Advantages of TOF-SIMS analysis of hydroxyapatite and fluorapatite in comparison with XRD, HR-TEM and FT-IR.

PubMed

Okazaki, Masayuki; Hirata, Isao; Matsumoto, Takuya; Takahashi, Junzo

2005-12-01

The chemical analysis of hydroxyapatite and fluorapatite was carried out using time-of-flight secondary ion mass spectrometry (TOF-SIMS). Hydroxyapatite and fluorapatite were synthesized at 80 +/- 1 degrees C and pH 7.4 +/- 0.2. Fluorapatite was better crystallized, with its (300) reflection shifted to a slightly higher angle. High-resolution transmission electron microscopy clearly revealed a typical, regular hexagonal cross section perpendicular to the c-axis for fluorapatite and a flattened hexagonal cross section for hydroxyapatite. FT-IR spectra of fluorapatite confirmed the absence of OH absorption peak--which was seen in hydroxyapatite at about 3570 cm(-1). TOF-SIMS mass spectra showed a peak at 40 amu due to calcium. In addition, a peak at 19 amu due to fluorine could be clearly seen, although the intensities of PO, PO2, and PO3 were very low. It was confirmed that TOF-SIMS clearly showed the differences between positive and negative mass spectra of hydroxyapatite and fluorapatite, especially for F-. We concluded that TOF-SIMS exhibited distinct advantages compared with other methods of analysis.

Coupling Graphene Sheets with Magnetic Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

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

Microwave assisted facile green synthesis of silver and gold nanocatalysts using the leaf extract of Aerva lanata.

PubMed

Joseph, Siby; Mathew, Beena

2015-02-05

Herein, we report a simple microwave assisted method for the green synthesis of silver and gold nanoparticles by the reduction of aqueous metal salt solutions using leaf extract of the medicinal plant Aerva lanata. UV-vis., FTIR, XRD, and HR-TEM studies were conducted to assure the formation of nanoparticles. XRD studies clearly confirmed the crystalline nature of the synthesized nanoparticles. From the HR-TEM images, the silver nanoparticles (AgNPs) were found to be more or less spherical and gold nanoparticles (AuNPs) were observed to be of different morphology with an average diameter of 18.62nm for silver and 17.97nm for gold nanoparticles. In order to evaluate the effect of microwave heating upon rate of formation, the synthesis was also conducted under ambient condition without the assistance of microwave radiation and the former method was found to be much faster than the later. The synthesized nanoparticles were used as nanocatalysts in the reduction of 4-nitrophenol to 4-aminophenol by NaBH4. Copyright © 2014 Elsevier B.V. All rights reserved.

Swelling induced by alpha decay in monazite and zirconolite ceramics: A XRD and TEM comparative study

NASA Astrophysics Data System (ADS)

Deschanels, X.; Seydoux-Guillaume, A. M.; Magnin, V.; Mesbah, A.; Tribet, M.; Moloney, M. P.; Serruys, Y.; Peuget, S.

2014-05-01

Zirconolite and monazite matrices are potential ceramics for the containment of actinides (Np, Cm, Am, Pu) which are produced over the reprocessing of spent nuclear fuel. Actinides decay mainly through the emission of alpha particles, which in turn causes most ceramics to undergo structural and textural changes (amorphization and/or swelling). In order to study the effects of alpha decays on the above mentioned ceramics two parallel approaches were set up. The first involved the use of an external irradiation source, Au, which allowed the deposited recoil energy to be simulated. The second was based on short-lived actinide doping with 238Pu, (i.e. an internal source), via the incorporation of plutonium oxide into both the monazite and zirconolite structures during synthesis. In both types of irradiation experiments, the zirconolite samples became amorphous at room temperature with damage close to 0.3 dpa; corresponding to a critical dose of 4 × 1018 α g-1 (i.e. ∼1.3 × 1021 keV cm-3). Both zirconolite samples also showed the same degree of macroscopic swelling at saturation (∼6%), with ballistic processes being the predominant damaging effect. In the case of the monazite however, the macroscopic swelling and amorphization were dependent on the nature of the irradiation. Externally, (Au), irradiated samples became amorphous while also demonstrating a saturation swelling of up to 8%. In contrast to this, the swelling of the 238Pu doped samples was much smaller at ∼1%. Also, unlike the externally (Au) irradiated monazite these 238Pu doped samples remained crystalline up to 7.5 × 1018 α g-1 (0.8 dpa). XRD, TEM and swelling measurements were used to fully characterize and interpret this behavior. The low swelling and the conservation of the crystalline state of 238Pu doped monazite samples indicates that alpha annealing took place within this material.

Quantitative XRD analysis of {110} twin density in biotic aragonites.

PubMed

Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Nagasawa, Hiromichi; Kogure, Toshihiro

2012-12-01

{110} Twin densities in biotic aragonite have been estimated quantitatively from the peak widths of specific reflections in powder X-ray diffraction (XRD) patterns, as well as direct confirmation of the twins using transmission electron microscopy (TEM). Influence of the twin density on the peak widths in the XRD pattern was simulated using DIFFaX program, regarding (110) twin as interstratification of two types of aragonite unit layers with mirrored relationship. The simulation suggested that the twin density can be estimated from the difference of the peak widths between 111 and 021, or between 221 and 211 reflections. Biotic aragonite in the crossed-lamellar microstructure (three species) and nacreous microstructure (four species) of molluscan shells, fish otoliths (two species), and a coral were investigated. The XRD analyses indicated that aragonite crystals in the crossed-lamellar microstructure of the three species contain high density of the twins, which is consistent with the TEM examination. On the other hand, aragonite in the nacre of the four species showed almost no difference of the peak widths between the paired reflections, indicating low twin densities. The results for the fish otoliths were varied between the species. Such variation of the twin density in biotic aragonites may reflect different schemes of crystal growth in biomineralization. Copyright © 2012 Elsevier Inc. All rights reserved.

Coupling Graphene Sheets with Iron Oxide Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

of highly oriented pyrolytic graphite ( HOPG ) flake. Two electrode system containing platinum as counter electrode and HOPG as working electrode is... XRD ) patterns of the HOPG , exfoliated graphene, PyDop1-ɤ-Fe2O3 and PyDop1-ɤ-Fe2O3-graphene are given in Figure 1e. HOPG show a very sharp diffraction...atoms arranged in hexagonal pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG

Chemical synthesis of hierarchical NiCo2S4 nanosheets like nanostructure on flexible foil for a high performance supercapacitor.

PubMed

Kim, D -Y; Ghodake, G S; Maile, N C; Kadam, A A; Sung Lee, Dae; Fulari, V J; Shinde, S K

2017-08-29

In this study, hierarchical interconnected nickel cobalt sulfide (NiCo 2 S 4 ) nanosheets were effectively deposited on a flexible stainless steel foil by the chemical bath deposition method (CBD) for high-performance supercapacitor applications. The resulting NiCo 2 S 4 sample was characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), and electrochemical measurements. XRD and X-ray photoelectron spectroscopy (XPS) results confirmed the formation of the ternary NiCo 2 S 4 sample with a pure cubic phase. FE-SEM and HR-TEM revealed that the entire foil surface was fully covered with the interconnected nanosheets like surface morphology. The NiCo 2 S 4 nanosheets demonstrated impressive electrochemical characteristics with a specific capacitance of 1155 F g -1 at 10 mV s -1 and superior cycling stability (95% capacity after 2000 cycles). These electrochemical characteristics could be attributed to the higher active area and higher conductivity of the sample. The results demonstrated that the interconnected NiCo 2 S 4 nanosheets are promising as electrodes for supercapacitor and energy storage applications.

Improvement of the piezoelectric properties in (K,Na)NbO3-based lead-free piezoelectric ceramic with two-phase co-existing state

NASA Astrophysics Data System (ADS)

Yamada, H.; Matsuoka, T.; Kozuka, H.; Yamazaki, M.; Ohbayashi, K.; Ida, T.

2015-06-01

Two phases of (K,Na)NbO3 (KNN) co-exist in a KNN-based composite lead-free piezoelectric ceramic 0.910(K1-xNax)0.86Ca0.04Li0.02Nb0.85O3-δ-0.042K0.85Ti0.85Nb1.15O5-0.036BaZrO3-0.0016Co3O4- 0.0025Fe2O3-0.0069ZnO system, over a wide range of Na fractions, where 0.56 ≤ x ≤ 0.75. The crystal systems of the two KNN phases are identified to tetragonal and orthorhombic by analyzing the synchrotron powder X-ray diffraction (XRD) data, high-resolution transmission electron microscopy (HR-TEM), and selected-area electron diffraction (SAD). In the range 0.33 ≤ x ≤ 0.50, the main component of the composite system is found to be single-phase KNN with a tetragonal structure. Granular nanodomains of the orthorhombic phase dispersed in the tetragonal matrix have been identified by HR-TEM and SAD for 0.56 ≤ x ≤ 0.75. Only a trace amount of the orthorhombic phase has been found in the SAD patterns at the composition x = 0.56. However, the number of orthorhombic nanodomains gradually increases with increasing Na content up to x < 0.75, as observed from the HR-TEM images. An abrupt increase and agglomeration of the nanodomains are observed at x = 0.75, where weak diffraction peaks of the orthorhombic phase have also become detectable from the XRD data. The maximum value of the electromechanical coupling coefficient, kp = 0.56, has been observed at the composition x = 0.56.

Structure and properties of electrodeposited nanocrystalline Ni and Ni-Fe alloy continuous foils

NASA Astrophysics Data System (ADS)

Giallonardo, Jason Derek

This research work presents the first comprehensive study on nanocrystalline materials produced in bulk quantities using a novel continuous electrodeposition process. A series of nanocrystalline Ni and Ni-Fe alloy continuous foils were produced and an intensive investigation into their structure and various properties was carried out. High-resolution transmission electron microscopy (HR-TEM) revealed the presence of local strain at high and low angle, and twin boundaries. The cause for these local strains was explained based on the interpretation of non-equilibrium grain boundary structures that result when conditions of compatibility are not satisfied. HR-TEM also revealed the presence of twin faults of the growth type, or "growth faults", which increased in density with the addition of Fe. This observation was found to be consistent with a corresponding increase in the growth fault probabilities determined quantitatively using X-ray diffraction (XRD) pattern analysis. Hardness and Young's modulus were measured by nanoindentation. Hardness followed the regular Hall-Petch behaviour down to a grain size of 20 nm after which an inverse trend was observed. Young's modulus was slightly reduced at grain sizes less than 20 nm and found to be affected by texture. Microstrain based on XRD line broadening was measured for these materials and found to increase primarily with a decrease in grain size or an increase in intercrystal defect density (i.e., grain boundaries and triple junctions). This microstrain is associated with the local strains observed at grain boundaries in the HR-TEM image analysis. A contribution to microstrain from the presence of growth faults in the nanocrystalline Ni-Fe alloys was also noted. The macrostresses for these materials were determined from strain measurements using a two-dimensional XRD technique. At grain sizes less than 20 nm, there was a sharp increase in compressive macrostresses which was also owed to the corresponding increase in

Facile synthesis of Co3O4 hexagonal plates by flux method

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Carbon-encapsulated cobalt nanoparticles: synthesis, properties, and magnetic particle hyperthermia efficiency

NASA Astrophysics Data System (ADS)

Kotoulas, A.; Dendrinou-Samara, C.; Sarafidis, C.; Kehagias, Th.; Arvanitidis, J.; Vourlias, G.; Angelakeris, M.; Kalogirou, Orestis

2017-12-01

A facile and low-cost method for structuring carbon-encapsulated cobalt nanoparticles (Co@C) is presented. Three samples were solvothermally prepared in one step at 220 °C and one in two steps at 200 °C. Three different polyols such as propylene glycol, triethylene glycol, and tetraethylene glycol were used as carbon sources, solvents, and reducing agents. The samples were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. Concerning the crystal structure of the particles, a mixture of hcp/ fcc Co phases was obtained in three of the samples, independently of the polyol used. The coexistence of cubic and hexagonal phases was revealed both from XRD and high-resolution TEM (HRTEM). The formation of the cubic fcc structure, despite the relatively low reaction temperature, is attributed to the role of the interface between carbon coating and metallic core. The presence of carbon coating was demonstrated by Raman spectrometry, exhibiting the characteristic D and G graphitic bands, and by HRTEM observations. All samples showed ferromagnetic behavior with saturation magnetization up to 158 emu/g and coercivity up to 206 Oe. From the magnetic particle hyperthermia measurements recorded at a frequency of 765 kHz, a maximum SLP value of 241 W/g was obtained.

Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

2016-10-01

Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV-vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Spinel NixZn1-xFe2O4 (0.0 ≤ x ≤ 1.0) nano-photocatalysts: Synthesis, characterization and photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Padmapriya, G.; Manikandan, A.; Krishnasamy, V.; Jaganathan, Saravana Kumar; Antony, S. Arul

2016-09-01

Spinel NixZn1-xFe2O4 (x = 0.0 to 1.0) nanoparticles were successfully synthesized by a simple microwave combustion method (MCM) using metal nitrates as raw materials and glycine as the fuel. The structural, morphological and opto-magnetic properties of the spinel NixZn1-xFe2O4 ferrites were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray (EDX) spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) pattern, UV-Visible diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). Powder XRD, and EDX analysis was confirmed the formation of pure phase of spinel ferrites. HR-SEM and HR-TEM analysis was confirmed the formation of sphere like-particle morphology of the samples with smaller agglomeration. VSM analysis clearly showed the superparamagnetic and ferromagnetic nature of the samples. The Ms value is 3.851 emu/g for undoped ZnFe2O4 sample and it increased with increase in Ni content. Photo-catalytic degradation (PCD) of methylene blue (MB) dye using the samples were carried out and observed good PCD results.

[Hydrothermal synthesis and luminescence of one-dimensional Mn(2+)-doped CdS nanocrystals].

PubMed

Yuan, Qiu-Li; Zhao, Jin-Tao; Nie, Qiu-Lin

2007-06-01

One-dimensional Mn(2+)-doped CdS nanocrystals were synthesized by the hydrothermal route. The products were characterized by SEM, EDS, XRD, TEM, HRTEM and PL, respectively. The results revealed that dopant Mn2+ completely substitutes Cd2+ in CdS nanocrystals, and the product was of good crystallite. Further more, a complete suppression of the emission from surface states at room temperature when doping with ions Mn2+ has been observed.

Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

PubMed

Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

2008-01-01

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

Novel Crystalline SiO2 Nanoparticles via Annelids Bioprocessing of Agro-Industrial Wastes

PubMed Central

2010-01-01

The synthesis of nanoparticles silica oxide from rice husk, sugar cane bagasse and coffee husk, by employing vermicompost with annelids (Eisenia foetida) is reported. The product (humus) is calcinated and extracted to recover the crystalline nanoparticles. X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and dynamic light scattering (DLS) show that the biotransformation allows creating specific crystalline phases, since equivalent particles synthesized without biotransformation are bigger and with different crystalline structure. PMID:20802789

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

NASA Astrophysics Data System (ADS)

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

2006-11-01

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

Formation of crystalline Zn-Al layered double hydroxide precipitates on γ-alumina: the role of mineral dissolution.

PubMed

Li, Wei; Livi, Kenneth J T; Xu, Wenqian; Siebecker, Matthew G; Wang, Yujun; Phillips, Brian L; Sparks, Donald L

2012-11-06

To better understand the sequestration of toxic metals such as nickel (Ni), zinc (Zn), and cobalt (Co) as layered double hydroxide (LDH) phases in soils, we systematically examined the presence of Al and the role of mineral dissolution during Zn sorption/precipitation on γ-Al(2)O(3) (γ-alumina) at pH 7.5 using extended X-ray absorption fine structure spectroscopy (EXAFS), high-resolution transmission electron microscopy (HR-TEM), synchrotron-radiation powder X-ray diffraction (SR-XRD), and (27)Al solid-state NMR. The EXAFS analysis indicates the formation of Zn-Al LDH precipitates at Zn concentration ≥0.4 mM, and both HR-TEM and SR-XRD reveal that these precipitates are crystalline. These precipitates yield a small shoulder at δ(Al-27) = +12.5 ppm in the (27)Al solid-state NMR spectra, consistent with the mixed octahedral Al/Zn chemical environment in typical Zn-Al LDHs. The NMR analysis provides direct evidence for the existence of Al in the precipitates and the migration from the dissolution of γ-alumina substrate. To further address this issue, we compared the Zn sorption mechanism on a series of Al (hydr)oxides with similar chemical composition but differing dissolubility using EXAFS and TEM. These results suggest that, under the same experimental conditions, Zn-Al LDH precipitates formed on γ-alumina and corundum but not on less soluble minerals such as bayerite, boehmite, and gibbsite, which point outs that substrate mineral surface dissolution plays an important role in the formation of Zn-Al LDH precipitates.

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

PubMed

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

2018-06-01

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

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

Yamada, H., E-mail: hide-yamada@mg.ngkntk.co.jp; Matsuoka, T.; Kozuka, H.

Two phases of (K,Na)NbO{sub 3} (KNN) co-exist in a KNN-based composite lead-free piezoelectric ceramic 0.910(K{sub 1−x}Na{sub x}){sub 0.86}Ca{sub 0.04}Li{sub 0.02}Nb{sub 0.85}O{sub 3−δ}–0.042K{sub 0.85}Ti{sub 0.85}Nb{sub 1.15}O{sub 5} –0.036BaZrO{sub 3}–0.0016Co{sub 3}O{sub 4}– 0.0025Fe{sub 2}O{sub 3}–0.0069ZnO system, over a wide range of Na fractions, where 0.56 ≤ x ≤ 0.75. The crystal systems of the two KNN phases are identified to tetragonal and orthorhombic by analyzing the synchrotron powder X-ray diffraction (XRD) data, high-resolution transmission electron microscopy (HR-TEM), and selected-area electron diffraction (SAD). In the range 0.33 ≤ x ≤ 0.50, the main component of the composite system is found to be single-phase KNN with a tetragonal structure. Granular nanodomains ofmore » the orthorhombic phase dispersed in the tetragonal matrix have been identified by HR-TEM and SAD for 0.56 ≤ x ≤ 0.75. Only a trace amount of the orthorhombic phase has been found in the SAD patterns at the composition x = 0.56. However, the number of orthorhombic nanodomains gradually increases with increasing Na content up to x < 0.75, as observed from the HR-TEM images. An abrupt increase and agglomeration of the nanodomains are observed at x = 0.75, where weak diffraction peaks of the orthorhombic phase have also become detectable from the XRD data. The maximum value of the electromechanical coupling coefficient, k{sub p} = 0.56, has been observed at the composition x = 0.56.« less

Nanorods, nanospheres, nanocubes: Synthesis, characterization and catalytic activity of nanoferrites of Mn, Co, Ni, Part-89

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

Singh, Supriya; Srivastava, Pratibha; Singh, Gurdip, E-mail: gsingh4us@yahoo.com

2013-02-15

Graphical abstract: Prepared nanoferrites were characterized by FE-SEM and bright field TEM micrographs. The catalytic effect of these nanoferrites was evaluated on the thermal decomposition of ammonium perchlorate using TG and TG–DSC techniques. The kinetics of thermal decomposition of AP was evaluated using isothermal TG data by model fitting as well as isoconversional method. Display Omitted Highlights: ► Synthesis of ferrite nanostructures (∼20.0 nm) by wet-chemical method under different synthetic conditions. ► Characterization using XRD, FE-SEM, EDS, TEM, HRTEM and SAED pattern. ► Catalytic activity of ferrite nanostructures on AP thermal decomposition by thermal techniques. ► Burning rate measurements ofmore » CSPs with ferrite nanostructures. ► Kinetics of thermal decomposition of AP + nanoferrites. -- Abstract: In this paper, the nanoferrites of Mn, Co and Ni were synthesized by wet chemical method and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive, X-ray spectra (EDS), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HR-TEM). It is catalytic activity were investigated on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellants (CSPs) using thermogravimetry (TG), TG coupled with differential scanning calorimetry (TG–DSC) and ignition delay measurements. Kinetics of thermal decomposition of AP + nanoferrites have also been investigated using isoconversional and model fitting approaches which have been applied to data for isothermal TG decomposition. The burning rate of CSPs was considerably enhanced by these nanoferrites. Addition of nanoferrites to AP led to shifting of the high temperature decomposition peak toward lower temperature. All these studies reveal that ferrite nanorods show the best catalytic activity superior to that of nanospheres and nanocubes.« less

Multi-scale characterization by FIB-SEM/TEM/3DAP.

PubMed

Ohkubo, T; Sepehri-Amin, H; Sasaki, T T; Hono, K

2014-11-01

In order to improve properties of functional materials, it is important to understand the relation between the structure and the properties since the structure has large effect to the properties. This can be done by using multi-scale microstructure analysis from macro-scale to nano and atomic scale. Scanning electron microscope (SEM) equipped with focused ion beam (FIB), transmission electron microscope (TEM) and 3D atom probe (3DAP) are complementary analysis tools making it possible to know the structure and the chemistry from micron to atomic resolution. SEM gives us overall microstructural and chemical information by various kinds of detectors such as secondary electron, backscattered electron, EDS and EBSD detectors. Also, it is possible to analyze 3D structure and chemistry via FIB serial sectioning. In addition, using TEM we can focus on desired region to get more complementary information from HRTEM/STEM/Lorentz images, SAED/NBD patterns and EDS/EELS to see the detail micro or nano-structure and chemistry. Especially, combination of probe Cs corrector and split EDS detectors with large detector size enable us to analyze the atomic scale elemental distribution. Furthermore, if the specimen has a complicated 3D nanostructure, or we need to analyze light elements such as hydrogen, lithium or boron, 3DAP can be used as the only technique which can visualize and analyze distribution of all constituent atoms of our materials within a few hundreds nm area. Hence, site-specific sample preparation using FIB/SEM is necessary to get desired information from region of interest. Therefore, this complementary analysis combination works very well to understand the detail of materials.In this presentation, we will show the analysis results obtained from some of functional materials by Carl Zeiss CrossBeam 1540EsB FIB/SEM, FEI Tecnai G(2) F30, Titan G2 80-200 TEMs and locally build laser assisted 3DAP. As the one of the example, result of multi-scale characterization for

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

NASA Technical Reports Server (NTRS)

Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

2012-01-01

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Green synthesis of gold nanoparticles using aqueous extract of Dillenia indica

NASA Astrophysics Data System (ADS)

Sett, Arghya; Gadewar, Manoj; Sharma, Pragya; Deka, Manab; Bora, Utpal

2016-06-01

In this study, we report a novel method of gold nanoparticle (AuNP) synthesis using aqueous fruit extract of Dillenia indica. The phytochemicals present in the fruit extract act as an effective reducing and capping agent to synthesize AuNPs. The synthesized AuNPs were characterized by spectrophotometry, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. TEM studies revealed the particles of various sizes and mainly spherical in shape. Selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images confirmed the crystallinity of the particles. The XRD patterns showed peaks at (111), (200), (220) which exhibited preferential orientation of the AuNPs as face-centered cubic crystal. FTIR measurements confirmed the coating of phenolic compounds on the AuNPs indicating a possible role of biomolecules for the capping and efficient stabilization of the AuNPs. The synthesized AuNPs did not show any form of cytotoxicity in the normal fibroblast cell line L929.

The dual role of sulfur-containing amino acids in the synthesis of IV-VI semiconductor nanocrystals: a mechanochemical approach.

PubMed

Baláž, Peter; Baláž, Matej; Caplovičová, Mária; Zorkovská, Anna; Caplovič, Lubomír; Psotka, Miroslav

2014-01-01

PbS@cystine nanocrystals were synthesized mechanochemically, with lead acetate and L-cystine being used as the lead and sulfur precursors, respectively. The resulting nanocrystals are 22-34 nm in size, well-faceted and octahedral in shape. Characterization by XRD, FT-IR, NMR, FE-SEM, EDS, TEM (HRTEM) and surface area measurement methods showed that the particles are single, defect-free crystals with a high crystallinity. Furthermore, the crystals were prepared using a solvent-free procedure that was performed under ambient temperature and atmospheric pressure.

Morphology and Chemical Composition of soot particles emitted by Wood-burning Cook-Stoves: a HRTEM, XPS and Elastic backscattering Studies.

NASA Astrophysics Data System (ADS)

Carabali-Sandoval, G. A., Sr.; Castro, T.; Peralta, O.; De la Cruz, W.; Días, J.; Amelines, O.; Rivera-Hernández, M.; Varela, A.; Muñoz-Muñoz, F.; Policroniades, R.; Murillo, G.; Moreno, E.

2014-12-01

The morphology, microstructure and the chemical composition on surface of soot particles were studied by using high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and elastic backscattering spectrometry. In order to obtain freshly soot particles emitted by home-made wood-burning cook stoves, copper grids for Transmission Electron Microscope (TEM) were placed on the last two of an 8-stages MOUDI cascade impactor. The analysis of HRTEM micrographs revealed the nanostructure and the particle size of soot particles. The XPS survey spectra show a large carbon peak around 285 eV and the oxygen signal at 533 eV. Some differences observed in the carbon/oxygen (C/O) ratio of the particles probably depend on the combustion process efficiency of each cook-stove analyzed. The C-1s XPS spectra show an asymmetric broad peak and other with low intensity that corresponds to sp2 and sp3hybridization, which were fitted with a convolution using Gaussian functions. Elastic backscattering technique allows a chemical elemental analysis of samples and confirms the presence of C, O and Si observed by XPS. Additionally, the morphological properties of soot aggregates were analyzed calculating the border-based fractal dimension (Df). Particles exhibit complex shapes with high values of Df. Also, real-time absorption (σabs) and scattering (σsct) coefficients of fine (with aerodynamic diameter < 2.5 µm) soot particles were measured. The trend in σabs and σsct indicate that the cooking process has two important combustion stages which varied in its flaming strength, being vigorous in the first stage and soft in the second one.

Atom by atom: HRTEM insights into inorganic nanotubes and fullerene-like structures

PubMed Central

Sadan, Maya Bar; Houben, Lothar; Enyashin, Andrey N.; Seifert, Gotthard; Tenne, Reshef

2008-01-01

The characterization of nanostructures down to the atomic scale is essential to understand some physical properties. Such a characterization is possible today using direct imaging methods such as aberration-corrected high-resolution transmission electron microscopy (HRTEM), when iteratively backed by advanced modeling produced by theoretical structure calculations and image calculations. Aberration-corrected HRTEM is therefore extremely useful for investigating low-dimensional structures, such as inorganic fullerene-like particles and inorganic nanotubes. The atomic arrangement in these nanostructures can lead to new insights into the growth mechanism or physical properties, where imminent commercial applications are unfolding. This article will focus on two structures that are symmetric and reproducible. The first structure that will be dealt with is the smallest stable symmetric closed-cage structure in the inorganic system, a MoS2 nanooctahedron. It is investigated by means of aberration-corrected microscopy which allowed validating the suggested DFTB-MD model. It will be shown that structures diverging from the energetically most stable structures are present in the laser ablated soot and that the alignment of the different shells is parallel, unlike the bulk material where the alignment is antiparallel. These findings correspond well with the high-energy synthetic route and they provide more insight into the growth mechanism. The second structure studied is WS2 nanotubes, which have already been shown to have a unique structure with very desirable mechanical properties. The joint HRTEM study combined with modeling reveals new information regarding the chirality of the different shells and provides a better understanding of their growth mechanism. PMID:18838681

Atom by atom: HRTEM insights into inorganic nanotubes and fullerene-like structures.

PubMed

Bar Sadan, Maya; Houben, Lothar; Enyashin, Andrey N; Seifert, Gotthard; Tenne, Reshef

2008-10-14

The characterization of nanostructures down to the atomic scale is essential to understand some physical properties. Such a characterization is possible today using direct imaging methods such as aberration-corrected high-resolution transmission electron microscopy (HRTEM), when iteratively backed by advanced modeling produced by theoretical structure calculations and image calculations. Aberration-corrected HRTEM is therefore extremely useful for investigating low-dimensional structures, such as inorganic fullerene-like particles and inorganic nanotubes. The atomic arrangement in these nanostructures can lead to new insights into the growth mechanism or physical properties, where imminent commercial applications are unfolding. This article will focus on two structures that are symmetric and reproducible. The first structure that will be dealt with is the smallest stable symmetric closed-cage structure in the inorganic system, a MoS(2) nanooctahedron. It is investigated by means of aberration-corrected microscopy which allowed validating the suggested DFTB-MD model. It will be shown that structures diverging from the energetically most stable structures are present in the laser ablated soot and that the alignment of the different shells is parallel, unlike the bulk material where the alignment is antiparallel. These findings correspond well with the high-energy synthetic route and they provide more insight into the growth mechanism. The second structure studied is WS(2) nanotubes, which have already been shown to have a unique structure with very desirable mechanical properties. The joint HRTEM study combined with modeling reveals new information regarding the chirality of the different shells and provides a better understanding of their growth mechanism.

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

PubMed

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

2018-01-01

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

Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

NASA Astrophysics Data System (ADS)

Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

2017-09-01

Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

A series of BCN nanosheets with enhanced photoelectrochemical performances

NASA Astrophysics Data System (ADS)

Li, Junqi; Lei, Nan; Hao, Hongjuan; Zhou, Jian

2017-03-01

A series of flake-like BCN compounds were produced by calcination at different reaction temperatures via thermal substitution of C atoms with B atoms of boric acid substructures in graphitic carbon nitrides (g-C3N4). The structural and optical properties of the samples were characterized by XRD, TEM, HRTEM, XPS and UV-vis absorption. The photoelectrochemical (PEC) performance of all samples were characterized through photocurrent and electrochemical impedance spectroscopy (EIS) measurement. The test results demonstrated that BCN nanosheets exhibited higher PEC performance with increasing substituted amount of boron.

Nanoscale characterization of the thermal interface resistance of a heat-sink composite material by in situ TEM.

PubMed

Kawamoto, Naoyuki; Kakefuda, Yohei; Mori, Takao; Hirose, Kenji; Mitome, Masanori; Bando, Yoshio; Golberg, Dmitri

2015-11-20

We developed an original method of in situ nanoscale characterization of thermal resistance utilizing a high-resolution transmission electron microscope (HRTEM). The focused electron beam of the HRTEM was used as a contact-free heat source and a piezo-movable nanothermocouple was developed as a thermal detector. This method has a high flexibility of supplying thermal-flux directions for nano/microscale thermal conductivity analysis, and is a powerful way to probe the thermal properties of complex or composite materials. Using this method we performed reproducible measurements of electron beam-induced temperature changes in pre-selected sections of a heat-sink α-Al(2)O(3)/epoxy-based resin composite. Observed linear behavior of the temperature change in a filler reveals that Fourier's law holds even at such a mesoscopic scale. In addition, we successfully determined the thermal resistance of the nanoscale interfaces between neighboring α-Al(2)O(3) fillers to be 1.16 × 10(-8) m(2)K W(-1), which is 35 times larger than that of the fillers themselves. This method that we have discovered enables evaluation of thermal resistivity of composites on the nanoscale, combined with the ultimate spatial localization and resolution sample analysis capabilities that TEM entails.

Fabrication of Worm-Like Nanorods and Ultrafine Nanospheres of Silver Via Solid-State Photochemical Decomposition

PubMed Central

2009-01-01

Worm-like nanorods and nanospheres of silver have been synthesized by photochemical decomposition of silver oxalate in water by UV irradiation in the presence of CTAB and PVP, respectively. No external seeds have been employed for the synthesis of Ag nanorods. The synthesized Ag colloids have been characterized by UV-visible spectra, powder XRD, HRTEM, and selected area electron diffraction (SAED). Ag nanospheres of average size around 2 nm have been obtained in the presence of PVP. XRD and TEM analyses revealed that top and basal planes of nanorods are bound with {111} facets. Williamson–Hall plot has revealed the presence of defects in the Ag nanospheres and nanorods. Formation of defective Ag nanocrystals is attributed to the heating effect of UV-visible irradiation. PMID:20596513

Green synthesis and characterization of graphene nanosheets

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

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductantmore » but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.« less

Facile and fast synthesis of SnS2 nanoparticles by pulsed laser ablation in liquid

NASA Astrophysics Data System (ADS)

Johny, J.; Sepulveda-Guzman, S.; Krishnan, B.; Avellaneda, D.; Shaji, S.

2018-03-01

Nanoparticles (NPs) of tin disulfide (SnS2) were synthesized using pulsed laser ablation in liquid (PLAL) technique. Effects of different liquid media and ablation wavelengths on the morphology and optical properties of the nanoparticles were studied. Nd: YAG laser wavelengths of 532 nm and 1064 nm (frequency 10 Hz and pulse width 10 ns) were used to irradiate SnS2 target immersed in liquid for the synthesis of SnS2 nanoparticles. Here PLAL was a fast synthesis technique, the ablation was only for 30 s. Transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis absorption spectroscopy and photoluminescence spectroscopy were used to characterize the SnS2 NPs. TEM images showed that the liquid medium and laser wavelength influence the morphology of the NPs. SAED patterns and high resolution TEM (HRTEM) images confirmed the crystallinity of the particles. XRD and XPS analyses confirmed that SnS2 NPs were having exact crystalline structure and chemical states as that of the target. Raman analysis also supported the results obtained by XRD and XPS. Optical band gaps of the nanocolloids evaluated from their UV-vis absorption spectra were 2.4-3.05 eV. SnS2 NPs were having luminescence spectra in the blue-green region irrespective of the liquid media and ablation wavelength.

Thin film assembly of nanosized cobalt(II) bis(5-phenyl-azo-8-hydroxyquinolate) using static step-by-step soft surface reaction technique: Structural characterization and optical properties.

PubMed

Seleim, S M; Hamdalla, Taymour A; Mahmoud, Mohamed E

2017-09-05

Nanosized (NS) cobalt (II) bis(5-phenyl-azo-8-hydroxyquinolate) (NS Co(II)-(5PA-8HQ) 2 ) thin films have been synthesized using static step-by-step soft surface reaction (SS-b-SSR) technique. Structural and optical characterizations of these thin films have been carried out using thermal gravimetric analysis (TGA), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD). The HR-TEM results revealed that the assembled Co(II)-complex exhibited a uniformly NS structure particles in the form of nanorods with width and length up to 16.90nm and 506.38nm, respectively. The linear and nonlinear optical properties have been investigated. The identified energy gap of the designed thin film materials was found 4.01eV. The refractive index of deposited Co(II)-complex thin film was identified by thickness-dependence and found as 1.9 at wavelength 1100nm. In addition, the refractive index was varied by about 0.15 due to an increase in the thickness by 19nm. Copyright © 2017 Elsevier B.V. All rights reserved.

Evolution of TEM-type enzymes: biochemical and genetic characterization of two new complex mutant TEM enzymes, TEM-151 and TEM-152, from a single patient.

PubMed

Robin, Frédéric; Delmas, Julien; Schweitzer, Cédric; Tournilhac, Olivier; Lesens, Olivier; Chanal, Catherine; Bonnet, Richard

2007-04-01

Two clinical isolates of Escherichia coli, CF1179 and CF1295, were isolated from a patient hospitalized in the hematology unit of the University Hospital of Clermont-Ferrand, Clermont-Ferrand, France. They were resistant to penicillin-clavulanate combinations and to ceftazidime. The double-disk synergy test was positive only for isolate CF1179. Molecular comparison of the isolates showed that they were clonally related. E. coli recombinant strains exhibiting the resistance phenotype of the clinical strains were obtained by cloning. The clones corresponding to strains CF1179 and CF1295 produced TEM-type beta-lactamases with pI values of 5.7 and 5.3, respectively. Sequencing analysis revealed two novel blaTEM genes encoding closely related complex mutant TEM enzymes, designated TEM-151 (pI 5.3) and TEM-152 (pI 5.7). These two genes also harbored a new promoter region which presented a 9-bp deletion. The two novel beta-lactamases differed from the parental enzyme, TEM-1, by the substitution Arg164His, previously observed in extended-spectrum beta-lactamases (ESBLs), and by the substitutions Met69Val and Asn276Asp, previously observed in the inhibitor-resistant penicillinase TEM-36/IRT-7. They differed by two amino acid substitutions: TEM-152 harbored a Glu240Lys ESBL-type substitution and TEM-151 had an Ala284Gly substitution. Functional analysis of TEM-151 and TEM-152 showed that both enzymes had hydrolytic activity against ceftazidime (kcat, 5 and 16 s-1, respectively). TEM-152 was more resistant than TEM-151 to the inhibitor clavulanic acid (50% inhibitory concentrations, 1 versus 0.17 microM). These results confirm the evolution of TEM-type enzymes toward complex enzymes harboring the two kinds of substitutions which confer an extended spectrum of action against beta-lactam antibiotics and resistance to inhibitors.

Effect of Pt and Fe catalysts in the transformation of carbon black into carbon nanotubes

NASA Astrophysics Data System (ADS)

Asokan, Vijayshankar; Myrseth, Velaug; Kosinski, Pawel

2015-06-01

In this research carbon nanotubes and carbon nano onion-like structures were synthesized from carbon black using metal catalysts at 400 °C and 700 °C. Platinum and iron-group metals were used as catalysts for the transformation of CB into graphitized nanocarbon and the effect of both metals was compared. The synthesized products were characterized using X-ray diffraction (XRD), transmission electron microscope (TEM), high resolution transmission electron microscope (HRTEM) and Raman spectroscopy. The characterization shows that this process is very efficient in the synthesis of high quality graphitized products from amorphous carbon black, even though the process temperature was relatively low in comparison with previous studies. Distinguished graphitic walls of the newly formed carbon nanostructures were clearly visible in the HRTEM images. Possible growth difference related to the type of catalyst used is briefly explained with the basis of electron vacancies in d-orbitals of metals.

