is a potential material for applications in spintronics and high power laser devices.

Structural Transitions in Nanosized Zn0.97Al0.03O Powders under High Pressure Analyzed by in Situ Angle-Dispersive X-ray Diffraction

PubMed Central

Lin, Chih-Ming; Liu, Hsin-Tzu; Zhong, Shi-Yao; Hsu, Chia-Hung; Chiu, Yi-Te; Tai, Ming-Fong; Juang, Jenh-Yih; Chuang, Yu-Chun; Liao, Yen-Fa

2016-01-01

Nanosized aluminum-doped zinc oxide Zn1−xAlxO (AZO) powders (AZO-NPs) with x = 0.01, 0.03, 0.06, 0.09 and 0.11 were synthesized by chemical precipitation method. The thermogravimetric analysis (TGA) indicated that the precursors were converted to oxides from hydroxides near 250 °C, which were then heated to 500 °C for subsequent thermal processes to obtain preliminary powders. The obtained preliminary powders were then calcined at 500 °C for three hours. The structure and morphology of the products were measured and characterized by angle-dispersive X-ray diffraction (ADXRD) and scanning electron microscopy (SEM). ADXRD results showed that AZO-NPs with Al content less than 11% exhibited würtzite zinc oxide structure and there was no other impurity phase in the AZO-NPs, suggesting substitutional doping of Al on Zn sites. The Zn0.97Al0.03O powders (A3ZO-NPs) with grain size of about 21.4 nm were used for high-pressure measurements. The in situ ADXRD measurements revealed that, for loading run, the pressure-induced würtzite (B4)-to-rocksalt (B1) structural phase transition began at 9.0(1) GPa. Compared to the predicted phase-transition pressure of ~12.7 GPa for pristine ZnO nanocrystals of similar grain size (~21.4 nm), the transition pressure for the present A3ZO-NPs exhibited a reduction of ~3.7 GPa. The significant reduction in phase-transition pressure is attributed to the effects of highly selective site occupation, namely Zn2+ and Al3+, were mainly found in tetrahedral and octahedral sites, respectively. PMID:28773683

Growth and characterization of 4-chloro-3-nitrobenzophenone single crystals using vertical Bridgman technique

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

Aravinth, K., E-mail: anandcgc@gmail.com; Babu, G. Anandha, E-mail: anandcgc@gmail.com; Ramasamy, P., E-mail: anandcgc@gmail.com

2014-04-24

4-chloro-3-nitrobenzophenone (4C3N) has been grown by using vertical Bridgman technique. The grown crystal was confirmed by Powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was examined by high-resolution X-ray diffraction study. The fluorescence spectra of grown 4C3N single crystals exhibit emission peak at 575 nm. The micro hardness measurements were used to analyze the mechanical property of the grown crystal.

Luminescent silver(I) tert-butylethynide compounds with nicotinic/isonicotinic acid as ligands

NASA Astrophysics Data System (ADS)

Xie, Yi-Ming; Fan, Yue-Yue; Lin, Fu-Lin; Hu, Ting; Liu, Jia; Lu, Can-Zhong

2017-12-01

Solvothermal reaction of tBuC≡CAg, AgBF4 and nicotinic/isonicotinic acid in acetonitrile afforded two new silver(I) tert-butylethynide double salts, namely [(tBuC≡CAg)(AgL1)3] (HL1 = nicotinic acid) (1) and [(tBuC≡CAg)(AgL1)2] (HL2 = isonicotinic acid) (2). These compounds have been characterized by elemental analysis, infrared spectra, single-crystal X-ray analysis, X-ray powder diffraction, thermogravimetric analysis, UV-visible absorption spectra, and luminescent measurement. 1 exhibits a two-dimensional coordination network, and 2 features a three-dimensional coordination architecture. Luminescence measurements indicate that 1 shows a fluorescent emission band centered at 568 nm, and 2 exhibits an intense emission maximum at 550 nm and a shoulder peak at 436 nm.

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.

Complex doping chemistry owing to Mn incorporation in nanocrystalline anatase TiO2 powders.

PubMed

Guo, Meilan; Gao, Yun; Shao, G

2016-01-28

Mn-doped TiO2 powders with a wide range of nominal doping levels were fabricated using a one-step hydrothermal method followed by 400 °C annealing. Anatase powders with a uniform size distribution below 10 nm were obtained. The maximum solubility of Mn in the TiO2 lattice was around 30%, beyond which the Mn3O4 compound appeared as a secondary phase. The optical absorption edges for Mn-doped anatase TiO2 were red-shifted effectively through increasing Mn content. Alloying chemistry and associated elemental valences were elaborated through combining X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and theoretical simulation in the framework of density functional theory (DFT). The results showed that the Mn species exhibited mixed valence states of 3+ and 4+ in anatase TiO2, with the latter being the key to remarkable photocatalytic performance.

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

NASA Astrophysics Data System (ADS)

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

2013-09-01

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

Preparation and X-Ray diffraction studies of curium hydrides

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

Gibson, J.K.; Maire, R.G.

Curium hydrides were prepared by reaction of curium-248 metal with hydrogen and characterized by X-ray powder diffraction. Several of the syntheses resulted in a hexagonal compound with average lattice parameters of a/sub 0/ = 0.3769(8) nm and c/sub 0/ = 0.6732(12) nm. These products are considere to be CmH/sub 3//sup -//sub 8/ by analogy with the behavior of lanthanide-hydrogen and lighter actinide-hydrogen systems. Face-centered cubic products with an average lattice parameter of a/sub 0/ = 0.5322(4) nm were obtained from other curium hydride preparations. This parameter is slightly smaller than that reported previously for cubic curium dihydride, CmH /SUB 2-x/more » (B.M. Bansal and D. Damien. Inorg. Nucl. Chem. Lett. 6 603, 1970). The present results established a continuation of typical heavy trivalent lanthanidelike behavior of the transuranium actinide-hydrogen systems through curium.« less

Preparation and X-ray diffraction studies of curium hydrides

NASA Astrophysics Data System (ADS)

Gibson, J. K.; Haire, R. G.

1985-10-01

Curium hydrides were prepared by reaction of curium-248 metal with hydrogen and characterized by X-ray powder diffraction. Several of the syntheses resulted in a hexagonal compound with average lattice parameters of a0 = 0.3769(8) nm and c0 = 0.6732(12) nm. These products are considered to be CmH 3-δ by analogy with the behavior of lanthanide-hydrogen and lighter actinide-hydrogen systems. Face-centered cubic products with an average lattice parameter of a0 = 0.5322(4) nm were obtained from other curium hydride preparations. This parameter is slightly smaller than that reported previously for cubic curium dihydride, CmH 2+ x (B. M. Bansal and D. Damien, Inorg. Nucl. Chem. Lett., 6, 603, 1970). The present results established a continuation of typical heavy trivalent lanthanide-like behavior of the transuranium actinide-hydrogen systems through curium.

One-Step Hydrothermal-Electrochemical Route to Carbon-Stabilized Anatase Powders

NASA Astrophysics Data System (ADS)

Tao, Ying; Yi, Danqing; Zhu, Baojun

2013-04-01

Black carbon-stabilized anatase particles were prepared by a simple one-step hydrothermal-electrochemical method using glucose and titanium citrate as the carbon and titanium source, respectively. Morphological, chemical, structural, and electrochemical characterizations of these powders were carried out by Raman spectroscopy, Fourier-transform infrared spectroscopy, x-ray diffraction, scanning electron microscopy, and cyclic voltammetry. It was revealed that 200-nm carbon/anatase TiO2 was homogeneously dispersed, and the powders exhibited excellent cyclic performance at high current rates of 0.05 V/s. The powders are interesting potential materials that could be used as anodes for lithium-ion batteries.

Structure, morphology and optical properties of undoped and MN-doped ZnO(1-x)Sx nano-powders prepared by precipitation method

NASA Astrophysics Data System (ADS)

Dejene, F. B.; Onani, M. O.; Koao, L. F.; Wako, A. H.; Motloung, S. V.; Yihunie, M. T.

2016-01-01

The undoped and Mn-doped ZnO(1-x)Sx nano-powders were successfully synthesized by precipitation method without using any capping agent. Its structure, morphology, elemental analysis, optical and luminescence properties were determined by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), UV-vis spectroscopy (UV) and photoluminescence spectroscopy (PL). A typical SEM image of the un-doped ZnO(1-x)Sx nanoparticles exhibit flake like structures that changes to nearly spherical particles with Mn-doping. The XRD of undoped and Mn doped ZnO(1-x)Sx pattern reveals the formation of a product indexed to the hexagonal wurtzite phase of ZnS. The nanopowders have crystallite sizes estimated from XRD measurements were in the range of 10-20 nm. All the samples showed absorption maximum of ZnO(1-x)Sx at 271 nm and high transmittance in UV and visible region, respectively. The undoped ZnO(1-x)Sx nanoparticles show strong room-temperature photoluminescence with four emission bands centering at 338 nm, 384 nm, 448 nm and 705 nm that may originate to the impurity of ZnO(1-x)Sx, existence of oxide related defects. The calculated bandgap of the nanocrystalline ZnO(1-x)Sx showed a blue-shift with respect to the Mn-doping. The PL spectra of the Mn-doped samples exhibit a strong orange emission at around 594 nm attributed to the 4T1-6A1 transition of the Mn2+ ions.

Boron-doped diamond synthesized at high-pressure and high-temperature with metal catalyst

NASA Astrophysics Data System (ADS)

Shakhov, Fedor M.; Abyzov, Andrey M.; Kidalov, Sergey V.; Krasilin, Andrei A.; Lähderanta, Erkki; Lebedev, Vasiliy T.; Shamshur, Dmitriy V.; Takai, Kazuyuki

2017-04-01

The boron-doped diamond (BDD) powder consisting of 40-100 μm particles was synthesized at 5 GPa and 1500-1600 °C from a mixture of 50 wt% graphite and 50 wt% Ni-Mn catalyst with an addition of 1 wt% or 5 wt% boron powder. The size of crystal domains of doped and non-doped diamond was evaluated as a coherent scattering region by X-ray diffraction (XRD) and using small-angle neutron scattering (SANS), being ≥180 nm (XRD) and 100 nm (SANS). Magnetic impurities of NiMnx originating from the catalyst in the synthesis, which prevent superconductivity, were detected by magnetization measurements at 2-300 K. X-ray photoelectron spectroscopy, the temperature dependence of the resistivity, XRD, and Raman spectroscopy reveal that the concentration of electrically active boron is as high as (2±1)×1020 cm-3 (0.1 at%). To the best of our knowledge, this is the highest boron content for BDD synthesized in high-pressure high-temperature process with metal catalysts.

CoO doping effects on the ZnO films through EBPDV technique

NASA Astrophysics Data System (ADS)

Inês Basso Bernardi, Maria; Queiroz Maia, Lauro June; Antonelli, Eduardo; Mesquita, Alexandre; Li, Maximo Siu; Gama, Lucianna

2014-03-01

Nanometric Zn1-xCo xO (x = 0.020, 0.025 and 0.030 in mol.%) nanopowders were obtained from low temperature calcination of a resin prepared using the Pechini's method. Firing the Zn1-xCoxO resin at 400 °C/2 h a powder with hexagonal structure was obtained as measured by X-ray diffraction (XRD). The powder presented average particle size of 40 nm observed by field emission scanning electronic microscopy (FE-SEM) micrographs and average crystallite size of 10 nm calculated from the XRD using Scherrer's equation. Nanocrystalline Zn1-xCo xO films with good homogeneity and optical quality were obtained with 280-980 nm thicknesses by electron beam physical vapour deposition (EBPVD) under vacuum onto silica substrate at 25 °C. Scanning electron microscopy with field emission gun showed that the film microstructure is composed by spherical grains and some needles. In these conditions of deposition the films presented only hexagonal phase observed by XRD. The UV-visible-NIR and diffuse reflectance properties of the films were measured and the electric properties were calculated using the reflectance and transmittance spectra.

Coriandrum sativum mediated synthesis of silver nanoparticles and evaluation of their biological characteristics

NASA Astrophysics Data System (ADS)

Senthilkumar, N.; Aravindhan, V.; Ruckmani, K.; Vetha Potheher, I.

2018-05-01

Silver (Ag) nanoparticles (NPs) were prepared by percolated green synthesis method using Coriandrum sativum leaf, root, seed and stem extracts and reported its antibacterial activity. The synthesized Ag NPs were confirmed by UV–visible Spectroscopy, Powder x-ray Diffraction (PXRD), Fourier Transform Infra Red (FT-IR) Spectroscopy analyzes. The Maximum absorbance observed around 400–450 nm reveal the characteristic absorbance of Ag NPs. The Dynamic Light Scattering (DLS) analysis shows the stability of synthesized NPs with average size varying from 35 to 53 nm and also zeta potential stability varying from ‑20 to ‑30 mV. The cubic structure, crystalline nature and purity of the material was confirmed by powder x-ray diffraction studies. FT-IR spectrum shows the presence of various functional groups in the resultant material. The Field Emission Scanning Electron Microscopy (FESEM) image shows the surface morphology of the synthesized NPs and the Energy Dispersive x-ray Analysis (EDAX) confirms the presence of silver metal ions. The Coriandrum sativum aqueous extract exhibited excellent antimicrobial activity against Klebsiella pneumoniae (Gram -ve) bacteria. Numerous studies have been made previously in our field of study but optimization has not been carried out by both extract (different parts like leaf, root, seed and stem) and without addition of any external source such as chemicals, heat etc.

On the response of Y 3Al 5O 12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

NASA Astrophysics Data System (ADS)

Kandarakis, I.; Cavouras, D.; Sianoudis, I.; Nikolopoulos, D.; Episkopakis, A.; Linardatos, D.; Margetis, D.; Nirgianaki, E.; Roussou, M.; Melissaropoulos, P.; Kalivas, N.; Kalatzis, I.; Kourkoutas, K.; Dimitropoulos, N.; Louizi, A.; Nomicos, C.; Panayiotakis, G.

2005-02-01

The aim of this study was to examine Y 3Al 5O 12:Ce (also known as YAG:Ce) powder scintillator under X-ray imaging conditions. This material shows a very fast scintillation decay time and it has never been used in X-ray medical imaging. In the present study various scintillator layers (screens) with coating thickness ranging from 13 to 166 mg/cm 2 were prepared in our laboratory by sedimentation of Y 3Al 5O 12: Ce powder. Optical emission spectra and light emission efficiency (spectrum area over X-ray exposure) of the layers were measured under X-ray excitation using X-ray tube voltages (80-120 kVp) often employed in general medical radiography and fluoroscopy. Spectral compatibility with various optical photon detectors (photodiodes, photocathodes, charge coupled devices, films) and intrinsic conversion efficiency values were determined using emission spectrum data. In addition, parameters related to X-ray detection, energy absorption efficiency and K-fluorescence characteristic emission were calculated. A theoretical model describing radiation and light transfer through scattering media was used to fit experimental data. Intrinsic conversion efficiency (η≈0.03-0.05) and light attenuation coefficients (σ≈26.5 cm/g) were derived through this fitting. Y 3Al 5O 12:Ce showed peak emission in the wavelength range 530-550 nm. The light emission efficiency was found to be maximum for the 107 mg/cm 2 layer. Due to its "green" emission spectrum, Y 3Al 5O 12:Ce showed excellent compatibility (of the order of 0.9) with the sensitivity of many currently used photodetectors. Taking into account its very fast response Y 3Al 5O 12:Ce could be considered for application in X-ray imaging especially in various digital detectors.

In-situ observation of stacking fault evolution in vacuum-deposited C60

NASA Astrophysics Data System (ADS)

Hardigree, J. F. M.; Ramirez, I. R.; Mazzotta, G.; Nicklin, C.; Riede, M.

2017-12-01

We report an in-situ study of stacking fault evolution in C60 thin films using grazing-incidence x-ray scattering. A Williamson-Hall analysis of the main scattering features during growth of a 15 nm film on glass indicates lattice strain as high as 6% in the first 5 nm of the film, with a decrease to 2% beyond 8 nm thickness. Deformation stacking faults along the {220} plane are found to occur with 68% probability and closely linked to the formation of a nanocrystalline powder-like film. Our findings, which capture monolayer-resolution growth, are consistent with previous work on crystalline and powder C60 films, and provide a crystallographic context for the real-time study of organic semiconductor thin films.

Room temperature luminescence and ferromagnetism of AlN:Fe

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

Li, H., E-mail: lihui@mail.iee.ac.cn, E-mail: wjwang@aphy.iphy.ac.cn; Cai, G. M.; Wang, W. J., E-mail: lihui@mail.iee.ac.cn, E-mail: wjwang@aphy.iphy.ac.cn

2016-06-15

AlN:Fe polycrystalline powders were synthesized by a modified solid state reaction (MSSR) method. Powder X-ray diffraction and transmission electron microscopy results reveal the single phase nature of the doped samples. In the doped AlN samples, Fe is in Fe{sup 2+} state. Room temperature ferromagnetic behavior is observed in AlN:Fe samples. Two photoluminescence peaks located at about 592 nm (2.09 eV) and 598 nm (2.07 eV) are observed in AlN:Fe samples. Our results suggest that AlN:Fe is a potential material for applications in spintronics and high power laser devices.

Formation and mechanism of nanocrystalline AZ91 powders during HDDR processing

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

Liu, Yafen; Fan, Jianfeng, E-mail: fanjianfeng@tyu

2017-03-15

Grain sizes of AZ91 alloy powders were markedly refined to about 15 nm from 100 to 160 μm by an optimized hydrogenation-disproportionation-desorption-recombination (HDDR) process. The effect of temperature, hydrogen pressure and processing time on phase and microstructure evolution of AZ91 alloy powders during HDDR process was investigated systematically by X-ray diffraction, optical microscopy, scanning electron microscopy and transmission electron microscopy, respectively. The optimal HDDR process for preparing nanocrystalline Mg alloy powders is hydriding at temperature of 350 °C under 4 MPa hydrogen pressure for 12 h and dehydriding at 350 °C for 3 h in vacuum. A modified unreacted coremore » model was introduced to describe the mechanism of grain refinement of during HDDR process. - Highlights: • Grain size of the AZ91 alloy powders was significantly refined from 100 μm to 15 nm. • The optimal HDDR technology for nano Mg alloy powders is obtained. • A modified unreacted core model of grain refinement mechanism was proposed.« less

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.

Perylene and Perylene-Derivative Nano-Cocrystals: Preparation and Physicochemical Property

NASA Astrophysics Data System (ADS)

Baba, Koichi; Konta, Sayaka; Oliveira, Daniel; Sugai, Kenji; Onodera, Tsunenobu; Masuhara, Akito; Kasai, Hitoshi; Oikawa, Hidetoshi; Nakanishi, Hachiro

2012-12-01

Organic nano-cocrystals of functional dyes of perylene and a perylene derivative were successfully prepared by the reprecipitation method. The particle sizes, optical properties, and powder X-ray diffraction patterns of nano-cocrystals were evaluated. Typically, the size with size distribution of nano-cocrystals was 55±15 nm when the molar ratio of perylene to the perylene derivative was 50:50. The particular intermolecular electronic interaction between perylene and the perylene derivative in the nano-cocrystal state was observed by absorption and fluorescence spectra measurements. The powder X-ray diffraction pattern analysis confirmed that the structure of nano-cocrystals was different from those prepared from perylene and the perylene derivative. The nano-cocrystal having unique physicochemical properties will be potentially classified as a new type of functional nanomaterial.

Controlling the sol–gel process of nano-crystalline lithium-mica glass-ceramic by its chemical composition and synthesis parameters

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

Tohidifar, M.R., E-mail: tohidifar@znu.ac.ir; Alizadeh, P.; Aghaei, A.R.

2015-01-15

This paper aims to explore the impact of the parameters such as pH of the system, refluxing temperature, water quantity and chemical composition on the sol–gel synthesis of lithium-mica glass-ceramic nano-powder. The synthesis process was accomplished using two chemical composition formula (Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} and LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2}). X-ray diffraction, Brunauer–Emmett–Teller surface area measurement and scanning electron microscopy techniques were applied to evaluate a variety of as-synthesized samples. Consequently, a transparent homogeneous sol was obtained under the conditions as pH ≤ 4, synthesis temperature ≤ 50 °C, and mol ratio of water to chemicals ≤more » 2. The prepared nano-powders under such conditions were in the range of 60–100 nm. The results also revealed that the mica glass-ceramics prepared based on the composition Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} possessed finer powders due to their slow hydrolysis process. Moreover, any reduction in the stoichiometric deviation of lithium mica (x) leads to acquiring finer powders. - Highlights: • A transparent homogeneous sol leads to prepare nanopowders in the range of 60–100 nm. • The particles synthesized at lower temperatures possess finer sizes. • The acquired product which is prepared with excessive water offers larger sizes. • Any reduction in stoichiometric deviation leads to acquiring finer powders. • Taking synthesis composition as Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} offers finer powders.« less

A simple method to synthesize polyhedral hexagonal boron nitride nanofibers

NASA Astrophysics Data System (ADS)

Lin, Liang-xu; Zheng, Ying; Li, Zhao-hui; shen, Xiao-nv; Wei, Ke-mei

2007-12-01

Hexagonal boron nitride (h-BN) fibers with polyhedral morphology were synthesized with a simple-operational, large-scale and low-cost method. The sample obtained was studied by X-ray photoelectron spectrometer (XPS), electron energy lose spectroscopy (EELS), X-ray powder diffraction (XRD), Fourier transformation infrared spectroscopy (FT-IR), etc., which matched with h-BN. Environment scanning electron microscopy (ESEM) and transmission electron microscope (TEM) indicated that the BN fibers possess polyhedral morphology. The diameter of the BN fibers is mainly in the range of 100-500 nm.

Structural and spectral properties of MgZnO2:Sm3+ phosphor

NASA Astrophysics Data System (ADS)

Rajput, Preasha; Sharma, Pallavi; Biswas, Pankaj; Kamni

2018-05-01

The samarium doped MgZnO2 phosphor was synthesized by the low-cost combustion method. The powder X-ray diffraction (XRD) analysis confirmed the crystallinity and phase purity of the phosphor. The lattice parameters were determined by indexing the diffraction peaks. The photoluminescence (PL) study revealed that the phosphor exhibited a broad excitation band in the UV region ranging between 200 to 350 nm. The 601 nm emission was ascribed to 4G5/2 to 6H7/2 transitions of the Sm3+ ion. The optical bandgap of MgZnO2:Sm3+ was obtained to be 3.56 eV. The phosphor can be projected as a useful material in X- and gamma-ray scintillators.

X-ray peak broadening analysis of AA 6061{sub 100-x} - x wt.% Al{sub 2}O{sub 3} nanocomposite prepared by mechanical alloying

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

Sivasankaran, S., E-mail: sivasankarangs1979@gmail.com; Sivaprasad, K., E-mail: ksp@nitt.edu; Narayanasamy, R., E-mail: narayan@nitt.edu

2011-07-15

Nanocrystalline AA 6061 alloy reinforced with alumina (0, 4, 8, and 12 wt.%) in amorphized state composite powder was synthesized by mechanical alloying and consolidated by conventional powder metallurgy route. The as-milled and as-sintered (573 K and 673 K) nanocomposites were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The peaks corresponding to fine alumina was not observed by XRD patterns due to amorphization. Using high-resolution transmission electron microscope, it is confirmed that the presence of amorphized alumina observed in Al lattice fringes. The crystallite size, lattice strain, deformation stress, and strain energy density of AA 6061 matrixmore » were determined precisely from the first five most intensive reflection of XRD using simple Williamson-Hall models; uniform deformation model, uniform stress deformation model, and uniform energy density deformation model. Among the developed models, uniform energy density deformation model was observed to be the best fit and realistic model for mechanically alloyed powders. This model evidenced the more anisotropic nature of the ball milled powders. The XRD peaks of as-milled powder samples demonstrated a considerable broadening with percentage of reinforcement due to grain refinement and lattice distortions during same milling time (40 h). The as-sintered (673 K) unreinforced AA 6061 matrix crystallite size from well fitted uniform energy density deformation model was 98 nm. The as-milled and as-sintered (673 K) nanocrystallite matrix sizes for 12 wt.% Al{sub 2}O{sub 3} well fitted by uniform energy density deformation model were 38 nm and 77 nm respectively, which indicate that the fine Al{sub 2}O{sub 3} pinned the matrix grain boundary and prevented the grain growth during sintering. Finally, the lattice parameter of Al matrix in as-milled and as-sintered conditions was also investigated in this paper. Research highlights: {yields} Integral breadth methods using various Williamson-Hall models were investigated for line profile analysis. {yields} Uniform energy density deformation model is observed to the best realistic model. {yields} The present analysis is used for understanding the stress and the strain present in the nanocomposites.« less

Compositional dependence of magnetic anisotropy in chemically synthesized Co3- x Fe x O4 (0 ≤ x ≤ 2)

NASA Astrophysics Data System (ADS)

Hayashi, Kensuke; Yamada, Keisuke; Shima, Mutsuhiro

2018-01-01

Magnetic anisotropy of Co3- x Fe x O4 (CFO, 0 ≤ x ≤ 2) thin-film and powder samples prepared by a sol-gel method has been investigated as a function of Fe composition x. Structural analyses by X-ray diffraction show that CFO powder samples exhibit diffraction peaks associated with the spinel structure when x < 2, while CFO thin-film samples with thickness of 130-510 nm yield the peaks when 0 ≤ x ≤ 2. CFO thin-film samples are highly (111)-oriented with the Lotgering factor greater than 0.9 when 0.6 ≤ x ≤ 1.3. The magnetic anisotropy constant K 1 of CFO powder samples estimated from their room-temperature hysteresis loops yields a minimum when x = 0.9. Relatively large in-plane magnetic anisotropy (K eff = 5.7 × 105 erg/cm3) is observed for the CFO thin-film sample when x = 1.3. With increasing x, the magnetic easy axis of the spinel CFO changes from 〈111〉 to 〈100〉 when x = 0.9.

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

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

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

2016-04-19

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

The effect of milling time on the synthesis of Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy

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

Kursun, C., E-mail: celalkursun@ksu.edu.tr; Gogebakan, M., E-mail: gogebakan@ksu.edu.tr

In the present work, nanocrystalline Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy was produced by mechanical alloying from mixtures of pure crystalline Cu, Mg, Ti and Ni powders using a Fritsch planetary ball mill with a ball to powder ratio of 10:1. Morphological changes, microstructural evolution and thermal behaviour of the Cu-Mg-Ti-Ni powders at different stages of milling were characterised by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray detection (SEM/EDX) and differential thermal analysis (DTA). This alloy resulted in formation of single phase solid solution with FCC structure α-Cu (Mg, Ti, Ni) after 80 h of milling. In the initialmore » stage of milling different sized and shaped elemental powders became uniform during mechanical alloying. The homogeneity of the Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy increased with increasing milling time. The EDX result also confirmed the compositional homogeneity of the powder alloy. The crystallite size of alloy was calculated below 10 nm from XRD data.« less

Synthesis and characterization of NiO nanopowder by sol-gel process

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

Ningsih, Sherly Kasuma Warda

2015-09-30

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

Template-free solution approach to synthesize CdS dendrites with SCN based ionic liquid

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

Li, Kangfeng; Li, Jiajia; Cheng, Xianyi

2011-07-15

Highlights: {yields} Template-free solution approach to synthesize CdS hierarchical dendrites. {yields} The 1-butyl-3-methlyimidazole thiocyanate ([BMIM][SCN]) plays doubly functional roles in the progress. {yields} The CdS hierarchical dendrites exhibit a more intense emission at 710 nm belongs to infrared band. -- Abstract: Cadmium sulfide dendrites were synthesized by a facile hydrothermal treatment from CdCl{sub 2} and ionic liquid 1-butyl-3-methlyimidazole thiocyanate acted both as sulfur source and surfactant. The product was characterized by means of X-ray powder diffraction and scanning electron microscopy. X-ray powder diffraction studies indicated that the product was well-crystallized hexagonal phase of CdS, and the scanning electron microscopy imagesmore » showed that the obtained powders consisted of a wealth of well-defined CdS dendritic microstructures with a pronounced trunk and highly ordered branches. The UV-Vis and photoluminescence spectroscopy measurements were taken as well. The possible formation mechanism of CdS dendrites was simply proposed in the end.« less

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

PubMed

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

2018-08-01

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

Thermoelectric properties of CuS/Ag{sub 2}S nanocomposites synthesed by modified polyol method

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

Tarachand,, E-mail: tarachand@csr.res.in; Sharma, Vikash; Ganesan, V.

This is the report on successful synthesis of Ag doped CuS nanostructures by modified polyol method. The resulting samples were characterized by powder X-ray diffraction (XRD), energy dispersive X-ray (EDX), atomic force microscopy (AFM) and dynamic light scattering (DLS). Particle size of pure CuS nanoparticles (NPs) was 17 nm, 38 nm and 97 nm as determined from Scherrer formula, AFM and DLS, respectively. Introduction of Ag led to formation of CuS/Ag{sub 2}S composites. A transition at 55 K in thermopower is ascribed to structural transformation from hexagonal to orthorhombic structure. Further, their thermoelectric properties exhibit remarkable change owing to Agmore » doping in CuS nanostructures. The power factor improves with increasing Ag content. They reveal that CuS/Ag{sub 2}S nanocomposites are some of the potential candidates for generation of thermoelectricity in future.« less

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

Soni, Abhishek Kumar; Rai, Vineet Kumar, E-mail: vineetkrrai@yahoo.co.in

Erbium ion (Er{sup 3+}) doped BaMoO{sub 4} phosphor has been synthesized via co-precipitation technique. Phase formation of the prepared phosphor has been recognized by powder X-ray diffraction analysis. The photoluminescence emission spectrum has been recorded in 400-800nm wavelength range under 380nm excitation. The observed photoluminescence peaks are explained with the help of energy level structure. The prepared phosphor seems capable to produce efficient blue colour emission which can be useful for making blue light emitting diodes (LEDs).

Effect of drying environment on grain size of titanium dioxide nano-powder synthesized via sol-gel method

NASA Astrophysics Data System (ADS)

Zandi, Pegah; Hosseini, Elham; Rashchi, Fereshteh

2018-01-01

Titanium dioxide Nano powder has been synthesized from titanium isopropoxide (TTIP) in chloride media by sol-gel method. In this research, the effect of the drying environment, from air to oven drying at 100 °C, calcination time and temperature on nano TiO2 grain size was investigated. The synthesized powder was analyzed by x-ray diffraction and scanning electron microscope. Based on the results, the powder has been crystallized in anatase and rutile phases, due to different calcination temperatures. At temperatures above 600 °C, the Titanium dioxide nano powder has been crystallized as rutile. The crystalline structure of titanium dioxide nano powder changed because of the different calcination temperatures and time applied. The average particle size of the powder dried in air was larger than the powder dried in oven. The minimum particle size of the powder dried in air was 50 nm and in the oven was 9 nm, observed and calculated Williamson-Hall equation. All in all, with overall increasing of calcination time and temperature the grain size increased. Moreover, in the case of temperature, after a certain temperature, the grain size became constant and didn't change significantly.

Near-infrared quantum cutting in Yb3+ ion doped strontium vanadate

NASA Astrophysics Data System (ADS)

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

2016-05-01

The materials Sr3-x(VO4)2:xYb were successfully synthesized by co-precipitation method varying the concentration of Yb3+ ions from 0 to 0.06 mol. It was characterize by powder X-ray powder diffraction (XRD) and surface morphology was studied by scanning electronic microscope (SEM). The photoluminescence (PL) properties were studied by spectrophotometers in near infra red (NIR) and ultra violet visible (UV-VIS) region. The Yb3+ ion doped tristrontium vanadate (Sr3(VO4)2) phosphors that can convert a photon of UV region (349 nm) into photons of NIR region (978, 996 and 1026 nm). Hence this phosphor could be used as a quantum cutting (QC) luminescent convertor in front of crystalline silicon solar cell (c-Si) panels to reduce thermalization loss due to spectral mismatch of the solar cells. The theoretical value of quantum efficiency (QE) was calculated from steady time decay measurement and the maximum efficiency approached up to 144.43%. The Sr(3-x) (VO4)2:xYb can be potentiality used for betterment of photovoltaic (PV) technology.

Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

NASA Astrophysics Data System (ADS)

Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

2017-12-01

The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

Surfactant-assisted morphological studies of α-Al2O3 nanoparticles

NASA Astrophysics Data System (ADS)

Shah, Janki; Ranjan, Mukesh; Gupta, Sanjeev K.; Sonvane, Yogesh

2018-05-01

The present study deals with the synthesis and characterization of aluminum oxide (Al2O3) nanopowders, it is very useful material as dielectric, ceramic and catalyst. The high-quality nanopowders were obtained by adding surfactants urea and sodium acetate. Further, all characterizations are done for with (urea and sodium acetate) and without surfactant. X-ray diffraction was used to characterize phase formation and the crystallite size of powder while, FTIR gives information about the particle composition and surface intermediates. X-ray diffraction spectra revealed the synthesized nanoparticles phase transformation were γ-Al2O3 to α-Al2O3 phase. Furthermore, the addition of urea and sodium acetate significantly reduced the crystalline size of α-Al2O3 nanoparticles from 43.94 nm to 35.12 nm respectively.

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

NASA Astrophysics Data System (ADS)

Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

2017-01-01

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

Growth and characterization of organic NLO material: Clobetasol propionate

NASA Astrophysics Data System (ADS)

Purusothaman, R.; Rajesh, P.; Ramasamy, P.

2015-06-01

Single crystals of clobetasol propionate (CP) have been grown by slow evaporation solution technique using mixed solvent of methanol-acetone. The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm their lattice parameter and space group. The powder X-ray diffraction pattern of the grown CP has been indexed. Thermal analysis was performed to study the thermal stability of the grown crystals. Photoluminescence spectrum shows broad emission peak observed at 421 nm. Nonlinear optical studies were carried out for the grown crystal and second harmonic generation (SHG) efficiency was found in the crystal.

Improved camera for better X-ray powder photographs

NASA Technical Reports Server (NTRS)

Parrish, W.; Vajda, I. E.

1969-01-01

Camera obtains powder-type photographs of single crystals or polycrystalline powder specimens. X-ray diffraction photographs of a powder specimen are characterized by improved resolution and greater intensity. A reasonably good powder pattern of small samples can be produced for identification purposes.

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

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

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.

Characterization of ceramic powders by an X-ray measuring method

NASA Technical Reports Server (NTRS)

Ziegler, B.

1983-01-01

X-ray line broadening analysis gives quantitative data on structural changes of ceramic powders after different processing steps. Various Al2O3 powders were investigated and the following points are discussed on the basis of these results: X-ray line broadening analysis, structural changes during grinding, structural changes during annealing, influence of structural properties on sintering behavior and application of line broadening analysis to quality control of powders.

Investigation of the nanoscale two-component ZnS-ZnO heterostructures by means of HR-TEM and X-ray based analysis

NASA Astrophysics Data System (ADS)

Pankin, I. A.; Polozhentsev, O. E.; Soldatov, M. A.; Bugaev, A. L.; Tsaturyan, A.; Lomachenko, K. A.; Guda, A. A.; Budnyk, A. P.; Lamberti, C.; Soldatov, A. V.

2018-06-01

This article is devoted to the spectroscopic characterization of ZnS-ZnO nanoscale heterostructures synthesized by the microwave-assisted solvothermal method. The synthesized samples were investigated by means of X-ray powder diffraction (XRPD), high energy resolution fluorescence detected X-ray absorption near-edge-structure (HERFD-XANES) spectroscopy, valence-to-core X-ray emission spectroscopy (VtC-XES) and high resolution transmission electron microscopy (HR-TEM) as well as energy dispersive X-ray spectroscopy (EDX). The average crystallite size estimated by the broadening of XRPD peaks increases from 2.7 nm to 3.7 nm in the temperature range from 100 °C to 150 °C. HR-TEM images show that nanoparticles are arranged in aggregates with the 60-200 nm size. Theoretical estimation shows that the systems synthesized at higher temperatures more prone to the agglomeration. The full profile Reitveld analysis of XRPD data reveals the formation of hexagonal zinc sulfide structure, whereas electron diffraction data reveal also the formation of cubic zinc sulfide and claim the polymorphous character of the system. High energy resolution Zn K-edge XANES data unambiguously demonstrate the presence of a certain amount of the zinc oxide which is likely to have an amorphous structure and could not be detected by XRPD. Qualitative analysis of XANES data allows deriving ZnS/ZnO ratio as a function of synthesis temperature. EDX analysis depicts homogeneous distribution of ZnS and amorphous ZnO phases across the conglomerates. A complementary element-selective valence to core X-ray emission spectroscopy evidences formation of two-component system and confirms estimations of ZnS/ZnO fractions obtained by linear combination fit of XANES data.

A general route for the rapid synthesis of one-dimensional nanostructured single-crystal Te, Se and Se Te alloys directly from Te or/and Se powders

NASA Astrophysics Data System (ADS)

Zhou, Bo; Zhu, Jun-Jie

2006-03-01

A general and template-free 'disproportionation and reversal' route was developed to synthesize one-dimensional (1D) nanostructures of Te, Se and Se-Te alloys directly from Te or/and Se powders. The products were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and scanning electron microscopy (SEM). Te nanorods and nanowires with a width varying from about 40 nm to about 300 nm, Se nanowires with a width of 60-100 nm and a length of 4-6 µm, and SexTe100-x alloy nanorods with x in a wide range, and with a width of 30-70 nm and an aspect ratio of three to five, were prepared. The mechanism of formation of the nanorods and nanowires and the effects of the experimental conditions, such as solution concentration, cooling rate, solvent nature and heating process, on the morphology and size of the products have been discussed. We believe that this general route and some other proper reversible processes between solid state and solution state can be extended to the transformations from various bulk materials into nanosized materials with various morphologies.

Sintering and Microstructure of BaTiO3 Nano Particles Synthesized by Molten Salt Method.

PubMed

Lee, Chang-Hyun; Shin, Hyo-Soon; Yeo, Dong-Hun; Ha, Gook-Hyun; Nahm, Sahn

2016-05-01

In order to establish thinner dielectric layers in thick film electronic components such as MLCC (Multilayer ceramic capacitor), BaTiO3 nanoparticles have been utilized. However, studies on the synthesis of nanoparticles smaller than 20 nm, the characteristics of the BaTiO3 powder, and the powder's sintering are lacking. Therefore, this paper aims to synthesize BaTiO3 particles smaller than 20 nm by using the molten salt method and evaluate the microstructure and dielectric properties by varying the sintering temperature from 750 degrees C to 1200 degrees C. Through the molten salt method and by using KOH-KCl mixed salt, 20 nm BaTiO3 powder was synthesized at a low temperature of 150 degrees C. Sintering the pellets formed from the synthesized 20 nm BaTiO3 nano powder led to the observation of an unusual phenomenon where the particles grew to approximate sizes below 850 degrees C where densification progressed. At sintering temperatures above 950 degrees C, particles that expanded into rod shapes were observed and these particles were identified to be unreacted TiO2 based on the results of the EDX (Energy Dispersive X-ray Spectroscopy) analysis and phase analysis results.

Crystal structure and europium luminescence of NaMgH3-xFx

NASA Astrophysics Data System (ADS)

Pflug, Christian; Franz, Alexandra; Kohlmann, Holger

2018-02-01

The solid solution series NaMgH3-xFx (x = 0, 0.5, 1, 1.5, 2, 2.5, 3) was synthesized by solid-state reactions under hydrogen gas pressure from binary ionic hydrides, fluorides and magnesium. Rietveld refinement based on X-ray powder diffraction data revealed the GdFeO3-structure type for all compounds and a trend of lattice parameters according to Vegard's law. The anion distribution in NaMgD2F and NaMgD1.5F1.5 was found to be statistical by Rietveld refinement based on neutron powder diffraction data. Photoluminescence measurements on europium(II) substituted NaMgH3-xFx revealed a strong red shift of the emission wavelength (λem = 665 nm for NaMgH2F:Eu) in comparison to violet emitting NaMgF3:Eu.

Exploring the Nature of Cellulose Microfibrils

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

Su, Ying; Burger, Christian; Ma, Hongyang

2015-03-20

Ultrathin cellulose microfibril fractions were extracted from spruce wood powder using combined delignification, TEMPO-catalyzed oxidation, and sonication processes. Small-angle X-ray scattering of these microfibril fractions in a “dilute” aqueous suspension (concentration 0.077 wt %) revealed that their shape was in the form of nanostrip with 4 nm width and only about 0.5 nm thicknesses. We found that these dimensions were further confirmed by TEM and AFM measurements. The 0.5 nm thickness implied that the nanostrip could contain only a single layer of cellulose chains. At a higher concentration (0.15 wt %), SAXS analysis indicated that these nanostrips aggregated into amore » layered structure. The X-ray diffraction of samples collected at different preparation stages suggested that microfibrils were delaminated along the (110) planes from the Iβ cellulose crystals. Moreover, the degree of oxidation and solid-state 13C NMR characterizations indicated that, in addition to the surface molecules, some inner molecules of microfibrils were also oxidized, facilitating the delamination into cellulose nanostrips.« less

Exploring the nature of cellulose microfibrils.

PubMed

Su, Ying; Burger, Christian; Ma, Hongyang; Chu, Benjamin; Hsiao, Benjamin S

2015-04-13

Ultrathin cellulose microfibril fractions were extracted from spruce wood powder using combined delignification, TEMPO-catalyzed oxidation, and sonication processes. Small-angle X-ray scattering of these microfibril fractions in a "dilute" aqueous suspension (concentration 0.077 wt %) revealed that their shape was in the form of nanostrip with 4 nm width and only about 0.5 nm thicknesses. These dimensions were further confirmed by TEM and AFM measurements. The 0.5 nm thickness implied that the nanostrip could contain only a single layer of cellulose chains. At a higher concentration (0.15 wt %), SAXS analysis indicated that these nanostrips aggregated into a layered structure. The X-ray diffraction of samples collected at different preparation stages suggested that microfibrils were delaminated along the (11̅0) planes from the Iβ cellulose crystals. The degree of oxidation and solid-state (13)C NMR characterizations indicated that, in addition to the surface molecules, some inner molecules of microfibrils were also oxidized, facilitating the delamination into cellulose nanostrips.

Facile one-pot synthesis of hexagons of NaSrB5O9:Tb3+ phosphor for solid-state lighting

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Deva Prasad Raju, B.; Somasundaram, K.; Prasad Peddi, Siva; de Carvalho dos Anjos, Virgilio; Joo, S. W.

2017-04-01

NaSrB5O9:Tb3+ hexagons were synthesized by a facile solid-state reaction method. The synthesized powders were structurally examined by x-ray diffraction analysis (XRD), and Rietveld refinement was performed using the XRD data and Fullprof software. Hexagon-like morphology was observed using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The elemental composition of the phosphors was investigated qualitatively by energy dispersive x-ray analysis (EDS) and quantitatively by x-ray photoelectron spectroscopy (XPS). The phosphor has a strong green emission at 545 nm under excitation of 379 nm, which is due to the 5{{\\text{D}}4}{{\\to}7}{{\\text{F}}5} transition of the Tb3+ ion. A lifetime of 3.48 ms was obtained for the phosphor. The important parameters of the light source were determined, such as the thermal quenching, critical distance, the nature of the dopant ion interaction, color coordinates, and quantum yield values. Other reported properties include the site occupancy of the dopant, surface properties, morphological properties, and optical properties.

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith

2015-09-01

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

Structure investigations of ferromagnetic Co-Ni-Al alloys obtained by powder metallurgy.

PubMed

Maziarz, W; Dutkiewicz, J; Lityńska-Dobrzyńska, L; Santamarta, R; Cesari, E

2010-03-01

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.

Crystal Growth and Luminescence Properties of Yb-doped Gd3Al2Ga3O12 Infra-red Scintillator

NASA Astrophysics Data System (ADS)

Suzuki, Akira; Kurosawa, Shunsuke; Nagata, Shinji; Yamamura, Tomoo; Pejchal, Jan; Yamaji, Akihiro; Yokota, Yuui; Shirasaki, Kenji; Homma, Yoshiya; Aoki, Dai; Shikama, Tatsuo; Yoshikawa, Akira

2014-07-01

1-mol%-Yb-doped Gd3Al2Ga3O12 infra-red scintillator crystal has been studied as a novel implantable radiation monitor in radiation therapy. Powder X-ray diffraction measurement and chemical analysis with a field emission scanning microscope and wavelength dispersive spectrometer determined its garnet structure and average chemical composition of Yb0.03±0.01Gd2.99±0.07Al2.21±0.08Ga2.64±0.09O12.10±0.09. Transmittance measurements reached high values of approximately 70% in the human body transparency region between 650 to 1200 nm. Photoluminescence peaks were detected around 970 and 1030 nm under the 940 nm excitation with a Xe lamp. Infra-red scintillation emissions were clearly observed around 970 and 1030 nm due to Yb3+ 4f-4f transitions under X-ray excitation. Therefore, these results suggest that Yb-doped Gd3Al2Ga3O12 might be used as an infra-red scintillator material.

Copper doped TiO2 nanoparticles characterized by X-ray absorption spectroscopy, total scattering, and powder diffraction--a benchmark structure-property study.

PubMed

Lock, Nina; Jensen, Ellen M L; Mi, Jianli; Mamakhel, Aref; Norén, Katarina; Qingbo, Meng; Iversen, Bo B

2013-07-14

Metal functionalized nanoparticles potentially have improved properties e.g. in catalytic applications, but their precise structures are often very challenging to determine. Here we report a structural benchmark study based on tetragonal anatase TiO2 nanoparticles containing 0-2 wt% copper. The particles were synthesized by continuous flow synthesis under supercritical water-isopropanol conditions. Size determination using synchrotron PXRD, TEM, and X-ray total scattering reveals 5-7 nm monodisperse particles. The precise dopant structure and thermal stability of the highly crystalline powders were characterized by X-ray absorption spectroscopy and multi-temperature synchrotron PXRD (300-1000 K). The combined evidence reveals that copper is present as a dopant on the particle surfaces, most likely in an amorphous oxide or hydroxide shell. UV-VIS spectroscopy shows that copper presence at concentrations higher than 0.3 wt% lowers the band gap energy. The particles are unaffected by heating to 600 K, while growth and partial transformation to rutile TiO2 occur at higher temperatures. Anisotropic unit cell behavior of anatase is observed as a consequence of the particle growth (a decreases and c increases).

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

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

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

2016-07-27

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

Aqueous Combustion Synthesis and Characterization of Nanosized Tetragonal Zirconia Single Crystals

NASA Astrophysics Data System (ADS)

Reddy, B. S. B.; Mal, Indrajit; Tewari, Shanideep; Das, Karabi; Das, Siddhartha

2007-08-01

Nanocrystalline zirconia powder has been synthesized by an aqueous combustion synthesis route using glycine as fuel and nitrate as oxidizer. The powders have been prepared by using different glycine to zirconyl nitrate molar ratios (G/N). The powders produced with different G/N ratios have been characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) to determine the parameters resulting from powder with attractive properties. The theoretical combustion temperature (T ad ) has been calculated for different G/N ratios, and it is correlated with powder characteristics. An attempt is also made to explain the stability of tetragonal zirconia on the basis of extrinsic factors such as the morphology of nanocrystallites. Nanocrystalline metastable tetragonal zirconia (˜25 nm) powder (TZ) with disc-shaped morphology has been produced with a weak agglomeration in fuel deficient mixtures.

Effect of Zn2+, Fe3+ and Cr3+ addition to hydroxyapatite for its application as an active constituent of sunscreens

NASA Astrophysics Data System (ADS)

de Araujo, T. S.; de Souza, S. O.; de Sousa, E. M. B.

2010-11-01

Biocompatible phosphate materials are used in different applications like bone and dental implants, drug delivery systems and others, but could also be applied in inorganic sunscreens. Using sunscreens is extremely necessary, because long time exposure to sun can cause skin cancer. In this work chemical precipitation method has been used to produce hydroxyapatite. Cr3+, Zn2+ and Fe3+ doped samples were characterized using powder X-Ray Diffraction (XRD) and Optical Absorption techniques. X-ray diffraction measurements confirmed the materials were in the expected crystalline structures. The crystallite size as measured from the X-ray pattern was 23-27 nm (±1). The absorption spectra in the ultraviolet and visible ranges indicate that appropriately doped and sized hydroxyapatite particles may have potential applications as active constituents of sunscreens.

Fabrication of Spherical AlSi10Mg Powders by Radio Frequency Plasma Spheroidization

NASA Astrophysics Data System (ADS)

Wang, Linzhi; Liu, Ying; Chang, Sen

2016-05-01

Spherical AlSi10Mg powders were prepared by radio frequency plasma spheroidization from commercial AlSi10Mg powders. The fabrication process parameters and powder characteristics were investigated. Field emission scanning electron microscope, X-ray diffraction, laser particle size analyzer, powder rheometer, and UV/visible/infrared spectrophotometer were used for analyses and measurements of micrographs, phases, granulometric parameters, flowability, and laser absorption properties of the powders, respectively. The results show that the obtained spherical powders exhibit good sphericity, smooth surfaces, favorable dispersity, and excellent fluidity under appropriate feeding rate and flow rate of carrier gas. Further, acicular microstructures of the spherical AlSi10Mg powders are composed of α-Al, Si, and a small amount of Mg2Si phase. In addition, laser absorption values of the spherical AlSi10Mg powders increase obviously compared with raw material, and different spectra have obvious absorption peaks at a wavelength of about 826 nm.

Solid-state synthesis of nano-sized Ba(Ti1- x Sn x )O3 powders and dielectric properties of corresponding ceramics

NASA Astrophysics Data System (ADS)

Ansaree, Md. Jawed; Kumar, Upendra; Upadhyay, Shail

2017-06-01

Powders of a few compositions of solid solution BaTi1- x Sn x O3 ( x = 0.0, 0.1, 0.2, 0.3 and 0.40) have been synthesized at 800 °C for 8 h using Ba(NO3)2, TiO2 and SnCl4·5H2O as starting materials. The thermogravimetric (TG) and differential scanning calorimetric (DSC) analysis of mixture in the stoichiometric proportion for sample BaTi0.80Sn0.20O3 have been carried out to understand the formation of solid solutions. Single-phase pure compounds (except x = 0.40) of the samples have been obtained at a lower calcination temperature (800 °C) than that of those reported in the literature for traditional solid-state synthesis making use of oxides and or carbonates as starting material (≥1200 °C). Tetragonal symmetry for compositions x = 0.0 and 0.10, cubic for x = 0.2 and 0.30 were found by X-ray diffraction (XRD) analysis. The transmission electron microscopic (TEM) analysis confirmed that calcined powders have a particle size between 30 and 50 nm. Ceramics of these powders were prepared by sintering at 1350 °C for 4 h. Properties of ceramics obtained in this work have been compared with properties reported in the literature.

Upconversion luminescence in BaMoO{sub 4}:Pr{sup 3+} phosphor for display devices

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

Soni, Abhishek Kumar; Rai, Vineet Kumar, E-mail: vineetkrrai@yahoo.co.in

2015-08-28

The frequency upconversion is an important nonlinear optical property by which near infrared light is converted into the visible light. The BaMoO{sub 4}:Pr{sup 3+} powder phosphor has been synthesized by solid state reaction method. The upconversion emission bands are recorded under the excitation of 808 nm diode laser. The phase formation of the prepared phosphor has been identified by powder X-ray diffraction (XRD) technique. The upconversion emission mechanism and colour coordinate have been explained by using energy level and CIE (International Commission on Illumination) chromaticity diagram study, respectively.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

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

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

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

2014-09-03

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

X-ray Diffraction from Membrane Protein Nanocrystals

PubMed Central

Hunter, M.S.; DePonte, D.P.; Shapiro, D.A.; Kirian, R.A.; Wang, X.; Starodub, D.; Marchesini, S.; Weierstall, U.; Doak, R.B.; Spence, J.C.H.; Fromme, P.

2011-01-01

Membrane proteins constitute >30% of the proteins in an average cell, and yet the number of currently known structures of unique membrane proteins is <300. To develop new concepts for membrane protein structure determination, we have explored the serial nanocrystallography method, in which fully hydrated protein nanocrystals are delivered to an x-ray beam within a liquid jet at room temperature. As a model system, we have collected x-ray powder diffraction data from the integral membrane protein Photosystem I, which consists of 36 subunits and 381 cofactors. Data were collected from crystals ranging in size from 100 nm to 2 μm. The results demonstrate that there are membrane protein crystals that contain <100 unit cells (200 total molecules) and that 3D crystals of membrane proteins, which contain <200 molecules, may be suitable for structural investigation. Serial nanocrystallography overcomes the problem of x-ray damage, which is currently one of the major limitations for x-ray structure determination of small crystals. By combining serial nanocrystallography with x-ray free-electron laser sources in the future, it may be possible to produce molecular-resolution electron-density maps using membrane protein crystals that contain only a few hundred or thousand unit cells. PMID:21190672

Mössbauer study of Cu1-xZnxFe2O4 catalytic materials

NASA Astrophysics Data System (ADS)

Koleva, K.; Velinov, N.; Tsoncheva, T.; Mitov, I.

2014-04-01

Copper zinc ferrites (Cu1-xZnxFe2O4) with different composition (x = 1; 0.2; 0.5; 0.8) were prepared by conventional thermal method. Formation of well crystallized ferrite phase with cubic structure and crystallites size of about 19.08-24.39 nm was observed by Powder X-ray diffraction and Mössbauer spectroscopy. The ferrite materials were tested as catalysts in methanol decomposition to CO and H2. A strong dependence of the catalytic behaviour of Cu1-xZnxFe2O4 ferrites of their composition and the phase transformations which occurred under the reaction medium was established.

Characterization of Metal Powders Used for Additive Manufacturing.

PubMed

Slotwinski, J A; Garboczi, E J; Stutzman, P E; Ferraris, C F; Watson, S S; Peltz, M A

2014-01-01

Additive manufacturing (AM) techniques can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process.

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.

Synthesis of SiO2-Coated Core-Shell ZnO Composites for Preparing High-Voltage Varistors

NASA Astrophysics Data System (ADS)

Qu, Xiao; Yao, Da-Chuan; Liu, Jin-Ran; Wang, Mao-Hua; Zhang, Han-Ping

2018-01-01

Monodispersed ZnO composite microspheres were successfully prepared by a facile ultrasound irradiation method. Then, the uniform core-shell structured composites were synthesized through the hydrolysis of tetraethyl orthosilicate on the surface of the ZnO composite microspheres. Microstructural studies of the as-obtained powders were carried out using the techniques of the x-ray powder diffraction, field emission scanning electron microscopy and transmission electron microscopy with energy dispersive x-ray spectroscopy. The results show that the pink ZnO composite powders as the core were spherical structures with the size of approximately 100 nm, and the SiO2 shell was fully coated on the surface of the core. On the basis of these results, the effect of SiO2 content on the thickness of the synthesized composites and microstructure, as well as the electrical properties of the ZnO varistors sintered in air at 1150°C for 2 h, were fully studied. In particular, the ZnO varistor prepared with the appropriate amount of the SiO2 coating (˜40 nm) leads to a superior electrical performance with the high breakdown voltage of 418 V mm-1 and an excellent nonlinear coefficient of 70.7, compared with the varistors obtained without the SiO2 coating. The high performance is attributed to the smaller and more homogeneous ZnO grains obtained via the SiO2 coating.

Pt-B System Revisited: Pt2B, a New Structure Type of Binary Borides. Ternary WAl12-Type Derivative Borides.

PubMed

Sologub, Oksana; Salamakha, Leonid; Rogl, Peter; Stöger, Berthold; Bauer, Ernst; Bernardi, Johannes; Giester, Gerald; Waas, Monika; Svagera, Robert

2015-11-16

On the basis of a detailed study applying X-ray single-crystal and powder diffraction, differential scanning calorimetry, and scanning electron microscopy analysis, it was possible to resolve existing uncertainties in the Pt-rich section (≥65 atom % Pt) of the binary Pt-B phase diagram above 600 °C. The formation of a unique structure has been observed for Pt2B [X-ray single-crystal data: space group C2/m, a = 1.62717(11) nm, b = 0.32788(2) nm, c = 0.44200(3) nm, β = 104.401(4)°, RF2 = 0.030]. Within the homogeneity range of "Pt3B", X-ray powder diffraction phase analysis prompted two structural modifications as a function of temperature. The crystal structure of "hT-Pt3B" complies with the hitherto reported structure of anti-MoS2 [space group P63/mmc, a = 0.279377(2) nm, c = 1.04895(1) nm, RF = 0.075, RI = 0.090]. The structure of the new "[Formula: see text]T-Pt3B" is still unknown. The formation of previously reported Pt∼4B has not been confirmed from binary samples. Exploration of the Pt-rich section of the Pt-Cu-B system at 600 °C revealed a new ternary compound, Pt12CuB6-y [X-ray single-crystal data: space group Im3̅, a = 0.75790(2) nm, y = 3, RF2 = 0.0129], which exhibits the filled WAl12-type structure accommodating boron in the interstitial trigonal-prismatic site 12e. The isotypic platinum-aluminum-boride was synthesized and studied. The solubility of copper in binary platinum borides has been found to attain ∼7 atom % Cu for Pt2B but to be insignificant for "[Formula: see text]T-Pt3B". The architecture of the new Pt2B structure combines puckered layers of boron-filled and empty [Pt6] octahedra (anti-CaCl2-type fragment) alternating along the x axis with a double layer of boron-semifilled [Pt6] trigonal prisms interbedded with a layer of empty tetrahedra and tetragonal pyramids (B-deficient α-T[Formula: see text]I fragment). Assuming boron vacancies ordering (space group R3), the Pt12CuB6-y structure exhibits serpentine-like columns of edge-connected boron-filled [Pt6] trigonal prisms running infinitely along the z axis and embedding the icosahedrally coordinated Cu atom. Pt2B, (Pt1-yCuy)2B (y = 0.045), and Pt12CuB6-y (y = 3) behave metallically, as revealed by temperature-dependent electrical resistivity measurements.

Ba2Mg(BO3)2:Bi3+ - A new phosphor with ultraviolet light emission

NASA Astrophysics Data System (ADS)

Lakshminarasimhan, N.; Jayakiruba, S.; Prabhavathi, K.

2017-10-01

Ultraviolet light emission was observed in a new Ba2Mg(BO3)2:Bi3+ phosphor. Bi3+ substitution for Ba2+ in the lattice was supplemented with K+ to maintain the charge neutrality. The samples of the formula Ba2-2xBixKxMg(BO3)2 [x = 0, 0.001, 0.01, 0.02, and 0.05] synthesized by solid state reaction were characterized using powder X-ray diffraction for their phase formation. Raman and diffuse reflectance UV-Vis spectroscopic techniques were used to obtain information on the vibrational modes and optical properties, respectively. The room temperature photoluminescence measurements revealed an ultraviolet emission at 370 nm when excited using 304 nm wavelength and the Stokes shift is 5868 cm-1.

Investigation of nanocrystalline zinc chromite obtained by two soft chemical routes

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

Gingasu, Dana; Mindru, Ioana, E-mail: imandru@yahoo.com; Culita, Daniela C.

2014-01-01

Graphical abstract: - Highlights: • Two soft chemical routes to synthesize zinc chromites are described. • Glycine is used as chelating agent (precursor method) and fuel (solution combustion method). • The synthesized chromites have crystallite size in the range of 18–27 nm. • An antiferromagnetic (AFM) transition is observed at about T{sub N} ∼ 18 K. - Abstract: Zinc chromite (ZnCr{sub 2}O{sub 4}) nanocrystalline powders were obtained by two different chemical routes: the precursor method and the solution combustion method involving glycine-nitrates. The complex compound precursors, [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COO){sub 8}]·9H{sub 2}O and [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COOH){sub 4.5}]·(NO{sub 3}){sub 8}·6H{submore » 2}O, were characterized by chemical analysis, infrared spectroscopy (IR), ultraviolet–visible spectroscopy (UV–vis) and thermal analysis. The structure, morphology, surface chemistry and magnetic properties of ZnCr{sub 2}O{sub 4} powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), infrared and Raman spectroscopy (RS), ultraviolet–visible spectroscopy (UV–vis) and magnetic measurements. X-ray diffraction patterns indicated the chromite spinel phase with good crystallinity and an average crystallite size of approximately 18–27 nm. The band gap values ranged between 3.31 and 3.33 eV. The magnetic measurements indicated an antiferromagnetic transition at T{sub N} ∼ 17.5/18 K.« less

Combustion synthesis and characterization of blue long lasting phosphor CaAl2O4: Eu2+, Dy3+ and its novel application in latent fingerprint and lip mark detection

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vijay; Kumar, Vinay; Verma, Kartikey; Swart, H. C.

2018-04-01

This work investigates the structural, optical and photometric characterization of a Eu2+/Dy3+ doped calcium aluminates phosphor (CaAl2O4: Eu2+/Dy3+) for finger and lip print detections. Synthesis of CaAl2O4: Eu2+/Dy3+ (CAED) phosphors were carried out via a combustion synthesis method with urea as a fuel. Eu2+/Dy3+ doped CaAl2O4 phosphors have been studied with X-ray diffraction (XRD, Energy Dispersive X-Ray Spectroscopy Selected Area Diffraction (SAED) and High resolution Transmission Electron Microscope (HR-TEM). The XRD pattern shows that the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphor have a single monoclinic structure and show that the addition of the dopant/co-dopants didn't change the crystal structure. The formation of monoclinic phase was confirmed by the selected area diffraction pattern. The TEM micrograph displays the morphology of the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphors as spherical particles with an average particle size of 33 nm. The optical band gap was calculated using the diffuse reflectance for the synthesized nanophosphor powders. The photoluminescence emission spectra was recorded for the synthesized powder, with an excitation wavelength of 326 nm and the major bands was recorded at 447 nm corresponding to the blue color and two minor bands were recorded at 577 nm and 616 nm. To the best of our knowledge, this work is the first to show the use of CaAl2O4: Eu2+/Dy3+ nanophosphor in developing latent fingerprint and lip print effectively.

Studies on the sensing behaviour of nanocrystalline CuGa(2)O(4) towards hydrogen, liquefied petroleum gas and ammonia.

PubMed

Biswas, Soumya Kanti; Sarkar, Arpita; Pathak, Amita; Pramanik, Panchanan

2010-06-15

In the present article, the gas sensing behaviour of nanocrystalline CuGa(2)O(4) towards H(2), liquefied petroleum gas (LPG) and NH(3) has been reported for the first time. Nanocrystalline powders of CuGa(2)O(4) having average particle sizes in the range of 30-60nm have been prepared through thermal decomposition of an aqueous precursor solution comprising copper nitrate, gallium nitrate and triethanol amine (TEA), followed by calcination at 750 degrees C for 2h. The synthesized nanocrystalline CuGa(2)O(4) powders have been characterised through X-ray diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM) study, energy dispersive X-ray (EDX) analysis and BET (Brunauer-Emmett-Teller) surface area measurement. The synthesized CuGa(2)O(4) having spinel structure with specific surface area of 40m(2)/g exhibits maximum sensitivity towards H(2), LPG, and NH(3) at 350 degrees C.

Luminescence and antibacterial studies of silver nanoparticles using the esterases-containing latex of E. Tirucalli plant via green route

NASA Astrophysics Data System (ADS)

Sudheerkumar, K. H.; Dhananjaya, N.; Reddy Yadav, L. S.

2016-04-01

Silver nanoparticles (Ag NPs) synthesized from silver nitrate solutions using the esterase-containing latex of the E. Tirucalli plant widely found in a large region in Karnataka, India. Plant-mediated synthesis of nanoparticles is a green chemistry approach that intercom-nects nanotechnology and plant biotechnology. The effect of extract concentration, contact time, and temperature on the reaction rate and the shape of the Ag nanoparticles was investigated. The nanoparticles have been characterized by powder X-ray diffraction, UV-visible spectroscopy, photoluminescence spectroscopy and morphology by scanning electron microscope, transmission electron microscopy, as a function of the ratio of silver ions to reducing agent molecules. Powder X-ray diffraction patterns show that the crystal structure obtained is face-centered cubic (fcc). The morphology of the silver nanoparticle was uniform with well-distributed elliptical particles with a range from 15 to 25nm. Ag NPs exhibit significant antibacterial activity against Bacillus cereus using the agar well diffusion method.