XRD measurement of mean crystallite thickness of illite and illite/smectite: Reappraisal of the Kubler index and the Scherrer equation

USGS Publications Warehouse

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

1997-01-01

The standard form of the Scherrer equation, which has been used to calculate the mean thickness of the coherent scattering domain (CSD) of illite crystals from X-ray diffraction (XRD) full width data at half maximum (FWHM) intensity, employs a constant, Ksh, of 0.89. Use of this constant is unjustified, even if swelling has no effect on peak broadening, because this constant is valid only if all CSDs have a single thickness. For different thickness distributions, the Scherrer “constant” has very different values.Analysis of fundamental particle thickness data (transmission electron microscopy, TEM) for samples of authigenic illite and illite/smectite from diagenetically altered pyroclastics and filamentous illites from sandstones reveals a unique family of lognormal thickness distributions for these clays. Experimental relations between the distributions' lognormal parameters and mean thicknesses are established. These relations then are used to calculate the mean thickness of CSDs for illitic samples from XRD FWHM, or from integral XRD peak widths (integrated intensity/maximum intensity).For mixed-layer illite/smectite, the measured thickness of the CSD corresponds to the mean thickness of the mixed-layer crystal. Using this measurement, the mean thickness of the fundamental particles that compose the mixed-layer crystals can be calculated after XRD determination of percent smectitic interlayers. The effect of mixed layering (swelling) on XRD peak width for these samples is eliminated by using the 003 reflection for glycolated samples, and the 001, 002 or 003 reflection for dehydrated, K-saturated samples. If this technique is applied to the 001 reflection of air-dried samples (Kubler index measurement), mean CSD thicknesses are underestimated due to the mixed-layering effect.The technique was calibrated using NEW MOD©-simulated XRD profiles of illite, and then tested on well-characterized illite and illite/smectite samples. The XRD measurements are in good

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

PubMed

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

2018-01-01

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

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.

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

PubMed

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Biological and catalytic applications of green synthesized fluorescent N-doped carbon dots using Hylocereus undatus.

PubMed

Arul, Velusamy; Edison, Thomas Nesakumar Jebakumar Immanuel; Lee, Yong Rok; Sethuraman, Mathur Gopalakrishnan

2017-03-01

In this work, a simple hydrothermal route for the synthesis of fluorescent nitrogen doped carbon dots (N-CDs) is reported. The Hylocereus undatus (H. undatus) extract and aqueous ammonia are used as carbon and nitrogen source, respectively. The optical properties of synthesized N-CDs are analyzed using UV-Visible (UV-Vis) and fluorescence spectroscopy. The surface morphology, elemental composition, crystallinity and functional groups present in the N-CDs are examined using high resolution transmission electron microscopy (HR-TEM) with energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy, respectively. The synthesized N-CDs emit strong blue fluorescence at 400nm under the excitation of 320nm. Further, the excitation dependent emission properties are also observed from the fluorescence of synthesized N-CDs. The HR-TEM results reveal that synthesized N-CDs are in spherical shape with average diameter of 2.5nm. The XRD pattern exhibits, the graphitic nature of synthesized N-CDs. The doping of nitrogen is confirmed from the EDS and FT-IR studies. The cytotoxicity and biocompatibility of N-CDs are evaluated through MTT assay on L-929 (Lymphoblastoid-929) and MCF-7 (Michigan Cancer Foundation-7) cells. The results indicate that the fluorescent N-CDs show less cytotoxicity and good biocompatibility on both L-929 and MCF-7 cells. Moreover, the N-CDs show excellent catalytic activity towards the reduction of methylene blue by sodium borohydride. Copyright © 2017 Elsevier B.V. All rights reserved.

Influence of a cellulosic ether carrier on the structure of biphasic calcium phosphate ceramic particles in an injectable composite material.

PubMed

Dupraz, A; Nguyen, T P; Richard, M; Daculsi, G; Passuti, N

1999-04-01

An injectable composite material based on biphasic calcium phosphate (BCP) and a nonionic cellulose ether has been elaborated for use in percutaneous surgery for spine fusion. This paper reports the characterization results of this material by spectroscopic techniques including X-ray diffraction (XRD), infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) fitted with an energy dispersive X-Ray analysis system and high-resolution transmission electron microscopy (HR-TEM). From FTIR and XPS results, it was observed that the adhesion between the polymer and the ceramic might be insured by oxygen bridging developed through an ionic bonding between calcium ions and (C-O) groups of the polymer. Moreover, XPS showed attraction of Ca2+ ions in the polymer matrix, while the ceramic surface was modified in a HPO4(2-) -rich layer. These results suggest a possible dissolution/precipitation process at the interface ceramic/polymer. HR-TEM observations supported this hypothesis, showing a light contrasted fringe at the surface of the ceramic grains in the composite paste. As well, changes in the XRD spectra could indicate a small decrease in the crystal size of the BCP powder through the contact to polymer solution. In addition, SEM observation showed a decrease of the initial BCP granulometry. Aggregates of 80-200 microm seemed to be mostly dissociated in micrograins. The ceramic grains were coated with and bonded between each other by the polymer matrix, which acted as spacer in between the ceramic grains, creating a macroporous-like material structure.

Role of Cu in engineering the optical properties of SnO2 nanostructures: Structural, morphological and spectroscopic studies

NASA Astrophysics Data System (ADS)

Kumar, Virender; Singh, Kulwinder; Jain, Megha; Manju; Kumar, Akshay; Sharma, Jeewan; Vij, Ankush; Thakur, Anup

2018-06-01

We have carried out a systematic study to investigate the effect of Cu doping on the optical properties of SnO2 nanostructures synthesized by chemical route. Synthesized nanostructures were characterized using X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM), High resolution transmission electron microscopy (HR-TEM), Energy dispersive X-ray spectroscopy, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, UV-visible and Photoluminescence (PL) spectroscopy. The Rietveld refinement analysis of XRD patterns of Cu-doped SnO2 samples confirmed the formation of single phase tetragonal rutile structure, however some localized distortion was observed for 5 mol% Cu-doped SnO2. Crystallite size was found to decrease with increase in dopant concentration. FE-SEM images indicated change in morphology of samples with doping. HR-TEM images revealed that synthesized nanostructures were nearly spherical and average crystallite size was in the range 12-21 nm. Structural defects, crystallinity and size effects on doping were investigated by Raman spectroscopy and results were complemented by FTIR spectroscopy. Optical band gap of samples was estimated from reflectance spectra. We have shown that band gap of SnO2 can be engineered from 3.62 to 3.82 eV by Cu doping. PL emission intensity increased as the doping concentration increased, which can be attributed to the development of defect states in the forbidden transition region of band gap of SnO2 with doping. We have also proposed a band model owing to defect states in SnO2 to explain the observed PL in Cu doped SnO2 nanostructures.

MnMoO4 nanolayers : Synthesis characterizations and electrochemical detection of QA

NASA Astrophysics Data System (ADS)

Muthamizh, S.; Kumar, S. Praveen; Munusamy, S.; Narayanan, V.

2018-04-01

MnMoO4 nanolayers were prepared by precipitation method. The MnMoO4 nanolayers were synthesized by using commercially available (CH3COO)2Mn.4H2O and Na2WO4.2H2O. The XRD pattern reveals that the synthesized MnMoO4 has monoclinic structure. In addition, lattice parameter values were also calculated using XRD data. The Raman analysis confirm the presence of Mo-O in MnMoO4 nanolayers. DRS-UV analysis shows that MnMoO4 has a band gap of 2.59 eV. FE-SEM and HR-TEM analysis along with EDAX confirms the material morphology in stacked layers like structure in nano scale. Synthesized nanolayers were utilized for the detection of biomolecule quercetin (QA).

In situ supported MnOx-CeOx on carbon nanotubes for the low-temperature selective catalytic reduction of NO with NH3

NASA Astrophysics Data System (ADS)

Zhang, Dengsong; Zhang, Lei; Shi, Liyi; Fang, Cheng; Li, Hongrui; Gao, Ruihua; Huang, Lei; Zhang, Jianping

2013-01-01

The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods.The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ

Tem Observation of Precipitates in Ag-Added Al-Mg-Si Alloys

NASA Astrophysics Data System (ADS)

Nagai, Takeshi; Matsuda, Kenji; Nakamura, Junya; Kawabata, Tokimasa; Marioara, Calin; Andersen, Sigmund J.; Holmestad, Randi; Hirosawa, Shoichi; Horita, Zenji; Terada, Daisuke; Ikeno, Susumu

The influence of addition of the small amount of transition metals to Al-Mg-Si alloy had reported by many researchers. In the previous our work, β' phase in alloys Al — 1.0 mass% Mg2Si -0.5 mass% Ag (Ag-addition) and Al -1.0 mass% Mg2Si (base) were investigated by high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), in order to understand the effect of Ag. In addition, the distribution of Ag was investigated by energy filtered mapping and high annular angular dark field scanning transmission electron microscopy (HAADF-STEM). One Ag-containing atomic column was observed per β' unit cell, and the unit cell symmetry is slightly changed as compared with the Ag-free β'. In this work, the microstructure of G.P. zone and β'' phase was investigated by TEM observation, which were formed before β' phase. The deformed sample by high pressure torsion (HPT) technique before aging was also investigated to understand its effect for aging in this alloy.

Epitaxial CuInSe2 thin films grown by molecular beam epitaxy and migration enhanced epitaxy

NASA Astrophysics Data System (ADS)

Abderrafi, K.; Ribeiro-Andrade, R.; Nicoara, N.; Cerqueira, M. F.; Gonzalez Debs, M.; Limborço, H.; Salomé, P. M. P.; Gonzalez, J. C.; Briones, F.; Garcia, J. M.; Sadewasser, S.

2017-10-01

While CuInSe2 chalcopyrite materials are mainly used in their polycrystalline form to prepare thin film solar cells, epitaxial layers have been used for the characterization of defects. Typically, epitaxial layers are grown by metal-organic vapor phase epitaxy or molecular beam epitaxy (MBE). Here we present epitaxial layers grown by migration enhanced epitaxy (MEE) and compare the materials quality to MBE grown layers. CuInSe2 layers were grown on GaAs (0 0 1) substrates by co-evaporation of Cu, In, and Se using substrate temperatures of 450 °C, 530 °C, and 620 °C. The layers were characterized by high resolution X-ray diffraction (HR-XRD), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, and atomic force microscopy (AFM). HR-XRD and HR-TEM show a better crystalline quality of the MEE grown layers, and Raman scattering measurements confirm single phase CuInSe2. AFM shows the previously observed faceting of the (0 0 1) surface into {1 1 2} facets with trenches formed along the [1 1 0] direction. The surface of MEE-grown samples appears smoother compared to MBE-grown samples, a similar trend is observed with increasing growth temperature.

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

PubMed

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

2013-12-01

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

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

PubMed

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

2015-06-01

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

Arsenic(V) removal from groundwater using nano scale zero-valent iron as a colloidal reactive barrier material.

PubMed

Kanel, Sushil Raj; Greneche, Jean-Mark; Choi, Heechul

2006-03-15

The removal of As(V), one of the most poisonous groundwater pollutants, by synthetic nanoscale zero-valent iron (NZVI) was studied. Batch experiments were performed to investigate the influence of pH, adsorption kinetics, sorption mechanism, and anionic effects. Field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Mossbauer spectroscopy were used to characterize the particle size, surface morphology, and corrosion layer formation on pristine NZVI and As(V)-treated NZVI. The HR-TEM study of pristine NZVI showed a core-shell-like structure, where more than 90% of the nanoparticles were under 30 nm in diameter. Mössbauer spectroscopy further confirmed its structure in which 19% were in zero-valent state with a coat of 81% iron oxides. The XRD results showed that As(V)-treated NZVI was gradually converted into magnetite/maghemite corrosion products over 90 days. The XPS study confirmed that 25% As(V) was reduced to As(III) by NZVI after 90 days. As(V) adsorption kinetics were rapid and occurred within minutes following a pseudo-first-order rate expression with observed reaction rate constants (Kobs) of 0.02-0.71 min(-1) at various NZVI concentrations. Laser light scattering analysis confirmed that NZVI-As(V) forms an inner-sphere surface complexation. The effects of competing anions revealed that HCO3-, H4SiO4(0), and H2PO4(2-) are potential interfering agents in the As(V) adsorption reaction. Our results suggest that NZVI is a suitable candidate for As(V) remediation.

Crystallization kinetics of the Cu{sub 50}Zr{sub 50} metallic glass under isothermal conditions

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

Gao, Qian; Jian, Zengyun, E-mail: jianzengyun@xatu.edu.cn; Xu, Junfeng

2016-12-15

Amorphous structure of the melt-spun Cu{sub 50}Zr{sub 50} amorphous alloy ribbons were confirmed by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HR-TEM). Isothermal crystallization kinetics of these alloy ribbons were investigated using differential scanning calorimetry (DSC). Besides, Arrhenius and Johnson-Mehl-Avrami (JMA) equations were utilized to obtain the isothermal crystallization kinetic parameters. As shown in the results, the local activation energy E{sub α} decreases by a large margin at the crystallized volume fraction α<0.1, which proves that crystallization process is increasingly easy. In addition, the local activation energy E{sub α} is basically constant at 0.1

MWCNT/CdS hybrid nanocomposite for enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Chaudhary, Deepti; Khare, Neeraj; Vankar, V. D.

2016-05-01

Multi-walled carbon nanotubes (MWCNT)/CdS hybrid nanocomposite were synthesized by one step hydrothermal method. MWCNTs were used as a substrate for the growth of CdS nanoparticles. MWCNT/CdS nanocomposite and pure CdS were characterized by XRD, TEM, UV-vis and photoluminescence spectroscopy. HRTEM study confirms the intimate contact of CdS with MWCNT. The photocatalytic activity of nanocomposite was studied for the degradation of methylene blue dye under UV irradiation. The enhanced photocatalytic activity of MWCNT/CdS nanocomposite as compared to pure CdS has been attributed to reduced recombination of photogenerated charge carriers due to interfacial electron transfer from CdS to MWCNT.

Preparation of Sm-doped ceria (SDC) nanowires and tubes by gas-liquid co-precipitation at room temperature

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

Gu Lina; School of Chemistry and Chemical Engineering, Anhui University, 230039 Hefei; Meng Guangyao

Sm-doped cerium dioxide (SDC) with fcc structure was formed using a gas-liquid chemical co-precipitation process at room temperature. Morphology and structure of the as-prepared samples were characterized using TG, XRD, TEM, HRTEM and SAED techniques. Under our specific experimental conditions, two kinds of 1D nano-structures SDC have been mainly obtained. SDC nanowires are 0.3-1.2 {mu}m in lengths and 5-20 nm in diameters. SDC nanotubes have outer diameters in 10-40 nm with lengths up to 2 {mu}m. The as-prepared SDC shows very strong UV absorption ability and the maximum absorption peak redshifts compared with that of SDC nanoparticles.

Formation of MoS2 inorganic fullerenes (IFs) by the reaction of MoO3 nanobelts and S.

PubMed

Li, Xiao Lin; Li, Ya Dong

2003-06-16

The reaction of MoO3 and S at temperatures higher than 300 degrees C in an argon atmosphere provides a convenient and effective method for the synthesis of MoS2 nanocrystalline substances. MoS2 nanotubes and fullerene-like nanoparticles have been obtained by the reaction at 850 degrees C under well-controlled conditions. The influences of reaction temperature and duration were carefully investigated in this paper. All of the nanostructures were characterized by Xray powder diffraction (XRD), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). A stepwise reaction model and rolling mechanism were proposed based on the experimental results.

Synthesis and evaluation of optical and antimicrobial properties of Ag-SnO2 nanocomposites

NASA Astrophysics Data System (ADS)

Kumar Nair, Kishore; Kumar, Promod; Kumar, Vinod; Harris, R. A.; Kroon, R. E.; Viljoen, Bennie; Shumbula, P. M.; Mlambo, M.; Swart, H. C.

2018-04-01

We report on the sol-gel based room temperature synthesis of undoped SnO2 and Ag-SnO2 nanostructures. The synthesized nanostructures were characterized by Fourier transform infrared spectroscopy, X-ray diffraction (XRD), Raman spectroscopy, High-resolution transmission electron microscopy (HR-TEM) and UV-visible spectroscopy. The XRD pattern confirmed that the obtained nanostructures have a tetragonally rutile structure. No extra phase changes were observed after Ag doping. UV-visible spectroscopy measurements indicated that the band gap of 3.59 eV for pure SnO2 nanostructures, decreased to 3.39 eV after doping. TEM analysis showed that no regular shape morphology existed and some rod-shaped particles were also detected in the nanostructures. The antibacterial activity of the nanostructures against E. coli was evaluated and a continuous decrease of microbial count was observed. The microbial population decreased from 6 × 105 cfu/ml to 7 × 104 cfu/ml and 5 × 104 cfu/ml on SnO2 and Ag-SnO2 treatments, respectively. Thus, the nanostructures can be used for the biorational management of E. coli for waste water treatment before discharge.

Influence of Mg doping on ZnO nanoparticles decorated on graphene oxide (GO) crumpled paper like sheet and its high photo catalytic performance under sunlight

NASA Astrophysics Data System (ADS)

Labhane, P. K.; Sonawane, S. H.; Sonawane, G. H.; Patil, S. P.; Huse, V. R.

2018-03-01

Mg doped ZnO nanoparticles decorated on graphene oxide (GO) sheets were synthesized by a wet impregnation method. The effect of Mg doping on ZnO and ZnO-GO composite has been evaluated by using x-ray diffraction (XRD), Williamson-Hall Plot (Wsbnd H Plot), field emission scanning electron microscope (FESEM), transmission electron microscopy (TEM) and energy dispersive x-ray spectroscopy (EDX). The physical parameters of as-prepared samples were estimated by XRD data. FESEM and HR-TEM images showed the uniform distribution of nanoparticles on GO crumpled paper like sheet. Solar light photocatalytic activities of samples were evaluated spectrophotometrically by the degradation of p-nitrophenol (PNP) and indigo carmine (IC) solution. Mgsbnd ZnO decorated on GO sheets exhibit excellent catalytic efficiency compared to all other prepared samples under identical conditions, degrading PNP and IC nearly 99% within 60 min under sunlight. The effective degradation by Mgsbnd ZnO decorated on GO sheet would be due to extended solar light absorption, enhanced adsorptivity on the composite catalyst surface and efficient charge separation of photo-induced electrons. Finally, plausible mechanism was suggested with the help of scavengers study.

Effect of porphyrin on photocatalytic activity of TiO2 nanoparticles toward Rhodamine B photodegradation.

PubMed

Ahmed, M A; Abou-Gamra, Z M; Medien, H A A; Hamza, M A

2017-11-01

As known, porphyrins have central role in photosynthesis, biological oxidation and reduction and oxygen transport beside to their intensive color which qualify them to be good photosensitizers. Herein, tetra (4-carboxyphenyl) porphyrin (TCPP) was prepared by a simple one-pot synthesis to use as a visible antenna for TiO 2 nanoparticles that were prepared via a simple template-free sol-gel method. Various loading percentages of TCPP (0.05-1%) were incorporated on the surface of TiO 2 as photosensitizer for photocatalytic degradation of Rhodamine B (Rh B) dye as a primary cationic pollutant model. Among them, 0.1% TCPP-TiO 2 was the most reactive sample. It was found that the photoactivity of 0.1% TCPP-TiO 2 sample (0.5g/L) was approximately 1.5 times greater than that of pure TiO 2 (0.5g/L) toward the degradation of Rh B (1×10 -5 M) under UV-A irradiation. Transient fluorescence decay measurements showed that the life time of TiO 2 excited state has doubled after anchoring TCPP, thus the probability of electron-hole recombination has decreased. The samples were characterized by XRD, HR-TEM, DRS and N 2 adsorption-desorption isotherms. The XRD patterns confirmed the successful preparation of TiO 2 nanoparticles with average crystalline size of 25.7nm. Also, XRD patterns suggested the presence of mixed phase TiO 2 nanoparticles of 77% anatase and 23% rutile. DRS showed that the characteristic peaks of TCPP covered the whole visible range 400-700nm. HR-TEM images showed the spheroids shape of TiO 2 nanoparticles and confirmed the presence of anatase and rutile phases as suggested from XRD data. The different parameters affecting the photodegradation of Rh B dye such as catalyst dose, dye concentration and pH were studied to obtain the optimum conditions. Almost complete degradation of Rh B was obtained which confirmed by HPLC and TOC measurements. The effect of scavengers was studied to indicate the most active species. TCPP-TiO 2 gave a good response toward the

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

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

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

2011-10-15

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

Aloe vera plant-extracted solution hydrothermal synthesis and magnetic properties of magnetite (Fe3O4) nanoparticles

NASA Astrophysics Data System (ADS)

Phumying, Santi; Labuayai, Sarawuth; Thomas, Chunpen; Amornkitbamrung, Vittaya; Swatsitang, Ekaphan; Maensiri, Santi

2013-06-01

Magnetite (Fe3O4) nanoparticles have been successfully synthesized by a novel hydrothermal method using ferric acetylacetonate (Fe(C5H8O2)3) and aloe vera plant-extracted solution. The influences of different reaction temperatures and times on the structure and magnetic properties of the synthesized Fe3O4 nanoparticles were investigated. The synthesized nanoparticles are crystalline and have particle sizes of ˜6-30 nm, as revealed by transmission electron microscopy (TEM). The results of X-ray diffraction (XRD), High resolution TEM (HRTEM) and selected area electron diffraction (SAED) indicate that the synthesized Fe3O4 nanoparticles have the inverse cubic spinel structure without the presence of any other phase impurities. The hysteresis loops of the Fe3O4 nanoparticles at room temperature show superparamagnetic behavior and the saturation magnetization of the Fe3O4 samples increases with increasing reaction temperature and time.

Fabrication of highly active Melem/Zn0.25Cd0.75S composites for the degradation of bisphenol A and methyl orange under visible light irradiation

NASA Astrophysics Data System (ADS)

Wang, Xiaodong; Yan, Tao; Liu, Xiaohuan; Ji, Pengge; Sun, Meng; Wei, Dong; Yan, Liangguo; Du, Bin

2016-11-01

Metal-free polymeric catalyst hold great promise owing to their abundant sources, low-cost fabrication and easy processibility. Melem, an important intermediate during condensation of melamine rings to graphitic carbon nitride (g-C3N4), was synthesized by simple solid phase polymerization process. A novel Melem/Zn0.25Cd0.75S composite was fabricated through a facile one-step hydrothermal method. The as-products were characterized by X-ray diffraction (XRD), UV-vis DRS spectroscopy, fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM). The TEM and HRTEM results reveal that Zn0.25Cd0.75S nanoparticles and Melem closely contact with each other to form an intimate interface. The as-prepared composites exhibit significantly enhanced visible light photocatalytic performance for the degradation of Methyl orange (MO) and Bisphenol A (BPA), which could be attributed to the effective photo-induced charges transfer and separation in Melem/Zn0.25Cd0.75S composites. On the basis of radical scavenger experiments, superoxide radicals and holes are suggested to play a critical role in MO degradation over Melem/Zn0.25Cd0.75S heterojunctions. A possible mechanism for charge separation and transfer in the Melem/Zn0.25Cd0.75S composites was proposed to explain the enhanced photocatalytic performance.

Epitaxy of Zn{sub 2}TiO{sub 4} (1 1 1) thin films on GaN (0 0 1)

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

Hsiao, Chu-Yun; Wu, Jhih-Cheng; Shih, Chuan-Feng, E-mail: cfshih@mail.ncku.edu.tw

2013-03-15

Highlights: ► High-permittivity spinel Zn{sub 2}TiO{sub 4} thin films were grown on GaN (0 0 1) by sputtering. ► Oxygen atmosphere and post heat-treatment annealing effectively enhanced epitaxy. ► The epitaxial Zn{sub 2}TiO{sub 4} modifies the dielectric properties of ceramic oxide. - Abstract: High-permittivity spinel Zn{sub 2}TiO{sub 4} thin films were grown on GaN (0 0 1) by rf-sputtering. Grazing-angle, powder, and pole-figure X-ray diffractometries (XRD) were performed to identify the crystallinity and the preferred orientation of the Zn{sub 2}TiO{sub 4} films. Lattice image at the Zn{sub 2}TiO{sub 4} (1 1 1)/GaN (0 0 1) interface was obtained by high-resolutionmore » transmission-electron microscopy (HR-TEM). An oxygen atmosphere in sputtering and post heat-treatment using rapid thermal annealing effectively enhanced the epitaxy. The epitaxial relationship was determined from the XRD and HR-TEM results: (111){sub Zn{sub 2TiO{sub 4}}}||(001){sub GaN}, (202{sup ¯}){sub Zn{sub 2TiO{sub 4}}}||(110){sub GaN},and[21{sup ¯}1{sup ¯}]{sub Zn{sub 2TiO{sub 4}}}||[01{sup ¯}10]{sub GaN}. Finally, the relative permittivity, interfacial trap density and the flat-band voltage of the Zn{sub 2}TiO{sub 4} based capacitor were ∼18.9, 8.38 × 10{sup 11} eV{sup −1} cm{sup −2}, and 1.1 V, respectively, indicating the potential applications of the Zn{sub 2}TiO{sub 4} thin film to the GaN-based metal-oxide-semiconductor capacitor.« less

Self-assembled spongy-like MnO2 electrode materials for supercapacitors

NASA Astrophysics Data System (ADS)

Dong, Meng; Zhang, Yu Xin; Song, Hong Fang; Qiu, Xin; Hao, Xiao Dong; Liu, Chuan Pu; Yuan, Yuan; Li, Xin Lu; Huang, Jia Mu

2012-08-01

Mesoporous spongy-like MnO2 has been synthesized via a facile and biphasic wet method, accompanied with tetraoctylammonium bromide (TOAB) as a soft template under ambient condition. A well-defined spongy morphology of MnO2 with uniform filament diameters 10-20 nm have been observed by FESEM, TEM, HRTEM, XRD, FT-IR,TGA-DSC studies. Further physical characterizations revealed that MnO2 sponges owned a large surface area of 155 m2 g-1 with typical mesoporous appearance. A specific capacitance value as high as 336 F g-1 was obtained. This improved capacitive behavior was attributed to the large surface area, morphology nature of nano-MnO2, and its broad pore size distribution.

Comparison of the morphology, chemical composition and microstructure of cryptocrystalline graphite and carbon black

NASA Astrophysics Data System (ADS)

Quan, Ying; Liu, Qinfu; Zhang, Shilong; Zhang, Shuai

2018-07-01

The structures of cryptocrystalline graphite (CG) and carbon black (CB) have been analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), organic elemental analysis (OEA), X-ray diffraction (XRD), RAMAN and high-resolution transmission electron microscopy (HRTEM). These results indicate that CG has the same elemental composition as CB, with carbon being the major element present. SL sample (CG with low graphitization degree) and CB exhibit similar microcrystalline structures. CG was shown to contain a layered graphitic structure that was significantly different to the primary spherical particles present in CB. It is proposed that these CG sheets may potentially be reduced and delaminated to afford multilayer graphene structures with improved material properties.

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.

Tuning effect of polysaccharide Chitosan on structural, morphological, optical and photoluminescence properties of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Magesh, G.; Bhoopathi, G.; Nithya, N.; Arun, A. P.; Ranjith Kumar, E.

2018-05-01

Chitosan/ZnO nanocomposites was synthesized by in-situ chemical precipitation method. The effect of polysaccharide Chitosan concentration (0.1 g, 0.5 g, 1 g and 3 g) was investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy dispersive spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), UV-visible (UV), Fourier Transform Infrared (FTIR) and Photoluminescence Spectroscopy (PL). XRD pattern confirms the hexagonal wurtzite structure of the Chitosan/ZnO nanocomposites. The structural morphology and the elemental composition of the samples were analysed by FESEM and EDX respectively. From TEM analysis, it is observed that the particles in spindle shape morphology with average particle size ranges 10-20 nm. UV-Vis analysis reveals that the Chitosan concentration affect the absorption band edge and shift towards lower wavelength. The oxygen vacancy induced photoluminescence of ZnO nanoparticles was observed and its intensity decreases by tuning the Chitosan concentration.

Structural and Magnetic Response in Bimetallic Core/Shell Magnetic Nanoparticles

PubMed Central

Nairan, Adeela; Khan, Usman; Iqbal, Munawar; Khan, Maaz; Javed, Khalid; Riaz, Saira; Naseem, Shahzad; Han, Xiufeng

2016-01-01

Bimagnetic monodisperse CoFe2O4/Fe3O4 core/shell nanoparticles have been prepared by solution evaporation route. To demonstrate preferential coating of iron oxide onto the surface of ferrite nanoparticles X-ray diffraction (XRD), High resolution transmission electron microscope (HR-TEM) and Raman spectroscopy have been performed. XRD analysis using Rietveld refinement technique confirms single phase nanoparticles with average seed size of about 18 nm and thickness of shell is 3 nm, which corroborates with transmission electron microscopy (TEM) analysis. Low temperature magnetic hysteresis loops showed interesting behavior. We have observed large coercivity 15.8 kOe at T = 5 K, whereas maximum saturation magnetization (125 emu/g) is attained at T = 100 K for CoFe2O4/Fe3O4 core/shell nanoparticles. Saturation magnetization decreases due to structural distortions at the surface of shell below 100 K. Zero field cooled (ZFC) and Field cooled (FC) plots show that synthesized nanoparticles are ferromagnetic till room temperature and it has been noticed that core/shell sample possess high blocking temperature than Cobalt Ferrite. Results indicate that presence of iron oxide shell significantly increases magnetic parameters as compared to the simple cobalt ferrite. PMID:28335200

Flux Growth of Highly Crystalline Photocatalytic BaTiO3 Particle Layers on Porous Titanium Sponge Substrate and Insights into the Formation Mechanism

NASA Astrophysics Data System (ADS)

Wang, Q.; Li, B.

2017-09-01

A unique architecture of idiomorphic and highly crystalline BaTiO3 particle layers directly grown on a porous titanium sponge substrate was successfully achieved for the first time using a facile molten salt method at a relatively low temperature of 700 °C. Specifically, the low-melting KCl-NaCl eutectic salts and barium hydroxide octahydrate were employed as the reaction medium and barium source, respectively. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and UV-vis diffuse reflectance spectrophotometry were used to characterize the structure, morphology and optical property of the obtained samples. The results revealed that the flux-grown tetragonal BaTiO3 products had well-defined and uniform morphology with an average size of 300 nm and a band gap of ∼3.16 eV. Based on XRD, EDS, SEM, and TEM, the possible formation mechanism responsible for the well-developed architecture of BaTiO3 particle layers was proposed and discussed. Furthermore, the photocatalytic activity of the flux-grown BaTiO3 products for organic pollutant degradation under simulated sunlight irradiation was also investigated.

Visible cathodoluminescence of Er ions in β-Ga(2)O(3) nanowires and microwires.

PubMed

Nogales, E; Méndez, B; Piqueras, J

2008-01-23

Erbium doped β-Ga(2)O(3) nanowires and microwires have been obtained by a vapour-solid process from an initial mixture of Ga(2)O(3) and Er(2)O(3) powders. X-ray diffraction (XRD) analysis reveals the presence of erbium gallium garnet as well as β-Ga(2)O(3) phases in the microwires. Scanning electron microscopy (SEM) images show that the larger microwires have a nearly rectangular cross-section. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) analysis show good crystal quality of the β-Ga(2)O(3) nanowires. The nanostructures have been studied by means of the cathodoluminescence technique in the scanning electron microscope. Er intraionic blue, green and red emission lines are observed in luminescence spectra even at room temperature, which confirms the optical activity of the rare earth ions in the grown structures. Mapping of the main 555 nm emission intensity shows a non-homogeneous distribution of Er ions in the microstructures.

Synthesis and Luminescence Properties of Core/Shell ZnS:Mn/ZnO Nanoparticles.

PubMed

Jiang, Daixun; Cao, Lixin; Liu, Wei; Su, Ge; Qu, Hua; Sun, Yuanguang; Dong, Bohua

2009-01-01

In this paper the influence of ZnO shell thickness on the luminescence properties of Mn-doped ZnS nanoparticles is studied. Transmission electron microscopy (TEM) images showed that the average diameter of ZnS:Mn nanoparticles is around 14 nm. The formation of ZnO shells on the surface of ZnS:Mn nanoparticles was confirmed by X-ray diffraction (XRD) patterns, high-resolution TEM (HRTEM) images, and X-ray photoelectron spectroscopy (XPS) measurements. A strong increase followed by a gradual decline was observed in the room temperature photoluminescence (PL) spectra with the thickening of the ZnO shell. The photoluminescence excitation (PLE) spectra exhibited a blue shift in ZnO-coated ZnS:Mn nanoparticles compared with the uncoated ones. It is shown that the PL enhancement and the blue shift of optimum excitation wavelength are led by the ZnO-induced surface passivation and compressive stress on the ZnS:Mn cores.

TEM Studies: The Key for Understanding the Origin of the 3.3 V and 4.5 V Steps Observed in LiMn 2O 4-based Spinels

NASA Astrophysics Data System (ADS)

Dupont, L.; Hervieu, M.; Rousse, G.; Masquelier, C.; Palacín, M. R.; Chabre, Y.; Tarascon, J. M.

2000-12-01

Transmission electron microscopy (TEM) measurements were performed on electrochemically partially delithiated prepared spinel Li1-xMn2O4 samples. The potential-composition profile of LiMn2O4 exhibits (besides the two plateaus at 4.05 and 4.1 V) two additional redox steps of identical capacity at 4.5 and 3.3/3.95 V. We found by TEM studies that these extra steps are the signature of a reversible phase transition between LiMn2O4 spinel type structure and a new Li1-xMn2O4 double hexagonal (DH) type structure (a≈5.8 Å, c≈8.9 Å, P63mc). The latter is isotypic with DH LiFeSnO4. Selected area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) made it possible to identify the mechanism by which this cubic-DH phase transition occurs within a particle. Based on the structural findings the origin as well as the similar electrochemical capacity of the 3.3/3.95 and 4.5 V anomalies are explained.

3D contour fluorescence spectroscopy with Brus model: Determination of size and band gap of double stranded DNA templated silver nanoclusters

NASA Astrophysics Data System (ADS)

Kamalraj, Devaraj; Yuvaraj, Selvaraj; Yoganand, Coimbatore Paramasivam; Jaffer, Syed S.

2018-01-01

Here, we propose a new synthetic methodology for silver nanocluster preparation by using a double stranded-DNA (ds-DNA) template which no one has reported yet. A new calculative method was formulated to determine the size of the nanocluster and their band gaps by using steady state 3D contour fluorescence technique with Brus model. Generally, the structure and size of the nanoclusters determine by using High Resolution Transmission Electron Microscopy (HR-TEM). Before imaging the samples by using HR-TEM, they are introduced to drying process which causes aggregation and forms bigger polycrystalline particles. It takes long time duration and expensive methodology. In this current methodology, we found out the size and band gap of the nanocluster in the liquid form without any polycrystalline aggregation for which 3D contour fluorescence technique was used as an alternative approach to the HR-TEM method.

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

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ballmore » milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.« less

Acetate- and thiol-capped monodisperse ruthenium nanoparticles: XPS, XAS, and HRTEM studies.

PubMed

Chakroune, Nassira; Viau, Guillaume; Ammar, Souad; Poul, Laurence; Veautier, Delphine; Chehimi, Mohamed M; Mangeney, Claire; Villain, Françoise; Fiévet, Fernand

2005-07-19

Monodisperse ruthenium nanoparticles were prepared by reduction of RuCl3 in 1,2-propanediol. The mean particle size was controlled by appropriate choice of the reduction temperature and the acetate ion concentration. Colloidal solutions in toluene were obtained by coating the metal particles with dodecanethiol. High-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and X-ray absorption spectroscopy (XANES and EXAFS for the Ru K-absorption edge) were performed on particles of two different diameters, 2 and 4 nm, and in different environments, polyol/acetate or thiol. For particles stored in polyol/acetate XPS studies revealed superficial oxidation limited to one monolayer and a surface coating containing mostly acetate ions. Analysis of the EXAFS spectra showed both oxygen and ruthenium atoms around the ruthenium atoms with a Ru-Ru coordination number N smaller than the bulk value, as expected for fine particles. In the case of 2 nm acetate-capped particles N is consistent with particles made up of a metallic core and an oxidized monolayer. For 2 nm thiol-coated particles, a Ru-S bond was evidenced by XPS and XAS. For the 4 nm particles XANES and XPS studies showed that most of the ruthenium atoms are in the zerovalent state. Nevertheless, in both cases, when capped with thiol, the Ru-Ru coordination number inferred from EXAFS is much smaller than for particles of the same size stored in polyol. This is attributed to a structural disorganization of the particles by thiol chemisorption. HRTEM studies confirm the marked dependence of the structural properties of the ruthenium particles on their chemical environment; they show the acetate-coated particles to be single crystals, whereas the thiol-coated particles appear to be polycrystalline.

Antifouling activities of β-cyclodextrin stabilized peg based silver nanocomposites

NASA Astrophysics Data System (ADS)

Punitha, N.; Saravanan, P.; Mohan, R.; Ramesh, P. S.

2017-01-01

Self-polishing polymer composites which release metal biocide in a controlled rate have been widely used in the design of antimicrobial agents and antifouling coatings. The present work focuses on the environmental friendly green synthesis of PEG based SNCs and their application to biocidal activity including marine biofouling. Biocompatible polymer β-CD and adhesive resistance polymer PEG were used to functionalize the SNPs and the as synthesized SNCs exhibit excellent micro fouling activities. The structural and optical properties were confirmed by XRD and UV-visible techniques respectively. The particle surface and cross sectional characteristics were examined by SEM-EDS, HR-TEM, AFM and FTIR. The surface potential was evaluated using ZP analysis and assessment of antibiofouling property was investigated using static immersion method.

Morphological and phase evolution of TiO 2 nanocrystals prepared from peroxotitanate complex aqueous solution: Influence of acetic acid

NASA Astrophysics Data System (ADS)

Chang, Jeong Ah; Vithal, Muga; Baek, In Chan; Seok, Sang Il

2009-04-01

Nanosized anatase and rutile TiO 2 having different shape, phase and size have been prepared from aqueous solutions of peroxo titanium complex starting from titanium(IV) isopropoxide (TTIP), acetic acid and hydrogen peroxide (H 2O 2) in water/isopropanol media by a facile sol-gel process. The TiO 2 nanocrystals are characterized by powder X-ray diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, TEM, high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) techniques. The influence of pH and the sequence of addition of reaction contents on the phase and morphology of TiO 2 are studied. The reasons for the observation of only anatase and/or mixture of anatase and rutile are given.

Optimization for rapid synthesis of silver nanoparticles and its effect on phytopathogenic fungi

NASA Astrophysics Data System (ADS)

Krishnaraj, C.; Ramachandran, R.; Mohan, K.; Kalaichelvan, P. T.

In this present study, silver nanoparticles were synthesized by green chemistry approach using Acalypha indica leaf extract as reducing agents. The reaction medium employed in the synthesis process was optimized to attain better yield, controlled size and stability. Further, the biosynthesized silver nanoparticles were conformed through UV-vis spectrum, XRD and HR-TEM analyses. Different concentration of silver nanoparticles were tested to know the inhibitory effect of fungal plant pathogens namely Alternaria alternata, Sclerotinia sclerotiorum, Macrophomina phaseolina, Rhizoctonia solani, Botrytis cinerea and Curvularia lunata. Interestingly, 15 mg concentration of silver nanoparticles showed excellent inhibitory activity against all the tested pathogens. Thus, the obtained results clearly suggest that silver nanoparticles may have important applications in controlling various plant diseases caused by fungi.