Rietveld analysis of the effect of annealing atmosphere on phase evolution of nanocrystalline TiO2 powders.

PubMed

Salari, M; Rezaee, M; Chidembo, A T; Konstantinov, K; Liu, H K

2012-06-01

The structural evolution of nanocrystalline TiO2 was studied by X-ray diffraction (XRD) and the Rietveld refinement method (RRM). TiO2 powders were prepared by the sol-gel technique. Post annealing of as-synthesized powders in the temperature range from 500 degrees C to 800 degrees C under air and argon atmospheres led to the formation of TiO2 nanoparticles with mean crystallite size in the range of 37-165 nm, based on the Rietveld refinement results. It was found that the phase structure, composition, and crystallite size of the resulting particles were dependent on not only the annealing temperature, but also the annealing atmosphere. Rietveld refinement of the XRD data showed that annealing the powders under argon atmosphere promoted the polymorphic phase transformation from anatase to rutile. Field emission scanning electron microscopy (FESEM) was employed to investigate the morphology and size of the annealed powders.

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl(6) and other alloys are twinned cubic crystals.

PubMed

Pauling, L

1987-06-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl(6) and Mg(32)(Al,Zn)(49) and the neutron powder diffraction pattern of MnAl(6) are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl(6) and 24.313 A (x-ray) for Mg(32)(Al,Zn)(49).

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl6 and other alloys are twinned cubic crystals

PubMed Central

Pauling, Linus

1987-01-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl6 and Mg32(Al,Zn)49 and the neutron powder diffraction pattern of MnAl6 are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 Å (x-ray) and 23.416 Å (neutron) for MnAl6 and 24.313 Å (x-ray) for Mg32(Al,Zn)49. PMID:16593841

Photocatalytic activity of SnO{sub 2} nanoparticles in methylene blue degradation

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

Kim, Sung Phil; Choi, Myong Yong, E-mail: mychoi@gnu.ac.kr; Choi, Hyun Chul, E-mail: chc12@chonnam.ac.kr

2016-02-15

Highlights: • Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method. • SnO{sub 2} nanoparticles displayed high photocatalytic activities for the MB degradation. • OH radicals are the main active species in photocatalysis on the SnO{sub 2} nanoparticles. - Abstract: Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method and were characterized by performing transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The powder XRD results revealed that the SnO{sub 2} nanoparticles have a typical tetragonal rutile (cassiterite) structure and the average crystallite size was found to be approximately 4.5 nm by usingmore » the Debye–Scherrer equation. The prepared SnO{sub 2} nanoparticles consist of agglomerated particles with a mean diameter of around 4–5 nm according to the analysis of TEM images. The XAS data confirmed that the prepared samples have cassiterite structures with tin oxidation state of +4. The prepared SnO{sub 2} nanoparticles were found to exhibit approximately 3.8 times higher activity than bulk SnO{sub 2} in the photodegradation of methylene blue. On the basis of a trapping experiment, we developed a possible mechanism for the photodegradation on SnO{sub 2} nanoparticles.« less

Flash microwave synthesis and sintering of nanosized La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}o{sub 3-{delta}} for fuel cell application

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

Combemale, L., E-mail: lionel.combemale@u-bourgogne.f; Caboche, G.; Stuerga, D.

2009-10-15

Perovskite-oxide nanocrystals of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} with a mean size around 10 nm were prepared by microwave flash synthesis. This reaction was performed in alcoholic solution using metallic salts, sodium ethoxide and microwave autoclave. The obtained powder was characterised after purification by energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), BET adsorption technique, photon correlation spectroscopy (PCS) and transmission electron microscopy (TEM). The results show that integrated perovskite-type phase and uniform particle size were obtained in the microwave treated samples. At last the synthesised powder was directly used in a sintering process. A porous solid, inmore » accordance with the expected applications, was then obtained at low sintering temperature (1000 deg. C) without use of pore forming agent. - Graphical abstract: TEM photograph of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} obtained by microwave flash synthesis. This picture confirms the nanometric size of the ceramic particles.« less

Solvent-Based Synthesis of Nano-Bi0.85Sb0.15 for Low-Temperature Thermoelectric Applications

NASA Astrophysics Data System (ADS)

Kaspar, K.; Fritsch, K.; Habicht, K.; Willenberg, B.; Hillebrecht, H.

2017-01-01

In this study we show a preparation method for nanostructured Bi0.85Sb0.15 powders via a chemical reduction route in a polyol medium, yielding material with particle sizes of 20-150 nm in scalable amounts. The powders were consolidated by spark plasma sintering (SPS) in order to maintain the nanostructure. To investigate influence of the sinter process, the powders were characterized by x-ray diffraction (XRD), energy dispersive x-ray spectroscopy (EDX), and scanning electron microscopy (SEM) measurements before and after SPS. Transport properties, Seebeck effect, and thermal conductivity were determined in the low temperature range below 300 K. The samples showed excellent thermal conductivity of 2.3-2.6 W/m × K at 300 K and Seebeck coefficients from -97 μV/K to -107 μV/K at 300 K with a maximum of -141 μV/K at 110 K, thus leading to ZT values of up to 0.31 at room temperature. The results show that Bi-Sb-alloys are promising materials for low-temperature applications. Our wet chemical approach gives access to scalable amounts of nano-material with increased homogeneity and good thermoelectric properties after SPS.

Iron-based soft magnetic composites with Mn-Zn ferrite nanoparticles coating obtained by sol-gel method

NASA Astrophysics Data System (ADS)

Wu, Shen; Sun, Aizhi; Xu, Wenhuan; Zhang, Qian; Zhai, Fuqiang; Logan, Philip; Volinsky, Alex A.

2012-11-01

This paper focuses on iron-based soft magnetic composites which were synthesized by utilizing Mn-Zn ferrite nanoparticles to coat iron powder. The nanocrystalline iron powders, with an average particle diameter of 20 nm, were obtained via the sol-gel method. Scanning electron microscopy, energy dispersive X-ray spectroscopy and distribution maps show that the iron particle surface is covered with a thin layer of Mn-Zn ferrites. Mn-Zn ferrite uniformly coated the surface of the powder particles, resulting in a reduced imaginary permeability, increased electrical resistivity and a higher operating frequency of the synthesized magnets. Mn-Zn ferrite coated samples have higher permeability and lower magnetic loss when compared with the non-magnetic epoxy resin coated compacts. The real part of permeability increases by 33.5% when compared with the epoxy resin coated samples at 10 kHz. The effects of heat treatment temperature on crystalline phase formation and on the magnetic properties of the Mn-Zn ferrite were investigated via X-ray diffraction and a vibrating sample magnetometer. Ferrites decomposed to FeO and MnO after annealing above 400 °C in nitrogen; thus it is the optimum annealing temperature to attain the desired permeability.

Characterization of Metal Powders Used for Additive Manufacturing

PubMed Central

Slotwinski, JA; Garboczi, EJ; Stutzman, PE; Ferraris, CF; Watson, SS; Peltz, MA

2014-01-01

Additive manufacturing (AM) techniques1 can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process. PMID:26601040

Zr doping dependence of structural and magnetic properties of cobalt ferrite synthesized by sol-gel based Pechini method

NASA Astrophysics Data System (ADS)

Motavallian, Pourya; Abasht, Behzad; Abdollah-Pour, Hassan

2018-04-01

Nanocrystalline CoZrxFe2-xO4 (0 ≤ x ≤ 0.3 in a step of 0.05) powders were synthesized by Pechini sol-gel method. The dry gel was grinded and calcined at 700 °C in a static air atmosphere for 1 h. Some tests such as thermo gravimetric analysis (TGA) combined with differential analysis (DTA), fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and vibrating sample magnetometer (VSM) were carried out to investigate the thermal behaviour, structural bonds identification, crystallographic properties, morphology and magnetic properties of the obtained powders. X-ray diffraction revealed a single-phase cubic spinel structure for all samples, where the crystallite size decreases; the lattice parameter simultaneously increases with substitution of Zr. The results of FE-SEM showed that the particle size is in the 20-70 nm range. The magnetic properties such as saturation magnetization (Ms), remanent magnetization (Mr) and coercivity (Hc) were measured from the hysteresis loops. The greatest amount of saturation magnetization for CoZr0.05Fe1.95O4 sample was 67.9 emu·g-1.

The Influence of Sintering Temperature on the Microstructure and Thermoelectric Properties of n-Type Bi2Te3- x Se x Nanomaterials

NASA Astrophysics Data System (ADS)

Du, Y.; Cai, K. F.; Li, H.; An, B. J.

2011-05-01

Pure Bi2Te3 and Bi2Se3 nanopowders were hydrothermally synthesized, and n-type Bi2Te3- x Se x bulk samples were prepared by hot pressing a mixture of Bi2Te3 and Bi2Se3 nanopowders at 623 K, 648 K or 673 K and 80 MPa in vacuum. The phase composition of the powders and bulk samples were characterized by x-ray diffraction. The morphology of the powders was examined by transmission electron microscopy. The microstructure and composition of the bulk samples were characterized by field-emission scanning electron microscopy and energy-dispersive x-ray spectroscopy, respectively. The density of the samples increased with sintering temperature. The samples were somewhat oxidized, and the amount of oxide (Bi2TeO5) present increased with sintering temperature. The samples consisted of sheet-like grains with a thickness less than 100 nm. Seebeck coefficient, electrical conductivity, and thermal conductivity of the samples were measured from room temperature up to 573 K. Throughout the temperature range investigated, the sample sintered at 623 K had a higher power factor than the samples sintered at 648 K or 673 K.

Synthesis and characterization of nanocrystalline Nd{sup 3+}-doped gadolinium scandium aluminum garnet powders by a gel-combustion method

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

Su, Jing, E-mail: zlj007@126.com; Miao, Ju-hong; Xu, Lin-hua

2012-07-15

Graphical abstract: The graph shows the emission spectra (λ{sub ex} = 808 nm) of 1 at.% Nd:GSAG powders sintered at different temperatures for 3 h. Compared with the powder sintered at 900 °C, the PL intensity of the powder sintered at 1000 °C decreased significantly. The changes in the PL intensity should mainly due to the crystallinity and dispersion of the powders. Highlights: ► We synthesized Nd:GSAG nano-powders by gel-combustion method successfully. ► We analyzed the structure and the morphology of the heat-treated products. ► We studied the optical characteristics of Nd:GSAG nano-powders. -- Abstract: Nd{sup 3+}-doped gadolinium scandium aluminummore » garnet (Nd:GSAG) precursor was synthesized by a gel combustion method using metal nitrates and citric acid as raw materials. The structure and morphology of the precursor and the sintered powders were studied by means of X-ray diffraction (XRD), infrared spectroscopy (IR) and transmission electron microscopy (TEM). The results showed that the precursor transformed into pure GSAG polycrystalline phase at about 800 °C, and the powders sintered at 800–1000 °C were well-dispersed with average particle sizes in the range of 30–80 nm. Optical properties of Nd:GSAG nano-powders were characterized by using photoluminescence spectroscopy. The highest photoluminescence intensity was achieved for the powder sintered at 900 °C.« less

Synthesis of nanocrystalline zirconia by amorphous citrate route: structural and thermal (HTXRD) studies

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

Bhagwat, Mahesh; Ramaswamy, Veda

Nanocrystalline zirconia powder with a fairly narrow particle size distribution has been synthesized by the amorphous citrate route. The sample obtained has a high BET surface area of 89 m{sup 2} g{sup -1}. Rietveld refinement of the powder X-ray diffraction (XRD) profile of the zirconia sample confirms stabilization of zirconia in the tetragonal phase with around 8% monoclinic impurity. The data show the presence of both anionic as well as cationic vacancies in the lattice. Crystallite size determined from XRD is 8 nm and is in close agreement with the particle size determined by TEM. The in situ high temperature-X-raymore » diffraction (HTXRD) study revealed high thermal stability of the mixture till around 1023 K after which the transformation of tetragonal phase into the monoclinic phase has been seen as a function of temperature till 1473 K. This transformation is accompanied by an increase in the crystallite size of the sample from 8 to 55 nm. The thermal expansion coefficients are 9.14 x 10{sup -6} K{sup -1} along 'a'- and 15.8 x 10{sup -6} K{sup -1} along 'c'-axis. The lattice thermal expansion coefficient in the temperature range 298-1623 K is 34.6 x 10{sup -6} K{sup -1}.« less

Physicochemical interaction mechanism between nanoparticles and tetrasaccharides (stachyose) during freeze-drying.

PubMed

Kamiya, Seitaro; Nakashima, Kenichiro

2017-12-01

Nanoparticle suspensions are thermodynamically unstable and subject to aggregation. Freeze-drying on addition of saccharides is a useful method for preventing aggregation. In the present study, tetrasaccharides (stachyose) was employed as an additive. In addition, we hypothesize the interactive mechanism between stachyose and the nanoparticles during freeze-drying for the first time. The mean particle size of the rehydrated freeze-dried stachyose-containing nanoparticles (104.7 nm) was similar to the initial particle size before freeze-drying (76.8 nm), indicating that the particle size had been maintained. The mean particle size of the rehydrated normal-dried stachyose-containing nanoparticles was 222.2 nm. The powder X-ray diffraction of the freeze-dried stachyose-containing nanoparticles revealed a halo pattern. The powder X-ray diffraction of the normally dried stachyose-containing nanoparticles produced mainly a halo pattern and a partial peak. These results suggest an interaction between the nanoparticles and stachyose, and that this relationship depends on whether the mixture is freeze-dried or dried normally. In the case of normal drying, although most molecules cannot move rapidly thereby settling irregularly, some stachyose molecules can arrange regularly leading to some degree of crystallization and potentially some aggregation. In contrast, during freeze-drying, the moisture sublimed, while the stachyose molecules and nanoparticles were immobilized in the ice. After sublimation, stachyose remained in the space occupied by water and played the role of a buffer material, thus preventing aggregation.

Intercalation of cellulase enzyme into a hydrotalcite layer structure

NASA Astrophysics Data System (ADS)

Zou, N.; Plank, J.

2015-01-01

A new inorganic-organic hybrid material whereby cellulase enzyme is incorporated into a hydrotalcite type layered double hydroxide (LDH) structure is reported. The Mg2Al-cellulase-LDH was synthesized via co-precipitation from Mg/Al nitrate at pH=9.6. Characterization was performed using X-ray powder diffraction (XRD), small angle X-ray scattering (SAXS), elemental analysis, infrared spectroscopy (IR) and thermogravimetry (TG). From XRD and SAXS measurements, a d-value of ~5.0 nm was identified for the basal spacing of the Mg2Al-cellulase-LDH. Consequently, the cellulase enzyme (hydrodynamic diameter ~6.6 nm) attains a slightly compressed conformation when intercalated. Formation of the LDH hybrid was also confirmed via scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Mg2Al-cellulase-LDH phases appear as ~20 nm thin foils which are intergrown to flower-like aggregates. Activity of the enzyme was retained after deintercalation from the Mg2Al-LDH framework using anion exchange. Accordingly, cellulase is not denatured during the intercalation process, and LDH presents a suitable host structure for time-controlled release of the biomolecule.

Nanocrystalline (U0.5Ce0.5)O2±x solid solutions through citrate gel-combustion

NASA Astrophysics Data System (ADS)

Maji, D.; Ananthasivan, K.; Venkata Krishnan, R.; Balakrishnan, S.; Amirthapandian, S.; Joseph, Kitheri; Dasgupta, Arup

2018-04-01

Nanocrystalline powders of (U0.5Ce0.5)O2±x solid solutions were synthesized in bulk (100-200 g) through the citrate gel combustion. The fuel (citric acid) to oxidant (nitrate) mole ratio (R) was varied from 0.1 to 1.0. Two independent lots of the products obtained through the gel-combustion were calcined at 973 K in air and in a mixture of argon containing 8% H2 respectively. All these powders were characterized for their bulk density, X-ray crystallite size, specific surface area, size distribution of the particles, porosity as well as residual carbon. The morphology and microstructures of these powders were studied by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) respectively. Nanocrystalline single phase fluorite solid solutions having a typical crystallite size of about (7-15 nm) were obtained. These powders were highly porous comprising cuboidal flaky agglomerates. The combustion mixture with an 'R' value of 0.25 was found to undergo volume combustion and was found to yield a product that was distinctly different. The systematic investigation on synthesis and characterization of nanocrystalline UCeO2 is reported for the first time.

The Morphology of Titanium Dioxide Aerogels

NASA Astrophysics Data System (ADS)

Zhu, Zhu

The morphology of titanium dioxide TiO _2 aerogels has been characterized by four major techniques. This work will discuss these complementary techniques such as nitrogen adsorption, X-ray powder diffraction (XRD), electron microscopies (EM- TEM, SEM), and small angle neutron scattering (SANS). The results of these characterizations have shown that the morphology of titanium dioxide TiO_2 aerogels can be characterized in terms of two length scales: 5 nm diameter, crystalline nanoparticles of anatase closely packed into mesoaggregates about 50 nm in size. The mesoaggregates are, in turn, packed into a loosely linked structure with an overall porosity of 80%.

Synthesis and optical properties of polycrystalline Li2Al2B2O7 (LABO)

NASA Astrophysics Data System (ADS)

Dagdale, S. R.; Muley, G. G.

2016-05-01

A polycrystalline lithium aluminum borate (Li2Al2B2O7, LABO) has been synthesized by using simple solid-state technique. The obtained LABO polycrystalline was characterized by powder X-ray diffraction; Fourier transform infrared (FT-IR) spectroscopy and second harmonic generation (SHG) efficiency measurement. The functional groups were identified using the FT-IR spectroscopic data. The SHG efficiency of the polycrystalline material was obtained by the classic Kurtz powder technique using a fundamental wavelength 1064 nm of Nd:YAG laser and it is found to be 1.4 times that of potassium dihydrogen phosphate (KDP).

Synchrotron X-ray powder diffraction data of LASSBio-1515: A new N-acylhydrazone derivative compound

NASA Astrophysics Data System (ADS)

Costa, F. N.; Braz, D.; Ferreira, F. F.; da Silva, T. F.; Barreiro, E. J.; Lima, L. M.; Colaço, M. V.; Kuplich, L.; Barroso, R. C.

2014-02-01

In this work, synchrotron X-ray powder diffraction data allowed for a successful indexing of LASSBio-1515 compound, candidate to analgesic and anti-inflammatory activity. X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze this compound. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.55054 Å. LASSBio-1515 was found to be monoclinic with space group P21/c and unit cell parameters a=11.26255(16) Å, b=12.59785(16) Å, c=8.8540(1) Å, β=90.5972(7)° and V=1256.17(3) Å3.

Luminescence concentration quenching and site-occupancy of Eu2+ ions in Na2Ca2Si3O9 phosphors derived from 45S5 glass-ceramics

NASA Astrophysics Data System (ADS)

Zhu, Yangguang; Tong, Chao; Xu, Chuanyan; Li, Yadong; Seo, Hyo Jin

2016-04-01

The phosphors of Na2Ca2-2xEu2xSi3O9 (x = 0, 0.03, 0.05, 0.07, 0.09) were first synthesized by sol-gel method. The crystal phase formations of the phosphors were detected by X-ray powder diffraction (XRD) measurements and the structure refinement. The photoluminescence spectra, the concentration quenching, the luminescence decay curves and the luminescence color chromaticity were measured, respectively. The excitation spectra indicate that the phosphors can be effectively excited by near UV-LED chips. Two kinds of Eu2+ sites centered at 545 nm and 505 nm were discussed by analyzing the spectra, concentration-dependent luminescence intensity and lifetimes. This is a potential tool for monitoring the bioactivity of 45S5 glass-ceramics in situ.

Enhanced efficiency of luminescence with stoichiometry control in LiGd(W(1-x)MoxO4)2:Eu3+ red phosphors

NASA Astrophysics Data System (ADS)

Kavi Rasu, K.; Balaji, D.; Moorthy Babu, S.

2017-06-01

A series of LiGd(W(1-x)MoxO4)2 [hereafter LGWM]:Eu3+(x=0.00 to 1.00) red-emitting phosphors were synthesized by sol-gel method. Metal nitrates were used as starting materials with citric acid as chelator and ethylene glycol as binder. Synthesized gel was pre-fired at 523 K and calcined at 1073 K using resistive furnace in air atmosphere. The crystallinity, surface morphology and luminescent properties of the phosphors were investigated using powder X-ray diffraction (XRD), scanning electron microscope (SEM) and fluorescence spectrophotometry respectively. The intensity of the red emission at 615 nm for 5D0→7F2 electric dipole transition increases as the content of Mo6+ was increased and reach a maximum, when the relative ratio of W/Mo is 1:1 under 396 nm excitation.

Enhancement of luminescence emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor by Li{sup +} co-doping

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

Gavrilović, Tamara V.; Jovanović, Dragana J., E-mail: draganaj@vinca.rs; Lojpur, Vesna M.

2014-09-15

This paper demonstrates the effects of Li{sup +} co-doping on the structure, morphology, and luminescence properties of GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor prepared using a high-temperature solid-state chemistry method. The GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} powders synthesized with the Li{sup +} co-dopant (in concentrations of 0, 5, 10, and 15 mol%) are characterized by X-ray powder diffraction, scanning electron microscopy, and photoluminescence spectroscopy. Structural analysis showed that powders co-doped with Li{sup +} have larger crystallite sizes and slightly smaller crystal lattice parameters than powders prepared without Li{sup +} ions. Photoluminescence down-conversion (345-nm excitation) and up-conversion (980-nm excitation) spectra show characteristic Er{supmore » 3+} emissions, with the most intense bands peaking at 525 nm ({sup 2}H{sub 11/2}→{sup 4}I{sub 15/2} transition) and 552 nm ({sup 4}S{sub 3/2}→{sup 4}I{sub 15/2}). The intensity of up-conversion emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} is enhanced (by a factor of four) by co-doping with 5 mol% of Li{sup +} ions. The mechanisms responsible for this emission enhancement are discussed. - Graphical abstract: UC emission spectra for GdVO{sub 4}:1.5-mol% Er{sup 3+}/20-mol% Yb{sup 3+} powders co-doped with different concentrations of Li{sup +} ions, recorded under 980-nm excitation. - Highlights: • 5-mol% Li{sup +} co-doped powders have 400% enhanced up-conversion emission intensity. • 15-mol% Li{sup +} co-doping produces 40% higher emission in down-conversion. • Li{sup +} co-doped powders have larger crystallite size and smaller lattice parameters.« less

Crucibleless crystal growth and Radioluminescence study of calcium tungstate single crystal fiber

NASA Astrophysics Data System (ADS)

Silva, M. S.; Jesus, L. M.; Barbosa, L. B.; Ardila, D. R.; Andreeta, J. P.; Silva, R. S.

2014-11-01

In this article, single phase and high optical quality scheelite calcium tungstate single crystal fibers were grown by using the crucibleless laser heated pedestal growth technique. The as-synthesized calcium tungstate powders used for shaping seed and feed rods were investigated by X-ray diffraction technique. As-grown crystals were studied by Raman spectroscopy and Radioluminescence measurements. The results indicate that in both two cases, calcined powder and single crystal fiber, only the expected scheelite CaWO4 phase was observed. It was verified large homogeneity in the crystal composition, without the presence of secondary phases. The Radioluminescence spectra of the as-grown single crystal fibers are in agreement with that present in Literature for bulk single crystals, presented a single emission band centered at 420 nm when irradiated with β-rays.

[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.

Mono- and bi-functional arenethiols as surfactants for gold nanoparticles: synthesis and characterization

PubMed Central

2011-01-01

Stable gold nanoparticles stabilized by different mono and bi-functional arenethiols, namely, benzylthiol and 1,4-benzenedimethanethiol, have been prepared by using a modified Brust's two-phase synthesis. The size, shape, and crystalline structure of the gold nanoparticles have been determined by high-resolution electron microscopy and full-pattern X-ray powder diffraction analyses. Nanocrystals diameters have been tuned in the range 2 ÷ 9 nm by a proper variation of Au/S molar ratio. The chemical composition of gold nanoparticles and their interaction with thiols have been investigated by X-ray photoelectron spectroscopy. In particular, the formation of networks has been observed with interconnected gold nanoparticles containing 1,4-benzenedimethanethiol as ligand. PMID:21711615

Synthesis and characterizations of spherical hollow composed of AgI nanoparticle using AgBr as the precursor

NASA Astrophysics Data System (ADS)

Yang, Ming; Zhou, Kui

2011-01-01

Hollow spheres of AgI with an average radius of 100-200 nm have been prepared by a simple reaction between AgBr suspension and KI in the presence of gelatin. Gelatin played a decisive role as an inhibitor of the direct attack of I- ions to AgBr surfaces and coagulation of the growing AgI in producing the spherical AgI particles. The products were characterized by X-ray powder diffraction, transmission electron microscopy, UV-vis absorption spectroscopy and X-ray photoelectron spectra techniques. The band gaps are estimated to be 2.95 eV according to the results of optical measurements of the hollow spheres of AgI.

Correlation between thermoluminescence glow curve and emission spectra of gamma ray irradiated LaAlO3

NASA Astrophysics Data System (ADS)

Shivaramu, N. J.; Lakshminarasappa, B. N.; Nagabhushana, K. R.; Coetsee, E.; Swart, H. C.

2018-04-01

Lanthanum aluminate (LaAlO3) is synthesized by solution combustion method and the resultant powder is annealed at 900°C for 2 hours. X-ray diffraction (XRD) pattern confirms the rhombohedral structure LaAlO3 with space group R3 ¯c. γ-irradiated nanocrystalline lanthanum aluminate gives two prominent TL glow with peaks at 399 and 639 K and weak one at 547 K. TL intensity at 399 K increases up to 9.0 kGy and then decreases with increasing γ-dose. TL emission shows at 650 nm and 736 nm is attributed to the charge transfer from oxygen to metal ions. The glow curves are analyzed and the trap parameters are calculated by glow curve deconvoluted technique.

Eu2+,Dy3+ codoped SrAl2O4 nanocrystalline phosphor for latent fingerprint detection in forensic applications

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vinay

2016-01-01

In this work, europium and dysprosium doped strontium aluminate (SrAl2O4:Eu2+,Dy3+) nanophosphor is synthesized and its novel application for the detection of latent fingerprints on various contact surfaces is reported. The SrAl2O4:Eu2+,Dy3+ is synthesized using a combustion method and shows long-lasting afterglow luminescence. The powder particles are characterized using field emission scanning electron microscopy (FE-SEM), SEM-energy dispersive x-ray analysis, x-ray diffraction and photoluminescence spectrophotometry. The FE-SEM image analysis reveals that the nanoparticles are mostly 8-15 nm in size with an irregular spherical shape. This nano-structured powder was applied to fresh and aged fingerprints deposited on porous, semi-porous and non-porous contact surfaces, such as ordinary colored paper, glossy paper, glass, aluminum foil, a yellow foil chocolate wrapper, a soft drink can, a PET bottle, a compact disc and a computer mouse. The results are reproducible and show great sensitivity and high contrast in the developed fingermark regions on these surfaces. These nanophosphor particles also show a strong and long-lasting afterglow property, making them a suitable candidate for use as a fingerprint developing agent on luminescent and highly patterned surfaces. These kinds of powders have shown that they can remove the interference from background luminescence, which is not possible using ordinary luminescent fingerprinting powders.

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

Comparative study of proteasome inhibitory, synergistic antibacterial, synergistic anticandidal, and antioxidant activities of gold nanoparticles biosynthesized using fruit waste materials.

PubMed

Patra, Jayanta Kumar; Baek, Kwang-Hyun

The aim of this study was to compare the biological synthesis of gold nanoparticles (AuNPs) generated using the aqueous extracts of outer oriental melon peel (OMP) and peach. The synthesized OMP-AuNPs and peach extract (PE)-AuNPs were characterized by ultraviolet-visible spectroscopy, field emission scanning electron microscopy, energy dispersive X-ray analysis, X-ray powder diffraction, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The surface plasmon resonance spectra were obtained at 545 nm and 540 nm for OMP-AuNPs and PE-AuNPs, respectively. The estimated absolute crystallite size of the synthesized AuNPs was calculated to be 78.11 nm for OMP-AuNPs and 39.90 nm for PE-AuNPs based on the Scherer equation of the X-ray powder diffraction peaks. Fourier transform infrared spectroscopy results revealed the involvement of bioactive compounds present in OMP and peach extracts in the synthesis and stabilization of synthesized AuNPs. Both the OMP-AuNPs and PE-AuNPs showed a strong antibacterial synergistic activity when combined with kanamycin (9.38-20.45 mm inhibition zones) and rifampicin (9.52-25.23 mm inhibition zones), and they also exerted a strong synergistic anticandidal activity (10.09-15.47 mm inhibition zones) when combined with amphotericin B against five pathogenic Candida species. Both the OMP-AuNPs and PE-AuNPs exhibited a strong antioxidant potential in terms of 1,1-diphenyl-2-picrylhydraxyl radical scavenging, nitric oxide scavenging, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) radical scavenging, and a reducing power, along with a strong proteasome inhibitory potential that could be useful in cancer drug delivery and cancer treatments. The PE-AuNPs showed comparatively higher activity than OMP-AuNPs, which could be attributed to the presence of rich bioactive compounds in the PE that acted as reducing and capping agents in the synthesis of PE-AuNPs. Overall, the results of the current investigation highlighted a novel green technology for the synthesis of AuNPs using food waste materials and their potential applications in the biomedical, pharmaceutical, and cosmetic industries.

Thermal analysis, X-ray powder diffraction and electron microscopy data related with the production of 1:1 Caffeine:Glutaric Acid cocrystals.

PubMed

Duarte, Íris; Andrade, Rita; Pinto, João F; Temtem, Márcio

2016-09-01

The data presented in this article are related to the production of 1:1 Caffeine:Glutaric Acid cocrystals as part of the research article entitled "Green production of cocrystals using a new solvent-free approach by spray congealing" (Duarte et al., 2016) [1]. More specifically, here we present the thermal analysis and the X-ray powder diffraction data for pure Glutaric Acid, used as a raw material in [1]. We also include the X-ray powder diffraction and electron microscopy data obtained for the 1:1 Caffeine:Glutaric Acid cocrystal (form II) produced using the cooling crystallization method reported in "Operating Regions in Cooling Cocrystallization of Caffeine and Glutaric Acid in Acetonitrile" (Yu et al., 2010) [2]. Lastly, we show the X-ray powder diffraction data obtained for assessing the purity of the 1:1 Caffeine:Glutaric cocrystals produced in [1].

Preparation and characterization of nanosilica from oil shale ash.

PubMed

Li, Jinhong; Qian, Tingting; Tong, Lingxin; Shen, Jie

2014-05-01

Nano-sized silica powders was prepared using oil shale ash (OSA) as starting materials. A combined process was proposed for the utilization of OSA in the production of the nanosilica, including three stages: calcination, alkaline leaching and carbon dioxide separation. Effects of the calcining temperature, sodium hydroxide concentration and holding time on the desilication ratio were investigated. The microstructure and morphologies of the nano-sized silica were characterized by X-ray diffraction, transmission electron microscopy, and Brunauer-Emmett-Teller nitrogen-gas adsorption method. The results indicated that the obtained powders with particle size of about 40 nm are homegeneously dispersed and its specific surface area is 387 m2/g. The properties of the nano-sized silica powder meet the requirements of the Chinese Chemical Industry Standard HG/T 3061-1999.

Nanoscale investigation of platinum nanoparticles on strontium titanium oxide grown via physical vapor deposition and atomic layer deposition

NASA Astrophysics Data System (ADS)

Christensen, Steven Thomas

This dissertation examines growth of platinum nanoparticles from vapor deposition on SrTiO3 using a characterization approach that combines imaging techniques and X-ray methods. The primary suite of characterization probes includes atomic force microscopy (AFM), grazing-incidence small-angle X-ray scattering (GISAXS), X-ray fluorescence (XRF), scanning electron microscopy (SEM), and X-ray absorption spectroscopy (XAS). The vapor deposition techniques include physical vapor deposition (PVD) by evaporation and atomic layer deposition (ALD). For the PVD platinum study, AFM/XRF showed ˜10 nm nanoparticles separated by an average of 100 nm. The combination of AFM, GISAXS, and XRF indicated that the nanoparticles observed with AFM were actually comprised of closely spaced, smaller nanoparticles. These conclusions were supported by high-resolution SEM. The unusual behavior of platinum nanoparticles to aggregate without coalescence or sintering was observed previously by other researchers using transmissision electron microscopy (TEM). Platinum nanoparticle growth was also investigated on SrTiO3 (001) single crystals using ALD to nucleate nanoparticles that subsequently grew and coalesced into granular films as the ALD progresses. The expected growth rate for the early stages of ALD showed a two-fold increase which was attributed to the platinum deposition occurring faster on the bare substrate. Once the nanoparticles had coalesced into a film, steady state ALD growth proceeded. The formation of nanoparticles was attributed to the atomic diffusion of platinum atoms on the surface in addition to direct growth from the ALD precursor gases. The platinum ALD nanoparticles were also studied on SrTiO3 nanocube powders. The SrTiO3 nanocubes average 60 nm on a side and the cube faces have a {001} orientation. The ALD proceeded in a similar fashion as on the single crystal substrates where the deposition rate was twice as fast as the steady state growth rate. The Pt nanoparticle size increased linearly starting at ˜0.7 nm for 1 ALD cycle to ˜3 nm for 5 ALD cycles. The platinum chemical state was also investigated using X-ray absorption spectroscopy. Platinum nanoparticles ˜1 nm or smaller tended to be oxidized. For larger nanoparticles, the platinum state systematically approached that of bulk platinum metal as the size (number of ALD cycles) increased. The platinum loading was exceptionally low, ˜10 -3 mg cm-2.

Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

2015-10-01

The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

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

Shang Yazhuo; Hu Jun; Liu Honglai, E-mail: yazhuoshang@ecust.edu.c

Novel large-scale hollow ZnO spherical shells were synthesized by ionic liquids assisted hydrothermal oxidization of pure zinc powder without any catalyst at a relatively low temperature of 160 deg. C. X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX) and scanning electron microscopy (SEM) patterns show that the shells are composed of ZnO and the structure of the shells is very unique. Textured flower-like ZnO consisting of ZnO rods is grown on the outer surfaces of shells forming a triple assembly. Room-temperature photoluminescence spectra of the oxidized material show a sharp peak at 379 nm and a wider broad peak centeredmore » at 498 nm. The possible growth mechanism of the triple assembly of ZnO is discussed in detail. - Graphical abstract: A proposed growth mechanism of large scale hollow ZnO. Bubbles provide the aggregation center for ionic liquids that leads to the formation of hollow Zn particle-dotted shells, buoyancy promotes shells to go upward, the breach occurs when shells are subjected to overpressure.« less

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

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

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

2016-05-06

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Green synthesis of nanocrystalline α-Al2O3 powders by both wet-chemical and mechanochemical methods

NASA Astrophysics Data System (ADS)

Gao, Huiying; Li, Zhiyong; Zhao, Peng

2018-03-01

Nanosized α-Al2O3 powders were prepared with AlCl3ṡ6H2O and NH4HCO3 as raw materials by both wet-chemical and mechanochemical methods, through the synthesis of the ammonium aluminum carbonate hydroxide (AACH) precursor followed by calcination. The environmentally benign starch was used as an effective dispersant during the preparation of nanocrystalline α-Al2O3 powders. X-ray diffraction (XRD), thermogravimetric differential thermal analysis (TG-DTA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were employed to characterize the precursor AACH and products. The results show that nanosized spherical α-Al2O3 powders without hard agglomeration and with particle size in the range of 20-40 nm can be obtained by the two methods. Comparing the two “green” processes, the mechanochemical method has better prospects for commercial production.

X-ray photoelectron spectroscopy (XPS) investigation of the surface film on magnesium powders.

PubMed

Burke, Paul J; Bayindir, Zeynel; Kipouros, Georges J

2012-05-01

Magnesium (Mg) and its alloys are attractive for use in automotive and aerospace applications because of their low density and good mechanical properties. However, difficulty in forming magnesium and the limited number of available commercial alloys limit their use. Powder metallurgy may be a suitable solution for forming near-net-shape parts. However, sintering pure magnesium presents difficulties due to surface film that forms on the magnesium powder particles. The present work investigates the composition of the surface film that forms on the surface of pure magnesium powders exposed to atmospheric conditions and on pure magnesium powders after compaction under uniaxial pressing at a pressure of 500 MPa and sintering under argon at 600 °C for 40 minutes. Initially, focused ion beam microscopy was utilized to determine the thickness of the surface layer of the magnesium powder and found it to be ~10 nm. The X-ray photoelectron analysis of the green magnesium sample prior to sintering confirmed the presence of MgO, MgCO(3)·3H(2)O, and Mg(OH)(2) in the surface layer of the powder with a core of pure magnesium. The outer portion of the surface layer was found to contain MgCO(3)·3H(2)O and Mg(OH)(2), while the inner portion of the layer is primarily MgO. After sintering, the MgCO(3)·3H(2)O was found to be almost completely absent, and the amount of Mg(OH)(2) was also decreased significantly. This is postulated to occur by decomposition of the compounds to MgO and gases during the high temperature of sintering. An increase in the MgO content after sintering supports this theory.

Effect of bismuth substitution in strontium hexaferrite

NASA Astrophysics Data System (ADS)

Sahoo, M. R.; Kuila, S.; Sweta, K.; Barik, A.; Vishwakarma, P. N.

2018-05-01

Bismuth (Bi) substituted M-type strontium hexaferrite (Sr1-xBix Fe12O19, x=0 and 0.02) are synthesized by sol-gel auto combustion method. Powder X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) shows increase in lattice parameter and particle size (500 nm to 3 micron) respectively, for Bi substituted sample. Magnetization via M-H shows decrease in magnetic hardness for Bi substituted samples. M-T data for parent (x=0) sample shows an antiferromagnetic transition in the ZFC plot at 495 °C. This antiferromagnetic transition is replaced by a ferromagnetic transition for FCW measurement. Similar behavior is displayed by the Bi substituted sample with transition temperature reduced to 455 °C.

Synthesis of nanocrystalline NiO/ZnO heterostructured composite powders by sol-gel auto combustion method and their characterizations

NASA Astrophysics Data System (ADS)

Tangcharoen, Thanit; Klysubun, Wantana; Kongmark, Chanapa

2018-03-01

Nanocrystalline NiO/ZnO heterostructured composite powders were prepared by the sol-gel auto combustion method, based on nickel and zinc nitrate precursors and using diethanolamine (DEA) as novel fuel. The composition of different NiO and ZnO ratios, ranging from 100/0, 95/5, 90/10, 80/20, 60/40, 50/50, 40/60, 20/80, 10/90, 5/95 to 0/100, were studied. The structural, chemical bonding, morphological, optical, and fluorescence properties including the local atomic structure of each calcined sample were systematically investigated by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), UV-visible diffuse reflectance spectroscopy (UV-DRS), photoluminescence (PL) spectroscopy, and synchrotron X-ray absorption spectroscopy (XAS), respectively. For the ZnO concentration below 20%, both XRD and Raman spectroscopy results revealed only the NiO phase. This conformed to the observation of Zn K-edge and Ni K-edge X-ray absorption near edge structure (XANES). The Zn ions found in the samples of low ZnO concentration exhibited six-fold coordination with oxygen atoms rather than the four-fold coordination found in the wurtzite (WZ) structure of ZnO. In contrast, the Ni ions which are found in the samples of low NiO concentration (≤10%) are coordinated both tetrahedrally and octahedrally by four or six oxygen atoms, respectively, rather than the six-fold coordination which is usually observed for Ni ions in the rock salt (RS) form of NiO. All analytical results obtained from experimental XANES spectra were verified by the theoretical calculation of absorption spectra using the FEFF9.7 code. The UV-DRS results showed that there was an increase in the reflectance efficiency for both infrared and visible light conditions as the content of ZnO increases; meanwhile, the values for the energy gap (Eg) of all composite samples were higher than that of pure NiO and ZnO. In addition, the PL spectra revealed major blue emission bands observed at 490 nm when the excitation wavelength was 300 nm. As the ZnO phase developed, a variety of violet emission bands occurred within the range of 400 nm-450 nm, which was obviously related to the change in Eg. The intrinsic defects occurred in the NiO/ZnO composite powders were probably responsible for this phenomenon.

Characterization of Beryllium Windows for Coherent X-ray Optics

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

Goto, Shunji; Yabashi, Makina; Tamasaku, Kenji

2007-01-19

Beryllium foils fabricated by several processes were characterized using spatially coherent x rays at 1-km beamline of SPring-8. By thickness dependence of bright x-ray spot density due to Fresnel diffraction from several-micron deficiencies, we found that speckles (bright x-ray spots) were due to voids with densities 103-104 mm-3 in powder foils and ingot foils. Compared with powder and ingot foils, a polished physical-vapor-deposited (PVD) beryllium foil gave highly uniform beams with no speckles. The PVD process eliminates the internal voids in principle and the PVD foil is the best for coherent x-ray applications.

Synthesis and luminescence properties of Ca3Ga2Si3O12:RE3+ (RE = Eu/Tb) powder phosphors.

PubMed

Reddy, M Bhushana; Sailaja, S; Raju, K Vemasevana; Raju, C Nageswara; Giridhar, P; Rao, B Vengala; Reddy, B Sudhakar

2011-01-01

Rare earth ions (Eu(3+) or Tb(3+) )-activated Ca(3) Ga(2) Si(3) O(12) (CaGaSi) phosphors were synthesized by using a sol-gel method. Photoluminescence spectra of Eu(3+):CaGaSi phosphors exhibited five emission bands at 578, 592, 612, 652 and 701 nm, which were assigned to the transitions ((5)D(0) → (7)F(0), (7)F(1,)(7)F(2), (7)F(3) and (7)F(4)), respectively, with an excitation wavelength of λ(exci) = 392 nm. Among these, the transition (5) D(0) → (7) F(2) (612 nm) displayed bright red emission. In the case of Tb(3+):CaGaSi phosphors, four emission bands were observed at 488 ((5)D(4) → (7)F(6)), 543 ((5)D(4) → (7)F(5)), 584 ((5)D(4) → (7)F(4)) and 614 nm ((5)D(4) → (7) F(3) ) from the measurement of PL spectra with λ(exci) = 376 nm. Among these, the transition (5)D(4) → (7) F(5) at 543 nm displayed bright green emission. The structure and morphology of the phosphors were studied from the measurements of X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDAX) results. Copyright © 2011 John Wiley & Sons, Ltd.

Characterization of powdered fish heads for bone graft biomaterial applications.

PubMed

Oteyaka, Mustafa Ozgür; Unal, Hasan Hüseyin; Bilici, Namık; Taşçı, Eda

2013-01-01

The aim of this study was to define the chemical composition, morphology and crystallography of powdered fish heads of the species Argyrosomus regius for bone graft biomaterial applications. Two sizes of powder were prepared by different grinding methods; Powder A (coarse, d50=68.5 µm) and Powder B (fine, d50=19.1 µm). Samples were analyzed using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), thermogravimetry (TG), and energy dispersive X-ray spectroscopy (EDS). The powder was mainly composed of aragonite (CaCO3) and calcite (CaCO3). The XRD pattern of Powder A and B matched standard aragonite and calcite patterns. In addition, the calcium oxide (CaO) phase was found after the calcination of Powder A. Thermogravimetry analysis confirmed total mass losses of 43.6% and 47.3% in Powders A and B, respectively. The microstructure of Powder A was mainly composed of different sizes and tubular shape, whereas Powder B showed agglomerated particles. The high quantity of CaO and other oxides resemble the chemical composition of bone. In general, the powder can be considered as bone graft after transformation to hydroxyapatite phase.

Generation of the Submicron Soft X-Ray Beam Using a Fresnel Zone Plate

NASA Astrophysics Data System (ADS)

Nishikino, M.; Kawazome, H.; Tanaka, M.; Kishimoto, M.; Hasegawa, N.; Ochi, Y.; Kawachi, T.; Sukegawa, K.; Yamatani, H.; Nagashima, K.; Kato, Y.

We have developed a fully coherent x-ray laser at 13.9 nm and the application research has been started. The generation of submicron x-ray beam is important for the application of high intensity x-ray beam, such as the non-linear optics, the material science, and the biology. The submicron x-ray bee am is generated by the soft x-ray laser with using a Fresnel zone plate. The spot diameter is estimated about 680 nm (290 nm at FWHM) by the theoretical calculation. In this experiment, the diameter of the x-ray beam is measured by the knife-edge scan. The diameter and the intensity are estimated 730 nm (310 nm at FWHM) and 3x1011 W/cm2, respectively.

Low power loss and field-insensitive permeability of Fe-6.5%Si powder cores with manganese oxide-coated particles

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

Li, Junnan, E-mail: junnanli1991@163.com, E-mail: rzhgong@hust.edu.cn; Wang, Xian; Xu, Xiaojun

Fe-6.5%Si alloy powders coated with manganese oxides using an innovative in situ process were investigated. The in-situ coating of the insulating oxides was realized with a KMnO{sub 4} solution by a chemical process. The insulating manganese oxides with mixed valance state were verified by X-ray photoelectron spectroscopy analysis. The thickness of the insulating layer on alloy particles was determined to be in a range of 20–210 nm, depending upon the KMnO{sub 4} concentration. The powder core loss and the change in permeability under a DC-bias field were measured at frequencies ranging from 50 to 100 kHz. The experiments indicated that themore » Fe-6.5%Si powder cores with a 210 nm-thick manganese oxide layer not only showed a low core loss of 459 mW/cm{sup 3} at 100 kHz but also showed a small reduction in permeability (μ(H)/μ(0) = 85% for μ = 42) at a DC-bias field of 80 Oe. This work has defined a novel pathway to realizing low core loss and field-insensitive permeability for Fe-Si powder cores.« less

Synthesis and spectroscopic study of CdS nanoparticles using hydrothermal method

NASA Astrophysics Data System (ADS)

AL-Mamoori, Mohammed H. K.; Mahdi, Dunia K.; Al-Shrefi, Saif M.

2018-05-01

In this work, cadmium sulfide nanoparticles (powder) with diameter 50.8 nm was prepared using hydrothermal method. The structural and optical properties of CdS nanoparticles was studied by X-ray diffraction, FESEM, EDS, FTIR, UV-Diffuse Reflectance spectroscopy and Photoluminance spectrum. X-ray diffraction reveal the formation the purity of prepared phase of CdS particles with hexagonal wurtzite structure with particle size 31.8nm by using sheerer equation. The energy dispersion scattering (EDS) examination explains that the sample is composed of a large amount of Cd and S which are exactly CdS nanoparticles and there is a very small trace of (Zn) and (O) element observed because of there is a small pollutions in the measurement place of samples. FESEM shows the spherical shape of nanoparticles with around 50.8 nm diameter. The optical absorption spectral study identified the red shift of the sample in comparison to bulk ZnO in three dimensions. Photoluminance spectrum (PL) at room temperature showed that there are two luminescence peaks at 433.14 nm and 518.21nm. Samples demonstrate a sharp emission band at around 433.18 nm, which is attributed to the typical exciton luminescence. The broad band at 518.21nm which were attributed to the trapped luminescence. The green emission band at 518.21 nm was associated with the emission due to electronic transition from the conduction band to an accepter level due to interstitial sulphur ion.

Outstanding features of Cu-doped ZnS nanoclusters

NASA Astrophysics Data System (ADS)

Tawfik, Wael Z.; Farghali, A. A.; Moneim, Ahmed; Imam, N. G.; El-Dek, S. I.

2018-05-01

ZnS and their Cu-doped nanoclusters (NCs) were synthesized successfully using the wet chemical route with different Cu content. The crystalline structure was investigated using x-ray powder diffraction which assured the single-phase formation in cubic symmetry. High-resolution transmission electron microscope indicated the microstructure of NCs with a size ranging from 2–4 nm. A butterfly hysteresis (M-H) loop was observed at room temperature with large values of coercivity for the Cu content of x = 0.05. Photoluminescence emission spectra were recorded from 500–615 nm for pure and Cu-doped ZnS NCs at a 350 nm excitation wavelength. The sample exhibited green fluorescence bands peaking at 535, 544, 552.5, 558.2, and 560.6 nm, which confirmed the characteristic feature of Zn2+ as luminescent centers in the lattice. The additional yellow and orange emissions are due to defect levels or/and impurity centers. The dielectric constant as well as the conductivity values increased with increasing Cu content.

Investigations on synthesis, growth and physicochemical properties of semi-organic NLO crystal bis(thiourea) ammonium nitrate for nonlinear frequency conversion

NASA Astrophysics Data System (ADS)

Anbarasi, A.; Ravi Kumar, S. M.; Sundar, G. J. Shanmuga; Mosses, M. Allen; Raj, M. Packiya; Prabhakaran, M.; Ravisankar, R.; Gunaseelan, R.

2017-10-01

Bis(thiourea) ammonium nitrate (BTAN), a new nonlinear optical crystal was grown successfully by slow evaporation technique using water as solvent at room temperature. The grown crystals were optically good quality with dimensions upto 10 × 6 × 3 mm3. Single crystal X-Ray diffraction analysis reveals that the crystal lattice is orthorhombic. From Powder X-ray diffraction analysis the diffraction planes have been indexed. The presence of the various functional groups of BTAN was identified through FTIR spectroscopic analysis. UV cut-off wavelength was observed from optical absorbance spectrum and it was found to be 240 nm. Second harmonic efficiency was determined using Kurtz powder method in comparison with KDP to confirm the nonlinearity of the material. Thermal analysis confirmed that grown crystal is thermally stable upto 184 °C. Microhardness studies show that hardness number (Hv) increases with load. Conductivity measurements such as dielectric, ac and photoconductivity were studied. Growth mechanism and surface features of the as grown single crystal was analysed by chemical etching analysis.

A novel method to delaminate nitrate-intercalated MgAl layered double hydroxides in water and application in heavy metals removal from waste water.

PubMed

Rahman, Mir Tamzid; Kameda, Tomohito; Kumagai, Shogo; Yoshioka, Toshiaki

2018-07-01

Nitrate-intercalated MgAl layered double hydroxide (LDH) was successfully delaminated in water by a facile and effective method upon reflux at 120 °C for 24 h followed by sonication at 40 °C for 5 h. This process is environmentally friendly since water is the only solvent used. The delaminated nanosheets were characterized by microscopic, spectroscopic, and particle size analyses. The delamination process successfully produced octahedron-shaped single-layer nanosheets 50-150 nm in size. X-ray photoelectron spectroscopy (XPS) data confirmed that the surface elements and their chemical status are consistent with the basic layer of MgAl LDH. The delaminated nanosheets displayed higher adsorption capacity for removing heavy metals from waste water than the original powdered LDH. After treating the waste water, a sharp and intense peak in the X-ray powder diffraction (XRD) pattern of the precipitate confirms the restacking of the LDH nanosheets. Copyright © 2018 Elsevier Ltd. All rights reserved.

Functional biocompatible magnetite-cellulose nanocomposite fibrous networks: Characterization by fourier transformed infrared spectroscopy, X-ray powder diffraction and field emission scanning electron microscopy analysis.

PubMed

Habibi, Neda

2015-02-05

The preparation and characterization of functional biocompatible magnetite-cellulose nano-composite fibrous material is described. Magnetite-cellulose nano-composite was prepared by a combination of the solution-based formation of magnetic nano-particles and subsequent coating with amino celluloses. Characterization was accomplished using X-ray powder diffraction (XRD), fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. The peaks of Fe3O4 in the XRD pattern of nanocomposite confirm existence of the nanoparticles in the amino cellulose matrix. Magnetite-cellulose particles exhibit an average diameter of roughly 33nm as demonstrated by field emission scanning electron microscopy. Magnetite nanoparticles were irregular spheres dispersed in the cellulose matrix. The vibration corresponding to the NCH3 functional group about 2850cm(-1) is assigned in the FTIR spectra. Functionalized magnetite-cellulose nano-composite polymers have a potential range of application as targeted drug delivery system in biomedical field. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Remarkably Enhancing Green-Excitation Efficiency for Solar Energy Utilization: Red Phosphors Ba2ZnS3:Eu2+, X- Co-Doped Halide Ions (X = Cl, Br, I).

PubMed

Luo, Tingting; Du, Yun; Qiu, Zhongxian; Li, Yanmei; Wang, Xiaofang; Zhou, Wenli; Zhang, Jilin; Yu, Liping; Lian, Shixun

2017-05-15

Eu 2+ -activated Ba 2 ZnS 3 has been reported as a red phosphor with a broad emission band peaking at 650 nm under blue excitation for white-LED. In this study, Ba 2 ZnS 3 :Eu 2+ , X - (X = F, Cl, Br, I) phosphors doped with halide ions were prepared by traditional high-temperature solid-state reaction. Phase identification of powders was performed by X-ray powder diffraction analysis, confirming the existence of single-phase Ba 2 ZnS 3 crystals without dopant. The corresponding excitation spectra showed an additional broad band in the green region peaking at 550 nm when the phosphor was halogenated except by the smallest F - . It was proved that the green-excitation efficiency successively strengthened from Cl - , to Br - , to I - , which suggested larger halide ions made a greater contribution to the further splitting of the t 2g energy level of the doped Eu 2+ ions in the host Ba 2 ZnS 3 , and the optimized formula Ba 1.995 ZnS 2.82 :Eu 2+ 0.005 , I - 0.18 showed a potential application in solar spectral conversion for agricultural greenhouse and solar cell. Defect chemistry theory and crystal field theory provided insights into the key role of halide ions in enhancing green-excitation efficiency.

Nanocrystalline ordered vanadium carbide: Superlattice and nanostructure

NASA Astrophysics Data System (ADS)

Kurlov, A. S.; Gusev, A. I.; Gerasimov, E. Yu.; Bobrikov, I. A.; Balagurov, A. M.; Rempel, A. A.

2016-02-01

The crystal structure, micro- and nanostructure of coarse- and nanocrystalline powders of ordered vanadium carbide V8C7 have been examined by X-ray and neutron diffraction and electron microscopy methods. The synthesized coarse-crystalline powder of ordered vanadium carbide has flower-like morphology. It was established that the real ordered phase has the composition V8C7-δ (δ ≅ 0.03) deviating from perfect stoichiometric composition V8C7. The vanadium atoms forming the octahedral environment □V6 of vacant sites in V8C7-δ are displaced towards the vacancy □. The presence of carbon onion-like structures was found in the vanadium carbide powders with a small content of free (uncombined) carbon. The nanopowders of V8C7-δ carbide with average particle size of 20-30 nm produced by high-energy milling of coarse-crystalline powder retain the crystal structure of the initial powder, but differ in the lattice deformation distortion anisotropy.

Low temperature molten-salt synthesis of nanocrystalline cubic Sr{sub 2}SbMnO{sub 6}

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

Baral, Antara; Varma, K.B.R., E-mail: kbrvarma@mrc.iisc.ernet.i

2009-12-15

Sr{sub 2}SbMnO{sub 6} (SSM) powders were successfully synthesized at reasonably low temperatures via molten-salt synthesis (MSS) method using eutectic composition of 0.635 Li{sub 2}SO{sub 4}-0.365 Na{sub 2}SO{sub 4} (flux). High-temperature cubic phase SSM was stabilized at room temperature by calcining the as-synthesized powders at 900 deg. C/10 h. The phase formation and morphology of these powders were characterized via X-ray powder diffraction and scanning electron microscopy, respectively. The SSM phase formation associated with {approx}60 nm sized crystallites was also confirmed by transmission electron microscopy. The activation energy associated with the particle growth was found to be 95+-5 kJ mol{sup -1}.more » The dielectric constant of the tetragonal phase of the ceramic (fabricated using this cubic phase powder) with and without the flux (sulphates) has been monitored as a function of frequency (100 Hz-1 MHz) at room temperature. Internal barrier layer capacitance (IBLC) model was invoked to rationalize the dielectric properties. - Graphical abstract: The as synthesized powders of Sr{sub 2}SbMnO{sub 6} calcined at 900 deg. C/10 h yielded a cubic phase ({approx}60 nm sized crystallites). Centrosymmetric tetragonal (I4/mcm) phase was obtained by increasing the calcination temperature to 1000 deg. C. Display Omitted« less

Synthesis of Gd2O3:Ho3+/Yb3+ upconversion nanoparticles for latent fingermark detection on difficult surfaces

NASA Astrophysics Data System (ADS)

Kumar, A.; Tiwari, S. P.; Singh, A. K.; Kumar, K.

2016-07-01

Infrared to visible upconversion fluorescent nanoparticles of Gd2O3 codoped with Ho3+/Yb3+ ions are synthesized via thermal decomposition process. The X-ray diffraction analysis of as-synthesized nanoparticles and annealed sample at 1000 °C has shown body-centered cubic phase of Gd2O3. The synthesized phosphor has shown intense green emission upon 980-nm excitation. High-contrast latent fingermarks on some difficult semi-porous and non-porous surfaces under 980-nm diode laser excitation were developed through powder dusting and colloidal solution spraying techniques and the results are compared with the commercial green luminescent fingermark powder. The latent fingermarks were developed on transparent (biological glass slides), single-color (aluminum foil) and multicolor (plywood, plastic bottle and book cover page) background surfaces. The present study depicts that the upconversion-based latent fingermarks detection using Gd2O3:Ho3+/Yb3+ phosphor material is suitable over the other conventional powders and has potential for practical applications in forensic science.

A novel energy transfer inducing strong enhancement of electric dipole transition in Na3Mo12PO40:xEu3+ phosphors

NASA Astrophysics Data System (ADS)

Long, Jinqiao; Wang, Tianman; Luo, Zhirong; Gao, Yong; Song, Baoling; Liang, Jing; Liao, Sen; Huang, Yingheng; Zhang, Huaxin

2017-08-01

A series of Na3Mo12PO40:xEu3+ phosphors have been successfully synthesized by a solid-state method, and characterized by powder x-ray diffraction (PXRD). The PXRD results confirm that the samples have crystal phases of Na3Mo12PO40. For PL spectra of Na3Mo12PO40:2.0Eu3+ excited by 394 and 465 nm, R (R is the peak area ratio of 5D0  →  7F2 to 5D0  →  7F1) is only 1.46 with an excitation of 394 nm, but increases to 3.03 with an excitation of 465 nm. Furthermore, a new enhancement of electric dipole transition is observed. Emission spectrum (PL) intensity at 617 nm excited by 465 nm is 1.95 times as high as the excitation spectrum (PLE) intensity at 465 nm. Thus, cooperative energy transfers from the magnetic dipole (MD) Eu3+ center to the electric dipole (ED) Eu3+ center when excited by 465 nm is demonstrated for the new fluorescent behavior.

Non Destructive 3D X-Ray Imaging of Nano Structures & Composites at Sub-30 NM Resolution, With a Novel Lab Based X-Ray Microscope

DTIC Science & Technology

2006-11-01

NON DESTRUCTIVE 3D X-RAY IMAGING OF NANO STRUCTURES & COMPOSITES AT SUB-30 NM RESOLUTION, WITH A NOVEL LAB BASED X- RAY MICROSCOPE S H Lau...article we describe a 3D x-ray microscope based on a laboratory x-ray source operating at 2.7, 5.4 or 8.0 keV hard x-ray energies. X-ray computed...tomography (XCT) is used to obtain detailed 3D structural information inside optically opaque materials with sub-30 nm resolution. Applications include

Chemical and Morphological Inhomogeneity of Aluminum Metal and Oxides from Soft X-ray Spectromicroscopy

DOE PAGES

Altman, Alison B.; Pemmaraju, C. Das; Alayoglu, Selim; ...

2017-05-04

Oxygen and aluminum K-edge X-ray absorption spectroscopy (XAS), imaging from a scanning transmission X-ray microscope (STXM), and first-principles calculations were used to probe the composition and morphology of bulk aluminum metal, α- and γ-Al 2 O 3 , and several types of aluminum nanoparticles. The imaging results agreed with earlier transmission electron microscopy studies that showed a 2 to 5 nm thick layer of Al 2 O 3 on all the Al surfaces. Spectral interpretations were guided by examination of the calculated transition energies, which agreed well with the spectroscopic measurements. The features we observed in the experimental O andmore » Al K-edge XAS were used to determine the chemical structure and phase of the Al 2 O 3 on the aluminum surfaces. For unprotected 18 and 100 nm Al nanoparticles, this analysis revealed an oxide layer that was similar to γ-Al 2 O 3 and comprised of both tetrahedral and octahedral Al coordination sites. For oleic acid-protected Al nanoparticles, only tetrahedral Al oxide coordination sites were observed. Our results were correlated to trends in the reactivity of the different materials, which suggests that the structures of different Al 2 O 3 layers have an important role in the accessibility of the underlying Al metal toward further oxidation. Combined, the Al K-edge XAS and STXM results provided detailed chemical information that was not obtained from powder X-ray diffraction or imaging from a transmission electron microscope.« less

Synthesis, structural, electronic and linear electro-optical features of new quaternary Ag{sub 2}Ga{sub 2}SiS{sub 6} compound

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

Piasecki, M., E-mail: m.piasecki@ajd.czest.pl; Myronchuk, G.L.; Parasyuk, O.V.

For the first time phase equilibria and phase diagram of the AgGaS{sub 2}–SiS{sub 2} system were successfully explored by differential thermal and X-ray phase analysis methods. Crystal structure of low-temperature (LT) modification of Ag{sub 2}Ga{sub 2}SiS{sub 6} (LРў- Ag{sub 2}Ga{sub 2}SiS{sub 6}) was studied by X-ray powder method and it belongs to tetragonal space group I-42d, with unit cell parameters a=5.7164(4) Å, c=9.8023(7) Å, V=320.32(7) Å{sup 3}. Additional details regarding the crystal structure exploration are available at the web page Fachinformationszentrum Karlsruhe. X-ray photoelectron core-level and valence-band spectra were measured for pristine LРў- Ag{sub 2}Ga{sub 2}SiS{sub 6} crystal surface. Inmore » addition, the X-ray photoelectron valence-band spectrum of LРў-Ag{sub 2}Ga{sub 2}SiS{sub 6} was matched on a common energy scale with the X-ray emission S Kβ{sub 1,3} and Ga Kβ{sub 2} bands, which give information on the energy distribution of the S 3p and Ga 4p states, respectively. The presented X-ray spectroscopy results indicate that the valence S p and Ga p atomic states contribute mainly to the upper and central parts of the valence band of LРў-Ag{sub 2}Ga{sub 2}SiS{sub 6}, respectively, with a less significant contribution also to other valence-band regions. Band gap energy was estimated by measuring the quantum energy in the spectral range of the fundamental absorption. We have found that energy gap Eg is equal to 2.35 eV at 300 K. LT-Ag{sub 2}Ga{sub 2}SiS{sub 6} is a photosensitive material and reveals two spectral maxima on the curve of spectral photoconductivity spectra at λ{sub max1} =590 nm and λ{sub max2} =860 nm. Additionally, linear electro-optical effect of LT-Ag{sub 2}Ga{sub 2}SiS{sub 6} for the wavelengths of a cw He-Ne laser at 1150 nm was explored. - Graphical abstract: Manuscript present the technology of growth and investigation of properties a new quaternary compound Ag{sub 2}Ga{sub 2}SiS{sub 6} including the detailed study of the phase equilibria in the AgGaS{sub 2}–SiS{sub 2} system to determine the physico-chemical conditions of its formation. We examined crystal structure of the compound by X-ray powder method, its electronic structure by XPS method. Finally we have found these crystals like promising material for nonlinear optical, electrooptical and piezoelectric applications. - Highlights: • Phase diagram of the AgGaS{sub 2}–SiS{sub 2} system was successfully described at first time. • Crystal Ag{sub 2}Ga{sub 2}SiS{sub 6} was grown and its structure was determined. • Electronic structure and chemical bonding of the Ag{sub 2}Ga{sub 2}SiS{sub 6} crystal were examined by. • X-ray photoelectron spectroscopy (XPS) and X-ray emission spectroscopy (XES) methods. • Optical and photoelectrical properties were investigated.« less

Low-temperature growth and photoluminescence property of ZnS nanoribbons.