Diagenetic Microcrystalline Opal Varieties from the Monterey Formation, CA: HRTEM Study of Structures and Phase Transformation Mechanisms

NASA Technical Reports Server (NTRS)

Cady, Sherry L.; Wenk, H.-R.; DeVincenzi, Don (Technical Monitor)

1994-01-01

Microcrystalline opal varieties form as intermediary precipitates during the diagenetic transformation of biogenically precipitated non-crystalline opal (opal-A) to microquartz. With regard to the Monterey Formation of California, X-ray powder diffraction studies have shown that a decrease in the primary d-spacing of opal-CT toward that of cristobalite occurs with increasing diagenesis. The initial timing of opal-CT/quartz formation and the value of the primary opal-CT d-spacing, are influenced by the sediment. lithology. Transmission electron microscopy methods (CTEM/HRTEM) were used to investigate the structure of the diagenetic phases and establish transformation mechanisms between the varieties of microcrystalline opals in charts and porcelanites from the Monterey Formation. HRTEM images revealed that the most common fibrous varieties of microcrystalline opals contain varying amounts of structural disorder. Finite lamellar units of cristobalite-and tridymite-type. layer sequences were found to be randomly stacked in a direction perpendicular to the fiber axis. Disordered and ordered fibers were found to have coprecipitated within the same radial fiber bundles that formed within the matrix of the Most siliceous samples. HRTEM images, which reveal that the fibers within radial and lepispheric fiber bundles branch non-crystallographically, support an earlier proposal that microspheres in chert grow via a spherulitic growth mechanism. A less common variety of opal-CT was found to be characterized by non-parallel (low-angle) stacking sequences that often contain twinned lamellae. Tabular-shaped crystals of orthorhombic tridymite (PO-2) were also identified in the porcelanite samples. A shift in the primary d-spacing of opal-CT has been interpreted as an indication of solid-state ordering g toward a predominantly cristobalite structure, (opal-C). Domains of opal-C were identified as topotactically-oriented overgrowths on discrete Sections of opal-CT fibers and as

Preparation and physicochemical characterization of cellulose nanocrystals from industrial waste cotton

NASA Astrophysics Data System (ADS)

Thambiraj, S.; Ravi Shankaran, D.

2017-08-01

We aimed to develop a simple and low-cost method for the production of high-performance cellulose nanomaterials from renewable and sustainable resources. Here, cellulose microcrystals (CMCs) were prepared by controlled acidic and basic hydrolysis of cotton from textile industry wastes. The resulted CMCs were further converted into cellulose nanocrystals (CNCs) with high crystallinity by acidic hydrolysis. The physicochemical characteristics and morphological feature of CMCs and CNCs were studied by various analytical techniques such as UV-vis spectroscopy, Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Fluorescence spectroscopy, Atomic force microscopy (AFM), High-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The isolated CNCs possess a needle-like morphological structure with the longitudinal and lateral dimensions of 180 ± 60 nm, 10 ± 1 nm, respectively. The AFM result reveals that the CNCs have a high aspect ratio of 40 ± 14 nm and the average thickness of 6.5 nm. The XRD and TEM analysis indicate that the synthesized CNCs possess face-centered cubic crystal structure. Preliminary experiments were carried out to fabricate CNCs incorporated poly (vinyl alcohol) (PVA) film. The results suggest that the concept of waste to wealth could be well executed from the prepared CNCs, which have great potential for various applications including bio-sensors, food packaging and drug delivery applications.

High-resolution transmission electron microscopy studies of graphite materials prepared by high-temperature treatment of unburned carbon concentrates from combustion fly ashes

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

Miguel Cabielles; Jean-Nol Rouzaud; Ana B. Garcia

2009-01-15

High-resolution transmission electron microscopy (HRTEM) has been used in this work to study the microstructural (structure and microtexture) changes occurring during the high-temperature treatment of the unburned carbon concentrates from coal combustion fly ashes. Emphasis was placed on two aspects: (i) the development of graphitic carbon structures and (ii) the disordered carbon forms remaining in the graphitized samples. In addition, by coupling HRTEM with energy-dispersive spectroscopy, the transformations with the temperature of the inorganic matter (mainly iron- and silicon-based phases) of the unburned carbon concentrates were evidenced. The HRTEM results were compared to the averaged structural order of the materialsmore » as evaluated by X-ray diffraction (XRD) and Raman spectroscopy. As indicated by XRD and Raman parameters, more-ordered materials were obtained from the unburned carbon concentrates with higher mineral/inorganic matter, thus inferring the catalytic effect of some of their components. However, the average character of the information provided by these instrumental techniques seems to be inconclusive in discriminating between carbon structures with different degrees of order (stricto sensu graphite, graphitic, turbostratic, etc.) in a given graphitized unburned carbon. Unlike XRD and Raman, HRTEM is a useful tool for imaging directly the profile of the polyaromatic layers (graphene planes), thus allowing the sample heterogeneity to be looked at, specifically the presence of disordered carbon phases. 49 refs., 9 figs., 3 tabs.« less

Comparison of antibacterial activities of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles

NASA Astrophysics Data System (ADS)

Dhanalekshmi, K. I.; Meena, K. S.

2014-07-01

Core-shell type Ag@TiO2 nanoparticles were prepared by one pot simultaneous reduction of AgNO3 and hydrolysis of Ti (IV) isopropoxide and Ag@SiO2 core-shell nanoparticles were prepared by Stober's method. They were characterized by absorption, XRD, and HR-TEM techniques. XRD patterns show the presence of anatase form of TiO2 and amorphous form of SiO2 and the noble metal (Ag). High resolution transmission electron microscopy measurements revealed that their size is below 50 nm. The antibacterial properties of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were examined by the agar diffusion method. As a result E. coli and S. aureus were shown to be substantially inhibited by Ag@TiO2 and Ag@SiO2 core-shell nanoparticles. These results demonstrated that TiO2 and SiO2 supported on the surface of Ag NPs without aggregation was proved to have enhanced antibacterial activity.

Comparison of antibacterial activities of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles.

PubMed

Dhanalekshmi, K I; Meena, K S

2014-07-15

Core-shell type Ag@TiO2 nanoparticles were prepared by one pot simultaneous reduction of AgNO3 and hydrolysis of Ti (IV) isopropoxide and Ag@SiO2 core-shell nanoparticles were prepared by Stober's method. They were characterized by absorption, XRD, and HR-TEM techniques. XRD patterns show the presence of anatase form of TiO2 and amorphous form of SiO2 and the noble metal (Ag). High resolution transmission electron microscopy measurements revealed that their size is below 50 nm. The antibacterial properties of Ag@TiO2 and Ag@SiO2 core-shell nanoparticles against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were examined by the agar diffusion method. As a result E. coli and S. aureus were shown to be substantially inhibited by Ag@TiO2 and Ag@SiO2 core-shell nanoparticles. These results demonstrated that TiO2 and SiO2 supported on the surface of Ag NPs without aggregation was proved to have enhanced antibacterial activity. Copyright © 2014 Elsevier B.V. All rights reserved.

Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Optical and structural properties of Mo-doped NiTiO3 materials synthesized via modified Pechini methods

NASA Astrophysics Data System (ADS)

Pham, Thanh-Truc; Kang, Sung Gu; Shin, Eun Woo

2017-07-01

In this study, molybdenum (Mo)-doped nickel titanate (NiTiO3) materials were successfully synthesized as a function of Mo content through a modified Pechini method followed by a solvothermal treatment process. Various characterization methods were employed to investigate the optical and structural properties of the materials. XRD patterns clearly showed that the NiTiO3 structure maintained a single phase with no observed crystalline structure transformations, even after the addition of 10 wt.% Mo. In the Raman spectra and XRD patterns, peak positions shifted with a change in Mo content, confirming that the NiTiO3 lattice was doped with Mo. On the other hand, Mo doping of NiTiO3 materials changed their optical properties. DRS-UV demonstrated that the addition of Mo increased photon absorption within the UV region. Relaxation processes were inhibited by Mo doping, which was evident in the PL spectra. Structural properties of the prepared materials were studied via FE-SEM and HR-TEM. The measured surface area increased proportionally with Mo content due to a reduction in grain size of the materials.

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

NASA Astrophysics Data System (ADS)

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

2012-11-01

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

Shape-controlled solvothermal synthesis of bismuth subcarbonate nanomaterials

NASA Astrophysics Data System (ADS)

Cheng, Gang; Yang, Hanmin; Rong, Kaifeng; Lu, Zhong; Yu, Xianglin; Chen, Rong

2010-08-01

Much effort has been devoted to the synthesis of novel nanostructured materials because of their unique properties and potential applications. Bismuth subcarbonate ((BiO) 2CO 3) is one of commonly used antibacterial agents against Helicobacter pylori ( H. pylori). Different (BiO) 2CO 3 nanostructures such as cube-like nanoparticles, nanobars and nanoplates, were fabricated from bismuth nitrate via a simple solvothermal method. The nanostructures were characterized by powder X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). It was found that the solvents and precursors have an influence on the morphologies of (BiO) 2CO 3 nanostructures. The possible formation mechanism of different (BiO) 2CO 3 nanostructures fabricated under different conditions was also discussed.

Characterisation of phases in nanostructured, multilayered titanium alloys by analytical and high-resolution electron microscopy.

PubMed

Czyrska-Filemonowicz, A; Buffat, P A

2009-01-01

Surface processing of a Ti-6Al-4V alloy led to a complex multilayered microstructure containing several phases of the Ni-Ti-P-Al-O system, which improves the mechanical and tribological surface properties. The microstructure, chemical and phase compositions of the hard layer formed on the surface were investigated by LM, XRD, SEM as well as analytical/high-resolution TEM, STEM, EDS, electron diffraction and FIB. Phase identification based on electron diffraction, HRTEM and EDS microanalysis revealed the presence of several binary and ternary phases in the system Ti-Ni-P, sometimes with partial substitution of Ti by Al. However some phases, mainly nanoparticles, still remain not identified satisfactorily. Electron microscopy techniques used for identification of phases present in surface multilayers and some practical limits to their routine application are reminded here.

Fabrication of Poly(styrene-co-maleic anhydride)@Ag Spheres with High Surface Charge Intensity and their Self-Assembly into Photonic Crystal Films.

PubMed

Bi, Jiajie; Fan, Genrui; Wu, Suli; Su, Xin; Xia, Hongbo; Zhang, Shu-Fen

2017-10-01

Herein, we developed a method to prepare monodisperse poly(styrene-co-maleic anhydride)@Ag (PSMA@Ag) core-shell microspheres with high surface charge intensity by using an in situ reduction method. In this method, ethylenediamine tetraacetic acid tetrasodium salt (Na 4 EDTA) was used as a reducing agent to promote the growth of Ag, and at the same time endowed the PSMA@Ag spheres with a surface charge. The monodispersity of PSMA and PSMA@Ag and the ordered array of the photonic crystal films were characterized by using SEM. The formation of Ag nanoparticles was confirmed by using TEM, HR-TEM, and XRD characterizations. Due to the existence of surface charges, the obtained PSMA@Ag microspheres easily self-assembled to form photonic crystal structures. In addition, the surface-enhanced Raman scattering (SERS) activity of the PSMA@Ag photonic crystal films was evaluated by detecting the signal from Raman probe molecules, 4-aminothiophenol (4-ATP). The PSMA@Ag photonic crystal films exhibited a high SERS effect, a low detection limit of up to 10 -8 for 4-ATP, good uniformity, and reproducibility.

Facile fabrication of BiOI decorated NaNbO3 cubes: A p-n junction photocatalyst with improved visible-light activity

NASA Astrophysics Data System (ADS)

Sun, Meng; Yan, Qing; Shao, Yu; Wang, Changqian; Yan, Tao; Ji, Pengge; Du, Bin

2017-09-01

To enhance the separation efficiency of photo-generated carriers, a p-n junction photocatalyst BiOI/NaNbO3 has been fabricated by a facile method. The obtained samples were characterized by XRD, SEM, TEM, HRTEM, PL, N2 sorption-desorption and DRS. DRS results showed that the light absorption edges of BiOI/NaNbO3 hybrids were red-shifted with the increase of BiOI content. The SEM and TEM images revealed that the BiOI was widely decorated over the surfaces of NaNbO3 cubes. The formation of p-n heterojunction at their interfaces was proved by the HRTEM image. The visible light-driven photocatalytic activity was evaluated by the degradation of methylene blue (MB) in aqueous solution. Compared with single NaNbO3 and BiOI, the BiOI/NaNbO3 hybrid photocatalysts have exhibited significantly enhanced activities. Meanwhile, the mass ratio of BiOI/NaNbO3 displayed important influence on the MB degradation. The hybrid photocatalyst with BiOI content of 40% performed the optimal activity. This activity enhancement should be attributed to the strong visible light absorption, the high migration and separation efficiency of photo-induced carriers. The photocurrent and PL measurements confirmed that the interfacial charge separation efficiency was greatly improved by coupling BiOI with NaNbO3. Controlled experiments proved that the degradation of pollutants was mainly attributed to the oxidizing ability of the generated holes (h+), ·O2-, and ·OH radicals.

Effective coating of titania nanoparticles with alumina via atomic layer deposition

NASA Astrophysics Data System (ADS)

Azizpour, H.; Talebi, M.; Tichelaar, F. D.; Sotudeh-Gharebagh, R.; Guo, J.; van Ommen, J. R.; Mostoufi, N.

2017-12-01

Alumina films were deposited on titania nanoparticles via atomic layer deposition (ALD) in a fluidized bed reactor at 180 °C and 1 bar. Online mass spectrometry was used for real time monitoring of effluent gases from the reactor during each reaction cycle in order to determine the optimal dosing time of precursors. Different oxygen sources were used to see which oxygen source, in combination with trimethyl aluminium (TMA), provides the highest alumina growth per cycle (GPC). Experiments were carried out in 4, 7 and 10 cycles using the optimal dosing time of precursors. Several characterization methods, such as high resolution transmission electron microscopy (HRTEM), Brunauer-Emmett-Teller (BET), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR), X-ray diffraction (XRD) and instrumental neutron activation analysis (INAA), were conducted on the products. Formation of the alumina film was confirmed by EDX mapping and EDX line profiling, FTIR and TEM. When using either water or deuterium oxide as the oxygen source, the thickness of the alumina film was greater than that of ozone. The average GPC measured by TEM for the ALD of TMA with water, deuterium oxide and ozone was about 0.16 nm, 0.15 nm and 0.11 nm, respectively. The average GPC calculated using the mass fraction of aluminum from INAA was close to those measured from TEM images. Excess amounts of precursors lead to a higher average growth of alumina film per cycle due to insufficient purging time. XRD analysis demonstrated that amorphous alumina was coated on titania nanoparticles. This amorphous layer was easily distinguished from the crystalline core in the TEM images. Decrease in the photocatalytic activity of titania nanoparticles after alumina coating was confirmed by measuring degradation of Rhodamine B by ultraviolet irradiation.

Influence of total beam current on HRTEM image resolution in differentially pumped ETEM with nitrogen gas.

PubMed

Bright, A N; Yoshida, K; Tanaka, N

2013-01-01

Environmental transmission electron microscopy (ETEM) enables the study of catalytic and other reaction processes as they occur with Angstrom-level resolution. The microscope used is a dedicated ETEM (Titan ETEM, FEI Company) with a differential pumping vacuum system and apertures, allowing aberration corrected high-resolution transmission electron microscopy (HRTEM) imaging to be performed with gas pressures up to 20 mbar in the sample area and with significant advantages over membrane-type E-cell holders. The effect on image resolution of varying the nitrogen gas pressure, electron beam current density and total beam current were measured using information limit (Young's fringes) on a standard cross grating sample and from silicon crystal lattice imaging. As expected, increasing gas pressure causes a decrease in HRTEM image resolution. However, the total electron beam current also causes big changes in the image resolution (lower beam current giving better resolution), whereas varying the beam current density has almost no effect on resolution, a result that has not been reported previously. This behavior is seen even with zero-loss filtered imaging, which we believe shows that the drop in resolution is caused by elastic scattering at gas ions created by the incident electron beam. Suitable conditions for acquiring high resolution images in a gas environment are discussed. Lattice images at nitrogen pressures up to 16 mbar are shown, with 0.12 nm information transfer at 4 mbar. Copyright © 2012 Elsevier B.V. All rights reserved.

Technical Evaluation Motor No. 7 (TEM-7)

NASA Technical Reports Server (NTRS)

Hughes, Phil

1991-01-01

The Technical Evaluation Motor No. 7 (TEM-7) test was a full-scale, full duration static test firing of a high performance motor-configuration solid rocket motor with nozzle vectoring. The final test report documents the procedures, performance, and results of the static test firing of TEM-7. All observations, discussions, conclusions, and recommendations included in the report are complete and final except for the TEM-7 fixed housing unbond investigation. A presentation and discussion of TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107, Rev A, Space Shuttle Technical Evaluation Motor No. 7 (TEM-7) Static Fire Test Plan are included.

In-situ heating TEM observation of microscopic structural changes of size-controlled metallic copper/gelatin composite.

PubMed

Narushima, Takashi; Hyono, Atsushi; Nishida, Naoki; Yonezawa, Tetsu

2012-10-01

Copper/gelatin composite particles with controlled sizes were prepared at room temperature from cupric sulfate pentahydrate in the presence of gelatin as a protective reagent by using hydrazine monohydrate as a reducing agent. The formed particles with the size between 190-940 nm were secondary aggregated particles which were composed of smaller nanosized particles ("particle-in-particle"), the presence of which was established by XRD patterns and a cross-sectional TEM image. The sintering behavior of these copper/gelatin composite particles was demonstrated by in-situ heating TEM under a high vacuum (approximately 10(-5) Pa) and separately with the oxygen partial pressure controlled at the 10(-4) Pa level. It was established that the particles began to sinter at about 330 degrees C with the oxygen and that they sublimate above 450 degrees C both in the vacuum and oxygen conditions. This result shows that the introduction of an adequate amount of oxygen was effective to remove the gelatin surrounding the particles. It can also be concluded that the sintering of the copper/gelatin composite particles occurred even in the absence of a reducing agent such as hydrogen gas.

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

PubMed

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

2017-06-01

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

Structural properties of ultrafine Ba-hexaferrite nanoparticles

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

Makovec, Darko, E-mail: Darko.Makovec@ijs.si; Primc, Darinka; Sturm, Saso

2012-12-15

Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was studied using X-ray diffractometry (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDXS), X-ray absorption fine structure (XAFS), and Moessbauer spectroscopy (MS), to be compared to the structure of larger nanoparticles and the bulk. The nanoparticles were synthesized with hydrothermal treatment of an appropriate suspension of Ba and Fe hydroxides in the presence of a large excess of OH{sup -}. The ultrafine nanoparticles were formed in a discoid shape, {approx}10 nm wide and only {approx}3 nm thick, comparable to the size of the hexagonal unit cell in the c-direction.more » The HRTEM image analysis confirmed the hexaferrite structure, whereas EDXS showed the composition matching the BaFe{sub 12}O{sub 19} formula. XAFS and MS analyses showed considerable disorder of the structure, most probably responsible for the low magnetization. - Graphical abstract: Left: HREM image of an ultrafine Ba-hexaferrite nanoparticle (inset: TEM image of the nanoparticles); Right: the experimental HRTEM image is compared with calculated image and corresponding atomic model. Highlights: Black-Right-Pointing-Pointer Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was compared to the structure of the bulk. Black-Right-Pointing-Pointer Thickness the discoid nanoparticles was comparable to the size of the hexagonal unit cell in the c-direction. Black-Right-Pointing-Pointer Considerable disorder of the nanoparticles' structure is most probably responsible for their low magnetization.« less

Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

NASA Technical Reports Server (NTRS)

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

2001-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Ultrasound with low intensity assisted the synthesis of nanocrystalline TiO2 without calcination.

PubMed

Ghows, Narjes; Entezari, Mohamad H

2010-06-01

A novel method has been developed for the preparation of nano-sized TiO(2) with anatase phase. Nanoparticles with diameter about 6 nm were prepared at a relatively low temperature (75 degrees C) and short time. The synthesis was carried out by the hydrolysis of titanium tetra-isopropoxide (TTIP) in the presence of water, ethanol, and dispersant under ultrasonic irradiation (500 kHz) at low intensity. The results show that variables such as water/ethanol ratio, irradiation time, and temperature have a great influence on the particle size and crystalline phases of TiO(2) nanoparticles. Characterization of the product was carried out by different techniques such as powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and UV-vis spectroscopy. (c) 2010 Elsevier B.V. All rights reserved.

Synthesis of boron nitride coatings on quartz fibers: Thickness control and mechanism research

NASA Astrophysics Data System (ADS)

Zheng, Yu; Wang, Shubin

2011-10-01

Boron nitride (BN) coatings were successfully synthesized on quartz fibers by dip-coating in boric acid and urea solutions at 700 °C. The SEM micrographs indicated that the quartz fibers were fully covered by coatings with smooth surface. The XRD, FT-IR, XPS spectra and HR-TEM results showed that the composition of the coatings which combined closely with the quartz fibers was polycrystalline h-BN. By changing the dip circles, the coating thickness was well controlled. The thicknesses of samples dipped less than six circles increased linearly with dipping-circles; and the increment of coating thickness would slow down when the fibers were dipped 10 circles. After being dipped for 10 circles, the thickness was about 300 nm. The coating thickness was also established by calculation and the calculated results were consistent with the results measured by micrograph.

Anisotropic growth of hydroxyapatite on the silk fibroin films

NASA Astrophysics Data System (ADS)

Li, Yucheng; Cai, Yurong; Kong, Xiangdong; Yao, Juming

2008-12-01

Bombyx mori silk fibroin is of practical interest for its excellent intrinsic properties utilizable in the biotechnological and biomedical fields. Here, the silk fibroin films were pretreated with different methods and then used as the template for the hydroxyapatite (HA) crystal growth. To study the effect of silk films' surface structure on the protein biomineralization, the films were immersed into 1.5 times simulated body fluid (1.5 × SBF) to induce the HA deposition at 37 °C. The results showed that an anisotropic growth of HA crystals was observed on the different films as judging from XRD, TEM and HRTEM data. This was thought that the positions and density of carboxyl groups, C dbnd O and amino groups on the surface of SF films may be different, which play the key effect on HA crystal growth.

Efficient production of ultrapure manganese oxides via electrodeposition.

PubMed

Cheney, Marcos A; Joo, Sang Woo; Banerjee, Arghya; Min, Bong-Ki

2012-08-01

A new process for the production of electrolytic amorphous nanomanganese oxides (EAMD) with uniform size and morphology is described. EAMD are produced for the first time by cathodic deposition from a basic aqueous solution of potassium permanganate at a constant temperature of 16°C. The synthesized materials are characterized by XRD, SEM, TEM, and HRTEM. The materials produced at 5.0 V at constant temperature are amorphous with homogeneous size and morphology with an average particle size around 20 nm, which appears to be much lesser than the previously reported anodic EAMD. A potentiostatic electrodeposition with much lesser deposition rate (with respect to previously reported anodic depositions) is considered to be the reason behind the very low and homogenous particle size distribution due to the lesser agglomeration of our as-synthesized nanoparticles. Copyright © 2012 Elsevier Inc. All rights reserved.

Technical Evaluation Motor No. 10 (TEM-10)

NASA Technical Reports Server (NTRS)

1993-01-01

Technical Evaluation Motor No. 10 (TEM-10) was static fired on 27 Apr. 1993 at the Thiokol Corporation full-scale motor static test bay, T-24. This final test report documents the procedures, performance, and results of the static test firing of TEM-10. All observations, discussions, conclusions, and recommendations contained are final. Included is a presentation and discussion of TEM-10 performance, anomalies, and test results in concurrence with the objectives outlined in CTP-0110, Revision D, Space Shuttle Technical Evaluation Motor No. 10 (TEM-10) Static Fire Test Plan.

Nano-Crystalline Diamond Films with Pineapple-Like Morphology Grown by the DC Arcjet vapor Deposition Method

NASA Astrophysics Data System (ADS)

Li, Bin; Zhang, Qin-Jian; Shi, Yan-Chao; Li, Jia-Jun; Li, Hong; Lu, Fan-Xiu; Chen, Guang-Chao

2014-08-01

A nano-crystlline diamond film is grown by the dc arcjet chemical vapor deposition method. The film is characterized by scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), x-ray diffraction (XRD) and Raman spectra, respectively. The nanocrystalline grains are averagely with 80 nm in the size measured by XRD, and further proven by Raman and HRTEM. The observed novel morphology of the growth surface, pineapple-like morphology, is constructed by cubo-octahedral growth zones with a smooth faceted top surface and coarse side surfaces. The as-grown film possesses (100) dominant surface containing a little amorphous sp2 component, which is far different from the nano-crystalline film with the usual cauliflower-like morphology.

Compressive Classification for TEM-EELS

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

Hao, Weituo; Stevens, Andrew; Yang, Hao

Electron energy loss spectroscopy (EELS) is typically conducted in STEM mode with a spectrometer, or in TEM mode with energy selction. These methods produce a 3D data set (x, y, energy). Some compressive sensing [1,2] and inpainting [3,4,5] approaches have been proposed for recovering a full set of spectra from compressed measurements. In many cases the final form of the spectral data is an elemental map (an image with channels corresponding to elements). This means that most of the collected data is unused or summarized. We propose a method to directly recover the elemental map with reduced dose and acquisitionmore » time. We have designed a new computational TEM sensor for compressive classification [6,7] of energy loss spectra called TEM-EELS.« less

Extracellular red Monascus pigment-mediated rapid one-step synthesis of silver nanoparticles and its application in biomedical and environment.

PubMed

Koli, Sunil H; Mohite, Bhavana V; Suryawanshi, Rahul K; Borase, Hemant P; Patil, Satish V

2018-05-01

The development of a safe and eco-friendly method for metal nanoparticle synthesis has an increasing demand, due to emerging environmental and biological harms of hazardous chemicals used in existing nanosynthesis methods. The present investigation reports a rapid one-step, eco-friendly and green approach for the formation of nanosized silver particles (AgNPs) using extracellular non-toxic-colored fungal metabolites (Monascus pigments-MPs). The formation of nanosized silver particles utilizing Monascus pigments was confirmed after exposure of reaction mixture to sunlight, by visually color change and further established by spectrophotometric analysis. The size, shape, and topography of synthesized MPs-AgNPs were well-defined using different microscopic and spectroscopic techniques, i.e., FE-SEM, HR-TEM, and DLS. The average size of MPs-AgNPs was found to be 10-40 nm with a spherical shape which was highly stable and dispersed in the solution. HR-TEM and XRD confirmed crystalline nature of MPs-AgNPs. The biocidal potential of MPs-AgNPs was evaluated against three bacterial pathogens such as Pseudomonas aeruginosa, Escherichia coli, and Staphylococcus aureus and it was observed that the MPs-AgNPs significantly inhibited the growth of all three bacterial pathogens. The anti-biofilm activity of MPs-AgNPs was recorded against antibiotic-resistant P. aeruginosa. Besides, the colorimetric metal sensing using MPs-AgNPs was studied. Among the metals tested, the selective Hg 2+ -sensing potential at micromolar concentration was observed. In conclusion, this is the rapid one-step (within 12-15 min), environment-friendly method for synthesis of AgNPs and synthesized MPs-AgNPs could be used as a potential antibacterial agent against antibiotic-resistant bacterial pathogens.

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

PubMed

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

2017-09-01

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

Synthesis of AuPd alloyed nanoparticles via room-temperature electron reduction with argon glow discharge as electron source.

PubMed

Yang, Manman; Wang, Zongyuan; Wang, Wei; Liu, Chang-Jun

2014-01-01

Argon glow discharge has been employed as a cheap, environmentally friendly, and convenient electron source for simultaneous reduction of HAuCl4 and PdCl2 on the anodic aluminum oxide (AAO) substrate. The thermal imaging confirms that the synthesis is operated at room temperature. The reduction is conducted with a short time (30 min) under the pressure of approximately 100 Pa. This room-temperature electron reduction operates in a dry way and requires neither hydrogen nor extra heating nor chemical reducing agent. The analyses using X-ray photoelectron spectroscopy (XPS) confirm all the metallic ions have been reduced. The characterization with X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) shows that AuPd alloyed nanoparticles are formed. There also exist some highly dispersed Au and Pd monometallic particles that cannot be detected by XRD and transmission electron microscopy (TEM) because of their small particle sizes. The observed AuPd alloyed nanoparticles are spherical with an average size of 14 nm. No core-shell structure can be observed. The room-temperature electron reduction can be operated in a larger scale. It is an easy way for the synthesis of AuPd alloyed nanoparticles.

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

PubMed

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

2012-04-01

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

One-step growth of nanosheet-assembled BiOCl/BiOBr microspheres for highly efficient visible photocatalytic performance

NASA Astrophysics Data System (ADS)

Zhang, Jinfeng; Lv, Jiali; Dai, Kai; Liang, Changhao; Liu, Qi

2018-02-01

In this work, we have developed a simple synthetic approach of nanosheet-assembled BiOCl/BiOBr microspheres by an ethylene glycol (EG)-assisted hydrothermal method. The crystalline form, morphology, chemical composition, optical performance and surface area of BiOCl/BiOBr microspheres were identified using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HRTEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy spectra (EDX), UV-vis diffuse reflectance spectroscopy (DRS) analysis, high resolution X-ray photoelectron spectra (XPS) and N2 adsorption-desorption isotherms. BiOCl/BiOBr microspheres were nanosheet-assembled particles, which possessed visible light absorption under LED light irridation. Additionally, the methylene blue (MB) photodegradation performance of different BiOCl/BiOBr microspheres irradiated under 410 nm LED light arrays were investigated, the results exhibited that as-prepared BiOCl/BiOBr products showed higher catalytic effiency than pure BiOCl or BiOBr. By optimizing the composition ration of the BiOCl and BiOBr, up to 93% degradation rate can be obtained in the 40%BiOCl/BiOBr microspheres. Finally, the photocatalytic mechanism of BiOCl/BiOBr microspheres had been proposed.

Methodical thermolysis of [Ba2Ti2(thd)4(OnPr)8(nPrOH)2] under autogenous pressure followed by combustion for the synthesis of dielectric tetragonal BaTiO3 nanopowder.

PubMed

Pol, Vilas G; Thiyagarajan, P; Moreno, Jose M Calderon; Popa, Monica; Kessler, Vadim G; Gohil, Suresh; Seisenbaeva, Gulaim A

2009-07-06

The tetragonal BaTiO(3) nanopowder is synthesized in a solvent-less, efficient process by the thermolysis of a single [Ba(2)Ti(2)(thd)(4)(OnPr)(8)(nPrOH)(2)] precursor in a closed reactor at 700 degrees C under autogenous pressure, followed by combustion. This paper compiles the synthesis of the [Ba(2)Ti(2)(thd)(4)(OnPr)(8)(nPrOH)(2)] precursor, its analysis by mass spectrometry, and implementation for the fabrication of dielectric tetragonal BaTiO(3) nanopowder by controlled efficient thermal decomposition. The as-prepared, intermediate, and final forms of the obtained nanomaterials are systematically analysed by XRD, Raman, and EDS measurements to gain structural and compositional information. Employing HR-SEM, TEM, and HR-TEM techniques, the morphological changes during the structural evolution of all the phases are pursued. The mechanistic elucidation for the fabrication of BaTiO(3) nanopowder is developed on the basis of TGA and DTA data obtained for the initial [Ba(2)Ti(2)(thd)(4)(OnPr)(8)(nPrOH)(2)] reactant as well as the as-prepared BaCO(3) with amorphous Ti phase.

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

NASA Astrophysics Data System (ADS)

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

2015-01-01

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

Recognition and Resistance in TEM [superscript beta]-Lactamase

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

Wang, Xiaojun; Minasov, George; Blazquez, Jesus

Developing antimicrobials that are less likely to engender resistance has become an important design criterion as more and more drugs fall victim to resistance mutations. One hypothesis is that the more closely an inhibitor resembles a substrate, the more difficult it will be to develop resistant mutations that can at once disfavor the inhibitor and still recognize the substrate. To investigate this hypothesis, 10 transition-state analogues, of greater or lesser similarity to substrates, were tested for inhibition of TEM-1 beta-lactamase, the most widespread resistance enzyme to penicillin antibiotics. The inhibitors were also tested against four characteristic mutant enzymes: TEM-30, TEM-32,more » TEM-52, and TEM-64. The inhibitor most similar to the substrate, compound 10, was the most potent inhibitor of the WT enzyme, with a K(i) value of 64 nM. Conversely, compound 10 was the most susceptible to the TEM-30 (R244S) mutant, for which inhibition dropped by over 100-fold. The other inhibitors were relatively impervious to the TEM-30 mutant enzyme. To understand recognition and resistance to these transition-state analogues, the structures of four of these inhibitors in complex with TEM-1 were determined by X-ray crystallography. These structures suggest a structural basis for distinguishing inhibitors that mimic the acylation transition state and those that mimic the deacylation transition state; they also suggest how TEM-30 reduces the affinity of compound 10. In cell culture, this inhibitor reversed the resistance of bacteria to ampicillin, reducing minimum inhibitory concentrations of this penicillin by between 4- and 64-fold, depending on the strain of bacteria. Notwithstanding this activity, the resistance of TEM-30, which is already extant in the clinic, suggests that there can be resistance liabilities with substrate-based design.« less

Photocatalytic mechanism of high-activity anatase TiO2 with exposed (001) facets from molecular-atomic scale: HRTEM and Raman studies

NASA Astrophysics Data System (ADS)

Wu, Jun; Shi, Chentian; Zhang, Yupeng; Fu, Qiang; Pan, Chunxu

2017-12-01

Anatase TiO2 with a variant percentage of exposed (001) facets was prepared under hydrothermal processes by adjusting the volume of HF, and the photocatalytic mechanism was studied from atomic-molecular scale by HRTEM and Raman spectroscopy. It was revealed that: 1) From HRTEM observations, the surface of original TiO2 with exposed (001) facets was clean without impurity, and the crystal lattice was clear and completed; however, when mixed with methylene blue (MB) solution, there were many 1 nm molecular absorbed at the surface of TiO2; after the photocatalytic experiment, MB molecules disappeared and the TiO2 lattice image became fuzzy. 2) The broken path of the MB chemical bond was obtained by Raman spectroscopy, i.e., after the irradiation of the light, the vibrational mode of C-N-C disappeared due to the chemical bond breakage, and the groups containing C-N bond and carbon rings were gradually decomposed. Accordingly, we propose that the driving force for breaking the chemical bond and the disappearance of groups is from the surface lattice distortion of TiO2 during photocatalyzation.

Two-phase nc-TiN/a-(C,CN{sub x}) nanocomposite films: A HRTEM and MC simulation study

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

Guo, J.; Lu, Y. H.; Hu, X. J.

2013-06-18

The grain growth in two-phase nanocomposite Ti-C{sub x}-N{sub y} thin films grown by reactive close-field unbalanced magnetron sputtering in an Ar-N{sub 2} gas mixture with microstructures comprising of nanocrystalline (nc-) Ti(N,C) phase surrounded by amorphous (a-) (C,CN{sub x}) phase was investigated by a combination of high-resolution transmission electron microscopy (HRTEM) and Monte Carlo (MC) simulations. The HRTEM results revealed that amorphous-free solid solution Ti(C,N) thin films exhibited polycrystallites with different sizes, orientations and irregular shapes. The grain size varied in the range between several nanometers and several decade nanometers. Further increase of C content (up to {approx}19 at.% C) mademore » the amorphous phase wet nanocrystallites, which strongly hindered the growth of nanocrystallites. As a result, more regular Ti(C,N) nanocrystallites with an average size of {approx}5 nm were found to be separated by {approx}0.5-nm amorphous phases. When C content was further increased (up to {approx}48 at.% in this study), thicker amorphous matrices were produced and followed by the formation of smaller sized grains with lognormal distribution. Our MC analysis indicated that with increasing amorphous volume fraction (i.e. increasing C content), the transformation from nc/nc grain boundary (GB)-curvature-driven growth to a/nc GB-curvature-driven growth is directly responsible for the observed grain growth from great inhomogeneity to homogeneity process.« less

A comparative study: Effect of plasma on V2O5 nanostructured thin films

NASA Astrophysics Data System (ADS)

Singh, Megha; Kumar, Prabhat; Sharma, Rabindar K.; Reddy, G. B.

2016-05-01

Vanadium pentoxide nanostructured thin films (NSTs) have been studied to analyze the effect of plasma on nanostructures grown and morphology of films deposited using sublimation process. Nanostructured thin films were deposited on glass substrates, one in presence of oxygen plasma and other in oxygen environment (absence of plasma). Films were characterized using XRD, Raman spectroscopy, SEM and HRTEM. XRD studies revealed α-V2O5 films (orthorhombic phase) with good crystallinity. However, film deposited in presence of plasma have higher peak intensities as compared to those deposited in absence of plasma. Raman studies also support these finding following same trends of considerable increase in intensity in case of film deposited in presence of plasma. SEM micrographs makes the difference more visible, as film deposited in plasma have well defined plate like structures whereas other film have not-clearly-defined petal-like structures. HRTEM results show orthorhombic phase with 0.39 nm interplanar spacing, as reported by XRD. Results are hereby in good agreement with each other.

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

NASA Technical Reports Server (NTRS)

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

2000-01-01

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

Technical Evaluation Motor no. 5 (TEM-5)

NASA Technical Reports Server (NTRS)

Cook, M.

1990-01-01

Technical Evaluation Motor No. 5 (TEM-5) was static test fired at the Thiokol Corporation Static Test Bay T-97. TEM-5 was a full scale, full duration static test fire of a high performance motor (HPM) configuration solid rocket motor (SRM). The primary purpose of TEM static tests is to recover SRM case and nozzle hardware for use in the redesigned solid rocket motor (RSRM) flight program. Inspection and instrumentation data indicate that the TEM-5 static test firing was successful. The ambient temperature during the test was 41 F and the propellant mean bulk temperature (PMBT) was 72 F. Ballistics performance values were within the specified requirements. The overall performance of the TEM-5 components and test equipment was nominal. Dissembly inspection revealed that joint putty was in contact with the inner groove of the inner primary seal of the ignitor adapter-to-forward dome (inner) joint gasket; this condition had not occurred on any previous static test motor or flight RSRM. While no qualification issues were addressed on TEM-5, two significant component changes were evaluated. Those changes were a new vented assembly process for the case-to-nozzle joint and the installation of two redesigned field joint protection systems. Performance of the vented case-to-nozzle joint assembly was successful, and the assembly/performance differences between the two field joint protection system (FJPS) configurations were compared.