PubMed

Zhang, Zengxing; Wang, Jianxiong; Yuan, Huajun; Gao, Yan; Liu, Dongfang; Song, Li; Xiang, Yanjuan; Zhao, Xiaowei; Liu, Lifeng; Luo, Shudong; Dou, Xinyuan; Mou, Shicheng; Zhou, Weiya; Xie, Sishen

2005-10-06

At a low temperature of 450 degrees C, ZnS nanoribbons have been synthesized on Si and KCl substrates by a simple chemical vapor deposition (CVD) method with a two-temperature-zone furnace. Zinc and sulfur powders are used as sources in the different temperature zones. X-ray diffraction (XRD), selected area electron diffraction (SEAD), and transmission electron microscopy (TEM) analysis show that the ZnS nanoribbons are the wurtzite structure, and there are two types-single-crystal and bicrystal nanoribbons. Photoluminescence (PL) spectrum shows that the spectrum mainly includes two parts: a purple emission band centering at about 390 nm and a blue emission band centering at about 445 nm with a weak green shoulder around 510 nm.

Synthesis, structural, electronic and linear electro-optical features of new quaternary Ag2Ga2SiS6 compound

NASA Astrophysics Data System (ADS)

Piasecki, M.; Myronchuk, G. L.; Parasyuk, O. V.; Khyzhun, O. Y.; Fedorchuk, A. O.; Pavlyuk, V. V.; Kozer, V. R.; Sachanyuk, V. P.; El-Naggar, A. M.; Albassam, A. A.; Jedryka, J.; Kityk, I. V.

2017-02-01

For the first time phase equilibria and phase diagram of the AgGaS2-SiS2 system were successfully explored by differential thermal and X-ray phase analysis methods. Crystal structure of low-temperature (LT) modification of Ag2Ga2SiS6 (LT- Ag2Ga2SiS6) was studied by X-ray powder method and it belongs to tetragonal space group I-42d, with unit cell parameters a=5.7164(4) Å, c=9.8023(7) Å, V=320.32(7) Å3. Additional details regarding the crystal structure exploration are available at the web page Fachinformationszentrum Karlsruhe. X-ray photoelectron core-level and valence-band spectra were measured for pristine LT- Ag2Ga2SiS6 crystal surface. In addition, the X-ray photoelectron valence-band spectrum of LT-Ag2Ga2SiS6 was matched on a common energy scale with the X-ray emission S Kβ1,3 and Ga Kβ2 bands, which give information on the energy distribution of the S 3p and Ga 4p states, respectively. The presented X-ray spectroscopy results indicate that the valence S p and Ga p atomic states contribute mainly to the upper and central parts of the valence band of LT-Ag2Ga2SiS6, respectively, with a less significant contribution also to other valence-band regions. Band gap energy was estimated by measuring the quantum energy in the spectral range of the fundamental absorption. We have found that energy gap Eg is equal to 2.35 eV at 300 K. LT-Ag2Ga2SiS6 is a photosensitive material and reveals two spectral maxima on the curve of spectral photoconductivity spectra at λmax1 =590 nm and λmax2 =860 nm. Additionally, linear electro-optical effect of LT-Ag2Ga2SiS6 for the wavelengths of a cw He-Ne laser at 1150 nm was explored.

Titanium doped LSCM anode for hydrocarbon fuelled SOFCs

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

Azad, Abul K.; Hakem, Afizul; Petra, Pg. M. Iskandar

2015-05-15

La{sub 0.75}Sr{sub 0.25}Cr{sub 0.5-x}Mn{sub 0.5}Ti{sub x}O{sub 3} (x = 0.1, 0.2) has been synthesized in solid state reaction method and tested as a potential anode material for solid oxide fuel cells. Rietveld refinement of X-ray powder diffraction data using Fullprof software shows that the materials crystallize in the rhombohedral symmetry in the R-3C space group. The cell parameters are: a = b = 5.5286 (4) Å, c = 13.408(1) Å, α = β = 90°, γ = 120°. Particle size distribution measurements show that the average particle size for x = 0.1 and 0.2 was 232.66 nm and 176.63 nm, respectively. Themore » potential on particles were found to be −22.86 mV and −27.73 mV, for x = 0.1 and x = 0.2, respectively. Thermal expansion measurement using thermo-mechanical analyzer shows that the thermal expansion coefficient is 13.96 × 10{sup −6}/°C which is close to the thermal expansion of the state-of–the art YSZ electrolyte. Microstructure has been observed from scanning electron microscopy which shows a porous structure. Energy dispersive X-ray shows that the percentage of the different cations and anions in the structure are close to the chemical occupancies.« less

Stereospecific growth of densely populated rutile mesoporous TiO2 nanoplate films: a facile low temperature chemical synthesis approach

NASA Astrophysics Data System (ADS)

Lee, Go-Woon; Ambade, Swapnil B.; Cho, Young-Jin; Mane, Rajaram S.; Shashikala, V.; Yadav, Jyotiprakash; Gaikwad, Rajendra S.; Lee, Soo-Hyoung; Jung, Kwang-Deog; Han, Sung-Hwan; Joo, Oh-Shim

2010-03-01

We report for the first time, using a simple and environmentally benign chemical method, the low temperature synthesis of densely populated upright-standing rutile TiO2 nanoplate films onto a glass substrate from a mixture of titanium trichloride, hydrogen peroxide and thiourea in triply distilled water. The rutile TiO2 nanoplate films (the phase is confirmed from x-ray diffraction analysis, selected area electron diffraction, energy-dispersive x-ray analysis, and Raman shift) are 20-35 nm wide and 100-120 nm long. The chemical reaction kinetics for the growth of these upright-standing TiO2 nanoplate films is also interpreted. Films of TiO2 nanoplates are optically transparent in the visible region with a sharp absorption edge close to 350 nm, confirming an indirect band gap energy of 3.12 eV. The Brunauer-Emmet-Teller surface area, Barret-Joyner-Halenda pore volume and pore diameter, obtained from N2 physisorption studies, are 82 m2 g - 1, 0.0964 cm3 g - 1 and 3.5 nm, respectively, confirming the mesoporosity of scratched rutile TiO2 nanoplate powder that would be ideal for the direct fabrication of nanoscaled devices including upcoming dye-sensitized solar cells and gas sensors.

Green synthesis, characterisation and bioactivity of plant-mediated silver nanoparticles using Decalepis hamiltonii root extract.

PubMed

Rashmi, Venkatasubbaiah; Sanjay, Konasur R

2017-04-01

Consistent search of plants for green synthesis of silver nanoparticles (SNPs) is an important arena in Nanomedicine. This study focuses on synthesis of SNPs using bioreduction of silver nitrate (AgNO 3 ) by aqueous root extract of Decalepis hamiltonii . The biosynthesis of SNPs was monitored by UV-vis analysis at absorbance maxima 432 nm. The fluorescence emission spectra of SNPs illustrated the broad emission peak 450-483 nm at different excitation wavelengths. The surface characteristics were studied by scanning electron microscope and atomic force microscopy, showed spherical shape of SNPs and dynamic light scattering analysis confirmed the average particle size 32.5 nm and the presence of metallic silver was confirmed by energy dispersive X-ray. Face centred cubic structure with crystal size 33.3 nm was revealed by powder X-ray diffraction. Fourier transform infrared spectroscopy indicated the biomolecules involved in the reduction mainly polyols and phenols present in root extracts were found to be responsible for the synthesis of SNPs. The stability and charge on SNPs were revealed by zeta potential analysis. In addition, on therapeutic forum, the synthesised SNPs elicit antioxidant and antimicrobial activity against Bacillus cereus , Bacillus licheniformis , Escherichia coli , Pseudomonas aeruginosa and Staphylococcus aureus .

Cooperative upconversion luminescence in Tb{sup 3+}:Yb{sup 3+} co-doped Y{sub 2}SiO{sub 5} powders prepared by combustion synthesis

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

Rakov, Nikifor, E-mail: nikifor.gomez@univasf.edu.br; Vieira, Simone A.; Guimarães, Renato B.

2014-03-15

Frequency upconversion (UC) luminescence via cooperative energy transfer (CET) process between pairs of Yb{sup 3+} and Tb{sup 3+} ions was investigated in Tb{sup 3+}:Yb{sup 3+}:Y{sub 2}SiO{sub 5} crystalline ceramic powders prepared by combustion synthesis. Surface morphology and structure of the powders were investigated by scanning electronic microscopy and X-ray powder diffraction. Photoluminescence experiments were performed in Tb{sup 3+}-singly doped samples using ultraviolet light (λ=255 nm) and in Tb{sup 3+}:Yb{sup 3+} co-doped samples using a near-infrared (NIR) diode laser (λ=975 nm). Upon excitation with the NIR diode laser, UC luminescence with an intense emission band centered at ∼549 nm, corresponding tomore » the 4f intraband {sup 5}D{sub 4}→{sup 7}F{sub 5} transition of Tb{sup 3+}, along with less intense emission bands at ∼490, ∼590 and ∼620 nm, corresponding to other {sup 5}D{sub 4}→{sup 7}F{sub J} transitions, was detected. The CET rate was estimated by analyzing the dynamics of UC luminescence with rate equations model of the electronic populations. -- Graphical Abstract: Left: Cooperative upconversion luminescence spectra of three powder samples prepared by combustion synthesis. Right: The SEM image of the powder showing that it consists of agglomerated flake-like shaped particles of various sizes. Full scale bar is 20 μm. Highlights: • Yttrium orthosilicate (Y{sub 2}SiO{sub 5}) powders were prepared by combustion synthesis. • Cooperative upconversion is observed for the first time in Tb{sup 3+}–Yb{sup 3+} doped Y{sub 2}SiO{sub 5}. • Energy transfer and back-transfer rates between Tb{sup 3+} and Yb{sup 3+} pairs were estimated.« less

Crystallographic and magnetic properties of nanocrystalline perovskite structure SmFeO3 orthoferrite

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

As-synthesis of nanostructure AgCl/Ag/MCM-41 composite

NASA Astrophysics Data System (ADS)

Sohrabnezhad, Sh.; Pourahmad, A.

2012-02-01

In this work, we present the simple synthetic route for silver chloride/silver nanoparticles (AgCl/Ag-NPs) using as-synthesis method. The structure, composition and optical properties of such material were investigated by transmission electron microscopy (TEM), UV-visible diffuse reflectance spectroscopy (UV-vis DRS), X-ray diffraction (XRD) and FTIR. Powder X-ray diffraction showed that when AgNO 3 content is below 0.1 wt.% in synthetic gel, the guest AgCl/Ag-NPs is formed on the silica channel wall, and lower exists in the crystalline state. When AgNO 3 content exceeds this value, AgCl/Ag nanoparticles can be observed in high crystalline state. The absorption at 327 nm ascribed to the characteristic absorption of the AgCl semiconductor. Ag nanoparticles have been shown to exist in the nanocomposite at 375 nm. When AgNO 3 content is above 0.1 wt.% in synthetic gel, spectra exhibited stronger absorption at 450-700 nm that was attributed to the surface plasmonic resonance of silver nanoparticles. The obtained AgCl/Ag/MCM-41 sample exhibit enhanced photocatalytic activity for the degradation of methylene blue under visible-light irradiation.

Synthesis, Optical and Structural Properties of Copper Sulfide Nanocrystals from Single Molecule Precursors

PubMed Central

Ajibade, Peter A.; Botha, Nandipha L.

2017-01-01

We report the synthesis and structural studies of copper sulfide nanocrystals from copper (II) dithiocarbamate single molecule precursors. The precursors were thermolysed in hexadecylamine (HDA) to prepare HDA-capped CuS nanocrystals. The optical properties of the nanocrystals studied using UV–visible and photoluminescence spectroscopy showed absorption band edges at 287 nm that are blue shifted, and the photoluminescence spectra show emission curves that are red-shifted with respect to the absorption band edges. These shifts are as a result of the small crystallite sizes of the nanoparticles leading to quantum size effects. The structural studies were carried out using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and atomic force microscopy. The XRD patterns indicates that the CuS nanocrystals are in hexagonal covellite crystalline phases with estimated particles sizes of 17.3–18.6 nm. The TEM images showed particles with almost spherical or rod shapes, with average crystallite sizes of 3–9.8 nm. SEM images showed morphology with ball-like microspheres on the surfaces, and EDS spectra confirmed the presence of CuS nanoparticles. PMID:28336865

The stability of self-organized 1-nonanethiol-capped gold nanoparticle monolayer

NASA Astrophysics Data System (ADS)

Jiang, Peng; Xie, Si-shen; Yao, Jian-nian; Pang, Shi-jin; Gao, Hong-jun

2001-08-01

1-Nonanethiol-protected gold nanoparticles with the size of about 2 nm have been prepared by a wet chemical method through choosing a suitable ratio of Au:S (2.5:1). Size selective precipitation of nanoparticles has been used to narrow their size distribution, which facilitates the formation of an ordered nanoparticle close-packed structure. A Fourier transform infrared investigation provides the evidence of the encapsulation of Au nanoparticles by 1-nonanethiol while an ultraviolet-visible spectrum shows a broad absorption around 520 nm, corresponding to surface plasmon band of Au nanoparticles. X-ray photoelectron spectroscopy of the samples demonstrates the metallic state of the gold (Au0) and the existence of sulfur (S). The data from x-ray powder diffraction measurements confirm that the gold nanoparticles have the same face-centred cubic crystalline structure as the bulk gold phase. Finally, transmission electron microscopy (TEM) characterization indicates that the size of the monodisperse colloidal gold nanoparticles is about 2 nm and they can self-organize to form a two-dimensional hexagonal close-packed structure after evaporating a concentrated drop of nanoparticles-toluene solution on a carbon-coated TEM copper grid.

Structural and magnetic properties of sol-gel Co2xNi0.5-x Zn0.5-xFe2O4 thin films

NASA Astrophysics Data System (ADS)

Rebrov, Evgeny V.; Gao, Pengzhao; Verhoeven, Tiny M. W. G. M.; Schouten, Jaap C.; Kleismit, Richard; Turgut, Zafer; Kozlowski, Gregory

2011-03-01

Nanocrystalline Co2xNi0.5-xZn0.5-xFe2O4 (x=0-0.5) thin films have been synthesized with various grain sizes by a sol-gel method on polycrystalline silicon substrates. The morphology as well as magnetic and microwave absorption properties of the films calcined at 1073 K were studied using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. All films were uniform without microcracks. The Co content in the Co-Ni-Zn films resulted in a grain size ranging from 15 to 32 nm while it ranged from 33 to 49 nm in the corresponding powders. Saturation and remnant magnetization increased with increase in grain size, while coercivity demonstrated a drop due to multidomain behavior of crystallites for a given value of x. Saturation magnetization increased and remnant magnetization had a maximum as a function of grain size independent of x. In turn, coercivity increased with x independent of grain size. Complex permittivity of the Co-Ni-Zn ferrite films was measured in the frequency range 2-15 GHz. The highest hysteretic heating rate in the temperature range 315-355 K was observed in CoFe2O4. The maximum absorption band shifted from 13 to 11 GHz as cobalt content increased from x=0.1 to 0.2.

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

NASA Astrophysics Data System (ADS)

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

2013-03-01

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

Amorphous iron–chromium oxide nanoparticles with long-term stability

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

Iacob, Mihail; Institute of Chemistry of ASM, Academiei str. 3, Chisinau 2028, Republic of Moldova; Cazacu, Maria, E-mail: mcazacu@icmpp.ro

2015-05-15

Highlights: • Fe–Cr oxide nanoparticles with pre-established metals ratio were obtained. • The amorphous state and its long-term stability were highlighted by X-ray diffraction. • The average diameter of dried nanoparticles was 3.5 nm, as was estimated by TEM, AFM. • In hexane dispersion, nanoparticles with diameter in the range 2.33–4.85 nm were found. • Superparamagnetic state of NPs co-exists with diamagnetism of the organic layer. - Abstract: Iron–chromium nanoparticles (NPs) were obtained through the thermal decomposition of μ{sub 3}-oxo heterotrinuclear (FeCr{sub 2}O) acetate in the presence of sunflower oil and dodecylamine (DA) as surfactants. The average diameter of themore » NPs was 3.5 nm, as estimated on the basis of transmission electron microscopy and atomic force microscopy images. Both techniques revealed the formation of roughly approximated spheres with some irregularities and agglomerations in larger spherical assemblies of 50–100 nm. In hexane, NPs with diameters in the 2.33–4.85 nm range are individually dispersed, as emphasized by dynamic light scattering measurements. The amorphous nature of the product was emphasized by X-ray powder diffraction. The study of the magnetic properties shows the presence of superparamagnetic state of iron–chromium oxide NPs and the diamagnetic contribution from DA layer forming a shell of NPs.« less

X-ray absorption fine structure and X-ray excited optical luminescence studies of II-VI semiconducting nanostructures

NASA Astrophysics Data System (ADS)

Murphy, Michael Wayne

2010-06-01

Various II-VI semiconducting nanomaterials such as ZnO-ZnS nanoribbons (NRs), CdSxSe1-x nanostructures, ZnS:Mn NRs, ZnS:Mn,Eu nanoprsims (NPs), ZnO:Mn nanopowders, and ZnO:Co nanopowders were synthesized for study. These materials were characterized by techniques such as scanning electron microscopy, transmission electron microscopy, element dispersive X-ray spectroscopy, selected area electron diffraction, and X-ray diffraction. The electronic and optical properties of these nanomaterials were studied by X-ray absorption fine structure (XAFS) spectroscopy and X-ray excited optical luminescence (XEOL) techniques, using tuneable soft X-rays from a synchrotron light source. The complementary nature ofthe XAFS and XEOL techniques give site, element and chemical specific measurements which allow a better understanding of the interplay and role of each element in the system. Chemical vapour deposition (CVD) of ZnS powder in a limited oxygen environment resulted in side-by-side biaxial ZnO-ZnS NR heterostructures. The resulting NRs contained distinct wurtzite ZnS and wurtzite ZnO components with widths of 10--100 nm and 20 --500 nm, respectively and a uniform interface region of 5-15 nm. XAFS and XEOL measurements revealed the luminescence of ZnO-ZnS NRs is from the ZnO component. The luminescence of CdSxSe1-x nanostructures is shown to be dependent on the S to Se ratio, with the band-gap emission being tunable between that of pure CdS and CdSe. Excitation of the CdSxSe 1-x nanostructures by X-ray in XEOL has revealed new de-excitation channels which show a defect emission band not seen by laser excitation. CVD of Mn2+ doped ZnS results in nanostructures with luminescence dominated by the yellow Mn2+ emission due to energy transfer from the ZnS host to the Mn dopant sites. The addition of EuCl3 to the reactants in the CVD process results in a change in morphology from NR to NP. Zn1-xMnxO and Zn1-xCOxO nanopowders were prepared by sol-gel methods at dopant concentrations of 0, 1,3, and 10% and annealed at 400, 600 and 800°C in air. XAFS spectra show that low dopant concentrations and low processing temperatures limit the amount of secondary phase formation. The nanopowders did not show roomtemperature ferromagnetism and increased secondary phase formation increases the paramagnetic character of the hysteresis curves at 5°K. Keywords: X-ray absorption fine structures (XAFS), X-ray absorption near-edge structures (XANES), extended X-ray absorption fine structure (EXAFS), X-ray absorption spectroscopy(XAS), X-ray excited optical luminescence (XEOL), time-resolved, II-VI semiconductors, nanostructure, nanomaterial, nanoribbon, nanowire, nanopartic1e, heterostructure, ZnO, ZnS, ZnO-ZnS, CdS, CdSe, CdSSe, ZnO:Mn, ZnO:Co, ZnS:Mn, dilute magnetic semiconductor (DMS), dilute magnetic oxide (DMO), spintronics, magnetism, paramagnetism, ferromagnetism.

Synthesis of nanostructured vanadium powder by high-energy ball milling: X-ray diffraction and high-resolution electron microscopy characterization

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran

2016-10-01

Vanadium metal powders, ball milled with different surfactants viz., stearic acid, KCl and NaCl, have been studied by X-ray diffraction and transmission electron microscopy. The surfactants alter the microstructural and morphological characteristics of the powders. Ball milling with stearic acid results in solid-state amorphization, while powders milled with KCl yield vanadium-tungsten carbide nanocomposite mixtures. NaCl proved to be an excellent surfactant for obtaining nanostructured fusion-grade vanadium powders. In order to understand the reaction mechanism behind any interstitial addition in the ball-milled powders, CHNOS analysis was performed.

The development of latent fingerprints by zinc oxide and tin oxide nanoparticles prepared by precipitation technique

NASA Astrophysics Data System (ADS)

Luthra, Deepali; Kumar, Sacheen

2018-05-01

Fingerprints are the very important evidence at the crime scene which must be developed clearly with shortest duration of time to solve the case. Metal oxide nanoparticles could be the mean to develop the latent fingerprints. Zinc oxide and Tin Oxide Nanoparticles were prepared by using chemical precipitation technique which were dried and characterized by X-ray diffraction, UV-Visible spectroscopy and FTIR. The size of zinc oxide crystallite was found to be 14.75 nm with minimum reflectance at 360 nm whereas tin oxide have the size of 90 nm and reflectance at minimum level 321 nm. By using these powdered samples on glass, plastic and glossy cardboard, latent fingerprints were developed. Zinc oxide was found to be better candidate than tin oxide for the fingerprint development on all the three types of substrates.

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

DOE PAGES

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

2016-10-06

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

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

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

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

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

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

Nanostructured and layered lithium manganese oxide and method of manufacturing the same

NASA Technical Reports Server (NTRS)

Singhal, Amit (Inventor); Skandan, Ganesh (Inventor)

2005-01-01

Nanostructured and layered lithium manganese oxide powders and methods of producing same. The powders are represented by the chemical formula, LixMn1-yMyO2, where 0.5

Discovery of superluminal velocities of X-rays and Bharat Radiation challenging the validity of Einstein's formula E= mc2

NASA Astrophysics Data System (ADS)

Rao, M. A. Padmanabha

2013-09-01

The current paper reports discovery of superluminal velocities of X-rays, and Bharat Radiation in 12.87 to 31 nm range from solar spectra. The discovery challenges the 100 year old Albert Einstein's assertion that nothing can go faster than velocity of light c in vacuum while formulating E = mc2 in his special theory of relativity reported in 1905 [1]. Several solar spectra recorded at various wavelengths by Woods et al in 2011 demonstrated GOES X-rays arriving earlier than 13.5 nm emission, which in turn arriving earlier than 33.5 nm emission [2]. Finally, the investigators faced difficulty in concluding that short wavelengths traveled fast because of lack of information whether all the three emissions originated from the same source and at the same time. Very recently the author has reported GOES X-rays (7.0 nm) cause 13.5 nm (Bharat Radiation), which in turn causes 33.5 nm Extreme ultraviolet (EUV) emission from same excited atoms present in solar flare by Padmanabha Rao Effect [3, 4]. Based on these findings, the author succeeded in explaining how the solar spectral findings provide direct evidences on superluminal velocities of GOES X-ray and 13.5 nm Bharat Radiation emissions, when 33.5 nm EUV emission is considered travelling at velocity of light c. Among X-ray wavelengths, the short wavelength 7.0 nm X-rays traveled faster than 9.4 nm X-rays, while X-rays go at superluminal velocities. Among Bharat radiation wavelengths, short wavelengths showed fast travel, while Bharat Radiation goes at superluminal velocities as compared to 33.5 EUV emission.

Potential of Sm3+ doped LiSrVO4 nanophosphor to fill amber gap in LEDs

NASA Astrophysics Data System (ADS)

Biswas, P.; Kumar, Vinay; Sharma, Vishal; Bedyal, A. K.; Padha, Naresh; Swart, H. C.

2018-04-01

The LiSrVO4:Sm3+ phosphor powders were synthesized by the combustion method by varying the concentration of the Sm3+ ions from 0.25 mol% to 2.5 mol%. The powder X-ray diffraction (XRD) studies confirmed that the phosphors were crystallized as monoclinic structure belonging to space group P2/m and the transmission electron microscopy (TEM) revealed nanosized grains of the powders. The Fourier transform infrared studies (FTIR) established the formation of non-hygroscopic vanadate powders. The photoluminescence (PL) and diffused reflectance studies (DRS) were also carried out and discussed. Under 401 nm excitation, the optimized phosphor exhibited the characteristic 568, 600, 646 and 704 nm emissions of Sm3+ which corresponded to the orange-red (amber) color with (0.59, 0.41) Commission Internationale de' Eclairage (CIE) chromaticity coordinates. Concentration quenching of phosphor intensity on account of non-radiative energy transfer was ascribed to dipole-dipole interaction between activators. DRS study reveals that the host of the phosphor is a wide bandgap material which accommodates the dopant successfully. The present results signify that the LiSrVO4:Sm3+ phosphor can suitably be excited by the GaN family of UV-LEDs chips for efficient amber LEDs applications.

Formation and morphology of Zn(2)Ti(3)O(8) powders using hydrothermal process without dispersant agent or mineralizer.

PubMed

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-28

Synthesis of Zn(2)Ti(3)O(8) powders for attenuating UVA using TiCl(4), Zn(NO(3))(2)·6H(2)O and NH(4)OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO(2) and Zn(2)Ti(3)O(8) coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn(2)TiO(4), rutile TiO(2) and ZnTiO(3). Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO(3) crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent.

Formation and Morphology of Zn2Ti3O8 Powders Using Hydrothermal Process without Dispersant Agent or Mineralizer

PubMed Central

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-01

Synthesis of Zn2Ti3O8 powders for attenuating UVA using TiCl4, Zn(NO3)2·6H2O and NH4OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO2 and Zn2Ti3O8 coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn2TiO4, rutile TiO2 and ZnTiO3. Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO3 crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent. PMID:21541035

Synthesis of fluorapatite–hydroxyapatite nanoparticles and toxicity investigations

PubMed Central

Montazeri, N; Jahandideh, R; Biazar, Esmaeil

2011-01-01

In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca10(PO4)6F2) and hydroxyapatite (HA; Ca10(PO4)6(OH)2), were prepared using the solgel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatibile and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering. PMID:21499417

Magnetic enhancement and coding in mechanosynthesized Ni{sub 0.3}Zn{sub 0.7}Fe{sub 2}O{sub 4} nanoparticles

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

Majumder, S.; Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata-700064; Dey, S.

2015-06-24

The nanosized Ni{sub 0.3}Zn{sub 0.7}Fe{sub 2}O{sub 4} (∼ 15 nm) has been synthesized by high energy ball milling of the bulk powder sample. The sample has been characterized by powder x-ray diffraction, field emission and transmission electron microscopic and dc magnetic measurement techniques. The dc magnetic measurement on the sample indicates that the sample exhibit enhancement of magnetization compared to its counterparts synthesized by chemical methods. Moreover, the system stores the memory of either decrease or increase of magnetic field enabling a magnetic coding of “0” and “1” which can be profitably used in magnetic storage and sensing devices.

Plasma induced sp 2 to sp 3 transition in boron nitride

NASA Astrophysics Data System (ADS)

Zhang, J.; Cui, Q.; Li, X.; He, Z.; Li, W.; Ma, Y.; Guan, Q.; Gao, W.; Zou, G.

2004-12-01

The transition from sp 2 to sp 3 hybridization in boron nitride has been induced in plasma. Nano-crystals of cubic boron nitride (cBN) have been synthesized by direct current arc discharge method using hexagonal boron nitride (hBN) as the starting material. The characterization of the as-grown powders is carried out by X-ray diffraction, Fourier transform infrared spectroscopy and transmission electron microscopy. It has been shown that cBN and hBN grains with 20-60 nm in size co-exist in the powders. A reaction route of sublimation - re-hybridization - crystallization had been put forward to explain the mechanism of the hybridization transition and the growth of cBN by this method.

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

Pathak, A. A., E-mail: anuapathak@yahoo.com; Yadav, P. J.; Talewar, R. A.

Blue-emitting phosphor LaMgAl{sub 11}O{sub 19}:Eu{sup 2+} has been synthesized successfully at 500 °C by one step combustion synthesis method. The as-synthesized materials were characterized by powder x-ray diffraction (XRD) and photoluminescence (PL) techniques. Upon 365 nm excitation, emission spectra of the LaMgAl{sub 11}O{sub 19}:Eu{sup 2+} phosphors show a blue band at 450 nm. The excitation spectra corresponding to 4f{sup 7}-4f{sup 6}5d transition of Eu{sup 2+} cover the spectral range of 280–430 nm. The concentration quenching of Eu{sup 2+} in the LaMgAl{sub 11}O{sub 19} host was determined to be 3 mol%. The CIE chromaticity of LAM: Eu{sup 2+} phosphors was compared with the commercial BAM.

Thermoluminescent properties of ZnS:Mn nanocrystalline powders.

PubMed

Ortiz-Hernández, Arturo Agustín; Méndez García, Víctor Hugo; Pérez Arrieta, María Leticia; Ortega Sígala, José Juan; Araiza Ibarra, José de Jesús; Vega-Carrillo, Héctor Rene; Falcony Guajardo, Ciro

2015-05-01

Thermoluminescent ZnS nanocrystals doped with Mn(2+) ions were synthesized by chemical co-precipitation method. From X-ray diffraction studies it was observed that the synthesized nanoparticles have cubic zinc blende structure with average sizes of about 40-50nm. Morphology was analyzed by TEM. Photoluminescence studies showed two transitions, one of them close to 396nm and other close to 598nm, which is enhanced with increasing dopant concentration, this behavior was also observed in the cathodoluminescence spectrum. The thermoluminescence gamma dose-response has linear behavior over dose range 5-100mGy, the glow curve structure shows two glow peaks at 436K and at 518K that were taken into account to calculate the kinetic parameters using the Computerized Glow Curve Deconvolution procedure. Copyright © 2015 Elsevier Ltd. All rights reserved.

Environment friendly route of iron oxide nanoparticles from Zingiber officinale (ginger) root extract

NASA Astrophysics Data System (ADS)

Xin Hui, Yau; Yi Peng, Teoh; Wei Wen, Liu; Zhong Xian, Ooi; Peck Loo, Kiew

2016-11-01

Iron oxide nanoparticles were prepared from the reaction between the Zingiber officinale (ginger) root extracts and ferric chloride solution at 50°C for 2 h in mild stirring condition. The synthesized powder forms of nanoparticles were further characterized by using UV-Vis spectroscopy and X-ray Diffraction spectrometry. UV-Vis analysis shows the absorption peak of iron oxide nanoparticles is appeared at 370 nm. The calculation of crystallite size from the XRD showed that the average particle size of iron oxide nanoparticles was 68.43 nm. Therefore, this eco-friendly technique is low cost and large scale nanoparticles synthesis to fulfill the demand of various applications.

In situ hydrothermal syntheses, structures and photoluminescent properties of four novel metal-organic frameworks constructed by lanthanide (Ln=Ce(III), Pr(III), Eu(III)) and Cu(I) metals with flexible dicarboxylate acids and piperazine-based ligands

NASA Astrophysics Data System (ADS)

Ay, Burak; Karaca, Serkan; Yildiz, Emel; Lopez, Valerie; Nanao, Max H.; Zubieta, Jon

2016-01-01

Four novel metal-organic frameworks,[Cu2Cl2(pyrz)]n (1) and (H2pip)n[Ln2(pydc)4(H2O)2]n (Ln=Ce (2), Pr (3) and Eu (4), H2pzdc=2,3-pyrazinedicarboxylic acid, pyrz=pyrazine, H2pydc=2,6-pyridinedicarboxylic acid, H2pip=piperazine) have been synthesized under hydrothermal conditions and characterized by the elemental analysis, ICP, Far IR (FIR), FT-IR spectra, TGA, single crystal X-ray diffraction analysis and powder X-ray diffraction (PXRD). Compound 1 is two-dimensional containing Cl-Cu-Cl sites, while the lanthanide complexes contain one-dimensional infinite Ln-O-Ln chains. All the complexes show high thermal stability. The complexes 1-3 exhibit luminescence emission bands at 584, 598 and 614 nm at room temperature when excited at 300 nm. Complex 4 exhibits bright red solid-state phosphorescence upon exposure to UV radiation at room temperature.

Highly selective electrodeposition of sub-10 nm crystalline noble metallic nanorods inside vertically aligned multiwall carbon nanotubes.

PubMed

Wang, Xuyang; Wang, Ranran; Wu, Qiang; Zhang, Xiaohua; Yang, Zhaohui; Guo, Jun; Chen, Muzi; Tang, Minghua; Cheng, Yajun; Chu, Haibin

2016-07-08

In this paper crystalline noble metallic nanorods including Au and Ag with sub-10 nm diameter, are encapsulated within prealigned and open-ended multiwall carbon nanotubes (MWCNTs) through an electrodeposition method. As the external surface of CNTs has been insulated by the epoxy the CNT channel becomes the only path for the mass transport as well as the nanoreactor for the metal deposition. Highly crystallized Au and Ag2O nanorods parallel to the radial direction of CNTs are confirmed by high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy and x-ray powder diffraction spectroscopy. The Ag2O nanorods are formed by air oxidation on the Ag metals and show a single crystalline structure with (111) planes. The Au nanorods exhibit a complex crystalline structure including twin-crystal and lattice dislocation with (111) and (200) planes. These crystalline noble metallic nanostructures may have important applications for nanocatalysts for fuel cells as well as nanoelectronic and nanophotonic devices. This method is deemed to benefit the precise deposition of other crystalline nanostructures inside CNTs with a small diameter.

Highly selective electrodeposition of sub-10 nm crystalline noble metallic nanorods inside vertically aligned multiwall carbon nanotubes

NASA Astrophysics Data System (ADS)

Wang, Xuyang; Wang, Ranran; Wu, Qiang; Zhang, Xiaohua; Yang, Zhaohui; Guo, Jun; Chen, Muzi; Tang, Minghua; Cheng, Yajun; Chu, Haibin

2016-07-01

In this paper crystalline noble metallic nanorods including Au and Ag with sub-10 nm diameter, are encapsulated within prealigned and open-ended multiwall carbon nanotubes (MWCNTs) through an electrodeposition method. As the external surface of CNTs has been insulated by the epoxy the CNT channel becomes the only path for the mass transport as well as the nanoreactor for the metal deposition. Highly crystallized Au and Ag2O nanorods parallel to the radial direction of CNTs are confirmed by high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy and x-ray powder diffraction spectroscopy. The Ag2O nanorods are formed by air oxidation on the Ag metals and show a single crystalline structure with (111) planes. The Au nanorods exhibit a complex crystalline structure including twin-crystal and lattice dislocation with (111) and (200) planes. These crystalline noble metallic nanostructures may have important applications for nanocatalysts for fuel cells as well as nanoelectronic and nanophotonic devices. This method is deemed to benefit the precise deposition of other crystalline nanostructures inside CNTs with a small diameter.

Synthesis and characterization of metastable, 20 nm-sized Pna21-LiCoPO4 nanospheres

NASA Astrophysics Data System (ADS)

Ludwig, Jennifer; Nordlund, Dennis; Doeff, Marca M.; Nilges, Tom

2017-04-01

The majority of research activities on LiCoPO4 are focused on the phospho-olivine (space group Pnma), which is a promising high-voltage cathode material for Li-ion batteries. In contrast, comparably little is known about its metastable Pna21 modification. Herein, we present a comprehensive study on the structure-property relationships of 15-20 nm Pna21-LiCoPO4 nanospheres prepared by a simple microwave-assisted solvothermal process. Unlike previous reports, the results indicate that the compound is non-stoichiometric and shows cation-mixing with Co ions on the Li sites, which provides an explanation for the poor electrochemical performance. Co L2,3-edge X-ray absorption spectroscopic data confirm the local tetrahedral symmetry of Co2+. Comprehensive studies on the thermal stability using thermogravimetric analysis, differential scanning calorimetry, and in situ powder X-ray diffraction show an exothermic phase transition to olivine Pnma-LiCoPO4 at 527 °C. The influence of the atmosphere and the particle size on the thermal stability is also investigated.

Facile synthesis of high-temperature (1000 °C) phase-stable rice-like anatase TiO2 nanocrystals

NASA Astrophysics Data System (ADS)

Lv, Lizhen; Chen, Qirong; Liu, Xiuyun; Wang, Miaomiao; Meng, Xiangfu

2015-05-01

High-temperature phase-stable rice-like anatase TiO2 nanocrystals were synthesized by one-pot solvothermal method using soluble titania xerogel and isopropyl alcohol (IPA) as the precursor and the solvent, respectively. Sample characterization was carried out by powder X-ray diffraction, high-resolution transmission electron microscopy, field emission scanning electron microscope, X-ray photoelectron spectroscopy, and N2 adsorption-desorption isotherms. The results showed that TiO2 nanocrystals had rice-like shapes with an average size of 5 nm in width and 35 nm in length. The BET surface area was 153 m2/g. Unexpectedly, the rice-like TiO2 nanocrystals exhibited high-temperature phase stability, which could remain as pure anatase phase after calcinations at 1000 °C. Growth mechanism investigation revealed that the IPA solvent played a key role in nucleation and growth of rice-like anatase TiO2 nanocrystals. The photodegradation of rhodamine B demonstrated that rice-like anatase TiO2 nanocrystals exhibited enhanced photocatalytic activity under visible light irradiation.

Critical size of crystalline ZrO(2) nanoparticles synthesized in near- and supercritical water and supercritical isopropyl alcohol.

PubMed

Becker, Jacob; Hald, Peter; Bremholm, Martin; Pedersen, Jan S; Chevallier, Jacques; Iversen, Steen B; Iversen, Bo B

2008-05-01

Nanocrystalline ZrO(2) samples with narrow size distributions and mean particle sizes below 10 nm have been synthesized in a continuous flow reactor in near and supercritical water as well as supercritical isopropyl alcohol using a wide range of temperatures, pressures, concentrations and precursors. The samples were comprehensively characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), and small-angle X-ray scattering (SAXS), and the influence of the synthesis parameters on the particle size, particle size distribution, shape, aggregation and crystallinity was studied. On the basis of the choice of synthesis parameters either monoclinic or tetragonal zirconia phases can be obtained. The results suggest a critical particle size of 5-6 nm for nanocrystalline monoclinic ZrO(2) under the present conditions, which is smaller than estimates reported in the literature. Thus, very small monoclinic ZrO(2) particles can be obtained using a continuous flow reactor. This is an important result with respect to improvement of the catalytic properties of nanocrystalline ZrO(2).

Immobilized TiO2 nanoparticles produced by flame spray for photocatalytic water remediation

NASA Astrophysics Data System (ADS)

Bettini, Luca Giacomo; Diamanti, Maria Vittoria; Sansotera, Maurizio; Pedeferri, Maria Pia; Navarrini, Walter; Milani, Paolo

2016-08-01

Anatase/rutile mixed-phase titanium dioxide (TiO2) photocatalysts in the form of nanostructured powders with different primary particle size, specific surface area, and rutile content were produced from the gas-phase by flame spray pyrolysis (FSP) starting from an organic solution containing titanium (IV) isopropoxide as Ti precursor. Flame spray-produced TiO2 powders were characterized by means of X-ray diffraction, Raman spectroscopy, and BET measurements. As-prepared powders were mainly composed of anatase crystallites with size ranging from 7 to 15 nm according to the synthesis conditions. TiO2 powders were embedded in a multilayered fluoropolymeric matrix to immobilize the nanoparticles into freestanding photocatalytic membranes. The photocatalytic activity of the TiO2-embedded membranes toward the abatement of hydrosoluble organic pollutants was evaluated employing the photodegradation of rhodamine B in aqueous solution as test reaction. The photoabatement rate of best performing membranes significantly overcomes that of membranes produced by the same method and incorporating commercial P25-TiO2.

Effect of annealing on the structural and optical properties of TiO2 powder prepared by sol-gel route

NASA Astrophysics Data System (ADS)

Halder, Nilanjan; Misra, Kamakhya Prakash

2016-05-01

Using titanium isopropoxide as the precursor, Titanium dioxide (TiO2) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO2 samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increase with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO2 nano powder samples.

Gold nanoparticles interacting with β-cyclodextrin-phenylethylamine inclusion complex: a ternary system for photothermal drug release.

PubMed

Sierpe, Rodrigo; Lang, Erika; Jara, Paul; Guerrero, Ariel R; Chornik, Boris; Kogan, Marcelo J; Yutronic, Nicolás

2015-07-22

We report the synthesis of a 1:1 β-cyclodextrin-phenylethylamine (βCD-PhEA) inclusion complex (IC) and the adhesion of gold nanoparticles (AuNPs) onto microcrystals of this complex, which forms a ternary system. The formation of the IC was confirmed by powder X-ray diffraction and NMR analyses ((1)H and ROESY). The stability constant of the IC (760 M(-1)) was determined using the phase solubility method. The adhesion of AuNPs was obtained using the magnetron sputtering technique, and the presence of AuNPs was confirmed using UV-vis spectroscopy (surface plasmon resonance effect), which showed an absorbance at 533 nm. The powder X-ray diffractograms of βCD-PhEA were similar to those of the crystals decorated with AuNPs. A comparison of the one- and two-dimensional NMR spectra of the IC with and without AuNPs suggests partial displacement of the guest to the outside of the βCD due to attraction toward AuNPs, a characteristic tropism effect. The size, morphology, and distribution of the AuNPs were analyzed using TEM and SEM. The average size of the AuNPs was 14 nm. Changes in the IR and Raman spectra were attributed to the formation of the complex and to the specific interactions of this group with the AuNPs. Laser irradiation assays show that the ternary system βCD-PhEA-AuNPs in solution enables the release of the guest.

Comparative study of proteasome inhibitory, synergistic antibacterial, synergistic anticandidal, and antioxidant activities of gold nanoparticles biosynthesized using fruit waste materials

PubMed Central

Patra, Jayanta Kumar; Baek, Kwang-Hyun

2016-01-01

The aim of this study was to compare the biological synthesis of gold nanoparticles (AuNPs) generated using the aqueous extracts of outer oriental melon peel (OMP) and peach. The synthesized OMP-AuNPs and peach extract (PE)-AuNPs were characterized by ultraviolet–visible spectroscopy, field emission scanning electron microscopy, energy dispersive X-ray analysis, X-ray powder diffraction, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The surface plasmon resonance spectra were obtained at 545 nm and 540 nm for OMP-AuNPs and PE-AuNPs, respectively. The estimated absolute crystallite size of the synthesized AuNPs was calculated to be 78.11 nm for OMP-AuNPs and 39.90 nm for PE-AuNPs based on the Scherer equation of the X-ray powder diffraction peaks. Fourier transform infrared spectroscopy results revealed the involvement of bioactive compounds present in OMP and peach extracts in the synthesis and stabilization of synthesized AuNPs. Both the OMP-AuNPs and PE-AuNPs showed a strong antibacterial synergistic activity when combined with kanamycin (9.38–20.45 mm inhibition zones) and rifampicin (9.52–25.23 mm inhibition zones), and they also exerted a strong synergistic anticandidal activity (10.09–15.47 mm inhibition zones) when combined with amphotericin B against five pathogenic Candida species. Both the OMP-AuNPs and PE-AuNPs exhibited a strong antioxidant potential in terms of 1,1-diphenyl-2-picrylhydraxyl radical scavenging, nitric oxide scavenging, 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) radical scavenging, and a reducing power, along with a strong proteasome inhibitory potential that could be useful in cancer drug delivery and cancer treatments. The PE-AuNPs showed comparatively higher activity than OMP-AuNPs, which could be attributed to the presence of rich bioactive compounds in the PE that acted as reducing and capping agents in the synthesis of PE-AuNPs. Overall, the results of the current investigation highlighted a novel green technology for the synthesis of AuNPs using food waste materials and their potential applications in the biomedical, pharmaceutical, and cosmetic industries. PMID:27695326

Phase modification of copper phthalocyanine semiconductor by converting powder to thin film

NASA Astrophysics Data System (ADS)

Ai, Xiaowei; Lin, Jiaxin; Chang, Yufang; Zhou, Lianqun; Zhang, Xianmin; Qin, Gaowu

2018-01-01

Thin films of copper phthalocyanine (CuPc) semiconductor were deposited on glass substrates by a thermal evaporation system using the CuPc powder in a high vacuum. The crystal structures of both the films and the powder were measured by the X-ray diffraction spectroscopy technique. It is observed that CuPc films only show one peak at 6.84°, indicating a high texture of α phase along (200) orientation. In comparison, CuPc powder shows a series of peaks, which are confirmed from the mixture of both α and β phases. The effects of substrate anneal temperature on the film structure, grain size and optical absorption property of CuPc films were also investigated. All the films are of α phase and the full width of half maximum for (200) diffraction peak becomes narrow with increasing the substrate temperatures. The average grain size calculated by the Scherrer's formula is 33.63 nm for the film without anneal, which is increased up to 58.29 nm for the film annealed at 200 °C. Scanning electron microscope was further measured to prove the growth of crystalline grain and to characterize the morphologies of CuPc films. Ultraviolet-visible absorption spectra were employed to study the structure effect on the optical properties of both CuPc films and powder. Fourier Transform infrared spectroscopy was used to identify the crystalline nature of both CuPc powder and film.

Synthesis and characterization of CoFe2O4/polyaniline nanocomposites for electromagnetic interference applications.

PubMed

Praveena, K; Srinath, S

2014-06-01

The Cobalt ferrite (CoFe2O4) powders were synthesized by Co-precipitation method. The as prepared ferrite powders were incorporated into a polyaniline matrix at various volumetric ratios. The as prepared composites of ferrite and polyaniline powders were characterized using X-ray diffraction (XRD), transmission electron microscope (TEM). The particle size of CoFe2O4 is found to be 20 nm. The saturation magnetization (M(s)) of all the composites was found to be decreasing with decrease of ferrite content, while coercivity (H(c)) remained at the value corresponding to pure cobalt ferrite nanopowders. The complex permittivity (epsilon' and epsilon") and permeability (mu' and mu") of composite samples were measured in the range of 1 MHz to 1.1 GHz. The value of epsilon' and mu' found to be increased with ferrite volume concentration.

Low cost synthesis of TiO2-C nanocomposite powder for high efficiency visible light photocatalysis

NASA Astrophysics Data System (ADS)

Mohapatra, A. K.; Nayak, J.

2018-04-01

Titanium dioxide-carbon nanocomposite powder was synthesized via a low cost chemical route using oleic acid and titanium tetra-isopropoxide. Since the carbon remained mainly on the surface of the TiO2 nanoparticles, the powder had black color. The composition of the powder was analyzed by X-ray photoelectron spectroscopy and the structure was studied with X-ray diffraction and transmission electron microscopy. The visible photocatalytic activity of the black TiO2 powder was investigated by studying the photo-bleaching of methylene blue under visible light. Our experimental observation showed that the black-TiO2 powder had a higher visible photocatalytic activity compared to the commercial TiO2 powder (P25 Degussa).

X-ray structural investigation of nonsymmetrically and symmetrically alkylated [1]benzothieno[3,2-b]benzothiophene derivatives in bulk and thin films.

PubMed

Gbabode, Gabin; Dohr, Michael; Niebel, Claude; Balandier, Jean-Yves; Ruzié, Christian; Négrier, Philippe; Mondieig, Denise; Geerts, Yves H; Resel, Roland; Sferrazza, Michele

2014-08-27

A detailed structural study of the bulk and thin film phases observed for two potential high-performance organic semiconductors has been carried out. The molecules are based on [1]benzothieno[3,2-b]benzothiophene (BTBT) as conjugated core and octyl side groups, which are anchored either symmetrically at both sides of the BTBT core (C8-BTBT-C8) or nonsymmetrically at one side only (C8-BTBT). Thin films of different thickness (8-85 nm) have been prepared by spin-coating for both systems and analyzed by combining specular and grazing incidence X-ray diffraction. In the case of C8-BTBT-C8, the known crystal structure obtained from single-crystal investigations is observed within all thin films, down to a film thickness of 9 nm. In the case of C8-BTBT, the crystal structure of the bulk phase has been determined from X-ray powder diffraction data with a consistent matching of experimental and calculated X-ray diffraction patterns (Rwp = 5.8%). The packing arrangement of C8-BTBT is similar to that of C8-BTBT-C8, that is, consisting of a lamellar structure with molecules arranged in a "herringbone" fashion, yet with lamellae composed of two head-to-head (or tail-to-tail as the structure is periodic) superimposed molecules instead of only one molecule for C8-BTBT-C8. As for C8-BTBT-C8, we demonstrate that the same phase is observed in bulk and thin films for C8-BTBT whatever the film thickness investigated.

A novel contrast agent with rare earth-doped up-conversion luminescence and Gd-DTPA magnetic resonance properties

NASA Astrophysics Data System (ADS)

Lu, Qing; Wei, Daixu; Cheng, Jiejun; Xu, Jianrong; Zhu, Jun

2012-08-01

The magnetic-luminescent multifunctional nanoparticles based on Gd-DTPA and NaYF4:Yb, Er were successfully synthesized by the conjugation of activated DTPA and silica-coated/surface-aminolated NaYF4:Yb, Er nanoparticles through EDC/NHS coupling chemistry. The as-prepared products were characterized by powder X-ray diffraction, transmission electron microscopy, dynamic light scattering, energy dispersive X-ray analysis, and fourier transform infrared spectrometry. The room-temperature upconversion luminescent spectra and T1-weighted maps of the obtained nanoparticles were carried out by 980 nm NIR light excitation and a 3T MR imaging scanner, respectively. The results indicated that the as-synthesized multifunctional nanoparticles with small size, highly solubility in water, and both high MR relaxivities and upconversion luminescence may have potential usage for MR imaging in future.

Investigation on the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ manganites

NASA Astrophysics Data System (ADS)

Arun, B.; Athira, M.; Akshay, V. R.; Sudakshina, B.; Mutta, Geeta R.; Vasundhara, M.

2018-02-01

We have investigated the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ Perovskite manganites. Rietveld refinement of the X-ray powder diffraction patterns confirms that all the studied compounds have crystallized into an orthorhombic structure with Pbnm space group. Transmission electron microscopy analysis reveals nanocrystalline compounds with crystallite size less than 50 nm. The selected area electron diffraction patterns reveal the highly crystalline nature of the compounds and energy dispersive X-ray spectroscopic analysis shows that the obtained compositions are nearly identical with the nominal one. The oxygen stoichiometry is estimated by iodometric titration method and stoichiometric compositions are confirmed by X-ray Fluorescence Spectrometry analysis. A large bifurcation is observed in the ZFC/FC curves and Arrott plots not show a linear relation but have a convex curvature nature. The temperature dependence of inverse magnetic susceptibility at higher temperature confirms the existence of ferromagnetic clusters. The experimental results reveal that the reduction of crystallite size to nano metric scale in Pr-deficient manganites adversely influences structural, magnetic and magnetocaloric properties as compared to its bulk counterparts reported earlier.

A Direct Ultrasound Irradiation Method Synthesis of Monodisperse ZnO Microspheres for Varistors Ceramics Application

NASA Astrophysics Data System (ADS)

Chen, Tao; Wang, Mao-Hua; Zhang, Han-Ping; Liu, Jin-Ran; Yao, Da-Chuan

2016-08-01

Monodisperse and uniform ZnO microspheres were synthesized via an ultrasound irradiation method. The microstructure and morphology of the as-prepared sample were characterized by x-ray powder diffraction, Fourier transformation infrared spectra and scanning electron microscopy. The results indicate that the size of ZnO microspheres was strongly affected by the Zn(NO3)2·6H2O. As the amount of the precursor increased, the diameters of the ZnO microspheres can be turned from ˜500 nm to ˜2 μm. The electrical properties of the varistors ceramics prepared from the as-obtained ZnO powders were investigated. The results show that the varistors ceramics made from ZnO with a size of ˜500 nm and sintered in air at 1150°C for 2 h possess a density of 5.50 g/cm3 corresponding to 95.1% of the theoretical density, with breakdown voltage of 280.9 V/mm and nonlinear coefficient of ˜61.3.

Spectral downshifting from blue to near infer red region in Ce3+-Nd3+ co-doped YAG phosphor

NASA Astrophysics Data System (ADS)

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

2016-07-01

The YAG phosphors co-doped with Ce3+-Nd3+ ions by varying concentration of Nd3+ ion from 1 mol% to 15 mol% were successfully synthesized by conventional solid state reaction method. The phosphors were characterized by powder X-ray powder diffraction (XRD) and surface morphology was studied by scanning electronic microscope (SEM). The photoluminescence (PL) properties were studied in near infra red (NIR) and ultra violet visible (UV-VIS) region. The synthesized phosphors can convert a blue region photon (453 nm) into photons of NIR region (1063 nm). The energy transfer (ET) process was studied by time decay curve and PL spectra. The theoretical value of energy transfer efficiency (ETE) was calculated from time decay luminescence measurement and the maximum efficiency approached up to 82.23%. Hence this phosphor could be prime candidate as a downshifting (DS) luminescent convertor (phosphor) in front of crystalline silicon solar cell (c-Si) panels to reduce thermalization loss in the solar cells.

Synthesis, crystal growth and characterization of a phase matchable nonlinear optical single crystal: p-chloro dibenzylideneacetone

NASA Astrophysics Data System (ADS)

Ravindra, H. J.; John Kiran, A.; Nooji, Satheesha Rai; Dharmaprakash, S. M.; Chandrasekharan, K.; Kalluraya, Balakrishna; Rotermund, Fabian

2008-05-01

Good quality single crystals of p-chloro dibenzylideneacetone (CDBA) of size 13 mm×8 mm×2 mm were grown by slow evaporation solution growth technique. The grown crystals were confirmed by elemental analysis, Fourier transform infrared (FTIR) analysis and single crystal X-ray diffraction techniques. From the thermo gravimetric/differential thermal (TG/DT) analysis, the CDBA was found to be thermally stable up to 250 °C. The mechanical stability of the crystal is comparable with that of the other reported chalcones. The lower optical cut-off wavelength for this crystal was observed at 440 nm. The laser damage threshold of the crystal was 0.6 GW/cm 2 at 532 nm. The second harmonic generation conversion efficiency of the powder sample of CDBA was found to be 4.5 times greater than that of urea. We also demonstrate the existence of the phase matching property in this crystal using Kurtz powder technique.

Effect of the temperature on structural and optical properties of zinc oxide nanoparticles.

PubMed

Hadia, N M A; García-Granda, Santiago; García, José R

2014-07-01

Zinc nitrate hexahydrate, Zn(NO3)2 x 6H2O was used as a precursor with urea NH2CONH2 to prepare hydrozincite Zn5(CO3)2(OH)6 powder using hydrothermal method for 8 h at 90 degrees C. Zinc oxide (ZnO) nanoparticles (NPs) were prepared by thermal annealing of hydrozincite powder at different annealing temperatures, i.e., 350, 550 750 and 950 degrees C in air for 2 h. The resulting materials were characterized by X-ray diffraction, scanning electron microscopy (SEM) and thermal gravimetric analysis (TGA). The optical properties of the products were characterized by Fourier transform infrared spectroscopy (FT-IR), UV-Vis spectroscopy and photoluminescence (PL) spectra. It was found that the particle size increased from - 33 to 250 nm with increasing in the annealing temperatures. FTIR results showed that the standard peaks of zinc oxide were presented at 428.17 and 532.32 cm(-1). Thermal analysis study showed that the primary weight loss starts at - 93 degrees C is due to solvent evaporation. The secondary weight loss, observed at - 378 degrees C, is due to phase transition from hydrated zinc oxide to zinc oxide. The band gaps of the products were in the range - 3.26-3.30 eV. The PL spectrum showed that the as-synthesized ZnO nanoparticles had UV (381 nm) and green (537 nm) emissions.

Effect of Cu2+ substitution on the structural, optical and magnetic behaviour ofchemically derived manganese ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Vasuki, G.; Balu, T.

2018-06-01

Mixed spinel copper manganese ferrite (CuXMn1‑XFe2O4, X = 0, 0.25, 0.5, 0.75, 1) nanoparticles were synthesized by chemical co-precipitation technique. From the powder x-ray diffraction analysis the lattice constant, volume of unit cell, x-ray density, hopping lengths, crystallite size, surface area, dislocation density and microstrain were calculated. The substitution of Cu2+ ions shows a considerable reduction in the crystallite size of manganese ferrite from 34 nm to 22 nm. Further a linear fit of Williamson-Hall plot has been drawn to determine the microstrain and crystallite size. The crystallite size and morphology were further observed through high resolution transmission electron microscope and scanning electron microscope. The diffraction rings observed from selected area electron diffraction pattern exhibits the crystalline nature of all the samples. The energy dispersive x-ray analysis shows the composition of all the elements incorporated in the synthesized nanomaterials. FTIR studies reveal the absorption peaks that correspond to the metal-oxygen vibrations in the tetrahedral and octahedral sites. From the UV–vis absorption spectra the band gap energy, refractive index and optical dielectric constant were determined. Magnetic studies carried out using vibrating sample magnetometer shows interesting behaviour in the variation of magnetisation and coercivity. Peculiar magnetic behaviour is observed when Cu2+ ions are substituted in manganese ferrites. All the synthesized materials have very low value of squareness ratio which attributes to the superparamagnetic behaviour.

Atmospheric plasma sprayed (APS) coatings of Al2O3-TiO2 system for photocatalytic application.

PubMed

Stengl, V; Ageorges, H; Ctibor, P; Murafa, N

2009-05-01

The goal of this study is to examine the photocatalytic ability of coatings produced by atmospheric plasma spraying (APS). The plasma gun used is a common gas-stabilized plasma gun (GSP) working with a d.c. current and a mixture of argon and hydrogen as plasma-forming gas. The TiO(2) powders are particles of about 100 nm which were agglomerated to a mean size of about 55 mum, suitable for spraying. Composition of the commercial powder is 13 wt% of TiO(2) in Al(2)O(3), whereas also in-house prepared powder with the same nominal composition but with agglomerated TiO(2) and conventional fused and crushed Al(2)O(3) was sprayed. The feedstock materials used for this purpose are alpha-alumina and anatase titanium dioxide. The coatings are analyzed by scanning electron microscopy (SEM), energy dispersion probe (EDS) and X-ray diffraction. Photocatalytic degradation of acetone is quantified for various coatings. All plasma sprayed coatings show a lamellar structure on cross section, as typical for this process. Anatase titania from feedstock powder is converted into rutile titania and alpha-alumina partly to gamma-alumina. Coatings are proven to catalyse the acetone decomposition when irradiated by UV rays.

Growth, structural, thermal, linear and nonlinear optical and laser damage threshold studies of picolinium tartrate monohydrate single crystals.

PubMed

Peramaiyan, G; Pandi, P; Sornamurthy, B M; Bhagavannarayana, G; Mohan Kumar, R

2012-09-01

Picolinium tartrate monohydrate (PTM), a novel organic nonlinear optical material was synthesized and bulk crystals were grown from aqueous solution by slow cooling technique. The cell parameters of the grown crystal were found by single and powder X-ray diffraction analyses. The crystalline perfection of the grown crystals has been analyzed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. The presence of functional groups in the grown crystal was identified by FTIR and FT-Raman spectral analyses. UV-Vis spectral studies reveal PTM crystals are transparent in the wavelength region of 295-1100 nm. The thermal characteristics of PTM were analyzed by TGA/DTA studies. The dielectric and mechanical behaviours of PTM crystals were investigated. Dislocation density was estimated to be 2.89 × 10(3) cm(-2) on the flat-surface of PTM crystals from the etching studies. The laser induced surface damage threshold for the grown crystal was measured using Nd:YAG laser. Its second harmonic generation relative efficiency was measured by Kurtz and Perry powder technique and was observed to be comparable with KDP crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Growth, nonlinear optical, thermal, dielectric and laser damage threshold studies of semiorganic crystal: monohydrate piperazine hydrogen phosphate.

PubMed

Krishnan, P; Gayathri, K; Bhagavannarayana, G; Gunasekaran, S; Anbalagan, G

2013-02-01

Monohydrate piperazine hydrogen phosphate (MPHP), a semi organic nonlinear optical material has been synthesized and single crystals were grown from aqueous solution by slow evaporation technique. Single crystal X-ray diffraction study on grown crystal reveals that they belong to monoclinic crystal system with space group P2(1)/c; (a=6.39Å; b=12.22Å; c=11.16Å; β=97.14°; V=864Å(3)). The structural perfection of the grown crystal was analyzed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. FTIR spectrum confirms the presence of the functional groups in synthesized material. UV-Vis spectrum indicates that the crystal is transparent in the entire visible region with a lower cut off wavelength of 387 nm. The variation of dielectric properties of the grown crystal with respect to frequency has been investigated at different temperatures. Thermal analysis carried out on the MPHP crystal shows that the crystal is stable up to 135°C. Relative powder second harmonic generation efficiency tested by Kurtz-Perry powder technique, which was about 0.638 times that of Potassium dihydrogen phosphate. Copyright © 2012 Elsevier B.V. All rights reserved.

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.

Synthesis and characterization of nanosized lithium manganate and its derivatives

NASA Astrophysics Data System (ADS)

Iqbal, Muhammad Javed; Zahoor, Sabia

Spinel lithium manganese oxide, LiMn 2O 4 and its derivatives are prepared by the sol-gel method. The lattice constant of the pure material is calculated as 8.23 Å. Different transition metal cations of chromium, iron, cobalt, nickel, copper and zinc (0.05 and 0.15 M) are doped in place of manganese in the LiMn 2O 4. X-ray powder diffraction data show that the spinel framework preserved its integrity upon doping. Formation of a single phase and the purity of the samples are confirmed by X-ray powder diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). The crystallite size of the samples is calculated by use of the Scherrer formula and is found to be within a range of 43-66 nm. The electrical conductivity of the samples is determined over a temperature range of 200-300 K by means of four-point probe method. An increasing trend of conductivity with increase in temperature is noted for all the samples. The parent compound LiMn 2O 4 has a conductivity value of 3.47 × 10 -4 ohm -1 cm -1 at room temperature. This value increases on doping with the above-mentioned transition metal cations.

Structural, morphological and optical properties of ZnSe quantum dot thin films.

PubMed

Zedan, I T; Azab, A A; El-Menyawy, E M

2016-02-05

ZnSe powder was prepared via hydrothermal technique using zinc acetate and sodium selenite as source materials. The prepared ZnSe powder was used for preparing film with different thickness values (95, 135 and 230 nm) via thermal evaporation technique. X-ray diffraction showed that the prepared powder has cubic zinc-blende structure with a space group, F43m. The high resolution transmittance electron microscope results show that the films are composed of spherical-shaped nanoparticles with a diameter in the range of 2-8 nm. The optical properties of ZnSe films with differing thicknesses are investigated by means of spectrophotometric measurements of the photoluminescence, transmittance and reflectance. The absorption coefficient of the films is calculated and the optical band gap is estimated. The refractive index of the films is determined and its normal dispersion behavior is analyzed on the basis of a single oscillator model, in which oscillator energy, dispersion energy and dielectric constant at high frequency are evaluated. Drude model is also applied to determine the lattice dielectric constant and the ratio of the carriers' concentration to their effective mass. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of CdS Nanostructures by Thermal Decomposition of Aminocaproic Acid-Mixed Cd-Thiourea Complex Precursor: Structural, Optical and Photocatalytic Characterization.

PubMed

Patel, Jayesh D; Mighri, Frej; Ajji, Abdellah; Chaudhuri, Tapas K

2015-04-01

The present work deals with two different CdS nanostructures produced via hydrothermal and solvothermal decompositions of aminocaproic acid (ACA)-mixed Cd-thiourea complex precursor at 175 °C. Both nanostructures were extensively characterized for their structural, morphological and optical properties. The powder X-ray diffraction characterization showed that the two CdS nanostructures present a wurtzite morphology. Scanning electron microscopy and energy-dispersive X-ray characterizations revealed that the hydrothermal decomposition produced well-shaped CdS flowers composed of six dendritic petals, and the solvothermal decomposition produced CdS microspheres with close stoichiometric chemical composition. The UV-vis absorption and photoluminescence spectra of CdS dendritic flowers and microsphere nanostructures showed that both nanostructures present a broad absorption between 200 and 700 nm and exhibit strong green emissions at 576 and 520 nm upon excitations at 290 nm and 260 nm, respectively. The transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) characterizations confirmed that CdS microspheres were mesoporous and were composed of small nanocrystals. A possible growth mechanism in the formation of the CdS nanostructures was proposed based on morphology evolution as a function of the reaction time. Furthermore, the as-synthesized CdS nanostructures were found to exhibit highly efficient photocatalytic activities for the degradation of methyl orange (MeO) and rhodamine B (RhB) dyes.