Plasma assisted synthesis of vanadium pentoxide nanoplates

NASA Astrophysics Data System (ADS)

Singh, Megha; Sharma, Rabindar Kumar; Kumar, Prabhat; Reddy, G. B.

2015-08-01

In this work, we report the growth of α-V2O5 (orthorhombic) nanoplates on glass substrate using plasma assisted sublimation process (PASP) and Nickel as catalyst. 100 nm thick film of Ni is deposited over glass substrate by thermal evaporation process. Vanadium oxide nanoplates have been deposited treating vanadium metal foil under high vacuum conditions with oxygen plasma. Vanadium foil is kept at fixed temperature growth of nanoplates of V2O5 to take place. Samples grown have been studied using XPS, XRD and HRTEM to confirm the growth of α-phase of V2O5, which revealed pure single crystal of α- V2O5 in orthorhombic crystallographic plane. Surface morphological studies using SEM and TEM show nanostructured thin film in form of plates. Uniform, vertically aligned randomly oriented nanoplates of V2O5 have been deposited.

Biosynthesis of ZnO nanoparticles using rambutan (Nephelium lappaceumL.) peel extract and their photocatalytic activity on methyl orange dye

NASA Astrophysics Data System (ADS)

Karnan, Thenmozhi; Selvakumar, Stanly Arul Samuel

2016-12-01

In the present study, describes the synthesis of ZnO nanoparticles from rambutan (Nephelium lappaceumL.) peel extract via bio synthesis method and developed a new low cost technology to prepare ZnO nanoparticles. During the synthesis, fruit peel extract act as a natural ligation agent. The successfully prepared product was analyzed with some standard characterization studies like X-Ray Diffraction (XRD), UV-VIS Diffuse reflectance spectra (UV-Vis DRS), Field Emission Scanning Electron Microscope (FESEM), High resolution transmittance electron microscope (HR-TEM), N2 adsorption-desorption isotherm and UV-Vis absorption Spectroscopy. The photocatalytic activity of ZnO nanoparticles was evaluated by photodegradation of methyl orange (MO) dye under UV light and the result depicts around 83.99% decolorisation efficiency at 120 min of illumination. In addition with photodecolorisation, mineralization was also achieved. The mineralization has been confirmed by measuring Chemical Oxygen Demand (COD) values.

Single-phase and well-dispersed Cu1.75S nanocrystals by ambient pressure diethylene glycol solution synthesis

NASA Astrophysics Data System (ADS)

Zheng, Xuerong; Jin, Zhengguo; Liu, Hui; Wang, Yueqiu; Wang, Xin; Du, Haiyan

2013-02-01

Single-phase, well-dispersed Cu1.75S nanocrystals were synthesized by an ambient pressure, hydrazine hydrate and ethylenediamine co-assisted diethylene glycol based solution chemical process using copper chloride and thioacetamide as precursors at the temperature range from 180 to 210 °C. Influence of hydrazine hydrate and ethylenediamine adding amounts, synthetic temperature on crystal growth, size distribution and optical properties of the synthesized Cu1.75S nanocrystals were investigated by XRD, TEM, HRTEM, EDX and UV-vis measurements. The synthetic reaction at above 200 °C grew flaky-shaped nanocrystals with relatively narrow size distribution. The formation of single-phase Cu1.75S nanocrystals in the diethylene glycol based solution process might be involved in the presence of intermediate [Cu(en)n]1+ and [Cu(NH3)4]2+ complexes in reaction solution, providing a stable Cu(I) and Cu(II) valent-mixed precursor.

Effect of Ce doping on structural, optical and photocatalytic properties of ZnO nano-structures.

PubMed

Selvam, N Clament Sagaya; Vijaya, J Judith; Kennedy, L John

2014-03-01

A novel self-assembled pure and Ce doped ZnO nano-particles (NPs) were successfully synthesized by a simple low temperature co-precipitation method. The prepared photocatalysts were characterized by X-ray diffraction (XRD), High resolution scanning electron microscopy (HR-SEM), High resolution transmission electron microscopy (HR-TEM), diffuse reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The results indicated that the prepared photocatalysts shows a novel morphology, high crystallinity, uniform size distribution, and more defects. Photocatalytic degradation (PCD) of nonylphenol, a potent endocrine disrupting chemical in aqueous medium was investigated. Higher amount of oxygen defects exhibits enhanced PCD of nonylphenol. In addition, the influence of the Ce contents on the structure, morphology, absorption, emission and photocatalytic activity of ZnO nanoparticles (NPs) were investigated systematically. The relative PCD efficiency of pure ZnO, Ce-doped ZnO NPs and commercial TiO2 (Degussa P-25) have also been discussed.

Ferromagnetically filled carbon nano-onions: the key role of sulfur in dimensional, structural and electric control

PubMed Central

Medranda, D.; Borowiec, J.; Zhang, Xiao; Wang, S.; Yan, K.; Zhang, J.; He, Y.; Ivaturi, S.

2018-01-01

A key challenge in the fabrication of ferromagnetically filled carbon nano-onions (CNOs) is the control of their thickness, dimensions and electric properties. Up to now literature works have mainly focused on the encapsulation of different types of ferromagnetic materials including α-Fe, Fe3C, Co, FeCo, FePd3 and others within CNOs. However, no report has yet shown a suitable method for controlling both the number of shells, diameter and electric properties of the produced CNOs. Here, we demonstrate an advanced chemical vapour deposition approach in which the use of small quantities of sulfur during the pyrolysis of ferrocene allows for the control of (i) the diameter of the CNOs, (ii) the number of shells and (iii) the electric properties. We demonstrate the morphological, structural, electric and magnetic properties of these new types of CNOs by using SEM, XRD, TEM, HRTEM, EIS and VSM techniques. PMID:29410810

Novel symmetrical coralloid Cu 3D superstructures: Solid-state synthesis from a Cu-carboxylate MOF and their in-situ thermal conversion

NASA Astrophysics Data System (ADS)

Chen, Lingyun; Shen, Yongming; Bai, Junfeng; Wang, Chunzhao

2009-08-01

We describe here a one-step solid-state process for the synthesis of metal three-dimensional (3D) superstructures from a metal-organic framework (MOF). Novel symmetrical coralloid Cu 3D superstructures with surface interspersed with clusters of Cu nanoparticles were successfully synthesized by thermolysis of the [Cu 3( btc) 2] ( btc=benzene-1,3,5-tricarboxylato) MOF in a one-end closed horizontal tube furnace (OCTF). The obtained products were characterized by TGA, FT-IR, XRD, EDX, SEM, TEM, HRTEM and SAED. Different reaction conditions were discussed. Furthermore, the synthesized Cu samples were converted into CuO microstructures by in-situ calcination in the air. In addition, the possible formation mechanism was also proposed. This method is a simple and facile route, which builds a direct linkage between metal-carboxylate MOF crystals and metal nano- or microstructures and also opens a new application field of MOFs.

In vitro antioxidant, antimicrobial, cytotoxic potential of gold and silver nanoparticles prepared using Embelia ribes.

PubMed

Dhayalan, Manikandan; Denison, Michael Immanuel Jesse; L, Anitha Jegadeeshwari; Krishnan, Kathiravan; N, Nagendra Gandhi

2017-02-01

In recent years, the green synthesis of gold (GNPs) and silver (SNPs) nanoparticles has gained great interest among chemists and researchers. The present study reports an eco-friendly, cost-effective, rapid and easy method for the synthesis of gold and silver nanoparticles using the seed extract of Embelia ribes (SEEr) as capping and reducing agent. The synthesised GNPs and SNPs were characterised using the following techniques: UV-vis spectroscopy, DLS, HR-TEM, FT-IR and XRD. The free radical scavenging potential of GNPs and SNPs was measured by DPPH assay and Phosphomolybdenum assay. Further, the antimicrobial activity against two micro-organisms were tested using disc diffusion method and cytotoxicity of GNPs and SNPs was determined against MCF-7 cell lines at different concentrations by MTT assay. Both the GNPs and SNPs prepared from E. ribes comparatively showed promising results thereby proving their clinical importance.

From waste to high-value product: Jackfruit peel derived pectin/apatite bionanocomposites for bone healing applications.

PubMed

Govindaraj, Dharman; Rajan, Mariappan; Hatamleh, Ashraf A; Munusamy, Murugan A

2018-01-01

Public requirements encouraged by the current asset framework drive industry to expand its general effectiveness by enhancing existing procedures or finding new uses for waste. Thus, the aim of this study was the isolation, fabrication, and characterization of pectin derived from jackfruit (Artocarpus heterophyllus) peels and the generation of hybrid of pectin (P)/apatite (HA) (P/HA) bionanocomposites. In this process, the natural pectin polymer derived from the peel of jackfruits was used in different concentrations for the fabrication of HA bionanocomposites. Characterization of the isolated pectin and bionanocomposites samples was performed with 1 H NMR and 13 C NMR, FTIR, XRD, SEM-EDX, and HR-TEM. Cytocompatibility, ALP, fibroblast stem cells, anti-inflammatory and cell adhesion testing of the fabricated bionanocomposites was showed good biocompatibility. Our results signify that the fabricated bionanocomposites might be applicable as bone graft materials. Copyright © 2017 Elsevier B.V. All rights reserved.

Controllable Fabrication and Optical Properties of Uniform Gadolinium Oxysulfate Hollow Spheres

PubMed Central

Chen, Fashen; Chen, Gen; Liu, Tao; Zhang, Ning; Liu, Xiaohe; Luo, Hongmei; Li, Junhui; Chen, Limiao; Ma, Renzhi; Qiu, Guanzhou

2015-01-01

Uniform gadolinium oxysulfate (Gd2O2SO4) hollow spheres were successfully fabricated by calcination of corresponding Gd-organic precursor obtained via a facile hydrothermal process. The Gd2O2SO4 hollow spheres have a mean diameter of approximately 550 nm and shell thickness in the range of 30–70 nm. The sizes and morphologies of as-prepared Gd2O2SO4 hollow spheres could be deliberately controlled by adjusting the experimental parameters. Eu-doped Gd2O2SO4 hollow spheres have also been prepared for the property modification and practical applications. The structure, morphology, and properties of as-prepared products were characterized by XRD, TEM, HRTEM, SEM and fluorescence spectrophotometer. Excited with ultraviolet (UV) pump laser, successful downconversion (DC) could be achieved for Eu-doped Gd2O2SO4 hollow spheres. PMID:26671661

Heterojunction CuO-TiO2 nanocomposite synthesis for significant photocatalytic hydrogen production

NASA Astrophysics Data System (ADS)

Manjunath, K.; Souza, V. S.; Ramakrishnappa, T.; Nagaraju, G.; Scholten, J. D.; Dupont, J.

2016-11-01

Effective and low-cost photocatalysts have been synthesized by a simple hydrothermal process. In this process, the two CuO and TiO2 bound one over the other and formed a heterojunction CuO-TiO2 nanocomposite. CuO serves as electron reservoir by receiving electrons from TiO2, which suppresses the recombination of e-/h+ and transfers the received electron to split water, which results in enhanced H2 production. Heterojunction CuO-TiO2 nanocomposite material recorded a maximum of 9284 μmolg-1 H2 production for 2.5 h. The recorded result is 15 times higher than bare TiO2 and 16 times higher than bare CuO. The synthesized materials were characterized and analyzed using various analytical techniques such as XRD, FTIR, UV-vis spectra and the morphology was studied using SEM, TEM, and HRTEM images.

Bio-derived hierarchically macro-meso-micro porous carbon anode for lithium/sodium ion batteries

NASA Astrophysics Data System (ADS)

Elizabeth, Indu; Singh, Bhanu Pratap; Trikha, Sunil; Gopukumar, Sukumaran

2016-10-01

Nitrogen doped hierarchically porous carbon derived from prawn shells have been efficiently synthesized through a simple, economically viable and environmentally benign approach. The prawn shell derived carbon (PSC) has high inherent nitrogen content (5.3%) and possesses a unique porous structure with the co-existence of macro, meso and micropores which can afford facile storage and transport channels for both Li and Na ions. PSC is well characterized using X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Transmission electron Microscopy (TEM), High resolution TEM (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Electron Paramagnetic Resonance (EPR) and Solid state-Nuclear Magnetic Resonance (NMR) studies have been conducted on pristine PSC and Li/Na interacted PSC. PSC as anode for Lithium ion batteries (LIBs) delivers superior electrochemical reversible specific capacity (740 mAh g-1 at 0.1 Ag-1 current density for 150 cycles) and high rate capability. When used as anode material for Sodium ion batteries (SIBs), PSC exhibits excellent reversible specific capacity of 325 mAh g-1 at 0.1 Ag-1 for 200 cycles and rate capability of 107 mAh g-1 at 2 Ag-1. Furthermore, this study demonstrates the employment of natural waste material as a potential anode for both LIB and SIB, which will definitively make a strike in the energy storage field.

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

2004-01-01

Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

TEM Derivative-Producing Enterobacter aerogenes Strains: Dissemination of a Prevalent Clone

PubMed Central

Dumarche, P.; De Champs, C.; Sirot, D.; Chanal, C.; Bonnet, R.; Sirot, J.

2002-01-01

TEM-24 (CAZ-6) extended-spectrum β-lactamase (ESBL) was detected in 1988 in Clermont-Ferrand, France, in Klebsiella pneumoniae (blaTEM-24) and Enterobacter aerogenes (blaTEM-24b), and since 1994, a TEM-24-producing E. aerogenes clonal strain has been observed elsewhere in the country. To determine if the spread of this clonal strain was restricted to TEM-24-producing E. aerogenes strains, 84 E. aerogenes strains (non-TEM/SHV-producing strains, TEM-1- or -2-producing strains, and different ESBL-producing strains), isolated from 1988 to 1999 in Clermont-Ferrand (n = 59) and in 11 other French hospitals in 1998 (n = 25), were studied. A clonal strain was found for TEM-24- but also for TEM-3- and TEM-1- or 2-producing isolates. This study shows that there is a clonal strain dependent on acquisition of the TEM-type enzyme (TEM-24 and other TEM types). PMID:11897606

Properties of CuInS₂ Nano-Particles on TiO₂ by Spray Pyrolysis for CuInS₂/TiO₂ Composite Solar Cell.

PubMed

Park, Gye-Choon; Li, Zhen-Yu; Yang, O-Bong

2017-04-01

In this letter, for the absorption layer of a CuInS₂/TiO₂ composite solar cell, I–III–VI2 chalcopyrite semiconductor CuInS₂ nano-particles were deposited by using spray pyrolysis method on TiO2 porous film. Their material characteristics including structural and optical properties of CuInS₂ nano-particles on TiO₂ nanorods were analyzed as a function of its composition ratios of Cu:In:S. Crystalline structure, surface morphology and crystalline size were also investigated by X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), and High-Resolution TEM (HRTEM), respectively. On the other hand, optical property was characterized by an UV-Visible Spectrophotometer. As a result, it was found that the size of CuInS₂ nano-particles, which was formed at 300±5 °C, was smaller than 16 nm from HRTEM analyses, and it was identified that the CuInS₂ particle size was increased as increasing the heat-treatment temperature and time. However, as the size of CuInS₂ nano-particle becomes smaller, optical absorption edge of ternary compound film tends to move to the blue wavelength band. It turns out that the optical energy-band gap of the compound films was ranging from 1.48 eV to 1.53 eV.

TEM PSHA2015 Reliability Assessment

NASA Astrophysics Data System (ADS)

Lee, Y.; Wang, Y. J.; Chan, C. H.; Ma, K. F.

2016-12-01

The Taiwan Earthquake Model (TEM) developed a new probabilistic seismic hazard analysis (PSHA) for determining the probability of exceedance (PoE) of ground motion over a specified period in Taiwan. To investigate the adequacy of the seismic source parameters adopted in the 2015 PSHA of the TEM (TEM PSHA2015), we conducted several tests of the seismic source models. The observed maximal peak ground acceleration (PGA) of the ML > 4.0 mainshocks in the 23-year data period of 1993-2015 were used to test the predicted PGA of PSHA from the areal and subduction zone sources with the time-independent Poisson assumption. This comparison excluded the observations from 1999 Chi-Chi earthquake, as this was the only earthquake associated with the identified active fault in this past 23 years. We used tornado diagrams to analyze the sensitivities of these source parameters to the ground motion values of the PSHA. This study showed that the predicted PGA for a 63% PoE in the 23-year period corresponded to the empirical PGA and the predicted numbers of PGA exceedances to a threshold value 0.1g close to the observed numbers, confirming the parameter applicability for the areal and subduction zone sources. We adopted the disaggregation analysis from a hazard map to determine the contribution of the individual seismic sources to hazard for six metropolitan cities in Taiwan. The sensitivity tests of the seismogenic structure parameters indicated that the slip rate and maximum magnitude are dominant factors for the TEM PSHA2015. For densely populated faults in SW Taiwan, maximum magnitude is more sensitive than the slip rate, giving the concern on the possible multiple fault segments rupture with larger magnitude in this area, which was not yet considered in TEM PSHA2015. The source category disaggregation also suggested that special attention is necessary for subduction zone earthquakes for long-period shaking seismic hazards in Northern Taiwan.

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

PubMed

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

2011-01-01

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

High performance Sb2S3/carbon composite with tailored artificial interface as an anode material for sodium ion batteries

NASA Astrophysics Data System (ADS)

Choi, Jeong-Hee; Ha, Chung-Wan; Choi, Hae-Young; Shin, Heon-Cheol; Lee, Sang-Min

2017-11-01

The electrochemical comparison between Sb2S3 and its composite with carbon (Sb2S3/C) involved by sodium ion carrier are explained by enhanced kinetics, particularly with respect to improved interfacial conductivity by surface modulation by carbon. Sb2S3 and Sb2S3/C are synthesized by a high energy mechanical milling process. The successful synthesis of these materials is confirmed with X-ray diffraction (XRD), scanning electron microscopy, and transmission electron microscopy (TEM). As an anode material for sodium ion batteries, Sb2S3 exhibits an initial sodiation/desodiation capacity of 1,021/523 mAh g-1 whereas the Sb2S3/C composite exhibits a higher reversible capacity (642 mAh g-1). Furthermore, the cycle performance and rate capability of the Sb2S3/C composite are estimated to be much better than those of Sb and Sb2S3. Electrochemical impedance spectroscopy analysis shows that the Sb2S3/C composite exhibited charge transfer resistance and surface film resistance much lower than Sb2S3. X-ray photoelectron spectroscopy analyses of both electrodes demonstrate that NaF layer on Sb2S3/C composite electrode leads to the better electrochemical performances. In order to clarify the electrochemical reaction mechanism, ex-situ XRD based on differential capacity plots and ex-situ HR-TEM analyses of the Sb2S3/C composite electrode are carried out and its reaction mechanism was established.

RBS/C, HRTEM and HRXRD study of damage accumulation in irradiated SrTiO3

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

Jagielski, Jacek; Jozwik, Przemyslaw A.; Jozwik Biala, Iwona

2013-05-14

Damage accumulation in argon-irradiated SrTiO3 single crystals has been studied by using combination of Rutherford Backscattering/Channeling (RBS/C), High Resolution Transmission Electron Microscopy (HRTEM) and High Resolution X-Ray Diffraction (HRXRD) techniques. The RBS/C spectra were fitted using McChasy, a Monte Carlo simulation code allowing the quantitative analysis of amorphous-like and dislocation-like types of defects. The results were interpreted by using a Multi-Step Damage Accumulation model which assumes, that the damage accumulation occurs in a series of structural transformations, the defect transformations are triggered by a stress caused by formation of a free volume in the irradiated crystal. This assumption has beenmore » confirmed by High Resolution Transmission Electron Microscopy and High Resolution X-Ray Diffraction analysis.« less

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

Örnek, Ahmet, E-mail: ahmetornek@kafkas.edu.tr; Can, Mustafa; Yeşildağ, Ali

Nanostructured LiCo{sub 1−x}Mn{sub x}PO{sub 4}/C (x = 0 and 0.05) materials were successfully produced as superior quality cathodes by combined sol-gel and carbothermal reduction methods. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma (ICP), cyclic voltammetry (CV) and galvanostatic measurements were applied to determine the phase purity, morphology and electrochemical qualifications. HR-TEM analysis reveals that the thickness of the surface carbon layer of 5 to 10 nm range with the uniform distribution. LiCo{sub 0·95}Mn{sub 0·05}PO{sub 4}/C particles were betweenmore » 40 and 80 nm and the same material exhibits a higher and stable reversible capacity (140 mA h g{sup −1}) with the long voltage plateau (4.76 V). Substitution of Co{sup 2+} with Mn{sup 2+} in LiCoPO{sub 4}/C has an influence on the initial discharge capacity and excellent cycling behaviour. The obtained results have attributed that production dynamics in nano-synthesis, the coating process with proper carbon source and an effective doping represent three parameters to prepare favorable cathode materials. - Highlights: • Structural, morphological and electrochemical effects of Mn doped LiCo{sub 1−x}Mn{sub x}PO{sub 4}–C electrodes are investigated. • Cheap, effective and simple sol-gel assisted carbothermal reduction approach is used. • After 60th cycle, capacity retention is almost 92% for LiCo{sub 0·95}Mn{sub 0.05}PO{sub 4}–C electrode. • Mn-doped sample exhibits distinctive oxidation (4.76 V and 4.12 V) peaks.« less

In situ TEM of radiation effects in complex ceramics.

PubMed

Lian, Jie; Wang, L M; Sun, Kai; Ewing, Rodney C

2009-03-01

In situ transmission electron microscopy (TEM) has been extensively applied to study radiation effects in a wide variety of materials, such as metals, ceramics and semiconductors and is an indispensable tool in obtaining a fundamental understanding of energetic beam-matter interactions, damage events, and materials' behavior under intense radiation environments. In this article, in situ TEM observations of radiation effects in complex ceramics (e.g., oxides, silicates, and phosphates) subjected to energetic ion and electron irradiations have been summarized with a focus on irradiation-induced microstructural evolution, changes in microchemistry, and the formation of nanostructures. New results for in situ TEM observation of radiation effects in pyrochlore, A(2)B(2)O(7), and zircon, ZrSiO(4), subjected to multiple beam irradiations are presented, and the effects of simultaneous irradiations of alpha-decay and beta-decay on the microstructural evolution of potential nuclear waste forms are discussed. Furthermore, in situ TEM results of radiation effects in a sodium borosilicate glass subjected to electron-beam exposure are introduced to highlight the important applications of advanced analytical TEM techniques, including Z-contrast imaging, energy filtered TEM (EFTEM), and electron energy loss spectroscopy (EELS), in studying radiation effects in materials microstructural evolution and microchemical changes. By combining ex situ TEM and advanced analytical TEM techniques with in situ TEM observations under energetic beam irradiations, one can obtain invaluable information on the phase stability and response behaviors of materials under a wide range of irradiation conditions. (c) 2009 Wiley-Liss, Inc.

TEM-nanoindentation studies of semiconducting structures.

PubMed

Le Bourhis, E; Patriarche, G

2007-01-01

This paper reviews the application of nanoindentation coupled with transmission electron microscopy (TEM) to investigations of the plastic behaviour of semiconducting structures and its implication for device design. Instrumented nanoindentation has been developed to extract the mechanical behaviour of small volumes scaled to those encountered in semiconductor heterostructures. We illustrate that TEM is a powerful complementary tool for the study of local plasticity induced by nanoindentation. TEM-nanoindentation allows for detailed understanding of the plastic deformation in semiconducting structures and opens practical routes for improvement of devices. Performances of heterostructures are deteriously affected by dislocations that relax the lattice mismatched layers. Different ways to obtain compliant substructures are being developed in order to concentrate the plastic relaxation underneath the heterostructure. Such approaches allow for mechanical design of micro- and opto-electronic devices to be considered throughout the fabrication process.

Comparing Time Domain Electromagnetics (TEM) and Early-Time TEM for Mapping Highly Conductive Groundwater in Mars Analog Environments

NASA Astrophysics Data System (ADS)

Jernsletten, J. A.

2005-05-01

Introduction: The purpose of this study is to evaluate the use of (diffusive) Time Domain Electromagnetics (TEM) for sounding of subsurface water in conductive Mars analog environments. To provide a baseline for such studies, I show data from two field studies: 1) Diffusive sounding data (TEM) from Pima County, Arizona; and 2) Shallower sounding data using the Fast-Turnoff TEM method from Peña de Hierro in the Rio Tinto region of Spain. The latter is data from work conducted under the auspices of the Mars Analog Research and Technology Experiment (MARTE). Pima County TEM Survey: A TEM survey was carried out in Pima County, Arizona, in January 2003. Data was collected using 100 m Tx loops and a ferrite-cored magnetic coil Rx antenna, and processed using commercial software. The survey used a 16 Hz sounding frequency, which is sensitive to slightly salty groundwater. Prominent features in the data from Arizona are the ~500 m depth of investigation and the ~120 m depth to the water table, confirmed by data from four USGS test wells surrounding the field area. Note also the conductive (~20-40 ω m) clay-rich soil above the water table. Rio Tinto Fast-Turnoff TEM Survey: During May and June of 2003, a Fast-Turnoff (early time) TEM survey was carried out at the Peña de Hierro field area of the MARTE project, near the town of Nerva, Spain. Data was collected using 20 m and 40 m Tx loop antennae and 10 m loop Rx antennae, with a 32 Hz sounding frequency. Data from Line 4 (of 16) from this survey, collected using 40 m Tx loops, show ~200 m depth of investigation and a conductive high at ~90 m depth below Station 20 (second station of 10 along this line). This is the water table, matching the 431 m MSL elevation of the nearby pit lake. The center of the "pileup" below Station 60 is spatially coincident with the vertical fault plane located here. Data from Line 15 and Line 14 of the Rio Tinto survey, collected using 20 m Tx loops, achieve ~50 m depth of investigation and

SEM and TEM characterization of the microstructure of post-compressed TiB2/2024Al composite.

PubMed

Guo, Q; Jiang, L T; Chen, G Q; Feng, D; Sun, D L; Wu, G H

2012-02-01

In the present work, 55 vol.% TiB(2)/2024Al composites were obtained by pressure infiltration method. Compressive properties of 55 vol.% TiB(2)/2024Al composite under the strain rates of 10(-3) and 1S(-1) at different temperature were measured and microstructure of post-compressed TiB(2)/2024Al composite was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). No trace of Al(3)Ti compound flake was found. TiB(2)-Al interface was smooth without significant reaction products, and orientation relationships ( [Formula: see text] and [Formula: see text] ) were revealed by HRTEM. Compressive strength of TiB(2)/2024Al composites decreased with temperature regardless of strain rates. The strain-rate-sensitivity of TiB(2)/2024Al composites increased with the increasing temperature. Fracture surface of specimens compressed at 25 and 250°C under 10(-3)S(-1) were characterized by furrow. Under 10(-3)S(-1), high density dislocations were formed in Al matrix when compressed at 25°C and dynamic recrystallization occurred at 250°C. Segregation of Mg and Cu on the subgrain boundary was also revealed at 550°C. Dislocations, whose density increased with temperature, were formed in TiB(2) particles under 1S(-1). Deformation of composites is affected by matrix, reinforcement and strain rate. Copyright © 2011 Elsevier Ltd. All rights reserved.

Dynamic XRD, Shock and Static Compression of CaF2

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew; Smith, Jesse; Sinogeikin, Stanislav

2017-06-01

The high-pressure behavior of CaF2 is probed with x-ray diffraction (XRD) combined with both dynamic compression, using a two-stage light gas gun, and static compression, using diamond anvil cells. We use XRD to follow the unfolding of a shock-driven, fluorite to cotunnite phase transition, on the timescale of nanoseconds. The dynamic behavior of CaF2 under shock loading is contrasted with that under static compression. This work leverages experimental capabilities at the Advanced Photon Source: dynamic XRD and shock experiments at the Dynamic Compression Sector, as well as XRD and static compression in diamond anvil cell at the High-Pressure Collaborative Access Team. These experiments and cross-platform comparisons, open the door to an unprecedented understanding of equations of state and phase transitions at the microstructural level and at different time scales and will ultimately improve our capability to simulate the behavior of materials at extreme conditions. Sandia National Laboratories is a multi-mission laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

Automatic software correction of residual aberrations in reconstructed HRTEM exit waves of crystalline samples

DOE PAGES

Ophus, Colin; Rasool, Haider I.; Linck, Martin; ...

2016-11-30

We develop an automatic and objective method to measure and correct residual aberrations in atomic-resolution HRTEM complex exit waves for crystalline samples aligned along a low-index zone axis. Our method uses the approximate rotational point symmetry of a column of atoms or single atom to iteratively calculate a best-fit numerical phase plate for this symmetry condition, and does not require information about the sample thickness or precise structure. We apply our method to two experimental focal series reconstructions, imaging a β-Si 3N 4 wedge with O and N doping, and a single-layer graphene grain boundary. We use peak and latticemore » fitting to evaluate the precision of the corrected exit waves. We also apply our method to the exit wave of a Si wedge retrieved by off-axis electron holography. In all cases, the software correction of the residual aberration function improves the accuracy of the measured exit waves.« less

Automatic software correction of residual aberrations in reconstructed HRTEM exit waves of crystalline samples

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

Ophus, Colin; Rasool, Haider I.; Linck, Martin

We develop an automatic and objective method to measure and correct residual aberrations in atomic-resolution HRTEM complex exit waves for crystalline samples aligned along a low-index zone axis. Our method uses the approximate rotational point symmetry of a column of atoms or single atom to iteratively calculate a best-fit numerical phase plate for this symmetry condition, and does not require information about the sample thickness or precise structure. We apply our method to two experimental focal series reconstructions, imaging a β-Si 3N 4 wedge with O and N doping, and a single-layer graphene grain boundary. We use peak and latticemore » fitting to evaluate the precision of the corrected exit waves. We also apply our method to the exit wave of a Si wedge retrieved by off-axis electron holography. In all cases, the software correction of the residual aberration function improves the accuracy of the measured exit waves.« less

Imaging active topological defects in carbon nanotubes

NASA Astrophysics Data System (ADS)

Suenaga, Kazu; Wakabayashi, Hideaki; Koshino, Masanori; Sato, Yuta; Urita, Koki; Iijima, Sumio

2007-06-01

A single-walled carbon nanotube (SWNT) is a wrapped single graphene layer, and its plastic deformation should require active topological defects-non-hexagonal carbon rings that can migrate along the nanotube wall. Although in situ transmission electron microscopy (TEM) has been used to examine the deformation of SWNTs, these studies deal only with diameter changes and no atomistic mechanism has been elucidated experimentally. Theory predicts that some topological defects can form through the Stone-Wales transformation in SWNTs under tension at 2,000 K, and could act as a dislocation core. We demonstrate here, by means of high-resolution (HR)-TEM with atomic sensitivity, the first direct imaging of pentagon-heptagon pair defects found in an SWNT that was heated at 2,273 K. Moreover, our in situ HR-TEM observation reveals an accumulation of topological defects near the kink of a deformed nanotube. This result suggests that dislocation motions or active topological defects are indeed responsible for the plastic deformation of SWNTs.

Effect of cobalt doping on structural and optical properties of ZnO nanoparticles

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

Singh, J.; Chanda, A., E-mail: anupamamatsc@gmail.com; Gupta, S.

Cobalt doped ZnO nanoparticles of uniform sizes were prepared by a chemical method using ZnCl{sub 2} and NaOH as the source materials. The formation of Co-doped ZnO nanoparticles was confirmed by transmission electron microscopy (TEM), high resolution TEM (HR-TEM) and selected area electron diffraction (SAED) studies. The optical properties of obtained products were examined using room temperature UV-visible and FTIR spectroscopy. SAED of cobalt doped ZnO nanoparticles shows homogeneous distribution of nanoparticles with hexagonal structure. The HRTEM image of the Co-doped ZnO nanoparticles reveals a clear lattice spacing of 0.52 nm corresponding to the interplanar spacing of wurtzite ZnO (002) plane.more » The absorption band at 857 cm{sup −1} in FTIR spectra confirmed the tetrahedral coordination of Zn and a shift of absorption peak to shorter wavelength region and decrease in absorbance with Co doping.is observed in UV-Visible spectra.« less

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Synthesis of ZnO and Zn nanoparticles in microwave plasma and their deposition on glass slides.

PubMed

Irzh, Alexander; Genish, Isaschar; Klein, Lior; Solovyov, Leonid A; Gedanken, Aharon

2010-04-20

This work represents a new method to synthesis of ZnO and/or Zn nanoparticles by means of microwave plasma whose electrons are the reducing agents. Glass quadratic slides sized 2.5 x 2.5 cm were coated by ZnO and/or Zn particles whose sizes ranged from a few micrometers to approximately 20 nm. The size of the particles can be controlled by the type of the precursor and its concentration. In the current paper, the mechanism of the reactions of ZnO and/or Zn formation was proposed. Longer plasma irradiation and lower precursor concentration favor the fabrication of metallic Zn nanoparticles. The nature of the precursor's ion (acetate, nitrate, or chloride) is also of importance in determining the composition of the product. The glass slides coated by ZnO and/or Zn nanoparticles were characterized by HR-SEM, HR-TEM, AFM, XRD, ESR, contact angle and diffuse reflectance spectroscopy (DRS).

Synthesis and characterization of (3-Aminopropyl)trimethoxy-silane (APTMS) functionalized Gd2O3:Eu(3+) red phosphor with enhanced quantum yield.

PubMed

Jain, Akhil; Hirata, G A; Farías, M H; Castillón, F F

2016-02-12

We report the surface modification of nanocrystalline Gd2O3:Eu(3+) phosphor by (3-Aminopropyl)trimethoxysilane (APTMS). The nanoparticles were first coated with silica using the Stöber process, and then annealed at 650 °C for 2 h. Afterwards, APTMS was functionalized onto the silica layer to obtain Gd2O3:Eu(3+) nanoparticles bearing amine groups on the surface. The effect of silica coating, and the subsequent annealing process on the crystallization of the nanophosphor were analyzed by x-ray diffraction (XRD). High-resolution transmission electron microscopy (HR-TEM) confirmed the presence of a silica layer of ∼45 nm thickness. X-ray photoelectron (XPS) and Fourier transform infrared (FTIR) spectroscopy confirmed the presence of silica and the amine groups. Photoluminescence (PL) analysis demonstrated an increased emission after functionalization of nanoparticles. Absolute quantum yield (QY) measurements revealed an 18% enhancement in QY in functionalized nanoparticles compared with unmodified nanoparticles, which is of great importance for their biomedical applications.

Synthesis and characterization of (3-Aminopropyl)trimethoxy-silane (APTMS) functionalized Gd2O3:Eu3+ red phosphor with enhanced quantum yield

NASA Astrophysics Data System (ADS)

Jain, Akhil; Hirata, G. A.; Farías, M. H.; Castillón, F. F.

2016-02-01

We report the surface modification of nanocrystalline Gd2O3:Eu3+ phosphor by (3-Aminopropyl)trimethoxysilane (APTMS). The nanoparticles were first coated with silica using the Stöber process, and then annealed at 650 °C for 2 h. Afterwards, APTMS was functionalized onto the silica layer to obtain Gd2O3:Eu3+ nanoparticles bearing amine groups on the surface. The effect of silica coating, and the subsequent annealing process on the crystallization of the nanophosphor were analyzed by x-ray diffraction (XRD). High-resolution transmission electron microscopy (HR-TEM) confirmed the presence of a silica layer of ∼45 nm thickness. X-ray photoelectron (XPS) and Fourier transform infrared (FTIR) spectroscopy confirmed the presence of silica and the amine groups. Photoluminescence (PL) analysis demonstrated an increased emission after functionalization of nanoparticles. Absolute quantum yield (QY) measurements revealed an 18% enhancement in QY in functionalized nanoparticles compared with unmodified nanoparticles, which is of great importance for their biomedical applications.

Synthesis of bi-phase dispersible core-shell FeAu@ZnO magneto-opto-fluorescent nanoparticles

NASA Astrophysics Data System (ADS)

Li, Xue-Mei; Liu, Hong-Ling; Liu, Xiao; Fang, Ning; Wang, Xian-Hong; Wu, Jun-Hua

2015-11-01

Bi-phase dispersible core-shell FeAu@ZnO magneto-opto-fluorescent nanoparticles were synthesized by a modified nanoemulsion process using poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEO-PPO-PEO) as the surfactant. The morphology and crystal structure of the nanoparticles were studied by TEM/HRTEM and XRD. The nanoparticles manifest soft ferromagnetic and/or near superparamagnetic behavior with a small coercivity of ~19 Oe at room temperature. The corresponding magnetic hysteresis curves were elucidated by the modified Langevin equation. The FTIR study confirms the PEO-PPO-PEO molecules on the surface of the nanoparticles. The UV-vis and PL results reveal the well-behaved absorption bands including surface plasmon resonance and multiple visible fingerprint photoluminescent emissions of the nanoparticles dispersed in both hydrophilic and hydrophobic solvents. Moreover, the processes of solvent dispersion-collection of the nanoparticles were demonstrated for application readiness of such core-shell nanostructures.

Up-conversion green emission of Yb3+/Er3+ ions doped YVO4 nanocrystals obtained via modified Pechini's method

NASA Astrophysics Data System (ADS)

Szczeszak, Agata; Runowski, Marcin; Wiglusz, Rafal J.; Grzyb, Tomasz; Lis, Stefan

2017-12-01

A series of lanthanide doped yttrium vanadates were prepared by Pechini's method (sol-gel process). The as-prepared precursors, in the presence of citric acid, were calcined in the temperature range of 600-900 °C. The obtained products were composed of small nanoparticles, in the size range of 20-50 nm, depending on the annealing temperature, exhibiting a bright green up-conversion emission, under NIR laser irradiation, and emission lifetimes in the range of 4.7-18.3 μs. Their structural, morphological and spectroscopic properties were investigated in detail by XRD, HR-TEM including FFT analysis, EDX and spectroscopic techniques (emission, power dependence and emission kinetics). The luminescence quenching phenomenon, manifested in a decrease of up-conversion intensity and shortening of emission lifetime, was observed with increasing of the Yb3+ ion concentration and decreasing the particle size. The optimal concentration of the Yb3+ ions was found to be 15 mol% (YVO4: Yb3+ 15 mol%, Er3+ 2 mol%).