An Inquiry-Based Project Focused on the X-Ray Powder Diffraction Analysis of Common Household Solids

ERIC Educational Resources Information Center

Hulien, Molly L.; Lekse, Jonathan W.; Rosmus, Kimberly A.; Devlin, Kasey P.; Glenn, Jennifer R.; Wisneski, Stephen D.; Wildfong, Peter; Lake, Charles H.; MacNeil, Joseph H.; Aitken, Jennifer A.

2015-01-01

While X-ray powder diffraction (XRPD) is a fundamental analytical technique used by solid-state laboratories across a breadth of disciplines, it is still underrepresented in most undergraduate curricula. In this work, we incorporate XRPD analysis into an inquiry-based project that requires students to identify the crystalline component(s) of…

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…

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.

Sealed-tube synthesis and phase diagram of Li{sub x}TiS{sub 2} (0 ≤ x ≤1)

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

Zhang, Ziping; National Laboratory for Superconductivity, Institute of Physics, Chinese Academy of Science, Beijing 100190; Dong, Cheng, E-mail: chengdon@aphy.iphy.ac.cn

2015-01-15

Graphical abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S aslithium source. A schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed based on the DTA and XRD data. - Abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S as lithium source. The Li{sub x}TiS{sub 2} samples were characterized by powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and differential thermal analysis. Themore » variations of the lattice parameters with lithium content x in Li{sub x}TiS{sub 2} were determined by X-ray powder diffraction analysis for both 1T and 3R phases. The phase transition between low-temperature 1T phase and high-temperature 3R phase was confirmed by the powder X-ray diffraction analysis. Based on the differential thermal analysis and X-ray diffraction results, a schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed, providing a guideline to synthesize Li{sub x}TiS{sub 2} in 1T structure or 3R structure.« less

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

Yoon, Songhak; Maegli, Alexandra E.; Karvonen, Lassi

Polycrystalline SrTiO{sub 3} and SrTi(O,F){sub 3} powders were synthesized by a solid-state reaction. A partial substitution of oxygen by nitrogen was subsequently carried out using thermal ammonolysis resulting in SrTi(N,O){sub 3} and SrTi(N,O,F){sub 3}. Powder X-ray diffraction (XRD) revealed a cubic perovskite structure with space group Pm-3m for all samples. The thermal ammonolysis slightly increased the lattice parameters, crystallite sizes and strain. As a result from the co-substitution of oxygen with nitrogen and fluorine for SrTi(N,O,F){sub 3}, highly distorted TiO{sub 6} octahedra were detected using X-ray absorption near edge structure (XANES) spectroscopy. The weakening of all active modes of themore » Raman spectra after thermal ammonolysis also indicated enhanced distortions in the local crystal structure. SrTi(N,O,F){sub 3} has the largest amount of nitrogen as well as fluorine among all four samples as determined by thermogravimetric analysis (TGA), elemental analysis and X-ray photoelectron spectroscopy (XPS). In the UV–vis spectra a distinctive shift of the absorption-edge energy was observed exclusively for the SrTi(N,O,F){sub 3} sample from 390 to 510 nm corresponding to a bandgap narrowing from 3.18 to 2.43 eV. - Graphical abstract: Figure shows the shift of the absorption-edge energy for the SrTi(N,O,F){sub 3} sample from 390 to 510 nm corresponding to a bandgap narrowing from 3.18 to 2.43 eV. Display Omitted - Highlights: • Synthesis of phase-pure SrTi(N,O,F){sub 3} via solid-state reaction. • The incorporated nitrogen contents increase by the presence of fluorine in SrTi(N,O,F){sub 3}. • Co-substitution with nitrogen and fluorine is beneficial for the bandgap narrowing compared to by only nitrogen or fluorine substitution.« less

Synthesis, Characterization, and Gas-Sensing Properties of Mesoporous Nanocrystalline Sn(x)Ti(1-x)O2.

PubMed

Zhong, Cheng; Lin, Zhidong; Guo, Fei; Wang, Xuehua

2015-06-01

A nanocomposite mesoporous material composed by SnO2 and TiO2 with the size of -5-9 nm were prepared via a facile wet-chemical approach combining with an annealing process. The microstructure of obtained Sn(x)Ti(1-x)O2 powders were characterized by X-ray diffraction, X-ray Photo-electronic Spectroscopy, scanning electron microscope, transmission electron microscope and nitrogen adsorption-desorption experiment. The gas sensing performances to several gases of the mesoporous material were studied. The sensors of Sn(x)Ti(1-x)O2 (ST10, with 9.1% Ti) exhibited very high responses to volatile organic compounds at 160 degrees C. The order of the responses to volatile gases based on ST10 was ethanol > formaldehyde > acetone > toluene > benzene > methane. Sensor based on ST10 displays a highest sensitivity to hydrogen at 200 degrees C. Sensor responses to H2 at 200 degrees C have been measured and analyzed in a wide concentration range from 5 to 2000 ppm. The solid solution Sn(x)Ti(1-x)O2 can be served as a potential gas-sensing material for a broad range of future sensor applications.

Synthesis, second-harmonic generation (SHG), and photoluminescence (PL) properties of noncentrosymmetric bismuth selenite solid solutions, Bi2-xLnxSeO5 (Ln = La and Eu; x = 0-0.3)

NASA Astrophysics Data System (ADS)

Qi, Hai-Xin; Jo, Hongil; Oh, Seung-Jin; Ok, Kang Min

2018-02-01

A series of La3+ or Eu3+-doped noncentrosymmetric (NCS) bismuth selenite solid solutions, Bi2-xLnxSeO5 (x = 0.1, 0.2, and 0.3), have been successfully synthesized via standard solid-state reactions under vacuum with Bi2O3, La2O3 (or Eu2O3), and SeO2 as starting materials. Crystal structures and phase purities of the resultant materials were thoroughly characterized by powder X-ray diffraction using the Rietveld method. The results clearly show that the reported materials crystallize in the orthorhombic space group, Abm2 (No. 39), and exhibit pseudo-three-dimensional frameworks consisting of BiO3, BiO5, and SeO3 polyhedra that share edges and corners. Detailed diffraction studies indicate that the cell volume of Bi2-xLnxSeO5 decreases with an increasing amount of Ln3+ on the Bi3+ sites. However, no ordering between Ln3+ and Bi3+ was observed in the Bi2-xLnxSeO5 solid solutions. Powder second-harmonic generation (SHG) measurements, using 1064 nm radiation, reveal that SHG efficiencies of Bi2-xLnxSeO5 solid solutions continuously decrease as more Ln3+ cations are added to the sites of polarizable Bi3+ cations. Photoluminescence (PL) measurements on Bi2-xEuxSeO5 exhibit three specific emission peaks at 592, 613, and 702 nm (5D0 → 7F1, 2, 4) owing to the 4f-4f intrashell transitions of Eu3+ ions.

Thermal, spectroscopic and laser properties of Nd3+ in gadolinium scandium gallium garnet crystal produced by optical floating zone method

NASA Astrophysics Data System (ADS)

Tian, Li; Wang, Shuxian; Wu, Kui; Wang, Baolin; Yu, Haohai; Zhang, Huaijin; Cai, Huaqiang; Huang, Hui

2013-12-01

A neodymium-doped gadolinium scandium gallium garnet (Nd:GSGG) single crystal with dimensions of Φ 5 × 20 mm2 has been grown by means of optical floating zone (OFZ). X-ray powder diffraction (XRPD) result shows that the as-grown Nd:GSGG crystal possesses a cubic structure with space group Ia3d and a cell parameter of a = 1.2561 nm. Effective elemental segregation coefficients of the Nd:GSGG as-grown crystal were calculated by using X-ray fluorescence (XRF). The thermal properties of the Nd:GSGG crystal were systematically studied by measuring the specific heat, thermal expansion and thermal diffusion coefficient, and the thermal conductivity of this crystal was calculated. The absorption and luminescence spectra of Nd:GSGG were measured at room temperature (RT). By using the Judd-Ofelt (J-O) theory, the theoretical radiative lifetime was calculated and compared with the experimental result. Continuous wave (CW) laser performance was achieved with the Nd:GSGG at the wavelength of 1062 nm when it was pumped by a laser diode (LD). A maximum output power of 0.792 W at 1062 nm was obtained with a slope efficiency of 11.89% under a pump power of 7.36 W, and an optical-optical conversion efficiency of 11.72%.

Effects of N precursor on the agglomeration and visible light photocatalytic activity of N-doped TiO2 nanocrystalline powder.

PubMed

Hu, Yulong; Liu, Hongfang; Rao, Qiuhua; Kong, Xiaodong; Sun, Wei; Guo, Xingpeng

2011-04-01

N-doped TiO2 nanocrystalline powders were prepared by the sol-gel method using various N precursors, including triethylamine, hydrazine hydrate, ethylenediamine, ammonium hydroxide, and urea. The samples were characterized by X-ray diffraction, N2 adsorption isotherms, transmission electron microscopy, ultraviolet-visible diffuse reflectance spectroscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The photocatalytic activities of as-prepared samples under irradiation of visible light (lambda > 405 nm) were evaluated by photodecomposition of methyl orange. The alkalinity of N precursor was found to play a key role in the gel process. The N precursor with moderate alkalinity causes TiO2 nanoparticles to be sol-transformed into a loosely agglomerated gel. This transformation facilitates the preparation of an N-doped TiO2 powder with small nanocrystal size, large specific surface area, and high N doping level and results in high visible light photocatalytic activity. The N in TiO2 with N is binding energy at 399-400 eV may be assigned to the N-H species located in interstitial sites of TiO2 lattice which is the active N species responsible for the visible light photocatalytic activity. The N species of N 1s peak at 402 and 405 eV are ineffective to the visible light photocatalytic activity and may inhibit the photocatalytic activity. Moreover, a TiO2 nanoparticle powder with large specific area can be achieved by using urea as a template and then by using ammonium hydroxide to transform the sol into gel.

Lasers, extreme UV and soft X-ray

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

Nilsen, Joseph

2015-09-20

Three decades ago, large ICF lasers that occupied entire buildings were used as the energy sources to drive the first X-ray lasers. Today X-ray lasers are tabletop, spatially coherent, high-repetition rate lasers that enable many of the standard optical techniques such as interferometry to be extended to the soft X-ray regime between wavelengths of 10 and 50 nm. Over the last decade X-ray laser performance has been improved by the use of the grazing incidence geometry, diode-pumped solid-state lasers, and seeding techniques. The dominant X-ray laser schemes are the monopole collisional excitation lasers either driven by chirped pulse amplification (CPA)more » laser systems or capillary discharge. The CPA systems drive lasing in neon-like or nickel-like ions, typically in the 10 – 30 nm range, while the capillary system works best for neon-like argon at 46.9 nm. Most researchers use nickel-like ion lasers near 14 nm because they are well matched to the Mo:Si multilayer mirrors that have peak reflectivity near 13 nm and are used in many applications. As a result, the last decade has seen the birth of the X-ray free electron laser (XFEL) that can reach wavelengths down to 0.15 nm and the inner-shell Ne laser at 1.46 nm.« less

Preparation and Characterization of Mesoporous Zirconia Made by Using a Poly (methyl methacrylate) Template

NASA Astrophysics Data System (ADS)

Duan, Guorong; Zhang, Chunxiang; Li, Aimei; Yang, Xujie; Lu, Lude; Wang, Xin

2008-03-01

Superfine powders of poly (methyl methacrylate) (PMMA) have been prepared by means of an emulsion polymerization method. These have been used as templates in the synthesis of tetragonal phase mesoporous zirconia by the sol gel method, using zirconium oxychloride and oxalic acid as raw materials. The products have been characterized by infrared spectroscopy, X-ray diffraction analysis, transmission electron microscopy, N2 adsorption-desorption isotherms, and pore size distribution. The results indicate that the average pore size was found to be 3.7 nm.

Apparatus Notes.

ERIC Educational Resources Information Center

Eaton, Bruce G., Ed.

1982-01-01

Presents a technique to produce samples for x-ray diffraction studies on the Tel-X-Ometer 80 x-ray apparatus from readily available crystalline powders and discusses observations of transverse modes of an optical resonator. (SK)

Normal-incidence reflectance of optimized W/B4C x-ray multilayers in the range 1.4 nm < λ < 2.4 nm

NASA Astrophysics Data System (ADS)

Windt, David L.; Gullikson, Eric M.; Walton, Christopher C.

2002-12-01

We have fabricated W/B4C multilayers having periods in the range d = 0.8-1.2 nm and measured their soft-x-ray performance near normal incidence in the wavelength range 1.4 < λ < 2.4 nm. By adjusting the fractional layer thickness of W we have produced structures having interface widths σ ~ 0.29 nm (i.e., as determined from normal-incidence reflectometry), thus having optimal soft-x-ray performance. We describe our results and discuss their implications, particularly with regard to the development of short-wavelength normal-incidence x-ray optics.

[The study of ultra-fine diamond powder used in magnetic head polishing slurry].

PubMed

Jin, Hong-Yun; Hou, Shu-En; Pan, Yong; Xiao, Hong-Yan

2008-05-01

In the present paper, atomic absorption spectrometry(AAS), inductively-coupled plasma mass spectrometry (ICP-MS), transmission electron microscopy (TEM), X-ray diffraction (XRD) and laser Raman spectroscopy (RM) were employed to study the commercial ultra-fine diamond powders prepared by the static pressure-catalyst method and used in magnetic head polishing slurry. The results of AAS and ICP-MS indicated that there were silicon oxide, Fe, Ni, Al and some other metal elements in the ultra-fine powders. XRD patterns showed the peaks of SiO2 at 2theta = 35.6 degrees, 39.4 degrees and 59.7 degrees and diamond sharp peaks in agreement with the results above. Diamond sharp peaks implied perfect crystal and high-hardness beneficial to high-efficiency in polishing. The broader Raman band of graphite at 1 592 cm(-1) observed by Raman analysis proved graphite existing in the diamond powders. In the TEM images, the size of ultra-fine powders was estimated between 0.1 and 0.5 microm distributed in a wide scope, however, sharp edges of the powder particles was useful to polish. The ultra-fine diamond powders have many advantages, for example, high-hardness, well abrasion performance, high-polishing efficiency and being useful in magnetic head polishing slurry. But, the impurities influence the polishing efficiency, shortening its service life and the wide distribution reduces the polishing precision. Consequently, before use the powders must be purified and classified. The purity demands is 99.9% and trace silicon oxide under 0.01% should be reached. The classification demands that the particle distribution should be in a narrower scope, with the mean size of 100 nm and the percentage of particles lager than 200 nm not over 2%.

Mechanically induced self-propagating reaction and consequent consolidation for the production of fully dense nanocrystalline Ti{sub 55}C{sub 45} bulk material

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

Sherif El-Eskandarany, M., E-mail: msherif@kisr.edu.kw; Al-Hazza, Abdulsalam

2014-11-15

We employed a high-energy ball mill for the synthesis of nanograined Ti{sub 55}C{sub 45} powders starting from elemental Ti and C powders. The mechanically induced self-propagating reaction that occurred between the reactant materials was monitored via a gas atmosphere gas-temperature-monitoring system. A single phase of NaCl-type TiC was obtained after 5 h of ball milling. To decrease the powder and grain sizes, the material was subjected to further ball milling time. The powders obtained after 200 h of milling possessed spherical-like morphology with average particle and grain sizes of 45 μm and 4.2 nm, respectively. The end-products obtained after 200more » h of ball milling time, were then consolidated into full dense compacts, using hot pressing and spark plasma sintering at 1500 and 34.5 MPa, with heating rates of 20 °C/min and 500 °C/min, respectively. Whereas hot pressing of the powders led to severe grain growth (∼ 436 nm in diameter), the as-spark plasma sintered powders maintained their nanograined characteristics (∼ 28 nm in diameter). The as-synthesized and as-consolidated powders were characterized, using X-ray diffraction, high-resolution electron microscopy, and scanning electron microscopy. The mechanical properties of the consolidated samples obtained via the hot pressing and spark plasma sintering techniques were characterized, using Vickers microhardness and non-destructive testing techniques. The Vickers hardness, Young's modulus, shear modulus and fracture toughness of as-spark plasma sintered samples were 32 GPa, 358 GPa, 151 GPa and 6.4 MPa·m{sup 1/2}, respectively. The effects of the consolidation approach on the grain size and mechanical properties were investigated and are discussed. - Highlights: • Room-temperature synthesizing of NaCl-type TiC • Dependence on the grain size on the ball milling time • Fabrication of equiaxed nanocrystalline grains with a diameter of 4.2 nm • Fabrication of nanocrystalline bulk TiC material by SPS with minimal grain growth • Dependence of improved mechanical properties on the consolidation techniques.« less

Combustion synthesis of MgO nanoparticles using plant extract: Structural characterization and photoluminescence studies

NASA Astrophysics Data System (ADS)

Kumar, Danith; Yadav, L. S. Reddy; Lingaraju, K.; Manjunath, K.; Suresh, D.; Prasad, Daruka; Nagabhushana, H.; Sharma, S. C.; Naika, H. Raja; Chikkahanumantharayappa, Nagaraju, G.

2015-06-01

Magnesium oxide nanoparticles (MgO Nps) have been successfully synthesized via solution combustion method using Parthenium plant extract as fuel for the first time. Powder X-ray diffraction (PXRD) pattern reveal that product belongs to the cubic phase (Periclase). FTIR spectrum shows the band at 822 cm-1 indicates the formation of cubic periclase MgO. The optical band gap of MgO Nps estimated from UV -Vis spectrum was found to be in the range 5.40-5.45 eV. SEM images showed that, the product is agglomerated and particle in nature. Photoluminescence (PL) studies shows violet emission at 390 nm, blue emission at 470 nm and green emission at 550 nm. MgO Nps shows good photocatalytic activity for the degradation of methylene blue (MB) dye under UV/Sun light irradiation.

Intense green and red upconversion emission of Er3+,Yb3+ co-doped CaZrO3 obtained by a solution combustion reaction

NASA Astrophysics Data System (ADS)

Singh, Vijay; Kumar Rai, Vineet; Haase, Markus

2012-09-01

CaZrO3 phosphors co-doped with Er3+ and Yb3+ ions have been prepared by the urea combustion route. The formation of the orthorhombic phase of CaZrO3 was confirmed by powder x-ray diffraction. The absorption in the 280-1800 nm region and excitation spectrum corresponding to the emission at 545 nm for CaZrO3:Er3+/CaZrO3:Er3+,Yb3+ phosphors have been recorded. Upon excitation at 978 nm, the material displays strong energy transfer upconversion emission in the green and red spectral regions. The upconversion emission of the CaZrO3:Er3+,Yb3+ co-doped material shows an increased red-to-green ratio, indicating cross relaxation between Er3+ ions.

Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders.

PubMed

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong; Zheng, Feng

2017-09-21

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH₄)₂C₂O₄·H₂O and Na₂CO₃) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7-10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na₂CO₃ precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed.

Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil.

PubMed

Kappen, P; Arhatari, B D; Luu, M B; Balaur, E; Caradoc-Davies, T

2013-06-01

This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography∕diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

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

2008-08-29

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

Mg(1 + x)Ir(1 - x) (x = 0, 0.037 and 0.054), a binary intermetallic compound with a new orthorhombic structure type determined from powder and single-crystal X-ray diffraction.

PubMed

Cerný, Radovan; Renaudin, Guillaume; Favre-Nicolin, Vincent; Hlukhyy, Viktor; Pöttgen, Rainer

2004-06-01

The new binary compound Mg(1 + x)Ir(1 - x) (x = 0-0.054) was prepared by melting the elements in the Mg:Ir ratio 2:3 in a sealed tantalum tube under an argon atmosphere in an induction furnace (single crystals) or by annealing cold-pressed pellets of the starting composition Mg:Ir 1:1 in an autoclave under an argon atmosphere (powder sample). The structure was independently solved from high-resolution synchrotron powder and single-crystal X-ray data: Pearson symbol oC304, space group Cmca, lattice parameters from synchrotron powder data a = 18.46948 (6), b = 16.17450 (5), c = 16.82131 (5) A. Mg(1 + x)Ir(1 - x) is a topologically close-packed phase, containing 13 Ir and 12 Mg atoms in the asymmetric unit, and has a narrow homogeneity range. Nearly all the atoms have Frank-Kasper-related coordination polyhedra, with the exception of two Ir atoms, and this compound contains the shortest Ir-Ir distances ever observed. The solution of a rather complex crystal structure from powder diffraction, which was fully confirmed by the single-crystal method, shows the power of powder diffraction in combination with the high-resolution data and the global optimization method.

On the reactive occlusion of the (uranium trichloride + lithium chloride + potassium chloride) eutectic salt in zeolite 4A

NASA Astrophysics Data System (ADS)

Lexa, Dusan; Leibowitz, Leonard; Kropf, Jeremy

2000-03-01

The interaction between the (uranium trichloride + lithium chloride + potassium chloride) eutectic salt and zeolite 4A has been studied by temperature-resolved synchrotron powder X-ray diffraction, evolved gas analysis and differential scanning calorimetry, between 300 and 900 K. The onset of salt occlusion by the zeolite has been detected at 450 K. Evidence of a reaction between zeolitic water and uranium trichloride, leading to the formation of uranium dioxide, has appeared at 600 K. The uranium dioxide particle size increases from 2 nm at 600 K to 25 nm at 900 K - an indication of their extra-zeolitic location. No appreciable degradation of the zeolite structure has been observed.

Gas sensing performance of nano zinc oxide sensors

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

Sharma, Shiva, E-mail: shivasharmaau@gmail.com; Chauhan, Pratima, E-mail: mangu167@yahoo.co.in

We report nano Zinc Oxide (ZnO) synthesized by sol-gel method possessing the crystallite size which varies from 25.17 nm to 47.27 nm. The Scanning electron microscope (SEM) image confirms the uniform distribution of nanograins with high porosity. The Energy dispersion X-ray (EDAX) spectrum gives the atomic composition of Zn and O in ZnO powders and confirms the formation of nano ZnO particles. These factors reveals that Nano ZnO based gas sensors are highly sensitive to Ammonia gas (NH{sub 3}) at room temperature, indicating the maximum response 86.8% at 800 ppm with fast response time and recovery time of 36 sec and 23 secmore » respectively.« less

Colloidal synthesis of monodispersed ZnS and CdS nanocrystals from novel zinc and cadmium complexes

NASA Astrophysics Data System (ADS)

Onwudiwe, Damian C.; Mohammed, Aliyu D.; Strydom, Christien A.; Young, Desmond A.; Jordaan, Anine

2014-06-01

Monodispersed spherical and hexagonal shaped ZnS and CdS nanocrystals respectively, have been synthesized using novel heteroleptic complexes of xanthate (S2CObu) and dithiocarbamate (S2CNMePh). The nanocrystals were prepared via colloidal route and stabilized in hexadecylamine (HDA). The morphology of the as-prepared nanocrystals was characterized using transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), and powdered X-ray diffraction (p-XRD) analysis. An average diameter of 7.2 nm and 8.6 nm were obtained for the ZnS and CdS respectively. The optical properties of the nanoparticles studied by UV-vis and photoluminescence (PL) spectroscopy showed a blue shift in the absorption spectra, and band edge emission respectively.

Phosphine-free synthesis and characterization of type-II ZnSe/CdS core-shell quantum dots

NASA Astrophysics Data System (ADS)

Ghasemzadeh, Roghayyeh; Armanmehr, Mohammad Hasan; Abedi, Mohammad; Fateh, Davood Sadeghi; Bahreini, Zaker

2018-01-01

A phosphine-free route for synthesis of type-II ZnSe/CdS core-shell quantum dots, using green, low cost and environmentally friendly reagents and phosphine-free solvents such as 1-octadecene (ODE) and liquid paraffin has been reported. Hot-injection technique has been used for the synthesis of ZnSe core quantum dots. The CdS shell quantum dots prepared by reaction of CdO precursor and S powder in 1-octadecene (ODE). The ZnSe/CdS core-shell quantum dots were synthesized via successive ion layer adsorption and reaction (SILAR) technique. The characterization of produced quantum dots were performed by absorption and fluorescence spectroscopy, X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX) and transmission electron microscopy (TEM). The results showed the formation of type-II ZnSe/CdS core-shell quantum dots with FWHM 32 nm and uniform size distribution.

Structural and optical properties of furfurylidenemalononitrile thin films

NASA Astrophysics Data System (ADS)

Ali, H. A. M.

2013-03-01

Thin films of furfurylidenemalononitrile (FMN) were deposited on different substrates at room temperature by thermal evaporation technique under a high vacuum. The structure of the powder was confirmed by Fourier transformation infrared (FTIR) technique. The unit cell dimensions were determined from X-ray diffraction (XRD) studies. The optical properties were investigated using spectrophotometric measurements of the transmittance and reflectance at normal incidence of light in the wavelength range from 200 to 2500 nm. The refractive index (n), the absorption index (k) and the absorption coefficient (α) were calculated. The analysis of the spectral behavior of the absorption coefficient in the absorption region revealed an indirect allowed transition. The refractive index dispersion was analyzed using the single oscillator model. Some dispersion parameters were estimated. Complex dielectric function and optical conductivity were determined. The influence of the irradiation with high-energy X-rays (6 MeV) on the studied properties was also investigated.

Synthesis and Characterization of Multi Wall Carbon Nanotubes (MWCNT) Reinforced Sintered Magnesium Matrix Composites

NASA Astrophysics Data System (ADS)

Vijaya Bhaskar, S.; Rajmohan, T.; Palanikumar, K.; Bharath Ganesh Kumar, B.

2016-04-01

Metal matrix composites (MMCs) reinforced with ceramic nano particles (less than 100 nm), termed as metal matrix nano composites (MMNCs), can overcome those disadvantages associated with the conventional MMCs. MMCs containing carbon nanotubes are being developed and projected for diverse applications in various fields of engineering like automotive, avionic, electronic and bio-medical sectors. The present investigation deals with the synthesis and characterization of hybrid magnesium matrix reinforced with various different wt% (0-0.45) of multi wall carbon nano tubes (MWCNT) and micro SiC particles prepared through powder metallurgy route. Microstructure and mechanical properties such as micro hardness and density of the composites were examined. Microstructure of MMNCs have been investigated by scanning electron microscope, X-ray diffraction and energy dispersive X-ray spectroscopy (EDS) for better observation of dispersion of reinforcement. The results indicated that the increase in wt% of MWCNT improves the mechanical properties of the composite.

Synthesis and characterization of nanocrystalline Co-Fe-Nb-Ta-B alloy

NASA Astrophysics Data System (ADS)

Raanaei, Hossein; Fakhraee, Morteza

2017-09-01

In this research work, structural and magnetic evolution of Co57Fe13Nb8Ta4B18 alloy, during mechanical alloying process, have been investigated by using, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron dispersive X-ray spectroscopy, differential thermal analysis and also vibrating sample magnetometer. It is observed that at 120 milling time, the crystallite size reaches to about 7.8 nm. Structural analyses show that, the solid solution of the initial powder mixture occurs at160 h milling time. The coercivity behavior demonstrates a rise, up to 70 h followed by decreasing tendency up to final stage of milling process. Thermal analysis of 160 h milling time sample reveals two endothermic peaks. The characterization of annealed milled sample for 160 h milling time at 427 °C shows crystallite size growth accompanied by increasing in saturation magnetization.

Nano-crystalline hydroxyapatite bio-mineral for the treatment of strontium from aqueous solutions.

PubMed

Handley-Sidhu, Stephanie; Renshaw, Joanna C; Yong, Ping; Kerley, Robert; Macaskie, Lynne E

2011-01-01

Hydroxyapatites were analysed using electron microscopy, X-ray diffraction (XRD) and X-ray fluorescence (XRF) analysis. Examination of a bacterially produced hydroxyapatite (Bio-HA) by scanning electron microscopy showed agglomerated nano-sized particles; XRD analysis confirmed that the Bio-HA was hydroxyapatite, with an organic matter content of 7.6%; XRF analysis gave a Ca/P ratio of 1.55, also indicative of HA. The size of the Bio-HA crystals was calculated as ~25 nm from XRD data using the Scherrer equation, whereas Comm-HA powder size was measured as ≤ 50 μm. The nano-crystalline Bio-HA was ~7 times more efficient in removing Sr(2+) from synthetic groundwater than Comm-HA. Dissolution of HA as indicated by the release of phosphate into the solution phase was higher in the Comm-HA than the Bio-HA, indicating a more stable biomaterial which has a potential for the remediation of contaminated sites.

Fabrication of ZnO and doped ZnO waveguides deposited by Spin Coating

NASA Astrophysics Data System (ADS)

Mohan, Rosmin Elsa; R, Neha P.; T, Shalu; C, Darshana K.; Sreelatha, K. S.

2015-02-01

In this paper, the synthesis of ZnO and doped Zn1-xAgxO (where x=0.03) nanoparticles by co- precipitation is reported. The precursors used were Zinc Nitrate and Potassium hydroxide pellets. For doping, 3% AgNO3 in ZnNO3 was considered as a separate buffer solution. The prepared nanoparticles were subsequently spin coated onto silica glass substrates at a constant chuck rate of 3000 rpm. The substrate acts as the lower cladding of a waveguide structure. The upper cladding is assumed to be air in the present investigation. The nanostructures of the ZnO powders in the doped and undoped cases were studied using X-ray Diffraction patterns. There was a decrease in the grain size with doping which increase the tunability of the powders to be used as photoluminescent devices. The optical characteristics of the sample were also investigated using UV-Visible spectrophotometer at 200-900 nm wavelengths. The photoluminescence peaks also report a dramatic increase in intensity at the same wavelength for the doped case compared to the undoped one.

Synthesis, surface chemistry and pseudocapacitance mechanisms of VN nanocrystals derived by a simple two-step halide approach

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

Choi, Daiwon; Jampani, Prashanth H.; Jayakody, J. R. P.

Chloroamide precursors generated via a simple two-step ammonolysis reaction of transition metal chloride in the liquid phase at room temperature were heat treated in ammonia at moderate temperature to yield nano-sized VN crystallites. Grain growth inhibited by lowering the synthesis temperature (≈400°C) yielded agglomerated powders of spherical crystallites of cubic phase of VN with particle sizes as small as 6nm in diameter. X-ray diffraction, FTIR, mass spectroscopy (MS), and nuclear magnetic resonance (NMR) spectroscopy assessed the ammonolysis and nitridation reaction of the VCl 4-NH 3 system. X-ray Rietveld refinement, the BET technique and high-resolution transmission microscopy (HRTEM), energy dispersive x-raymore » (EDX) and thermogravimetric analysis (TGA) helped assess the crystallographic and microstructural nature of the VN nanocrystals. The surface chemistry and redox reaction leading to the gravimetric pseudo-capacitance value of (≈855 F/g) measured for the VN nanocrystals was determined and validated using FTIR, XPS and cyclic voltammetry analyses.« less

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

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

Comparison of microstructure and magnetic properties of gas-atomized and melt-spun MRE-Fe-Co-M-B (MRE=Y+Dy+Nd,M=Zr+TiC)

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

Tang, W.; Wu, Y. Q.; Dennis, K. W.

2007-05-01

An MRE{sub 2}(Fe,Co){sub 14}B alloy with Zr substitution and TiC addition was systematically studied. It was found by means of X-ray diffraction, transmission electron microscopy (TEM) and magnetic measurements that the combination of Zr substitution and TiC addition yields adequate microstructural control in both gas atomization (GA) and melt spinning (MS) techniques. For MS ribbons, an H{sub cj} of 11.7 kOe and (BH){sub max} of 11.9 MGOe at 27 degree sign C were obtained in the ribbons spun at 16 m/s and annealed at 700 degree sign C for 15 min. For GA powders, an H{sub cj} of 9.1 kOemore » and (BH){sub max} of 9.2 MGOe at 27 degree sign C were obtained in 20-25 {mu}m GA powder annealed at 700 degree sign C for 15 min. The temperature coefficients of B{sub r} and H{sub cj} are 0.06 and 0.36%/ degree sign C for the MS ribbon and 0.09 and 0.4%/ degree sign C for the GA powder in the temperature range of 27-100 degree sign C, respectively. TEM images revealed that the MS ribbon consists of a fine and uniform microstructure with an average size of 30 nm, while the GA spherical powder consists of an interior coarsened microstructure with a grain size of 80 nm and a rim area with a grain size of 10 nm.« less

Some Structural Properties of the Mixed Lead-Magnesium Hydroxyapatites

NASA Astrophysics Data System (ADS)

Kaaroud, K.; Ben Moussa, S.; Brigui, N.; Badraoui, B.

2018-02-01

Lead-magnesium hydroxyapatite solid solutions Pb(10- x)Mg x (PO4)6(OH)2 have been prepared via a hydrothermal process. They were characterized by X-ray powder diffraction, Transmission Electron Microscopy (TEM), chemical and IR spectroscopic analyses. The results of the structural refinement indicated that the limits of lead-magnesium solid solutions ( x ≤ 1.5), a regular decrease of the lattice constant a and a preferential magnesium distribution in site S(I). Through the progressive replacement of Pb2+ ( r = 0.133 nm) by the smaller cation Mg2+ ( r = 0.072 nm), all interatomic distances decrease in accordance with the decrease of the cell parameters. According to what could be expected from the coordinance of the metallic sites S(I) (hexacoordination) and S(II) (heptacoordination), the small magnesium cation preferentially occupies the four sites S(I). The results of the TEM analysis confirm the presence of magnesium in the starting solution and reveals the decrease in the average size of crystals. The IR spectra show the presence of the absorption bands characteristic for the apatite structure.

Heats of immersion of titania powders in primer solutions

NASA Technical Reports Server (NTRS)

Siriwardane, R.; Wightman, J. P.

1983-01-01

The oxide layer present on titanium alloys can play an important role in determining the strength and durability of adhesive bonds. Here, three titania powders in different crystalline phases, rutile-R1, anatase-A1, and anatase-A2, are characterized by several techniques. These include microelectrophoresis, X-ray diffractometry, surface area pore volume analysis, X-ray photoelectron spectroscopy, and measurements of the heats of immersion. Of the three powders, R1 has the highest heat of immersion in water, while the interaction between water and A1 powder is low. Experimental data also suggest a specific preferential interaction of polyphenylquinoxaline with anatase.

Morphology and structural development of reduced anatase-TiO{sub 2} by pure Ti powder upon annealing and nitridation: Synthesis of TiO{sub x} and TiO{sub x}N{sub y} powders

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

Bolokang, A.S., E-mail: Sylvester.Bolokang@transnet.net; DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria 0001; Transnet Engineering, Product Development, Private Bag X 528, Kilnerpark 0127

2015-02-15

It is well known that nitriding of titanium is suitable for surface coating of biomaterials and in other applications such as anti-reflective coating, while oxygen-rich titanium oxynitride has been applied in thin film resistors and photocatalysis. Thus in this work anatase was reduced with pure titanium powder during annealing in argon. This was done to avoid any metallic contamination and unwanted residual metal doping. As a result, interesting and different types of particle morphology were synthesized when the pre-milled elemental anatase and titanium powders were mixed. The formation of metastable face centred cubic and monoclinic titanium monoxide was detected bymore » the X-ray diffraction technique. The phases were confirmed by energy dispersive X-ray spectroscopy analysis. Raman analysis revealed weak intensity peaks for samples annealed in argon as compared to those annealed under nitrogen. - Graphical abstract: Display Omitted - Highlights: • Reaction of TiO{sub 2} and Ti induced metastable FCC and monoclinic TiO{sub x}. • Compositions of mixed powder were prepared from the unmilled and pre-milled powders. • Nitridation of TiO{sub x} yielded TiO{sub x}N{sub y} phase. • Mixed morphology was observed on all three powder samples.« less

Sub-10 nm Water-Dispersible β-NaGdF4:X% Eu3+ Nanoparticles with Enhanced Biocompatibility for in Vivo X-ray Luminescence Computed Tomography.

PubMed

Zhang, Wenli; Shen, Yingli; Liu, Miao; Gao, Peng; Pu, Huangsheng; Fan, Li; Jiang, Ruibin; Liu, Zonghuai; Shi, Feng; Lu, Hongbing

2017-11-22

As a novel molecular and functional imaging modality, X-ray luminescence computed tomography (XLCT) has shown its potentials in biomedical and preclinic applications. However, there are still some limitations of X-ray-excited luminescent materials, such as low luminescence efficiency, poor biocompatibility, and cytotoxicity, making in vivo XLCT imaging quite challenging. In this study, for the very first time, we present on using sub-10 nm β-NaGdF 4 :X% Eu 3+ nanoparticles with poly(acrylic acid) (PAA) surface modification, which demonstrate outstanding luminescence efficiency, uniform size distribution, water dispersity, and biosafety, as the luminescent probes for in vivo XLCT application. The pure hexagonal phase (β-) NaGdF 4 has been successfully synthesized and characterized by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM), and then the results of X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectrometry  (EDX), and elemental mapping further confirm Eu 3+ ions doped into NaGdF 4 host. Under X-ray excitation, the β-NaGdF 4 nanoparticles with a doping level of 15% Eu 3+ exhibited the most efficient luminescence intensity. Notably, the doping level of Eu 3+ has no effect on the crystal phase and morphology of the NaGdF 4 -based host. Afterward, β-NaGdF 4 :15% Eu 3+ nanoparticles were modified with PAA to enhance the water dispersity and biocompatibility. The compatibility of in vivo XLCT imaging using such nanoparticles was systematically studied via in vitro cytotoxicity, physical phantom, and in vivo imaging experiments. The ultralow cytotoxicity of PAA-modified nanoparticles, which is confirmed by over 80% cell viability of SH-SY5Y cells when treated by high nanoparticle concentration of 200 μg/mL, overcome the major obstacle for in vivo application. In addition, the high luminescence intensity of PAA-modified nanoparticles enables the location error of in vivo XLCT imaging less than 2 mm, which is comparable to that using commercially available bulk material Y 2 O 3 :15% Eu 3+ . The proposed nanoparticles promote XLCT research into an in vivo stage. Further modification of these nanoparticles with biofunctional molecules could enable the potential of targeting XLCT imaging.

Synthesis, characterization and magnetic properties of nanocrystalline FexNi80-xCo20 ternary alloys

NASA Astrophysics Data System (ADS)

Dalavi, Shankar B.; Theerthagiri, J.; Raja, M. Manivel; Panda, R. N.

2013-10-01

Fe-Ni-Co alloys of various compositions (FexNi80-xCo20,x=20-50) were synthesized by using a sodium borohydride reduction route. The phase purity and crystallite size was ascertained by using powder X-ray diffraction (XRD). The alloys crystallize in the face centered cubic (fcc) structure with lattice parameters, a=3.546-3.558 Å. The XRD line broadening indicates the fine particle nature of the materials. The estimated crystallite sizes were found to be 27.5, 27, 24, and 22.8 nm for x=20, 30, 40, and 50; alloys respectively. Scanning electron micrograph studies indicates particle sizes to be in the range of 83-60 nm for Fe-Ni-Co alloys. The values of saturation magnetization for FexNi80-xCo20 are found to be in the range of 54.3-41.2 emu/g and are significantly lower than the bulk values (175-180 emu/g). The coercivity decreases from 170 to 122 Oe with decrease in Fe content. The observed magnetic behavior has been explained on the basis of size, surface effects, spin canting and the presence of superparamagnetic fractions in the ultrafine materials.

Synthesis and characterization of copper zinc oxide nanoparticles obtained via metathesis process

NASA Astrophysics Data System (ADS)

Phoohinkong, Weerachon; Foophow, Tita; Pecharapa, Wisanu

2017-09-01

Copper-doped zinc oxide nanoparticles were successfully synthesized by grinding copper acetate and zinc acetate powder with different starting molar ratios in combined with sodium hydroxide. The effect of initial copper and zinc molar ratios on the product samples was investigated and discussed. Relevant ligand coordination type of reactant acetate salt precursors and product samples were investigated by Fourier transform infrared spectroscopy (FTIR). The particle shapes and surface morphologies were characterized by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Phase structures of prepared samples were studied by x-ray powder diffraction (XRD) and x-ray absorption near-edge spectroscopy (XANES) was applied to investigate the local structure of Cu and Zn environment atoms. The results demonstrate that the, particle size of as-synthesized products affected by copper concentration in the precursor trend to gradually decreases from nanorod shape with diameter around 50-100 nm to irregular particle structure around 5 nm associated with an increase in the concentration of copper in precursor. Moreover, it is noticed that shape and morphology of the products are strongly dependent on Cu:Zn ratios during the synthesis. Nanocrystallines Cu-doped ZnO by the substitution in Zn site with a high crystallization degree of hexagonal wurtzite structure were obtained. This synthesis technique is suggested as a potential effective technique for preparing copper zinc oxide nanoparticles with various atomic ratio in wide range of applications. Contribution at the 4th Southeast Asia Conference on Thermoelectrics 2016 (SACT 2016), 15-18 December 2016, Da Nang City, Vietnam.

Physical and Chemical Characterization of Therapeutic Iron Containing Materials: A Study of Several Superparamagnetic Drug Formulations with the β-FeOOH or Ferrihydrite Structure

NASA Astrophysics Data System (ADS)

Funk, Felix; Long, Gary J.; Hautot, Dimitri; Büchi, Ruth; Christl, Iso; Weidler, Peter G.

2001-03-01

The effectiveness of therapeutically used iron compounds is related to their physical and chemical properties. Four different iron compounds used in oral, intravenous, and intramuscular therapy have been examined by X-ray powder diffraction, iron-57 Mössbauer spectroscopy, transmission electron microscopy, BET surface area measurement, potentiometric titration and studied through dissolution kinetics determinations using acid, reducing and chelating agents. All compounds are nanosized with particle diameters, as determined by X-ray diffraction, ranging from 1 to 4.1 nm. The superparamagnetic blocking temperatures, as determined by Mössbauer spectroscopy, indicate that the relative diameters of the aggregates range from 2.5 to 4.1 nm. Three of the iron compounds have an akaganeite-like structure, whereas one has a ferrihydrite-like structure. As powders the particles form large and dense aggregates which have a very low surface area on the order of 1 m2 g-1. There is evidence, however, that in a colloidal solution the surface area is increased by two to three orders of magnitude, presumably as a result of the break up of the aggregates. Iron release kinetics by acid, chelating and reducing agents reflect the high surface area, the size and crystallinity of the particles, and the presence of the protective carbohydrate layer coating the iron compound. Within a physiologically relevant time period, the iron release produced by acid or large chelating ligands is small. In contrast, iron is rapidly mobilized by small organic chelating agents, such as oxalate, or by chelate-forming reductants, such as thioglycolate.

Cationic surfactant assisted sonochemical synthesis of Nd3+ doped Zn2SiO4 nanostructures for solid state lighting applications

NASA Astrophysics Data System (ADS)

Basavaraj, R. B.; Malleshappa, J.; Darshan, G. P.; Prasad, B. Daruka; Nagabhushana, H.

2018-04-01

For the first time cationic surfactant assisted ultrasound synthesis route has been used for the preparation of pure and Nd3+ (0.5-9 mol %) doped Zn2SiO4 nanophosphors. The shape, size and morphology of the products were tuned by controlling the various experimental parameters. The final product was well characterized by sophisticated techniques viz. powder X-ray diffraction (PXRD), Ultraviolet visible spectroscopy (UV-Vis) and photoluminescence (PL). The powder X-ray diffraction patterns confirmed that the synthesized samples exhibit hexagonal phase without any impurity. The DRS spectra showed major peaks at 275, 360, 529, 586, 680, 742 and 806 nm due to the transitions of the 4f electrons of Nd3+ from the ground-state 4I9/2 to 2F5/2, 4D3/2 + 4D5/2 + 2I11/2, 2K13/2 + 4G7/2 + 4G9/2, 4G5/2 + 2G7/2, 4F7/2 + 4S3/2, 4F5/2 + 2H9/2 and 4F3/2 respectively. The band energy gap (Eg) of the samples were estimated and found to be in the range 5.32 - 5.52 eV. Under 421 nm excitation, PL spectra exhibit strong near ultraviolet emission peaks at˜444 nm, 459 nm and 520 nm were attributed to 2P3/2 → 4I13/2, 2P3/2 → 4I15/2, 1I6 → 3H4, 2P1/2 → 4I9/2 and 4G7/2 → 4I9/2 transitions respectively. The photometric studies indicate that the synthesized Zn2SiO4: Nd3+ nanophosphors can be tuned from blue to pale green by varying the dopant concentration. The current synthesis route is rapid, environmentally benign, cost-effective and useful for industrial applications such as solid state lighting and display devices.

Synthesis and luminescence studies of Eu (III) doped Sr2P2O7 phosphor for white LED applications

NASA Astrophysics Data System (ADS)

Khan, Z. S.; Ingale, N. B.; Omanwar, S. K.

2018-05-01

Europium (III) doped distrontium diphosphate (Sr2P2O7) is synthesized by slow vaporization method and its luminescence properties are carried out. Using X-Ray diffraction, the crystal structure of this material was confirmed. Photoluminescence (PL) measurement make clear the phosphor exhibited intense emission at 593 nm (yellow) and 612 nm (orange) respectively corresponding to 5D0→7F1 and 5D0→7F2 transitions of Eu3+ on excitation with most favourable 394 nm wavelengths. The remaining excitation peaks at 381 nm and 465 nm with broad band 200-310 nm are also witness in the excitation spectra. The particle morphology using SEM images shows micro level particles for this phosphor. The effect of concentration of Eu3+ ions on the PL intensity has also been investigated. It has been observed that the powder sample exhibits highest PL emission intensity for Eu3+ concentration of about 0.02 moles. The emission spectra exhibit orange performance (CIE chromaticity coordinates: X = 0.672, Y = 0.328), which is due to the 5D0→7F2 transitions of Eu3+ ions. This phosphor is very good for white LED applications.

Investigation of structural, magnetic and dielectric properties of Cr3+ substituted Cu0.75Co0.25Fe2-xO4 ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Reddi, M. Sushma; Ramesh, M.; Sreenivasu, T.; Rao, G. S. N.; Samatha, K.

2018-05-01

Chromium doped Copper-Cobalt ferrite Nanoparticles were obtained by sol-gel auto-combustion method using citric acid as a fuel. The metal nitrates to citric acid ratio was taken as 1:1. The prepared powder of Cr3+ doped copper-cobalt ferrite nanoparticles is annealed at 600°C for 5 hrs and the same powder was used for characterization and investigations of structural properties. The phase composition, micro-structural, micro morphological and elemental analysis studies were carried out by X-ray diffraction (XRD), scanning electron microscope (SEM) technique and energy dispersive spectroscopy (EDS). The FTIR spectra of these samples are recorded to ensure the presence of the metallic compounds. The average crystallite size obtained by Scherrer's formula is of the order of 19.28 nm to 32.92 nm. The dielectric properties are investigated as a function of frequency at room temperature using LCR-Q meter. The saturation magnetization (Ms) of the Cr3+ substituted Cu-Co ferrite sintered at 1100°C lies in the range of 5.4136-28.9943 emu/g, the coercivity (Hc) dropped desperately from about 2091.3-778.53Oe as Cr3+ composition increases from 0.0 to 0.25.

Fabrication and Magnetic Properties of Co₂MnAl Heusler Alloys by Mechanical Alloying.

PubMed

Lee, Chung-Hyo

2018-02-01

We have applied mechanical alloying (MA) to produce nanocrystalline Co2MnAl Heusler alloys using a mixture of elemental Co50Mn25Al25 powders. An optimal milling and heat treatment conditions to obtain a Co2MnAl Heusler phase with fine microstructure were investigated by X-ray diffraction, differential scanning calorimeter and vibrating sample magnetometer measurements. α-(Co, Mn, Al) FCC phases coupled with amorphous phase are obtained after 3 hours of MA without any evidence for the formation of Co2MnAl alloys. On the other hand, a Co2MnAl Heusler alloys can be obtained by the heat treatment of all MA samples up to 650 °C. X-ray diffraction result shows that the average grain size of Co2MnAl Heusler alloys prepared by MA for 5 h and heat treatment is in the range of 95 nm. The saturation magnetization of MA powders decreases with MA time due to the magnetic dilution by alloying with nonmagnetic Mn and Al elements. The magnetic hardening due to the reduction of the grain size with ball milling is also observed. However, the saturation magnetization of MA powders after heat treatment increases with MA time and reaches to a maximum value of 105 emu/g after 5 h of MA. It can be also seen that the coercivity of 5 h MA sample annealed at 650 °C is fairly low value of 25 Oe.

Recent progress of hard x-ray imaging microscopy and microtomography at BL37XU of SPring-8

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

Suzuki, Yoshio, E-mail: yoshio@spring8.or.jp; Takeuchi, Akihisa; Terada, Yasuko

2016-01-28

A hard x-ray imaging microscopy and microtomography system is now being developed at the beamline 37XU of SPring-8. In the latest improvement, a spatial resolution of about 50 nm is achieved in two-dimensional imaging at 6 keV x-ray energy using a Fresnel zone plate objective with an outermost zone width of 35 nm. In the tomographic measurement, a spatial resolution of about 100 nm is achieved at 8 keV using an x-ray guide tube condenser optic and a Fresnel zone plate objective with an outermost zone width of 50 nm.

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.

XPEEM valence state imaging of mineral micro-intergrowths with a spatial resolution of 100nm

NASA Astrophysics Data System (ADS)

Smith, A. D.; Schofield, P. F.; Scholl, A.; Pattrick, R. A. D.; Bridges, J. C.

2003-03-01

The crystal chemistry and textural relationships of minerals hold a vast amount of information relating to the formation, history and stability of natural materials. The application of soft X-ray spectroscopy to mineralogical material has revealed that 2p (L{2,3}) spectra provide a sensitive fingerprint of the electronic states of 3d metals. In bulk powdered samples much of the textural and microstructural information is lost, but the area-selectivity capability of X-ray Photo-Emission Electron Microscopy (XPEEM) provides the ability to obtain valence state information from mineral intergrowths with a submicron spatial resolution. Using the state-of-the-art PEEM2 facility on beamline 7.3.1.1 at the Advanced Light Source, Berkeley, USA, a range of minerals, mineral intergrowths and mineralogical textures have been studied for a broad suite of geological, planetary and environmental science materials. High-quality, multi-element valence images have been obtained showing the distribution/variation of the metal valence states across single grains or mineral intergrowths/textures at the l00 nm scale and quantitative valence state ratios can be obtained from areas of 0.01 μ m^2.

Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Neuefiend, J.; Weber, H.-P.; Proffen, T.; VonDreele, R.; Palosz, W.;

Effect of annealing on the structural and optical properties of TiO{sub 2} powder prepared by sol-gel route

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

Halder, Nilanjan; Misra, Kamakhya Prakash

2016-05-06

Using titanium isopropoxide as the precursor, Titanium dioxide (TiO{sub 2}) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO{sub 2} samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increasemore » with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO{sub 2} nano powder samples.« less

The fracture strength of cryomilled 99.7 Al nanopowders consolidated by high frequency induction sintering

NASA Astrophysics Data System (ADS)

El-Danaf, Ehab A.; Baig, Muneer; Almajid, Abdulhakim A.; Soliman, Mahmoud S.

2014-08-01

Mechanical Attrition of metallic powders induces severe plastic deformation and consequently reduces the average grain size. Powders of 99.7 Al (45μm particle size), cryomilled for 7 hrs having a crystal size of ~ 20 nm, were consolidated by high frequency induction sintering under a constant pressure of 50 MPa and at two temperatures of 500 and 550 °C for two sintering dwell times of 1 and 3 minutes at a constant heating rate of 400 °C/min. The bright field TEM image and X-ray line broadening technique, for the cryomilled powders, were used to measure-the crystallite size. Simple compression at an initial strain rate of 10-4 s-1 was conducted at room temperature, 373 and 473 K, and the yield strength was documented and correlated with the sintering parameters. The as-received 99.7 Al powders-consolidated using one of the sintering parameters was used as a reference material to compare the mechanical properties. Hardness, density and crystal size of the consolidated sample, that gave the highest yield and fracture strength, were measured.

Single-Photon Ionization Soft-X-Ray Laser Mass Spectrometry of Potential Hydrogen Storage Materials

NASA Astrophysics Data System (ADS)

Dong, F.; Bernstein, E. R.; Rocca, J. J.

A desk-top size capillary discharge 46.9 nm lasear is applied in the gas phase study of nanoclusters. The high photon energy allows for single-photon ionization mass spectrometry with reduced cluster fragmentation. In the present studies, neutral Al m C n and Al m C n H x cluster are investigation for the first time. Single photon ionization through 46.9 nm, 118 nm, 193 nm lasers is used to detect neutral cluster distributions through time of flight mass spectrometry. Al m C n clusters are generated through laser ablation of a mixture of Al and C powders pressed into a disk. An oscillation of the vertical ionization energies (VIEs) of Al m C n clusters is observed in the experiments. The VIEs of Al m C n clusters changes as a function of the numbers of Al and C atoms in the clusters. Al m C n H x clusters are generated through an Al ablation plasma-hydrocarbon reaction, an Al-C ablation plasma reacting with H2 gas, or through cold Al m C n clusters reacting with H2 gas in a fast flow reactor. DFT and ab inito calculations are carried out to explore the structures, IEs, and electronic structures of Al m C n H x clusters. C=C bonds are favored for the lowest energy structures for Al m C n clusters. Be m C n H x are generated through a beryllium ablation plasma-hydrocarbon reaction and detected by single photon ionization of 193 nm laser. Both Al m C n H x and Be m C n H x are considered as potential hydrogen storage materials.

Process Parameters on the Crystallization and Morphology of Hydroxyapatite Powders Prepared by a Hydrolysis Method

NASA Astrophysics Data System (ADS)

Wang, Moo-Chin; Hon, Min-Hsiung; Chen, Hui-Ting; Yen, Feng-Lin; Hung, I.-Ming; Ko, Horng-Huey; Shih, Wei-Jen

2013-07-01

The effects of process parameters on the crystallization and morphology of hydroxyapatite (Ca10(PO4)6(OH)2, HA) powders synthesized from dicalcium phosphate dihydrate (CaHPO4·2H2O, DCPD) using a hydrolysis method have been investigated. X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were used to characterize the synthesized powders. When DCPD underwent hydrolysis in 2.5 NaOH solution (Na(aq)) at 303 K to 348 K (30 °C to 75 °C) for 1 hour, the XRD results revealed that HA was obtained for all the as-dried samples. The SEM morphology of the HA powders for DCPD hydrolysis produced at 348 K (75 °C) shows regular alignment and a short rod shape with a size of 200 nm in length and 50 nm in width. With DCPD hydrolysis in 2.5 M NaOH(aq) holding at 348 K (75 °C) for 1 to 24 hours, XRD results demonstrated that all samples were HA and no other phases could be detected. Moreover, the XRD results also show that all the as-dried powders still maintained the HA structure when DCPD underwent hydrolysis in 0.1 to 5 M NaOH(aq) at 348 K (75 °C) for 1 hour. Otherwise, the full transformation from HA to octa-calcium phosphate (OCP, Ca8H2(PO4)6·5H2O) occurred when hydrolysis happened in 10 M NaOH(aq). FT-IR spectra analysis revealed that some carbonated HA (Ca10(PO4)6(CO3), CHA) had formed. The SEM morphology results show that the 60 to 65 nm width of the uniformly long rods with regular alignment formed in the HA powder aggregates when DCPD underwent hydrolysis in 2.5 M NaOH(aq) at 348 K (75 °C) for 1 hour.

Effect of Co2+ Ions Doping on the Structural and Optical Properties of Magnesium Aluminate

NASA Astrophysics Data System (ADS)

Kanwal, Kiran; Ismail, Bushra; Rajani, K. S.; Kissinger, N. J. Suthan; Zeb, Aurang

2017-07-01

Cobalt-doped nanosized magnesium aluminate (Mg1-xCoxAl2O4) samples having different compositions ( x = 0.2, 0.4, 0.6, 0.8, 1.0) were synthesized by a chemical co-precipitation method. All samples were characterized by means of x-ray diffraction (XRD), scanning electron microscopy, Fourier transform infrared spectroscopy, ultra violet-visible spectroscopy, photoluminescence and diffused reflectance spectroscopy. The results of XRD revealed that the samples were spinel single phase cubic close packed crystalline materials. The lattice constant and x-ray density were found to be affected by the ionic radii of the doped metal cations. Using the Debye-Scherrer formula, the calculated crystalline size was found to be Co2+ ion concentration-dependent and varied between 32 nm and 40 nm. Nano-dimensions and phase of the Mg1-xCoxAl2O4 samples were analyzed and the replacement of Mg2+ ions with Co2+ ions was confirmed by elemental analysis. Three strong absorption bands at 540 nm, 580 nm and 630 nm were observed for the doped samples which are attributed to the three spin-allowed 4T1g (4F) → 4T2g, 4A2g, 4T1g (4P) electronic transitions of Co2+ at tetrahedral lattice sites. Nanophosphors have optical properties different from bulk because of spatial confinement and non-radiative relaxation. Decreases in particle size can increase the surface area and the defects, which can in turn increase the luminescent efficiency to make it very useful for tunable laser operations, persistent phosphorescence, color centers, photoconductivity and luminescence for display technology. MgAl2O4 was doped with Co2+ ions using a co-precipitation method and the optical absorption studies revealed that there is a decrease of band gap due to the increase of Co2+ content. The emission intensity of this phosphor is observed at 449 nm with a sharp peak attributed to the smaller size of the particles and the homogeneity of the powder.

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

Liu, Zhi-jie; Dai, Le-yang; Yang, De-zheng

Highlights: • A novel and high efficiency synthesizing AlN powders method combining mechanical ball milling and DBDP has been developed. • The particle size, the crystallite size, the lattice distortion, the morphology of Al{sub 2}O{sub 3} powders, and the AlN conversion rate are investigated and compared under the ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP. • The ball milled Al{sub 2}O{sub 3} powders with DBDP have small spherical structure morphology with very fine particles size and high specific surface area, which result in a higher chemical efficiency and a higher AlN conversion rate at lower thermalmore » temperature. - Abstract: In this paper, aluminum nitride (AlN) powers have been produced with a novel and high efficiency method by thermal annealing at 1100–1600 °C of alumina (Al{sub 2}O{sub 3}) powders which were previously ball milled for various time up to 40 h with and without the assistant of dielectric barrier discharge plasma (DBDP). The ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP and the corresponding synthesized AlN powers are characterized by X-ray diffraction, scanning electron microscope, and transmission electron microscopy. From the characteristics of the ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP, it can be seen that the ball milled Al{sub 2}O{sub 3} powders with DBDP have small spherical structure morphology with very fine particles size and high specific surface area, which result in a higher chemical efficiency and a higher AlN conversion rate at lower thermal temperature. Meanwhile, the synthesized AlN powders can be known as hexagonal AlN with fine crystal morphology and irregular lump-like structure, and have uniform distribution with the average particle size of about between 500 nm and 1000 nm. This provides an important method for fabricating ultra fine powders and synthesizing nitrogen compounds.« less

Phase Structures and Magnetic Properties of Graphite Nanosheets and Ni-Graphite Nanocomposite Synthesized by Electrical Explosion of Wire in Liquid

NASA Astrophysics Data System (ADS)

Nguyen, Minh-Thuyet; Kim, Jin-Hyung; Lee, Jung-Goo; Kim, Jin-Chun

2018-03-01

The present work studied on phases and magnetic properties of graphite nanosheets and Ni-graphite nanocomposite synthesized using the electrical explosion of wire (EEW) in ethanol. X-ray diffraction and field emission scanning electron microscope were used to investigate the phases and the morphology of the nanopowders obtained. It was found that graphite nanosheets were absolutely fabricated by EEW with a thickness of 29 nm and 3 μm diameter. The as-synthesized Ni-graphite composite powders had a Ni-coating on the surfaces of graphite sheets. The hysteresis loop of the as-exploded, the hydrogen-treated composite nanopowders and the sintered samples were examined with a vibrating sample magnetometer at room temperature. The Ni-graphite composite exposed the magnetic behaviors which are attributed to Ni component. The magnetic properties of composite had the improvement from 10.2 emu/g for the as-exploded powders to 15.8 emu/g for heat-treated powders and 49.16 emu/g for sintered samples.

Synthesis and characterization of CdO nano particles by the sol-gel method

NASA Astrophysics Data System (ADS)

Vadgama, V. S.; Vyas, R. P.; Jogiya, B. V.; Joshi, M. J.

2017-05-01

Cadmium Oxide (CdO) is an inorganic compound and one of the main precursors to other cadmium compounds. It finds applications in cadmium plating, storage batteries, in transparent conducting film, etc. Here, an attempt is made to synthesize CdO nano particles by sol-gel technique. The gel was prepared using cadmium nitrate tetra hydrate (Cd(NO3)2.4H2O) and aqueous ammonium hydroxide (NH4OH) as a precursor. The synthesized powder is further characterized by techniques like Powder X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Thermal gravimetric analysis (TGA). Powder XRD analysis suggested the nano-crystalline nature of the sample with the cubic crystal system. Nano scaled particles of spherical morphology with the size ranging from 50-100 nm are observed from TEM images. While, FT-IR study is used to confirm the presence of different functional groups. Thermo-gravimetric analysis suggests the highly thermally stable nature of the samples. The results are discussed.

Morphology and stability in a half-metallic ferromagnetic CrO 2 compound of nanoparticles synthesized via a polymer precursor

NASA Astrophysics Data System (ADS)

Biswas, S.; Ram, S.

2004-11-01

Nanoparticles of stable CrO2 of a half-metallic ferromagnet are synthesized with a novel chemical method involving a Cr4+-polymer composite precursor. A single phase CrO2 of D4h 14 : P42 / mnm tetragonal crystal structure (lattice parameters a = 0.4250 and c = 0.3190 nm) lies after firing the precursor at 350 °C for 1 h in air. Microstructure reveals single domain CrO2 particles of thin platelets (aspect ratio ∼1) of average 50 nm diameter and 35 nm thickness. In air, unless heating at temperatures above 500 °C, no due CrO2 → Cr2O3 phase transformation encounters. The results are presented in terms of X-ray diffraction and thermal or thermogravimetric analysis of precursor and derived CrO2 powder.

Luminescence studies of CdS spherical particles via hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Xu, Guo Qin; Liu, Bing; Xu, Shi Jie; Chew, Chwee Har; Chua, Soo Jin; Gana, Leong Ming

2000-06-01

The spherical particles of CdS consisting of nanoparticles (∼100 nm) were synthesized by a hydrothermal process. The particle formation and growth depend on the rate of sulfide-ion generation and diffusion-controlled aggregation of nanoparticles. As demonstrated in the profiles of powder X-ray diffraction, the crystalline phases are governed by the reaction temperature. Photoluminescence studies on CdS particles show two emission bands at the room temperature. The red emission at 680 nm is due to sulfur vacancies, and a new infrared red (IR) emission at 760 nm is attributed to self-activated centers. A red shift of IR band with the decrease of temperature was explained with a configurational coordinate model. The different saturation limits for the red and IR bands are discussed in terms of the formation of donor-acceptor pairs and exciton in CdS particles.

Combustion synthesis of MgO nanoparticles using plant extract: Structural characterization and photoluminescence studies

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

Kumar, Danith; Chikkahanumantharayappa; Yadav, L. S. Reddy

Magnesium oxide nanoparticles (MgO Nps) have been successfully synthesized via solution combustion method using Parthenium plant extract as fuel for the first time. Powder X-ray diffraction (PXRD) pattern reveal that product belongs to the cubic phase (Periclase). FTIR spectrum shows the band at 822 cm{sup −1} indicates the formation of cubic periclase MgO. The optical band gap of MgO Nps estimated from UV –Vis spectrum was found to be in the range 5.40–5.45 eV. SEM images showed that, the product is agglomerated and particle in nature. Photoluminescence (PL) studies shows violet emission at 390 nm, blue emission at 470 nm and green emissionmore » at 550 nm. MgO Nps shows good photocatalytic activity for the degradation of methylene blue (MB) dye under UV/Sun light irradiation.« less

The Effect of Sintering Temperature on Linear and Nonlinear Optical Properties of YAG Nanoceramics

NASA Astrophysics Data System (ADS)

Gayvoronsky, V. Ya.; Popov, A. S.; Brodyn, M. S.; Uklein, A. V.; Multian, V. V.; Shul'zhenko, O. O.