Synthesis of bi-phase dispersible core-shell FeAu@ZnO magneto-opto-fluorescent nanoparticles

PubMed Central

Li, Xue-Mei; Liu, Hong-Ling; Liu, Xiao; Fang, Ning; Wang, Xian-Hong; Wu, Jun-Hua

2015-01-01

Bi-phase dispersible core-shell FeAu@ZnO magneto-opto-fluorescent nanoparticles were synthesized by a modified nanoemulsion process using poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEO-PPO-PEO) as the surfactant. The morphology and crystal structure of the nanoparticles were studied by TEM/HRTEM and XRD. The nanoparticles manifest soft ferromagnetic and/or near superparamagnetic behavior with a small coercivity of ~19 Oe at room temperature. The corresponding magnetic hysteresis curves were elucidated by the modified Langevin equation. The FTIR study confirms the PEO-PPO-PEO molecules on the surface of the nanoparticles. The UV-vis and PL results reveal the well-behaved absorption bands including surface plasmon resonance and multiple visible fingerprint photoluminescent emissions of the nanoparticles dispersed in both hydrophilic and hydrophobic solvents. Moreover, the processes of solvent dispersion-collection of the nanoparticles were demonstrated for application readiness of such core-shell nanostructures. PMID:26548369

Process dependent thermoelectric properties of EDTA assisted bismuth telluride

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

Kulsi, Chiranjit; Banerjee, Dipali, E-mail: dipalibanerjeebesu@gmail.com; Kargupta, Kajari

2016-04-13

Comparison between the structure and thermoelectric properties of EDTA (Ethylene-diamine-tetra-acetic acid) assisted bismuth telluride prepared by electrochemical deposition and hydrothermal route is reported in the present work. The prepared samples have been structurally characterized by high resolution X-ray diffraction spectra (HRXRD), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopic images (HRTEM). Crystallite size and strain have been determined from Williamson-Hall plot of XRD which is in conformity with TEM images. Measurement of transport properties show sample in the pellet form (S{sub 1}) prepared via hydrothermal route has higher value of thermoelectric power (S) than the electrodepositedmore » film (S{sub 2}). But due to a substantial increase in the electrical conductivity (σ) of the film (S{sub 2}) over the pellet (S{sub 1}), the power factor and the figure of merit is higher for sample S{sub 2} than the sample S{sub 1} at room temperature.« less

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

NASA Astrophysics Data System (ADS)

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

2015-11-01

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

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.

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 graphene oxide and reduced graphene oxide by needle platy natural vein graphite

NASA Astrophysics Data System (ADS)

Rathnayake, R. M. N. M.; Wijayasinghe, H. W. M. A. C.; Pitawala, H. M. T. G. A.; Yoshimura, Masamichi; Huang, Hsin-Hui

2017-01-01

Among natural graphite varieties, needle platy vein graphite (NPG) has very high purity. Therefore, it is readily used to prepare graphene oxide (GO) and reduced graphene oxide (rGO). In this study, GO and rGO were prepared using chemical oxidation and reduction process, respectively. The synthesized materials were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy. XRD studies confirmed the increase of the interlayer spacing of GO and rGO in between 3.35 to 8.66 A°. AFM studies showed the layer height of rGO to be 1.05 nm after the reduction process. TEM micrographs clearly illustrated that the prepared GO has more than 25 layers, while the rGO has only less than 15 layers. Furthermore, the effect of chemical oxidation and reduction processes on surface morphology of graphite were clearly observed in FESEM micrographs. The calculated RO/C of GO and rGO using XPS analysis are 5.37% and 1.77%, respectively. The present study revealed the successful and cost effective nature of the chemical oxidation, and the reduction processes for the production of GO and rGO out of natural vein graphite.

MultiLaue: A Technique to Extract d-spacings from Laue XRD

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

Gainsforth, Zack; Marcus, Matthew A.; Tamura, Nobumichi

We present that broad spectrum X-ray Diffraction (XRD) is named Laue after Max von Laue, and is the original XRD technique. Today, monochromatic XRD is more common because Bragg's equation allows determination of d-spacings where Laue does not. Laue still remains in use for single crystal systems because it can be used to make very accurate unit cell determinations as well as for strain and orientation mapping. Lastly, a Laue technique which could provide unambiguous determination of lattice spacings, a la Bragg's equation would be a huge leap forward, especially for multiphase samples such as meteorites, interplanetary dust particles andmore » some geological specimens.« less

MultiLaue: A Technique to Extract d-spacings from Laue XRD

DOE PAGES

Gainsforth, Zack; Marcus, Matthew A.; Tamura, Nobumichi; ...

2016-07-25

We present that broad spectrum X-ray Diffraction (XRD) is named Laue after Max von Laue, and is the original XRD technique. Today, monochromatic XRD is more common because Bragg's equation allows determination of d-spacings where Laue does not. Laue still remains in use for single crystal systems because it can be used to make very accurate unit cell determinations as well as for strain and orientation mapping. Lastly, a Laue technique which could provide unambiguous determination of lattice spacings, a la Bragg's equation would be a huge leap forward, especially for multiphase samples such as meteorites, interplanetary dust particles andmore » some geological specimens.« less

Objective function analysis for electric soundings (VES), transient electromagnetic soundings (TEM) and joint inversion VES/TEM

NASA Astrophysics Data System (ADS)

Bortolozo, Cassiano Antonio; Bokhonok, Oleg; Porsani, Jorge Luís; Monteiro dos Santos, Fernando Acácio; Diogo, Liliana Alcazar; Slob, Evert

2017-11-01

Ambiguities in geophysical inversion results are always present. How these ambiguities appear in most cases open to interpretation. It is interesting to investigate ambiguities with regard to the parameters of the models under study. Residual Function Dispersion Map (RFDM) can be used to differentiate between global ambiguities and local minima in the objective function. We apply RFDM to Vertical Electrical Sounding (VES) and TEM Sounding inversion results. Through topographic analysis of the objective function we evaluate the advantages and limitations of electrical sounding data compared with TEM sounding data, and the benefits of joint inversion in comparison with the individual methods. The RFDM analysis proved to be a very interesting tool for understanding the joint inversion method of VES/TEM. Also the advantage of the applicability of the RFDM analyses in real data is explored in this paper to demonstrate not only how the objective function of real data behaves but the applicability of the RFDM approach in real cases. With the analysis of the results, it is possible to understand how the joint inversion can reduce the ambiguity of the methods.

Technical Evaluation Motor No. 7 (TEM-07)

NASA Technical Reports Server (NTRS)

Hugh, Phil

1991-01-01

Technical Evaluation Motor Number 7 (TEM-7) was a full scale, full-duration static test firing of a high performance motor (HPM) configuration solid rocket motor (SRM) with nozzle vectoring. The static test fire occurred on 11 December 1990 at the Thiokol Corporation Static Test Bay T-97. Documented here are the procedures, performance, and results available through 22 January 1991. Critical post test hardware activities and assessment of the test data are not complete. A completed test report will be submitted 60 days after the test date. Included here is a presentation and discussion of the TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107 Revision A, Space Shuttle Technical Evaluation Motor number 7 (TEM-07) Static Fire Test Plan.

Synthesis and study of photovoltaic performance on various photoelectrode materials for DSSCs: Optimization of compact layer on nanometer thickness

NASA Astrophysics Data System (ADS)

Surya, Subramanian; Thangamuthu, Rangasamy; Senthil Kumar, Sakkarapalayam Murugesan; Murugadoss, Govindhasamy

2017-02-01

Dye-sensitized solar cells (DSSCs) have gained widespread attention in recent years because of their low production costs, ease of fabrication process and tuneable optical properties, such as colour and transparency. In this work, we explored a strategy wherein nanoparticles of pure TiO2, TiO2sbnd SnO2 nanocomposite, Sn (10%) doped TiO2 and SnO2 synthesized by the simple chemical precipitation method were employed as photoelectrodes to enhance the photovoltaic conversion efficiency of solar cells. The nanoparticles were characterized by different characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM with EDX), transmission electron microscopy (TEM), high resolution electron microscopy (HR-TEM), UV-Visible absorbance (UV-vis), photoluminescence (PL), thermal gravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS) measurements. Moreover, we also demonstrated the effect of thin compact layer in DSSCs by architecture with various precursor materials of different concentrations. We found that the optimized compact layer material TDIP (titanium diisopropoxide) with a concentration of 0.3 M % is produced the highest efficiency of 2.25% for Sn (10%) doped TiO2 electron transport material (ETM) and 4.38% was achieved for pure TiO2 ETM using SnCl2 compact layer with 0.1 M concentrations.

Morphology and structure of TixOy nanoparticles generated by femtosecond laser ablation in water

NASA Astrophysics Data System (ADS)

Donėlienė, Jolanta; Rudzikas, Matas; Rades, Steffi; Dörfel, Ilona; Peplinski, Burkhard; Sahre, Mario; Pellegrino, Francesco; Maurino, Valter; Ulbikas, Juras; Galdikas, Algirdas; Hodoroaba, Vasile-Dan

2018-04-01

In this work femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD (two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation.

Hydrothermal synthesis of superparamagnetic Fe{sub 3}O{sub 4} nanoparticles with ionic liquids as stabilizer

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

Liu, Xiao-Di, E-mail: liuxiaodiny@126.com; Chen, Hao; Liu, Shan-Shan

2015-02-15

Highlights: • Superparamagnetic Fe{sub 3}O{sub 4} nanoparticles with good dispersity have been synthesized via hydrothermal method. • Ionic liquid [C{sub 16}mim]Cl acts as stabilizer for the Fe{sub 3}O{sub 4} nanoparticles. • Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 67.69 emu/g at 300 K. - Abstract: Superparamagnetic Fe{sub 3}O{sub 4} nanoparticles have been successfully synthesized under hydrothermal condition with the assistant of ionic liquid 1-hexadecyl-3-methylimidazolium chloride ([C{sub 16}mim]Cl). The structure and morphology of the sample have been investigated by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), transmission electron microscopy (TEM), and high-resolution TEM (HRTEM), and the results indicate thatmore » the as-synthesized inverse spinel Fe{sub 3}O{sub 4} nanoparticles have an average diameter of about 10 nm and exhibit relatively good dispersity. More importantly, it is found that [C{sub 16}mim]Cl acts as stabilizer for the Fe{sub 3}O{sub 4} nanoparticles by adsorbing on the particles surfaces to prevent the agglomeration. In addition, the obtained superparamagnetic Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 67.69 emu/g at 300 K.« less

Characterization and activity of Pd-modified TiO2 catalysts for photocatalytic oxidation of NO in gas phase.

PubMed

Wu, Zhongbiao; Sheng, Zhongyi; Liu, Yue; Wang, Haiqiang; Tang, Nian; Wang, Jie

2009-05-30

Pd-modified TiO(2) prepared by thermal impregnation method was used in this study for photocatalytic oxidation of NO in gas phase. The physico-chemical properties of Pd/TiO(2) catalysts were characterized by X-ray diffraction analysis (XRD), Brunauer-Emmett-Teller measurements (BET), X-ray photoelectron spectrum analysis (XPS), transmission electron microscopy (TEM), high resolution-transmission electron microscopy (HR-TEM), UV-vis diffuse reflectance spectra (UV-vis DRS) and photoluminescence spectra (PL). It was found that Pd dopant existed as PdO particles in as-prepared photocatalysts. The results of PL spectra indicated that the photogenerated electrons and holes were efficiently separated after Pd doping. During in situ XPS study, it was found that the content of hydroxyl groups on the surface of Pd/TiO(2) increased when the catalyst was irradiated by UV light, which could result in the improvement of photocatalytic activity. The activity test showed that the optimum Pd dopant content was 0.05 wt.%. And the maximum conversion of NO was about 72% higher than that of P25 when the initial concentration of NO was 200 ppm, which showed that Pd/TiO(2) photocatalysts could be potentially applied to oxidize higher concentration of NO.

Gas-sensing performances of Cd-doped ZnO nanoparticles synthesized by a surfactant-mediated method for n-butanol gas

NASA Astrophysics Data System (ADS)

Zhao, Rongjun; Li, Kejin; Wang, Zhezhe; Xing, Xinxin; Wang, Yude

2018-01-01

Zinc oxide nanoparticles with the different Cd doping contents were prepared by with a surfactant-mediated method in this paper. The effects of Cd doping on the gas sensing properties of the ZnO nanoparticles were studied. The morphology and microstructure of as-prepared samples were characterized by X-ray diffraction (XRD); scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution TEM (HRTEM), respectively. The results reveal that all the products are the high crystalline hexagonal wurtzite ZnO crystal structure. The gas-sensing characteristics of the Cd doped ZnO nanoparticles for volatile organic compounds (VOCs) were investigated. At its optimal operation temperature of 300 °C, the sensing properties of the Cd doped ZnO nanoparticles for n-butanol gas exhibit a high-performance gas sensing performances including high gas response, good selectivity, response/recovery time, and repeatability as well as stability. Especially, its response reaches 130 for 100 ppm n-butanol of ZnO nanoparticles with 2.5% Cd doping. Those values demonstrate the potential of using as-prepared Cd doped ZnO nanoparticles for n-butanol gas detection, making them to be promising candidates for practical detectors to n-butanol gas. Apart from these, the mechanism related to the advanced properties was also investigated and presented.

CdS quantum dots modified CuO inverse opal electrodes for ultrasensitive electrochemical and photoelectrochemical biosensor

PubMed Central

Xia, Lei; Xu, Lin; Song, Jian; Xu, Ru; Liu, Dali; Dong, Biao; Song, Hongwei

2015-01-01

The CuO inverse opal photonic crystals (IOPCs) were synthesized by the sol-gel method and modified with CdS quantum dots by successive ionic layer adsorption and reaction (SILAR). CdS QDs modified CuO IOPCs FTO electrodes of different SILAR cycles were fabricated and their electrochemical properties were studied by cyclic voltammetry (CV) and chronoamperometry (I–t). Structure and morphology of the samples were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), high-resolution TEM (HRTEM), Energy-dispersive X-ray analysis (EDX) and X-ray diffraction pattern (XRD). The result indicated that the structure of IOPCs and loading of CdS QDs could greatly improve the electrochemical properties. Three SILAR cycles of CdS QDs sensitization was the optimum condition for preparing electrodes, it exhibited a sensitivity of 4345 μA mM-1 cm-2 to glucose with a 0.15 μM detection limit (S/N= 3) and a linear range from 0.15 μM to 0.5 mM under a working potential of +0.7 V. It also showed strong stability, good reproducibility, excellent selectivity and fast amperometric response. This work provides a promising approach for realizing excellent photoelectrochemical nonenzymatic glucose biosensor of similar composite structure. PMID:26042520

Structure of Z-scheme CdS/CQDs/BiOCl heterojunction with enhanced photocatalytic activity for environmental pollutant elimination

NASA Astrophysics Data System (ADS)

Pan, Jinbo; Liu, Jianjun; Zuo, Shengli; Khan, Usman Ali; Yu, Yingchun; Li, Baoshan

2018-06-01

Z-scheme CdS/CQDs/BiOCl heterojunction was synthesized by a facile region-selective deposition process. Owing to the electronegativity of the groups on the surface of Carbon Quantum Dots (CQDs), they can be sandwiched between CdS and BiOCl, based on the stepwise region-selective deposition process. The samples were systematically characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), photoelectrochemical measurements and photoluminescence (PL). The results indicate that CQDs with size of 2-5 nm and CdS nanoparticles with size of 5-10 nm dispersed uniformly on the surface of cuboid BiOCl nanosheets. The photocatalytic performance tests reveal that the CdS/CQDs/BiOCl heterojunction exhibits much higher photocatalytic activity than that of BiOCl, CdS/BiOCl and CQDs/BiOCl for Rhodamine B (RhB) and phenol photodegradation under visible and UV light illumination, respectively. The enhanced photocatalytic performance should be attributed to the Z-scheme structure of CdS/CQDs/BiOCl, which not only improves visible light absorption and the migration efficiency of the photogenerated electron-holes but also keeps high redox ability of CdS/CQDs/BiOCl composite.

Preparation of carbon-free TEM microgrids by metal sputtering.

PubMed

Janbroers, S; de Kruijff, T R; Xu, Q; Kooyman, P J; Zandbergen, H W

2009-08-01

A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775K under vacuum conditions.

Revelation of graphene-Au for direct write deposition and characterization

NASA Astrophysics Data System (ADS)

Bhandari, Shweta; Deepa, Melepurath; Joshi, Amish G.; Saxena, Aditya P.; Srivastava, Avanish K.

2011-06-01

Graphene nanosheets were prepared using a modified Hummer's method, and Au-graphene nanocomposites were fabricated by in situ reduction of a gold salt. The as-produced graphene was characterized by X-ray photoelectron spectroscopy, ultraviolet-visible spectroscopy, scanning electron microscopy, and high-resolution transmission electron microscopy (HR-TEM). In particular, the HR-TEM demonstrated the layered crystallites of graphene with fringe spacing of about 0.32 nm in individual sheets and the ultrafine facetted structure of about 20 to 50 nm of Au particles in graphene composite. Scanning helium ion microscopy (HIM) technique was employed to demonstrate direct write deposition on graphene by lettering with gaps down to 7 nm within the chamber of the microscope. Bare graphene and graphene-gold nanocomposites were further characterized in terms of their composition and optical and electrical properties.

ToTem: a tool for variant calling pipeline optimization.

PubMed

Tom, Nikola; Tom, Ondrej; Malcikova, Jitka; Pavlova, Sarka; Kubesova, Blanka; Rausch, Tobias; Kolarik, Miroslav; Benes, Vladimir; Bystry, Vojtech; Pospisilova, Sarka

2018-06-26

High-throughput bioinformatics analyses of next generation sequencing (NGS) data often require challenging pipeline optimization. The key problem is choosing appropriate tools and selecting the best parameters for optimal precision and recall. Here we introduce ToTem, a tool for automated pipeline optimization. ToTem is a stand-alone web application with a comprehensive graphical user interface (GUI). ToTem is written in Java and PHP with an underlying connection to a MySQL database. Its primary role is to automatically generate, execute and benchmark different variant calling pipeline settings. Our tool allows an analysis to be started from any level of the process and with the possibility of plugging almost any tool or code. To prevent an over-fitting of pipeline parameters, ToTem ensures the reproducibility of these by using cross validation techniques that penalize the final precision, recall and F-measure. The results are interpreted as interactive graphs and tables allowing an optimal pipeline to be selected, based on the user's priorities. Using ToTem, we were able to optimize somatic variant calling from ultra-deep targeted gene sequencing (TGS) data and germline variant detection in whole genome sequencing (WGS) data. ToTem is a tool for automated pipeline optimization which is freely available as a web application at  https://totem.software .

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.

Retrofit implementation of Zernike phase plate imaging for cryo-TEM

PubMed Central

Marko, Michael; Leith, ArDean; Hsieh, Chyongere; Danev, Radostin

2011-01-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. PMID:21272647

Design of a TEM cell EMP simulator

NASA Astrophysics Data System (ADS)

Sevat, Pete

1991-06-01

Electromagnetic pulse (EMP) simulators are designed to simulate the EMP generated by a nuclear weapon and are used to harden equipment against the effects of EMP. A transverse electromagnetic (TEM) cell is a square or rectangular coaxial transmission line tapered at each end to form a closed cell. The cell is fed at one end with a signal generator, a continuous wave or pulse generator, and terminated at the other end with a resistor equal to the characteristic impedance of the line. An advantage of the TEM cell is that the field is well characterized and reasonably uniform. A small, symmetric, TEM cell EMP simulator is described which is intended for applications such as susceptibility testing of small equipment, calibration of sensors, design and testing of countermeasures, measurement of transfer functions, and research and development. A detailed design is presented for a 50 ohm and 100 ohm TEM cell with an inner volume of 4 m(exp 3) and a test volume of 0.24 m(exp 3). The pulse generator and terminating network are integrated into the cell to form a completely shielded structure. In this way no interference from the inside of the cell to the outside, or vice versa, will occur.

Retrofit implementation of Zernike phase plate imaging for cryo-TEM.

PubMed

Marko, Michael; Leith, Ardean; Hsieh, Chyongere; Danev, Radostin

2011-05-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. Copyright © 2011 Elsevier Inc. All rights reserved.

Nanoscale deformation analysis with high-resolution transmission electron microscopy and digital image correlation

DOE PAGES

Wang, Xueju; Pan, Zhipeng; Fan, Feifei; ...

2015-09-10

We present an application of the digital image correlation (DIC) method to high-resolution transmission electron microscopy (HRTEM) images for nanoscale deformation analysis. The combination of DIC and HRTEM offers both the ultrahigh spatial resolution and high displacement detection sensitivity that are not possible with other microscope-based DIC techniques. We demonstrate the accuracy and utility of the HRTEM-DIC technique through displacement and strain analysis on amorphous silicon. Two types of error sources resulting from the transmission electron microscopy (TEM) image noise and electromagnetic-lens distortions are quantitatively investigated via rigid-body translation experiments. The local and global DIC approaches are applied for themore » analysis of diffusion- and reaction-induced deformation fields in electrochemically lithiated amorphous silicon. As a result, the DIC technique coupled with HRTEM provides a new avenue for the deformation analysis of materials at the nanometer length scales.« less

TEM investigations on twin boundary structures of feathery crystals in aluminum alloys during Bridgman solidification

NASA Astrophysics Data System (ADS)

Yang, Luyan; Li, Shuangming; Fan, Kai; Li, Yang; Zhong, Hong; Fu, Hengzhi

2018-06-01

Feathery crystals are an ensemble of twinned dendrites, and are characterized by a unique twin boundary (TB) structure in the solidification pattern of aluminum alloys. In this work, the high-density twinned dendrites of Al-4.5 wt% Cu alloys, produced during the Bridgman solidification, have been studied using electron backscattered diffraction (EBSD) and high-resolution transmission electron microscopy (HRTEM). The experimental results showed that, after systematically decreasing the growth rate from 3000 μm/s to 1 μm/s, the TBs remained stable, while the solute field around the TBs changed significantly. According to the HRTEM results, successive stacking faults were occurred near the TBs at 1 μm/s, while slight distortion was observed around the TBs at 3000 μm/s. The composition analysis revealed an obvious solute enrichment near the TBs. Furthermore, the solute gradient profile within the TBs became smoother with the decrease in the growth speed. This is due to the more sufficient solid-state back diffusion occurring perpendicular to the twin plane after the solidification.

A green chemistry approach for the synthesis and characterization of bioactive gold nanoparticles using Azolla microphylla methanol extract

NASA Astrophysics Data System (ADS)

Kunjiappan, Selvaraj; Chowdhury, Ranjana; Bhattacharjee, Chiranjib

2014-06-01

This article reports the environmentally benign synthesis of gold nanoparticles (GNPs) using methanol extract of Azolla microphylla as the stabilizing and reducing agent. The GNPs were characterized by UV-vis spectrophotometry and FTIR, and the morphological characteristics were analyzed by XRD, FESEM-EDX and HRTEM. The GNPs could be formed in very short time, even in less than 30 min. The nanoparticles measured by UV-spectrophotometer demonstrated a peak at 540 nm corresponding to surface plasmon resonance spectra, and the peaks showed by FTIR suggested the presence of organic biomolecules on the surface of the GNPs. XRD results confirmed the crystalline nature of the GNPs, and FESEM-EDX and HRTEM analyses had been performed in the size ranges of 17-40 nm and 1.25-17.5 nm respectively. The synthesized GNPs showed excellent antioxidant activity. This study shows the feasibility of using plant sources for the biosynthesis of GNPs.

Development of Ternary and Quaternary Catalysts for the Electrooxidation of Glycerol

PubMed Central

Artem, L. M.; Santos, D. M.; De Andrade, A. R.; Kokoh, K. B.; Ribeiro, J.

2012-01-01

This work consisted in the preparation of platinum-based catalysts supported on carbon (Vulcan XC-72) and investigation of their physicochemical and electrochemical properties. Catalysts of the C/Pt-Ni-Sn-Me (Me = Ru or Ir) type were prepared by the Pechini method at temperature of 350°C. Four different compositions were homemade: C/Pt60Sn10Ni30, C/Pt60Sn10Ni20Ru10, C/Pt60Sn10Ni10Ru20, and C/Pt60Sn10Ni10Ir20. These catalysts were electrochemically and physically characterized by cyclic voltammetry (CV), chronoamperometry (CA) in the presence of glycerol 1.0 mol dm−3, X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM). XRD results showed the main peaks of face-centered cubic Pt. The particle sizes obtained from XRD and HRTEM experiments were close to values ranging from 3 to 8.5 nm. The CV results indicate behavior typical of Pt-based catalysts in acid medium. The CV and CA data reveal that quaternary catalysts present the highest current density for the electrooxidation of glycerol. PMID:22623905

Study of the phase transformation of single particles of Ga2O3 by UV-Raman spectroscopy and high-resolution TEM.

PubMed

Wang, Xiang; Xu, Qian; Fan, Fengtao; Wang, Xiuli; Li, Mingrun; Feng, Zhaochi; Li, Can

2013-09-01

By taking advantage of UV-Raman spectroscopy and high-resolution TEM (HRTEM), combined with the focused ion beam (FIB) technique, the transformation from GaOOH into α-Ga2O3 and then into β-Ga2O3 was followed. We found that the stepwise transformations took place from the surface region before developing into the bulk of single particles without particle agglomeration and growth. During the transformation from GaOOH into α-Ga2O3, the elimination of water vapor through the dehydroxylation of GaOOH resulted in the formation of micropores in the single particles, whilst maintaining their particle size. For the phase transformation from α-Ga2O3 into β-Ga2O3, the nucleation of β-Ga2O3 was found to occur at the surface defects and this process could be retarded by occupying these defects with a small amount of La2O3. By finely controlling the process of the phase transformation, the β-Ga2O3 domains gradually developed from the surface into the bulk of the single particles without particle agglomeration. Therefore, the surface structure of the α-Ga2O3 single particles can be easily tuned and a particle with an α@β core-shell phase structure has been obtained. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

RECENT DEVELOPMENT IN TEM CHARACTERIZATION OF IRRADIATED RERTR FUELS

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

J. Gan; B.D. Miller; D.D. Keiser Jr.

2011-10-01

The recent development on TEM work of irradiated RERTR fuels includes microstructural characterization of the irradiated U-10Mo/alloy-6061 monolithic fuel plate, the RERTR-7 U-7Mo/Al-2Si and U-7Mo/Al-5Si dispersion fuel plates. It is the first time that a TEM sample of an irradiated nuclear fuel was prepared using the focused-ion-beam (FIB) lift-out technical at the Idaho National Laboratory. Multiple FIB TEM samples were prepared from the areas of interest in a SEM sample. The characterization was carried out using a 200kV TEM with a LaB6 filament. The three dimensional orderings of nanometer-sized fission gas bubbles are observed in the crystalline region of themore » U-Mo fuel. The co-existence of bubble superlattice and dislocations is evident. Detailed microstructural information along with composition analysis is obtained. The results and their implication on the performance of these fuels are discussed.« less

Synthesis, characterization and magnetic property of maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles and their protective coating with pepsin for bio-functionalization

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

Bandhu, A.; Sutradhar, S.; Mukherjee, S.

Highlights: • Maghemite nanoparticles were prepared by a modified co-precipitation method. • Nanoparticles were then successfully coated with pepsin for bio-functionlization. • XRD and Mössbauer spectra confirmed the maghemite phase of the nanoparticles. • Magnetic data were analysed to evaluate particle size, anisotropy etc. - Abstract: Maghemite nanoparticles (γ-Fe{sub 2}O{sub 3}) are prepared by co-precipitation method. To obtain bio-functionalized magnetic nanoparticles for magnetically controlled drug delivery, the prepared nanoparticles are successfully coated with pepsin, a bio-compatible polymer and digestive enzyme. Crystallographic phase of the nanoparticles is confirmed by X-ray diffractograms (XRD), high resolution transmission electron microscopy (HRTEM) and {sup 57}Femore » Mössbauer spectrometry. The average size of nanoparticles/nanocrystallites is estimated from the (3 1 1) peak of the XRD pattern using Debye–Scherrer formula. Results of HRTEM of coated and bare samples are in good agreement with those extracted from the XRD analysis. The dynamic magnetic properties are observed and different quantities viz., coercive field, magnetization, remanence, hysteresis losses etc., are estimated, which confirmed the presence of superparamagnetic relaxation of nanoparticles. Mössbauer spectra of the samples recorded at both 300 and 77 K, confirmed that the majority of particles are maghemite together with a very small fraction of magnetite nanoparticles.« less

Interfacial effect on the structural and optical properties of pure SnO2 and dual shells (ZnO; SiO2) coated SnO2 core-shell nanospheres for optoelectronic applications

NASA Astrophysics Data System (ADS)

Selvi, N.; Sankar, S.; Dinakaran, K.

2014-12-01

Nanocrystallites of SnO2 core and dual shells (ZnO, SiO2) coated SnO2 core-shell nanospheres were successfully synthesized by co-precipitation method. The as prepared and annealed samples were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), High resolution transmission electron microscopy (HRTEM) and UV-Vis analysis. XRD pattern confirms the obtained SnO2 core with tetragonal rutile crystalline structure and the shell ZnO with hexagonal structure. FTIR result shows the functional groups present in the samples. The spherical morphology and the formation of the core-shell structures have been confirmed by HRTEM measurements. The UV-Vis showed that band gap is red shifted for as-prepared and the shells coated core-shell samples. From this investigation it can be concluded that the surface modification with different metal and insulating oxides strongly influences the optical properties of the core-shell materials which enhance their potential applications towards optical devices fabrication.

Crystal Structure Variations of Sn Nanoparticles upon Heating

NASA Astrophysics Data System (ADS)

Mittal, Jagjiwan; Lin, Kwang-Lung

2018-04-01

Structural changes in Sn nanoparticles during heating below the melting point have been investigated using differential scanning calorimetry (DSC), x-ray diffraction (XRD) analysis, electron diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). DSC revealed that the heat required to melt the nanoparticles (28.43 J/g) was about half compared with Sn metal (52.80 J/g), which was attributed to the large surface energy contribution for the nanoparticles. ED and XRD analyses of the Sn nanoparticles revealed increased intensity for crystal planes having large interplaner distances compared with regular crystal planes with increasing heat treatment temperature (HTT). HRTEM revealed an increase in interlayer spacing at the surface and near joints between nanoparticles with the HTT, leading to an amorphous structure of nanoparticles at the surface at 220°C. These results highlight the changes that occur in the morphology and crystal structure of Sn nanoparticles at the surface and in the interior with increase of the heat treatment temperature.

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Chongad, L. S.; Sharma, A.; Banerjee, M.; Jain, A.

2016-10-01

Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H2S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD.

Characteristics of layered tin disulfide deposited by atomic layer deposition with H2S annealing

NASA Astrophysics Data System (ADS)

Lee, Seungjin; Shin, Seokyoon; Ham, Giyul; Lee, Juhyun; Choi, Hyeongsu; Park, Hyunwoo; Jeon, Hyeongtag

2017-04-01

Tin disulfide (SnS2) has attracted much attention as a two-dimensional (2D) material. A high-quality, low-temperature process for producing 2D materials is required for future electronic devices. Here, we investigate tin disulfide (SnS2) layers deposited via atomic layer deposition (ALD) using tetrakis(dimethylamino)tin (TDMASn) as a Sn precursor and H2S gas as a sulfur source at low temperature (150° C). The crystallinity of SnS2 was improved by H2S gas annealing. We carried out H2S gas annealing at various conditions (250° C, 300° C, 350° C, and using a three-step method). Angle-resolved X-ray photoelectron spectroscopy (ARXPS) results revealed the valence state corresponding to Sn4+ and S2- in the SnS2 annealed with H2S gas. The SnS2 annealed with H2S gas had a hexagonal structure, as measured via X-ray diffraction (XRD) and the clearly out-of-plane (A1g) mode in Raman spectroscopy. The crystallinity of SnS2 was improved after H2S annealing and was confirmed using the XRD full-width at half-maximum (FWHM). In addition, high-resolution transmission electron microscopy (HR-TEM) images indicated a clear layered structure.

Fabrication of a transparent ultraviolet detector by using n-type Ga2O3 and p-type Ga-doped SnO2 core-shell nanowires.

PubMed

Hsu, Cheng-Liang; Lu, Ying-Ching

2012-09-21

This study investigates the feasibility of synthesizing high-density transparent Ga(2)O(3)/SnO(2):Ga core-shell nanowires on a sapphire substrate at 1000 °C by VLS. The doping Ga concentrations are 0.46, 1.07, 2.30 and 17.53 atomic%. The XRD spectrum and HR-TEM reveal Ga(2)O(3) and SnO(2) as having monoclinic and tetragonal rutile structures, respectively. Experimental results indicate that the XRD peak shift of SnO(2) to a larger angle increases with the increasing amount of Ga doping. According to the CL spectrum, SnO(2) and Ga(2)O(3) peak at approximately 528-568 nm and 422-424 nm, respectively. The maximum quantum efficiency of Ga(2)O(3)/SnO(2):Ga core-shell nanowires is around 0.362%. The UV light on-off current contrast ratio of Ga(2)O(3)/SnO(2):Ga core-shell nanowires is around 1066.7 at a bias of 5 V. Moreover, the dynamic response of Ga(2)O(3)/SnO(2):Ga core-shell nanowires has an on-off current contrast ratio of around 16. Furthermore, the Ga(2)O(3) region functions similar to a capacitor and continues to accumulate SnO(2):Ga excited electrons under UV light exposure.

Double-tilt in situ TEM holder with ultra-high stability.

PubMed

Xu, Mingjie; Dai, Sheng; Blum, Thomas; Li, Linze; Pan, Xiaoqing

2018-05-06

A double tilting holder with high stability is essential for acquiring atomic-scale information by transmission electron microscopy (TEM), but the availability of such holders for in situ TEM studies under various external stimuli is limited. Here, we report a unique design of seal-bearing components that provides ultra-high stability and multifunctionality (including double tilting) in an in situ TEM holder. The seal-bearing subsystem provides superior vibration damping and electrical insulation while maintaining excellent vacuum sealing and small form factor. A wide variety of in situ TEM applications including electrical measurement, STM mapping, photovoltaic studies, and CL spectroscopy can be performed on this platform with high spatial resolution imaging and electrical sensitivity at the pA scale. Copyright © 2018 Elsevier B.V. All rights reserved.

Electrospun PVA/HAp nanocomposite nanofibers: biomimetics of mineralized hard tissues at a lower level of complexity.

PubMed

Kim, Gyeong-Man; Asran, Ashraf Sh; Michler, Georg H; Simon, Paul; Kim, Jeong-Sook

2008-12-01

Based on the biomimetic approaches the present work describes a straightforward technique to mimic not only the architecture (the morphology) but also the chemistry (the composition) of the lowest level of the hierarchical organization of bone. This technique uses an electrospinning (ES) process with polyvinyl alcohol (PVA) and hydroxyapatite (HAp) nanoparticles. To determine morphology, crystalline structures and thermal properties of the resulting electrospun fibers with the pure PVA and PVA/HAp nanocomposite (NC) before electrospinning various techniques were employed, including transmission electron microscopy (TEM), high-resolution TEM (HR-TEM), scanning electron microscopy (SEM), x-ray diffraction (XRD), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). In addition, FT-IR spectroscopy was carried out to analyze the complex structural changes upon undergoing electrospinning as well as interactions between HAp and PVA. The morphological and crystallographic investigations revealed that the rod-like HAp nanoparticles exhibit a nanoporous morphology and are embedded within the electrospun fibers. A large number of HAp nanorods are preferentially oriented parallel to the longitudinal direction of the electrospun PVA fibers, which closely resemble the naturally mineralized hard tissues of bones. Due to abundant OH groups present in PVA and HAp nanorods, they strongly interact via hydrogen bonding within the electrospun PVA/HAp NC fibers, which results in improved thermal properties. The unique physiochemical features of the electrospun PVA/HAp NC nanofibers prepared by the ES process will open up a wide variety of future applications related to hard tissue replacement and regeneration (bone and dentin), not limited to coating implants.

Complete Tem-Tomography: 3D Structure of Gems Cluster

NASA Technical Reports Server (NTRS)

Matsuno, J.; Miyake, A.; Tsuchiyama, A.; Messenger, S.; Nakamura-Messenger, K.

2015-01-01

GEMS (glass with embedded metal and sulfide) grains in interplanetary dust particles (IDPs) are considered to be one of the ubiquitous and fundamental building blocks of solids in the Solar System. They have been considered to be interstellar silicate dust that survived various metamorphism or alteration processes in the protoplanetary disk but the elemental and isotopic composition measurements suggest that most of them have been formed in the protoplanetary disk as condensates from high temperature gas. This formation model is also supported by the formation of GEMS-like grains with respect to the size, mineral assemblage, texture and infrared spectrum by condensation experiments from mean GEMS composition materials. Previous GEMS studies were performed only with 2D observation by transmission electron microscopy (TEM) or scanning TEM (STEM). However, the 3D shape and structure of GEMS grains and the spatial distribution of Fe/FeS's has critical information about their formation and origin. Recently, the 3D structure of GEMS grains in ultrathin sections of cluster IDPs was revealed by electron tomography using a TEM/STEM (JEM-2100F, JEOL). However, CT images of thin sections mounted on Cu grids acquired by conventional TEM-tomography are limited to low tilt angles (e. g., less than absolute value of 75 deg. In fact, previous 3D TEM observations of GEMS were affected by some artifacts related to the limited tilt range in the TEM used. Complete tomographic images should be acquired by rotating the sample tilt angle over a range of more than absolute value of 80 deg otherwise the CT images lose their correct structures. In order to constrain the origin and formation process of GEMS grains more clearly, we performed complete electron tomography for GEMS grains. Here we report the sample preparation method we have developed for this study, and the preliminary results.

Cl-Assisted Large Scale Synthesis of Cm-Scale Buckypapers of Fe₃C-Filled Carbon Nanotubes with Pseudo-Capacitor Properties: The Key Role of SBA-16 Catalyst Support as Synthesis Promoter.