Recent improvements in powder synthesis and ceramics sintering made it possible to fabricate high-quality optical materials. The work is devoted to the structural and optical characterization of the ({Y_3}{Al_5}{O_{12}}, YAG) ceramics prepared by high-pressure low-temperature technique. The structural properties of the studied ceramic samples was obtained by X-ray diffraction. The studies of the total and in-line transmittance as well as optical scattering indicatrices were performed in visible and NIR ranges. The scatterer size ˜200 nm was estimated by Rayleigh-Gans-Debye model. It was shown that the studied samples demonstrate high transparency at 1064 nm. The nonlinear optical characterization of the samples was done by the self-action of the picosecond laser pulses at 1064 nm. The measured nonlinear optical response (χ^(3)) ˜ 10^{-11} esu) showed significant dependence on the sintering temperature variation.

Preparation and characterization of CdS/Si coaxial nanowires

NASA Astrophysics Data System (ADS)

Fu, X. L.; Li, L. H.; Tang, W. H.

2006-04-01

CdS/Si coaxial nanowires were fabricated via a simple one-step thermal evaporation of CdS powder in mass scale. Their crystallinities, general morphologies and detailed microstructures were characterized by using X-ray diffraction, scanning electron microscope, transmission electron microscope and Raman spectra. The CdS core crystallizes in a hexagonal wurtzite structure with lattice constants of a=0.4140 nm and c=0.6719 nm, and the Si shell is amorphous. Five Raman peaks from the CdS core were observed. They are 1LO at 305 cm -1, 2LO at 601 cm -1, A 1-TO at 212 cm -1, E 1-TO at 234 cm -1, and E 2 at 252 cm -1. Photoluminescence measurements show that the nanowires have two emission bands around 510 and 590 nm, which originate from the intrinsic transitions of CdS cores and the amorphous Si shells, respectively.

Synthesis of Zn1- x Co x Al2O4 Spinel Nanoparticles by Liquid-Feed Flame Spray Pyrolysis: Ceramic Pigments Application

NASA Astrophysics Data System (ADS)

Betancur Granados, Natalia; Yi, Eongyu; Laine, Richard M.; Restrepo Baena, Oscar Jaime

2016-01-01

Zn1- x Co x Al2O4 ( x = 0.0, 0.2, 0.4, 0.6, 0.8, and 1.0) spinel nanoparticles were synthesized by a liquid-feed flame spray pyrolysis (LF-FSP) method by combusting metallorganic precursor solutions to produce nanopowders with precise composition control. The precursor solutions were aerosolized into a methane/oxygen flame where it was combusted in an oxygen-rich environment to result in nanopowders at a single step. The nanopowders were analyzed by x-ray diffraction, Fourier transform infrared spectroscopy, colorimetry, field emission scanning electron microscopy, transmission electron microscopy, and BET (Brunauer-Emmett-Teller) N2 adsorption. Results show formation of spherical nanopowders with specific surface areas of 42 m2/g to 50 m2/g, which correspond to average particle sizes of 26 nm to 31 nm. Single-phase materials were obtained with a high control of composition, which indicates that LF-FSP is an excellent method to produce mixed-metal oxides for applications in which powder homogeneity is crucial. The products were evaluated for ceramic pigment application, where the ratio of Zn to Co was gradually changed to observe the color change in the structure with the increase of cobalt concentration. The resulting pigments were calcined at 1200°C, which aimed to identify the color stability after a high-temperature process, whereby the colors were measured using the color space CIE L*a*b* under standardized light, D65. Finally, the powders were tested for ceramic decoration using transparent glazes and ceramic bodies. The application was carried out at 1250°C to evaluate the color performance after a decoration process.

Synthesis of strontium substituted barium titanate nanoparticles by mechanical alloying and high power ultrasonication destruction

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

Yustanti, Erlina, E-mail: erlina.yustanti@ui.ac.id; Department of Metallurgy, Faculty of Engineering University of Sultan AgengTirtayasa Jl. Jenderal Sudirman KM 03 Cilegon-Banten 65134; Hafizah, Mas Ayu Elita, E-mail: kemasayu@yahoo.com

2016-04-19

This paper reports the particle and crystallite size characterizations of mechanically alloyed Ba{sub (1-x)}Sr{sub x}TiO{sub 3} (BST) with x = 0.3 and 0.7 prepared with the assistance of a high-power sonicator. Analytical grade BaCO{sub 3}, TiO{sub 2} and SrCO{sub 3} precursors with a purity of greater than 99 wt.% were mixed and milled using a planetary ball mill to a powder weight ratio of 10:1. Powders obtained after 20 hours of milling time were then sintered at 1200°C for 4 hours to form crystalline powders.These powders were further treated ultrasonically under a fixed 6.7 gr/l particle concentration in demineralized watermore » for 1, 3, 5, 7 hours and a fixed ultrasonic irradiation time of 1 hour to the dispersion of 6.7; 20; 33.3 gr/l concentrations. As to the results of crystallite size characterization, it is demonstrated that the mean crystallite size of BST with x = 0.3 and 0.7 undergo a slight change after the first 1 hour irradiation time and then remain almost unchanged. This was in contrary to the particle size in which the mean particle size of BST with x = 0.3 increased from 765 nm to 1405 nm after 7 hours irradiation time, while that of x = 0.7 increased from 505 nm to 1298 nm after 3 hours and then reduced back to the initial size after 7 hours ultra sonication time. The increase in particle size was due to large of cohesive forces among fine particles. It is also demonstrated that the concentration of particles in a dispersion with anionic surfactant do not effective to reduce the particle sizes ultrasonically. Nanoparticles with the mean size respectively 40 and 10 times larger than their respective crystallite size were successfully obtained respectively in x = 0.3 and x = 0.7.« less

Thermal and ultrasonic influence in the formation of nanometer scale hydroxyapatite bio-ceramic

PubMed Central

Poinern, GJE; Brundavanam, R; Le, X Thi; Djordjevic, S; Prokic, M; Fawcett, D

2011-01-01

Hydroxyapatite (HAP) is a widely used biocompatible ceramic in many biomedical applications and devices. Currently nanometer-scale forms of HAP are being intensely investigated due to their close similarity to the inorganic mineral component of the natural bone matrix. In this study nano-HAP was prepared via a wet precipitation method using Ca(NO3)2 and KH2PO4 as the main reactants and NH4OH as the precipitator under ultrasonic irradiation. The Ca/P ratio was set at 1.67 and the pH was maintained at 9 during the synthesis process. The influence of the thermal treatment was investigated by using two thermal treatment processes to produce ultrafine nano-HAP powders. In the first heat treatment, a conventional radiant tube furnace was used to produce nano-particles with an average size of approximately 30 nm in diameter, while the second thermal treatment used a microwave-based technique to produce particles with an average diameter of 36 nm. The crystalline structure and morphology of all nanoparticle powders produced were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR). Both thermal techniques effectively produced ultrafine powders with similar crystalline structure, morphology and particle sizes. PMID:22114473

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

Ce3+-doped LaF3 nanoparticles: Wet-chemical synthesis and photo-physical characteristics "optical properties of LaF3:Ce nanomaterials"

NASA Astrophysics Data System (ADS)

Tabatabaee, F.; Sabbagh Alvani, A. A.; Sameie, H.; Moosakhani, S.; Salimi, R.; Taherian, M.

2014-01-01

The most effective process parameters were determined to synthesize spherical LaF3 nanoparticles with controllable size based on ethylenediaminetetraacetic acid (EDTA) via co-precipitation technique. Thermogravimetricdifferential thermal analysis, X-ray diffraction, scanning electron microscopy, dynamic light scattering and FT-IR spectroscopy were used to characterize the resulting powders. Detailed investigations revealed that the optimal LaF3 host nano-material was obtained when NH4F was used as a fluoride source in the presence of EDTA at pH = 5. Furthermore, photoluminescence spectra showed an intense double emission peak at 289 and 302 nm for cerium-doped LaF3 nanocrystals excited at 253 nm, which was assigned to the well-known 5d→4f (2F5/2 and 2F7/2) transitions of Ce3+ levels due to luminescence center mechanism. The experimental results indicate that the synthesized LaF3:0.05Ce powders with a band gap of 5.3 eV are promising phosphors for high density scintillators.

A Novel Gas Sensor Based on MgSb2O6 Nanorods to Indicate Variations in Carbon Monoxide and Propane Concentrations

PubMed Central

Guillén-Bonilla, Héctor; Flores-Martínez, Martín; Rodríguez-Betancourtt, Verónica-María; Guillen-Bonilla, Alex; Reyes-Gómez, Juan; Gildo-Ortiz, Lorenzo; de la Luz Olvera Amador, María; Santoyo-Salazar, Jaime

2016-01-01

Bystromite (MgSb2O6) nanorods were prepared using a colloidal method in the presence of ethylenediamine, after a calcination step at 800 °C in static air. From X-ray powder diffraction analyses, a trirutile-type structure with lattice parameters a = 4.64 Å and c = 9.25 Å and space group P42/mnm was identified. Using scanning electron microscopy (SEM), microrods with sizes from 0.2 to 1.6 μm were observed. Transmission electron microscopy (TEM) analyses revealed that the nanorods had a length of ~86 nm and a diameter ~23.8 nm. The gas-sensing properties of these nanostructures were tested using pellets elaborated with powders of the MgSb2O6 oxide (calcined at 800 °C) at temperatures 23, 150, 200, 250 and 300 °C. The pellets were exposed to different concentrations of carbon monoxide (CO) and propane (C3H8) at these temperatures. The results showed that the MgSb2O6 nanorods possess excellent stability and high sensitivity in these atmospheres. PMID:26840318

A Novel Gas Sensor Based on MgSb2O6 Nanorods to Indicate Variations in Carbon Monoxide and Propane Concentrations.

PubMed

Guillén-Bonilla, Héctor; Flores-Martínez, Martín; Rodríguez-Betancourtt, Verónica-María; Guillen-Bonilla, Alex; Reyes-Gómez, Juan; Gildo-Ortiz, Lorenzo; de la Luz Olvera Amador, María; Santoyo-Salazar, Jaime

2016-01-30

Bystromite (MgSb2O6) nanorods were prepared using a colloidal method in the presence of ethylenediamine, after a calcination step at 800 °C in static air. From X-ray powder diffraction analyses, a trirutile-type structure with lattice parameters a = 4.64 Å and c = 9.25 Å and space group P4₂/mnm was identified. Using scanning electron microscopy (SEM), microrods with sizes from 0.2 to 1.6 μm were observed. Transmission electron microscopy (TEM) analyses revealed that the nanorods had a length of ~86 nm and a diameter ~23.8 nm. The gas-sensing properties of these nanostructures were tested using pellets elaborated with powders of the MgSb2O6 oxide (calcined at 800 °C) at temperatures 23, 150, 200, 250 and 300 °C. The pellets were exposed to different concentrations of carbon monoxide (CO) and propane (C3H8) at these temperatures. The results showed that the MgSb2O6 nanorods possess excellent stability and high sensitivity in these atmospheres.

Large-scale synthesis of ear-like Si{sub 3}N{sub 4} dendrites from SiO{sub 2}/Fe composites and Si powders

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

Wang Feng; Graduate School of the Chinese Academy of Sciences, Beijing 100039; Jin Guoqiang

2008-07-01

Large-scale ear-like Si{sub 3}N{sub 4} dendrites were prepared by the reaction of SiO{sub 2}/Fe composites and Si powders in N{sub 2} atmosphere. The product was characterized by field emission scanning electron microscopy, X-ray diffraction, and transmission electron microscopy. The results reveal that the product mainly consists of ear-like Si{sub 3}N{sub 4} dendrites with crystal structures, which have a length of several microns and a diameter of 100-200 nm. Nanosized ladder-like Si{sub 3}N{sub 4} was also obtained when changing the Fe content in the SiO{sub 2}/Fe composites. The Si{sub 3}N{sub 4} nanoladders have a length of hundreds nanometers to several micronsmore » and a width of 100-300 nm. The ear-like Si{sub 3}N{sub 4} dendrites are formed from a two-step growth process, the formation of inner stem structures followed by the epitaxial growth of secondary branches.« less

Study on optical properties of L-valine doped ADP crystal

NASA Astrophysics Data System (ADS)

Shaikh, R. N.; Anis, Mohd.; Shirsat, M. D.; Hussaini, S. S.

2015-02-01

Single crystal of L-valine doped ammonium dihydrogen phosphate has been grown by slow evaporation method at room temperature. The crystalline nature of the grown crystal was confirmed using powder X-ray diffraction technique. The different functional groups of the grown crystal were identified using Fourier transform infrared analysis. The UV-visible studies were employed to examine the high optical transparency and influential optical constants for tailoring materials suitability for optoelectronics applications. The cutoff wavelength of the title crystal was found to be 280 nm with wide optical band gap of 4.7 eV. The dielectric measurements were carried to determine the dielectric constant and dielectric loss at room temperature. The grown crystal has been characterized by thermogravimetric analysis. The second harmonic generation efficiency of the grown crystal was determined by the classical Kurtz powder technique and it is found to be 1.92 times that of potassium dihydrogen phosphate. The grown crystal was identified as third order nonlinear optical material employing Z-scan technique using He-Ne laser operating at 632.8 nm.

Synthetic aspects, spectral, thermal studies and antimicrobial screening on bis(N,N-dimethyldithiocarbamato-S,S‧)antimony(III) complexes with oxo or thio donor ligands

NASA Astrophysics Data System (ADS)

Chauhan, H. P. S.; Carpenter, Jaswant; Joshi, Sapana

2014-09-01

The bis(N,N-dimethyldithiocarbamato-S,S‧)antimony(III) complexes have been obtained by the reaction of chloro bis(N,N-dimethyldithiocarbamato-S,S‧)antimony(III) with corresponding oxo or thio donor ligands such as sodium benzoate 1, sodium thioglycolate 2, phenol 3, sodium 1-propanethiolate 4, potassium thioacetate 5, sodium salicylate 6, ethane-1,2-dithiolate 7 and disodium oxalate 8. These complexes have been characterized by the physicochemical [melting point, molecular weight determination and elemental analysis (C, H, N, S and Sb)], spectral [UV-Visible, FT-IR, far IR, NMR (1H and 13C)], thermogravimetric (TG & DTA) analysis, ESI-Mass and powder X-ray diffraction studies. Thermogravimetric analysis of the complexes confirmed the final decomposition product as highly pure antimony sulfide (Sb2S3) and powder X-ray diffraction studies show that the complexes are in lower symmetry with monoclinic crystal lattice and nano-ranged particle size (11.51-20.82 nm). The complexes have also been screened against some bacterial and fungal strains for their antibacterial and antifungal activities and compared with standard drugs. These show that the complexes have greater activities against some human pathogenic bacteria and fungi than the activities of standard drugs.

Analysis of a nanocrystalline polymer dispersion of ebselen using solid-state NMR, Raman microscopy, and powder X-ray diffraction.

PubMed

Vogt, Frederick G; Williams, Glenn R

2012-07-01

Nanocrystalline drug-polymer dispersions are of significant interest in pharmaceutical delivery. The purpose of this work is to demonstrate the applicability of methods based on two-dimensional (2D) and multinuclear solid-state NMR (SSNMR) to a novel nanocrystalline pharmaceutical dispersion of ebselen with polyvinylpyrrolidone-vinyl acetate (PVP-VA), after initial characterization with other techniques. A nanocrystalline dispersion of ebselen with PVP-VA was prepared and characterized by powder X-ray diffraction (PXRD), confocal Raman microscopy and mapping, and differential scanning calorimetry (DSC), and then subjected to detailed 1D and 2D SSNMR analysis involving ¹H, ¹³C, and ⁷⁷Se isotopes and ¹H spin diffusion. PXRD was used to show that dispersion contains nanocrystalline ebselen in the 35-60 nm size range. Confocal Raman microscopy and spectral mapping were able to detect regions where short-range interactions may occur between ebselen and PVP-VA. Spin diffusion effects were analyzed using 2D SSNMR experiments and are able to directly detect interactions between ebselen and the surrounding PVP-VA. The methods used here, particularly the 2D SSNMR methods based on spin diffusion, provided detailed structural information about a nanocrystalline polymer dispersion of ebselen, and should be useful in other studies of these types of materials.

Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

NASA Astrophysics Data System (ADS)

Aivazoglou, E.; Metaxa, E.; Hristoforou, E.

2018-04-01

The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG) or PEG and β-cyclodextrin (β-CD)/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD), Transition Electron Microscopy (TEM), Fourier-transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Vibrating Sample Magnetometer (VSM), X-Ray Photoelectron Spectroscopy (XPS) and Thermal analysis (TG/DSC). The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

Crystal structure and phase transformations of calcium yttrium orthophosphate, Ca 3Y(PO 4) 3

NASA Astrophysics Data System (ADS)

Fukuda, Koichiro; Iwata, Tomoyuki; Niwa, Takahiro

2006-11-01

Crystal structure and phase transformations of calcium yttrium orthophosphate Ca 3Y(PO 4) 3 were investigated by X-ray powder diffraction, selected-area electron diffraction, transmission electron microscopy and optical microscopy. The high-temperature phase is isostructural with eulytite, cubic (space group I4¯3d) with a=0.983320(5) nm, V=0.950790(8) nm 3, Z=4 and D x=3.45 Mg m -3. The crystal structure was refined with a split-atom model, in which the oxygen atoms are distributed over two partially occupied sites. Below the stable temperature range of eulytite, the crystal underwent a martensitic transformation, which is accompanied by the formation of platelike surface reliefs. The inverted crystal is triclinic (space group P1) with a=1.5726(1) nm, b=0.84267(9) nm, c=0.81244(8) nm, α=109.739(4)°, β=90.119(5)°, γ=89.908(7)°, V=1.0134(1) nm 3, Z=4 and D x=3.24 Mg m -3. The crystal grains were composed of pseudo-merohedral twins. The adjacent twin domains were related by the pseudo-symmetry mirror planes parallel to {101¯} with the composition surface {101¯}. When the eulytite was cooled relatively slowly from the stable temperature range, the decomposition reaction of Ca 3Y(PO 4) 3→ β-Ca 3(PO 4) 2+YPO 4 occurred.

Preparation and Characterization of Nano-CL-20 Explosive

NASA Astrophysics Data System (ADS)

Bayat, Yadollah; Zeynali, Vida

2011-10-01

Nano-CL-20 was prepared via precipitative crystallization by spraying a solution of CL-20 in a solvent (ethyl acetate) into a nonsolvent (isooctane). Scanning electron microscopy (SEM) and X-ray powder diffraction (XRD) were used to characterize the appearance and the size of the particles. The results revealed that nano-CL-20 particles have the shape of spheres or ellipsoids with an average size of 95 nm. Due to their small diameter and high surface energy, the particles tended to agglomerate. Impact sensitivity of nanosize CL-20 was decreased in comparison to micrometer-size CL-20.

Synthesis of mesoporous silica materials (MCM-41) from iron ore tailings

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

Yu Honghao, E-mail: honghaoyu@hotmail.com; College of Material Science and Engineering, Shenyang Ligong University, Shenyang, 110168; Xue Xiangxin

2009-11-15

Highly ordered mesoporous materials were successfully synthesized by using the iron ore tailings as the silica source and n-hexadecyltrimethyl ammonium bromide as the template. The samples were detail characterized by powder X-ray diffraction, scanning electron microscope, high-resolution transmission electron microscopy and N{sub 2} physisorption. The as-synthesized materials had high surface area of 527 m{sup 2} g{sup -1} and the mean pore diameter of 2.65 nm with a well-ordered two-dimensional hexagonal structure. It is feasible to prepare mesoporous MCM-41 materials using the iron ore tailings as precursor.

The effect of nanoparticles size on photocatalytic and antimicrobial properties of Ag-Pt/TiO2 photocatalysts

NASA Astrophysics Data System (ADS)

Zielińska-Jurek, Anna; Wei, Zhishun; Wysocka, Izabela; Szweda, Piotr; Kowalska, Ewa

2015-10-01

Ag-Pt-modified TiO2 nanocomposites were synthesized using the sol-gel method. Bimetallic modified TiO2 nanoparticles exhibited improved photocatalytic activity under visible-light irradiation, better than monometallic Ag/TiO2 and Pt/TiO2 nanoparticles (NPs). All modified powders showed localized surface plasmon resonance (LSPR) in visible region. The photocatalysts' characteristics by X-ray diffractometry (XRD), scanning transmission electron microscopy (STEM), diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption (BET method for specific surface area) showed that sample with the highest photocatalytic activity had anatase structure, about 93 m2/g specific surface area, maximum plasmon absorption at ca. 420 nm and contained small NPs of silver of 6 nm and very fine platinum NPs of 3 nm. The photocatalytic activity was estimated by measuring the decomposition rate of phenol in 0.2 mM aqueous solution under Vis and UV/vis light irradiation. It was found that size of platinum was decisive for the photocatalytic activity under visible light irradiation, i.e., the smaller Pt NPs were, the higher was photocatalytic activity. While, antimicrobial activities, estimated for bacteria Escherichia coli and Staphylococcus aureus, and pathogenic fungi belonging to Candida family, were only observed for photocatalysts containing silver, i.e., Ag/TiO2 and Ag-Pt/TiO2 nanocomposites.

X-ray diffraction studies of shocked lunar analogs

NASA Technical Reports Server (NTRS)

Hanss, R. E.

1979-01-01

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

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

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

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Relative impact of H2O and O2 in the oxidation of UO2 powders from 50 to 300 °C

NASA Astrophysics Data System (ADS)

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; Roberts, Sarah K.; Nelson, Art J.

2017-12-01

The reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO2) powder at elevated temperature was studied by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). Oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice was observed and quantified. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

DOE PAGES

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; ...

2017-10-04

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

NASA Astrophysics Data System (ADS)

Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

2018-04-01

A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

Challenges in Additive Manufacturing of Space Parts: Powder Feedstock Cross-Contamination and Its Impact on End Products

PubMed Central

Brandão, Ana D.; Gerard, Romain; Gumpinger, Johannes; Beretta, Stefano; Makaya, Advenit; Pambaguian, Laurent; Ghidini, Tommaso

2017-01-01

This work studies the tensile properties of Ti-6Al-4V samples produced by laser powder bed based Additive Manufacturing (AM), for different build orientations. The results showed high scattering of the yield and tensile strength and low fracture elongation. The subsequent fractographic investigation revealed the presence of tungsten particles on the fracture surface. Hence, its detection and impact on tensile properties of AM Ti-6Al-4V were investigated. X-ray Computed Tomography (X-ray CT) scanning indicated that these inclusions were evenly distributed throughout the samples, however the inclusions area was shown to be larger in the load-bearing plane for the vertical specimens. A microstructural study proved that the mostly spherical tungsten particles were embedded in the fully martensitic Ti-6Al-4V AM material. The particle size distribution, the flowability and the morphology of the powder feedstock were investigated and appeared to be in line with observations from other studies. X-ray CT scanning of the powder however made the high density particles visible, where various techniques, commonly used in the certification of powder feedstock, failed to detect the contaminant. As the detection of cross contamination in the powder feedstock proves to be challenging, the use of only one type of powder per AM equipment is recommended for critical applications such as Space parts. PMID:28772882

Challenges in Additive Manufacturing of Space Parts: Powder Feedstock Cross-Contamination and Its Impact on End Products.

PubMed

Brandão, Ana D; Gerard, Romain; Gumpinger, Johannes; Beretta, Stefano; Makaya, Advenit; Pambaguian, Laurent; Ghidini, Tommaso

2017-05-12

This work studies the tensile properties of Ti-6Al-4V samples produced by laser powder bed based Additive Manufacturing (AM), for different build orientations. The results showed high scattering of the yield and tensile strength and low fracture elongation. The subsequent fractographic investigation revealed the presence of tungsten particles on the fracture surface. Hence, its detection and impact on tensile properties of AM Ti-6Al-4V were investigated. X-ray Computed Tomography (X-ray CT) scanning indicated that these inclusions were evenly distributed throughout the samples, however the inclusions area was shown to be larger in the load-bearing plane for the vertical specimens. A microstructural study proved that the mostly spherical tungsten particles were embedded in the fully martensitic Ti-6Al-4V AM material. The particle size distribution, the flowability and the morphology of the powder feedstock were investigated and appeared to be in line with observations from other studies. X-ray CT scanning of the powder however made the high density particles visible, where various techniques, commonly used in the certification of powder feedstock, failed to detect the contaminant. As the detection of cross contamination in the powder feedstock proves to be challenging, the use of only one type of powder per AM equipment is recommended for critical applications such as Space parts.

NASA Astrophysics Data System (ADS)

Wang, Mao-Hua; Zhang, Bo; Zhou, Fu

2014-07-01

Silica was homogeneously coated on the surface of CaCu3Ti4O12 (CCTO) particles via the sol-gel method. The obtained powders were characterized by x-ray diffraction analysis, Fourier-transform infrared spectroscopy, transmission electron microscopy (TEM), energy-dispersive spectroscopy, scanning electron microscopy, and zeta potential analysis. The results demonstrate that there were silica layers on the surface of the CCTO particles. Physical and dielectric properties of silica-coated CCTO were also studied. TEM imaging showed that the thickness of the silica layer on the CCTO particles was about 20 nm to 35 nm. The specimen coated with 1.0 wt.% silica showed the maximum relative density of 96.7% with high dielectric constant (12.78 × 104) and low dielectric loss (0.005) at 20°C after sintering at 1000°C for 6 h.

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.

Controlled phase evolution and the occurrence of single domain CoFe2O4 nanoparticles synthesized by PVA assisted sol-gel method

NASA Astrophysics Data System (ADS)

Srinivasa Rao, K.; Ranga Nayakulu, S. V.; Chaitanya Varma, M.; Choudary, G. S. V. R. K.; Rao, K. H.

2018-04-01

The present investigation describes the development of cobalt ferrite nanoparticles having size less than 10 nm, by a sol-gel method using polyvinyl alcohol as chelating agent. X-ray results show all the samples, annealed above 700 °C have spinel structure. The information about phase evolution with reaction temperatures was obtained by subjecting the as-prepared powder for DSC/TGA study. High saturation magnetization of 84.63 emu/g has been observed for a particle size of 8.1 nm, a rare event reported till date. The dM/dH versus H curves suggest that the transition from single domain state to multi-domain state occurs with increasing annealing temperature and the critical size for the single domain nature of CoFe2O4 is around 6.5 nm. The estimated critical diameter for single domain particle (6.7 nm) is in good agreement with that (6.5 nm) obtained from Transmission Electron Micrographs. The highest coercivity (1645 Oe) has been found for a particle of size 6.5 nm.

Growth of single crystals, thermal dependency of lattice parameters and Raman scattering in the Nd 2- xCe xCuO 4- δ system

NASA Astrophysics Data System (ADS)

Sadowski, W.; Hagemann, H.; François, M.; Bill, H.; Peter, M.; Walker, E.; Yvon, K.

1990-09-01

We report on the growth of Nd 2- xCe xCuO 4- δ single crystals (0< x<0.2) from Cu 2O flux. Free separated crystals with maximum size of 5x8x0.15 nm 3 have been obtained. Magnetic AC susceptibility measurements show a sharp superconducting transition at temperatures up to 23 K. The temperature dependence of the lattice parameters has been measured by means of X-ray powder diffraction between 10 K ( a=3.9413(3) Å, c=12.0290(18) Å) and 290 K ( a=3.9482(3) Å, c=12.0590(18) Å). Room temperature Raman spectra reveal a new band at 320 cm -1 which is not observed in Nd 2CuO 4. Raman spectra of crystals with Tc ranging from 7 to 22 K show a systematic intensity change of the broad band at 590 cm -1.

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.

Near-infrared photoluminescence in La0.98AlO3: 0.02Ln3+(Ln = Nd/Yb) for sensitization of c-Si solar cells

NASA Astrophysics Data System (ADS)

Sawala, N. S.; Koparkar, K. A.; Bajaj, N. S.; Omanwar, S. K.

2016-05-01

The host matrix LaAlO3 was synthesized by conventional solid state reaction method in which the Nd3+ ions and Yb3+ ions successfully doped at 2mol% concentrations. The phase purity was confirmed by X ray powder diffraction (XRD) method. The photoluminescence (PL) properties were studied by spectrophotometer in near infra red (NIR) and ultra violet visible (UV-VIS) region. The Nd3+ ion doped LaAlO3 converts a visible (VIS) green photon (587 nm) into near infrared (NIR) photon (1070 nm) while Yb3+ ion doped converts ultra violet (UV) photon (221 nm) into NIR photon (980 nm). The La0.98AlO3: 0.02Ln3+(Ln = Nd / Yb) can be potentiality used for betterment of photovoltaic (PV) technology. This result further indicates its potential application as a luminescence converter layer for enhancing solar cells performance.

Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders

PubMed Central

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong

2017-01-01

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH4)2C2O4·H2O and Na2CO3) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7–10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na2CO3 precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed. PMID:28934147

Effect of Graphite Powder Amount on Surface Films Formed on Molten AZ91D Alloy

NASA Astrophysics Data System (ADS)

Li, Weihong; Zhou, Jixue; Ma, Baichang; Wang, Jinwei; Wu, Jianhua; Yang, Yuansheng

2017-10-01

Graphite powder was adopted to prevent AZ91D magnesium alloy from oxidizing during the melting and casting process. The microstructure of the resultant surface films formed on the molten alloy protected by 0, 2.7, 5.4, 8.1, and 10.8 g dm-2 graphite powder at 973 K (700 °C) for holding time of 30 minutes was investigated by scanning electron microscopy, energy dispersive spectrometer, X-ray diffraction, and the thermodynamic method. The results indicated that the surface films were composed of a protective layer and the underneath MgF2 particles with different morphology. The protective layer was continuous with a thickness range from 200 to 550 nm consisting of magnesium, oxygen, fluorine, carbon, and a small amount of aluminium, possibly existing in the form of MgO, MgF2, C, and MgAl2O4. The surface films were the result of the interaction between the graphite powder, the melt, and the ambient atmosphere. The unevenness of the micro surface morphology and the number and size of the underneath MgF2 particles increased with graphite powder amount. The mechanism of the effect of graphite powder amount on the resultant surface films was also discussed.

Tungsten carbide precursors as an example for influence of a binder on the particle formation in the nanosecond laser ablation of powdered materials.

PubMed

Holá, Markéta; Mikuska, Pavel; Hanzlíková, Renáta; Kaiser, Jozef; Kanický, Viktor

2010-03-15

A study of LA-ICP-MS analysis of pressed powdered tungsten carbide precursors was performed to show the advantages and problems of nanosecond laser ablation of matrix-unified samples. Five samples with different compositions were pressed into pellets both with silver powder as a binder serving to keep the matrix unified, and without any binder. The laser ablation was performed by nanosecond Nd:YAG laser working at 213 nm. The particle formation during ablation of both sets of pellets was studied using an optical aerosol spectrometer allowing the measurement of particle concentration in two size ranges (10-250 nm and 0.25-17 microm) and particle size distribution in the range of 0.25-17 microm. Additionally, the structure of the laser-generated particles was studied after their collection on a filter using a scanning electron microscope (SEM) and the particle chemical composition was determined by an energy dispersive X-ray spectroscope (EDS). The matrix effect was proved to be reduced using the same silver powdered binder for pellet preparation in the case of the laser ablation of powdered materials. The LA-ICP-MS signal dependence on the element content present in the material showed an improved correlation for Co, Ti, Ta and Nb of the matrix-unified samples compared to the non-matrix-unified pellets. In the case of W, the ICP-MS signal of matrix-unified pellets was influenced by the changes in the particle formation. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Study of crystal structure and unique photoluminescence properties of Eu2-xFexO3 (x = 0 - 0.5) orthoferrites

NASA Astrophysics Data System (ADS)

Dhilip, M.; Anbarasu, V.; Kumar, K. Saravana; Sivakumar, K.

2018-04-01

A series of Europium orthoferrites, Eu2-xFexO3 (x = 0 - 0.5) are successfully prepared by employing solid state reaction technique. The structural analysis through powder X-Ray diffraction technique reveals the multiphase formation of all the prepared compounds. Further, the unit cell visualization of all the prepared compounds confirms the change of crystal structure from cubic to orthorhombic phase. The crystal structure analysis confirms the typical framework of Eu - Fe - O chains with unprecedented ratio of Eu3+ and Fe3+ ions. The optical properties of prepared compounds are investigated using photoluminescence (PL) analysis. Upon excitation at 495 nm wavelength, the emission spectrum of prepared compounds exhibits a broad band in the range of 500-700nm with maximum intensity peak at 548 nm (Blue - 2.26eV). Hence, the substitution of Fe3+ ion yields with intrinsic blue photoluminescence (5D0 → 7F0) of Eu3+ and is easily shielded by the substitution of Fe3+ which may be due to the closer conduction band gap of Eu3+ (2.26 eV) with Fe3+ (2.67 eV). The schematic energy level diagram for Fe3+ in the Eu3+ host matrix has been proposed for the better understanding of photoluminescence processes. The variation of intensity of PL peak between 500 and 700 nm for the substitution of Fe in the range of x = 0 - 0.5 yields with interesting optical properties for exploring new phosphor materials for optoelectronic device fabrications.

Single-pulse coherent diffraction imaging using soft x-ray laser.

PubMed

Kang, Hyon Chol; Kim, Hyung Taek; Kim, Sang Soo; Kim, Chan; Yu, Tae Jun; Lee, Seong Ku; Kim, Chul Min; Kim, I Jong; Sung, Jae Hee; Janulewicz, Karol A; Lee, Jongmin; Noh, Do Young

2012-05-15

We report a coherent diffraction imaging (CDI) using a single 8 ps soft x-ray laser pulse at a wavelength of 13.9 nm. The soft x-ray pulse was generated by a laboratory-scale intense pumping laser providing coherent x-ray pulses up to the level of 10(11) photons/pulse. A spatial resolution below 194 nm was achieved with a single pulse, and it was shown that a resolution below 55 nm is feasible with improved detector capability. The single-pulse CDI might provide a way to investigate dynamics of nanoscale molecules or particles.

Synthesis of strontium substituted barium titanate nanoparticles by mechanical alloying and high power ultrasonication destruction

NASA Astrophysics Data System (ADS)

Yustanti, Erlina; Hafizah, Mas Ayu Elita; Manaf, Azwar

2016-04-01

This paper reports the particle and crystallite size characterizations of mechanically alloyed Ba(1-x)SrxTiO3 (BST) with x = 0.3 and 0.7 prepared with the assistance of a high-power sonicator. Analytical grade BaCO3, TiO2 and SrCO3 precursors with a purity of greater than 99 wt.% were mixed and milled using a planetary ball mill to a powder weight ratio of 10:1. Powders obtained after 20 hours of milling time were then sintered at 1200°C for 4 hours to form crystalline powders.These powders were further treated ultrasonically under a fixed 6.7 gr/l particle concentration in demineralized water for 1, 3, 5, 7 hours and a fixed ultrasonic irradiation time of 1 hour to the dispersion of 6.7; 20; 33.3 gr/l concentrations. As to the results of crystallite size characterization, it is demonstrated that the mean crystallite size of BST with x = 0.3 and 0.7 undergo a slight change after the first 1 hour irradiation time and then remain almost unchanged. This was in contrary to the particle size in which the mean particle size of BST with x = 0.3 increased from 765 nm to 1405 nm after 7 hours irradiation time, while that of x = 0.7 increased from 505 nm to 1298 nm after 3 hours and then reduced back to the initial size after 7 hours ultra sonication time. The increase in particle size was due to large of cohesive forces among fine particles. It is also demonstrated that the concentration of particles in a dispersion with anionic surfactant do not effective to reduce the particle sizes ultrasonically. Nanoparticles with the mean size respectively 40 and 10 times larger than their respective crystallite size were successfully obtained respectively in x = 0.3 and x = 0.7.

High-resolution x-ray tomography using laboratory sources

NASA Astrophysics Data System (ADS)

Tkachuk, Andrei; Feser, Michael; Cui, Hongtao; Duewer, Fred; Chang, Hauyee; Yun, Wenbing

2006-08-01

X-ray computed tomography (XCT) is a powerful nondestructive 3D imaging technique, which enables the visualization of the three dimensional structure of complex, optically opaque samples. High resolution XCT using Fresnel zone plate lenses has been confined in the past to synchrotron radiation centers due to the need for a bright and intense source of x-rays. This confinement severely limits the availability and accessibility of x-ray microscopes and the wide proliferation of this methodology. We are describing a sub-50nm resolution XCT system operating at 8 keV in absorption and Zernike phase contrast mode based on a commercially available laboratory x-ray source. The system utilizes high-efficiency Fresnel zone plates with an outermost zone width of 35 nm and 700 nm structure height resulting in a current spatial resolution better than 50 nm. In addition to the technical description of the system and specifications, we present application examples in the semiconductor field.

XAFS and X-Ray and Electron Microscopy Investigations of Radionuclide Transformations at the Mineral-Microbe Interface

NASA Astrophysics Data System (ADS)

Kemner, Ken; O'Loughlin, Ed; Kelly, Shelly; Ravel, Bruce; Boyanov, Maxim; Sholto-Douglas, Deirdre; Lai, Barry; Cook, Russ; Carpenter, Everett; Harris, Vince; Nealson, Ken

2007-02-01

The microenvironment at and adjacent to surfaces of actively metabolizing cells, whether in a planktonic state or adhered to mineral surfaces, can be significantly different from the bulk environment. Microbial polymers (polysaccharides, DNA, RNA, and proteins), whether attached to or released from the cell, can contribute to the development of steep chemical gradients over very short distances. It is currently difficult to predict the behavior of contaminant radionuclides and metals in such microenvironments, because the chemistry there has been difficult or impossible to define. The behavior of contaminants in such microenvironments can ultimately affect their macroscopic fates. We have successfully performed a series of U LIII edge x-ray absorption fine structure (XAFS) spectroscopy, hard x-ray fluorescence (XRF) microprobe (150 nm resolution), and electron microscopy (EM) measurements on lepidocrocite thin films (˜1 micron thickness) deposited on kapton films that have been inoculated with the dissimilatory metal reducing bacterium Shewanella oneidensis MR-1 and exposed to 0.05 mM uranyl acetate under anoxic conditions. Similarly, we have performed a series of U LIII edge EXAFS measurements on lepidocrocite powders exposed to 0.05 mM uranyl acetate and exopolymeric components harvested from S. oneidensis MR-1 grown under aerobic conditions. These results demonstrate the utility of combining bulk XAFS with x-ray and electron microscopies.

New Possibilities for Understanding Complex Metal Hydrides via Synchrotron X-ray Studies

NASA Astrophysics Data System (ADS)

Dobbins, Tabbetha

2008-03-01

Ultrasmall-angle x-ray scattering (USAXS) and X-ray absorption spectroscopy (XAS) are used for the study of chemical and morphological changes in metal hydride powder (e.g. NaAlH4) both before and after transition metal salt catalytic dopant additions by high energy ball milling. The variation in surface fractal dimension and particle size with milling time and dopant content were tracked. These studies show that dopant content level (e.g. 2 mol % and 4 mol %) and dopant type (i.e. TiCl2, TiCl3, VCl3, and ZrCl4) markedly affects NaAlH4 powder particle surface area (determined using USAXS surface fractal dimension). As well, the chemical reaction between the catalyst and hydride powder was further elucidated using XAS. Ti-metal reacts with the Al desorption product (from NaAlH4) to form TiAlx product phases. These studies were able to link powder particle surface area to catalytic doping and were able to link dopant chemical state with dehydrogenation reactant and product phases.

Nano-Crystalline Thermally Evaporated Bi2Se3 Thin Films Synthesized from Mechanically Milled Powder

NASA Astrophysics Data System (ADS)

Amara, A.; Abdennouri, N.; Drici, A.; Abdelkader, D.; Bououdina, M.; Chaffar Akkari, F.; Khemiri, N.; Kanzari, M.; Bernède, J. C.

2017-08-01

Bi2Se3 powder has been successfully synthesized via mechanical ball milling of bismuth and selenium as starting materials. X-ray diffraction characterization revealed the formation of the rhombohedral and orthorhombic phases of Bi2Se3 material belonging to systems with space groups R\\bar{3}m and Pbnm, respectively. The advantageous last finding is confirmed by the Rietveld refinement of the x-ray diffraction data. Furthermore, the analysis of the x-ray data of thermally deposited thin films revealed that both orthorhombic and rhombohedral phases are coexisting in the layer. The morphology of the ball milled powder was studied by scanning electron microscopy. The phase formation of the material is confirmed by Raman spectroscopy. M-H (Magnetization versus Magnetic field) curve indicates that Bi2Se3 powder has a ferromagnetic behavior. Additionally, absorbance and transmittance measurements were carried out on the obtained thermally evaporated thin films and yielded a band gap of 1.33 eV supporting the potential application of the heterogeneous rhombohedral/orthorhombic Bi2Se3 material in photovoltaics.

X-Ray Diffraction of Intermetallic Compounds: A Physical Chemistry Laboratory Experiment

ERIC Educational Resources Information Center

Varberg, Thomas D.; Skakuj, Kacper

2015-01-01

Here we describe an experiment for the undergraduate physical chemistry laboratory in which students synthesize the intermetallic compounds AlNi and AlNi3 and study them by X-ray diffractometry. The compounds are synthesized in a simple one-step reaction occurring in the solid state. Powder X-ray diffractograms are recorded for the two compounds…

X-ray chemical analyzer for field applications

DOEpatents

Gamba, Otto O. M.

1977-01-01

A self-supporting portable field multichannel X-ray chemical analyzer system comprising a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an X-ray energy dispersive spectrometry technique.

Enhanced luminescence in Mg{sup 2+} codoped CaTiO{sub 3}:Eu{sup 3+} phosphor prepared by solid state reaction

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

Vandana, C. Sai; Rudramadevi, B. Hemalatha

2016-05-23

CaTiO{sub 3} phosphors doped with Eu{sup 3+} and codoped with Mg{sup 2+} were prepared by Solid State Reaction method. The powders were characterized by X-ray diffraction, SEM with EDS, Raman scattering, and photoluminescence spectroscopy. The Crystalline phase and vibrational modes of the phosphors were studied using XRD pattern and Raman Spectrum respectively. The morphological studies of the phosphor samples were carried out using SEM analysis. From PL spectra we have observed two prominent red emission peaks around at 595 nm ({sup 5}D{sub 0}→{sup 7}F{sub 1}), 619 nm ({sup 5}D{sub 0}→{sup 7}F{sub 2}) with the excitation of 399 nm for Eu{supmore » 3+} doped CaTiO{sub 3} powders. The PL intensity of CaTiO{sub 3}:Eu{sup 3+} phosphor is enhanced significantly on codoping with Mg{sup 2+}. The observed enhanced emissions are due to energy transfer from Mg{sup 2+} to Eu{sup 3+}, which is due to radiative recombination. Eu{sup 3+} doped phosphors are well known to be promising materials for electroluminescent devices, optical amplifiers, and lasers.« less

Technological Challenges to X-Ray FELs

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

Nuhn, Heinz-Dieter

1999-09-16

There is strong interest in the development of x-ray free electron lasers (x-ray FELs). The interest is driven by the scientific opportunities provided by intense, coherent x-rays. An x-ray FEL has all the characteristics of a fourth-generation source: brightness several orders of magnitude greater than presently achieved in third-generation sources, full transverse coherence, and sub-picosecond long pulses. The SLAC and DESY laboratories have presented detailed design studies for X-Ray FEL user facilities around the 0.1 nm wavelength-regime (LCLS at SLAC, TESLA X-Ray FEL at DESY). Both laboratories are engaged in proof-of-principle experiments are longer wavelengths (TTF FEL Phase I atmore » 71 nm, VISA at 600-800 nm) with results expected in 1999. The technologies needed to achieve the proposed performances are those of bright electron sources, of acceleration systems capable of preserving the brightness of the source, and of undulators capable of meeting the magnetic and mechanical tolerances that are required for operation in the SASE mode. This paper discusses the technological challenges presented by the X-Ray FEL projects.« less

Synchrotron hard X-ray imaging of shock-compressed metal powders

NASA Astrophysics Data System (ADS)

Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

2015-06-01

This poster will present the application of a new, high-energy (50 to 250 keV) synchrotron X-ray radiography technique to the study of shock-compressed granular materials. Following plate-impact loading, transmission radiography was used to quantitatively observe the compaction and release processes in a range of high-Z metal powders (e.g. Fe, Ni, Cu). By comparing the predictions of 3D numerical models initialized from X-ray tomograms-captured prior to loading-with experimental results, this research represents a new approach to refining mesoscopic compaction models. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

Additional evidence from x-ray powder diffraction patterns that icosahedral quasi-crystals of intermetallic compounds are twinned cubic crystals

PubMed Central

Pauling, Linus

1988-01-01

Analysis of the measured values of Q for the weak peaks (small maxima, usually considered to be background fluctuations, “noise”) on the x-ray powder diffraction curves for 17 rapidly quenched alloys leads directly to the conclusion that they are formed by an 820-atom or 1012-atom primitive cubic structure that by icosahedral twinning produces the so-called icosahedral quasi-crystals. PMID:16593948

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.;

Synthesis, characterization and photocatalytic properties of Mg1-xZnxAl2O4 spinel nanoparticles

NASA Astrophysics Data System (ADS)

Li, Hui; Liu, Yuqin; Tang, Junkai; Deng, Yanxi

2016-08-01

Mg1-xZnxAl2O4 spinel nanoparticles with x = 0, 0.05, 0.10, 0.15 and 0.20 were prepared via the chemical coprecipitation method. The obtained samples were characterised by thermal gravimetric and differential scanning calorimetry, X-ray diffraction, Fourier transform infrared spectroscopy, UV-Vis diffuse reflection spectrum, transmission electron microscopy and 27Al MAS-NMR spectroscopy. Mg1-xZnxAl2O4 spinel powders with the mean crystallite size of around 11 nm-14 nm were obtained. The crystallinity of the MgAl2O4 samples increases with the increase in the calcination temperature. At the same calcination temperature, higher amount of Zn2+ substitution leads to the higher level of crystallinity, but has no apparent influence on the mean crystallite size of the samples. The photocatalytic activity of the obtained Mg1-xZnxAl2O4 spinel nanoparticles was evaluated by monitoring the degradation of methylene blue under UV light. The degradation rates of methylene blue using the MgAl2O4 nanoparticles prepared at the calcination temperatures of 700 °C and 800 °C are much higher than those prepared at 900 °C and 1000 °C. The photocatalytic activities of the spinel powders with lower level of Zn2+ substitution such as Mg0.95Zn0.05Al2O4 are inferior to that of MgAl2O4. Results of 27Al MAS-NMR spectroscopy analysis and the first principle total density of state calculations reveal that this is probably due to the substitutions of Zn2+ decreasing the degree of Al3+ ions inversion over the sites of tetrahedral and octahedral coordination. With the increase in the amounts of Zn2+ substitution, the effects of Zn2+ additions on the photocatalytic activities become gradually predominant, leading to the increases in the degradation rates. The methylene blue degraded by 99% within 4 h using the Mg0.8Zn0.2Al2O4 spinel powders.

Room-temperature ferromagnetic Zn1- x Ni x S nanoparticles

NASA Astrophysics Data System (ADS)

Kunapalli, Chaitanya Kumar; Shaik, Kaleemulla

2018-05-01

Nickel-doped zinc sulfide nanoparticles (Zn1- x Ni x S) at x = 0.00, 0.02, 0.05, 0.08 and 0.10 were synthesized by solid-state reaction. The (nickel sulfide) NiS and (zinc sulfide) ZnS nanoparticles in desired ratios were taken, mixed and ground for 6 h at a speed rate of 300 rpm using a planetary ball mill. The milled nanoparticles were sintered at 600 °C for 8 h using a high-temperature vacuum furnace. The structural, optical, luminescence and magnetic properties of the Zn1- x Ni x S nanoparticles were characterized by powder X-ray diffraction (XRD), UV-Vis-NIR diffuse reflectance spectroscopy, photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). No change in crystal structure was observed from XRD by substitution of Ni into ZnS lattice. The mean crystallite size was found to be 37 nm. The band gap of Zn1- x Ni x S nanoparticles decreased from 3.57 to 3.37 eV on increasing the dopant concentration. The room-temperature photoluminescence (PL) spectra of Zn1- x Ni x S nanoparticles showed two broad and intense emission peaks at 420 and 438 nm with excitation wavelength of 330 nm. The Zn1- x Ni x S nanoparticles showed ferromagnetism at 100 K and at room temperature (300 K) and also the strength of magnetization increased with Ni concentration. The maximum magnetization value of 0.18 emu/g was observed for x = 0.10 at 100 K. The strength of the magnetization observed at 100 K was higher than that of magnetization observed at 300 K.

Zn(1-x)Cu(x)O (0.02 ≤ x ≤ 0.1) Nanomaterials Prepared by Ball Milling, Citrate Sol Gel, and Molten Salt Flux Methods.

PubMed

Balamurugan, S; Melba, K

2015-06-01

The Cu doped ZnO, (Zn(1-x)Cu(x))O (x = 0.02, 0.04, 0.06, 0.08, and 0.1) nanomaterials were prepared by ball milling technique (BMT), citrate sol gel (CSG), and molten salt flux (MSF) methods. The various as-prepared (Zn(1-x)Cu(x))O materials were analyzed by powder X-ray diffraction (pXRD), FT-IR, and SEM-EDX measurements in order to check the phase formation, purity, surface morphology and elements present in the annealed materials. Due to the preparation methods as well as doping of 'x' slight variations in cell parameters are seen. The average crystalline size of CSG method shows smaller size (25-35 nm) than BMT and MSF approaches. The materials obtained by MSF technique reveal the average crystalline size in the range of 32-72 nm whereas the BMT materials exhibit 36-50 nm for the composition, 0.02 ≤ x ≤ 0.1. The presence of functional groups and the chemical bonding in (Zn(1-x)Cu(x))O system is confirmed through FT-IR measurements. It is evident from the FT-IR data that bands seen at 400-500 cm(-1) are characteristics of M-O (M = metal ion) bonding in the studied materials. The micro images observed by SEM exhibiting polycrystalline character as compared with the crystallite size obtained from XRD. Among the three approaches employed in the present investigations, in terms of average particle size the CSG method may be concluded as an efficient method for the preparation of Zn(1-x)Cu(x)O nanomaterials.

Accommodating High Transformation Strains in Battery Electrodes via the Formation of Nanoscale Intermediate Phases: Operando Investigation of Olivine NaFePO 4 [Accommodation of High Transformation Strain in Battery Electrodes via Formation of Nanoscale Intermediate Phases: Operando Structure Investigation of Olivine Sodium Iron Phosphate

DOE PAGES

Xiang, Kai; Xing, Wenting; Ravnsbaek, Dorthe B.; ...

2017-02-21

Virtually all intercalation compounds used as battery electrodes exhibit significant changes in unit cell volume during use. Na xFePO 4 (0 < x < 1, NFP) olivine, of interest as a cathode for sodium-ion batteries, is a model for topotactic, high strain systems as it exhibits one of the largest discontinuous volume changes (~17% by volume) during its first-order transition between two otherwise isostructural phases. Using synchrotron radiation powder X-ray diffraction (PXD) and pair distribution function (PDF) analysis, we discover a new strain-accommodation mechanism wherein a third, <10 nm scale nanocrystalline phase forms to buffer the large lattice mismatch betweenmore » primary phases. The new phase has a and b lattice parameters matching one crystalline endmember phase and c lattice parameter matching the other, and is not detectable by powder diffraction alone. Finally, we suggest that this strain-accommodation mechanism may apply to systems with large transformation strains but in which true “amorphization” does not occur.« less

Accommodating High Transformation Strains in Battery Electrodes via the Formation of Nanoscale Intermediate Phases: Operando Investigation of Olivine NaFePO 4 [Accommodation of High Transformation Strain in Battery Electrodes via Formation of Nanoscale Intermediate Phases: Operando Structure Investigation of Olivine Sodium Iron Phosphate

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

Xiang, Kai; Xing, Wenting; Ravnsbaek, Dorthe B.

Virtually all intercalation compounds used as battery electrodes exhibit significant changes in unit cell volume during use. Na xFePO 4 (0 < x < 1, NFP) olivine, of interest as a cathode for sodium-ion batteries, is a model for topotactic, high strain systems as it exhibits one of the largest discontinuous volume changes (~17% by volume) during its first-order transition between two otherwise isostructural phases. Using synchrotron radiation powder X-ray diffraction (PXD) and pair distribution function (PDF) analysis, we discover a new strain-accommodation mechanism wherein a third, <10 nm scale nanocrystalline phase forms to buffer the large lattice mismatch betweenmore » primary phases. The new phase has a and b lattice parameters matching one crystalline endmember phase and c lattice parameter matching the other, and is not detectable by powder diffraction alone. Finally, we suggest that this strain-accommodation mechanism may apply to systems with large transformation strains but in which true “amorphization” does not occur.« less

Quantitative analysis of packed and compacted granular systems by x-ray microtomography

NASA Astrophysics Data System (ADS)

Fu, Xiaowei; Milroy, Georgina E.; Dutt, Meenakshi; Bentham, A. Craig; Hancock, Bruno C.; Elliott, James A.

2005-04-01

The packing and compaction of powders are general processes in pharmaceutical, food, ceramic and powder metallurgy industries. Understanding how particles pack in a confined space and how powders behave during compaction is crucial for producing high quality products. This paper outlines a new technique, based on modern desktop X-ray tomography and image processing, to quantitatively investigate the packing of particles in the process of powder compaction and provide great insights on how powder densify during powder compaction, which relate in terms of materials properties and processing conditions to tablet manufacture by compaction. A variety of powder systems were considered, which include glass, sugar, NaCl, with a typical particle size of 200-300 mm and binary mixtures of NaCl-Glass Spheres. The results are new and have been validated by SEM observation and numerical simulations using discrete element methods (DEM). The research demonstrates that XMT technique has the potential in further investigating of pharmaceutical processing and even verifying other physical models on complex packing.

[Two-photon up-conversion fluorescence of a neodymium organic framework Nd(BTC)].

PubMed

Xu, Hui; Jin, Run-zhi; Wu, Chun-yang; Yang, Yu; Qian, Guo-dong

2008-08-01

In the present work, a neodymium organic framework Nd(BTC) was synthesized by the solvothermal reaction of Nd(NO3)3 x 5H2O and H3BTC (BTC = 1,3,5-benzenetricarboxylate) in mixed solvents of DMF, ethanol and water, and was identified by elemental analysis. This MOF complex was characterized using X-ray diffraction (XRD), thermogravimetry-differential scanning calorimetry (TGA-DSC) analysis, UV-visible absorption spectra and fluorescence spectra. This polycrystalline powder lost DMF and H2O when heated to 120 degrees C, then remained stable till the temperature reached 500 degrees C. Near infrared fluorescence at 1064 nm due to the 4 F3/2--> 4 I11/2 transition of Nd3+ ions was exhibited when excited by 808 nm laser beam. It was also been found that up-conversion fluorescence of Nd(BTC) peaked at about 450 nm due to 2 D5/2 -->4 I11/2 transition of Nd3+ ions can be observed under the excitation of a 580 nm laser line. The mechanism of the up-conversion fluorescence of Nd(BTC) at around 450 nm under the excitation of 580 nm laser can be ascribed to both excited-state absorption and energy transfer up-conversion. This result indicated that such MOF can be employed as an up-conversion luminescence material in many potential application areas such as bio-labeling and fluorescence image.

Local surrounding of Mn in LaMn 1-xCo xO 3 compounds by means of EXAFS on Mn-K

NASA Astrophysics Data System (ADS)

Procházka, Vít; Sikora, Marcin; Kapusta, Czeslaw; Štěpánková, Helena; Chlan, Vojtěch; Knížek, Karel; Jirák, Zdeněk

2010-05-01

A systematic study of LaMn 1-xCo xO 3 perovskite series by means of X-ray absorption spectroscopy in the extended X-ray absorption fine structure (EXAFS) range of the K-absorption edge of Mn is reported. The Mn-K edge absorption measurements in the EXAFS region were performed to study the local surrounding of Mn ions. Polycrystalline powder samples of LaMn 1-xCo xO 3 ( x=0, 0.02; 0.2; 0.4; 0.5; 0.6; 0.8) prepared by solid-state reaction were used. The EXAFS spectra were analyzed with the FEFF8 computer program. The Mn-O distances of Mn to the nearest oxygen surroundings were evaluated for the samples in the series and compared with the Co-O distances obtained by EXAFS in V. Procházka et al., JMMM 310 (2007) 197 and with results of X-ray powder diffraction in C. Autret, J. Phys. Condens. Matter 17 (2005) 1601.

Luminescent spectroscopy and structural properties of Ce3+-doped low-temperature X1-Y2SiO5 material prepared by polymer-assisted sol-gel method

NASA Astrophysics Data System (ADS)

Hamroun, M. S. E.; Guerbous, L.; Bensafi, A.

2016-04-01

Cerium (Ce3+)-doped monoclinic X1-Y2SiO5 (YSO)-type oxyorthosilicates powders were prepared by monomer and polymer-assisted sol-gel method. The present work aims to study the influence of ethylene glycol (EG) monomer, polyethylene glycol (PEG) polymer and polyvinyl alcohol (PVA) polymer, as fuels and nucleating agents for the crystallization, on structural and luminescence properties of the Ce3+ (xCe = 0.01)-doped Y2SiO5. The X-ray diffraction technique, field emission scanning electron microscopy, Fourier transform infrared spectroscopy and steady photoluminescence have been used to characterize the samples. It is found that the types of fuels affect the phase purity and luminescent characteristics of phosphors. All samples exhibit intense violet-blue asymmetric emission band in the range of 370-540 nm with a maximum intensity centered at around 420 nm assigned to the 5d → 4f (2F5/2, 2F7/2) interconfigurational transitions of Ce3+ ion in YSO nanomaterial. Finally, the vibronic coupling parameters are estimated and discussed.

Fabrication by Electrophoretic Deposition of Nano-Fe3O4 and Fe3O4@SiO2 3D Structure on Carbon Fibers as Supercapacitor Materials

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Abouzari-Lotf, Ebrahim; Etemadifar, Reza; Abbasi-Chianeh, Vahid; Kianvash, Abbas

2018-05-01

Core-shell nanostructured magnetic Fe3O4@SiO2 with particle size ranging from 3 nm to 40 nm has been synthesized via a facile precipitation method. Tetraethyl orthosilicate was employed as surfactant to prepare core-shell structures from Fe3O4 nanoparticles synthesized from pomegranate peel extract using a green method. X-ray diffraction analysis, Fourier-transform infrared and ultraviolet-visible (UV-Vis) spectroscopies, transmission electron microscopy, and scanning electron microscopy with energy-dispersive spectroscopy were employed to characterize the samples. The prepared Fe3O4 nanoparticles were approximately 12 nm in size, and the thickness of the SiO2 shell was 4 nm. Evaluation of the magnetic properties indicated lower saturation magnetization for Fe3O4@SiO2 powder ( 11.26 emu/g) compared with Fe3O4 powder ( 13.30 emu/g), supporting successful wrapping of the Fe3O4 nanoparticles by SiO2. As-prepared powders were deposited on carbon fibers (CFs) using electrophoretic deposition and their electrochemical behavior investigated. The rectangular-shaped cyclic voltagrams of Fe3O4@CF and Fe3O4@C@CF samples indicated electrochemical double-layer capacitor (EDLC) behavior. The higher specific capacitance of 477 F/g for Fe3O4@C@CF (at scan rate of 0.05 V/s in the potential range of - 1.13 to 0.45 V) compared with 205 F/g for Fe3O4@CF (at the same scan rate in the potential range of - 1.04 to 0.24 V) makes the former a superior candidate for use in energy storage applications.

Synthesis and characterization of scandia ceria stabilized zirconia powders prepared by polymeric precursor method for integration into anode-supported solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Tu, Hengyong; Liu, Xin; Yu, Qingchun

2011-03-01

Scandia ceria stabilized zirconia (10Sc1CeSZ) powders are synthesized by polymeric precursor method for use as the electrolyte of anode-supported solid oxide fuel cell (SOFC). The synthesized powders are characterized in terms of crystalline structure, particle shape and size distribution by X-ray diffraction (XRD), transmission electron microscopy (TEM) and photon correlation spectroscopy (PCS). 10Sc1CeSZ electrolyte films are deposited on green anode substrate by screen-printing method. Effects of 10Sc1CeSZ powder characteristics on sintered films are investigated regarding the integration process for application as the electrolytes in anode-supported SOFCs. It is found that the 10Sc1CeSZ films made from nano-sized powders with average size of 655 nm are very porous with many open pores. In comparison, the 10Sc1CeSZ films made from micron-sized powders with average size of 2.5 μm, which are obtained by calcination of nano-sized powders at higher temperatures, are much denser with a few closed pinholes. The cell performances are 911 mW cm-2 at the current density of 1.25 A cm-2 and 800 °C by application of Ce0.8Gd0.2O2 (CGO) barrier layer and La0.6Sr0.4CoO3 (LSC) cathode.

Quantitative analysis of crystalline pharmaceuticals in powders and tablets by a pattern-fitting procedure using X-ray powder diffraction data.

PubMed

Yamamura, S; Momose, Y

2001-01-16

A pattern-fitting procedure for quantitative analysis of crystalline pharmaceuticals in solid dosage forms using X-ray powder diffraction data is described. This method is based on a procedure for pattern-fitting in crystal structure refinement, and observed X-ray scattering intensities were fitted to analytical expressions including some fitting parameters, i.e. scale factor, peak positions, peak widths and degree of preferred orientation of the crystallites. All fitting parameters were optimized by the non-linear least-squares procedure. Then the weight fraction of each component was determined from the optimized scale factors. In the present study, well-crystallized binary systems, zinc oxide-zinc sulfide (ZnO-ZnS) and salicylic acid-benzoic acid (SA-BA), were used as the samples. In analysis of the ZnO-ZnS system, the weight fraction of ZnO or ZnS could be determined quantitatively in the range of 5-95% in the case of both powders and tablets. In analysis of the SA-BA systems, the weight fraction of SA or BA could be determined quantitatively in the range of 20-80% in the case of both powders and tablets. Quantitative analysis applying this pattern-fitting procedure showed better reproducibility than other X-ray methods based on the linear or integral intensities of particular diffraction peaks. Analysis using this pattern-fitting procedure also has the advantage that the preferred orientation of the crystallites in solid dosage forms can be also determined in the course of quantitative analysis.

Optical performance of W/B4C multilayer mirror in the soft x-ray region

NASA Astrophysics Data System (ADS)

Pradhan, P. C.; Majhi, A.; Nayak, M.

2018-03-01

W/B4C x-ray multilayers (MLs) with 300 layer pairs and a period in the range of d = 2-1.6 nm are fabricated and investigated for the x-ray optical element in the soft x-ray regime. The structural analyses of the MLs are carried out by using hard x-ray reflectivity (HXR) measurements at 8.047 keV. Well-defined successive higher order Bragg peaks (up to 3rd order) in HXR data collected up to glancing incidence angles of ˜9° reveal a good quality of the periodic structure. The ML mirrors have an average interface width of ˜0.35 nm and have a compressive residual stress of ˜0.183 GPa and 0. 827 GPa for d = 1.62 nm and d = 1.98 nm, respectively. MLs maintain structural stability over a long time, with a slight increase in interface widths of the W layers by 0.1 nm due to self-diffusion. Soft x-ray reflectivity (SXR) performances are evaluated in the energy range of 650 to 1500 eV. At energy ˜ 1489 eV, measured reflectivities (energy resolution, ΔE) are ˜ 10% (19 eV) and 4.5% (13 eV) at glancing incident angles of 12.07° and 15° for MLs having periods of 1.98 nm and 1.62 nm, respectively. The optical performance from 1600 eV to 4500 eV is theoretically analysed by considering the measured structural parameters. The structure-stress-optical performance is correlated on the basis of the mechanism of film growth. The implications of W/B4C MLs are discussed, particularly with respect to the development of ML optics with high spectral selectivity and reflectance for soft x-ray instruments.

Oxidized nanocrystalline Fe-Cu pseudoalloy subjected to high pressure and electrodischarge pulses: Mössbauer and x-ray investigations

NASA Astrophysics Data System (ADS)

Gavriliuk, A. G.; Voitkovsky, V. S.; Sidorov, V. A.; Filonenko, V. P.; Tsiok, O. B.; Khvostantsev, L. G.

1998-05-01

Nanocrystalline Fe15Cu85 pseudoalloy has been subjected to pulsed heating up to 1500 K at high pressure (8 GPa). Two regimes were studied: the direct heating using electrodischarge through the sample and indirect heating with the use of cylindrical heater around the sample. The temperature and time conditions in both types of experiments were adjusted to be equivalent. The discharge parameters (stored energy, discharge time, and magnitude of current pulse) were sufficient to move defects by conduction electrons, but insufficient to melt the sample. The properties of treated samples were studied using Mössbauer absorption spectra and x-ray diffraction for three types of samples: (a) primary powder treated by high pressure up to 8 GPa, (b) powder subjected to indirect pulsed heating at 8 GPa, (c) powder treated by electrical pulses at 8 GPa. The x-ray diffraction pattern of primary powder exhibits peaks of copper, iron, and copper oxide (CuO). The Mössbauer spectrum of primary powder exhibits six peaks of alpha iron and some peaks near zero velocity due to the small iron clusters in the copper matrix and ultrafine clusters of paramagnetic phase x-Fe2O3. The transformation of CuO to Cu2O takes place in the course of indirect heating, the Mössbauer spectrum being almost unchanged. The direct electrodischarge heating causes the appearance of new magnetic phase with the magnetic field on iron nucleus 505 kOe, which corresponds to α-Fe2O3. The formation of α-Fe2O3 was confirmed by x-ray diffraction. At the same time the transformation of CuO to Cu2O is incomplete. These experiments demonstrate that high density current pulses, causing the electron wind, can be a useful tool to influence the structure of nanocrystalline powder.

Beamline P02.1 at PETRA III for high-resolution and high-energy powder diffraction

PubMed Central

Dippel, Ann-Christin; Liermann, Hanns-Peter; Delitz, Jan Torben; Walter, Peter; Schulte-Schrepping, Horst; Seeck, Oliver H.; Franz, Hermann

2015-01-01

Powder X-ray diffraction techniques largely benefit from the superior beam quality provided by high-brilliance synchrotron light sources in terms of photon flux and angular resolution. The High Resolution Powder Diffraction Beamline P02.1 at the storage ring PETRA III (DESY, Hamburg, Germany) combines these strengths with the power of high-energy X-rays for materials research. The beamline is operated at a fixed photon energy of 60 keV (0.207 Å wavelength). A high-resolution monochromator generates the highly collimated X-ray beam of narrow energy bandwidth. Classic crystal structure determination in reciprocal space at standard and non-ambient conditions are an essential part of the scientific scope as well as total scattering analysis using the real space information of the pair distribution function. Both methods are complemented by in situ capabilities with time-resolution in the sub-second regime owing to the high beam intensity and the advanced detector technology for high-energy X-rays. P02.1’s efficiency in solving chemical and crystallographic problems is illustrated by presenting key experiments that were carried out within these fields during the early stage of beamline operation. PMID:25931084

Energy transfer from Pr3+ to Gd3+ ions in BaB8O13 phosphor for phototherapy lamps

NASA Astrophysics Data System (ADS)

Tamboli, Sumedha; Nair, Govind B.; Dhoble, S. J.; Burghate, D. K.

2018-04-01

A series of BaB8O13 phosphors doped with different concentrations of Gd3+ ions and co-doped with Pr3+ ions were synthesized by solid state synthesis method. X-ray powder diffraction (XRD) analysis confirmed the formation of the compound in a crystalline and homogeneous form. Scanning Electron Microscopy (SEM) was performed to study the surface morphology of the compound and Fourier Transform Infrared (FT-IR) spectroscopy measurements determined the nature of bonding between elements of the compounds. The photoluminescence (PL) excitation spectra of BaB8O13:Gd3+ phosphor showed excitation peaks at 246 nm, 252 nm and 274 nm. The prominent emission peak was observed at 313 nm which is in narrow band ultraviolet B (NB-UVB) range. Energy transfer was achieved by co-doping Pr3+ ions with Gd3+ ions. PL decay time was also measured for BaB8O13: Gd3+, Pr3+ phosphor. Emission at 313 nm can be used for the treatment of skin diseases.

Vapor-phase photo-oxidation of methanol over nanosize titanium dioxide clusters dispersed in MCM-41 host material part 1: synthesis and characterization.

PubMed

Bhattacharya, K; Tripathi, A K; Dey, G K; Gupta, N M

2005-05-01

Nanosize clusters of titania were dispersed in mesoporous MCM-41 silica matrix with the help of the incipient wet-impregnation route, using an isopropanol solution of titanium isopropoxide as precursor. The clusters thus formed were of pure anatase phase and their size depended upon the titania loading. In the case of low (< 15 wt %) loadings, the TiO2 particles were X-ray and laser-Raman amorphous, confirming very high dispersion. These particles were mostly of < or = 2 nm size. On the other hand, larger size clusters (2-15 nm) were present in a sample with a higher loading of approximately 21 wt %. These particles of titania, irrespective of their size, exhibited an absorbance behavior similar to that of bulk TiO2. Powder X-ray diffraction, N2-adsorption and transmission electron microscopy results showed that while smaller size particles were confined mostly inside the pore system, the larger size particles occupied the external surface of the host matrix. At the same time, the structural integrity of the host was maintained even though some deformation in the pore system was noticed in the case of the sample having highest loading. The core level X-ray photoelectron spectroscopy results revealed a + 4 valence state of Ti in all the samples. A positive binding energy shift and the increase of the width of Ti 2p peaks were observed, however, with the decrease in the particle size of supported titania crystallites, indicative of a microenvironment for surface sites that is different from that of the bulk.

Comparative study of particle structure evolution during water sorption: skim and whole milk powders.

PubMed

Murrieta-Pazos, I; Gaiani, C; Galet, L; Cuq, B; Desobry, S; Scher, J

2011-10-01

Surface composition of dairy powders influences significantly a quantity of functional properties such as rehydration, caking, agglomeration. Nevertheless, the kinetic of water uptake by the powders was never directly related to the structure and the composition of the surface. In this work, the effect of relative humidity on the structural reorganization of two types of dairy powder was studied. The water-powder interaction for industrial whole milk powder, and skim milk powder was studied using dynamic vapor sorption. The water sorption isotherms were fitted with a Brunner-Emmet-Teller model and each stage of the sorption curve was analyzed with a Fickian diffusion. The water content in the monolayer predicted for each powder and the moisture diffusivity calculated were discussed and compared. Concurrently, powders microstructure and powders surface under variable relative humidity were assessed by X-ray photoelectron spectroscopy, scanning electron microscopy coupled with energy dispersive X-ray and atomic force microscopy. A correlation between the data obtained from the sorption isotherms and the modifications of structure allowed us to conclude that powder microstructure and chemical state of the components could play an important role in determining the water diffusivity. Copyright © 2011 Elsevier B.V. All rights reserved.

CdTe quantum-dot-modified ZnO nanowire heterostructure

NASA Astrophysics Data System (ADS)

Shahi, Kanchana; Singh, R. S.; Singh, Ajaya Kumar; Aleksandrova, Mariya; Khenata, Rabah

2018-03-01

The effect of CdTe quantum-dot (QD) decoration on the photoluminescence (PL) behaviour of ZnO nanowire (NW) array is presented in the present work. Highly crystalline and vertically 40-50 nm diameter range and 1 µm in length aligned ZnO NWs are synthesized using low-cost method. The crystallinity and morphology of the NWs are studied by scanning electron microscopy and X-ray powder diffraction methods.Optical properties of the nanowires are studied using photo-response and PL spectroscopy. CdTe QDs are successfully synthesized on ZnO nanowire surface by dip-coating method. ZnO NWs are sensitized with CdTe QDs characterized by transmission electron microscopy, energy-dispersive X-ray spectroscopy, and PL spectroscopy. The highly quenched PL intensity indicates the charge transfer at interface between CdTe QDs and ZnO NWs and is due to the formation of type-II heterostructure between QDs and NWs. Photo-response behaviour of heterostructure of the film is also been incorporated in the present work.

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO₃ Ceramics Fabricated by Spark Plasma Sintering.

PubMed

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-03-07

Based on precursor powders with a size of 200-300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO₃ ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO₃ ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe 3+ to Fe 2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO₃ ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage.

Studies on synthesis, growth, structural, thermal, linear and nonlinear optical properties of organic picolinium maleate single crystals.

PubMed

Pandi, P; Peramaiyan, G; Sudhahar, S; Chakkaravarthi, G; Mohan Kumar, R; Bhagavannarayana, G; Jayavel, R

2012-12-01

Picolinium maleate (PM), an organic material has been synthesised and single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal X-ray diffraction analysis. PM crystal belongs to the monoclinic crystallographic system with space group P2(1)/c. The crystalline perfection of the grown crystals was analyzed by high-resolution X-ray diffraction rocking curve measurements. The presence of functional groups in PM was identified by FTIR and FT-NMR spectral analyses. Thermal behaviour and stability of picolinium maleate were studied by TGA/DTA analyses. UV-Vis spectral studies reveal that PM crystals are transparent in the wavelength region 327-1100 nm. The laser damage threshold value of PM crystal was found to be 4.3 GW/cm(2) using Nd:YAG laser. The Kurtz and Perry powder second harmonic generation technique confirms the nonlinear optical property of the grown crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Decolorization of reactive dye using a photo-ferrioxalate system with brick grain-supported iron oxide.

PubMed

Cheng, Hui-Pin; Huang, Yao-Hui; Lee, Changha

2011-04-15

The photocatalytic activity of a brick grain-supported iron oxide (denoted as B1) was tested for its activity to degrade Reactive Black 5 (RB5) in the presence of oxalic acid. B1 was obtained as a solid waste from a wastewater treatment plant, and characterized using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD) and N(2) adsorption/desorption isotherm analyses. The decolorization experiments were performed in a fluidized bed reactor with aeration under UV-A irradiation (λ = 365 nm). The effects of various factors such as solution pH, concentration of oxalic acid and dissolved oxygen on the decolorization of RB5 were evaluated considering the contributions of adsorption and photo-catalytic degradation. The role of dissolved iron in the removal of RB5 and the stability of B1 were also examined. In addition, the removal of TOC during the photo-catalytic reaction was monitored. Copyright © 2011 Elsevier B.V. All rights reserved.

Multi-Layer SnSe Nanoflake Field-Effect Transistors with Low-Resistance Au Ohmic Contacts

NASA Astrophysics Data System (ADS)

Cho, Sang-Hyeok; Cho, Kwanghee; Park, No-Won; Park, Soonyong; Koh, Jung-Hyuk; Lee, Sang-Kwon

2017-05-01

We report p-type tin monoselenide (SnSe) single crystals, grown in double-sealed quartz ampoules using a modified Bridgman technique at 920 °C. X-ray powder diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX) measurements clearly confirm that the grown SnSe consists of single-crystal SnSe. Electrical transport of multi-layer SnSe nanoflakes, which were prepared by exfoliation from bulk single crystals, was conducted using back-gated field-effect transistor (FET) structures with Au and Ti contacts on SiO2/Si substrates, revealing that multi-layer SnSe nanoflakes exhibit p-type semiconductor characteristics owing to the Sn vacancies on the surfaces of SnSe nanoflakes. In addition, a strong carrier screening effect was observed in 70-90-nm-thick SnSe nanoflake FETs. Furthermore, the effect of the metal contacts to multi-layer SnSe nanoflake-based FETs is also discussed with two different metals, such as Ti/Au and Au contacts.

Efficient photodegradation of methylthioninium chloride dye in aqueous using barium tungstate nanoparticles

NASA Astrophysics Data System (ADS)

AlShehri, Saad M.; Ahmed, Jahangeer; Ahamad, Tansir; Almaswari, Basheer M.; Khan, Aslam

2017-08-01

BaWO4 nanoparticles were successfully used as the photocatalysts in the degradation of methylthioninium chloride (MTC) dye at different pH levels of aqueous solution. Pure phase of barium tungstate (BaWO4) nanoparticles was synthesized by modified molten salt process at 500 °C for 6 h. Structural and morphological characterizations of BaWO4 nanoparticles (average particle size of 40 nm) were studied in details using powder x-ray diffraction (XRD), FTIR, Raman, energy-dispersive, electron microscopic, and x-ray photoelectron spectroscopy (XPS) techniques. Direct band gap energy of BaWO4 nanoparticles was found to be 3.06 eV from the UV-visible absorption spectroscopy followed by Tauc's model. Photocatalytic properties of the nanoparticles were also investigated systematically for the degradation of MTC dye solution in various mediums. BaWO4 nanoparticles claim the significant enhancement of the photocatalytic degradation of aqueous MTC dye to non-hazardous inorganic constitutes under alkaline, neutral, and acidic mediums. [Figure not available: see fulltext.

Green synthesis of size controllable gold nanoparticles

NASA Astrophysics Data System (ADS)

Mohan Kumar, Kesarla; Mandal, Badal Kumar; Kiran Kumar, Hoskote A.; Maddinedi, Sireesh Babu

2013-12-01

A facile rapid green eco-friendly method to synthesize gold nanoparticles (Au NPs) of tunable size using aqueous Terminalia arjuna fruit extracts has been demonstrated herein. Formation of Au NPs was confirmed by Surface Plasmon Resonance (SPR) study at 528 nm using UV-visible spectrophotometer. The time of reduction, size and morphological variations of Au NPs were studied with varying quantities of T. arjuna fruit aqueous extracts. Synthesized Au NPs were characterized using UV-visible spectroscopy, Fourier transformed infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and Energy dispersive X-ray spectroscopy (EDAX). Polyphenols responsible for reduction of Au3+ to Au0 were identified using High Performance Liquid Chromatography (HPLC) as ascorbic acid, gallic acid and pyrogallol. The oxidized forms of polyphenols formed coordination with surface of Au NPs which protected their further growth and aggregation. We also propose a plausible mechanism how to tune size and shape of Au NPs by varying the quantity of extracts. Thus obtained Au NPs were stable for more than four months.

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

NASA Astrophysics Data System (ADS)

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

2015-09-01

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

The Fabrication and High-Efficiency Electromagnetic Wave Absorption Performance of CoFe/C Core-Shell Structured Nanocomposites

NASA Astrophysics Data System (ADS)

Wan, Gengping; Luo, Yongming; Wu, Lihong; Wang, Guizhen

2018-03-01

CoFe/C core-shell structured nanocomposites (CoFe@C) have been fabricated through the thermal decomposition of acetylene with CoFe2O4 as precursor. The as-prepared CoFe@C was characterized by X-ray powder diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy, transmission electron microscopy, and thermogravimetric analysis. The results demonstrate that the carbon shell in CoFe@C has a poor crystallization with a thickness about 5-30 nm and a content approximately 48.5 wt.%. Due to a good combination between intrinsic magnetic properties and high-electrical conductivity, the CoFe@C exhibits not only excellent absorption intensity but also wide frequency bandwidth. The minimum RL value of CoFe@C can reach - 44 dB at a thickness of 4.0 mm, and RL values below - 10 dB is up to 4.3 GHz at a thickness of 2.5 mm. The present CoFe@C may be a potential candidate for microwave absorption application.

Controllable synthesis of protein-conjugated lead sulfide nanocubes by using bovine hemoglobin as a capping agent

NASA Astrophysics Data System (ADS)

Yang, Guangrui; Qin, Dezhi; Zhang, Li

2014-06-01

A simple, convenient, and controllable strategy was reported in this contribution for protein-assisted synthesis BHb-conjugated PbS nanocubes. Powder X-ray diffraction, energy disperse X-ray spectroscopy, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area electron diffraction characterizations were used to determine the structure and morphology of BHb-conjugated PbS nanocubes. The prepared PbS nanocrystals with cubic rock salt structure were uniform and monodispersed with homogeneous size around 12 nm. The results of Fourier transform infrared and circular dichroism assay proved that Pb2+/PbS had coordination interaction with functional groups of BHb besides physical-binding effect, and the secondary structure of protein significantly changed with this interaction. Thermogravimetric analysis results confirmed the existence of BHb in PbS nanocrystals and indicated that the conjugate bonds existed between PbS and BHb. A clear perspective was shown here that special nanostructure could be created by using proteins as a mediating template at the inorganic-organic interface.

Synthesis, characteristics and antimicrobial activity of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Janaki, A. Chinnammal; Sailatha, E.; Gunasekaran, S.

2015-06-01

The utilization of various plant resources for the bio synthesis of metallic nano particles is called green technology and it does not utilize any harmful protocols. Present study focuses on the green synthesis of ZnO nano particles by Zinc Carbonate and utilizing the bio-components of powder extract of dry ginger rhizome (Zingiber officinale). The ZnO nano crystallites of average size range of 23-26 nm have been synthesized by rapid, simple and eco friendly method. Zinc oxide nano particles were characterized by using X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive X-ray spectroscopy (EDX). FTIR spectra confirmed the adsorption of surfactant molecules at the surface of ZnO nanoparticles and the presence of ZnO bonding. Antimicrobial activity of ZnO nano particles was done by well diffusion method against pathogenic organisms like Klebsiella pneumonia, Staphylococcus aureus and Candida albicans and Penicillium notatum. It is observed that the ZnO synthesized in the process has the efficient antimicrobial activity.

Soft x-ray reduction camera for submicron lithography

DOEpatents

Hawryluk, Andrew M.; Seppala, Lynn G.

1991-01-01

Soft x-ray projection lithography can be performed using x-ray optical components and spherical imaging lenses (mirrors), which form an x-ray reduction camera. The x-ray reduction is capable of projecting a 5x demagnified image of a mask onto a resist coated wafer using 4.5 nm radiation. The diffraction limited resolution of this design is about 135 nm with a depth of field of about 2.8 microns and a field of view of 0.2 cm.sup.2. X-ray reflecting masks (patterned x-ray multilayer mirrors) which are fabricated on thick substrates and can be made relatively distortion free are used, with a laser produced plasma for the source. Higher resolution and/or larger areas are possible by varying the optic figures of the components and source characteristics.

A new large area scintillator screen for X-ray imaging

NASA Astrophysics Data System (ADS)

Nagarkar, V. V.; Miller, S. R.; Tipnis, S. V.; Lempicki, A.; Brecher, C.; Lingertat, H.

2004-01-01

We report on the development of a new, large area, powdered scintillator screen based on Lu 2O 3(Eu). As reported earlier, the transparent ceramic form of this material has a very high density of 9.4 g/cm 3, a high light output comparable to that of CsI(Tl), and emits in a narrow spectral band centered at about 610 nm. Research into fabrication of this ceramic scintillator in a large area format is currently underway, however the process is not yet practical for large scale production. Here we have explored fabrication of large area screens using precursor powders from which the ceramics are fabricated. To date we have produced up to 16 × 16 cm 2 area screens with thickness in the range of 18 mg/cm 2. This paper outlines the screen fabrication technique and presents its imaging performance in comparison with a commercial Gd 2O 2S:Tb (GOS) screen.

Microstructural, optical and electrical transport properties of Cd-doped SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

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

2018-03-01

We have successfully investigated the structural, optical and dielectric properties of Cd assimilated SnO2 nanoparticles synthesized via very convenient precipitation route. The structural properties were studied by x-ray diffraction method (XRD) and Fourier Transform Infrared (FTIR) Spectroscopy. As-synthesized samples in the form of powder were examined for its morphology and average particle size by Transmission electron microscopy (TEM). The optical properties were studied by diffuse reflectance spectroscopy. Dielectric properties such that complex dielectric constant and ac conductivity were investigated by LCR meter. Average crystallite size calculated by XRD and average particle size obtained from TEM were found to be consistent and below 50 nm for all samples. The optical band gap of as-synthesized powder samples from absorption study was found in the range of 3.76 to 3.97 eV. The grain boundary parameters such that Rgb, Cgb and τ were evaluated using impedance spectroscopy.

Synthesis, growth and characterization of 3-nitroacetanilide—A new organic nonlinear optical crystal by Bridgman technique

NASA Astrophysics Data System (ADS)

Lenin, M.; Ramasamy, P.

2008-10-01

Single crystals of 3-nitroacetanilide, an organic nonlinear optical material has been grown by the Bridgman-Stockbarger method. The single crystal X-ray diffraction (XRD) data revealed the noncentrosymmetric crystal structure, which is an essential criterion for second harmonic generation. The crystalline nature of the grown crystals was confirmed using powder XRD techniques. The functional group of the compound is identified by FTIR spectrum. The thermal stability and its tendency to grow as single crystal in solution and in melt have been identified for the new title compound. The UV-vis spectrum of mNAA shows the lower optical cut off at 400 nm and was transparent in the visible region. The second harmonic generation efficiency was found using Kurtz powder technique. The dielectric constant and dielectric loss of the crystal were measured as a function of frequency and temperature, and the results are discussed.

Synthesis of the complex fluoride LiBaF 3 and optical spectroscopy properties of LiBaF 3: M( M=Eu,Ce) through a solvothermal process

NASA Astrophysics Data System (ADS)

Hua, Ruinian; Lei, Bingfu; Xie, Demin; Shi, Chunshan

2003-11-01

The complex fluoride LiBaF 3 and LiBaF 3: M( M=Eu, Ce) is solvothermally synthesized at 180°C and characterized by means of X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis and infrared spectroscopy. In the solvothermal process, the solvents, molar ratios of initial mixtures and reaction temperature play important roles in the formation of products. The excitation and emission spectra of the LiBaF 3: M( M=Eu,Ce) have been measured by fluorescence spectrophotometer. In the LiBaF 3:Eu emission spectra, there is one sharp line emission located at 360 nm arising from f→ f transition of Eu 2+ in the host lattice, and typical doublet 5 d-4 f emission of Ce 3+ in LiBaF 3 powder is shown.

Synthesis of thoria nano-particles at low temperature through base electrogeneration on steel 316L surface: Effect of current density

NASA Astrophysics Data System (ADS)

Yousefi, Taher; Torab-Mostaedi, Meisam; Mobtaker, Hossein Ghasemi; Keshtkar, Ali Reza

2016-10-01

The strategy developed in this study, offers significant advantages (simplicity and cleanness of method and also a product purity and new morphology of the product) over the conventional routes for the synthesis of ThO2 nanostructure. The effect of current density on morphology was studied. The synthesized powder was characterized by means of Powder X-ray Diffraction (PXRD), Transmission Electron Microscopy (TEM, Phillips EM 2085) Brunauer-Emmett-Teller (BET) and Fourier Transform Infrared (FT-IR) spectroscopy. The results show that the current density has a great effect on the morphology of the samples. The average size of the particles decreases as the applied current density increases and the average size of the samples decreases from 50 to 15 nm when the current density increases from 2 to 5 mA cm-2.

Insertion of Guest Molecules into a Mixed Ligand Metal-Organic Framework via Single-Crystal-to-Single Crystal Guest Exchange

DTIC Science & Technology

2014-07-01

powder x-ray diffraction (PXRD), thermogravimentric analysis (TGA), and Fourier transform infrared (FTIR). 15. SUBJECT TERMS Metal organic frame work...the inclusion by using a variety of analytical techniques, such as powder x-ray diffraction (PXRD), thermo-gravimetric analysis (TGA), Fourier...Characterizations Analysis of the MOF and the complexes with the MOF and the guest molecules was performed using an Agilent GC-MS (Model 6890N GC and Model 5973N

Development of scanning electron and x-ray microscope

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

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

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

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

Aldridge, James D.; Womick, Jordan M.; Rosmus, Kimberly A.

Novel quaternary lanthanide-substituted oxides of stoichiometry LnxY2-xTi2O7 (where Ln is lanthanum, neodymium, samarium, gadolinium, or ytterbium) were prepared by traditional high-temperature, solid-state techniques and characterized by X-ray powder diffraction. Samples with nominal values of x up to 1.0 were attempted. The well-studied ternary cubic pyrochlore compound yttrium titanium oxide (Y2Ti2O7, space group Fd-3m, Z = 8), served as a parent structural framework in which Ln3+ cations were substituted on the Y3+ site. Laboratory-grade X-ray powder diffraction data revealed pure quaternary pyrochlore phases for LnxY2-xTi2O7 with x ≤ 0.2. Pyrochlore phase purity was verified by Rietveld analysis using high-resolution synchrotron X-raymore » powder diffraction data when x ≤ 0.2, however, for La3+ substitution specifically, pure quaternary pyrochlore formed at x<0.1. Band gap energies on selected samples were determined using optical diffuse reflectance spectroscopy and showed that these materials can be classified as electrical insulators with indirect band gap energies around 3.7 eV.« less

Normal incidence x-ray mirror for chemical microanalysis

DOEpatents

Carr, M.J.; Romig, A.D. Jr.

1987-08-05

An x-ray mirror for both electron column instruments and micro x-ray fluorescence instruments for making chemical, microanalysis comprises a non-planar mirror having, for example, a spherical reflecting surface for x-rays comprised of a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on a substrate and whose layers have a thickness which is a multiple of the wavelength being reflected. For electron column instruments, the wavelengths of interest lie above 1.5nm, while for x-ray fluorescence instruments, the range of interest is below 0.2nm. 4 figs.

X-ray lithography using holographic images

DOEpatents

Howells, Malcolm R.; Jacobsen, Chris

1995-01-01

A non-contact X-ray projection lithography method for producing a desired X-ray image on a selected surface of an X-ray-sensitive material, such as photoresist material on a wafer, the desired X-ray image having image minimum linewidths as small as 0.063 .mu.m, or even smaller. A hologram and its position are determined that will produce the desired image on the selected surface when the hologram is irradiated with X-rays from a suitably monochromatic X-ray source of a selected wavelength .lambda.. On-axis X-ray transmission through, or off-axis X-ray reflection from, a hologram may be used here, with very different requirements for monochromaticity, flux and brightness of the X-ray source. For reasonable penetration of photoresist materials by X-rays produced by the X-ray source, the wavelength X, is preferably chosen to be no more than 13.5 nm in one embodiment and more preferably is chosen in the range 1-5 nm in the other embodiment. A lower limit on linewidth is set by the linewidth of available microstructure writing devices, such as an electron beam.

Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

NASA Astrophysics Data System (ADS)

Kara, P.; Csetényi, L. J.; Borosnyói, A.

2016-04-01

In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

Fabrication, characterization and fracture study of a machinable hydroxyapatite ceramic.

PubMed

Shareef, M Y; Messer, P F; van Noort, R

1993-01-01

In this study the preparation of a machinable hydroxyapatite from mixtures of a fine, submicrometer powder and either a coarse powder composed of porous aggregates up to 50 microns or a medium powder composed of dense particles of 3 microns median size is described. These were characterized using X-ray diffraction, transmission and scanning electron microscopy and infra-red spectroscopy. Test-pieces were formed by powder pressing and slip casting mixtures of various combinations of the fine, medium and coarse powders. The fired test-pieces were subjected to measurements of firing shrinkage, porosity, bulk density, tensile strength and fracture toughness. The microstructure and composition were examined using scanning electron microscopy and X-ray diffraction. For both processing methods, a uniform interconnected microporous structure was produced of a high-purity hydroxyapatite. The maximum tensile strength and fracture toughness that could be attained while retaining machinability were 37 MPa and 0.8 MPa m1/2 respectively.

Eco-friendly synthesis of Solanum trilobatum extract-capped silver nanoparticles is compatible with good antimicrobial activities

NASA Astrophysics Data System (ADS)

Ramanathan, Santheraleka; Gopinath, Subash C. B.; Anbu, Periasamy; Lakshmipriya, Thangavel; Kasim, Farizul Hafiz; Lee, Choul-Gyun

2018-05-01

This study focused on the evaluation of antimicrobial activity of silver nanoparticles (AgNPs) after their green synthesis by means of a Solanum trilobatum bark extract. The obtained product with an intense surface plasmon resonance band at ∼442 nm with UV-visible spectroscopic analysis indicated the formation of AgNPs. The morphology of AgNPs was observed under transmission electron microscopy and field emission scanning electron microscopy, displayed that the eco-friendly synthesized AgNPs have a spherical shape with an average size of ∼25 nm in diameter. X-ray powder diffraction and selected area electron diffraction analyses confirmed that the AgNPs are crystalline in nature. Fourier transform infrared spectroscopy indicated that the AgNPs capped with active ingredients of the bark extract. X-ray photoelectron spectroscopy revealed elemental composition of the AgNPs. The performance of S. trilobatum bark extract-capped AgNPs in terms of inhibition of microbial growth was studied by disc diffusion and well diffusion assays. Eco-friendly synthesized S. trilobatum extract-capped AgNPs were found to possess enhanced antimicrobial properties: growth inhibition of gram-negative and gram-positive bacteria and of fungal species. These results demonstrated the potential applications of the indigenous medicinal plants to the field of nanotechnology.

In situ hydrothermal syntheses, structures and photoluminescent properties of four novel metal-organic frameworks constructed by lanthanide (Ln=Ce(III), Pr(III), Eu(III)) and Cu(I) metals with flexible dicarboxylate acids and piperazine-based ligands

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

Ay, Burak; Karaca, Serkan; Yildiz, Emel, E-mail: eeyildiz@cu.edu.tr

2016-01-15

Four novel metal-organic frameworks,[Cu{sub 2}Cl{sub 2}(pyrz)]{sub n} (1) and (H{sub 2}pip){sub n}[Ln{sub 2}(pydc){sub 4}(H{sub 2}O){sub 2}]{sub n} (Ln=Ce (2), Pr (3) and Eu (4), H{sub 2}pzdc=2,3-pyrazinedicarboxylic acid, pyrz=pyrazine, H{sub 2}pydc=2,6-pyridinedicarboxylic acid, H{sub 2}pip=piperazine) have been synthesized under hydrothermal conditions and characterized by the elemental analysis, ICP, Far IR (FIR), FT-IR spectra, TGA, single crystal X-ray diffraction analysis and powder X-ray diffraction (PXRD). Compound 1 is two-dimensional containing Cl-Cu-Cl sites, while the lanthanide complexes contain one-dimensional infinite Ln–O-Ln chains. All the complexes show high thermal stability. The complexes 1–3 exhibit luminescence emission bands at 584, 598 and 614 nm at roommore » temperature when excited at 300 nm. Complex 4 exhibits bright red solid-state phosphorescence upon exposure to UV radiation at room temperature. - Graphical abstract: Four novel metal-organic frameworks have been synthesized under hydrothermal conditions. Thermal and luminescent properties of the compounds have been investigated.« less

Design and evaluation of self-nanoemulsifying pellets of repaglinide.

PubMed

Desai, N S; Nagarsenker, M S

2013-09-01

The aim of study was to develop self-nanoemulsifying pellets (SNEP) for oral delivery of poorly water soluble drug, repaglinide (RPG). Solubility of RPG in oily phases and surfactants was determined to identify components of self-nanoemulsifying drug delivery system (SNEDDS). The surfactants and cosurfactants were screened for their ability to emulsify oily phase. Ternary phase diagrams were constructed to identify nanoemulsification area for the selected systems. SNEDDS formulations with globule size less than 100 nm were evaluated for in vivo anti-hyperglycemic activity in neonatal streptozotocin rat model. A significant reduction in glucose levels was produced by optimized SNEDDS formulation in comparison to the control group. The optimized SNEDDS formulations were pelletized via extrusion/spheronization technique using microcrystalline cellulose and lactose. SNEP were characterized by X-ray powder diffraction and scanning electron microscopy. X-ray diffraction study indicated loss of crystallinity of RPG in SNEP. The SNEP exhibited good flow properties, mechanical strength and formed nanoemulsion with globule size less than 200 nm. SNEP showed in vitro release of more than 80% RPG in 10 min which was significantly higher than RPG containing reference pellets. In conclusion, our studies illustrated that RPG, a poorly water soluble drug can be successfully formulated into SNEP which can serve as a promising system for the delivery of poorly water soluble drugs.

Monodisperse colloidal gallium nanoparticles: synthesis, low temperature crystallization, surface plasmon resonance and Li-ion storage.

PubMed

Yarema, Maksym; Wörle, Michael; Rossell, Marta D; Erni, Rolf; Caputo, Riccarda; Protesescu, Loredana; Kravchyk, Kostiantyn V; Dirin, Dmitry N; Lienau, Karla; von Rohr, Fabian; Schilling, Andreas; Nachtegaal, Maarten; Kovalenko, Maksym V

2014-09-03

We report a facile colloidal synthesis of gallium (Ga) nanoparticles with the mean size tunable in the range of 12-46 nm and with excellent size distribution as small as 7-8%. When stored under ambient conditions, Ga nanoparticles remain stable for months due to the formation of native and passivating Ga-oxide layer (2-3 nm). The mechanism of Ga nanoparticles formation is elucidated using nuclear magnetic resonance spectroscopy and with molecular dynamics simulations. Size-dependent crystallization and melting of Ga nanoparticles in the temperature range of 98-298 K are studied with X-ray powder diffraction, specific heat measurements, transmission electron microscopy, and X-ray absorption spectroscopy. The results point to delta (δ)-Ga polymorph as a single low-temperature phase, while phase transition is characterized by the large hysteresis and by the large undercooling of crystallization and melting points down to 140-145 and 240-250 K, respectively. We have observed size-tunable plasmon resonance in the ultraviolet and visible spectral regions. We also report stable operation of Ga nanoparticles as anode material for Li-ion batteries with storage capacities of 600 mAh g(-1), 50% higher than those achieved for bulk Ga under identical testing conditions.

Monodisperse Colloidal Gallium Nanoparticles: Synthesis, Low Temperature Crystallization, Surface Plasmon Resonance and Li-Ion Storage

PubMed Central

2015-01-01

We report a facile colloidal synthesis of gallium (Ga) nanoparticles with the mean size tunable in the range of 12–46 nm and with excellent size distribution as small as 7–8%. When stored under ambient conditions, Ga nanoparticles remain stable for months due to the formation of native and passivating Ga-oxide layer (2–3 nm). The mechanism of Ga nanoparticles formation is elucidated using nuclear magnetic resonance spectroscopy and with molecular dynamics simulations. Size-dependent crystallization and melting of Ga nanoparticles in the temperature range of 98–298 K are studied with X-ray powder diffraction, specific heat measurements, transmission electron microscopy, and X-ray absorption spectroscopy. The results point to delta (δ)-Ga polymorph as a single low-temperature phase, while phase transition is characterized by the large hysteresis and by the large undercooling of crystallization and melting points down to 140–145 and 240–250 K, respectively. We have observed size-tunable plasmon resonance in the ultraviolet and visible spectral regions. We also report stable operation of Ga nanoparticles as anode material for Li-ion batteries with storage capacities of 600 mAh g–1, 50% higher than those achieved for bulk Ga under identical testing conditions. PMID:25133552

Upconversion luminescence of Er3+/Yb3+ doped Sr5(PO4)3OH phosphor powders

NASA Astrophysics Data System (ADS)

Mokoena, P. P.; Swart, H. C.; Ntwaeaborwa, O. M.

2018-04-01

Sr5(PO4)3OH co-doped with Er3+and Yb3+ powder phosphors were synthesized by urea combustion method. The crystal structure was analyzed using X-ray diffraction (XRD). Particle morphology was analyzed using a Jeol JSM 7800F thermal field emission scanning electron microscope (FE-SEM) and the chemical composition analysis was carried out using an Oxford Instruments AzTEC energy dispersive spectrometer (EDS) attached to the FE-SEM. Upconversion emission was measured by using a FLS980 Spectrometer equipped with a 980 nm NIR laser as the excitation source, and a photomultiplier (PMT) detector. The XRD data of the Sr5(PO4)3OH powder exhibited characteristic diffraction patterns of the hexagonal structure referenced in the standard JCPDS card number 00-033-1348. The sharp peaks revealed the formation of crystalline Sr5(PO4)3OH. The powders were made up of hexagonal nanospheres. The enhanced red emission due to the 4F9/2 → 4I15/2 transitions of Er3+ was observed and was attributed to up conversion (UC) energy transfer from Yb3+. The upconversion energy transfer mechanism from Yb3+ to Er3+ is discussed.

Preparation and characterization of natural bentonite in to nanoparticles by co-precipitation method

NASA Astrophysics Data System (ADS)

Sirait, Makmur; Bukit, Nurdin; Siregar, Nurdin

2017-01-01

The nanoparticle based on natural bentonite from Pahae village had been prepared using co-precipitation method. Bentonite was dried in the oven at 100°C during a week. Bentonite is crushed using a mortal and milled by planetary ball mill to obtain the powder form. Further, the bentonite powder is activated with chemical reaction by dissolves the 50 g bentonite to 100 ml of HCl at 10 M. The magnetic stirrer was employed to mix the solution at 300 rpm and temperature 70°C. After that, the bentonite solution is washed using distilled water until the pH is neutral. The bentonite powder is calcined at temperature of 600°C for 1 hour with fix increment 150°C. Finally, the powder is given High Energy Milling (HEM) treatment for 30 minutes to obtain the particle size. The X-ray Difractometer (XRD) and Scanning Electron Microscope (SEM) were used to characterize. From the characterization results it is reported that the average of bentonite nanoparticle size is 35.26 nm and the chemical constituents of natural bentonite Pahae are Al, Si, Ca, Fe and Ti.

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

Mossaad, Christina; Starr, Matthew; Payzant, E Andrew

The objective of the present paper was to produce nanoscale hydroxyapatite at room temperature under 10 nm through a simple method that requires no specialized equipment, surfactants, or additives. The Ca(C2H3O2)2-K3PO4-H2O synthesis system explored in previous literature was employed and the nanoscale powder product completely characterized through x-ray diffraction, transmission electron microscopy, BET nitrogen surface area adsorption, helium pycnometry, TGA and Karl Fisher titration. In accordance with other materials, it was found that hydroxyapatite under 5 nm produced by this chemistry undergoes an uphill phase transformation when left in dry storage over 5 months. Although it is possible to producemore » hydroxyapatite (and other materials) in this size range, it is imperative that care is taken through storage alterations to prevent any undesirable changes in structure or surface chemistry« less

Synthesis and spectroscopic characterization of gold nanobipyramids prepared by a chemical reduction method

NASA Astrophysics Data System (ADS)

Thanh Ngo, Vo Ke; Phat Huynh, Trong; Giang Nguyen, Dang; Phuong Uyen Nguyen, Hoang; Lam, Quang Vinh; Dat Huynh, Thanh

2015-12-01

Gold nanobipyramids (NBPs) have attracted much attention because they have potential for applications in smart sensing devices, such as medical diagnostic equippments. This is due to the fact that they show more advantageous plasmonic properties than other gold nanostructures. We describe a chemical reduction method for synthesizing NBPs using conventional heating with ascorbic acid reduction and cetyltrimethylamonium bromide (CTAB) + AgNO3 as capping agents. The product was characterized by ultraviolet-visible spectroscopy (UV-vis), Fourier transmission infrared spectroscopy (FTIR), transmission electron microscopy (TEM), x-ray powder diffraction (XRD). The results showed that gold nanoparticles were formed with bipyramid shape (tip-to-tip distance of 88.4 ± 9.4 nm and base length of 29.9 ± 3.2 nm) and face-centered-cubic crystalline structure. Optimum parameters for preparation of NBPs are also found.

Study on photocatalytic activity of nanosized Co0.3Zn0.7Fe2O4 synthesized by hydrothermal method

NASA Astrophysics Data System (ADS)

Mondal, R.; Sarkar, K.; Dey, S.; Bhattacharjee, S.; Ghosh, C. K.; Kumar, S.

2018-04-01

We have reported the photocatalytic activity of nanosized Co0.3Zn0.7Fe2O4 (CZM) synthesized by hydrothermal method. Powder x-ray diffraction (PXRD), field emission and transmission electron microscopic techniques have been employed for structural and microstructural characterization of the sample. The Rietveld refinement of the PXRD pattern of CZM reveals that the sample is a single phase spinel ferrite of F d 3 ¯m symmetry having crystallite size ˜ 20 nm. The average particle size is ˜ 23 nm. The photocatalytic study suggests that CZM can be suitably used as an efficient (rate constant and % degradation are 7.4×10-2 min-1, 95.76 % at 40 min, respectively), magnetically separable, recyclable photocatalyst for removal of Congo Red from its aqueous solution.

Defect Control of the WC Hardmetal by Mixing Recycled WC Nano Powder and Tungsten Powder

NASA Astrophysics Data System (ADS)

Hur, Man Gyu; Shin, Mi Kyung; Kim, Deug Joong; Yoon, Dae Ho

2018-03-01

Tungsten metal powder was added to recycled WC nano powder to control the macro and micro defects of WC hardmetal. The macro and micro defects caused by the excess carbon in the recycled WC powder were markedly removed after the addition of tungsten metal powder ranging from 2 to 6 wt%. The density and hardness of the WC hardmetals also increased due to the removal of defects after adding the tungsten metal powder. The density and hardness of WC hardmetals with the addition of W metal powder ranged from 8 to 12 wt% increased linearly as the W metal powder content increased due to the formation of a new (Co- and W-rich WC) composition. The surface morphology of the WC hardmetals was observed via field emission scanning electron microscopy, and a quantitative elemental analysis was conducted via X-ray fluorescence spectrometry and energy dispersive X-ray analysis. The density and hardness of the WC hardmetals were respectively measured using an analytical balance and a Vikers hardness tester. The effect on the defects in the recycled WC hardmetals through the addition of the tungsten metal powder was discussed in detail.

Synthesis and Characterization of Manganese Doped Silicon Nanoparticles

PubMed Central

Zhang, Xiaoming; Brynda, Marcin; Britt, R. David; Carroll, Elizabeth; Larsen, Delmar S.; Louie, Angelique Y.; Kauzlarich, Susan M.

2008-01-01

Mn doped Si nanoparticles have been synthesized via a low temperature solution route and characterize by X-ray powder diffraction, TEM, optical and emission spectroscopy and by EPR. The particle diameter was 4 nm and the surface was capped by octyl groups. 5% Mn doping resulted in a green emission with slightly lower quantum yield than undoped Si nanoparticles prepared by the same method. Mn2+ doped into the nanoparticle is confirmed by epr hyperfine and the charge carrier dynamics were probed by ultrafast transient absorption spectroscopy. Both techniques are consistent with Mn2+ on or close to the surface of the nanoparticle. PMID:17691792

Development of a Novel Ni-Fe-Cr-B-Si Interlayer Material for Transient Liquid Phase Bonding of Inconel 718

NASA Astrophysics Data System (ADS)

Tarai, U. K.; Robi, P. S.; Pal, Sukhomay

2018-04-01

A Ni-Cr-Fe-Si-B based interlayer material was developed by mechanical alloying (MA) process in a high-energy planetary ball mill. Equiaxed alloy powders of size 12 µm was obtained after milling for 50 hours. X-ray diffraction analysis of the milled powder revealed that milling of elemental powders initially resulted in microcrystalline alloy powder having face centered cubic structure, which on subsequent milling resulted in nano-crystallice alloy powder with a crystallite size of 3.2 nm. XRD analysis also reveals formation of metastable eutectic alloys resulting in lowering of the melting point of the interlayer material to 1025 °C. IN 718 superalloy samples were joined at 1050°C using the developed interlayer. A homogeneous joint was formed by the newly developed interlayer material. Three different zones were observed at the bond (i) isothermally solidified zone, (ii) diffusion affected zone and (iii) unaffected base metal. In the diffusion-affected zone, boron was present at the grain boundaries of Ni γ matrix in bulky metal borides form. The diffusion of boron from interlayer material into the base material was mechanism of isothermal solidification and bond formation in transient liquid phase bonding of IN 718.

K3Na(SO4)2 : Eu nanoparticles for high dose of ionizing radiation

NASA Astrophysics Data System (ADS)

Sahare, P. D.; Ranjan, Ranju; Salah, Numan; Lochab, S. P.

2007-02-01

K3Na(SO4)2 : Eu nanocrystalline powder was synthesized by the chemical co-precipitation method. The x-ray diffraction pattern of the nanomaterials shows a hexagonal structure for its crystals having grain size of ~28 nm. Transmission electron microscopy revealed that the K3Na(SO4)2 : Eu nanoparticles are single crystals with almost a uniform shape and size. Thermoluminescence (TL) was taken after irradiating the samples at various exposures of γ-rays from a 60Co source. A prominent TL glow peak is observed at 423 K along with three small peaks/shoulders at around 382, 460 and 509 K. The observed TL sensitivity of the prepared nanocrystalline powder is around 4 times more than that of LiF : Mg,Ti (TLD-100) phosphor. The 423 K peak of the nanomaterial phosphor eventually shows a near linear response with exposures increasing up to very high values (as high as 70 kGy), where all the other TLD phosphors saturate. This property along with its other desired properties such as high sensitivity, relatively simple glow curve structure and low fading makes the nanocrystalline phosphor a suitable dosimeter to estimate low as well as high exposures of γ-rays. TL analysis using the glow curve deconvolution technique was also done for determining different trapping parameters.

Spectromicroscope for the PHotoelectron Imaging of Nanostructures with X-rays (SPHINX): performance in biology, medicine and geology.

PubMed

Frazer, Bradley H; Girasole, Marco; Wiese, Lisa M; Franz, Torsten; De Stasio, Gelsomina

2004-05-01

Several X-ray PhotoElectron Emission spectroMicroscopes (X-PEEMs) exist around the world at this time. We present recent performance and resolution tests of one of them, the Spectromicroscope for PHotoelectron Imaging of Nanostructures with X-rays (SPHINX) X-PEEM, installed at the University of Wisconsin Synchrotron Radiation Center. With this state-of-the-art instrument we demonstrate chemical analysis capabilities on conducting and insulating specimens of diverse interests, and an unprecedented lateral resolution of 10 nm with monochromatic X-rays and 7.2 nm with ultraviolet illumination.

Synthesis and Characterization of Cholesterol Nano Particles by Using w/o Microemulsion Technique

NASA Astrophysics Data System (ADS)

Vyas, Poorvesh M.; Vasant, Sonal R.; Hajiyani, Rakesh R.; Joshi, Mihir J.

2010-10-01

Cholesterol is one of the most abundant and well known steroids in the animal kingdom. Cholesterol rich micro-emulsions and nano-emulsions are useful for the treatment of breast cancer and gynecologic cancers. The nano particles of cholesterol and other pharmaceutically important materials have been reported. In the present investigation, the nano particles of cholesterol were synthesized by direct precipitation technique using triton X-100/water/n-butanol micro-emulsion. The average particle size of cholesterol nano particles was estimated by applying Scherrer's formula to the powder X-ray diffraction pattern, which was found to be 22 nm. The nanoparticles of cholesterol were observed by using TEM and the particle size was found within the range from 15 nm-31 nm. The distribution of particle size was studied through DLS. The nanoparticles of cholesterol were characterized by using FT-IR spectroscopy and the force constant was also calculated for O-H, C-H and C-O bonds. The thermal response of nanoparticles of cholesterol was studied by TGA, which showed that the nanoparticles were stable up to 200 °C and then decomposed. Kinetic and thermodynamic parameters of decomposition process were also calculated by applying Coats and Redfern formula to thermo-gram.

Characterization of composite materials based on cement-ceramic powder blended binder

NASA Astrophysics Data System (ADS)

Kulovaná, Tereza; Pavlík, Zbyšek

2016-06-01

Characterization of newly developed composite mortars with incorporated ceramic powder coming from precise brick cutting as partial Portland cement replacement up to 40 mass% is presented in the paper. Fine ceramic powder belongs to the pozzolanic materials. Utilization of pozzolanic materials is accompanied by lower request on energy needed for Portland clinker production which generally results in lower production costs of blended binder and lower CO2 emission. In this paper, the ceramic powder is used in cement based mortar composition in amount of 8, 16, 24, 32, and 40 mass% of cement. Chemical composition of ceramic powder is analyzed by X-Ray Fluorescence and X-Ray Diffraction. The particle size distribution of ceramics is accessed on laser diffraction principle. For 28 days cured mortar samples, basic physical and mechanical properties are experimentally determined. The obtained results demonstrate that ceramic powder has potential to replace a part of Portland cement in composition of cement based composites and to reduce negative environmental impact of their production.

Neutron and X-ray diffraction of plasma-sprayed zirconia-yttria thermal barrier coatings

NASA Technical Reports Server (NTRS)

Shankar, N. R.; Herman, H.; Singhal, S. P.; Berndt, C. C.

1984-01-01

ZrO2-7.8mol. pct. YO1.5, a fused powder, and ZrO2-8.7mol. pct. YO1.5, a prereacted powder, were plasma-sprayed onto steel substrates. Neutron diffraction and X-ray diffraction of the as-received powder, the powder plasma sprayed into water, as-sprayed coatings, and coatings heat-treated for 10 and 100 h were carried out to study phase transformations and ordering of the oxygen ions on the oxygen sublattice. The as-received fused powder has a much lower monoclinic percentage than does the pre-reacted powder, this resulting in a much lower monoclinic percentage in the coating. Heat treatment increases the percentages of the cubic and monoclinic phases, while decreasing the tetragonal content. An ordered tetragonal phase is detected by the presence of extra neutron diffraction peaks. These phase transformations and ordering will result in volume changes. The implications of these transformations on the performance of partially stabilized zirconia thermal barrier coatings is discussed.

Characterization of composite materials based on cement-ceramic powder blended binder

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

Kulovaná, Tereza; Pavlík, Zbyšek

Characterization of newly developed composite mortars with incorporated ceramic powder coming from precise brick cutting as partial Portland cement replacement up to 40 mass% is presented in the paper. Fine ceramic powder belongs to the pozzolanic materials. Utilization of pozzolanic materials is accompanied by lower request on energy needed for Portland clinker production which generally results in lower production costs of blended binder and lower CO{sub 2} emission. In this paper, the ceramic powder is used in cement based mortar composition in amount of 8, 16, 24, 32, and 40 mass% of cement. Chemical composition of ceramic powder is analyzedmore » by X-Ray Fluorescence and X-Ray Diffraction. The particle size distribution of ceramics is accessed on laser diffraction principle. For 28 days cured mortar samples, basic physical and mechanical properties are experimentally determined. The obtained results demonstrate that ceramic powder has potential to replace a part of Portland cement in composition of cement based composites and to reduce negative environmental impact of their production.« less

Synthesis, nucleation, growth, structural, spectral, thermal, linear and nonlinear optical studies of novel organic NLO crystal: 4-fluoro 4-nitrostilbene (FONS).

PubMed

Dinakaran, Paul M; Kalainathan, S

2013-03-15

A novel organic nonlinear optical material 4-fluoro 4-nitrostilbene (FONS), with molecular formula (C(14)H(10)FNO(2)) has been synthesized. Using ethyl methyl ketone as solvent, the synthesized material has been repeatedly recrystallized to minimize the impurities and good optical quality single crystals were harvested by slow evaporation method. Single crystal X-ray diffraction analysis reveals that the grown FONS crystal belongs to monoclinic system with noncentrosymmetric space group "P2(1)". The powder X-ray diffraction pattern of FONS has been recorded. Functional groups of the title compound were confirmed by FTIR and the molecular structure was confirmed by (1)HNMR. The UV-vis-NIR absorption study reveals no absorption in the visible region and the cut-off wavelength was found to be at 408 nm. Optical band gap (E(g)) of the grown crystal was found to be 3.27 eV and also the optical constants were determined. Thermal behaviour of the FONS has been studied by TGA/DTA analyses. From the mass spectrum, the ratio of compound formation of FONS was analyzed. The NLO property has been confirmed by Kurtz and Perry powder SHG technique and the SHG efficiency of FONS (262 mV) crystal was found to be 12 times greater than that of KDP (21.7 mV). Copyright © 2013 Elsevier B.V. All rights reserved.

Floral Biosynthesis of Mn3O4 and Fe2O3 Nanoparticles Using Chaenomeles sp. Flower Extracts for Efficient Medicinal Applications

NASA Astrophysics Data System (ADS)

Karunakaran, Gopalu; Jagathambal, Matheswaran; Kolesnikov, Evgeny; Dmitry, Arkhipov; Ishteev, Artur; Gusev, Alexander; Kuznetsov, Denis

2017-08-01

Manganese oxide (Mn3O4) and iron oxide (Fe2O3) nanoparticles were successfully synthesized with the flower extracts of Chaenomeles sp. This is the first ever approach to synthesize nanoparticles from Chaenomeles sp. flower extracts. The organic molecules present in the flower extracts actively converted the nitrate precursor into its corresponding nanoparticles. The organic molecules that are involved in the synthesis of nanoparticles are identified using different phytochemical and gas chromatography-mass spectrometry analyses. The identified components are glycosides, alkaloids, terpenoids, saponins, flavonoids, quinines, and steroids. The structural and chemical compositions of the synthesized powder were also analyzed. The x-ray powder diffraction analysis revealed that the particles show tetragonal and rhombohedral crystalline phases. The Fourier transform infrared spectroscopy analysis showed the functional groups that are involved in the reduction of nitrates into the corresponding nanoparticles. Energy-dispersive x-ray spectroscopy analysis confirmed the presence of the elements in the synthesized nanoparticles. Transmission electron microscopy images showed the formation of spherical nanoparticles with an average size of 30-100 nm. Antioxidant analysis showed that the synthesized nanoparticles had excellent antioxidant potential. The antibacterial study showed that they inhibit the growth of harmful bacteria such as Pseudomonas aeruginosa and Streptococcus pyogenes. Thus, this study proposes a new eco-friendly and nontoxic method to synthesize nanoparticles for medicinal applications.

STRUCTURAL ANALYSIS OF THE COMBUSTION SYNTHESIZED Y3+ DOPED CERIA (Ce0.9Y0.1O1.95)

NASA Astrophysics Data System (ADS)

Jeyanthi, C. Esther; Siddheswaran, R.; Kumar, Pushpendra; Mangalaraja, R. V.; Siva Shankar, V.; Rajarajan, K.

2013-07-01

Y3+ doped CeO2 nanopowders (Ce0.9Y0.1O1.95, abbreviated as YDC) were synthesized by citrate-nitrate-auto combustion process using cerium nitrate hexahydrate, yttrium nitrate hexahydrate and citric acid. The as-synthesized powders were calcined at 700°C and converted into dense bodies followed by sintering at 1200°C. The microstructure of the synthesized powders and sintered bodies were examined by scanning electron microscopy (SEM). The surface morphology of the nanoparticles and clusters were also analysed by transmission electron microscopy (TEM). The particles size of the YDC was found to be in the range from 10 to 30 nm, which is in good agreement with the crystallite size calculated from X-ray peak broadening method. Also, the X-ray diffraction confirmed that the Ce0.9Y0.1O1.95 crystallizes as the cubic fluorite structure of pure ceria. The optical absorption by functional molecules, impurities and oxygen vacancies were analysed by FTIR and Raman spectroscopic studies. From the FTIR spectrum, the absorption peak found at 530 cm-1 is attributed to the vibrations of metal-oxygen bonds. The characteristic Raman peak was found to be 468 cm-1, and the minute absorption of oxygen vacancies were observed in the region 500-640 cm-1.

Soft x-ray reduction camera for submicron lithography

DOEpatents

Hawryluk, A.M.; Seppala, L.G.

1991-03-26

Soft x-ray projection lithography can be performed using x-ray optical components and spherical imaging lenses (mirrors), which form an x-ray reduction camera. The x-ray reduction is capable of projecting a 5x demagnified image of a mask onto a resist coated wafer using 4.5 nm radiation. The diffraction limited resolution of this design is about 135 nm with a depth of field of about 2.8 microns and a field of view of 0.2 cm[sup 2]. X-ray reflecting masks (patterned x-ray multilayer mirrors) which are fabricated on thick substrates and can be made relatively distortion free are used, with a laser produced plasma for the source. Higher resolution and/or larger areas are possible by varying the optic figures of the components and source characteristics. 9 figures.

Synthesis of Cu/CuO nanoparticles in mesoporous material by solid state reaction

NASA Astrophysics Data System (ADS)

Sohrabnezhad, Sh.; Valipour, A.

2013-10-01

The Mobil Composition of Matter No. 41 (MCM-41) containing 1.0 and 5.0 wt.% of Cu was synthesized under solid state reaction. The calcinations of samples were done at two different temperatures, 500 and 300 °C. X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM) were used for samples characterization. Powder X-ray diffraction showed that when Cu(CH3COO)2 content is about 1.0 wt.% in Cu/MCM-41, the guest CuO-NPs and copper ions is formed on the silica channel wall, and more exists in the crystalline state. When Cu(CH3COO)2 content exceeds this value (5.0 wt.%), CuO nanoparticles and Cu2+ ions can be observed in low crystalline state. From the diffuse reflectance spectra it was confirmed that 5 wt.% Cu/MCM-41 sample calcined at 500 °C show plasmon resonance band due to Cu nanoparticles in the range between 500 and 600 nm and small copper clusters Cun in 450 nm. It also shows that some of the Cu2+ ions are present octahedrally in extraframework position in all samples. Both fourier transform infrared and diffuse reflectance spectra indicate that some of Cu2+ ions are tetrahedrally within the framework position in 1 wt.% Cu/MCM-41 samples. TEM images indicated that nanoparticles size of CuO is in range of 30-40 nm.

Photocatalytic Activity of Vanadium-Substituted ETS-10

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

Nash,M.; Rykov, S.; Lobo, R.

2007-01-01

Various amounts of vanadium have been isomorphously substituted for titanium in ETS-10, creating samples with V/(V+Ti) ratios of 0.13, 0.33, 0.43, and 1.00 and characterized experimentally using Raman, near-edge X-ray absorption fine structure (NEXAFS), X-ray powder diffraction, N{sub 2} adsorption, scanning electron microscopy (SEM), UV/vis spectroscopy, and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Raman spectra reveal a disordered chain structure that contains different V-O bonds along with the presence of a V-O-Ti peak. The UV/vis spectra of the vanadium samples have three new absorption features in the visible region at 450, 594, and 850 nm, suggesting both V{sup 4+}more » and V{sup 5+} are present in the samples. NEXAFS results confirm the presence of both V{sup 5+} and V{sup 4+} in the vanadium samples, with a fraction of V{sup 4+} within the range of 0.2-0.4. The addition of vanadium lowers the band gap energy of ETS-10 from 4.32 eV to a minimum of 3.58 eV for the 0.43ETVS-10 sample. Studies of the photocatalytic polymerization of ethylene show that the 594 nm transition has no photocatalytic activity. The visible transition around 450 nm in the vanadium-incorporated samples is photocatalytically active, and the lower-concentration vanadium samples have higher photocatalytic activity than that of ETS-10 and AM-6, the all-vanadium analogue of ETS-10.« less

Broad visible emission from GaN nanowires grown on n-Si (1 1 1) substrate by PVD for solar cell application

NASA Astrophysics Data System (ADS)

Saron, K. M. A.; Hashim, M. R.

2013-04-01

Nanostructured gallium nitrides (GaNs) were grown on a catalyst-free Si (1 1 1) substrates using physical vapor deposition via thermal evaporation of GaN powder at 1150 °C in the absence of NH3 gas for different deposition time. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectrometer (EDX) results indicated that the growth of GaN nanostructure varies with deposition time. Both X-ray diffraction (XRD) patterns and Raman spectra reveals a hexagonal GaN with wurtzite structure. Photoluminescence (PL) showed that the UV emission was suppressed, and the visible band emission was enhanced with increasing deposition time. Enhancement of visible band emission from the GaN NWs is due to the increasement of deep level states, which was resulted from growth process. Current-voltage (IV) characteristics of GaN/Si heterostructure were measured and good rectifying behavior was observed for this photodiode (PD). The forward current under illumination was almost three times than that in the dark current at +5 V. Responsivity of the photodetector was 10.5 A/W at range from 350 nm to 500 nm, which rapidly increased to 13.6 A/W at 700 nm. We found that the fabricated photodiode PD has an infra-red (IR) photoresponse behavior. The analysis of optical and electrical properties indications that the grown GaN in the absent of NH3 is a promising optical material and has potential applications in photo voltage solar cell.

Effect of milling atmosphere on structural and magnetic properties of Ni-Zn ferrite nanocrystalline

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Hashim, Mansor; Ebrahimi-Kahrizsangi, Reza; Masoudi Mohamad, Taghi

2015-04-01

Powder mixtures of Zn, NiO, and Fe2O3 are mechanically alloyed by high energy ball milling to produce Ni-Zn ferrite with a nominal composition of Ni0.36Zn0.64Fe2O4. The effects of milling atmospheres (argon, air, and oxygen), milling time (from 0 to 30 h) and heat treatment are studied. The products are characterized using x-ray diffractometry, field emission scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and transmitted electron microscopy. The results indicate that the desired ferrite is not produced during the milling in the samples milled under either air or oxygen atmospheres. In those samples milled under argon, however, Zn/NiO/Fe2O3 reacts with a solid-state diffusion mode to produce Ni-Zn ferrite nanocrystalline in a size of 8 nm after 30-h-milling. The average crystallite sizes decrease to 9 nm and 10 nm in 30-h-milling samples under air and oxygen atmospheres, respectively. Annealing the 30-h-milling samples at 600 °C for 2 h leads to the formation of a single phase of Ni-Zn ferrite, an increase of crystallite size, and a reduction of internal lattice strain. Finally, the effects of the milling atmosphere and heating temperature on the magnetic properties of the 30-h-milling samples are investigated. Project supported by the University Putra Malaysia Graduate Research Fellowship Section.

X-ray standing wave analysis of nanostructures using partially coherent radiation

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

Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in; Das, Gangadhar; Bedzyk, M. J.

2015-09-07

The effect of longitudinal (or temporal) coherence on total reflection assisted x-ray standing wave (TR-XSW) analysis of nanoscale materials is quantitatively demonstrated by showing how the XSW fringe visibility can be strongly damped by decreasing the spectral resolution of the incident x-ray beam. The correction for nonzero wavelength dispersion (δλ ≠ 0) of the incident x-ray wave field is accounted for in the model computations of TR-XSW assisted angle dependent fluorescence yields of the nanostructure coatings on x-ray mirror surfaces. Given examples include 90 nm diameter Au nanospheres deposited on a Si(100) surface and a 3 nm thick Zn layer trapped on top amore » 100 nm Langmuir-Blodgett film coating on a Au mirror surface. Present method opens up important applications, such as enabling XSW studies of large dimensioned nanostructures using conventional laboratory based partially coherent x-ray sources.« less

Synthesis of CdS nanorods in soft template under gamma-irradiation.

PubMed

Zhao, Bing; Wang, Yanli; Zhang, Haijiao; Jiao, Zheng; Wang, Haobo; Ding, Guoji; Wu, Minghong

2009-02-01

CdS nano material which has a band gap of 2.42 eV at room temperature is a typical II-VII semiconductor having many commercial or potential applications, e.g., light-emitting diodes, solar cell and optoelectronic devices. In this paper, we use a new strategy to synthesize CdS nanorods. CdS nanorods were prepared in soft template under gamma-irradiation though the reaction of cadmium sulphide and thiacetamide (TAA). The formation process and characters of CdS nanorods was investigated in detail by transmission electron microscopy (TEM), electron diffraction (ED) pattern, X-ray powder diffraction (XRD), ultraviolet spectrophotometer (UV) and photoluminescence spectrophotometer (PL). In the experiment we proposed that the irradiation of gamma-ray accelerated the formation of S(2-) under acidic condition (pH = 3) and vinyl acetate (VAc) monomer formed pre-organized nano polymer tubules which were used as both templates and nanoreacters for the growth of CdS nanorods. In this process, we have obtained the CdS polycrystal nanorods with PVAc nano tubules and CdS single-crystal nanorods. The result of X-ray powder diffraction confirms that the crystal type of CdS nanorods is cubic F-43 m (216). The results from transmission electron microscopy and electron diffraction show that the concentrations of reactants and the dose rate of gamma-ray are key to produce appropriate CdS nanorods. Relatively low concentrations (Cd2+: 0.008-0.02 mol/L, Cd2+ : S(2-) = 1 : 2) of reactants and long time (1-2 d) of irradiation in low dose rate (6-14 Gy/min) are propitious to form CdS single-crystal nanorods with small diameter (less than 100 nm) and well length (2-5 microm). UV and PL characterizations show the sample have well optical properties.