PubMed

Boi, Filippo S; He, Yi; Wen, Jiqiu; Wang, Shanling; Yan, Kai; Zhang, Jingdong; Medranda, Daniel; Borowiec, Joanna; Corrias, Anna

2017-10-23

We show a novel chemical vapour deposition (CVD) approach, in which the large-scale fabrication of ferromagnetically-filled cm-scale buckypapers is achieved through the deposition of a mesoporous supported catalyst (SBA-16) on a silicon substrate. We demonstrate that SBA-16 has the crucial role of promoting the growth of carbon nanotubes (CNTs) on a horizontal plane with random orientation rather than in a vertical direction, therefore allowing a facile fabrication of cm-scale CNTs buckypapers free from the onion-crust by-product observed on the buckypaper-surface in previous reports. The morphology and composition of the obtained CNTs-buckypapers are analyzed in detail by scanning electron microscopy (SEM), Energy Dispersive X-ray (EDX), transmission electron microscopy (TEM), high resolution TEM (HRTEM), and thermogravimetric analysis (TGA), while structural analysis is performed by Rietveld Refinement of XRD data. The room temperature magnetic properties of the produced buckypapers are also investigated and reveal the presence of a high coercivity of 650 Oe. Additionally, the electrochemical performances of these buckypapers are demonstrated and reveal a behavior that is compatible with that of a pseudo-capacitor (resistive-capacitor) with better performances than those presented in other previously studied layered-buckypapers of Fe-filled CNTs, obtained by pyrolysis of dichlorobenzene-ferrocene mixtures. These measurements indicate that these materials show promise for applications in energy storage systems as flexible electrodes.

Novel mesoporous FeAl bimetal oxides for As(III) removal: Performance and mechanism.

PubMed

Ding, Zecong; Fu, Fenglian; Cheng, Zihang; Lu, Jianwei; Tang, Bing

2017-02-01

In this study, novel mesoporous FeAl bimetal oxides were successfully synthesized, characterized, and employed for As(III) removal. Batch experiments were conducted to investigate the effects of Fe/Al molar ratio, dosage, and initial solution pH values on As(III) removal. The results showed that the FeAl bimetal oxide with Fe/Al molar ratio 4:1 (shorten as FeAl-4) can quickly remove As(III) from aqueous solution in a wide pH range. The FeAl-4 before and after reaction with As(III) was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), Brunauer-Emmett-Teller (BET) surface area measurement, and X-ray photoelectron spectroscopy (XPS). The BET results showed that the original FeAl-4 with a high surface area of 223.9 m 2 /g was a mesoporous material. XPS analysis indicated that the surface of FeAl-4 possessed a high concentration of M-OH (where M represents Fe and Al), which was beneficial to the immobility of As(III). The excellent performance of FeAl-4 makes it a potentially attractive material for As(III) removal from aqueous solution. Copyright © 2016 Elsevier Ltd. All rights reserved.

An efficient synthesis of graphenated carbon nanotubes over the tailored mesoporous molecular sieves by chemical vapor deposition

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

Atchudan, R.; Department of Chemistry, CEG Campus, Anna University, Chennai 600025; Joo, Jin., E-mail: joojin@knu.ac.kr

2013-06-01

Highlights: ► Tailored 3D cubic Ni/KIT-6 with large pores was synthesized successfully. ► The new hybrid g-CNTs in large scale were synthesized using Ni/KIT-6 by CVD method. ► The use of mesoporous material by CVD method would be an ideal choice to prepare g-CNTs at reasonable cost. ► This type of g-CNTs might be a new avenue for nano-electronic applications. - Abstract: The new hybrid of graphenated carbon nanotubes (g-CNTs) was superior to either CNTs or graphene. Mesoporous 3D cubic Ni/KIT-6 were synthesized hydrothermally through organic template route and then were used as catalytic template for the production of g-CNTsmore » using acetylene as a carbon precursor by chemical vapor deposition (CVD) method. The deposited new hybrid carbon materials were purified and analyzed by various physico-chemical techniques such as XRD, TGA, SEM, TEM and Raman spectroscopy techniques. The graphitization of CNTs was confirmed by TGA and HRTEM studies. Thermal stability, surface morphology, and structural morphology of these materials were revealed by TGA, SEM and TEM analysis, respectively. Moreover, the tailored mesoporous Ni/KIT-6 molecular sieves were found to possess better quality and massive quantity of g-CNTs produced compared to other catalytic template route.« less

Mesoporous silica wrapped with graphene oxide-conducting PANI nanowires as a novel hybrid electrode for supercapacitor

NASA Astrophysics Data System (ADS)

Javed, Mohsin; Abbas, Syed Mustansar; Siddiq, Mohammad; Han, Dongxue; Niu, Li

2018-02-01

A high charge-carrier transport is an important aim in the synthesis of nanostructures for an effective supercapacitor. This article describes a methodology to prepare mesoporous silica nanoparticles (MSNs) wrapped with graphene oxide (GO) together with conducting polyaniline (PANI) wires. The morphology and chemical structure of the prepared samples have been tested by transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and X-ray diffraction (XRD), whereas the stability and electrostatic interaction of the structures have been verified by thermogravimetric analysis (TGA) and Fourier-transform infrared (FT-IR) spectroscopy, respectively. The supercapacitive behaviour of these nanocomposites has been analysed by cyclic voltammetry (CV), charge-discharge tests, and electrochemical impedance spectroscopy (EIS). Compared with pristine MSNs and PANI, the 20%-GO@MSNs/PANI nanocomposite had the highest specific capacitance, reaching 412 F g-1. The nanocomposite structure maximizes the synergy between mesoporous metal oxide, conducting PANI, and GO, yielding a significantly enhanced specific capacitance, rapid charge-discharge rates, and good cycling stability of the resulting device. The wrapping with GO prevents the structural breakdown and acts as a highly conductive pathway by bridging the individual particles, whereas the MSNs nanoparticles greatly enlarge the specific surface area to facilitate ion transport and charge transfer throughout the cycling performance of supercapacitor. The approach adopted in this article can be applied for preparing similar novel functional materials in future for electrochemical applications.

2D Inversion of Transient Electromagnetic Method (TEM)

NASA Astrophysics Data System (ADS)

Bortolozo, Cassiano Antonio; Luís Porsani, Jorge; Acácio Monteiro dos Santos, Fernando

2017-04-01

A new methodology was developed for 2D inversion of Transient Electromagnetic Method (TEM). The methodology consists in the elaboration of a set of routines in Matlab code for modeling and inversion of TEM data and the determination of the most efficient field array for the problem. In this research, the 2D TEM modeling uses the finite differences discretization. To solve the inversion problem, were applied an algorithm based on Marquardt technique, also known as Ridge Regression. The algorithm is stable and efficient and it is widely used in geoelectrical inversion problems. The main advantage of 1D survey is the rapid data acquisition in a large area, but in regions with two-dimensional structures or that need more details, is essential to use two-dimensional interpretation methodologies. For an efficient field acquisition we used in an innovative form the fixed-loop array, with a square transmitter loop (200m x 200m) and 25m spacing between the sounding points. The TEM surveys were conducted only inside the transmitter loop, in order to not deal with negative apparent resistivity values. Although it is possible to model the negative values, it makes the inversion convergence more difficult. Therefore the methodology described above has been developed in order to achieve maximum optimization of data acquisition. Since it is necessary only one transmitter loop disposition in the surface for each series of soundings inside the loop. The algorithms were tested with synthetic data and the results were essential to the interpretation of the results with real data and will be useful in future situations. With the inversion of the real data acquired over the Paraná Sedimentary Basin (PSB) was successful realized a 2D TEM inversion. The results indicate a robust geoelectrical characterization for the sedimentary and crystalline aquifers in the PSB. Therefore, using a new and relevant approach for 2D TEM inversion, this research effectively contributed to map the most

Growth of boron doped hydrogenated nanocrystalline cubic silicon carbide (3C-SiC) films by Hot Wire-CVD

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

Pawbake, Amit; Tata Institute of Fundamental Research, Colaba, Mumbai 400 005; Mayabadi, Azam

Highlights: • Boron doped nc-3C-SiC films prepared by HW-CVD using SiH{sub 4}/CH{sub 4}/B{sub 2}H{sub 6}. • 3C-Si-C films have preferred orientation in (1 1 1) direction. • Introduction of boron into SiC matrix retard the crystallanity in the film structure. • Film large number of SiC nanocrystallites embedded in the a-Si matrix. • Band gap values, E{sub Tauc} and E{sub 04} (E{sub 04} > E{sub Tauc}) decreases with increase in B{sub 2}H{sub 6} flow rate. - Abstract: Boron doped nanocrystalline cubic silicon carbide (3C-SiC) films have been prepared by HW-CVD using silane (SiH{sub 4})/methane (CH{sub 4})/diborane (B{sub 2}H{sub 6}) gasmore » mixture. The influence of boron doping on structural, optical, morphological and electrical properties have been investigated. The formation of 3C-SiC films have been confirmed by low angle XRD, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Fourier transform infra-red (FTIR) spectroscopy and high resolution-transmission electron microscopy (HR-TEM) analysis whereas effective boron doping in nc-3C-SiC have been confirmed by conductivity, charge carrier activation energy, and Hall measurements. Raman spectroscopy and HR-TEM analysis revealed that introduction of boron into the SiC matrix retards the crystallanity in the film structure. The field emission scanning electron microscopy (FE-SEM) and non contact atomic force microscopy (NC-AFM) results signify that 3C-SiC film contain well resolved, large number of silicon carbide (SiC) nanocrystallites embedded in the a-Si matrix having rms surface roughness ∼1.64 nm. Hydrogen content in doped films are found smaller than that of un-doped films. Optical band gap values, E{sub Tauc} and E{sub 04} decreases with increase in B{sub 2}H{sub 6} flow rate.« less

Enhanced photo-catalytic activity of Sr and Ag co-doped TiO2 nanoparticles for the degradation of Direct Green-6 and Reactive Blue-160 under UV & visible light.

PubMed

Naraginti, Saraschandra; Thejaswini, T V L; Prabhakaran, D; Sivakumar, A; Satyanarayana, V S V; Arun Prasad, A S

2015-10-05

This work is focused on sol-gel synthesis of silver and strontium co-doped TiO2 nanoparticles and their utilization as photo-catalysts in degradation of two textile dyes. Effect of pH, intensity of light, amount of photo-catalyst, concentration of dye, sensitizers, etc., were studied to optimize conditions for obtaining enhanced photo-catalytic activity of synthesized nanoparticles. XRD, BET, HR-TEM, EDAX and UV-Vis (diffused reflectance mode) techniques were used to characterize the nanoparticles. Interestingly, band gap of Sr and Ag co-doped TiO2 nanoparticles showed considerable narrowing (2.6 eV) when compared to Ag doped TiO2 (2.7 eV) and undoped TiO2 (3.17 eV) nanoparticles. Incorporation of Ag and Sr in the lattice of TiO2 could bring isolated energy levels near conduction and valence bands thus narrowing band gap. The XRD analysis shows that both Ag and Sr nanoparticles are finely dispersed on the surface of titania framework, without disturbing its crystalline structure. TEM images indicate that representative grain sizes of Ag-doped TiO2 & Sr and Ag co-doped TiO2 nanoparticles are in the range of 8-20 nm and 11-25 nm, respectively. Effective degradation of Direct Green-6 (DG-6) and Reactive Blue-160 (RB-160) under UV and visible light has been achieved using the photo-catalysts. Sr and Ag co-doped TiO2 photo-catalysts showed higher catalytic activity during degradation process in visible region when compared to Ag-doped and undoped TiO2 nanoparticles which could be attributed to the interactive effect caused by band gap narrowing and enhancement in charge separation. For confirming degradation of the dyes, total organic carbon (TOC) content was monitored periodically. Copyright © 2015 Elsevier B.V. All rights reserved.

Self-Catalyzed Growth of Axial GaAs/GaAsSb Nanowires by Molecular Beam Epitaxy for Photodetectors

DTIC Science & Technology

2015-06-01

blende structure with mixture of stacking faults and twins and the presence of these faults were significantly reduced in the NWs grown on chemically...a) TEM image of the core NW (b) HR-TEM image displaying the stacking faults and twinning defects. (c)SAED pattern showing the ZB crystal structure...of stacking faults and twins and the presence of these faults were significantly reduced in the NWs grown on chemically etched substrates. For

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

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

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

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

TEM Study of Manganese Biosorption by Cyanobacterium Synechocystis 6803

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

Dohnalkova, Alice; Bilskis, Christina L.; Kennedy, David W.

2006-09-01

in cells with very low contrast produced principally by electron-dense manganese precipitates. Thin sections were imaged and analyzed using JEOL 2010 HRTEM coupled with EDS (Oxford) and EELS (Gatan) systems. Manganese uptake was measured using a colorimetric method. Cells incubated with Mn solutions were able to take up about 150uM of Mn(II) or Mn(IV) in 48 hours. The predominant accumulation of Mn was associated with the outer membrane for both Mn substrates. Massive deposits seemed to be related in a large extent to the external polymeric substances (EPS) as shown in Fig. 1A-C. Elemental analyses of these precipitates revealed a signal consistent with manganese phosphate. The potential of EPS such as polysaccharides for biosorption or reduction of metals has been described [4], however, the fact that Mn bound to the EPS withstood multiple washes during TEM sample processing is remarkable. From our work with Gram-negative soil bacteria, we hypothesized that the periplasm, an area between the outer and plasma membrane, might be the storage space for internal Mn in pool B. This phenomenon was not observed at any time point for either culture exposed to the Mn. Instead, thin layers of Mn deposits were often found lining the outer and plasma membrane (F). In the MnCl2 solution only, we also observed fine deposits of Mn precipitates along the thylakoid membranes deep inside the cells (Fig. E). Localization of Mn precipitation sites in Synechocystis has important implications for better understanding of the Mn transport and storage processes within cyanobacterial cells, as well as of metal precipitation, solubilization and cycling in the environment.« less

A novel strategy for water disinfection with a AgNPs/gelatin sponge filter.

PubMed

Wei, Feng; Zhao, Xiaole; Li, Chao; Han, Xiaojun

2018-05-05

Disinfection of bacteria in water with sustainable and energy-efficient methods is still a great challenge. Herein, a novel gelatin sponge with embedded AgNPs is fabricated via freeze-drying using gelatin as the reducing agent to synthesize AgNPs in situ. UV-vis spectroscopy, HRTEM, XRD, and XPS characterization prove the formation of AgNPs with an average size of 8.55 ± 0.35 nm. TEM and SEM images confirm the even distribution of AgNPs throughout the AgNPs/gelatin sponges. The composite sponge has a low bulk density of 20 ± 3.5 mg/cm 3 and a pore size of 6.2 ± 1.5 μm. The AgNPs/gelatin sponges exhibit excellent antibacterial performance to E. coli in water, probably by destroying their cell membranes. The porous AgNPs/gelatin composite sponges are promising filter materials for water disinfection. The removal rate of AgNPs/gelatin composite sponges on E. coli reached almost 100%. Graphical abstract ᅟ.

Simple solution-combustion synthesis of Ni-NiO@C nanocomposites with highly electrocatalytic activity for methanol oxidation

NASA Astrophysics Data System (ADS)

Yu, Jie; Ni, Yonghong; Zhai, Muheng

2018-01-01

Transition metal and its oxide composite nanomaterials are attracting increasing research interest due to their superior properties and extensive applications in many fields. In this paper, Ni-NiO@C nanocomposites were successfully synthesized in one step via a simple solution-combustion route, employing NiCl2 as the Ni source, oxygen in the atmosphere as the oxygen source, and ethanol as the solvent. The final product was characterized by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), (high resolution) transmission electron microscopy (TEM/HRTEM), and Raman spectra. N2 gas sorption-desorption experiments uncovered that the BET surface area of Ni-NiO@C nanocomposites reached 161.9 m2 g-1, far higher than 34.2 m2 g-1 of Ni-NiO. The electrochemical measurement showed that the as-produced Ni-NiO@C nanocomposites presented better catalytic activity for the electro-oxidation of methanol than Ni-NiO and NiO, which provides a new catalyst selection for the electro-oxidation of methanol.

Bluish green emitting carbon quantum dots synthesized from jackfruit (Artocarpus heterophyllus) and its sensing applications of Hg (II) and Cr (VI) ions

NASA Astrophysics Data System (ADS)

Rajendran, Kalimuthu; Rajendiran, Nagappan

2018-02-01

A simple, economical, and green method for the preparation of water soluble, high fluorescent carbon quantum dots (CQDs) has been prepared via hydrothermal process using jackfruit (Artocarpus heterophyllus) as a carbon source. The optical properties of synthesized CQDs were characterized by UV- visible and fluorescence spectroscopy. Fourier transform infrared spectroscopy (FT-IR), x-ray Diffraction (XRD) and high resolution transmission electron microscopy (HR-TEM) techniques were used to study the composition and size of the CQDs. The prepared CQDs were spherical in shape with an average size of 2.5 nm along with uniform distribution and showed bright bluish green emission properties, without any further surface modification. The prepared CQDs were exhibit high stability at neutral pH and showed high photo-stability under UV light irradiation at 365 nm. The obtained CQDs were effectively utilized as fluorescent probe for highly selective and sensitive detection of Hg2+ and Cr6+ ions in environmental samples with a limit of detection of about 8 and 10 nM respectively.

Enhanced photocatalytic CO2 reduction to CH4 over separated dual co-catalysts Au and RuO2

NASA Astrophysics Data System (ADS)

Dong, Chunyang; Hu, Songchang; Xing, Mingyang; Zhang, Jinlong

2018-04-01

A spatially separated, dual co-catalyst photocatalytic system was constructed by the stepwise introduction of RuO2 and Au nanoparticles (NPs) at the internal and external surfaces of a three dimensional, hierarchically ordered TiO2-SiO2 (HTSO) framework (the final photocatalyst was denoted as Au/HRTSO). Characterization by HR-TEM, EDS-mapping, XRD and XPS confirmed the existence and spatially separated locations of Au and RuO2. In CO2 photocatalytic reduction (CO2PR), Au/HRTSO (0.8%) shows the optimal performance in both the activity and selectivity towards CH4; the CH4 yield is almost twice that of the singular Au/HTSO or HRTSO (0.8%, weight percentage of RuO2) counterparts. Generally, Au NPs at the external surface act as electron trapping agents and RuO2 NPs at the inner surface act as hole collectors. This advanced spatial configuration could promote charge separation and transfer efficiency, leading to enhanced CO2PR performance in both the yield and selectivity toward CH4 under simulated solar light irradiation.

The toxic effects of l-Cysteine-capped cadmium sulfide nanoparticles on the aquatic plant Spirodela polyrrhiza

NASA Astrophysics Data System (ADS)

Khataee, Alireza; Movafeghi, Ali; Nazari, Fatemeh; Vafaei, Fatemeh; Dadpour, Mohammad Reza; Hanifehpour, Younes; Joo, Sang Woo

2014-12-01

Plants play an important role in the fate of nanoparticles in the environment through their uptake, bioaccumulation, and transfer to trophic chains. However, the impacts of nanoparticles on plants as essential components of all ecosystems are not well documented. In the present study, the toxic effects of l-Cysteine-capped CdS nanoparticles on Spirodela polyrrhiza as an aquatic higher plant species were studied. l-Cysteine-capped CdS nanoparticles were synthesized using hydrothermal method and their characteristics were determined by XRD, SEM, HR-TEM, and FT-IR techniques. The diameter of majority of synthesized nanoparticles was about 15-20 nm. Subsequently, the uptake of l-Cysteine-capped CdS nanoparticles by the plant species was confirmed using epifluorescence microscopy. The activity of peroxidase and superoxide dismutase as antioxidant enzymes was assayed and the relative frond number was calculated in the presence of different concentrations of l-Cysteine-capped CdS nanoparticles. The obtained results revealed the toxic effects of the synthesized nanoparticles on S. polyrrhiza, leading to growth reduction and significant changes in antioxidant enzymes' activity.

Performance and stability of Pd nanostructures in an alkaline direct ethanol fuel cell

NASA Astrophysics Data System (ADS)

Carrera-Cerritos, R.; Fuentes-Ramírez, R.; Cuevas-Muñiz, F. M.; Ledesma-García, J.; Arriaga, L. G.

2014-12-01

Pd nanopolyhedral, nanobar and nanorod particles were synthesised using the polyol process and evaluated as anodes in a direct ethanol fuel cell. The materials were physico-chemically characterised by high-resolution transmission electronic microscopy (HR-TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The effect of the operation parameters (i.e., temperature and fuel ethanol concentration) on the maximum power density (MPD) and open circuit voltage (OCV) was investigated. In addition, a stability test was performed by applying three current density steps for fifty cycles. The OCV values increased as the temperature increased for all of the catalysts at low ethanol concentration. Although the MPD increased with temperature for all of the catalyst independent of the ethanol concentration, the effect of the temperature on the MPD for each Pd structure results in different slopes due to the different crystal faces. Finally, a loss of electro-catalytic activity after fifty cycles was observed in all of the catalysts evaluated, which may be in response to morphological changes in the nanostructures.

HYDROTHERMAL SYNTHESIS OF α-MoO3 NANORODS FOR NO2 DETECTION

NASA Astrophysics Data System (ADS)

Bai, Shouli; Chen, Song; Tian, Yuan; Luo, Ruixian; Li, Dianqing; Chen, Aifan

2012-12-01

Thermodynamically stable molybdenum trioxide nanorods have been successfully synthesized by a simple hydrothermal process. The product exhibits high-quality, single-crystalline layered orthorhombic structure (α-MoO3), and aspect ratio over 20 by characterizations of X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and Fourier transform infrared (FT-IR). The growth mechanism of α-MoO3 nanorods can be understood by electroneutral and dehydration reaction, which is highly dependent on solution acidity and hydrothermal temperature. The sensing tests show that the sensor based on MoO3 nanorods exhibits high sensitivity to NO2 and is not interferred by CO and CH4, which makes this kind sensor a competitive candidate for NO2 detection. The intrinsic sensing performance of MoO3 maybe arise from its nonstoichiometry of MoO3 owing to the presence of Mo5+ and oxygen vacancy in MoO3 lattice, which has been confirmed by X-ray photoelectron spectroscopy (XPS) analysis. The sensing mechanism of MoO3 for NO2 is also discussed.

Facile Synthesis and Optical Properties of Small Selenium Nanocrystals and Nanorods

NASA Astrophysics Data System (ADS)

Jiang, Fengrui; Cai, Weiquan; Tan, Guolong

2017-06-01

Selenium is an important element for human's health, small size is very helpful for Se nanoparticles to be absorbed by human's body. Here, we present a facile approach to fabrication of small selenium nanoparticles (Nano-Se) as well as nanorods by dissolving sodium selenite (Na2SeO3) in glycerin and using glucose as the reduction agent. The as-prepared selenium nanoparticles have been characterized by X-ray diffraction (XRD), UV-Vis absorption spectroscopy and high resolution transmission electron microscope (HRTEM). The morphology of small Se nanoparticles and nanorods have been demonstrated in the TEM images. A small amount of 3-mercaptoproprionic acid (MPA) and glycerin play a key role on controlling the particle size and stabilize the dispersion of Nano-Se in the glycerin solution. In this way, we obtained very small and uniform Se nanoparticles; whose size ranges from 2 to 6 nm. This dimension is much smaller than the best value (>20 nm) ever reported in the literatures. Strong quantum confinement effect has been observed upon the size-dependent optical spectrum of these Se nanoparticles.

Fe-polyaniline composite nanofiber catalyst for chemoselective hydrolysis of oxime.

PubMed

Mahato, Sanjit Kumar; Bhaumik, Madhumita; Maji, Arun; Dutta, Abhijit; Maiti, Debabrata; Maity, Arjun

2018-03-01

A facile chemoselective one-pot strategy for the deprotection of oxime has been developed using Fe 0 -polyaniline composite nanofiber (Fe 0 -PANI), as a catalyst. Nano material based Fe 0 -PANI catalyst has been synthesized via in-situ polymerization of ANI monomer and followed by reductive deposition of Fe 0 onto PANI matrix. The catalyst was characterized by FE-SEM, HR-TEM, BET, XRD, ATR-FTIR, XPS and VSM techniques. The scope of the transformation was studied for aryl, alkyl and heteroarylketoxime with excellent chemoselectivity (>99%). Mechanistic investigations suggested the involvement of a cationic intermediate with Fe 3+ active catalytic species. Substituent effect showed a linear free energy relationship. The activation energy (E a ) was calculated to be 17.46 kJ mol -1 for acetophenone oxime to acetophenone conversion. The recyclability of the catalyst demonstrated up to 10 cycles without any significant loss of efficiency. Based on the preliminary experiments a plausible mechanism has been proposed involving a carbocationic intermediate. Copyright © 2017 Elsevier Inc. All rights reserved.

Questing and the application for silicon based ternary compound within ultra-thin layer of SIS intermediate region

NASA Astrophysics Data System (ADS)

Chen, Shumin; Gao, Ming; Wan, Yazhou; Du, Huiwei; Li, Yong; Ma, Zhongquan

2016-12-01

A silicon based ternary compound was supposed to be solid synthesized with In, Si and O elements by magnetron sputtering of indium tin oxide target (ITO) onto crystal silicon substrate at 250 °C. To make clear the configuration of the intermediate region, a potential method to obtain the chemical bonding of Si with other existing elements was exploited by X-ray photoelectron spectroscopy (XPS) instrument combined with other assisted techniques. The phase composition and solid structure of the interfacial region between ITO and Si substrate were investigated by X-ray diffraction (XRD) and high resolution cross sectional transmission electron microscope (HR-TEM). A photovoltaic device with structure of Al/Ag/ITO/SiOx/p-Si/Al was assembled by depositing ITO films onto the p-Si substrate by using magnetron sputtering. The new matter has been assumed to be a buffer layer for semiconductor-insulator-semiconductor (SIS) photovoltaic device and plays critical role for the promotion of optoelectronic conversion performance from the view point of device physics.

Superior lithium-ion insertion/extraction properties of a novel LiFePO4/C/graphene material used as a cathode in aqueous solution.

PubMed

Duan, Wenyuan; Zhao, Mingshu; Shen, Junfang; Zhao, Suixin; Song, Xiaoping

2017-09-28

Herein, olivine LiFePO 4 covered with graphene and carbon layers is prepared via a sol-gel method, followed by calcination, and the resultant composite is used as a cathode material in aqueous rechargeable lithium-ion batteries (ARLBs). The phase structure and morphology of the composite are characterized via X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and specific surface area analysis (BET). The ARLB system is fabricated using LiFePO 4 /C/graphene as the cathode and a zinc anode in 1 mol L -1 ZnSO 4 ·7H 2 O and saturated LiNO 3 aqueous solution without dissolved oxygen, which delivers a capacity of 153 mA h g -1 at 0.5C rate. Even at a 50C rate, it maintains a capacity of 95 mA h g -1 after 200 cycles. The excellent rate capabilities show that this cathode material exhibits good electrochemical performance and this novel ARLB has great potential in the fields of energy storage and high power sources.

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

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

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

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

Habit plane-driven P2-type manganese-based layered oxide as long cycling cathode for Na-ion batteries

NASA Astrophysics Data System (ADS)

Luo, Rui; Wu, Feng; Xie, Man; Ying, Yao; Zhou, Jiahui; Huang, Yongxin; Ye, Yusheng; Li, Li; Chen, RenJie

2018-04-01

Layered transition metal oxides are considered to be promising candidates as cathode materials for sodium-ion batteries. Herein, a facile solid-state reaction is developed to synthesize hexagons plate-like Na0.67Ni0.25Mn0.75O2+δ (denoted as P2-NNM) material with habit plane formed. The structure of this layered oxide is characterized by XRD, HR-TEM and SAED. The layered material delivers a high reversible capacity of 91.8 mAh g-1 at 0.2 C with a capacity retention of 94.4 % after 280 cycles, superior rate capability and long cycle life (84.2 % capacity retention after 1000 cycle). Ni2+ is an active ion and Ni doping alleviates the Jahn-Teller distortion, and Mn3+/Mn4+ coexist as Mn4+ is desired from the stability perspective. Particularly, CV and XPS results confirm these results. Moreover, the electrode exhibits a quasi-solid-solution reaction during the sodium extraction and insertion. This contribution demonstrates that P2-NNM is a promising cathode electrode for rechargeable long-life sodium-ion batteries.

Sonocatalytic removal of naproxen by synthesized zinc oxide nanoparticles on montmorillonite.

PubMed

Karaca, Melike; Kıranşan, Murat; Karaca, Semra; Khataee, Alireza; Karimi, Atefeh

2016-07-01

ZnO/MMT nanocomposite as sonocatalyst was prepared by immobilizing synthesized ZnO on the montmorillonite surface. The characteristics of as-prepared nanocomposite were studied by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD) techniques. The synthesized samples were used as a catalyst for sonocatalytic degradation of naproxen. ZnO/MMT catalyst in the presence of ultrasound irradiation was more effective compared to pure ZnO nanoparticles and MMT particles in the sonocatalysis of naproxen. The effect of different operational parameters on the sonocatalytic degradation of naproxen including initial drug concentration, sonocatalyst dosage, solution pH, ultrasonic power and the presence of organic and inorganic scavengers were evaluated. It was found that the presence of the scavengers suppressed the sonocatalytic degradation efficiency. The reusability of the nanocomposite was examined in several consecutive runs, and the degradation efficiency decreased only 2% after 5 repeated runs. The main intermediates of naproxen degradation were determined by gas chromatography-mass spectrometry (GC-Mass). Copyright © 2016 Elsevier B.V. All rights reserved.

Size dependent Raman and absorption studies of single walled carbon nanotubes synthesized by pulse laser deposition at room temperature

NASA Astrophysics Data System (ADS)

Dixit, Saurabh; Singhal, Sonal; Vankar, V. D.; Shukla, A. K.

2017-10-01

In this article, size dependent correlation of acoustic states is established for radial breathing mode (RBM). Single walled carbon nanotubes (SWCNTs) are synthesized along with carbon encapsulated iron nanoparticles by pulse laser deposition at room temperature. Ferrocene is used as a catalyst for growth of SWCNTs. Various studies such as HR-TEM, X-Ray Diffraction (XRD), Raman spectroscopy and NIR-Absorption spectroscopy are utilized to confirm the presence of SWCNTs in the as-synthesized and purified samples. RBM of SWCNTs can be differentiated here from Raman modes of carbon encapsulated iron nanoparticles by comparing their line shape asymmetry as well as oscillator strength. Furthermore, a quantum confinement model is proposed for RBM. It is invoked here that RBM is manifestation of quantum confinement of acoustic phonons. Well reported analytical relation of RBM is utilized to explore the nature of phonons responsible for RBM on the basis of quantum confinement model. Diameters of SWCNTs estimated by Raman studies are found to be in reasonably good agreement with that of NIR-absorption studies.

Green Synthesis of Silver Nanoparticles Stabilized with Mussel-Inspired Protein and Colorimetric Sensing of Lead(II) and Copper(II) Ions

PubMed Central

Cheon, Ja Young; Park, Won Ho

2016-01-01

This articles reports a simple and green method for preparing uniform silver nanoparticles (AgNPs), for which self-polymerized 3,4-dihydroxy-l-phenylalanine (polyDOPA) is used as the reducing and stabilizing agent in aqueous media. The AgNPs functionalized by polyDOPA were analyzed by UV–Vis spectroscopy, high-resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), Raman spectrophotometry, and X-ray diffraction (XRD) techniques. The results revealed that the polyDOPA-AgNPs with diameters of 25 nm were well dispersed due to the polyDOPA. It was noted that the polyDOPA-AgNPs showed selectivity for Pb2+ and Cu2+ detection with the detection limits for the two ions as low as 9.4 × 10−5 and 8.1 × 10−5 μM, respectively. Therefore, the polyDOPA-AgNPs can be applied to both Pb2+ and Cu2+ detection in real water samples. The proposed method will be useful for colorimetric detection of heavy metal ions in aqueous media. PMID:27916894

An insight into the influence of crystallite size on the performances of microsized spherical Li(Ni0.5Co0.2Mn0.3)O2 cathode material composed of aggregated nanosized particles

NASA Astrophysics Data System (ADS)

Fan, Guangxin; Wen, Yin; Liu, Baozhong; Yang, Wenpeng

2018-02-01

Relationships between the performance and the crystallite size of the microsized spherical Li(Ni0.5Co0.2Mn0.3)O2 cathode material composed of aggregated nanosized primary particles have been comprehensively studied. The cathode material was synthesized by a high-temperature solid-state method. The results obtained by XRD, Rietveld refinement, SEM, HR-TEM, DSC, and galvanostatic test show that the crystallite size (XS) of Li(Ni0.5Co0.2Mn0.3)O2 is greatly affected by the temperature in the range of 750 to 820 °C. Most of all, the crystallite size plays a unique role in the performance of the material. That is, the electrochemical characteristics of Li(Ni0.5Co0.2Mn0.3)O2, such as discharge capacity, rate performance, and thermal stability, are closely related to the crystallite size. Furthermore, the retention of discharge capacity is determined by that of crystallite size in Li(Ni0.5Co0.2Mn0.3)O2 after 100 cycles.

A thermal study on the structural changes of bimetallic ZrO2-modified TiO2 nanotubes synthesized using supercritical CO2.

PubMed

Lucky, R A; Charpentier, P A

2009-05-13

In this study the thermal behavior of bimetallic ZrO(2)-TiO(2) (10/90 mol/mol) nanotubes are discussed which were synthesized via a sol-gel process in supercritical carbon dioxide (scCO(2)). The effects of calcination temperature on the morphology, phase structure, mean crystallite size, specific surface area and pore volume of the nanotubes were investigated by using a variety of physiochemical techniques. We report that SEM and TEM images showed that the nanotubular structure was preserved at up to 800 degrees C calcination temperature. When exposed to higher temperatures (900-1000 degrees C) the ZrO(2)-TiO(2) tubes deformed and the crystallites fused together, forming larger crystallites, and a bimetallic ZrTiO(4) species was detected. These results were further examined using TGA, FTIR, XRD and HRTEM analysis. The BET textural properties demonstrated that the presence of a small amount of Zr in the TiO(2) matrix inhibited the grain growth, stabilized the anatase phase and increased the thermal stability.

Effect of Sn doping on the structural, optical and electrical properties of TiO2 films prepared by spray pyrolysis

NASA Astrophysics Data System (ADS)

Arunachalam, A.; Dhanapandian, S.; Manoharan, C.

2016-02-01

In this work, highly oriented pure and Tin-doped Titanium dioxide (Sn-doped TiO2) with porous nature photoelectrodes were deposited on ITO glass plates using spray pyrolysis technique. The XRD pattern revealed the formation of anatase TiO2 with the maximum intensity of (101) plane while doping 6 at% of Sn. The morphological studies depicted the porous nature with the uniform arrangement of small-sized grains. The presence of tin confirmed with the EDX spectra. The size of particles of 13 nm was observed from High Resolution Transmission Electron Microscopy (HR-TEM) analysis. The average transmittance was about 85% for the doped photoelectrode and was observed for the photoelectrode deposited with 6 at% of tin, with decreased energy band gap. The PL study showed the emission peak at 391 nm. The maximum carrier concentration and Hall mobility was observed for the photoelectrode deposited with 6 at% of tin. With these studies, the DSSCs were prepared separately with the dye extracted from Hibiscus Rosasinesis and Hibiscus Surttasinesis and their efficiency was maximum for the DSSC prepared with 6 at% of tin.

New insights into the toxicity of mineral fibres: A combined in situ synchrotron μ-XRD and HR-TEM study of chrysotile, crocidolite, and erionite fibres found in the tissues of Sprague-Dawley rats.

PubMed

Gualtieri, Alessandro F; Bursi Gandolfi, Nicola; Pollastri, Simone; Burghammer, Manfred; Tibaldi, Eva; Belpoggi, Fiorella; Pollok, Kilian; Langenhorst, Falko; Vigliaturo, Ruggero; Dražić, Goran

2017-05-15

Along the line of the recent research topic aimed at understanding the in vivo activity of mineral fibres and their mechanisms of toxicity, this work describes the morpho-chemical characteristics of the mineral fibres found in the tissues of Sprague-Dawley rats subjected to intraperitoneal/intrapleural injection of UICC chrysotile, UICC crocidolite and erionite-Na from Nevada (USA). The fibres are studied with in situ synchrotron powder diffraction and high resolution transmission electron microscopy to improve our understanding of the mechanisms of toxicity of these mineral fibres. In contact with the tissues of the rats, chrysotile fibres are prone to dissolve, with leaching of Mg and production of a silica rich relict. On the other hand, crocidolite and erionite-Na fibres are stable even for very long contact times within the tissues of the rats, showing just a thin dissolution amorphous halo. These findings support the model of a lower biopersistence of chrysotile with respect to crocidolite and erionite-Na but the formation of a silica-rich fibrous residue after the pseudo-amorphization of chrysotile may justify a higher cytotoxic potential and intense inflammatory activity of chrysotile in the short term in contact with the lung tissues. Copyright © 2017 Elsevier B.V. All rights reserved.

Study the oxidation kinetics of uranium using XRD and Rietveld method

NASA Astrophysics Data System (ADS)

Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

2010-03-01

The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

Development of 89Zr-Ontuxizumab for in vivo TEM-1/endosialin PET applications

PubMed Central

Lange, Sara E.S.; Zheleznyak, Alex; Studer, Matthew; O'Shannessy, Daniel J.; Lapi, Suzanne E.; Van Tine, Brian A.

2016-01-01

Purpose The complexity of sarcoma has led to the need for patient selection via in vivo biomarkers. Tumor endothelial marker-1 (TEM-1) is a cell surface marker expressed by the tumor microenvironment. Currently MORAb-004 (Ontuxizumab), an anti-TEM-1 humanized monoclonal antibody, is in sarcoma clinical trials. Development of positron emission tomography (PET) for in vivo TEM-1 expression may allow for stratification of patients, potentially enhancing clinical outcomes seen with Ontuxizumab. Results Characterization of cell lines revealed clear differences in TEM-1 expression. One high expressing (RD-ES) and one low expressing (LUPI) cell line were xenografted, and mice were injected with 89Zr-Ontuxizumab. PET imaging post-injection revealed that TEM-1 was highly expressed and readily detectable in vivo only in RD-ES. In vivo biodistribution studies confirmed high radiopharmaceutical uptake in tumor relative to normal organs. Experimental Design Sarcoma cell lines were characterized for TEM-1 expression. Ontuxizumab was labeled with 89Zr and evaluated for immunoreactivity preservation. 89Zr-Ontuxizumab was injected into mice with high or null expressing TEM-1 xenografts. In vivo PET imaging experiments were performed. Conclusion 89Zr-Ontuxizumab can be used in vivo to determine high versus low TEM-1 expression. Reliable PET imaging of TEM-1 in sarcoma patients may allow for identification of patients that will attain the greatest benefit from anti-TEM-1 therapy. PMID:26909615

Naturally occurring clay nanoparticles in Latosols of Brazil central region: detection and characterization

NASA Astrophysics Data System (ADS)

Dominika Dybowska, Agnieszka; Luciene Maltoni, Katia; Piella, Jordi; Najorka, Jens; Puntes, Victor; Valsami-Jones, Eugenia

2015-04-01

Stability and reactivity of minerals change as a particle size function, which makes mineral nanoparticles (defined here as <100 nm) fundamentally distinct from the larger size materials. Naturally occurring mineral nanoparticles contribute to many biogeochemical processes, however much remains to be learnt about these materials, their size dependent behavior and environmental significance. Advances in analytical, imaging and spectroscopic techniques made it now possible to study such particles; however we still have limited knowledge of their chemical, structural and morphological identity and reactivity, in particular in soils. The aim of this research was to characterize the naturally occurring nanoparticles in three soils from Brazil central region. The samples were collected in the A horizon, treated with H2O2 to remove organic material, dispersed in ultrasonic bath and wet sieved (53 µm) to remove the sand fraction. The clay fraction was collected by siphoning the supernatant, conditioned in 1000 ml cylinder, according to the Stock's law. This fraction was further processed by re-suspension in water, sonication and repeated centrifugation, to separate the fraction smaller than 100nm. This material, called here the soil "nanofraction", was analyzed using a range of techniques: 1) nanoparticle size/morphology and crystallinity with Transmission Electron Microscopy (TEM operateing in scanning (HAADF-STEM) and High Resolution (HRTEM) mode), 2) size distribution in water with Dynamic Light Scattering (DLS) and surface charge estimated from electrophoretic mobility measurements 3) crystal phase and crystallite size with X-ray Diffraction (XRD) 4) Chemical composition by quantitative analysis of elements (e.g., Si, Fe, Al, Ti) and their spatial distribution with HRTEM/EDS elemental mappings. The nanofraction had an average hydrodynamic particle diameter ranging from 83 to 92nm with a low polydispersity index of 0.13-0.17 and was found highly stable in aqueous

Exploring the potential reservoirs of non specific TEM beta lactamase (bla(TEM)) gene in the Indo-Gangetic region: A risk assessment approach to predict health hazards.

PubMed

Singh, Gulshan; Vajpayee, Poornima; Rani, Neetika; Amoah, Isaac Dennis; Stenström, Thor Axel; Shanker, Rishi

2016-08-15

The emergence of antimicrobial resistant bacteria is an important public health and environmental contamination issue. Antimicrobials of β-lactam group accounts for approximately two thirds, by weight, of all antimicrobials administered to humans due to high clinical efficacy and low toxicity. This study explores β-lactam resistance determinant gene (blaTEM) as emerging contaminant in Indo-Gangetic region using qPCR in molecular beacon format. Quantitative Microbial Risk Assessment (QMRA) approach was adopted to predict risk to human health associated with consumption/exposure of surface water, potable water and street foods contaminated with bacteria having blaTEM gene. It was observed that surface water and sediments of the river Ganga and Gomti showed high numbers of blaTEM gene copies and varied significantly (p<0.05) among the sampling locations. The potable water collected from drinking water facility and clinical settings exhibit significant number of blaTEM gene copies (13±0.44-10200±316 gene copies/100mL). It was observed that E.crassipes among aquatic flora encountered in both the rivers had high load of blaTEM gene copies. The information on prevalence of environmental reservoirs of blaTEM gene containing bacteria in Indo-Gangetic region and risk associated will be useful for formulating strategies to protect public from menace of clinical risks linked with antimicrobial resistant bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of copper on the preparation and characterization of Na-Ca-P borate glasses.

PubMed

Shailajha, S; Geetha, K; Vasantharani, P; Sheik Abdul Kadhar, S P

2015-03-05

Glasses in the system Na2O-CaO-B2O3-P2O5: CuO have been prepared by melt quenching at 1200°C and rapidly cooling at room temperature. The structural, optical and thermal properties have been investigated using X-ray diffraction (XRD), ultraviolet-visible (UV-VIS) spectroscopy, thermogravimetric-differential thermal analysis (TG-DTA), Fourier transform infrared (FTIR) spectroscopy, high resolution scanning electron microscopy (HRSEM) with energy dispersive X-ray (EDX) spectroscopy and high resolution transmission electron microscope (HRTEM) with energy dispersive X-ray (EDAX). The amorphous and crystalline nature of these samples was verified by XRD. Glass transition, crystallization and thermal stability were determined by TG-DTA investigations. Direct optical energy band gaps before and after doping with different percents of copper oxide were evaluated from 4.81eV to 2.99eV indicated the role of copper in the glassy matrix by UV spectra. FTIR spectrum reveals characteristic absorption bands due to various groups of triangular and tetrahedral borate network. Due to the amorphous nature, the particles like agglomerates on the glass surface were investigated by the HRSEM analysis. The crystalline nature of the samples in XRD is confirmed by SAED pattern using HRTEM. Copyright © 2014 Elsevier B.V. All rights reserved.

[Study of the phase transformation of TiO2 with in-situ XRD in different gas].

PubMed

Ma, Li-Jing; Guo, Lie-Jin

2011-04-01

TiO2 sample was prepared by sol-gel method from chloride titanium. The phase transformation of the prepared TiO2 sample was studied by in-situ XRD and normal XRD in different gas. The experimental results showed that the phase transformation temperatures of TiO2 were different under in-situ or normal XRD in different kinds of gas. The transformation of amorphous TiO2 to anatase was controlled by kinetics before 500 degrees C. In-situ XRD showed that the growth of anatase was inhibited, but the transformation of anatase to rutile was accelerated under inactive nitrogen in contrast to air. Also better crystal was obtained under hydrogen than in argon. These all showed that external oxygen might accelerate the growth of TiO2, but reduced gas might partly counteract the negative influence of lack of external oxygen. The mechanism of phase transformation of TiO2 was studied by in-situ XRD in order to control the structure in situ.

Crystal-phase intergradation in InAs nanostructures grown by van der Waals heteroepitaxy on graphene

NASA Astrophysics Data System (ADS)

Choi, Ji Eun; Yoo, Jinkyoung; Lee, Donghwa; Hong, Young Joon; Fukui, Takashi

2018-04-01

This study demonstrates the crystal-phase intergradation of InAs nanostructures grown on graphene via van der Waals epitaxy. InAs nanostructures with diverse diameters are yielded on graphene. High-resolution transmission electron microscopy (HR-TEM) reveals two crystallographic features of (i) wurtzite (WZ)-to-zinc blende (ZB) intergradation along the growth direction of InAs nanostructures and (ii) an increased mean fraction of ZB according to diameter increment. Based on the HR-TEM observations, a crystal-phase intergradation diagram is depicted. We discuss how the formation of a WZ-rich phase during the initial growth stage is an effective way of releasing heterointerfacial stress endowed by the lattice mismatch of InAs/graphene for energy minimization in terms of less in-plane lattice mismatching between WZ-InAs and graphene. The WZ-to-ZB evolution is responsible for the attenuation of the bottom-to-top surface charge interaction as growth proceeds.

Towards single crystalline, highly monodisperse and catalytically active gold nanoparticles capped with probiotic Lactobacillus plantarum derived lipase

NASA Astrophysics Data System (ADS)

Khan, Imran; Nagarjuna, Ravikiran; Ray Dutta, Jayati; Ganesan, Ramakrishnan

2018-03-01

Owing to the eco-friendly nature of biomolecules, there lies a huge interest in exploring them as capping agents for nanoparticles to achieve stability and biocompatibility. Lipase extracted from the probiotic Lactobacillus plantarum is utilized for the first time to study its efficacy in capping gold nanoparticles (GNPs) in the room temperature synthesis using HAuCl4. The synthesized lipase-capped GNPs are characterized using UV-visible spectroscopy, FT-IR, HR-TEM, DLS and zeta potential measurements. Importantly, selected area electron diffraction (SAED) studies with HR-TEM have revealed the effect of lipase capping in tuning the polycrystallinity of the GNPs. The lipase-capped GNPs are explored for their catalytic efficiency towards an environmentally and industrially important conversion of 4-nitrophenol to 4-aminophenol. Exploiting the amine functional groups in the protein, the recoverability and reusability of the GNPs have been demonstrated through immobilization over amine-functionalized Fe3O4 nanoparticles.

Limitations to the Measurement of Oxygen Concentrations by HRTEM Imposed by Surface Roughness

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

Lupini, Andrew R; Chisholm, Matthew F; van Benthem, Klaus

2005-01-01

In an article published in Microscopy and Microanalysis recently (Jia et al., 2004), it was claimed that aberration-corrected high resolution transmission electron microscopy (HRTEM) allows the quantitative measurement of oxygen concentrations in ceramic materials with atomic resolution. Similar claims have recently appeared elsewhere, based on images obtained through aberration correction (Jia et al., 2003; Jia & Urban, 2004) or very high voltages (Zhang et al., 2003). Seeing oxygen columns is a significant achievement of great importance (Spence, 2003) that will doubtlessly allow some exciting new science; however, other models could provide a better explanation for some of the experimental datamore » than variations in the oxygen concentration. Quantification of the oxygen concentrations was attempted by comparing experimental images with simulations in which the fractional occupancy in individual oxygen columns was reduced. The results were interpreted as representing nonstoichiometry within the bulk and at grain boundaries. This is plausible because previous studies have shown that grain boundaries can be nonstoichiometric (Kim et al., 2001), and it is indeed possible that oxygen vacancies are present at boundaries or in the bulk. However, is this the only possible interpretation? We show that for the thicknesses considered a better match to the images is obtained using a simple model of surface damage in which atoms are removed from the surface, which would usually be interpreted as surface damage or local thickness variation (from ion milling, for example).« less

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury

PubMed Central

Li, Cen; Yang, Hongxia; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao

2016-01-01

Zuotai (gTso thal) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100–800 nm, which commonly further aggregate into 1–30 μm loosely amorphous particles. XRD test shows that β-HgS, S8, and α-HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai, and it would play a positive role in interpreting this mysterious Tibetan drug. PMID:27738409

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury.

PubMed

Li, Cen; Yang, Hongxia; Du, Yuzhi; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao; Wei, Lixin

2016-01-01

Zuotai ( gTso thal ) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100-800 nm, which commonly further aggregate into 1-30  μ m loosely amorphous particles. XRD test shows that β -HgS, S 8 , and α -HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai , and it would play a positive role in interpreting this mysterious Tibetan drug.

Synthesis, analysis and processing of novel materials in the yttrium oxide-aluminum oxide system

NASA Astrophysics Data System (ADS)

Marchal, Julien Claudius

In the current work, liquid feed flame spray pyrolysis (LF-FSP) was used to create three novel nanopowders in the Y2O3-Al 2O3 system: alpha-Al2O3, YAG (garnet Y3Al5O12) and hexagonal Y3Al 5O12. For example, LF-FSP combustion of metalloorganic yttrium and aluminum precursors in a 3/5 ratio forms hexagonal Y3Al5O 12, a newly discovered crystalline phase detailed in this work. The resulting 15-35 nm average particle size, single crystal nanopowders were characterized by TGA-DTA, XRD, HR-TEM, electron diffraction and FTIR. The data was used to establish a model for the crystal structure of this new phase (hexagonal, with crystal parameter of a = 0.736 nm, c = 1.052) consisting of a superlattice of substituted hexagonal YAlO3. YAG has been extensively investigated for its applications as scintillators, phosphors and as a laser host. Fully dispersible, unaggregated single crystal YAG nanopowders with average particle sizes of 35-50 nm were obtained from hexagonal Y3Al5O12 after annealing at 850°C-1200°C (for 2h-8d). The resulting YAG nanopowder was processed into green bodies using cold isostatic pressing after adding binders. 99%+ dense monoliths were obtained after sintering at 1400°C in vacuum (6-8 h), while maintaining grain sizes < 500 nm. The ability to sinter while keeping sub-micron grains differs from present techniques (where translucency is obtained through exaggerated grain growth to 5-10 microns) reported in the literature for sintering polycrystalline YAG, and is the first step for improving polycrystalline YAG laser host optical properties. LF-FSP processing of transition Al2O3 nanopowders converts them to single crystal alpha-Al2O3 nanopowders, previously thought impossible to obtain. The alpha-Al2O 3 nanopowders thus obtained, consist of unaggregated 30-40 nm single particles. These nanopowders were characterized by XRD, HR-TEM, SEM, DLS, FTIR. Green bodies of alpha-Al2O3 nanopowders were sintered to 99% density without sintering aids at 1400°C (6

Facile synthesis of the Li-rich layered oxide Li1.23Ni0.09Co0.12Mn0.56O2 with superior lithium storage performance and new insights into structural transformation of the layered oxide material during charge-discharge cycle: in situ XRD characterization.

PubMed

Shen, Chong-Heng; Wang, Qin; Fu, Fang; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Su, Hang; Zheng, Xiao-Mei; Xu, Bin-Bin; Li, Jun-Tao; Sun, Shi-Gang

2014-04-23

In this work, the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 was synthesized through a facile route called aqueous solution-evaporation route that is simple and without waste water. The as-prepared Li1.23Ni0.09Co0.12Mn0.56O2 oxide was confirmed to be a layered LiMO2-Li2MnO3 solid solution through ex situ X-ray diffraction (ex situ XRD) and transmission electron microscopy (TEM). Electrochemical results showed that the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material can deliver a discharge capacity of 250.8 mAhg(-1) in the 1st cycle at 0.1 C and capacity retention of 86.0% in 81 cycles. In situ X-ray diffraction technique (in situ XRD) and ex situ TEM were applied to study structural changes of the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material during charge-discharge cycles. The study allowed observing experimentally, for the first time, the existence of β-MnO2 phase that is appeared near 4.54 V in the first charge process, and a phase transformation of the β-MnO2 to layered Li0.9MnO2 is occurred in the initial discharge process by evidence of in situ XRD pattrens and selected area electron diffraction (SAED) patterns at different states of the initial charge and discharge process. The results illustrated also that the variation of the in situ X-ray reflections during charge-discharge cycling are clearly related to the changes of lattice parameters of the as-prepared Li-rich oxide during the charge-discharge cycles.

Matching 4.7-Å XRD spacing in amelogenin nanoribbons and enamel matrix.

PubMed

Sanii, B; Martinez-Avila, O; Simpliciano, C; Zuckermann, R N; Habelitz, S

2014-09-01

The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. © International & American Associations for Dental Research.

Matching 4.7-Å XRD Spacing in Amelogenin Nanoribbons and Enamel Matrix

PubMed Central

Sanii, B.; Martinez-Avila, O.; Simpliciano, C.; Zuckermann, R.N.; Habelitz, S.

2014-01-01

The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. PMID:25048248

Strain and grain size of TiO2 nanoparticles from TEM, Raman spectroscopy and XRD: The revisiting of the Williamson-Hall plot method

NASA Astrophysics Data System (ADS)

Kibasomba, Pierre M.; Dhlamini, Simon; Maaza, Malik; Liu, Chuan-Pu; Rashad, Mohamed M.; Rayan, Diaa A.; Mwakikunga, Bonex W.

2018-06-01

The Williamson-Hall (W-H) equation, which has been used to obtain relative crystallite sizes and strains between samples since 1962, is revisited. A modified W-H equation is derived which takes into account the Scherrer equation, first published in 1918, (which traditionally gives more absolute crystallite size prediction) and strain prediction from Raman spectra. It is found that W-H crystallite sizes are on average 2.11 ± 0.01 times smaller than the sizes from Scherrer equation. Furthermore the strain from the W-H plots when compared to strain obtained from Raman spectral red-shifts yield factors whose values depend on the phases in the materials - whether anatase, rutile or brookite. Two main phases are identified in the annealing temperatures (350 °C-700 °C) chosen herein - anatase and brookite. A transition temperature of 550 °C has been found for nano-TiO2 to irreversibly transform from brookite to anatase by plotting the Raman peak shifts against the annealing temperatures. The W-H underestimation on the strain in the brookite phase gives W-H/Raman factor of 3.10 ± 0.05 whereas for the anatase phase, one gets 2.46 ± 0.03. The new βtot2cos2θ-sinθ plot and when fitted with a polynomial yield less strain but much better matching with experimental TEM crystallite sizes and the agglomerates than both the traditional Williamson-Hall and the Scherrer methods. There is greater improvement in the model when linearized - that is the βtotcos2θ-sinθ plot rather than the βtot2cos2θ-sinθ plot.

Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting (TEM) 2015

DTIC Science & Technology

2017-05-01

ARL-CR-0814 ● MAY 2017 US Army Research Laboratory Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting...0814 ● MAY 2017 US Army Research Laboratory Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting (TEM) 2015 by...SUBTITLE Robotics Collaborative Technology Alliance (RCTA): Technical Exchange Meeting (TEM) 2015 5a. CONTRACT NUMBER W911NF-10-2-0016 5b. GRANT

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Johnson, David K; Lee, Christopher; Dazen, Kevin

2015-07-04

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Lee, Christopher M; Dazen, Kevin; Kafle, Kabindra

2015-01-01

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Fabrication and textural characterization of nanoporous carbon electrodes embedded with CuO nanoparticles for supercapacitors.

PubMed

Prasad, Kumaresa P S; Dhawale, Dattatray S; Sivakumar, Thiripuranthagan; Aldeyab, Salem S; Zaidi, Javaid S M; Ariga, Katsuhiko; Vinu, Ajayan

2011-08-01

We introduce a novel strategy of fabricating nanoporous carbons loaded with different amounts of CuO nanoparticles via a hard templating approach, using copper-containing mesoporous silica as the template and sucrose as the carbon source. The nature and dispersion of the CuO nanoparticles on the surface of the nanoporous carbons were investigated by x-ray diffraction (XRD), high-resolution scanning electron microscopy (HRSEM) and high-resolution transmission electron microscopy (HRTEM). XRD results reveal that nanoporous carbons with embedded CuO nanoparticles exhibit a well-ordered mesoporous structure, whereas the nitrogen adsorption measurements indicate the presence of excellent textural characteristics such as high surface area, large pore volume and uniform pore size distribution. The amount of CuO nanoparticles in the nanochannels of the nanoporous carbon could be controlled by simply varying the Si/Cu molar ratio of the mesoporous silica template. Morphological characterization by SEM and TEM reveals that high-quality CuO nanoparticles are distributed homogeneously within the nanoporous carbon framework. The supercapacitance behavior of the CuO-loaded nanoporous carbons was investigated. The material with a small amount of CuO in the mesochannels and high surface area affords a maximum specific capacitance of 300 F g -1 at a 20 mV s -1 scan rate in an aqueous electrolyte solution. A supercapacitor containing the CuO-loaded nanoporous carbon is highly stable and exhibits a long cycle life with 91% specific capacitance retained after 1000 cycles.

Fabrication and textural characterization of nanoporous carbon electrodes embedded with CuO nanoparticles for supercapacitors

NASA Astrophysics Data System (ADS)

Prasad, Kumaresa P. S.; Dhawale, Dattatray S.; Sivakumar, Thiripuranthagan; Aldeyab, Salem S.; Zaidi, Javaid S. M.; Ariga, Katsuhiko; Vinu, Ajayan

2011-08-01

We introduce a novel strategy of fabricating nanoporous carbons loaded with different amounts of CuO nanoparticles via a hard templating approach, using copper-containing mesoporous silica as the template and sucrose as the carbon source. The nature and dispersion of the CuO nanoparticles on the surface of the nanoporous carbons were investigated by x-ray diffraction (XRD), high-resolution scanning electron microscopy (HRSEM) and high-resolution transmission electron microscopy (HRTEM). XRD results reveal that nanoporous carbons with embedded CuO nanoparticles exhibit a well-ordered mesoporous structure, whereas the nitrogen adsorption measurements indicate the presence of excellent textural characteristics such as high surface area, large pore volume and uniform pore size distribution. The amount of CuO nanoparticles in the nanochannels of the nanoporous carbon could be controlled by simply varying the Si/Cu molar ratio of the mesoporous silica template. Morphological characterization by SEM and TEM reveals that high-quality CuO nanoparticles are distributed homogeneously within the nanoporous carbon framework. The supercapacitance behavior of the CuO-loaded nanoporous carbons was investigated. The material with a small amount of CuO in the mesochannels and high surface area affords a maximum specific capacitance of 300 F g-1 at a 20 mV s-1 scan rate in an aqueous electrolyte solution. A supercapacitor containing the CuO-loaded nanoporous carbon is highly stable and exhibits a long cycle life with 91% specific capacitance retained after 1000 cycles.

Fabrication and textural characterization of nanoporous carbon electrodes embedded with CuO nanoparticles for supercapacitors

PubMed Central

Prasad, Kumaresa P S; Dhawale, Dattatray S; Sivakumar, Thiripuranthagan; Aldeyab, Salem S; Zaidi, Javaid S M; Ariga, Katsuhiko; Vinu, Ajayan

2011-01-01

We introduce a novel strategy of fabricating nanoporous carbons loaded with different amounts of CuO nanoparticles via a hard templating approach, using copper-containing mesoporous silica as the template and sucrose as the carbon source. The nature and dispersion of the CuO nanoparticles on the surface of the nanoporous carbons were investigated by x-ray diffraction (XRD), high-resolution scanning electron microscopy (HRSEM) and high-resolution transmission electron microscopy (HRTEM). XRD results reveal that nanoporous carbons with embedded CuO nanoparticles exhibit a well-ordered mesoporous structure, whereas the nitrogen adsorption measurements indicate the presence of excellent textural characteristics such as high surface area, large pore volume and uniform pore size distribution. The amount of CuO nanoparticles in the nanochannels of the nanoporous carbon could be controlled by simply varying the Si/Cu molar ratio of the mesoporous silica template. Morphological characterization by SEM and TEM reveals that high-quality CuO nanoparticles are distributed homogeneously within the nanoporous carbon framework. The supercapacitance behavior of the CuO-loaded nanoporous carbons was investigated. The material with a small amount of CuO in the mesochannels and high surface area affords a maximum specific capacitance of 300 F g-1 at a 20 mV s-1 scan rate in an aqueous electrolyte solution. A supercapacitor containing the CuO-loaded nanoporous carbon is highly stable and exhibits a long cycle life with 91% specific capacitance retained after 1000 cycles. PMID:27877410

Newly developed chitosan-silver hybrid nanoparticles: biosafety and apoptosis induction in HepG2 cells

NASA Astrophysics Data System (ADS)

El-Sherbiny, Ibrahim M.; Salih, Ehab; Yassin, Abdelrahman M.; Hafez, Elsayed E.

2016-07-01

The present study reports the biosafety assessment, the exact molecular effects, and apoptosis induction of newly developed chitosan-silver hybrid nanoparticles (Cs-Ag NPs) in HepG2 cells. The investigated hybrid NPs were green synthesized using Cs/grape leaves aqueous extract (Cs/GLE) or Cs/GLE NPs as reducing and stabilizing agents. The successful formation of Cs/GLE NPs and Cs-Ag hybrid NPs has been confirmed by UV-Vis spectrophotometry, FTIR spectroscopy, XRD, and HRTEM. From the TEM analysis, the prepared Cs/GLE NPs are uniform and spherical with an average size of 150 nm, and the AgNPs (5-10 nm) were formed mainly on their surface. The UV-Vis spectra of Cs-Ag NPs showed a surface plasmon resonance (SPR) peak at about 450 nm confirming their formation. The synthesized Cs-Ag NPs were found to be crystalline as shown by XRD patterns with fcc phase oriented along the (111), (200), (220), and (311) planes. The cytotoxicity patterns, the antiproliferative activities, and the possible mechanisms of anticancer activity at molecular level of the newly developed Cs-Ag hybrid NPs were investigated. Cytotoxicity patterns of all the preparations demonstrated that the nontoxic treatment concentrations are ranged from 0.39 to 50 %, and many of the newly prepared Cs-Ag hybrid NPs showed high anticancer activities against HpG2 cells, and induced cellular apoptosis by downregulating BCL2 gene and upregulating P53.

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

NASA Astrophysics Data System (ADS)

Aswathy Aromal, S.; Philip, Daizy

2012-11-01

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

UV-visible light-activated Ag-decorated, monodisperse TiO2 aggregates for treatment of the pharmaceutical oxytetracycline.

PubMed

Han, Changseok; Likodimos, Vlassis; Khan, Javed Ali; Nadagouda, Mallikarjuna N; Andersen, Joel; Falaras, Polycarpos; Rosales-Lombardi, Pablo; Dionysiou, Dionysios D

2014-10-01

Noble metal Ag-decorated, monodisperse TiO2 aggregates were successfully synthesized by an ionic strength-assisted, simple sol-gel method and were used for the photocatalytic degradation of the antibiotic oxytetracycline (OTC) under both UV and visible light (UV-visible light) irradiation. The synthesized samples were characterized by X-ray diffraction analysis (XRD); UV-vis diffuse reflectance spectroscopy; environmental scanning electron microscopy (ESEM); transmission electron microscopy (TEM); high-resolution TEM (HR-TEM); micro-Raman, energy-dispersive X-ray spectroscopy (EDS); and inductively coupled plasma optical emission spectrometry (ICP-OES). The results showed that the uniformity of TiO2 aggregates was finely tuned by the sol-gel method, and Ag was well decorated on the monodisperse TiO2 aggregates. The absorption of the samples in the visible light region increased with increasing Ag loading that was proportional to the amount of Ag precursor added in the solution over the tested concentration range. The Brunauer, Emmett, and Teller (The BET) surface area slightly decreased with increasing Ag loading on the TiO2 aggregates. Ag-decorated TiO2 samples demonstrated enhanced photocatalytic activity for the degradation of OTC under UV-visible light illumination compared to that of pure TiO2. The sample containing 1.9 wt% Ag showed the highest photocatalytic activity for the degradation of OTC under both UV-visible light and visible light illumination. During the experiments, the detected Ag leaching for the best TiO2-Ag photocatalyst was much lower than the National Secondary Drinking Water Regulation for Ag limit (0.1 mg L(-1)) issued by the US Environmental Protection Agency.

Application of Mythen detector: In-situ XRD study on the thermal expansion behavior of metal indium

NASA Astrophysics Data System (ADS)

Du, Rong; Chen, ZhongJun; Cai, Quan; Fu, JianLong; Gong, Yu; Wu, ZhongHua

2016-07-01

A Mythen detector has been equipped at the beamline 4B9A of Beijing Synchrotron Radiation Facility (BSRF), which is expected to enable BSRF to perform time-resolved measurement of X-ray diffraction (XRD) full-profiles. In this paper, the thermal expansion behavior of metal indium has been studied by using the in-situ XRD technique with the Mythen detector. The indium was heated from 303 to 433 K with a heating rate of 2 K/min. The in-situ XRD full-profiles were collected with a rate of one profile per 10 seconds. Rietveld refinement was used to extract the structural parameters. The results demonstrate that these collected quasi-real-time XRD profiles can be well used for structural analysis. The metal indium was found to have a nonlinear thermal expansion behavior from room temperature to the melting point (429.65 K). The a-axis of the tetragonal unit cell expands with a biquadratic dependency on temperature, while the c-axis contracts with a cubic dependency on temperature. By the time-resolved XRD measurements, it was observed that the [200] preferred orientation can maintain to about 403.15 K. While (110) is the last and detectable crystal plane just before melting of the polycrystalline indium foil. This study is not only beneficial to the application of metal indium, but also exhibits the capacity of in-situ time-resolved XRD measurements at the X-ray diffraction station of BSRF.

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

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

Don Pellinen and Michael Griffin

2009-01-23

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

XMCD and TEM studies of as-cast and rapidly quenched Fe50Nd50 alloys

NASA Astrophysics Data System (ADS)

Menushenkov, V. P.; Menushenkov, A. P.; Shchetinin, I. V.; Wilhelm, F.; Ivanov, A. A.; Rudnev, I. A.; Ivanov, V. G.; Rogalev, A.; Savchenko, A. G.; Zhukov, D. G.; Rafalskiy, A. V.; Ketov, S. V.

2017-12-01

We present the XMCD analysis of as-cast and melt spun Fe50Nd50 samples performed at L2,3 -Nd and K-Fe absorption edges at 5 and 50 K in comparison with macroscopic data of XRD, TEM and magnetic properties measurements. In addition, we have measured the magnetic field dependence of XMCD signal for both types of the samples in magnetic fields up/down to 17 T. The obtained results pointed to the strong difference between structure and magnetic properties of the as-cast and melt spun Fe50Nd50 alloys for both macroscopic and local measurements. The element selective XMCD loops for melt spun alloy show almost identical value of the coercive force Hci for L 2-Nd and K-Fe edges and practically do not depend on temperature. XMCD loop at K-Fe edge is a sum of contributions of the Fe-based phases. The main Fe-rich phase has high Hci ≈ 2,4 T as a highly anisotropic phase. The absence of the K-Fe XMCD loop saturation in the field up to 17 T points to presence of the second Nd-rich Nd-Fe phase which is ferromagnetic at temperature lower than 50 K. In accordance to the TEM results these both phases may coexist as the mixture of nanocrystals which was formed as a result of decomposition of the amorphous-like matrix phase. The XMCD loop at L2 -Nd edge with Hci ≈ 1,9 T is the sum of contributions from two Nd-based phases: hard Fe-rich phase (Hci ≈ 2,4 T) and Nd-Fe matrix phase of medium hardness with Hci ≈ 1,3 T. The macroscopic loop showed the higher Hci compared to XMCD loops. Such discrepancy may be caused by the fact that XMCD signal is collected from a 5-10 mcm thick surface layer, which contains many defects that reduce anisotropy and coercivity.

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.

Silver Trees: Chemistry on a TEM Grid

EPA Science Inventory

The copper/carbon substrate of a TEM grid reacted with aqueous silver nitrate solution within minutes to yield spectacular tree-like silver dendrites, without using any added capping or reducing reagents. These results demonstrate a facile, aqueous, room temperature synthesis of...

Achieving phase transformation and structure control of crystalline anatase TiO2@C hybrids from titanium glycolate precursor and glucose molecules.

PubMed

Cheng, Gang; Stadler, Florian J

2015-01-15

Considerable efforts have focused on functional TiO2@carbonaceous hybrid nanostructured materials (TiO2@C) to satisfy the future requirements of environmental photocatalysis and energy storage using these advanced materials. In this study, we developed a two-step solution-phase reaction to prepare hybrid TiO2@C with tuneable structure and composition from the hydrothermal carbonization (HTC) of glucose. X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis (TGA) were used to determine the crystallite size, composition, and phase purity. The results of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high resolution TEM (HRTEM) showed that the morphology of the as-synthesized TiO2@C hybrids could be controlled by varying the amount of glucose, also acting as the carbon source. Based on the observations made with different glucose concentrations, a formation mechanism of nanoparticulate and nanoporous TiO2@C hybrids was proposed. In addition, the as-synthesized TiO2@C hybrids with different compositions and structures showed enhanced adsorption of visible light and improved dye-adsorption capacity, which supported their potential use as photocatalysts with good activity. This new synthetic approach, using a nanoprecursor, provides a simple and versatile way to prepare TiO2@C hybrids with tuneable composition, structures, and properties, and is expected to lead to a family of composites with designed properties. Copyright © 2014 Elsevier Inc. All rights reserved.

Uniform 2 nm gold nanoparticles supported on iron oxides as active catalysts for CO oxidation reaction: structure-activity relationship

NASA Astrophysics Data System (ADS)

Guo, Yu; Gu, Dong; Jin, Zhao; Du, Pei-Pei; Si, Rui; Tao, Jing; Xu, Wen-Qian; Huang, Yu-Ying; Senanayake, Sanjaya; Song, Qi-Sheng; Jia, Chun-Jiang; Schüth, Ferdi

2015-03-01

Uniform Au nanoparticles (~2 nm) with narrow size-distribution (standard deviation: 0.5-0.6 nm) supported on both hydroxylated (Fe_OH) and dehydrated iron oxide (Fe_O) have been prepared by either deposition-precipitation (DP) or colloidal-deposition (CD) methods. Different structural and textural characterizations were applied to the dried, calcined and used gold-iron oxide samples. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) showed high homogeneity in the supported Au nanoparticles. The ex situ and in situ X-ray absorption fine structure (XAFS) characterization monitored the electronic and short-range local structure of active gold species. The synchrotron-based in situ X-ray diffraction (XRD), together with the corresponding temperature-programmed reduction by hydrogen (H2-TPR), indicated a structural evolution of the iron-oxide supports, correlating to their reducibility. An inverse order of catalytic activity between DP (Au/Fe_OH < Au/Fe_O) and CD (Au/Fe_OH > Au/Fe_O) was observed. Effective gold-support interaction results in a high activity for gold nanoparticles, locally generated by the sintering of dispersed Au atoms on the oxide support in the DP synthesis, while a hydroxylated surface favors the reactivity of externally introduced Au nanoparticles on Fe_OH support for the CD approach. This work reveals why differences in the synthetic protocol translate to differences in the catalytic performance of Au/FeOx catalysts with very similar structural characteristics in CO oxidation.

Green synthesis of carbon dots originated from Lycii Fructus for effective fluorescent sensing of ferric ion and multicolor cell imaging.

PubMed

Sun, Xiaohan; He, Jiang; Yang, Shenghong; Zheng, Mingda; Wang, Yingying; Ma, Shuang; Zheng, Haipeng

2017-10-01

Green, economical and effective method was developed for synthesis of fluorescent carbon dots (CDs), using one-pot hydrothermal treatment of Lycii Fructus. Optical and structural properties of the CDs have been extensively studied by UV-visible and fluorescence spectroscopic, x-ray diffraction (XRD) techniques, transmission electron microscopy (TEM) and high resolution TEM (HRTEM). Surface functionality and composition of CDs has been illustrated by Fourier transform infrared spectroscopy (FTIR), x-ray photoelectron spectroscopy (XPS) spectra and elemental analysis. The fabricated CDs possess stable fluorescent properties. The fluorescent quantum yield of the CDs can reach 17.2%. The prepared CDs emitted a broad fluorescence between 415 and 545nm and their fluorescence was tuned by changing excitation wavelength. Meanwhile, the fluorescence intensity of the CDs could be significantly quenched by Fe 3+ (turn-off). The CDs exhibit captivating sensitivity and selectivity toward Fe 3+ with a linear range from 0 to 30μM and a detection limit of 21nM. The prepared CDs were successfully applied to the determination of Fe 3+ in the urine samples, the water samples from the from the Yellow River and living HeLa (Henrietta Lacks) cells. Moreover, the low-toxicity and excellent biocompatibility of the CDs were evaluated through MTT assay on HeLa cells. The CDs were also employed as fluorescent probes for multicolor imaging of HeLa cells successfully. Copyright © 2017 Elsevier B.V. All rights reserved.

One-Step Synthesis of Titanium Oxyhydroxy-Fluoride Rods and Research on the Electrochemical Performance for Lithium-ion Batteries and Sodium-ion Batteries.

PubMed

Li, Biao; Gao, Zhan; Wang, Dake; Hao, Qiaoyan; Wang, Yan; Wang, Yongkun; Tang, Kaibin

2015-12-01

Titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O rods with a hexagonal tungsten bronze (HTB) structure, was synthesized via a facile one-step solvothermal method. The structure, morphology, and component of the products were characterized by X-ray powder diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), ion chromatograph, energy-dispersive X-ray (EDX) analyses, and so on. Different rod morphologies which ranged from nanoscale to submicron scale were simply obtained by adjusting reaction conditions. With one-dimension channels for Li/Na intercalation/de-intercalation, the electrochemical performance of titanium oxyhydroxy-fluoride for both lithium-ion batteries (LIBs) and sodium-ion batteries (SIBs) was also studied. Electrochemical tests revealed that, for LIBs, titanium oxyhydroxy-fluoride exhibited a stabilized reversible capacity of 200 mAh g(-1) at 25 mA g(-1) up to 120 cycles in the electrode potential range of 3.0-1.2 V and 140 mAh g(-1) at 250 mA g(-1) up to 500 cycles, especially; for SIBs, a high capacity of 100 mAh g(-1) was maintained at 25 mA g(-1) after 115 cycles in the potential range of 2.9-0.5 V.

Novel Co{sub 3}O{sub 4} porous polyhedrons derived from metal–organic framework toward high performance for electrochemical energy devices

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

Chen, Youcun, E-mail: chenyc@aqtc.edu.cn; Hu, Lin

2016-07-15

Co{sub 3}O{sub 4} polyhedrons with porous structure have been synthesized simply by annealing Prussian blue analogue (PBA) Co{sub 3}[Co(CN){sub 6}]{sub 2} polyhedrons at 400 °C in air. The product was characterized by a series of techniques, such as X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), Transmission Electron Microscopy (TEM), High-resolution TEM (HRTEM), X-ray Photoelectron Spectroscopy (XPS), and Brunauer–Emmett–Teller (BET) gas adsorption. Interestingly, when evaluated as an anode material for lithium-ion batteries (LIBs), the Co{sub 3}O{sub 4} porous polyhedrons manifested high reversible capacity (about 1200 mAh g{sup −1} at 50 mA g{sup −1}) and excellent cycling performance. Moreover, theymore » also exhibited a high specific capacitance of 110 Fg{sup −1} when used as an electrode in the supercapacitor. It is suggested that the special morphology and porous nanostructure lead to the promising electrochemical properties. - Graphical abstract: Novel and complicated mesoporous architectures of Co{sub 3}O{sub 4} have been fabricated by thermal decomposition of Prussian Blue Analog (PBA) Co{sub 3}[Co(CN){sub 6}]{sub 2} polyhedrons which obtained at the room temperature. When Co{sub 3}O{sub 4} product was evaluated for Li-ion batteries (LIBs), they exhibited high reversible capacity of 1000 mAh g{sup −1} with excellent cycle life because of the hollow/porous structure. Display Omitted.« less

Uniform 2 nm gold nanoparticles supported on iron oxides as active catalysts for CO oxidation reaction: Structure-activity relationship

DOE PAGES

Guo, Yu; Senanayake, Sanjaya; Gu, Dong; ...

2015-01-12

Uniform Au nanoparticles (~2 nm) with narrow size-distribution (standard deviation: 0.5–0.6 nm) supported on both hydroxylated (Fe_OH) and dehydrated iron oxide (Fe_O) have been prepared by either deposition-precipitation (DP) or colloidal-deposition (CD) methods. Different structural and textural characterizations were applied to the dried, calcined and used gold-iron oxide samples. The transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) described the high homogeneity in the supported Au nanoparticles. The ex-situ and in-situ X-ray absorption fine structure (XAFS) characterization monitored the electronic and short-range local structure of active gold species. The synchrotron-based in-situ X-ray diffraction (XRD), together with the corresponding temperature-programmed reductionmore » by hydrogen (H₂-TPR), indicated a structural evolution of the iron-oxide supports, correlating to their reducibility. An inverse order of catalytic activity between DP (Au/Fe_OH < Au/Fe_O) and CD (Au/Fe_OH > Au/Fe_O) was observed. Effective gold-support interaction results in a high activity for gold nanoparticles, locally generated by the sintering of dispersed Au atoms on the oxide support in the DP synthesis, while a hydroxylated surface favors the reactivity of externally introduced Au nanoparticles on Fe_OH support for the CD approach. This work reveals why differences in the synthetic protocol translate to differences in the catalytic performance of Au/FeO x catalysts with very similar structural characteristics in CO oxidation.« less

Optimization for extracellular biosynthesis of silver nanoparticles by Penicillium aculeatum Su1 and their antimicrobial activity and cytotoxic effect compared with silver ions.