X-ray diffraction-based electronic structure calculations and experimental x-ray analysis for medical and materials applications

NASA Astrophysics Data System (ADS)

Mahato, Dip Narayan

This thesis includes x-ray experiments for medical and materials applications and the use of x-ray diffraction data in a first-principles study of electronic structures and hyperfine properties of chemical and biological systems. Polycapillary focusing lenses were used to collect divergent x rays emitted from conventional x-ray tubes and redirect them to form an intense focused beam. These lenses are routinely used in microbeam x-ray fluorescence analysis. In this thesis, their potential application to powder diffraction and focused beam orthovoltage cancer therapy has been investigated. In conventional x-ray therapy, very high energy (˜ MeV) beams are used, partly to reduce the skin dose. For any divergent beam, the dose is necessarily highest at the entry point, and decays exponentially into the tissue. To reduce the skin dose, high energy beams, which have long absorption lengths, are employed, and rotated about the patient to enter from different angles. This necessitates large expensive specialized equipment. A focused beam could concentrate the dose within the patient. Since this is inherently skin dose sparing, lower energy photons could be employed. A primary concern in applying focused beams to therapy is whether the focus would be maintained despite Compton scattering within the tissue. To investigate this, transmission and focal spot sizes as a function of photon energy of two polycapillary focusing lenses were measured. The effects of tissue-equivalent phantoms of different thicknesses on the focal spot size were studied. Scatter fraction and depth dose were calculated. For powder diffraction, the polycapillary optics provide clean Gaussian peaks, which result in angular resolution that is much smaller than the peak width due to the beam convergence. Powder diffraction (also called coherent scatter) without optics can also be used to distinguish between tissue types that, because they have different nanoscale structures, scatter at different angles. Measurements were performed on the development of coherent scatter imaging to provide tissue type information in mammography. Atomic coordinates from x-ray diffraction data were used to study the nuclear quadrupole interactions and nature of molecular binding in DNA/RNA nucleobases and molecular solid BF3 systems.

Selective Laser Melting of Metal Powder Of Steel 3161

NASA Astrophysics Data System (ADS)

Smelov, V. G.; Sotov, A. V.; Agapovichev, A. V.; Tomilina, T. M.

2016-08-01

In this article the results of experimental study of the structure and mechanical properties of materials obtained by selective laser melting (SLM), metal powder steel 316L was carried out. Before the process of cultivation of samples as the input control, the morphology of the surface of the powder particles was studied and particle size analysis was carried out. Also, 3D X-ray quality control of the grown samples was carried out in order to detect hidden defects, their qualitative and quantitative assessment. To determine the strength characteristics of the samples synthesized by the SLM method, static tensile tests were conducted. To determine the stress X-ray diffraction analysis was carried out in the material samples.

Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments

NASA Astrophysics Data System (ADS)

Schlicker, Lukas; Doran, Andrew; Schneppmüller, Peter; Gili, Albert; Czasny, Mathias; Penner, Simon; Gurlo, Aleksander

2018-03-01

This work describes a device for time-resolved synchrotron-based in situ and operando X-ray powder diffraction measurements at elevated temperatures under controllable gaseous environments. The respective gaseous sample environment is realized via a gas-tight capillary-in-capillary design, where the gas flow is achieved through an open-end 0.5 mm capillary located inside a 0.7 mm capillary filled with a sample powder. Thermal mass flow controllers provide appropriate gas flows and computer-controlled on-the-fly gas mixing capabilities. The capillary system is centered inside an infrared heated, proportional integral differential-controlled capillary furnace allowing access to temperatures up to 1000 °C.

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

PubMed

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

2007-05-01

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

A green-yellow emitting oxyfluoride solid solution phosphor Sr[subscript 2]Ba(AlO[subscript 4]F)[subscript 1;#8722;x](SiO[subscript 5])x:Ce[superscript 3+] for thermally stable, high color rendition solid state white lighting

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

Denault, Kristin A.; George, Nathan C.; Paden, Sara R.

2012-10-23

A near-UV excited, oxyfluoride phosphor solid solution Sr{sub 1.975}Ce{sub 0.025}Ba(AlO{sub 4}F){sub 1-x}(SiO{sub 5}){sub x} has been developed for solid state white lighting applications. An examination of the host lattice, and the local structure around the Ce{sup 3+} activator ions through a combination of density functional theory, synchrotron X-ray and neutron powder diffraction and total scattering, and electron paramagnetic resonance, points to how chemical substitutions play a crucial role in tuning the optical properties of the phosphor. The maximum emission wavelength can be tuned from green ({lambda}{sub em} = 523 nm) to yellow ({lambda}{sub em} = 552 nm) by tuning themore » composition, x. Photoluminescent quantum yield is determined to be 70 {+-} 5% for some of the examples in the series. Excellent thermal properties were found for the x = 0.5 sample, with the photoluminescence intensity at 160 C only decreased to 82% of its room temperature value. Phosphor-converted LED devices fabricated using an InGaN LED ({lambda}{sub max} = 400 nm) exhibit high color rendering white light with R{sub a} = 70 and a correlated color temperature near 7000 K. The value of R{sub a} could be raised to 90 by the addition of a red component, and the correlated color temperature lowered to near 4000 K.« less

High spatial resolution PEELS characterization of FeAl nanograins prepared by mechanical alloying

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

Valdre, G.; Botton, G.A.; Brown, L.M.

The authors investigate the nanograin ``chemical`` structure in a nanostructured material of possible industrial application (Fe-Al system) prepared by conventional mechanical alloying via ball milling in argon atmosphere. They restrict themselves to the structural and nanochemical behavior of ball-milled nanocrystalline Fe-Al powders with atomic composition Fe{sub 3}Al, corresponding to a well-known intermetallic compound of the Fe-Al system. Scanning transmission electron microscopy (STEM) equipped with a parallel detection electron energy loss spectrometer (PEELS) has provided an insight on the ``chemical`` structure of both nanograins and their surface at a spatial resolution of better than 1 nm. The energy loss near edgemore » structure of the Al L loss reveals that the Al coordination is similar to a B2 compound and the oxidation of the powder during processing may play a significant role in the stabilization of the intermetallic phases. Conventional transmission electron microscopy (TEM) was used for the structural characterization of the material after the ball milling; powder X-ray diffraction (XRD) aided the investigation.« less

The effect of carbon nanotubes functionalization on the band-gap energy of TiO2-CNT nanocomposite

NASA Astrophysics Data System (ADS)

Shahbazi, Hessam; Shafei, Alireza; Sheibani, Saeed

2018-01-01

In this paper the morphology and structure of TiO2-CNT nanocomposite powder obtained by an in situ sol-gel process were investigated. The synthesized nanocomposite powders were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and diffuse reflectance spectroscopy (DRS). The effect of functionalizing of CNT on the properties was studied. XRD results showed amorphous structure before calcination. Also, anatase phase TiO2 was formed after calcination at 400 °C. The SEM results indicate different distributions of TiO2 on CNTs. As a result, well dispersed TiO2 microstructure on the surface of CNTs was observed after functionalizing, while compact and large aggregated particles were found without functionalizing. The average thickness of uniform and well-defined coated TiO2 layer was in the range of 30-40 nm. The DRS results have determined the reflective properties and band gap energies of nanocomposite powders and have shown that functionalizing of CNTs caused the change of band-gap energy from 2.98 to 2.87 eV.

Preparation and optical properties of iron-modified titanium dioxide obtained by sol-gel method

NASA Astrophysics Data System (ADS)

Hreniak, Agnieszka; Gryzło, Katarzyna; Boharewicz, Bartosz; Sikora, Andrzej; Chmielowiec, Jacek; Iwan, Agnieszka

2015-08-01

In this paper twelve TiO2:Fe powders prepared by sol-gel method were analyzed being into consideration the kind of iron compound applied. As a precursor titanium (IV) isopropoxide (TIPO) was used, while as source of iron Fe(NO3)3 or FeCl3 were tested. Fe doped TiO2 was obtained using two methods of synthesis, where different amount of iron was added (1, 5 or 10% w/w). The size of obtained TiO2:Fe particles depends on the iron compound applied and was found in the range 80-300 nm as it was confirmed by SEM technique. TiO2:Fe particles were additionally investigated by dynamic light scattering (DLS) method. Additionally, for the TiO2:Fe particles UV-vis absorption and the zeta potential were analyzed. Selected powders were additionally investigated by magnetic force microscopy (MFM) and X-ray diffraction techniques. Photocatalytic ability of Fe doped TiO2 powders was evaluated by means of cholesteryl hemisuccinate (CHOL) degradation experiment conducted under the 30 min irradiation of simulated solar light.

Synthesis, characterization and magnetic properties of MFe2O4 (M=Co, Mg, Mn, Ni) nanoparticles using ricin oil as capping agent

NASA Astrophysics Data System (ADS)

Gherca, Daniel; Pui, Aurel; Cornei, Nicoleta; Cojocariu, Alina; Nica, Valentin; Caltun, Ovidiu

2012-11-01

We focused on obtaining MFe2O4 nanoparticles using ricin oil solution as surfactant and on their structural characterization and magnetic properties. The annealed samples at 500 °C in air for 6 h were analyzed for the crystal phase identification by powder X-ray diffraction using CuKα radiation. The particle size, the chemical composition and the morphology of the calcinated powders were characterized by scanning electron microscopy. All sintered samples contain only one phase, which has a cubic structure with crystallite sizes of 12-21 nm. From the infrared spectra of all samples were observed two strong bands around 600 and 400 cm-1, which correspond to the intrinsic lattice vibrations of octahedral and tetrahedral sites of the spinel structure, respectively, and characteristic vibration for capping agent. The magnetic properties of fine powders were investigated at room temperature by using a vibrating sample magnetometer. The room temperature M-H hysteresis loops show ferromagnetic behavior of the calcined samples, with specific saturation magnetization (Ms) values ranging between 11 and 53 emu/g.

Mechanically activated synthesis of PZT and its electromechanical properties

NASA Astrophysics Data System (ADS)

Liu, X.; Akdogan, E. K.; Safari, A.; Riman, R. E.

2005-08-01

Mechanical activation was successfully used to synthesize nanostructured phase-pure Pb(Zr0.7Ti0.3)O3 (PZT) powders. Lead zirconium titanium (PbZrTi) hydrous oxide precursor, synthesized from chemical co-precipitation, was mechanically activated in a NaCl matrix. The synthesized PZT particles were characterized by using X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, laser-light diffraction, and nitrogen adsorption. Thermogravimetric analysis and differential thermal analysis were used to monitor dehydration and phase transformation of PbZrTi hydrous oxide precursor during mechanical activation. The best mechanical activation conditions corresponded to mechanically activating PbZrTi hydrous oxide precursor in a NaCl matrix with a NaCl/precursor weight ratio of 4:1 for 8 h. These conditions resulted in a dispersible phase-pure PZT powder with a median secondary-particle size of ˜110 nm. The properties of PZT 70/30 from mechanically activated powder, as measured on discs sintered at 1150 °C for 2 h, were found to be in close conformity to those obtained by a conventional mixed oxide solid state reaction route.

X-ray filter for x-ray powder diffraction

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

Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.

Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and wallsmore » defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.« less

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

PubMed

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

2014-07-15

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

Film calibration for soft x-ray wavelengths

NASA Astrophysics Data System (ADS)

Tallents, Gregory J.; Krishnan, J.; Dwivedi, L.; Neely, David; Turcu, I. C. Edmond

1997-10-01

The response of photographic film to X-rays from laser- plasma is of practical interest. Film is often used for the ultimate detection of x-rays in crystal and grating spectrometers and in imaging instruments such as pinhole cameras largely because of its high spatial resolution (approximately 1 - 10 microns). Characteristic curves for wavelengths--3 nm and 23 nm are presented for eight x-ray films (Kodak 101-01, 101-07, 104-02, Kodak Industrex CX, Russian UF-SH4, UF-VR2, Ilford Q plates and Shanghai 5F film). The calibrations were obtained from the emission of laser-produced carbon plasmas and a Ne-like Ge X-ray laser.

Pressure mapping for sphere and half-sphere enhanced diamond anvil cells using synchrotron x-ray diffraction and fluorescence techniques

NASA Astrophysics Data System (ADS)

Liu, H.; Liu, L. L.; Cai, Z.; Shu, J.

2015-12-01

The measurement for equation of state (EoS) of materials under pressure conditions above 200 GPa is a long-standing challenging subject. Recently, second stage anvil, which was loaded inside the diamond anvil cell (DAC), had been reported by various groups. This method could generate pressure over 300 GPa, or above 600 GPa from the EoS measurement of Re metal between the tiny anvil or 2 half-spheres. Several alternative approaches, using ruby balls, or glassy carbon, or diamond, with single sphere, 2 half-spheres, or multi spheres geometry inside DAC, were tested. The NIST X-ray powder standard, ZnO was selected as pressure marker. Focused ion beam (FIB) was used to cut the half-sphere from diamond anvil top directly to avoid the difficulty of alignment. The synchrotron x-ray diffraction with fine beam size down to 100 nm using zone plate set-up was used to map the pressure gradient at the sphere or half-sphere zone inside DAC. The pressure could be boosted at center of sphere by up to 10 - 70 GPa at about 200 GPa conditions. From broken anvils, trace element analysis using fine focusing synchrotron x-ray fluorescence method revealed the potential anvil damage from FIB cutting the diamond anvil tip, which might decrease the strength of anvils. Fine touch from FIB cutting at final stage using low ion beam current is suggested.

Assessment of surface roughness by use of soft x-ray scattering

NASA Astrophysics Data System (ADS)

Meng, Yan-li; Wang, Yong-gang; Chen, Shu-yan; Chen, Bo

2009-08-01

A soft x-ray reflectometer with laser produced plasma source has been designed, which can work from wavelength 8nm to 30 nm and has high performance. Using the soft x-ray reflectometer above, the scattering light distribution of silicon and zerodur mirrors which have super-smooth surfaces could be measured at different incidence angle and different wavelength. The measurement when the incidence angle is 2 degree and the wavelength is 11nm has been given in this paper. A surface scattering theory of soft x-ray grazing incidence optics based on linear system theory and an inverse scattering mathematical model is introduced. The vector scattering theory of soft x-ray scattering also is stated in detail. The scattering data are analyzed by both the methods above respectively to give information about the surface profiles. On the other hand, both the two samples are measured by WYKO surface profiler, and the surface roughness of the silicon and zerodur mirror is 1.3 nm and 1.5nm respectively. The calculated results are in quantitative agreement with those measured by WYKO surface profiler, which indicates that soft x-ray scattering is a very useful tool for the evaluation of highly polished surfaces. But there still some difference among the results of different theory and WYKO, and the possible reasons of such difference have been discussed in detail.

TL and PL studies on cubic fluoroperovskite single crystal (KMgF3: Eu2+, Ce3+)

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Madhusoodanan, U.; Annalakshmi, O.; Ramasamy, P.

2014-04-01

The perovskite-like KMgF3 polycrystalline compounds were synthesized by standard solid state reaction technique. Phase purity of the synthesized compounds was analyzed by powder X-ray diffraction technique. Single crystals of (0.2 mol% of EuF3 and CeF3) Co-doped KMgF3 have been grown from melt by using a vertical Bridgman-Stockbarger method. Thermoluminescence (TL) characteristics of KMgF3 samples doped with Eu2+ and Ce3+ have been studied after β-ray irradiation. At ambient conditions the photoluminescence spectra consisted of sharp line peaked of Eu2+ at 360 nm attributed to the f → f transition (6P7/2→8S7/2) could only be observed due to the energy transfer from Ce3+ to Eu2+.

Ultra-small plutonium oxide nanocrystals: an innovative material in plutonium science.

PubMed

Hudry, Damien; Apostolidis, Christos; Walter, Olaf; Janssen, Arne; Manara, Dario; Griveau, Jean-Christophe; Colineau, Eric; Vitova, Tonya; Prüssmann, Tim; Wang, Di; Kübel, Christian; Meyer, Daniel

2014-08-11

Apart from its technological importance, plutonium (Pu) is also one of the most intriguing elements because of its non-conventional physical properties and fascinating chemistry. Those fundamental aspects are particularly interesting when dealing with the challenging study of plutonium-based nanomaterials. Here we show that ultra-small (3.2±0.9 nm) and highly crystalline plutonium oxide (PuO2 ) nanocrystals (NCs) can be synthesized by the thermal decomposition of plutonyl nitrate ([PuO2 (NO3 )2 ]⋅3 H2 O) in a highly coordinating organic medium. This is the first example reporting on the preparation of significant quantities (several tens of milligrams) of PuO2 NCs, in a controllable and reproducible manner. The structure and magnetic properties of PuO2 NCs have been characterized by a wide variety of techniques (powder X-ray diffraction (PXRD), X-ray absorption fine structure (XAFS), X-ray absorption near edge structure (XANES), TEM, IR, Raman, UV/Vis spectroscopies, and superconducting quantum interference device (SQUID) magnetometry). The current PuO2 NCs constitute an innovative material for the study of challenging problems as diverse as the transport behavior of plutonium in the environment or size and shape effects on the physics of transuranium elements. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel synthesis of ZnO/PMMA nanocomposites for photocatalytic applications

PubMed Central

Di Mauro, Alessandro; Cantarella, Maria; Nicotra, Giuseppe; Pellegrino, Giovanna; Gulino, Antonino; Brundo, Maria Violetta; Privitera, Vittorio; Impellizzeri, Giuliana

2017-01-01

The incorporation of nanostructured photocatalysts in polymers is a strategic way to obtain novel water purification systems. This approach takes the advantages of: (1) the presence of nanostructured photocatalyst; (2) the flexibility of polymer; (3) the immobilization of photocatalyst, that avoids the recovery of the nanoparticles after the water treatment. Here we present ZnO-polymer nanocomposites with high photocatalytic performance and stability. Poly (methyl methacrylate) (PMMA) powders were coated with a thin layer of ZnO (80 nm thick) by atomic layer deposition at low temperature (80 °C). Then the method of sonication and solution casting was performed so to obtain the ZnO/PMMA nanocomposites. A complete morphological, structural, and chemical characterization was made by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) analyses. The remarkable photocatalytic efficiency of the nanocomposites was demonstrated by the degradation of methylene blue (MB) dye and phenol in aqueous solution under UV light irradiation. The composites also resulted reusable and stable, since they maintained an unmodified photo-activity after several MB discoloration runs. Thus, these results demonstrate that the proposed ZnO/PMMA nanocomposite is a promising candidate for photocatalytic applications and, in particular, for novel water treatment. PMID:28098229

One-pot hydrothermal synthesis of an assembly of magnetite nanoneedles on a scaffold of cyclic-diphenylalanine nanorods

NASA Astrophysics Data System (ADS)

Togashi, Takanari; Umetsu, Mitsuo; Naka, Takashi; Ohara, Satoshi; Hatakeyama, Yoshiharu; Adschiri, Tadafumi

2011-09-01

The assembly of metal oxide nanoparticles (NPs) on a biomolecular template by a one-pot hydrothermal synthesis method is achieved for the first time. Magnetite (Fe3O4) nanoneedles (length: 100 nm; width: 10 nm) were assembled on cyclic-diphenylalanine (cFF) nanorods (length: 2-10 μm; width: 200 nm). The Fe3O4 nanoneedles and cFF nanorods were simultaneously synthesized from FeSO4 and l-phenylalanine by hydrothermal synthesis (220 °C and 22 MPa), respectively. The samples were analyzed by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (IR), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. Experimental results indicate that Fe3O4 nanoneedles were assembled on cFF nanorods during the hydrothermal reaction. The composite contained 3.3 wt% Fe3O4 nanoneedles without any loss of the original magnetic properties of Fe3O4.

Synthesis and characterization of high quantum yield and oscillator strength 6-chloro-2-(4-cynophenyl)-4-phenyl quinoline (cl-CN-DPQ) organic phosphor for solid-state lighting.

PubMed

Ghate, Minakshi; Dahule, H K; Thejo Kalyani, N; Dhoble, S J

2018-03-01

A novel blue luminescent 6-chloro-2-(4-cynophenyl) substituted diphenyl quinoline (Cl-CN DPQ) organic phosphor has been synthesized by the acid-catalyzed Friedlander reaction and then characterized to confirm structural, optical and thermal properties. Structural properties of Cl-CN-DPQ were analyzed by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) spectroscopy, X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) and energy dispersive analysis of X-ray (EDAX) spectroscopy. FTIR spectra confirmed the presence of different functional groups and bond stretching. 1 H-NMR and 13 C-NMR confirmed the formation of an organic Cl-CN-DPQ compound. X-ray diffraction study provided its crystalline nature. The surface morphology of Cl-CN-DPQ was analyzed by SEM, while EDAX spectroscopy revealed the elemental analysis. Differential thermal analysis (TGA/DTA) disclosed its thermal stability up to 250°C. The optical properties of Cl-CN-DPQ were investigated by UV-vis absorption and photoluminescence (PL) measurements. Cl-CN-DPQ exhibits intense blue emission at 434 nm in a solid-state crystalline powder with CIE co-ordinates (0.157, 0.027), when excited at 373 nm. Cl-CN-DPQ shows remarkable Stokes shift in the range 14800-5100 cm -1 , which is the characteristic feature of intense light emission. A narrow full width at half-maximum (FWHM) value of PL spectra in the range 42-48 nm was observed. Oscillator strength, energy band gap, quantum yield, and fluorescence energy yield were also examined using UV-vis absorption and photoluminescence spectra. These results prove its applications towards developing organic luminescence devices and displays, organic phosphor-based solar cells and displays, organic lasers, chemical sensors and many more. Copyright © 2017 John Wiley & Sons, Ltd.

Synthesis and characterization of metastable, 20 nm-sized Pna2{sub 1}-LiCoPO{sub 4} nanospheres

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

Ludwig, Jennifer; Nordlund, Dennis; Doeff, Marca M.

The majority of research activities on LiCoPO{sub 4} are focused on the phospho-olivine (space group Pnma), which is a promising high-voltage cathode material for Li-ion batteries. In contrast, comparably little is known about its metastable Pna2{sub 1} modification. Herein, we present a comprehensive study on the structure–property relationships of 15–20 nm Pna2{sub 1}-LiCoPO{sub 4} nanospheres prepared by a simple microwave-assisted solvothermal process. Unlike previous reports, the results indicate that the compound is non-stoichiometric and shows cation-mixing with Co ions on the Li sites, which provides an explanation for the poor electrochemical performance. Co L{sub 2,3}-edge X-ray absorption spectroscopic data confirmmore » the local tetrahedral symmetry of Co{sup 2+}. Comprehensive studies on the thermal stability using thermogravimetric analysis, differential scanning calorimetry, and in situ powder X-ray diffraction show an exothermic phase transition to olivine Pnma-LiCoPO{sub 4} at 527 °C. The influence of the atmosphere and the particle size on the thermal stability is also investigated. - Graphical abstract: Blue nano-sized Pna2{sub 1}-LiCoPO{sub 4,} featuring tetrahedrally-coordinated Co{sup 2+}, was synthesized in a rapid one-step microwave-assisted solvothermal process. The phase relation between this metastable and the stable polymorph was analyzed and electrochemical properties are discussed. - Highlights: • Preparation of uniform 15–20 nm nanospheres of metastable Pna2{sub 1}-LiCoPO{sub 4} polymorph. • Structure redetermination shows cation-mixing (Co blocking Li sites). • In situ investigation of phase transformation to olivine Pnma-LiCoPO{sub 4} at 527 °C. • Pna2{sub 1}-LiCoPO{sub 4} reemerges as a stable high-temperature phase above 800 °C. • X-ray absorption spectroscopy confirms local tetrahedral symmetry (T{sub d} Co{sup 2+}).« less

Nano-scale composition of commercial white powders for development of latent fingerprints on adhesives.

PubMed

Jones, B J; Reynolds, A J; Richardson, M; Sears, V G

2010-09-01

Titanium dioxide based powders are regularly used in the development of latent fingerprints on dark surfaces. For analysis of prints on adhesive tapes, the titanium dioxide can be suspended in a surfactant and used in the form of a powder suspension. Commercially available products, whilst having nominally similar composition, show varying levels of effectiveness of print development, with some powders adhering to the background as well as the print. X-ray fluorescence (XRF), analytical transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and laser particle sizing of the fingerprint powders show TiO(2) particles with a surrounding coating, tens of nanometres thick, consisting of Al and Si rich material, with traces of sodium and sulphur. Such aluminosilicates are commonly used as anti-caking agents and to aid adhesion or functionality of some fingerprint powders; however, the morphology, thickness, coverage and composition of the aluminosilicates are the primary differences between the white powder formulations and could be related to variation in the efficacy of print development. Copyright © 2009 Forensic Science Society. All rights reserved.

Nm-scale spatial resolution x-ray imaging with MLL nanofocusing optics: instrumentational requirements and challenges

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

Nazaretski, E.; Yan, H.; Lauer, K.

2016-08-30

The Hard X-ray Nanoprobe (HXN) beamline at NSLS-II has been designed and constructed to enable imaging experiments with unprecedented spatial resolution and detection sensitivity. The HXN X-ray Microscope is a key instrument for the beamline, providing a suite of experimental capabilities which includes scanning fluorescence, diffraction, differential phase contrast and ptychography utilizing Multilayer Laue Lenses (MLL) and zoneplate (ZP) as nanofocusing optics. In this paper, we present technical requirements for the MLL-based scanning microscope, outline the development concept and present first ~15 x 15 nm 2 spatial resolution x-ray fluorescence images.

Effects of limestone petrography and calcite microstructure on OPC clinker raw meals burnability

NASA Astrophysics Data System (ADS)

Galimberti, Matteo; Marinoni, Nicoletta; Della Porta, Giovanna; Marchi, Maurizio; Dapiaggi, Monica

2017-10-01

Limestone represents the main raw material for ordinary Portland cement clinker production. In this study eight natural limestones from different geological environments were chosen to prepare raw meals for clinker manufacturing, aiming to define a parameter controlling the burnability. First, limestones were characterized by X-Ray Fluorescence, X-Ray Powder Diffraction and Optical Microscopy to assess their suitability for clinker production and their petrographic features. The average domains size and the microstrain of calcite were also determined by X-Ray Powder Diffraction line profile analysis. Then, each limestone was admixed with clay minerals to achieve the adequate chemical composition for clinker production. Raw meals were thermally threated at seven different temperatures, from 1000 to 1450 °C, to evaluate their behaviour on heating by ex situ X-Ray Powder Diffraction and to observe the final clinker morphology by Scanning Electron Microscopy. Results indicate the calcite microstrain is a reliable parameter to predict the burnability of the raw meals, in terms of calcium silicates growth and lime consumption. In particular, mixtures prepared starting from high-strained calcite exhibit a better burnability. Later, when the melt appears this correlation vanishes; however differences in the early burnability still reflect on the final clinker composition and texture.

M(II)-dipyridylamide-based coordination frameworks (M=Mn, Co, Ni): Structural transformation

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

Tzeng, Biing-Chiau; Selvam, TamilSelvi; Tsai, Miao-Hsin

2016-11-15

A series of 1-D double-zigzag (([M(papx){sub 2}(H{sub 2}O){sub 2}](ClO{sub 4}){sub 2}){sub n}; M=Mn, x=s (1), x=o (3); M=Co, x=s (4), x=o (5); M=Ni, x=s (6), x=o (7)) and 2-D polyrotaxane ([Mn(paps){sub 2}(ClO{sub 4}){sub 2}]{sub n} (2)) frameworks were synthesized by reactions of M(ClO{sub 4}){sub 2} (M=Mn, Co, and Ni) with papx (paps, N,N’-bis(pyridylcarbonyl)-4,4’-diaminodiphenylthioether; papo, N,N’-bis(pyridylcarbonyl)-4,4’-diaminodiphenyl ether), which have been isolated and structurally characterized by X-ray diffraction. Based on powder X-ray diffraction (PXRD) experiments, heating the double-zigzag frameworks underwent structural transformation to give the respective polyrotaxane ones. Moreover, grinding the solid samples of the respective polyrotaxanes in the presence of moisturemore » also resulted in the total conversion to the original double-zigzag frameworks. In this study, we have successfully extended studies to Mn{sup II}, Co{sup II}, and Ni{sup II} frameworks from the previous Zn{sup II}, Cd{sup II}, and Cu{sup II} ones, and interestingly such structural transformation is able to be proven experimentally by powder and single-crystal X-ray diffraction studies as well. - Graphical abstract: 1-D double-zigzag and 2-D polyrotaxane frameworks of M(II)-papx (x=s, o; M=Mn, Co, Ni) frameworks can be interconverted by heating and grinding in the presence of moiture, and such structural transformation has be proven experimentally by powder and single-crystal X-ray diffraction studies.« less

Powerful Solar Flares in September 2017. Comparison with the Largest Flares in Cycle 24

NASA Astrophysics Data System (ADS)

Bruevich, E. A.; Bruevich, V. V.

2018-06-01

Solar flare activity in cycle 24 is studied. Satellite observations of x-ray fluxes from GOES-15 and UV emission lines from the SDO/EVE experiment are used. The most powerful flares of cycle 24 in classes X9.3 and X8.2 in September 2017 are compared with powerful flares in classes M5-X6.9. The times at which the fluxes in the 30.4 and 9.4 nm lines and in the 0.1-0.8 nm x-ray range begin to increase are compared for 21 of the large flares. The total energies arriving at the earth from flares in the 30.4 and 9.4 nm lines and in the 0.1-0.9 nm x-ray range, E30.4, E9.4, and E0.1-0.8, from 25 flares during 2011 and 2012 are calculated. It is shown that the calculated energies of the flares in the analyzed lines from SDO/EVE and in the x-ray range from GOES-15 are closely interrelated.

Microwave combustion synthesis of Co1-xZnxFe2O4 (0⩽x⩽0.5): Structural, magnetic, optical and vibrational spectroscopic studies.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith; Aruldoss, Udaya

2015-04-05

Nanostructured pure and zinc doped cobalt ferrites (Co1-xZnxFe2O4 where x fraction ranging from 0 to 0.5) were prepared by microwave combustion method employing urea as a fuel. The nanostructured samples were characterized by using various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy, energy dispersive X-ray analysis, UV-visible diffuse reflectance spectroscopy, photoluminescence spectroscopy and Fourier transformed infrared (FT-IR) spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis and the FT-IR spectroscopy revealed the formation of cobalt ferrite cubic spinel-type structure. The average crystallite sizes for the samples were in the range of 3.07-11.30 nm. The direct band gap (Eg) was estimated using Kubelka-Munk method and is obtained from the UV-vis spectra. The band gap value decreased with an increase in zinc fraction (2.56-2.17 eV). The violet and green emission observed in the photoluminescence spectra revealed that cobalt ferrites are governed by defect controlled processes. The elemental analysis of zinc doped cobalt ferrites were obtained from energy dispersive X-ray (EDX) analysis. From the magnetic measurements, it is observed that cobalt ferrite and zinc doped cobalt ferrite systems fall under the soft ferrite category. The saturation magnetization (Ms) value of undoped cobalt ferrite is 14.26 emu/g, and it has reached a maximum of 29.61 emu/g for Co0.7Zn0.3Fe2O4. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and Characterization of Single-Source Molecular Precursors to Binary Metal Sulphides: Bis(Diethyldithiocarbamato) M(II)Trialkylphosphine (M=Zn and Cd) Adducts

DTIC Science & Technology

1994-05-06

while the heterobimetallic species, 7, thermally decomposed to give00 crystalline ZnO.5S according to X-ray powder diffraction data. A. SUBJECT TERMS 15... heterobimetallic species, 7, thermally decomposed to give crystalline ZnO.5CdO.5S according to X-ray powder diffraction data. LaGOSSIOn "or OTIS RA&I VT-iC TAB EU...on the NMR timescale, and a single heterobimetallic species. Attempts to distinguish these possibilities are described later. The variable temperature

Synthesis and characterization of Mn-Bi alloy

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Patil, Harsha; Jain, G.; Mishra, N.

2012-06-01

High purity MnBi low temperature phase has been prepared and analyzed using X-ray diffraction, Lorentz-Polarization Factor and Fourier transforms infrared measurement. After synthesis of samples structural characterization has done on samples by X-ray diffraction, which shows that after making the bulk sample is in no single phase MnBi has been prepared by sintering Mn and Bi powders. By Lorentz-Polarization Factor is affecting the relative intensity of diffraction lines on a powder form. And by FTIR which shows absorption peaks of MnBi alloys.

X-ray diffraction study of the caged magnetic compound DyFe 2 Zn 20 at low temperatures

NASA Astrophysics Data System (ADS)

Ohashi, M.; Ohashi, K.; Sawabu, M.; Miyagawa, M.; Maeta, K.; Isikawa, Y.

2018-05-01

We have carried out high-angle X-ray powder diffraction measurements of the caged magnetic compound DyFe2Zn20 at low temperature between 14 and 300 K. Even though a strong magnetic anisotropy exists in the magnetization and magnetic susceptibility due to strong exchange interaction between Fe and Dy, almost all X-ray powder diffraction peaks correspond to Bragg reflections of the cubic structural models not only at room temperature paramagnetic state but also at low temperature magnetic ordering state. The Debye temperature is obtained to be 227 K from the results of the volumetric thermal expansion coefficient, which is approximately coincident with that of CeRu2Zn20 (245 K) and that of pure Zn metal (235 K).

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

DOE PAGES

Nazaretski, E.; Yan, H.; Lauer, K.; ...

2017-10-05

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

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

Nazaretski, E.; Yan, H.; Lauer, K.

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Development of a spectro-electrochemical cell for soft X-ray photon-in photon-out spectroscopy

NASA Astrophysics Data System (ADS)

Ishihara, Tomoko; Tokushima, Takashi; Horikawa, Yuka; Kato, Masaru; Yagi, Ichizo

2017-10-01

We developed a spectro-electrochemical cell for X-ray absorption and X-ray emission spectroscopy, which are element-specific methods to study local electronic structures in the soft X-ray region. In the usual electrochemical measurement setup, the electrode is placed in solution, and the surface/interface region of the electrode is not normally accessible by soft X-rays that have low penetration depth in liquids. To realize soft X-ray observation of electrochemical reactions, a 15-nm-thick Pt layer was deposited on a 150-nm-thick film window with an adhesive 3-nm-thick Ti layer for use as both the working electrode and the separator window between vacuum and a sample liquid under atmospheric pressure. The designed three-electrode electrochemical cell consists of a Pt film on a SiC window, a platinized Pt wire, and a commercial Ag|AgCl electrode as the working, counter, and reference electrodes, respectively. The functionality of the cell was tested by cyclic voltammetry and X-ray absorption and emission spectroscopy. As a demonstration, the electroplating of Pb on the Pt/SiC membrane window was measured by X-ray absorption and real-time monitoring of fluorescence intensity at the O 1s excitation.

Near-infrared photoluminescence in La{sub 0.98}AlO{sub 3}: {sub 0.02}Ln{sup 3+}(Ln = Nd/Yb) for sensitization of c-Si solar cells

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

Sawala, N. S., E-mail: nssawala@gmail.com; Koparkar, K. A.; Omanwar, S. K.

2016-05-06

The host matrix LaAlO{sub 3} was synthesized by conventional solid state reaction method in which the Nd{sup 3+} ions and Yb{sup 3+} ions successfully doped at 2mol% concentrations. The phase purity was confirmed by X ray powder diffraction (XRD) method. The photoluminescence (PL) properties were studied by spectrophotometer in near infra red (NIR) and ultra violet visible (UV-VIS) region. The Nd{sup 3+} ion doped LaAlO{sub 3} converts a visible (VIS) green photon (587 nm) into near infrared (NIR) photon (1070 nm) while Yb{sup 3+} ion doped converts ultra violet (UV) photon (221 nm) into NIR photon (980 nm). The La{sub 0.98}AlO{sub 3}: {sub 0.02}Ln{supmore » 3+}(Ln = Nd / Yb) can be potentiality used for betterment of photovoltaic (PV) technology. This result further indicates its potential application as a luminescence converter layer for enhancing solar cells performance.« less

Study of energy transfer and spectral downshifting in Ce, RE (RE = Nd and Yb) co-doped lanthanum phosphate

NASA Astrophysics Data System (ADS)

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

2017-03-01

The phosphors LaPO4 (Lanthanum phosphate) doped with Ce(III)/Ce3+ and co-doped with Ce3+-Nd3+ and Ce3+-Yb3+ were effectively synthesized by conventional solid state reaction method. The prepared samples were characterized by powder X-ray diffraction (XRD) and surface morphology was studied by scanning electronic microscope (SEM). The photoluminescence (PL) properties were studied by spectrophotometers in near infrared (NIR) and ultraviolet visible (UV-VIS) region. Additionally the luminescence time decay curves of samples were investigated to confirm energy transfer (ET) process. The Ce3+-Nd3+ ion co-doped LaPO4 phosphors can convert a photon of UV region (278 nm) into photons of NIR region (1058 nm). While Ce3+-Yb3+ ion doped LaPO4 phosphors convert photons of UV region (278 nm) into photons of NIR region (979 nm). The Ce3+ ion acts like sensitizer and Nd3+/Yb3+ ions act as activators. Both kinds of emissions are suitable for improving spectral response of solar cells.

X-ray microfocusing with off-axis ellipsoidal mirror

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

Yumoto, Hirokatsu, E-mail: yumoto@spring8.or.jp; Koyama, Takahisa; Matsuyama, Satoshi

2016-07-27

High-precision ellipsoidal mirrors for two-dimensionally focusing X-rays to nanometer sizes have not been realized because of technical problems in their fabrication processes. The objective of the present study is to develop fabrication techniques for ellipsoidal focusing mirrors in the hard-X-ray region. We design an off-axis ellipsoidal mirror for use under total reflection conditions up to the X-ray energy of 8 keV. We fabricate an ellipsoidal mirror with a surface roughness of 0.3 nm RMS (root-mean-square) and a surface figure error height of 3.0 nm RMS by utilizing a surface profiler and surface finishing method developed by us. The focusing propertiesmore » of the mirror are evaluated at the BL29XUL beamline in SPring-8. A focusing beam size of 270 nm × 360 nm FWHM (full width at half maximum) at an X-ray energy of 7 keV is observed with the use of the knife-edge scanning method. We expect to apply the developed fabrication techniques to construct ellipsoidal nanofocusing mirrors.« less

Structure dependent electrical properties of Ni-Mg-Cu nano ferrites

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

Choudhari, Nagabhushan J., E-mail: nagabhushanchoudhari@gmail.com; Kakati, Sushanth S.; Hiremath, Chidanandayya S.

2016-05-06

Nano ferrites with the general chemical formula Ni{sub 0.5}Mg{sub x}Cu{sub 1-x} Fe{sub 2}O{sub 4} were synthesized by chemical route. They were characterized by x-ray diffraction by powder method. The diffraction patterns confirm the formation of single phase ferrites. The particle size is calculated by Scherrer formula which varies between 20nm to 60nm. DC resistivity was measured as a function of composition from room temperature to 700{sup o} C by two probe method. These ferrites show higher resistivity than those synthesized by ceramic method, due to control over composition and morphology. This leads to the elimination of domain wall resonance somore » that the materials can work at higher frequencies. AC resistivity was measured as a function of frequency at room temperature. Dielectric dispersion obeys Maxwell - Wagner model, in accordance with Koop’s phenomenological theory. The variation of loss angle follows the variation of ac resistivity with frequency and composition. The change in ac conductivity with frequency obeys the power law σ{sub a} = B.ω{sup n}. Such a behavior suggests that conductivity is due to polarons in all the samples.« less

Long term stable deep red light-emitting electrochemical cells based on an emissive, rigid cationic Ir(iii) complex

DOE PAGES

Namanga, Jude E.; Ruhr-Univ. Bochum, Bochum; Gerlitzki, Niels; ...

2017-02-17

Here, the new cationic iridium complex [Ir(bzq) 2(biq)][PF 6] (bzq = benzo[ h]quinolinato and biq = 2,2'-biquinoline) has been synthesized for application as an emitter in light emitting electrochemical cells (LECs). The molecular structure and crystal packing of this complex were established by single X-ray diffraction (SXRD). The electrochemical and photophysical properties of the complex were examined to determine the frontier orbital energies as well as the optical transitions that led to photoemission. The complex was found to emit at 644 nm and 662 nm for powder and thin films, respectively. A high powder photoluminescence quantum yield of 25% wasmore » determined, which is attributed to a reduction in vibrational modes of the complex due to the use of the rigid cyclometalated (C^N) bzq ligand. A LEC with [Ir(bzq) 2(biq)][PF 6] as the emitter was fabricated which showed a deep red emission (662 nm) with a luminance of 33.65 cd m –2, yielding a current efficiency of 0.33 cd A –1 and a power efficiency of 0.2 lm W –1. Most importantly, the LEC based on [Ir(bzq) 2(biq)][PF 6] demonstrated a lifetime of 280 hours which is among the longest device lifetimes reported for any deep red light emitting LEC.« less

Long term stable deep red light-emitting electrochemical cells based on an emissive, rigid cationic Ir(iii) complex

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

Namanga, Jude E.; Ruhr-Univ. Bochum, Bochum; Gerlitzki, Niels

Here, the new cationic iridium complex [Ir(bzq) 2(biq)][PF 6] (bzq = benzo[ h]quinolinato and biq = 2,2'-biquinoline) has been synthesized for application as an emitter in light emitting electrochemical cells (LECs). The molecular structure and crystal packing of this complex were established by single X-ray diffraction (SXRD). The electrochemical and photophysical properties of the complex were examined to determine the frontier orbital energies as well as the optical transitions that led to photoemission. The complex was found to emit at 644 nm and 662 nm for powder and thin films, respectively. A high powder photoluminescence quantum yield of 25% wasmore » determined, which is attributed to a reduction in vibrational modes of the complex due to the use of the rigid cyclometalated (C^N) bzq ligand. A LEC with [Ir(bzq) 2(biq)][PF 6] as the emitter was fabricated which showed a deep red emission (662 nm) with a luminance of 33.65 cd m –2, yielding a current efficiency of 0.33 cd A –1 and a power efficiency of 0.2 lm W –1. Most importantly, the LEC based on [Ir(bzq) 2(biq)][PF 6] demonstrated a lifetime of 280 hours which is among the longest device lifetimes reported for any deep red light emitting LEC.« less

Growth and characterization of a new nonlinear optical organic crystal: 2,4,6-Trimethylacetanilide

NASA Astrophysics Data System (ADS)

Upadhyaya, V.; Prabhu, Sharada G.

2015-09-01

A new nonlinear optical organic material, 2,4,6-trimethylacetanilide (246TMAA), also known as N-[2,4,6- trimethylphenyl]acetamide, has been synthesized and grown as a single crystal by the slow evaporation technique by organic solvents. The grown crystals have been characterized by morphology study. The crystals are prismatic. Surface examination shows granular dendritic pattern in optical micrograph. The Scanning Electron Micrograph shows the layered growth of the crystal. The Differential Scanning Calorimeter plot shows no phase change until melting point (219°C). The density of the crystals is 1.1g/cc and the crystals are soft. The crystals are transparent in the visible region and in the ultra-violet region till 280 nm. 246TMAA crystallizes with 2 molecules in a monoclinic unit cell in the noncentrosymmetric point group m, space group Pn. Refractive indices of this optically biaxial crystal along the three crystallophysical axes have been measured at 633 nm. The optical second harmonic generation efficiency of the crystal at 1064 nm is about half that of the urea crystal, measured by powder method using Nd:YAG laser. The results show that the 246TMAA crystal can efficiently be used for up-conversion of infrared radiation into visible green light. The powder X-ray diffraction spectrum of the crystal has been obtained.

Development of megestrol acetate solid dispersion nanoparticles for enhanced oral delivery by using a supercritical antisolvent process.

PubMed

Ha, Eun-Sol; Kim, Jeong-Soo; Baek, In-Hwan; Yoo, Jin-Wook; Jung, Yunjin; Moon, Hyung Ryong; Kim, Min-Soo

2015-01-01

In the present study, solid dispersion nanoparticles with a hydrophilic polymer and surfactant were developed using the supercritical antisolvent (SAS) process to improve the dissolution and oral absorption of megestrol acetate. The physicochemical properties of the megestrol acetate solid dispersion nanoparticles were characterized using scanning electron microscopy, differential scanning calorimetry, powder X-ray diffraction, and a particle-size analyzer. The dissolution and oral bioavailability of the nanoparticles were also evaluated in rats. The mean particle size of all solid dispersion nanoparticles that were prepared was <500 nm. Powder X-ray diffraction and differential scanning calorimetry measurements showed that megestrol acetate was present in an amorphous or molecular dispersion state within the solid dispersion nanoparticles. Hydroxypropylmethyl cellulose (HPMC) solid dispersion nanoparticles significantly increased the maximum dissolution when compared with polyvinylpyrrolidone K30 solid dispersion nanoparticles. The extent and rate of dissolution of megestrol acetate increased after the addition of a surfactant into the HPMC solid dispersion nanoparticles. The most effective surfactant was Ryoto sugar ester L1695, followed by D-α-tocopheryl polyethylene glycol 1000 succinate. In this study, the solid dispersion nanoparticles with a drug:HPMC:Ryoto sugar ester L1695 ratio of 1:2:1 showed >95% rapid dissolution within 30 minutes, in addition to good oral bioavailability, with approximately 4.0- and 5.5-fold higher area under the curve (0-24 hours) and maximum concentration, respectively, than raw megestrol acetate powder. These results suggest that the preparation of megestrol acetate solid dispersion nanoparticles using the supercritical antisolvent process is a promising approach to improve the dissolution and absorption properties of megestrol acetate.

Structural characterization and optical constants of CuIn3Se5 vacuum and air annealed thin films

NASA Astrophysics Data System (ADS)

Segmane, N. E. H.; Abdelkader, D.; Amara, A.; Drici, A.; Akkari, F. Chaffar; Khemiri, N.; Bououdina, M.; Kanzari, M.; Bernède, J. C.

2018-01-01

Milled powder of ordered defect compound (ODC) CuIn3Se5 phase was successfully synthesized via milling process. Thin films of CuIn3Se5 were deposited onto glass substrates at room temperature by thermal evaporation technique. The obtained layers were annealed in vacuum and air atmosphere. The structural and compositional properties of the powder were analyzed using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Powder XRD characterization, Rietveld analysis and chemical bounding confirm the tetragonal ordered defect compound phase formation with lattice constants a = 5.732 Å and c = 11.575 Å. Thin films were characterized by XRD, atomic force microscopy (AFM) and UV/Vis spectroscopy. Transmittance (T) and reflectance (R) spectra were measured in the spectral range of 300-1800 nm. The absorption coefficient α exhibits high values in the visible range and reaches a value of 105 cm-1. The band gap energy Eg of the annealed thin films is estimated to be approximately 1.75 eV. The refractive index n was estimated from transmittance data using Swanepoel's method. The refractive indices of the films as a function of wavelengths can be fitted with Cauchy dispersion equation. The oscillator energy E0, dispersion energy Ed, zero frequency refractive index n0, high frequency dielectric constant ε∞ and the carrier concentration per effective mass N/m∗ values were determined from the analysis of the experimental data using Wemple-DiDomenico and Spitzer-Fan models. We exploited the refractive index dispersion for the determination of the magneto-optical constant V, which characterizes the Faraday rotation. The nonlinear optical parameters namely nonlinear susceptibility χ(3), nonlinear refractive index and nonlinear absorption coefficient β are investigated for the first time for CuIn3Se5 material.

Synthesis and Characterization of Cu- and Co-Doped Bi4V2O11 for Intermediate-Temperature Solid Oxide Fuel Cell Electrolytes by Carbonate Coprecipitation

NASA Astrophysics Data System (ADS)

Lee, Jin Goo; Yoon, Hyon Hee

2011-01-01

Bi2MexV1-xO5.5-3x/2 (Me = Cu; 0≤x≤0.2) powders were prepared by the ammonium carbonate coprecipitation method. The starting salts were bismuth nitrate, copper nitrate, cobalt nitrate, and vanadium sulphate. The thermal decomposition of Bi2MexV1-xO5.5-3x/2 precursors was completed at about 500 °C. The crystallite structure, surface morphology, and ionic conductivity of the prepared powders and pellets were examined using X-ray diffractometry, field emission scanning electron microscopy, and an impedance analyzer, respectively. The average particle sizes of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 powders were 10-50 nm. The tetragonal structure (γ-phase) appeared at sintering temperatures higher than 700 °C and the peak intensity increased at higher sintering temperatures. The ionic conductivities of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 pellets sintered at 800 °C showed the highest values of 6.8×10-2 S cm-1 at 700 °C and 9.1×10-2 S cm-1 at 700 °C, respectively. The optimum concentration of the Cu and Co dopants in Bi2MexV1-xO5.5-3x/2 was determined to be 0.1. The results of this study demonstrated that the ammonium carbonate coprecipitation process could be used as an economical method for the preparation of Bi2MexV1-xO5.5-3x/2 electrolytes for intermediate-temperature solid oxide fuel cells.

Development of x-ray laminography under an x-ray microscopic condition

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

Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa

2011-07-15

An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatialmore » resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.« less

Transmission-geometry electrochemical cell for in-situ scattering and spectroscopy investigations

DOEpatents

Chupas, Peter J.; Chapman, Karena W.; Kurtz, Charles A.; Borkiewicz, Olaf J.; Wiaderek, Kamila Magdelena; Shyam, Badri

2015-05-05

The present invention relates to a test chamber that can be used to perform a variety of X-ray and neutron spectroscopy experiments including powder diffraction, small-angle scattering, X-ray absorption spectroscopy, and pair distribution functions, such chamber comprising a first electrode with an X-ray transparent window; a second electrode with an X-ray transparent window; a plurality of insulating gaskets providing a hermetic seal around the sample and preventing contact between said first and second electrodes; and an insulating housing into which the first electrode is secured.

Roller compaction of different pseudopolymorphic forms of theophylline: Effect on compressibility and tablet properties.

PubMed

Hadzović, Ervina; Betz, Gabriele; Hadzidedić, Seherzada; El-Arini, Silvia Kocova; Leuenberger, Hans

2010-08-30

The effect of roller compaction on disintegration time, dissolution rate and compressibility of tablets prepared from theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate was studied. In addition, the influence of adding microcrystalline cellulose, a commonly used excipient, in mixtures with these materials was investigated. Theophylline anhydrate powder was used as a model drug to investigate the influence of different compaction pressures on the tablet properties. Tablets with same porosity were prepared by direct compaction and by roller compaction/re-compaction. Compressibility was characterized by Heckel and modified Heckel equations. Due to the property of polymorphic materials to change their form during milling and compression, X-ray diffraction analysis of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate powders and granules was carried out. After roller compaction the disintegration time and the dissolution rate of the tablets were significantly improved. Compressibility of theophylline anhydrate powder and theophylline anhydrate fine powder was decreased, while theophylline monohydrate showed higher compressibility after roller compaction. Microcrystalline cellulose affected compressibility of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate whereby the binary mixtures showed higher compressibility than the individual materials. X-ray diffraction analyses confirmed that there were no polymorphic/pseudopolymorphic changes after roller compaction. Copyright 2010 Elsevier B.V. All rights reserved.

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

Lecointre, A., E-mail: lecointre.aurelie@gmail.com; Bessière, A., E-mail: aurelie-bessiere@chimie-paristech.fr; Department of Physics, Goa University, Taleigao Plateau, Goa 403 206

Highlights: ► Long-lasting phosphorescence of CaMgSi{sub 2}O{sub 6}:Mn is studied for bioimaging application. ► CaMgSi{sub 2}O{sub 6}:Mn yields orange and red luminescence of Mn{sup II}{sub Ca} and Mn{sup II}{sub Mg}, respectively. ► Red Mn{sup II}{sub Mg} emission dominates long-lasting phosphorescence spectra. ► Mn mainly substitutes Mg. ► Mn{sup II}{sub Mg} plays the role of hole trap in the persistent luminescence mechanism. - Abstract: Materials with red long-lasting phosphorescence, such as Mn{sup II}-doped diopsides, can be used for small animal in vivo imaging. CaMgSi{sub 2}O{sub 6}:Mn powders with various amounts of Mn were prepared by sol–gel to investigate their long-lasting phosphorescencemore » mechanism. X-ray diffraction, X-ray absorption fine and near-edge structure and electron paramagnetic resonance showed that manganese is quantitatively introduced in the structure as Mn{sup II}. Most of the Mn doping ions substitute Mg and possess a highly elongated octahedral environment. While photoluminescence and X-ray excited optical luminescence spectra show both orange (585 nm) and red (685 nm) {sup 4}T{sub 1} ({sup 4}G) → {sup 6}A{sub 1} ({sup 6}S) emission of Mn{sup II}{sub Ca} and Mn{sup II}{sub Mg}, respectively, Mn{sup II}{sub Mg} red emission dominates long-lasting phosphorescence and thermally stimulated luminescence spectra. These results point to Mn{sup II}{sub Mg} as the preferential hole trap and recombination center in the long-lasting phosphorescence mechanism. An intense persistent red emission suitable for in vivo imaging probes is obtained for the highest nominal Mn content (7.5%)« less

Optical properties of ZnO powder prepared by using a proteic sol-gel process

NASA Astrophysics Data System (ADS)

Kwon, Bong-Joon; Woo, Hyun-Joo; Park, Ji-Yeon; Jang, Kiwan; Lim, Seung-Hyuk; Cho, Yong-Hoon

2013-03-01

We have studied the optical properties of ZnO powder synthesized by using a proteic sol-gel process with coconut water as the precursor. The energy dispersive X-ray spectrometer and X-ray diffraction results show high purity of the synthesized ZnO powder. From the low-temperature (12 K) and power-dependent PL spectra, the donor-bound exciton, the acceptor-bound exciton, the donor-to-acceptor pair (DAP), and the phonon-replica of the DAP transition have been observed at 3.38, 3.34, 3.26, and 3.19 eV, respectively. The free exciton emission (˜3.3 eV) is also observed at 300 K in the temperature-dependent PL spectra.

Spectral features and antibacterial properties of Cu-doped ZnO nanoparticles prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Alireza, Samavati; A, F. Ismail; Hadi, Nur; Z, Othaman; M, K. Mustafa

2016-07-01

Zn1-x Cu x O (x = 0.00, 0.01, 0.03, and 0.05) nanoparticles are synthesized via the sol-gel technique using gelatin and nitrate precursors. The impact of copper concentration on the structural, optical, and antibacterial properties of these nanoparticles is demonstrated. Powder x-ray diffraction investigations have illustrated the organized Cu doping into ZnO nanoparticles up to Cu concentration of 5% (x = 0.05). However, the peak corresponding to CuO for x = 0.01 is not distinguishable. The images of field emission scanning electron microscopy demonstrate the existence of a nearly spherical shape with a size in the range of 30-52 nm. Doping Cu creates the Cu-O-Zn on the surface and results in a decrease in the crystallite size. Photoluminescence and absorption spectra display that doping Cu causes an increment in the energy band gap. The antibacterial activities of the nanoparticles are examined against Escherichia coli (Gram negative bacteria) cultures using optical density at 600 nm and a comparison of the size of inhibition zone diameter. It is found that both pure and doped ZnO nanoparticles indicate appropriate antibacterial activity which rises with Cu doping. Project supported by the Universiti Teknologi Malaysia (UTM) (Grant No. R. J1300000.7809.4F626). Dr. Samavati is thankful to RMC for postdoctoral grants.

Effect of replacing Sn4+ ions by Zn2+ ions on structural, optical and magnetic properties of SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Selvi, E. Thamarai; Sundar, S. Meenakshi

2017-05-01

This paper highlights on the consequence of replacing tetravalent Sn4+ ions of the SnO2 by divalent Zn2+ ions on their structural, optical, and magnetic properties. Samples of Sn1- x Zn x O2 with x = 0, 0.01, 0.02, 0.03, and 0.04 were synthesized using microwave irradiated solvothermal process. The X-ray powder diffraction patterns reveal the rutile tetragonal phase of all doped SnO2 samples with no secondary phases. The transmission electron microscopy results show the formation of spherical nanoparticles of size 10-30 nm. Morphological changes were observed by scanning electron microscopy. The functional groups were investigated using Fourier transform infrared spectroscopy studies. Optical studies were carried by UV-Vis spectroscopy and fluorescence spectroscopy. Electron paramagnetic resonance was used to calculate the Lande splitting factor ` g'. The magnetic properties using vibrating sample magnetometer exhibit room temperature ferromagnetism for all the samples.

New opportunities in the preparation of nanocomposites for biomedical applications: revised mechanosynthesis of magnetite-silica nanocomposites

NASA Astrophysics Data System (ADS)

Scano, Alessandra; Cabras, Valentina; Marongiu, Francesca; Peddis, Davide; Pilloni, Martina; Ennas, Guido

2017-02-01

Environmentally friendly preparation of functionalized magnetite-silica (Fe3O4/SiO2) nanocomposites (NCs) with different SiO2 content (6, 20 and 50 wt%) using revised mechanosynthesis is reported. High-energy ball milling of α-Fe2O3, Si and SiO2 mixtures was followed by hydrolysis and condensation of 3-aminopropyl-triethoxysilane. X-ray powder diffraction and transmission electron microscopy showed the formation of almost spherical Fe3O4 nanocrystals with a narrow size distribution (4-6 nm) uniformly dispersed in the amorphous 100-200 nm SiO2 agglomerates. Scanning electron microscopy and energy dispersive spectroscopy were used to study the elemental distribution in the sample. Fourier transform infrared spectroscopy confirmed the NC surface functionalization with amino groups. Magnetic properties were also explored, indicating a homogeneous distribution of magnetic nanoparticles in the silica matrix.

Nanocrystalline Chalcopyrite Materials (CuInS2 and CuInSe2) via Low-Temperature Pyrolysis of Molecular Single-Source Precursors

NASA Technical Reports Server (NTRS)

Castro, Stephanie L.; Bailey, Sheila G.; Raffaelle, Ryne P.; Banger, Kulbinder K.; Hepp, Aloysius F.

2003-01-01

Nanometer sized particles of the chalcopyrite compounds CuInS2 and CuInSe2 were synthesized by thermal decomposition of molecular single-source precursors (PPh3)2CuIn(SEt)4 and (PPh3)2CuIn(SePh)4, respectively, in the non-coordinating solvent dioctyl phthalate at temperatures between 200 and 300 C. The nanoparticles range in size from 3 - 30 nm and are aggregated to form roughly spherical clusters of about 500 nm in diameter. X-ray diffraction of the nanoparticle powders shows greatly broadened lines indicative of very small particle sizes, which is confirmed by TEM. Peaks present in the XRD can be indexed to reference patterns for the respective chalcopyrite compounds. Optical spectroscopy and elemental analysis by energy dispersive spectroscopy support the identification of the nanoparticles as chalcopyrites.

Molten salt synthesis, visible and near-IR region spectral properties of europium or neodymium doped CoNb2O6 columbite niobate.

PubMed

Ekmekçi, Mete Kaan; Erdem, Murat; Başak, Ali Sadi

2015-03-28

Pure Nd(3+)- or Eu(3+)-doped CoNb2O6 powders have been prepared by a molten salt synthesis method using a Li2SO4-Na2SO4 or NaCl-KCl salt mixture as a flux at relatively low temperatures as compared to the solid state reaction method. X-ray diffraction patterns of pure CoNb2O6 samples indicated an orthorhombic single phase. For Eu(3+)-doped CoNb2O6 samples, the luminescence of Eu(3+) was observed at 615 nm as red emission while the Nd(3+) doped sample showed a typical emission at 1064 nm varying with the Eu(3+) or Nd(3+) doping concentrations. These luminescence characteristics of the doped samples may be attributed to the energy transfer between rare earth ions and CoO6 octahedral groups in the columbite structure.

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

PubMed

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

2015-12-05

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

Synthesis and photoluminescence properties of Pb2+ doped inorganic borate phosphor NaSr4(BO3)3

NASA Astrophysics Data System (ADS)

Chauhan, A. O.; Koparkar, K. A.; Bajaj, N. S.; Omanwar, S. K.

2016-05-01

A series of Inorganic borate phosphors NaSr4(BO3)3 doped with Pb2+ was successfully synthesized by modified solid state diffusion method. The crystal structure and the phase purity of sample were characterized by powder X-ray diffraction (XRD). The photoluminescence properties of synthesized materials were investigated using spectrofluorometer at room temperature. The phosphor show strong broad band emission spectra in UVA region maximum at 370 nm under the excitation of 289 nm. The dependence of the emission intensity on the Pb2+ concentration for the NaSr4(BO3)3 were studied in details. The concentration quenching of Pb2+ doped NaSr4(BO3)3 was observed at 0.02 mol. The Stokes shifts of NaSr4(BO3)3: Pb2+ phosphor was calculated to be 7574 cm-1.

Growth of well-aligned ZnO nanorods using auge catalyst by vapor phase transportation.

PubMed

Ha, S Y; Jung, M N; Park, S H; Ko, H J; Ko, H; Oh, D C; Yao, T; Chang, J H

2006-11-01

Well-aligned ZnO nanorods have been achieved using new alloy (AuGe) catalyst. Zn powder was used as a source material and it was transported in a horizontal tube furnace onto an AuGe deposited Si substrates. The structural and optical properties of ZnO nanorods were characterized by scanning electron microscopy, high resolution X-ray diffraction, and photoluminescence. ZnO nanorods grown at 650 degrees C on 53 nm thick AuGe layer show uniform shape with the length of 8 +/- 0.5 microm and the diameter of 150 +/- 5 nm. Also, the tilting angle of ZnO nanorods (+/- 5.5 degrees) is confirmed by HRXRD. High structural quality of the nanorods is conformed by the photoluminescence measurement. All samples show strong UV emission without considerable deep level emission. However, weak deep level emission appears at high (700 degrees C) temperature due to the increase of oxygen desertion.

Preparation and characterization of 'green' hybrid clay-dye nanopigments

NASA Astrophysics Data System (ADS)

Kaya, Mehmet; Onganer, Yavuz; Tabak, Ahmet

2015-03-01

We obtained a low cost and abundant nanopigment material composed of Rhodamine B (Rh-B) organic dye compound and Unye bentonite (UB) clay from Turkey. The characterization of the nanopigment was investigated using scanning electron microscopy (SEM), particle size distribution, powder X-ray diffraction (PXRD), Fourier transformed infra-red spectroscopy (FT-IR) and thermal analysis techniques. According to the result of texture analyses, we showed that the particle size distribution (d: 0.5-mean distribution) of Rh-B/UB nanopigment material was around 100 nm diameter. It was also demonstrated that the samples had a particle size around nm diameter in SEM images. As seen in the PXRD and thermal analysis, there is a difference in basal spacing by 1.46° (2θ) and a higher mass loss by 7.80% in the temperature range 200-500 °C compared to the raw bentonite.

Ceramic materials with low thermal conductivity and low coefficients of thermal expansion

DOEpatents

Brown, Jesse; Hirschfeld, Deidre; Liu, Dean-Mo; Yang, Yaping; Li, Tingkai; Swanson, Robert E.; Van Aken, Steven; Kim, Jin-Min

1992-01-01

Compositions having the general formula (Ca.sub.x Mg.sub.1-x)Zr.sub.4 (PO.sub.4).sub.6 where x is between 0.5 and 0.99 are produced by solid state and sol-gel processes. In a preferred embodiment, when x is between 0.5 and 0.8, the MgCZP materials have near-zero coefficients of thermal expansion. The MgCZPs of the present invention also show unusually low thermal conductivities, and are stable at high temperatures. Macrostructures formed from MgCZP are useful in a wide variety of high-temperature applications. In a preferred process, calcium, magnesium, and zirconium nitrate solutions have their pH adjusted to between 7 and 9 either before or after the addition of ammonium dihydrogen phosphate. After dehydration to a gel, and calcination at temperatures in excess of 850.degree. C. for approximately 16 hours, single phase crystalline MgCZP powders with particle sizes ranging from approximately 20 nm to 50 nm result. The MgCZP powders are then sintered at temperatures ranging from 1200.degree. C. to 1350.degree. C. to form solid macrostructures with near-zero bulk coefficients of thermal expansion and low thermal conductivities. Porous macrostructures of the MgCZP powders of the present invention are also formed by combination with a polymeric powder and a binding agent, and sintering at high temperatures. The porosity of the resulting macrostructures can be adjusted by varying the particle size of the polymeric powder used.

Ceramic materials with low thermal conductivity and low coefficients of thermal expansion

DOEpatents

Brown, J.; Hirschfeld, D.; Liu, D.M.; Yang, Y.; Li, T.; Swanson, R.E.; Van Aken, S.; Kim, J.M.

1992-04-07

Compositions, having the general formula (Ca[sub x]Mg[sub 1[minus]x])Zr[sub 4](PO[sub 4])[sub 6] where x is between 0.5 and 0.99, are produced by solid state and sol-gel processes. In a preferred embodiment, when x is between 0.5 and 0.8, the MgCZP materials have near-zero coefficients of thermal expansion. The MgCZPs of the present invention also show unusually low thermal conductivities, and are stable at high temperatures. Macrostructures formed from MgCZP are useful in a wide variety of high-temperature applications. In a preferred process, calcium, magnesium, and zirconium nitrate solutions have their pH adjusted to between 7 and 9 either before or after the addition of ammonium dihydrogen phosphate. After dehydration to a gel, and calcination at temperatures in excess of 850 C for approximately 16 hours, single phase crystalline MgCZP powders with particle sizes ranging from approximately 20 nm to 50 nm result. The MgCZP powders are then sintered at temperatures ranging from 1200 C to 1350 C to form solid macrostructures with near-zero bulk coefficients of thermal expansion and low thermal conductivities. Porous macrostructures of the MgCZP powders of the present invention are also formed by combination with a polymeric powder and a binding agent, and sintering at high temperatures. The porosity of the resulting macrostructures can be adjusted by varying the particle size of the polymeric powder used. 7 figs.

Rare-earth doped gadolinia based phosphors for potential multicolor and white light emitting deep UV LEDs.

PubMed

Bedekar, Vinila; Dutta, Dimple P; Mohapatra, M; Godbole, S V; Ghildiyal, R; Tyagi, A K

2009-03-25

Gadolinium oxide host and europium/dysprosium/terbium doped gadolinium oxide nanoparticles were synthesized using the sonochemical technique. Gadolinium oxide nanocrystals were also co-doped with total 2 mol% of Eu(3+)/Dy(3+),Eu(3+)/Tb(3+),Dy(3+)/Tb(3+), and also Eu(3+)/Dy(3+)/Tb(3+) ions, by the same method. The nanoparticles obtained were characterized using powder x-ray diffraction (XRD), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) techniques. The size of the particles ranged from 15 to 30 nm. The triple doped samples showed multicolor emission on single wavelength excitation. The photoluminescence results were correlated with the lifetime data to get an insight into the luminescence and energy transfer processes taking place in the system. On excitation at 247 nm, the novel nanocrystalline Gd(2)O(3):RE (RE = Dy, Tb) phosphor resulted in having very impressive CIE chromaticity coordinates of x = 0.315 and y = 0.316, and a correlated color temperature of 6508 K, which is very close to standard daylight.

Influence of Different Aluminum Sources on the NH3 Gas-Sensing Properties of ZnO Thin Films

NASA Astrophysics Data System (ADS)

Ozutok, Fatma; Karaduman, Irmak; Demiri, Sani; Acar, Selim

2018-02-01

Herein we report Al-doped ZnO films (AZO) deposited on the ZnO seed layer by chemical bath deposition method. Al powder, Al oxide and Al chloride were used as sources for the deposition process and investigated for their different effects on the NH3 gas-sensing performance. The morphological and microstructural properties were investigated by employing x-ray powder diffraction, scanning electron microscopy analysis and energy-dispersive x-ray spectroscopy. The characterization studies showed that the AZO thin films are crystalline and exhibit a hexagonal wurtzite structure. Ammonia (NH3) gas-sensing measurements of AZO films were performed at different concentration levels and different operation temperatures from 50°C to 210°C. The sample based on powder-Al source showed a higher response, selectivity and short response/recovery time than the remaining samples. The powder Al sample exhibited 33% response to 10-ppm ammonia gas at 190°C, confirming a strong dependence on the dopant source type.

Cr/B 4C multilayer mirrors: Study of interfaces and X-ray reflectance

DOE PAGES

Burcklen, C.; Soufli, R.; Gullikson, E.; ...

2016-03-24

Here, we present an experimental study of the effect of layer interfaces on the x-ray reflectance in Cr/B 4C multilayer interference coatings with layer thicknesses ranging from 0.7 nm to 5.4 nm. The multilayers were deposited by magnetron sputtering and by ion beam sputtering. Grazing incidence x-ray reflectometry, soft x-ray reflectometry, and transmission electron microscopy reveal asymmetric multilayer structures with a larger B 4C-on-Cr interface, which we modeled with a 1–1.5 nm thick interfacial layer. Reflectance measurements in the vicinity of the Cr L 2,3 absorption edge demonstrate fine structure that is not predicted by simulations using the currently tabulatedmore » refractive index (optical constants) values for Cr.« less

An instrument for 3D x-ray nano-imaging

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

Holler, M.; Raabe, J.; Diaz, A.

We present an instrument dedicated to 3D scanning x-ray microscopy, allowing a sample to be precisely scanned through a beam while the angle of x-ray incidence can be changed. The position of the sample is controlled with respect to the beam-defining optics by laser interferometry. The instrument achieves a position stability better than 10 nm standard deviation. The instrument performance is assessed using scanning x-ray diffraction microscopy and we demonstrate a resolution of 18 nm in 2D imaging of a lithographic test pattern while the beam was defined by a pinhole of 3 {mu}m in diameter. In 3D on amore » test object of copper interconnects of a microprocessor, a resolution of 53 nm is achieved.« less

Preparation, characterization and X-ray attenuation property of Gd2O3-based nanocomposites

NASA Astrophysics Data System (ADS)

Jayakumar, Sangeetha; Saravanan, T.; Philip, John

2017-11-01

In an attempt to develop an alternate to lead-based X-ray shielding material, we describe the X-ray attenuation property of nanocomposites containing Gd2O3 as nanofiller and silicone resin as matrix, prepared by a simple solution-casting technique. Gd2O3 nanoparticles of size 30 and 56 nm are used at concentrations of 25 and 2.5 wt%. The nanoparticles and the nanocomposites are characterized using X-ray diffraction (XRD) studies, small angle X-ray spectroscopy (SAXS), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and atomic force microscopy (AFM). The X-ray attenuation property of nanocomposites, studied using an industrial X-ray unit, shows that nanocomposites containing nanoparticles of size 56 nm (G2) exhibit better attenuation than nanocomposites containing nanoparticles of size 30 nm (G1), which is attributed to the greater interfacial interaction between the G2 nanofillers and silicone matrix. In the case of nanocomposites containing G1 nanoparticles, the interfacial interaction between the nanofiller and the matrix is so weak that it results in pulling out of nanofillers, causing voids in the matrix, which act as X-ray transparent region, thereby reducing the overall X-ray attenuation property of G1 nanocomposites. This is further corroborated from the AFM images of the nanocomposites. The weight loss and heat flow curves of pure silicone matrix and the nanocomposites containing Gd2O3 nanoparticles of size 30 and 56 nm show the degradation of silicone resin, due to chain scission, between 403 and 622 °C. The same onset temperature (403 °C) of degradation of matrix with and without nanoparticles shows that the addition of nanofillers to the matrix does not deteriorate the thermal stability of the matrix. This confirms the thermal stability of nanocomposites. Therefore, our study shows that nanocomposites containing G2 nanoparticles are potential candidates for the development of X-ray opaque fabric material.

Effect of powder compaction on radiation-thermal synthesis of lithium-titanium ferrites

NASA Astrophysics Data System (ADS)

Surzhikov, A. P.; Lysenko, E. N.; Vlasov, V. A.; Malyshev, A. V.; Korobeynikov, M. V.; Mikhailenko, M. A.

2017-01-01

Effect of powder compaction on the efficiency of thermal and radiation-thermal synthesis of lithium-substituted ferrites was investigated by X-Ray diffraction and specific magnetization analysis. It was shown that the radiation-thermal heating of compacted powder reagents mixture leads to an increase in efficiency of lithium-titanium ferrites synthesis.

The Ti-Mn system revisited: experimental investigation and thermodynamic modelling.

PubMed

Khan, A U; Brož, P; Premović, M; Pavlů, J; Vřeštál, J; Yan, X; Maccio, D; Saccone, A; Giester, G; Rogl, P

2016-08-17

As the Ti-Mn phase diagram is part of numerous ternary and higher order systems of technological importance, the present paper defines phase relations which have been experimentally established throughout this work from 800 °C to the melting range based on Differential Thermal Analyses (DTA), X-ray powder diffraction, metallography and Electron Probe Micro Analysis (EPMA) techniques on ∼50 alloys, which were prepared by arc melting or high frequency melting under high purity argon starting from freshly cleaned metal ingots. Novel compounds were identified and reaction isotherms were redefined accordingly. In the Ti-rich region a novel compound TiMn was detected, sandwiched between the known phases: TiMn1-x (∼45 at% Mn) and TiMn1+x (∼55 at% Mn). In the Mn-rich region the hitherto unknown crystal structure of TiMn∼3 was solved from X-ray single crystal diffraction data and found to be of a unique structure type Ti6(Ti1-xMnx)6Mn25 (x = 0.462; space group Pbam (#55); a = 0.79081(3) nm, b = 2.58557(9) nm, c = 0.47931(2) nm), which consists of two consecutive layers of the hexagonal MgZn2-type Laves phase (TiMn2) and a combined layer of alternate structure blocks of MgZn2 type and Zr4Al3 type. Whereas TiMn can be considered as a line compound (solubility range <∼1 at%), the homogeneity regions of the Ti-Mn compounds are significant (determined by EPMA): TiMn1-x (44.0 to 46.6 at% Mn), TiMn1+x (54.6 to 56.3 at% Mn), Ti1+xMn2-x (MgZn2-type, 59 to 69 at% Mn at 1000 °C: -0.08 < x < 0.23), TiMn∼3 (unique type; 74 to 76.5 at% Mn) and TiMn∼4 (R-phase: Ti8(TixMn1-x)6Mn39, 80 to 84 at% Ti). Supported by ab initio calculations of the ground state energy for the Laves phase, the new experimental results enabled thermodynamic modelling of the entire Ti-Mn phase diagram providing a complete and novel set of thermodynamic data thus providing a sound basis for future thermodynamic predictions of higher order Ti-Mn-X-Y systems.

A multi-analytical approach for the characterization of powders from the Pompeii archaeological site.

PubMed

Canevali, Carmen; Gentile, Paolo; Orlandi, Marco; Modugno, Francesca; Lucejko, Jeannette Jacqueline; Colombini, Maria Perla; Brambilla, Laura; Goidanich, Sara; Riedo, Chiara; Chiantore, Oscar; Baraldi, Pietro; Baraldi, Cecilia; Gamberini, Maria Cristina

2011-10-01

Nine black powders found in Pompeii houses in three different types of bronze vessels (cylindrical theca atramentaria, unguentaries, and aryballoi) were characterized in order to assess a correspondence between the composition and the type of vessel and, possibly, to verify if these powders were inks or not. For the compositional characterization, a multi-analytical approach was adopted, which involved the use of scanning electron microscopy-energy dispersive X-ray, Fourier-transformed infrared spectroscopy, Raman, X-ray diffraction, electron paramagnetic resonance spectroscopy, thermogravimetric analysis, gas chromatography coupled with mass spectrometry (GC/MS), and pyrolysis GC/MS. Powders contained in cylindrical theca atramentaria form a homogeneous group, and their organic and inorganic compositions suggest that they were writing inks, while powders contained in unguentaries and aryballoi could have had several different uses, including writing inks and cosmetics. Furthermore, the composition profile of the powders found in cylindrical cases shows that, at 79 AD: , in Pompeii, carbon-based inks were still used for writing, and iron gall inks had not been introduced yet.

Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

NASA Astrophysics Data System (ADS)

Cheung, Eugene Y.; David, Sarah E.; Harris, Kenneth D. M.; Conway, Barbara R.; Timmins, Peter

2007-03-01

We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H 2NC(CH 3) 3-n(CH 2OH) n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family ( n=0, 1, 2), but significantly contrasting structural properties for the member with n=3.

Raman scattering and X-ray powder diffraction studies of hydrate layered perovskites: dirubidium aquapentafluoromanganate(III) and dipotassium aquapentafluoroferrate(III)

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

Galicka, Karolina; Slodczyk, Aneta; Ratuszna, Alicja

2004-06-08

The structural and vibrational properties of above mentioned crystals were determined using X-ray powder diffraction and Raman scattering experiments. At room temperature hydrate layered perovskites: Rb{sub 2}MnF{sub 5}{center_dot}H{sub 2}O and K{sub 2}FeF{sub 5}{center_dot}H{sub 2}O exhibit orthorhombic--Cmcm (D{sub 2h}{sup 17}) and monoclinic--C2/c (C{sub 2h}{sup 6}) symmetry. Their structure is built up of MnF{sub 6} or FeF{sub 5}{center_dot}H{sub 2}O octahedra forming trans-linked zig-zag chains or hydrogen bonded zig-zag chains along the major crystallographic direction [0 0 1], respectively. To confirm crystal structures and to describe lattice dynamics of these compounds the vibrational normal modes (in {gamma} point of first Brillouin zone) weremore » calculated on the base of the group theory analysis and compared with the spectra obtained from Raman scattering experiments. A relatively good reliability was obtained for both X-ray powder diffraction and Raman scattering.« less

Crystal growth, structural, optical, mechanical and thermal properties of a new nonlinear optical single crystal: L-Ornithine monohydrochloride.

PubMed

Balakrishnan, T; Ramamurthi, K

2009-03-01

Amino acid family crystals exhibit excellent nonlinear optical and electro optical properties. l-Ornithine monohydrochloride single crystal, belongs to the amino acid group, was grown by the slow evaporation solution growth technique at room temperature. The grown crystals were characterized by single crystal and powder X-ray diffraction analysis, Fourier transform infrared (FTIR) spectroscopy, TGA, DTA and DSC analyses. UV-vis-NIR spectrum shows excellent transmission in the UV, visible and NIR region (300-1600nm). The mechanical properties of grown crystals were studied using Vickers microhardness tester. Its second harmonic generation efficiency was tested using Nd:YAG laser and is 1.25 times that of KDP.

Preparation, characterization and catalytic application of CoFe2O4 nanoparticles in the synthesis of benzimidazoles

NASA Astrophysics Data System (ADS)

Borade, Ravikumar M.; Shinde, Pavan R.; Kale, Swati B.; Pawar, Rajendra P.

2018-05-01

A highly efficient magnetically recoverable cobalt ferrite nano-catalyst was prepared by sol-gel autocombustion method using glycine as green fuel. The prepared material has been characterized by X-ray powder diffraction and scanning. An investigation of its catalytic activity showed it to be a heterogeneous Lewis acid catalyst for the synthesis of substituted benzimidazoles. The aqueous ethanol used as green solvent for the reaction. The nm size range of these particles facilitates the catalysis process, as an increased surface area available for the reaction. The easy separation of the catalyst by an external magnet and their recovery and reuse in next cycle reaction are additional benefits.

Synthesis of Nano-Crystalline Cu-Cr Alloy by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Sheibani, S.; Heshmati-Manesh, S.; Ataie, A.

In this paper, the influence of toluene as the process control agent (PCA) and pre-milling on the extension of solid solubility of 7 wt.% Cr in Cu by mechanical alloying in a high energy ball mill was investigated. The structural evolution and microstructure were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques, respectively. The solid solution formation at different conditions was analyzed by copper lattice parameter change during the milling process. It was found that both the presence of PCA and pre-milling of Cr powder lead to faster dissolution of Cr. The mean crystallite size was also calculated and showed to be about 10 nm after 80 hours of milling.

Stability of a Cu0.7Co2.3O4 electrode during the oxygen evolution reaction for alkaline anion-exchange membrane water electrolysis

NASA Astrophysics Data System (ADS)

Kang, Kyoung Eun; Kim, Chi Ho; Lee, Myung Sup; Jung, Chang Wook; Kim, Yang Do; Lee, Jae Ho

2018-01-01

The electrode materials for oxygen evolution, especially non-platinum group metal oxides, have attracted increasing attention. Among the spinel-type transition metal oxides, Cu0.7Co2.3O4 powders were evaluated as a potential replacement for expensive dimensionally stabilized anode materials. Cu0.7Co2.3O4 powder for use as an electrode material for oxygen evolution in an alkaline anion-exchange membrane water electrolyzer was prepared using a thermal decomposition method. The Cu0.7Co2.3O4 powders heat-treated at 250 °C exhibited the same X-ray diffraction patterns without any secondary phases as the Co3O4 spinel structure did. The Cu0.7Co2.3O4 powders heat-treated at 250 °C for 30 minutes showed the smallest mean particle size of approximately 376 nm with the powders having a homogeneous shape and size distribution. The fine powders with a relatively homogeneous size distribution showed a higher current density during the oxygen evolution reaction. The lifetime of the Cu0.7Co2.3O4 electrode was relatively long at a low current density, but was quickly shortened due to physical detachment of the Cu0.7Co2.3O4 powders as the current density was increased. This study showed that the efficiency and the stability of Cu0.7Co2.3O4 powders during the oxygen evolution reaction were related directly to the active electrode area.

Effect of surface coating with magnesium stearate via mechanical dry powder coating approach on the aerosol performance of micronized drug powders from dry powder inhalers.

PubMed

Zhou, Qi Tony; Qu, Li; Gengenbach, Thomas; Larson, Ian; Stewart, Peter J; Morton, David A V

2013-03-01

The objective of this study was to investigate the effect of particle surface coating with magnesium stearate on the aerosolization of dry powder inhaler formulations. Micronized salbutamol sulphate as a model drug was dry coated with magnesium stearate using a mechanofusion technique. The coating quality was characterized by X-ray photoelectron spectroscopy. Powder bulk and flow properties were assessed by bulk densities and shear cell measurements. The aerosol performance was studied by laser diffraction and supported by a twin-stage impinger. High degrees of coating coverage were achieved after mechanofusion, as measured by X-ray photoelectron spectroscopy. Concomitant significant increases occurred in powder bulk densities and in aerosol performance after coating. The apparent optimum performance corresponded with using 2% w/w magnesium stearate. In contrast, traditional blending resulted in no significant changes in either bulk or aerosolization behaviour compared to the untreated sample. It is believed that conventional low-shear blending provides insufficient energy levels to expose host micronized particle surfaces from agglomerates and to distribute guest coating material effectively for coating. A simple ultra-high-shear mechanical dry powder coating step was shown as highly effective in producing ultra-thin coatings on micronized powders and to substantially improve the powder aerosolization efficiency.

Specimen charging in X-ray absorption spectroscopy: correction of total electron yield data from stabilized zirconia in the energy range 250-915 eV.

PubMed

Vlachos, Dimitrios; Craven, Alan J; McComb, David W

2005-03-01

The effects of specimen charging on X-ray absorption spectroscopy using total electron yield have been investigated using powder samples of zirconia stabilized by a range of oxides. The stabilized zirconia powder was mixed with graphite to minimize the charging but significant modifications of the intensities of features in the X-ray absorption near-edge fine structure (XANES) still occurred. The time dependence of the charging was measured experimentally using a time scan, and an algorithm was developed to use this measured time dependence to correct the effects of the charging. The algorithm assumes that the system approaches the equilibrium state by an exponential decay. The corrected XANES show improved agreement with the electron energy-loss near-edge fine structure obtained from the same samples.

The synthesis and the luminescence properties of Sr2Ga3La1-xDyxGe3O14

NASA Astrophysics Data System (ADS)

Wang, Qiang; Mu, Zhongfei; Yang, Lurong; Zhang, Shaoan; Zhu, Daoyun; Yang, Yibin; Luo, Dongxiang; Wu, Fugen

2018-02-01

A series of Sr2Ga3La1-xDyxGe3O14 (x = 0, 0.015, 0.03, 0.045, 0.06, 0.075, 0.09) phosphors were synthesized by high temperature solid state reactions. X-ray diffraction analysis proves that single-phase Sr2Ga3La1-xDyxGe3O14 (0 ≤ x ≤ 0.09) has been obtained. The particle size of these powders is in the range from 1 to 3 μm. The host Sr2Ga3LaGe3O14 emits blue white light under the excitation of 260 nm ultraviolet light. Dy3+ doped samples can be effectively excited with near ultraviolet light and exhibit two emission bands in the blue (4F9/2 → 6H15/2) and yellow regions (4F9/2 → 6H13/2), which can form white light. Present research indicates that Dy3+ doped Sr2Ga3LaGe3O14 have the potential to be a single-phase full-color emitting phosphor.

Fabrication of 0.25-um electrode width SAW filters using x-ray lithography with a laser plasma source

NASA Astrophysics Data System (ADS)

Bobkowski, Romuald; Li, Yunlei; Fedosejevs, Robert; Broughton, James N.

1996-05-01

A process for the fabrication of surface acoustic wave (SAW) devices with line widths of 250 nm and less, based on x-ray lithography using a laser-plasma source has been developed. The x-ray lithography process is based on keV x-ray emission from Cu plasma produced by 15 Hz, 50 ps, 248 nm KrF excimer laser pulses. The full structure of a 2 GHz surface acoustic wave filter with interdigital transducers in a split-electrode geometry has been manufactured. The devices require patterning a 150 nm thick aluminum layer on a LiNbO3 substrate with electrodes 250 nm wide. The manufacturing process has two main steps: x-ray mask fabrication employing e-beam lithography and x-ray lithography to obtain the final device. The x-ray masks are fabricated on 1 micrometers thick membranes of Si2N4. The line patterns on the masks are written into PMMA resist using a scanning electron microscope which has been interfaced to a personal computer equipped to control the x and y scan voltages. The opaque regions of the x-ray mask are then formed by electroplating fine grain gold into the open spaces in the etched PMMA. The mask and sample are mounted in an exposure cassette with a fixed spacer of 10 micrometers separating them. The sample consists of a LiNbO3 substrate coated with Shipley XP90104C x-ray resist which has been previously characterized. The x-ray patterning is carried out in an exposure chamber with flowing helium background gas in order to minimize debris deposition on the filters. After etching the x-ray resist, the final patterns are produced using metallization and a standard lift-off technique. The SAW filters are then bonded and packaged onto impedance matching striplines. The resultant devices are tested using Scalar Network Analyzers. The final devices produced had a center frequency of 1.93 GHz with a bandwidth of 98 MHz, close to the expected performance of our simple design.

Composition and phase analysis of nanocrystalline Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 1.0; 0.6; and 0.4) by using general structure analysis system

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

Gunanto, Y. E., E-mail: yohanes.gunanto@uph.edu; Jobiliong, E., E-mail: eric.jobiliong@uph.edu; Adi, Wisnu Ari, E-mail: dwisnuaa@batan.go.id

2016-03-11

Single phase of nanocrystalline Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 1.0; 0.6; and 0.4) was successfully synthesized by mechanical milling method and thermal process. Stoichiometric quantities of analytical-grade SrCO{sub 3}, BaCO{sub 3}, and Fe{sub 2}O{sub 3}, were mixed and milled using a high-energy milling. The mixture of all precursors was sintered at a temperature of 1000 °C for 10 hours. The refinement of x-ray diffraction trace for all samples confirmed a single phase material with a hexagonal structure. The increase of the amount of strontium content in the barium atoms in the Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} system canmore » decrease the lattice parameter which have been successfully substituted into the barium atoms. The calculation result of cationic distribution showed that the Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 0.6) and (x = 0.4) samples have nominal composition of Ba{sub 0,61}Sr{sub 0,39}Fe{sub 12}O{sub 19} and Ba{sub 0,37}Sr{sub 0,63}Fe{sub 12}O{sub 19}, respectively. Results of the mean of crystallite size evaluation for respective powder materials showed that the Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 1.0; 0.6; and 0.4) samples have the crystallite size of 22 nm, 25 nm and 34 nm, respectively. We concluded that the cationic distribution of barium atoms was successfully substituted by strontium atoms approaching the nominal stoichiometric composition.« less

Crystal Chemistry and Magnetism of Ternary Actinoid Boron Carbides UB 1- xC 1+ x and U 1- xMxB 2C with M = Sc, Lu, and Th

NASA Astrophysics Data System (ADS)

Rogl, P.; Rupp, B.; Felner, I.; Fischer, P.

1993-06-01

Within the homogeneous range of uranium monocarbide UB 1- xC 1+ x, the crystal structures of stoichiometric UBC and of the carbon-rich solid solution UB 0.78C 1.22, have been refined from single-crystal X-ray counter data. From X-ray analysis crystal symmetry in both cases is consistent with the centro-symmetric space group Cmcm and there are no indications of superstructure formation. In contrast to the fully ordered atom arrangement revealed for stoichiometric UBC ( a = 0.35899(4), b = 1.19781(12), c = 0.33474(3) nm), random occupation by boron and carbon atoms is observed for the boron site in UB 0.78C 1.22 ( a = 0.35752(4), b = 1.18584(3), c = 0.33881(4) nm). For 279(278) reflections (|F 0| > 3σ) the obtained reliability factors R x = ∑|ΔF|/∑| F0| were R x = 0.069 for UBC and R x = 0.050 for UB 0.78C 1.22. Neutron powder diffraction experiments at 9 and 295 K unambiguously revealed full occupancy by the nonmetal atoms in UB 0.78C 1.22 and prove the statistical occupation of B and C atoms in the B-sites. For the orthorhombic symmetry Cmcm, refinement was not better than R1 = 0.044. A model calculation in monoclinic symmetry C12/ m1, however, resulted in a significant reduction of the residual value to R1 = 0.030, releasing spatial constraints on the boron atoms. Thus the boron-boron chain in Cmcm (B-B = 0.1874 nm) is dissolved into boron pairs (B-B = 0.1706 nm) which are loosely bound at a distance of 0.2043 nm. The formation of C-B-B-C groups corresponds to the structure types of ThBC and Th 3B 2C 3. The magnetic behavior has been investigated in the temperature range from 4.2 K to 1000 K for UB 1- xC 1+ x (UBC-type) and U 1- xMxB 2C (ThB 2C-type for the high temperature modification and 1-UB 2C-type for the low temperature modification) with U partially substituted by Th or Sc, Lu. From magnetic susceptibilities, the alloys UB 1- xC 1+ x reveal temperature independent paramagnetism with typical intermediate valence fluctuation behavior ( TSF ˜ 350 K). ThB 2C and 1-UB 2C both are temperature independent paramagnets, whereas h-UB 2C is a ferromagnet with the rather high Curie temperature TM = 80(2) K. TM and the saturation magnetiziation per U atom both successively decrease on substitution of U by Th, Sc, or Lu in UB 2C, whereas the U-moments remain practically unchanged at μ eff(U) ˜ 1.9 μ B. Uranium L 3-XANES (X-ray Absorption Near Edge Structure) spectroscopy revealed increased d-band localization, comparable to uranium-transition metal alloys, in nonmagnetic UB 1- xC 1+ x ( x = 0, 0.22). No superconductivity was observed down to 1.5 K; no hydrogen uptake was observed for UB 2C and ThB 2C even under hydrogen pressures as high as 7 × 10 7 Pa at 670 K.

Layered surface structure of gas-atomized high Nb-containing TiAl powder and its impact on laser energy absorption for selective laser melting

NASA Astrophysics Data System (ADS)

Zhou, Y. H.; Lin, S. F.; Hou, Y. H.; Wang, D. W.; Zhou, P.; Han, P. L.; Li, Y. L.; Yan, M.

2018-05-01

Ti45Al8Nb alloy (in at.%) is designed to be an important high-temperature material. However, its fabrication through laser-based additive manufacturing is difficult to achieve. We present here that a good understanding of the surface structure of raw material (i.e. Ti45Al8Nb powder) is important for optimizing its process by selective laser melting (SLM). Detailed X-ray photoelectron spectroscopy (XPS) depth profiling and transmission electron microscopy (TEM) analyses were conducted to determine the surface structure of Ti45Al8Nb powder. An envelope structure (∼54.0 nm in thickness) was revealed for the powder, consisting of TiO2 + Nb2O5 (as the outer surface layer)/Al2O3 + Nb2O5 (as the intermediate layer)/Al2O3 (as the inner surface layer)/Ti45Al8Nb (as the matrix). During SLM, this layered surface structure interacted with the incident laser beam and improved the laser absorptivity of Ti45Al8Nb powder by ∼32.21%. SLM experiments demonstrate that the relative density of the as-printed parts can be realized to a high degree (∼98.70%), which confirms good laser energy absorption. Such layered surface structure with appropriate phase constitution is essential for promoting SLM of the Ti45Al8Nb alloy.

Optical properties of hydroxyapatite obtained by mechanical alloying

NASA Astrophysics Data System (ADS)

Silva, C. C.; Thomazini, D.; Pinheiro, A. G.; Lanciotti, F.; Sasaki, J. M.; Góes, J. C.; Sombra, A. S. B.

2002-09-01

Calcium phosphate based bioceramics, mainly in the form of hydroxyapatite (HA), have been in use in medicine and dentistry for the last 20 years. Applications include coatings of orthopaedic and dental implants, alveolar ridge augmentation, maxillofacial surgery, otolaryngology, and scaffolds for bone growth and as powders in total hip and knee surgery. These materials exhibit several problems of handling and fabrication, which can be overcome by mixing with a suitable binder. In this paper, mechanical alloying has been used successfully to produce nanocrystalline powders of HA using five different experimental procedures. The milled HA were studied by X-ray powder diffraction, infrared and Raman scattering spectroscopy. For four different procedures, HA was obtained after a couple of hours of milling (on an average, 20 h of milling depending on the reaction procedure). The XRD patterns indicate that the grain size is within the range of 29-103 nm. This milling process, used to produce HA, presents the advantage that melting is not necessary and the powder obtained is nanocrystalline with extraordinary mechanical properties. The material can be compacted and transformed in solid ceramic samples. The high efficiency of the process opens a way to produce commercial amount of nanocrystalline HA. Due to the nanocrystalline character of this powder, their mechanical properties have changed and for this reason a pressure of 1 GPa is enough to shape the sample into any geometry.

Direct Electrochemical Preparation of Cobalt, Tungsten, and Tungsten Carbide from Cemented Carbide Scrap

NASA Astrophysics Data System (ADS)

Xiao, Xiangjun; Xi, Xiaoli; Nie, Zuoren; Zhang, Liwen; Ma, Liwen

2017-02-01

A novel process of preparing cobalt, tungsten, and tungsten carbide powders from cemented carbide scrap by molten salt electrolysis has been investigated in this paper. In this experiment, WC-6Co and NaCl-KCl salt were used as sacrificial anode and electrolyte, respectively. The dissolution potential of cobalt and WC was determined by linear sweep voltammetry to be 0 and 0.6 V ( vs Ag/AgCl), respectively. Furthermore, the electrochemical behavior of cobalt and tungsten ions was investigated by a variety of electrochemical techniques. Results of cyclic voltammetry (CV) and square-wave voltammetry show that the cobalt and tungsten ions existed as Co2+ and W2+ on melts, respectively. The effect of applied voltage, electrolysis current, and electrolysis times on the composition of the product was studied. Results showed that pure cobalt powder can be obtained when the electrolysis potential is lower than 0.6 V or during low current and short times. Double-cathode and two-stage electrolysis was utilized for the preparation of cobalt, tungsten carbide, and tungsten powders. Additionally, X-ray diffraction results confirm that the product collected at cathodes 1 and 2 is pure Co and WC, respectively. Pure tungsten powder was obtained after electrolysis of the second part. Scanning electron microscope results show that the diameters of tungsten, tungsten carbide, and cobalt powder are smaller than 100, 200, and 200 nm, respectively.

Preparation and cathodoluminescence characteristics of rare earth activated BaAl2O4 phosphors.

PubMed

Benourdja, S; Kaynar, Ümit H; Ayvacikli, M; Karabulut, Y; Guinea, J Garcia; Canimoglu, A; Chahed, L; Can, N

2018-04-18

Undoped and Pr, Sm and Tb activated BaAl 2 O 4 phosphors have been synthesized by solid state reaction method and combustion method. The structure and morphological observation of the phosphor samples were monitored by X-ray powder diffraction (XRD) and environmental scanning electron microscope (ESEM) coupled to an energy dispersive X-ray spectrometer (EDS). The all diffraction peaks are well assigned to standard data card (PDF♯17-306). Emission properties of the samples were explored using light emission induced by an electron beam (i.e cathodoluminescence, CL) at room temperature (RT). Undoped BaAl 2 O 4 sample exhibits a broad defect emission from 300 to 500 nm from the aluminate defect centres. CL spectra recorded at room temperature display that the as-prepared BaAl 2 O 4 :Ln (Ln=Pr, Sm and Tb) phosphors exhibit different luminescence colors coming from different rare earth activator ions. The transition 4 G 5/2 → 6 H 7/2 located at 606 and 610 nm for Sm 3+ can occur as hypersensitive transition having the selection rule ΔJ = ± 1. For the Tb 3+ doped samples, they exhibit D45 green line emissions. The proposed luminescent mechanisms of all doped rare earth ions are also discussed. Copyright © 2018 Elsevier Ltd. All rights reserved.

High thermal stability of La 2O 3 and CeO 2-stabilized tetragonal ZrO 2

DOE PAGES

Wang, Shichao; Xie, Hong; Lin, Yuyuan; ...

2016-02-15

Catalyst support materials of tetragonal ZrO 2, stabilized by either La 2O 3 (La 2O 3-ZrO 2) or CeO 2 (CeO 2-ZrO 2), were synthesized under hydrothermal conditions at 200 °C with NH 4OH or tetramethylammonium hydroxide as the mineralizer. From In Situ synchrotron powder X-ray diffraction and small-angle X-ray scattering measurements, the calcined La 2O 3-ZrO 2 and CeO 2-ZrO 2 supports were nonporous nanocrystallites that exhibited rectangular shapes with thermal stability up to 1000 °C in air. These supports had an average size of ~10 nm and a surface area of 59-97 m 2/g. The catalysts Pt/La 2Omore » 3-ZrO 2 and Pt/CeO 2-ZrO 2 were prepared by using atomic layer deposition with varying Pt loadings from 6.3-12.4 wt %. Mono-dispersed Pt nanoparticles of ~3 nm were obtained for these catalysts. As a result, the incorporation of La 2O 3 and CeO 2 into the t-ZrO 2 structure did not affect the nature of the active sites for the Pt/ZrO 2 catalysts for the water-gas-shift (WGS) reaction.« less

Hydrogen sorption characteristics of nanostructured Pd–10Rh processed by cryomilling

DOE PAGES

Yang, Nancy; Yee, Joshua K.; Zhang, Zhihui; ...

2014-10-03

Palladium and its alloys are model systems for studying solid-state storage of hydrogen. Mechanical milling is commonly used to process complex powder systems for solid-state hydrogen storage; however, milling can also be used to evolve nanostructured powder to modify hydrogen sorption characteristics. In the present study, cryomilling (mechanical attrition milling in a cryogenic liquid) is used to produce nanostructured palladium-rhodium alloy powder. Characterization of the cryomilled Pd-10Rh using electron microscopy, X-ray diffraction, and surface area analysis reveals that (i) particle morphology evolves from spherical to flattened disk-like particles; while the (ii) crystallite size decreases from several microns to less thanmore » 100 nm and (iii) dislocation density increases with increased cryomilling time. Hydrogen absorption and desorption isotherms as well as the time scales for absorption were measured for cryomilled Pd-10Rh, and correlated with observed microstructural changes induced by the cryomilling process. In short, as the microstructure of the Pd-10Rh alloy is refined by cryomilling: (i) the maximum hydrogen concentration in the α-phase increases, (ii) the pressure plateau becomes flatter, and (iii) the equilibrium hydrogen capacity at 760 Torr increases. In addition, the rate of hydrogen absorption was reduced by an order of magnitude compared to non-cryomilled (atomized) powder.« less

Magnetic, Mössbauer and optical spectroscopic properties of the AFe3O(PO4)3 (A = Ca, Sr, Pb) series of powder compounds

NASA Astrophysics Data System (ADS)

El Hafid, Hassan; Velázquez, Matias; El Jazouli, Abdelaziz; Wattiaux, Alain; Carlier, Dany; Decourt, Rodolphe; Couzi, Michel; Goldner, Philippe; Delmas, Claude

2014-10-01

AFe3O(PO4)3 (A = Ca, Sr and Pb) powder compounds were studied by means of X-ray diffraction (XRD), electron-probe microanalysis (EPMA) coupled with wavelength dispersion spectroscopy (WDS), Raman and diffuse reflectance spectroscopies, specific heat and magnetic properties measurements. Magnetization, magnetic susceptibility and specific heat measurements carried out on AFe3O(PO4)3 (A = Sr, Ca and Pb) powders firmly establish a series of three ferromagnetic (FM)-like second order phase transitions spanned over the 32-8 K temperature range. Room temperature Mössbauer spectroscopy and associated DFT calculations confirm the existence of three crystallographically non equivalent Fe3+ sites in the three compounds. Mössbauer spectra recorded as a function of temperature in the PbFe3O(PO4)3 compound also establishes the occurrence of two purely magnetic and reversible phase transitions at 32 and 10 K. Diffuse reflectance measurements reveal two broad absorption bands at 1047 and 837 nm, in both PbFe3O(PO4)3 and SrFe3O(PO4)3 powders, with peak cross sections ∼10-20 cm2 typical of spin-forbidden and forced electric dipole intraconfigurational transitions.

One-Step Hydrothermal Synthesis of Zeolite X Powder from Natural Low-Grade Diatomite.

PubMed

Yao, Guangyuan; Lei, Jingjing; Zhang, Xiaoyu; Sun, Zhiming; Zheng, Shuilin

2018-05-28

Zeolite X powder was synthesized using natural low-grade diatomite as the main source of Si but only as a partial source of Al via a simple and green hydrothermal method. The microstructure and surface properties of the obtained samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), wavelength dispersive X-ray fluorescence (XRF), calcium ion exchange capacity (CEC), thermogravimetric-differential thermal (TG-DTA) analysis, and N₂ adsorption-desorption technique. The influence of various synthesis factors, including aging time and temperature, crystallization time and temperature, Na₂O/SiO₂ and H₂O/Na₂O ratio on the CEC of zeolite, were systematically investigated. The as-synthesized zeolite X with binary meso-microporous structure possessed remarkable thermal stability, high calcium ion exchange capacity of 248 mg/g and large surface area of 453 m²/g. In addition, the calcium ion exchange capacity of zeolite X was found to be mainly determined by the crystallization degree. In conclusion, the synthesized zeolite X using diatomite as a cost-effective raw material in this study has great potential for industrial application such as catalyst support and adsorbent.

Effect of Eu-doping on optical, structural and morphological properties of BaI2·nH2O powders

NASA Astrophysics Data System (ADS)

Salamakha, T.; Buryi, M.; Tratsiak, Y.

2018-04-01

The two-step approach to the Eu2+ doped BaI2·nH2O powders synthesis in Ar atmosphere from precursors containing different concentration of Eu3+ ions is reported. According to X-ray diffraction analysis the powders mainly consist of BaI2·2H2O phase. Their morphological, structural and luminescent properties depend on the Eu-ions concentration. The luminescence spectra are composed of broad and strong emission band peaking at 420 nm, which was related to the Eu2+ 5d-4f transition. Its intensity reaches maximum in the 2 at. % Eu2+ doped sample. Detailed analysis of the measured electron paramagnetic resonance spectra in the samples with different doping level confirms them belong to the Eu2+ ions substituting for the regular Ba2+ site in the BaI2 lattice. A sample exposed to the 330 nm UV irradiation exhibited an increase of the Eu2+ spectral intensity occurred exclusively due to the Eu3+ to Eu2+ transformation. No other signals either prior to or after the irradiation which might be attributed to the ions resided in e.g., interstitial positions or in any secondary phases were observed. Possible mechanisms of the Eu3+ stabilization in the host lattice with only divalent cation sites during the synthesis without additional treatment in reducing atmosphere are discussed as well.

Aerosolization properties, surface composition and physical state of spray-dried protein powders.

PubMed

Bosquillon, Cynthia; Rouxhet, Paul G; Ahimou, François; Simon, Denis; Culot, Christine; Préat, Véronique; Vanbever, Rita

2004-10-19

Powder aerosols made of albumin, dipalmitoylphosphatidylcholine (DPPC) and a protein stabilizer (lactose, trehalose or mannitol) were prepared by spray-drying and analyzed for aerodynamic behavior, surface composition and physical state. The powders exited a Spinhaler inhaler as particle aggregates, the size of which depending on composition, spray-drying parameters and airflow rate. However, due to low bulk powder tap density (<0.15 g/cm3), the aerodynamic size of a large fraction of aggregates remained respirable (<5 microm). Fine particle fractions ranged between 21% and 41% in an Andersen cascade impactor operated at 28.3 l/min, with mannitol and lactose providing the most cohesive and free-flowing powders, respectively. Particle surface analysis by X-ray photoelectron spectroscopy (XPS) revealed a surface enrichment with DPPC relative to albumin for powders prepared under certain spray-drying conditions. DPPC self-organized in a gel phase in the particle and no sugar or mannitol crystals were detected by X-ray diffraction. Water sorption isotherms showed that albumin protected lactose from moisture-induced crystallization. In conclusion, a proper combination of composition and spray-drying parameters allowed to obtain dry powders with elevated fine particle fractions (FPFs) and a physical environment favorable to protein stability.

The effect of ultrasonic irradiation on the crystallinity of nano-hydroxyapatite produced via the wet chemical method.

PubMed

Barbosa, Michelle C; Messmer, Nigel R; Brazil, Tayra R; Marciano, Fernanda R; Lobo, Anderson O

2013-07-01

Nanohydroxyapatite (nHAp) powders were produced via aqueous precipitation by adopting four different experimental conditions, assisted or non-assisted by ultrasound irradiation (UI). The nHAp powders were characterized by X-ray diffraction, energy-dispersive X-ray fluorescence, Raman and attenuated total reflection Fourier transform infrared spectroscopies, which showed typical surface chemical compositions of nHAp. Analysis found strong connections between UI and the crystallization process, crystal growth properties, as well as correlations between calcination and substitution reactions. Copyright © 2013 Elsevier B.V. All rights reserved.

Application of ultra-small-angle X-ray scattering / X-ray photon correlation spectroscopy to relate equilibrium or non-equilibrium dynamics to microstructure

NASA Astrophysics Data System (ADS)

Allen, Andrew; Zhang, Fan; Levine, Lyle; Ilavsky, Jan

2013-03-01

Ultra-small-angle X-ray scattering (USAXS) can probe microstructures over the nanometer-to-micrometer scale range. Through use of a small instrument entrance slit, X-ray photon correlation spectroscopy (XPCS) exploits the partial coherence of an X-ray synchrotron undulator beam to provide unprecedented sensitivity to the dynamics of microstructural change. In USAXS/XPCS studies, the dynamics of local structures in a scale range of 100 nm to 1000 nm can be related to an overall hierarchical microstructure extending from 1 nm to more than 1000 nm. Using a point-detection scintillator mode, the equilibrium dynamics at ambient temperature of small particles (which move more slowly than nanoparticles) in aqueous suspension have been quantified directly for the first time. Using a USAXS-XPCS scanning mode for non-equilibrium dynamics incipient processes within dental composites have been elucidated, prior to effects becoming detectable using any other technique. Use of the Advanced Photon Source, an Office of Science User Facility operated for the United States Department of Energy (U.S. DOE) Office of Science by Argonne National Laboratory, was supported by the U.S. DOE under Contract No. DE-AC02-06CH11357.

Structural and photoluminescence investigations of Sm{sup 3+} doped BaY{sub 2}ZnO{sub 5} nanophosphors

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

Chahar, Sangeeta; Taxak, V.B.; Dalal, Mandeep

2016-05-15

Highlights: • BaY{sub 2(1−x)}Sm{sub 2x}ZnO{sub 5} nanophosphors have been synthesized via solution combustion. • The nanophosphors have been characterized by XRD, TEM and PL spectroscopy. • The crystal structure reveals influence of doping on lattice parameters. • This nanophosphor executes orange–red emission under near UV excitation. - Abstract: BaY{sub 2}ZnO{sub 5}:Sm{sup 3+} nanophosphor was successfully synthesized using solution combustion process. XRD and photoluminescence (PL) techniques were used to analyze the structural and photoluminescence properties. Morphological study of the thermally stable powder was carried out using transmission electron microscope (TEM). Rietveld refinement technique has been used to analyze the samples qualitativelymore » as well as quantitatively. X-Ray diffraction analysis confirms that the highly crystalline single phased Sm{sup 3+} doped BaY{sub 2}ZnO{sub 5} nanophosphor crystallizes in orthorhombic lattice with Pbnm space group. The average particle size lies in the range 80–90 nm with spherical morphology. The photoluminescence excitation at 411 nm yields an intense orange–red emission centered at 610 nm due to {sup 4}G{sub 5/2}–{sup 6}H{sub 7/2} transition. The concentration dependent luminescent behavior of BaY{sub 2(1−x)}Sm{sub 2x}ZnO{sub 5} nanophosphor shows that the optimum concentration for best luminescence is 3 mol%. These results indicate that these nanophosphors find potential applications in the field of phosphor-converted white LED systems.« less

Thiazole derivative-modified upconversion nanoparticles for Hg2+ detection in living cells

NASA Astrophysics Data System (ADS)

Gu, Bin; Zhou, Yi; Zhang, Xiao; Liu, Xiaowang; Zhang, Yuhai; Marks, Robert; Zhang, Hua; Liu, Xiaogang; Zhang, Qichun

2015-12-01

Mercury ion (Hg2+) is an extremely toxic ion, which will accumulate in human bodies and cause severe nervous system damage. Therefore, the sensitive and efficient monitoring of Hg2+ in human bodies is of great importance. Upconversion nanoparticle (UCNPs) based nano probes exhibit no autofluorescence, deep penetration depth and chemical stability in biological samples, as well as a large anti-stokes shift. In this study, we have developed thiazole-derivative-functionalized UCNPs, and employed an upconversion emission intensity ratio of 540 nm to 803 nm (I540/I803) as a ratiometric signal to detect Hg2+ in living cells showing excellent photo stability and high selectivity. Our nano probe was characterized using transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD). The low cytotoxicity of our probe was confirmed by an MTT assay and the UCL test in HeLa cells was carried out by confocal microscopy. Our results demonstrated that organic-dye-functionalized UCNPs should be a good strategy for detecting toxic metal ions when studying cellular biosystems.Mercury ion (Hg2+) is an extremely toxic ion, which will accumulate in human bodies and cause severe nervous system damage. Therefore, the sensitive and efficient monitoring of Hg2+ in human bodies is of great importance. Upconversion nanoparticle (UCNPs) based nano probes exhibit no autofluorescence, deep penetration depth and chemical stability in biological samples, as well as a large anti-stokes shift. In this study, we have developed thiazole-derivative-functionalized UCNPs, and employed an upconversion emission intensity ratio of 540 nm to 803 nm (I540/I803) as a ratiometric signal to detect Hg2+ in living cells showing excellent photo stability and high selectivity. Our nano probe was characterized using transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD). The low cytotoxicity of our probe was confirmed by an MTT assay and the UCL test in HeLa cells was carried out by confocal microscopy. Our results demonstrated that organic-dye-functionalized UCNPs should be a good strategy for detecting toxic metal ions when studying cellular biosystems. Electronic supplementary information (ESI) available: NMR, MALDI-TOF MS spectra, etc. See DOI: 10.1039/c5nr05286f

Electron density distribution and disordered crystal structure of 15R-SiAlON, SiAl{sub 4}O{sub 2}N{sub 4}

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

Banno, Hiroki; Hanai, Takaaki; Asaka, Toru

2014-03-15

The crystal structure of SiAl{sub 4}O{sub 2}N{sub 4} was characterized by laboratory X-ray powder diffraction (CuKα{sub 1}). The title compound is trigonal with space group R3-bar m. The hexagonal unit-cell dimensions (Z=3) are a=0.301332(3) nm, c=4.18616(4) nm and V=0.3291825(5) nm{sup 3}. The initial structural model was successfully derived by the charge-flipping method and further refined by the Rietveld method. The final structural model showed the positional disordering of one of the three (Si,Al) sites. The maximum-entropy method-based pattern fitting (MPF) method was used to confirm the validity of the split-atom model, in which conventional structure bias caused by assuming intensitymore » partitioning was minimized. The reliability indices calculated from the MPF were R{sub wp}=5.05%, S (=R{sub wp}/R{sub e})=1.21, R{sub p}=3.77%, R{sub B}=1.29% and R{sub F}=1.01%. The disordered crystal structure was successfully described by overlapping three types of domains with ordered atom arrangements. The distribution of atomic positions in one of the three types of domains can be achieved in the space group R3-bar m. The atom arrangements in the other two types of domains are noncentrosymmetrical with the space group R3m. These two structural configurations are related by the pseudo-symmetry inversion. -- Graphical abstract: A bird's eye view of electron densities up to 75.3% (0.133 nm{sup −3}) of the maximum on the plane parallel to (110) with the corresponding atomic arrangements of SiAl{sub 4}O{sub 2}N{sub 4}. Highlights: • Crystal structure of SiAl{sub 4}O{sub 2}N{sub 4} is determined by laboratory X-ray powder diffraction. • The atom arrangements are represented by the split-atom model. • The maximum-entropy method-based pattern fitting method is used to confirm the validity of the model. • The disordered structure is described by overlapping three types of domains with ordered atom arrangements.« less

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

Ayob, M. T. M.; Ahmad, A. F.; Mohd, H. M. K.

Coral-spherical-shaped of copper oxide nanoparticles have been successfully synthesized with different ratios of triethanolamine:ethylenediamine surfactant under ultrasonic condition. By controlling the amplitude of the ultrasonic radiation and concentration of metal salt precursors and surfactant, the formation of CuO nanospheres was obtained. Energy dispersive X-ray spectrum confirmed that Cu and O are the only elementary components present with a ratio of approximately 1:1. Furthermore, X-ray powder diffraction spectra for all the examined ratios of CuO showed well crystalline structures. UV-Vis spectroscopy was utilized to estimate the band gap energies of the CuO nanoparticles produced, which were found to be in themore » range of 2.74 eV to 2.95 eV. The field emission scanning electron micrographs of these nanospheres showed that their dimensions were in the range of 5-30 nm. These results indicate that the triethanolamine:ethylenediamine ratio plays an important role in the formation of different sized CuO nanoparticles, displaying a decrement in particle size with the increment in amount of triethanolamine ratios. This might be the key to synthesizing nanoparticles with specific sizes for various applications.« less

A novel approach to synthesize, studies of structural and electrical characteristic of Bi(Ni0.30Ti0.30Fe0.40)O3 nanoceramics

NASA Astrophysics Data System (ADS)

Kumar, Nitin; Shukla, Alok

2018-03-01

In this study, we report a novel approach to synthesize the Bi(Ni0.30Ti0.30Fe0.40)O3 [arbitration BNTF30/40] nanoceramics by standard ceramic method at an ambient temperature of 1013 K. Carbonates and oxides powder were utilised as a raw materials in an appropriate stoichiometric amounts. X-ray diffraction pattern assigned that the BNTF30/40 sample presents a single phase of orthorhombic symmetry. The crystallite size obtain from X-ray data suggests the formation of BNTF30/40 nanoceramics in the range between 20 to 45 nm. Bulk density of the prepared pallets were measured and found to be more than 94 percent. The basic characterization tools have been used respectively with Field Emission Scanning Electron Microscope and Spectroscopy based techniques to obtain the correlation between surface morphology and electrical characteristic of specimen sample. Electrical characteristic of the as- synthesized material was studied in the experimental temperature range between RT to 623 K at different operated frequency (25 kHz - 500 kHz).

Synthesis and characterization of ZnO–CuO nanocomposites powder by modified perfume spray pyrolysis method and its antimicrobial investigation

NASA Astrophysics Data System (ADS)

Saravanakkumar, D.; Sivaranjani, S.; Kaviyarasu, K.; Ayeshamariam, A.; Ravikumar, B.; Pandiarajan, S.; Veeralakshmi, C.; Jayachandran, M.; Maaza, M.

2018-03-01

Pure ZnO, ZnO–CuO nanocomposites can be synthesized by using a modified perfume spray pyrolysis method (MSP). The crystallite size of the nanoparticles (NPs) has been observed by X-ray diffraction pattern and is nearly 36 nm. Morphological studies have been analyzed by using Field Emission Scanning Electron Microscopy (FESEM) and its elemental analysis was reported by Elemental X-ray Analysis (EDX); these studies confirmed that ZnO and CuO have hexagonal structure and monoclinic structure respectively. Fourier Transform Infrared (FTIR) spectra revealed that the presence of functional frequencies of ZnO and CuO were observed at 443 and 616 cm‑1. The average bandgap value at 3.25 eV using UV–vis spectra for the entitled composite has described a blue shift that has been observed here. The antibacterial study against both gram positive and negative bacteria has been studied by the disc diffusion method. To the best of our knowledge, it is the first report on ZnO–CuO nanocomposite synthesized by a modified perfume spray pyrolysis method.

Ligand exchange synthesis of organometallic Rh nanoparticles and application in explosive sensing

NASA Astrophysics Data System (ADS)

Srivastav, Amit K.; Agrawal, Bhavesh; Swami, Bhavya; Agrawal, Yadvendra K.; Maity, Prasenjit

2017-06-01

Alkyne {phenyl acetylene (PA) and 9-ethynylphenanthrene (EPT)}-ligated Rh nanoparticles ( 1 and 2, respectively) with mean diameter of 1.5 ± 0.2 nm were synthesized via a facile and high-yield biphasic ligand exchange protocol using similar sized ethylene glycol (EG)-stabilized Rh nanoparticles as precursors (EG:Rh). The synthesized organometallic Rh nanoparticles were convincingly characterized using several spectroscopic and microscopic techniques, e.g., Fourier transform infrared spectroscopy (FTIR), proton nuclear magnetic resonance (1H NMR), optical absorption spectroscopy (UV-Vis), photoluminescence spectroscopy (PL), powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscope (TEM). We propose that the syntheses mechanism relies on catalytic acetylenic (≡C-H, carbon-hydrogen) bond breaking by EG:Rh followed by strong metal-carbon bond formation with a vinyldiene (>C═C═M) motif. The obtained 1 and 2 showed luminescence property, which arises from ligand structure through intraparticle conjugation. Electron-rich phenanthrene-ligated Rh nanoparticles ( 2) showed good sensing performance for detection of electron deficient nitro-aromatic explosive molecules (NA) in solution phase through luminescence quenching method.

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.

Synthesis of TiO2 Nanoparticle and its phase Transition

NASA Astrophysics Data System (ADS)

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

2011-12-01

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

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO3 Ceramics Fabricated by Spark Plasma Sintering

PubMed Central

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-01-01

Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO3 ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO3 ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe3+ to Fe2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO3 ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage. PMID:28772626

Nanophase cobalt, nickel and zinc ferrites: synchrotron XAS study on the crystallite size dependence of metal distribution.

PubMed

Nordhei, Camilla; Ramstad, Astrid Lund; Nicholson, David G

2008-02-21

Nanophase cobalt, nickel and zinc ferrites, in which the crystallites are in the size range 4-25 nm, were synthesised by coprecipitation and subsequent annealing. X-Ray absorption spectroscopy using synchrotron radiation (supported by X-ray powder diffraction) was used to study the effects of particle size on the distributions of the metal atoms over the tetrahedral and octahedral sites of the spinel structure. Deviations from the bulk structure were found which are attributed to the significant influence of the surface on very small particles. Like the bulk material, nickel ferrite is an inverse spinel in the nanoregime, although the population of metals on the octahedral sites increases with decreasing particle size. Cobalt ferrite and zinc ferrite take the inverse and normal forms of the spinel structure respectively, but within the nanoregime both systems show similar trends in being partially inverted. Further, in zinc ferrite, unlike the normal bulk structure, the nanophase system involves mixed coordinations of zinc(ii) and iron(iii) consistent with increasing partial inversion with size.

The usability of ark clam shell (Anadara granosa) as calcium precursor to produce hydroxyapatite nanoparticle via wet chemical precipitate method in various sintering temperature.

PubMed

Khiri, Mohammad Zulhasif Ahmad; Matori, Khamirul Amin; Zainuddin, Norhazlin; Abdullah, Che Azurahanim Che; Alassan, Zarifah Nadakkavil; Baharuddin, Nur Fadilah; Zaid, Mohd Hafiz Mohd

2016-01-01

This paper reported the uses of ark clam shell calcium precursor in order to form hydroxyapatite (HA) via the wet chemical precipitation method. The main objective of this research is to acquire better understanding regarding the effect of sintering temperature in the fabrication of HA. Throughout experiment, the ratio of Ca:P were constantly controlled, between 1.67 and 2.00. The formation of HA at these ratio was confirmed by means of energy-dispersive X-ray spectroscopy analysis. In addition, the effect of sintering temperature on the formation of HA was observed using X-ray diffraction analysis, while the structural and morphology was determined by means of field emission scanning electron microscopy. The formation of HA nanoparticle was recorded (~35-69 nm) in the form of as-synthesize HA powder. The bonding compound appeared in the formation of HA was carried out using Fourier transform infrared spectroscopy such as biomaterials that are expected to find potential applications in orthopedic and biomedical industries .

Liquid Phase Plasma Synthesis of Iron Oxide Nanoparticles on Nitrogen-Doped Activated Carbon Resulting in Nanocomposite for Supercapacitor Applications.

PubMed

Lee, Heon; Lee, Won-June; Park, Young-Kwon; Ki, Seo Jin; Kim, Byung-Joo; Jung, Sang-Chul

2018-03-25

Iron oxide nanoparticles supported on nitrogen-doped activated carbon powder were synthesized using an innovative plasma-in-liquid method, called the liquid phase plasma (LPP) method. Nitrogen-doped carbon (NC) was prepared by a primary LPP reaction using an ammonium chloride reactant solution, and an iron oxide/NC composite (IONCC) was prepared by a secondary LPP reaction using an iron chloride reactant solution. The nitrogen component at 3.77 at. % formed uniformly over the activated carbon (AC) surface after a 1 h LPP reaction. Iron oxide nanoparticles, 40~100 nm in size, were impregnated homogeneously over the NC surface after the LPP reaction, and were identified as Fe₃O₄ by X-ray photoelectron spectroscopy and X-ray diffraction. NC and IONCCs exhibited pseudo-capacitive characteristics, and their specific capacitance and cycling stability were superior to those of bare AC. The nitrogen content on the NC surface increased the compatibility and charge transfer rate, and the composites containing iron oxide exhibited a lower equivalent series resistance.

Synthesis, characterization and thermodynamic study of carbon dioxide adsorption on akaganéite

DOE PAGES

Roque-Malherbe, R.; Lugo, F.; Rivera-Maldonado, C.; ...

2015-04-01

A mixture of akaganeite nanoparticles and sodium salts was synthesized and modi fied, first by washing, and then by Li exchange. The structural characterization of the produced materials was performed with: powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, thermogravimetric analysis, diffuse reflectance infrared Fourier transform spectrometry, Mossbauer spectros- € copy and magnetization measurements. Additionally low pressure nitrogen and high pressure carbon dioxide adsorption experiments were performed. The sum of the characterization information made possible to conclude that the produced akaganeite phases crystallized in a structure exhibiting the symmetry of the I2/m space group, where the measured equivalentmore » spherical diameter of the akaganeite crystallites yielded 9 nm, as well, the tested phases exhibited a standard behaviour under heating and displayed a superparamagnetic behaviour. Finally the high pressure carbon dioxide adsorption experiments demonstrated a pressure-responsive framework opening event due to a structural transformation of the adsorbent framework induced by the guest molecules. This fact opens new applications for akaganeite as a high pressure adsorbent.« less

Systematic investigations on fused π-system compounds of seven benzene rings prepared by photocyclization of diphenanthrylethenes.

PubMed

Fujino, Shota; Yamaji, Minoru; Okamoto, Hideki; Mutai, Toshiki; Yoshikawa, Isao; Houjou, Hirohiko; Tani, Fumito

2017-06-14

We studied the photoproducts of 1-(n-phenanthryl)-2-(m-phenanthryl)ethenes (nEm; n, m = 1, 3 and 9) for understanding photocyclization patterns based on NMR spectroscopy. The crystal structures of the photoproducts were analyzed by X-ray crystallography, and the photophysical features of the photocyclized molecules were investigated based on emission and transient absorption measurements. Phenanthrene derivatives substituted at the 1- and 3-positions were prepared for synthesizing nEm by photocyclization of stilbene derivatives. We obtained four types of primary photoproducts (n@m) from the corresponding nEm. Two of them were found to have racemic molecular structures in the single crystal determined by X-ray crystallography. Besides the primary photoproducts, two types of secondary photoproducts (n@mPP) were isolated. Fluorescence quantum yields and lifetimes of the obtained photoproducts were determined in solution whereas the definite fluorescence quantum yields were obtained in the powder. Observation of the triplet-triplet absorption spectra in solution by laser photolysis techniques showed that intersystem crossing to the triplet state competes with the fluorescence process.

Sub-500  nm hard x ray focusing by compound long kinoform lenses.

PubMed

Liao, Keliang; Liu, Jing; Liang, Hao; Wu, Xuehui; Zhang, Kai; Yuan, Qingxi; Yi, Futing; Sheng, Weifan

2016-01-01

The focusing performance of polymethyl methacrylate compound long kinoform lenses with 70 μm aperture and 19.5 mm focal length was characterized with 8 keV x rays using the knife-edge scan method at the 4W1A transmission x-ray microscope beamline of Beijing Synchrotron Radiation Facility. The experiment result shows a best FWHM focus size of 440 nm with 31% diffraction efficiency.

High throughput production of nanocomposite SiO x powders by plasma spray physical vapor deposition for negative electrode of lithium ion batteries.

PubMed

Homma, Keiichiro; Kambara, Makoto; Yoshida, Toyonobu

2014-04-01

Nanocomposite Si/SiO x powders were produced by plasma spray physical vapor deposition (PS-PVD) at a material throughput of 480 g h -1 . The powders are fundamentally an aggregate of primary ∼20 nm particles, which are composed of a crystalline Si core and SiO x shell structure. This is made possible by complete evaporation of raw SiO powders and subsequent rapid condensation of high temperature SiO x vapors, followed by disproportionation reaction of nucleated SiO x nanoparticles. When CH 4 was additionally introduced to the PS-PVD, the volume of the core Si increases while reducing potentially the SiO x shell thickness as a result of the enhanced SiO reduction, although an unfavorable SiC phase emerges when the C/Si molar ratio is greater than 1. As a result of the increased amount of Si active material and reduced source for irreversible capacity, half-cell batteries made of PS-PVD powders with C/Si = 0.25 have exhibited improved initial efficiency and maintenance of capacity as high as 1000 mAh g -1 after 100 cycles at the same time.

Synthesis of metal-fluoride nanoparticles supported on thermally reduced graphite oxide.

PubMed

Schmitz, Alexa; Schütte, Kai; Ilievski, Vesko; Barthel, Juri; Burk, Laura; Mülhaupt, Rolf; Yue, Junpei; Smarsly, Bernd; Janiak, Christoph

2017-01-01

Metal-fluoride nanoparticles, (MF x -NPs) with M = Fe, Co, Pr, Eu, supported on different types of thermally reduced graphite oxide (TRGO) were obtained by microwave-assisted thermal decomposition of transition-metal amidinates, (M{MeC[N(iPr)] 2 } n ) or [M(AMD) n ] with M = Fe(II), Co(II), Pr(III), and tris(2,2,6,6-tetramethyl-3,5-heptanedionato)europium, Eu(dpm) 3 , in the presence of TRGO in the ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF 4 ]). The crystalline phases of the metal fluorides synthesized in [BMIm][BF 4 ] were identified by powder X-ray diffraction (PXRD) to be MF 2 for M = Fe, Co and MF 3 for M = Eu, Pr. The diameters and size distributions of MF x @TRGO were from (6 ± 2) to (102 ± 41) nm. Energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) were used for further characterization of the MF x -NPs. Electrochemical investigations of the FeF 2 -NPs@TRGO as cathode material for lithium-ion batteries were evaluated by galvanostatic charge/discharge profiles. The results indicate that the FeF 2 -NPs@TRGO as cathode material can present a specific capacity of 500 mAh/g at a current density of 50 mA/g, including a significant interfacial charge storage contribution. The obtained nanomaterials show a good rate capacity as well (220 mAh/g and 130 mAh/g) at a current density of 200 and 500 mA/g, respectively.