PubMed

Ma, Liang; Su, Wei; Liu, Jian-Xin; Zeng, Xiao-Xi; Huang, Zhi; Li, Wen; Liu, Zheng-Chun; Tang, Jian-Xin

2017-08-01

The present study addresses an eco-friendly and energy-saving method for extracellular biosynthesis of silver nanoparticles (AgNPs) using a cell free filtrate of the fungus strain Penicillium aculeatum Su1 as a reducing agent. Parametric optimization of the biosynthesis process demonstrated different effects on the size, distribution, yield, and synthesis rate of biosynthesized AgNPs. The transmission electron microscopy (TEM) measurements demonstrated that AgNPs were spherical or approximately spherical, with a size between 4 and 55nm. High-resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD) analyses indicated that AgNPs were nanocrystalline by nature, with the character of a face-centered cubic (fcc). Fourier transform infrared spectroscopy (FTIR) analysis confirmed the existence of protein molecules that acted as a reducing agent and a capping agent during the biosynthesis process. Furthermore, the biosynthesized AgNPs exhibited higher antimicrobial activity than silver ions against Gram negative bacteria, Gram positive bacteria and fungi. Compared with silver ions, the biosynthesized AgNPs presented higher biocompatibility toward human bronchial epithelial (HBE) cells and high cytotoxicity in a dose-dependent manner with an IC 50 of 48.73μg/mL toward A549 cells. These results demonstrate that Penicillium aculeatum Su1 is a potential bioresource that can be used to produce low-cost and eco-friendly AgNPs as efficient antimicrobial agent, drug delivery vehicle or anticancer drug for clinic treatment. Copyright © 2017 Elsevier B.V. All rights reserved.

Ionic liquid-assisted preparation of square-shaped Y{sub 2}O{sub 3} nanoplates

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

Wang, Lei; Fang, Hao; Xu, Hualan

Highlights: • Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanosheets were prepared by an ionic liquid-assisted mixed solvothermal route. • Y{sub 2}O{sub 3} nanosheets were obtained after calcining the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanosheets. • The Y{sub 2}O{sub 3} nanosheets are with length of about 300 nm and thickness of several nanometers. - Abstract: Uniform square-shaped Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates with side length of about 300 nm and thickness of tens of nanometers have been successfully prepared by an ionic liquid-assisted mixed solvothermal route. Y{sub 2}O{sub 3} nanoplates with similar size were obtained after calcining the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates atmore » 800 °C. The products were analyzed by powder X-ray diffraction (XRD), thermogravimetric analysis (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution TEM (HRTEM), and electron diffraction (ED). The effects of reaction time, composition of solvents, and the molar ratio of reagents on the morphology of the products have been investigated. The possible formation mechanism of the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates was also discussed. Y{sub 2}O{sub 3}:Eu{sup 3+} nanoplates were also synthesized and their photoluminescent properties were examined.« less

Efficient solar light-driven degradation of Congo red with novel Cu-loaded Fe3O4@TiO2 nanoparticles.

PubMed

Arora, Priya; Fermah, Alisha; Rajput, Jaspreet Kaur; Singh, Harminder; Badhan, Jigyasa

2017-08-01

In this work, Cu-loaded Fe 3 O 4 @TiO 2 core shell nanoparticles were prepared in a single pot by coating of TiO 2 on Fe 3 O 4 nanoparticles followed by Cu loading. X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM), thermogravimetric analysis (TGA), Brunauer-Emmett- Teller (BET), vibrating sample magnetometry (VSM), X-ray photoelectron spectroscopy (XPS), and valence band X-ray photoelectron spectroscopy (VB XPS) techniques were used for characterization of as prepared nanoparticles. Synergism between copper and titania was evaluated by studying the solar light-driven photodegradation of Congo red dye solution in the presence of Fe 3 O 4 @TiO 2 nanoparticles on one side and Cu-loaded Fe 3 O 4 @TiO 2 nanoparticles on the other side. The latter performed better than the former catalyst, indicating the enhanced activity of copper-loaded catalyst. Further photodegradation was studied by three means, i.e., under ultraviolet (UV), refluxing, and solar radiations. Cu-loaded Fe 3 O 4 @TiO 2 enhanced the degradation efficiency of Congo red dye. Thus, Cu act possibly by reducing the band gap of TiO 2 and widening the optical response of semiconductor, as a result of which solar light could be used to carry out photocatalysis. Graphical abstract Photodegradation of congo red over Cu-loaded Fe 3 O 4 @TiO 2 nanoparticles.

Femtosecond nonlinear optical properties of laser ablated gold nanoparticles in water

NASA Astrophysics Data System (ADS)

Krishnakanth, K. N.; Bharathi, M. S. S.; Hamad, S.; Rao, S. Venugopal

2018-04-01

Femtosecond third order nonlinear optical (NLO) properties of ultrafast laser ablated gold (Au) colloidsin distilled waterare investigatedusing degenerate four wave mixing technique with 50fs pulses at 800nm wavelength. The estimated value of χ(3) obtained for Au nanoparticles is 1.93×10-14 e.s.u. The characterization of the NPs was achieved done using TEM and HR-TEM techniques. We also present the time resolved studies of Au colloids by using DFWM technique in the forward BOXCAR phase matching geometry.

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

Comparison between measured and predicted turbulence frequency spectra in ITG and TEM regimes

NASA Astrophysics Data System (ADS)

Citrin, J.; Arnichand, H.; Bernardo, J.; Bourdelle, C.; Garbet, X.; Jenko, F.; Hacquin, S.; Pueschel, M. J.; Sabot, R.

2017-06-01

The observation of distinct peaks in tokamak core reflectometry measurements—named quasi-coherent-modes (QCMs)—are identified as a signature of trapped-electron-mode (TEM) turbulence (Arnichand et al 2016 Plasma Phys. Control. Fusion 58 014037). This phenomenon is investigated with detailed linear and nonlinear gyrokinetic simulations using the Gene code. A Tore-Supra density scan is studied, which traverses through a linear (LOC) to saturated (SOC) ohmic confinement transition. The LOC and SOC phases are both simulated separately. In the LOC phase, where QCMs are observed, TEMs are robustly predicted unstable in linear studies. In the later SOC phase, where QCMs are no longer observed, ion-temperature-gradient (ITG) modes are identified. In nonlinear simulations, in the ITG (SOC) phase, a broadband spectrum is seen. In the TEM (LOC) phase, a clear emergence of a peak at the TEM frequencies is seen. This is due to reduced nonlinear frequency broadening of the underlying linear modes in the TEM regime compared with the ITG regime. A synthetic diagnostic of the nonlinearly simulated frequency spectra reproduces the features observed in the reflectometry measurements. These results support the identification of core QCMs as an experimental marker for TEM turbulence.

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y; Mori, S.; Asthana, R.

2017-01-01

Silicon Carbide (SiC) is a promising material for thermostructural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, Mo-B and TiCu. In this presentation, we report the microstructure of diffusion bonded SA-THX mainly with TiCu interlayers obtained by TEM observations, and the influence of metallic interlayers on the joint microstructure and microhardness will be discussed.

Geoelectrical characterization by joint inversion of VES/TEM in Paraná basin, Brazil

NASA Astrophysics Data System (ADS)

Bortolozo, C. A.; Couto, M. A.; Almeida, E. R.; Porsani, J. L.; Santos, F. M.

2012-12-01

For many years electrical (DC) and transient electromagnetic (TEM) soundings have been used in a great number of environmental, hydrological and mining exploration studies. The data of both methods are interpreted usually by individual 1D models resulting in many cases in ambiguous models. This can be explained by how the two different methodologies sample the subsurface. The vertical electrical sounding (VES) is good on marking very resistive structures, while the transient electromagnetic sounding (TEM) is very sensitive to map conductive structures. Another characteristic is that VES is more sensitive to shallow structures, while TEM soundings can reach deeper structures. A Matlab program for joint inversion of VES and TEM soundings, by using CRS algorithm was developed aiming explore the best of the both methods. Initially, the algorithm was tested with synthetic data and after it was used to invert experimental data from Paraná sedimentary basin. We present the results of a re-interpretation of 46 VES/TEM soundings data set acquired in Bebedouro region in São Paulo State - Brazil. The previous interpretation was based in geoelectrical models obtained by single inversion of the VES and TEM soundings. In this work we present the results with single inversion of VES and TEM sounding inverted by the Curupira Program and a new interpretation based in the joint inversion of both methodologies. The goal is increase the accuracy in determining the underground structures. As a result a new geoelectrical model of the region is obtained.

A Combined XRD/XRF Instrument for Lunar Resource Assessment

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.

1992-01-01

Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of

Synthesis and characterization of RuS2 nanostructures.

PubMed

Díaz, David; Castillo-Blum, Silvia E; Alvarez-Fregoso, Octavio; Rodríguez-Gattorno, Geonel; Santiago-Jacinto, Patricia; Rendon, Luis; Ortiz-Frade, Luis; León-Paredes, Yolia-Judith

2005-12-08

Small naked ruthenium sulfide nanoparticles (NPs) with narrow size distribution (2.5 +/- 0.4 nm of diameter) were synthesized in DMSO colloidal dispersions, under mild reaction conditions and using commercial RuCl3 as precursor. To test the chemical reactivity with soft and hard bases, fresh presynthesized RuS2 colloids were mixed with triethylamine (N(Et)3) and ammonium tetrathiomolybdate ((NH4)2MoS4) dimethyl sulfoxide solutions. Naked N(Et)3 and [MoS4](2-)-capped RuS2 nanoparticle colloids were characterized using UV-visible electronic absorption and emission spectroscopies and high-resolution transmission electron microscopy (HR-TEM). It has also been shown that capped RuS2-[MoS4]2- nanoparticles yield MoO3 crystalline matrix by means of HR-TEM experiments. The emission spectra of RuS2 and N(Et)3-RuS2 dispersions show that both nanosized materials have strong fluorescence. The existence of the ruthenium precursor species in solution was established by cyclic voltammetry. Moreover, naked RuS2 NPs were mixed with a chemical mixture with composition similar to gasoline (dibenzothiophene (Bz2S, 400 ppm), hexane, and toluene (55:45% v/v)). The reaction mixture consisted of two phases; in the polar phase, we found evidences of a strong interaction of Bz2S and toluene with the naked RuS2 NPs. We have also obtained self-organized thin films of capped N(Et)3- and RuS2-[MoS4]2- nanoparticles. In both cases, the shape and thickness of the resulting thin films were controlled by a dynamic vacuum procedure. The thin films have been characterized by atomic force microscopy, scanning electron microscopy, HR-TEM, energy dispersion spectroscopy, X-ray diffraction, and absorbance and fluorescence spectroscopies.

Nanominerals and potentially hazardous elements from coal cleaning rejects of abandoned mines: Environmental impact and risk assessment.

PubMed

Fdez-Ortiz de Vallejuelo, Silvia; Gredilla, Ainara; da Boit, Kátia; Teixeira, Elba C; Sampaio, Carlos H; Madariaga, Juan Manuel; Silva, Luis F O

2017-02-01

Soils around coal mining are important reservoir of hazardous elements (HEs), nanominerals, and ultrafine compounds. This research reports and discusses the soil concentrations of HEs (As, Cd, Cr, Cu, Ni, Pb, and Zn) in coal residues of abandoned mines. To assess differences regarding environmental impact and risk assessment between coal abandoned mines from the Santa Catarina state, eighteen coal cleaning rejects with different mineralogical and chemical composition, from eight abandoned mines were collected. Nanominerals and ultra-fine minerals from mining-contaminated areas were analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high-resolution transmission electron microscope (HR-TEM), providing new information on the mineralogy and nano-mineralogy of these coal residues. The total contents of 57 elements (HEs, alkali metals, and rare earth elements) were analyzed by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The calculation of NWACs (Normalized Average Weighted Concentration), together with the chemometric analysis by Principal component analysis (PCA) confirmed the variability of the samples regarding their city and their mine of origin. Moreover, the results confirmed the existence of hotspots in mines near urban areas. Copyright © 2016 Elsevier Ltd. All rights reserved.

Hierarchical Mesoporous NiO/MnO2@PANI Core-Shell Microspheres, Highly Efficient and Stable Bifunctional Electrocatalysts for Oxygen Evolution and Reduction Reactions.

PubMed

He, Junkai; Wang, Mingchao; Wang, Wenbo; Miao, Ran; Zhong, Wei; Chen, Sheng-Yu; Poges, Shannon; Jafari, Tahereh; Song, Wenqiao; Liu, Jiachen; Suib, Steven L

2017-12-13

We report on the new facile synthesis of mesoporous NiO/MnO 2 in one step by modifying inverse micelle templated UCT (University of Connecticut) methods. The catalyst shows excellent electrocatalytic activity and stability for both the oxygen evolution reaction (OER) and the oxygen reduction reaction (ORR) in alkaline media after further coating with polyaniline (PANI). For electrochemical performance, the optimized catalyst exhibits a potential gap, ΔE, of 0.75 V to achieve a current of 10 mA cm -2 for the OER and -3 mA cm -2 for the ORR in 0.1 M KOH solution. Extensive characterization methods were applied to investigate the structure-property of the catalyst for correlations with activity (e.g., XRD, BET, SEM, HRTEM, FIB-TEM, XPS, TGA, and Raman). The high electrocatalytic activity of the catalyst closely relates to the good electrical conductivity of PANI, accessible mesoporous structure, high surface area, as well as the synergistic effect of the specific core-shell structure. This work opens a new avenue for the rational design of core-shell structure catalysts for energy conversion and storage applications.

Preparation and Characterization of Ato Nanoparticles by Coprecipitation with Modified Drying Method

NASA Astrophysics Data System (ADS)

Liu, Shimin; Liang, Dongdong; Liu, Jindong; Jiang, Weiwei; Liu, Chaoqian; Ding, Wanyu; Wang, Hualin; Wang, Nan

Antimony-doped tin oxide (ATO) nanoparticles were prepared by coprecipitation by packing drying and traditional direct drying (for comparison) methods. The as-prepared ATO nanoparticles were characterized by TG, XRD, EDS, TEM, HRTEM, BET, bulk density and electrical resistivity measurements. Results indicated that the ATO nanoparticles obtained by coprecipitation with direct drying method featured hard-agglomerated morphology, high bulk density, low surface area and low electrical resistivity, probably due to the direct liquid evaporation during drying, the fast shrinkage of the precipitate, the poor removal efficiency of liquid molecules and the hard agglomerate formation after calcination. Very differently, the ATO product obtained by the packing and drying method featured free-agglomerated morphology, low bulk density, high surface area and high electrical resistivity ascribed probably to the formed vapor cyclone environment and liquid evaporation-resistance, avoiding fast liquid removal and improving the removal efficiency of liquid molecules. The intrinsic formation mechanism of ATO nanoparticles from different drying methods was illustrated based on the dehydration process of ATO precipitates. Additionally, the packing and drying time played key roles in determining the bulk density, morphology and electrical conductivity of ATO nanoparticles.

Preparation of electrospun pyrochlore-structure KGdTa2O7:Eu3+ phosphor: the optical and structural properties for white light emitting diode applications.

PubMed

Yim, Chul Jin; Unithrattil, Sanjith; Chung, Woon Jin; Im, Won Bin

2013-12-01

Red emitting nanofibers, KGdTa2O7:Eu3+ were synthesized by electrospinning technique followed by heat treatment. As-prepared uniform fiber precursor with diameter ranging from about 700 nm to about 900 nm were calcined after removing organic species by calcination. The fiber surface become rough and diameter decreased to about 250-340 nm range due to decomposition of organic species and formation of inorganic phase. Morphology, structural and photoluminescent properties of fibers were analyzed using thermogravimetric and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and photoluminescence (PL). TG-DTA analysis indicates that KGdTa2O7:Eu3+ began to crystalize at 520 degrees C. Fibers annealed at 900 degrees C formed well crystallized uniform fibers. Under ultraviolet excitation KGdTa2O7:Eu3+ exhibits red emission due to transitions in 4f states of Eu3+. The excitation band is dominated by the Eu(3+)--O2-charge transfer band peaked at 289 nm. The emission peak is in the region that is ideal for red light emission.

Soybean peroxidase immobilized onto silica-coated superparamagnetic iron oxide nanoparticles: Effect of silica layer on the enzymatic activity.

PubMed

Donadelli, Jorge A; García Einschlag, Fernando S; Laurenti, Enzo; Magnacca, Giuliana; Carlos, Luciano

2018-01-01

Peroxidase immobilization onto magnetic supports is considered an innovative strategy for the development of technologies that involves enzymes in wastewater treatment. In this work, magnetic biocatalysts were prepared by immobilization of soybean peroxidase (SBP) onto different silica-coated superparamagnetic iron oxide nanoparticles. The obtained magnetic biocatalysts were tested for the degradation of malachite green (MG), a pollutant often found in industrial wastewaters and with significant drawbacks for the human and environmental health. A deep physicochemical characterization of the materials was performed by means of X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), High Resolution-Transmission Electron Microscope (HR-TEM) and magnetization measurements among others techniques. Results showed high immobilization yield of SBP onto nanomaterials with excellent properties for magnetic recoverability. A partial loss of activity with respect to free SBP was observed, compatible with the modification of the conformational structure of the enzyme after immobilization. The structural modification depended on the amount (and thickness) of silica present in the hybrid materials and the activity yield of 43% was obtained for the best biocatalyst. Thermal stability and reusability capacity were also evaluated. Copyright © 2017 Elsevier B.V. All rights reserved.

Physicochemcial characteristic of CdS-anchored porous WS2 hybrid in the photocatalytic degradation of crystal violet under UV and visible light irradiation

NASA Astrophysics Data System (ADS)

Vattikuti, S. V. Prabhakar; Ngo, Ich-Long; Byon, Chan

2016-11-01

In this work, we report the synthesis of CdS-incorporated porous WS2 by a simple hydrothermal method. The structural, morphological, and optical properties of the samples were examined by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR), high resolution X-ray photoelectron spectroscopy (XPS) and UV-visible spectrometry. The photocatalytic activities were established for degradation of crystal violet (CV) under UV and visible light irradiation. The CdS-incorporated porous WS2 hybrid demonstrated high photocatalytic activity for degradation of CV pollutant compared to pure CdS nanoparticles and porous WS2 sheets. This result implies that the CdS-incorporated porous WS2 promoted more electron-hole pair transformation under UV and visible light irradiation. This significant enhancement of photocatalytic efficiency of CdS-incorporated porous WS2 photocatalyst under visible light can be ascribed to the presence of CdS nanospheres on the meshed-like WS2 sheets which potentially improves absorption in the visible range enabled by surface plasmon resonance effect of CdS nanospheres. The photostability and reusability of the CdS-porous WS2 were examined through recycling experiments.

A new analytical device incorporating a nitrogen doped lanthanum metal oxide with reduced graphene oxide sheets for paracetamol sensing.

PubMed

Ponnaiah, Sathish Kumar; Prakash, Periakaruppan; Vellaichamy, Balakumar

2018-06-01

The novel N-CeO 2 nanoparticles decorated on reduced graphene oxide (N-CeO 2 @rGO) composite has been synthesized by sonochemical method. The characterization of as prepared nanocomposite was intensely performed by UV-Vis, FT-IR, EDX, FE-SEM, HR-TEM, XRD, and TGA analysis. The synthesized nanomaterial was further investigated for its selective and sensitive sensing of paracetamol (PM) based on a N-CeO 2 @rGO modified glassy carbon electrode. A distinct and improved reversible redox peak of PM is obtained at N-CeO 2 @rGO nanocomposite compared to the electrodes modified with N-CeO 2 and rGO. It displays a very good performance with a wide linear range of 0.05-0.600 μM, a very low detection limit of 0.0098 μM (S/N = 3), a high sensitivity of 268 μA µM -1  cm -2 and short response time (<3 s). Also, the fabricated sensor shows a good sensibleness for the detection of PM in various tablet samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Size-dependent magnetic anisotropy of PEG coated Fe3O4 nanoparticles; comparing two magnetization methods

NASA Astrophysics Data System (ADS)

Nayek, C.; Manna, K.; Imam, A. A.; Alqasrawi, A. Y.; Obaidat, I. M.

2018-02-01

Understanding the size dependent magnetic anisotropy of iron oxide nanoparticles is essential for the successful application of these nanoparticles in several technological and medical fields. PEG-coated iron oxide (Fe3O4) nanoparticles with core diameters of 12 nm, 15 nm, and 16 nm were synthesized by the usual co-precipitation method. The morphology and structure of the nanoparticles were investigated using transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD). Magnetic measurements were conducted using a SQUID. The effective magnetic anisotropy was calculated using two methods from the magnetization measurements. In the first method the zero-field-cooled magnetization versus temperature measurements were used at several applied magnetic fields. In the second method we used the temperature-dependent coercivity curves obtained from the zero-field-cooled magnetization versus magnetic field hysteresis loops. The role of the applied magnetic field on the effective magnetic anisotropy, calculated form the zero-field-cooled magnetization versus temperature measurements, was revealed. The size dependence of the effective magnetic anisotropy constant Keff obtained by the two methods are compared and discussed.

Synthesis and properties of electrically conductive, ductile, extremely long (~50 μm) nanosheets of K(x)CoO2·yH2O.

PubMed

Aksit, Mahmut; Hoselton, Benjamin C; Kim, Ha Jun; Ha, Don-Hyung; Robinson, Richard D

2013-09-25

Extremely long, electrically conductive, ductile, free-standing nanosheets of water-stabilized KxCoO2·yH2O are synthesized using the sol-gel and electric-field induced kinetic-demixing (SGKD) process. Room temperature in-plane resistivity of the KxCoO2·yH2O nanosheets is less than ~4.7 mΩ·cm, which corresponds to one of the lowest resistivity values reported for metal oxide nanosheets. The synthesis produces tens of thousands of very high aspect ratio (50,000:50,000:1 = length/width/thickness), millimeter length nanosheets stacked into a macro-scale pellet. Free-standing nanosheets up to ~50 μm long are readily delaminated from the stacked nanosheets. High-resolution transmission electron microscopy (HR-TEM) studies of the free-standing nanosheets indicate that the delaminated pieces consist of individual nanosheet crystals that are turbostratically stacked. X-ray diffraction (XRD) studies confirm that the nanosheets are stacked in perfect registry along their c-axis. Scanning electron microscopy (SEM) based statistical analysis show that the average thickness of the nanosheets is ~13 nm. The nanosheets show ductility with a bending radius as small as ~5 nm.

Laminarin based AgNPs using brown seaweed Turbinaria ornata and its induction of apoptosis in human retinoblastoma Y79 cancer cell lines

NASA Astrophysics Data System (ADS)

Remya, R. R.; Radhika Rajasree, S. R.; Suman, T. Y.; Aranganathan, L.; Gayathri, S.; Gobalakrishnan, M.; Karthih, M. G.

2018-03-01

Biosynthesis of nanoparticles using isolated compounds from various sources is accepting interest due to their broad array of biological activities and biocompatibility. This paper presents a simple; cost effective and green synthesis of silver nanoparticles (AgNPs) using the polysaccharide, laminarin a storage compound obtained from the brown algae Turbinaria ornata (T. ornata). Initially, the water soluble polysaccharide, laminarin was extracted, purified and analyzed using Matrix Assisted Laser Desorption Ionization Time-of-Flight Mass Spectroscopy (MALDI-TOF MS) and Proton Nuclear Magnetic Resonance (1H NMR). Further, the silver nanoparticles (AgNPs) were synthesized using the isolated laminarin and were characterized by Ultraviolet - visible (UV-vis) spectrophotometer, colour value analysis, Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD) and High Resolution Transmission Electron Microscopy (HR-TEM). The free radical scavenging activities were performed and the effect of cytotoxicity against retinoblastoma Y79 cell lines was also evaluated by in vitro studies. Induction of apoptosis was evident by the percentage of cells arrested in G2/M phase using flow cytometry analysis and was further confirmed by DNA fragmentation study which identified the presence of double strand break.

Synthesis of germanium nanocrystals in high temperature supercritical CO2

NASA Astrophysics Data System (ADS)

Lu, Xianmao; Korgel, Brian A.; Johnston, Keith P.

2005-07-01

Germanium nanocrystals were synthesized in supercritical (sc) CO2 by thermolysis of diphenylgermane (DPG) or tetraethylgermane (TEG) with octanol as a capping ligand at 500 °C and 27.6 MPa. The Ge nanocrystals were characterized with high resolution transmission electron microscopy (HRTEM), energy-dispersive x-ray spectroscopy (EDS), and x-ray diffraction (XRD). On the basis of TEM, the mean diameters of the nanocrystals made from DPG and TEG were 10.1 and 5.6 nm, respectively. The synthesis in sc-CO2 produced much less organic contamination compared with similar reactions in organic supercritical fluids. When the same reaction of DPG with octanol was performed in the gas phase without CO2 present, bulk Ge crystals were formed instead of nanocrystals. Thus, the solvation of the hydrocarbon ligands by CO2 was sufficient to provide steric stabilization. The presence of steric stabilization in CO2 at a reduced temperature of 2.5, with a reduced solvent density of only 0.4, may be attributed to a reduction in the differences between ligand-ligand interactions and ligand-CO2 interactions relative to thermal energy.

High-efficiency and conveniently recyclable photo-catalysts for dye degradation based on urchin-like CuO microparticle/polymer hybrid composites

NASA Astrophysics Data System (ADS)

Liu, Xiong; Cheng, Yuming; Li, Xuefeng; Dong, Jinfeng

2018-05-01

In this work, we developed a new type of photo-catalysts composed of the urchin-like cupric oxide (CuO) microparticle and polyvinylidene fluoride (PVDF) hybrid composites by the convenient organic-inorganic hybrid strategy, which show high-efficiency and conveniently recyclable for dye degradation including methylene blue (MB), Congo red (CR), and malachite green (MG) by visible light irradiation. The micro-structural characteristics of urchin-like CuO microparticles are crucial and dominant over the photo-degrading efficiency of hybrid catalyst because of their highly exposed {0 0 2} facet and larger specific surface area. Simultaneously, the intrinsic porous framework of PVDF membrane not only remains the excellent photo-catalytic activity of urchin-like CuO microparticles but also facilitates the enrichment of dyes on the membrane, and thereby synergistically contributing to the photo-catalytic efficiency. The microstructures of both urchin-like CuO microparticles and hybrid catalysts are systematically characterized by various techniques including scanning electron microscopy (SEM), transmission electron microscope (TEM), high-resolution transmission electron microscope (HRTEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and nitrogen adsorption/desorption isotherms, which evidently support the mentioned mechanism.

Heterogeneous Fenton-like discoloration of methyl orange using Fe3O4/MWCNTs as catalyst: combination mechanism and affecting parameters

NASA Astrophysics Data System (ADS)

Xu, Huan-Yan; Wang, Yuan; Shi, Tian-Nuo; Zhao, Hang; Tan, Qu; Zhao, Bo-Chao; He, Xiu-Lan; Qi, Shu-Yan

2018-03-01

Multi-walled carbon nanotubes (MWCNTs) can act not only as a support for Fe3O4 nanoparticles (NPs) but also as a coworker with synergistic effect, accordingly improving the heterogeneous Fenton-like efficiency of Fe3O4 NPs. In this study, Fe3O4 NPs were in situ anchored onto MWCNTs by a moderate co-precipitation method and the as-prepared Fe3O4/MWCNTs nanocomposites were employed as the highly efficient Fenton-like catalysts. The analyses of XRD, FTIR, Raman, FESEM, TEM and HRTEM results indicated the formation of Fe3O4 crystals in Fe3O4/MWCNTs nanocomposites prepared at different conditions and the interaction between Fe3O4 NPs and MWCNTs. Over a wide pH range, the surface of modified MWCNTs possessed negative charges. Based on these results, the possible combination mechanism between Fe3O4 NPs and MWCNTs was discussed and proposed. Moreover, the effects of preparation and catalytic conditions on the Fenton-like catalytic efficiency were investigated in order to gain further insight into the heterogeneous Fenton-like reaction catalyzed by Fe3O4/MWCNTs nanocomposites.

Temperature induced CuInSe2 nanocrystal formation in the Cu2Se-In3Se2 multilayer thin films

NASA Astrophysics Data System (ADS)

Mohan, A.; Rajesh, S.

2017-04-01

The paper deals with the impact of annealing on Cu2Se-In3Se2 multilayer structure and discusses the quantum confinements. Thermal evaporation technique was used to prepare multilayer films over the glass substrates. The films were annealed at different temperatures (150 °C-350 °C) under vacuum atmosphere. The XRD pattern reveals that the films exhibit (112) peaks with CuInSe2 Chalcopyrite structure and upon annealing crystallinity improved. The grain size comes around 13-19 nm. The optical band gap value was found to be 2.21 to 2.09 eV and band gap splitting was observed for higher annealing temperatures. The increase in the band gap is related to quantum confinement effect. SEM image shows nano crystals spread over the entire surface for higher annealing temperatures. Optical absorption and PL spectra shows the blue shift during annealing. The HR-TEM shows the particle size in the nano range and which confirms the CuInSe2 nanocrystal formation. AFM image shows the rough surface with homogenous grains for the as deposited films and smooth surface for annealed films.

Novel symmetrical coralloid Cu 3D superstructures: Solid-state synthesis from a Cu-carboxylate MOF and their in-situ thermal conversion

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

Chen Lingyun, E-mail: lychen@cqu.edu.c; Shen Yongming; Bai Junfeng, E-mail: bjunfeng@nju.edu.c

2009-08-15

We describe here a one-step solid-state process for the synthesis of metal three-dimensional (3D) superstructures from a metal-organic framework (MOF). Novel symmetrical coralloid Cu 3D superstructures with surface interspersed with clusters of Cu nanoparticles were successfully synthesized by thermolysis of the [Cu{sub 3}(btc){sub 2}] (btc=benzene-1,3,5-tricarboxylato) MOF in a one-end closed horizontal tube furnace (OCTF). The obtained products were characterized by TGA, FT-IR, XRD, EDX, SEM, TEM, HRTEM and SAED. Different reaction conditions were discussed. Furthermore, the synthesized Cu samples were converted into CuO microstructures by in-situ calcination in the air. In addition, the possible formation mechanism was also proposed. Thismore » method is a simple and facile route, which builds a direct linkage between metal-carboxylate MOF crystals and metal nano- or microstructures and also opens a new application field of MOFs. - Graphical abstract: Novel symmetrical coralloid Cu 3D superstructures were synthesized by thermolysis of the [Cu{sub 3}(btc){sub 2}] (btc=benzene-1,3,5-tricarboxylato) MOF microcrystals in a one-end closed horizontal tube furnace (OCTF).« less

Ex Situ Investigation of Anisotropic Interconnection in Silicon-Titanium-Nickel Alloy Anode Material

DOE PAGES

Cho, Jong -Soo; Alaboina, Pankaj Kumar; Kang, Chan -Soon; ...

2017-03-10

Herein we investigate the nanostructural evolution of Silicon-Titanium-Nickel (Si-Ti-Ni) ternary alloy material synthesized by melt spinning process for advanced lithium-ion battery anode. The synthesized material was found to have nano-Silicon particles dispersed in the Ti 4Ni 4Si 7 (STN) alloy buffering matrix and was characterized by X-ray diffraction (XRD), High resolution- transmission electron microscope (HR-TEM), Scanning transmission electron microscopes - energy dispersive X-ray spectrometer (STEM-EDS), and electrochemical performance test. The role of STN matrix is to accommodate the volume expansion stresses of the dispersed Si nanoparticles. However, an interesting behavior was observed during cycling. The Si nanoparticles were observed tomore » form interconnection channels growing through the weak STN matrix cracks and evolving to a network isolating the STN matrix into small puddles. In conclusion, this unique nanostructural evolution of Si particles and isolation of the STN matrix failing to offer significant buffering effect to the grown Si network eventually accelerates more volume expansions during cycling due to less mechanical confinement and leads to performance degradation and poor cycle stability.« less

Pd-NiO decorated multiwalled carbon nanotubes supported on reduced graphene oxide as an efficient electrocatalyst for ethanol oxidation in alkaline medium

NASA Astrophysics Data System (ADS)

Rajesh, Dhanushkotti; Indra Neel, Pulidindi; Pandurangan, Arumugam; Mahendiran, Chinnathambi

2018-06-01

The synthesis of Pd-NiO nanoparticles decorated multiwalled carbon nanotubes (MWCNTs) on reduced graphene oxide (rGO) for ethanol electrooxidation is reported. NiO nanoparticles (NPs) were deposited on functionalized MWCNTs by wet impregnation method. Pd nanoparticles were formed on NiO-MWCNTs by the addition of PdCl2 and its reduction using NaBH4. The Pd-NiO/MWCNTs nanocomposite then deposited on rGO support using ultrasound irradiation which led to the formation of the Pd-NiO/MWCNTs/rGO electrocatalyst. The prepared electrocatalysts were characterized by XRD, SEM, HR-TEM and XPS analysis. Electrochemical measurements demonstrate that as synthesized Pd-NiO/MWCNTs/rGO electrocatalyst exhibit higher catalytic activity (90.89 mA/cm2) than either Pd/MWCNTs/rGO (43.05 mA/cm2) or Pd/C (28.0 mA/cm2) commercial catalyst. Chronoamperometry study of Pd-NiO/MWCNTs/rGO electrocatalyst showed long-term electrochemical stability. The enhanced catalytic activity of Pd-NiO/MWCNTs/rGO electrocatalyst for electrooxidation of ethanol can be attributed to the synergistic effect between Pd & NiO active sites.

Silver nanoparticles synthesized using aqueous leaf extract of Ziziphus oenoplia (L.) Mill: Characterization and assessment of antibacterial activity.

PubMed

Soman, Soumya; Ray, J G

2016-10-01

Biological approach to synthesis of metal nanoparticles using aqueous leaf extract is a highly relevant and recent theme in nanotechnological research. Phytosynthesized AgNPs have better inhibitory and antimicrobial effects compared to aqueous leaf extract and silver nitrate. In the present investigation crystalline silver nanoparticles (AgNPs) with size of 10nm have been successfully synthesized using aqueous leaf extract (AQLE) of Ziziphus oenoplia (L.) Mill., which act as both reducing as well as capping agent. The particles were characterized using UV Visible spectroscopy, HRTEM-EDAX, XRD, FT-IR and DLS. An evaluation of the anti bacterial activity was carried out using Agar well diffusion method and MIC determination against four bacterial strains, Klebsiella pneumoniae, Pseudomonas aeruginosa, Escherichia coli and Salmonella typhi; the AgNPs exhibited quite high antibacterial activity. Furthermore, bactericidal studies with TEM at different time intervals after AgNPs treatment showed the presence of AgNPs near cell membrane of bacteria at about 30min exposure and the bacterial-lysis was found completed at 24h. This gave an insight on the mechanism of bacterial-lysis by direct damage to the cell membrane. Copyright © 2016 Elsevier B.V. All rights reserved.

Green Synthesis of Silver Nanoparticles by using Eucalyptus Globulus Leaf Extract

NASA Astrophysics Data System (ADS)

Balamurugan, Madheswaran; Saravanan, Shanmugam

2017-12-01

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

Minimum depth of investigation for grounded-wire TEM due to self-transients

NASA Astrophysics Data System (ADS)

Zhou, Nannan; Xue, Guoqiang

2018-05-01

The grounded-wire transient electromagnetic method (TEM) has been widely used for near-surface metalliferous prospecting, oil and gas exploration, and hydrogeological surveying in the subsurface. However, it is commonly observed that such TEM signal is contaminated by the self-transient process occurred at the early stage of data acquisition. Correspondingly, there exists a minimum depth of investigation, above which the observed signal is not applicable for reliable data processing and interpretation. Therefore, for achieving a more comprehensive understanding of the TEM method, it is necessary to perform research on the self-transient process and moreover develop an approach for quantifying the minimum detection depth. In this paper, we first analyze the temporal procedure of the equivalent circuit of the TEM method and present a theoretical equation for estimating the self-induction voltage based on the inductor of the transmitting wire. Then, numerical modeling is applied for building the relationship between the minimum depth of investigation and various properties, including resistivity of the earth, offset, and source length. It is guide for the design of survey parameters when the grounded-wire TEM is applied to the shallow detection. Finally, it is verified through applications to a coal field in China.

Reduction of Off-Boresight Fields for a TEM Horn Antenna

DTIC Science & Technology

1994-12-01

model predicts the tapers will reduce the diffraction. Experimental results verify the TPS’s ability to reduce the peak off-hureslht ld& for a. TElL horn...diffractin. Experimental results verify the PS’s ability to reduce the fields foi a T14 horn anitnna xi Reduction of Off-Boresight Fields for a TEM Horn...geometry, has a constant amplitude response. Two simple models repiesent a TEM horn - a high frequency model and a low frequency model [5). At high

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

Binding of TEM-1 beta-lactamase to beta-lactam antibiotics by frontal affinity chromatography.

PubMed

Chen, Xiu; Li, Yuhua; Zhang, Yan; Yang, Jianting; Bian, Liujiao

2017-04-15

TEM-1 beta-lactamases can accurately catalyze the hydrolysis of the beta-lactam rings in beta-lactam antibiotics, which make beta-lactam antibiotics lose its activity, and the prerequisite for the hydrolysis procedure in the binding interaction of TEM-1 beta-lactamases with beta-lactam antibiotics is the beta-lactam rings in beta-lactam antibiotics. Therefore, the binding of TEM-1 beta-lactamase to three beta-lactam antibiotics including penicillin G, cefalexin as well as cefoxitin was explored here by frontal affinity chromatography in combination with fluorescence spectra, adsorption and thermodynamic data in the temperature range of 278-288K under simulated physiological conditions. The results showed that all the binding of TEM-1 beta-lactamase to the three antibiotics were spontaneously exothermic processes with the binding constants of 8.718×10 3 , 6.624×10 3 and 2.244×10 3 (mol/L), respectively at 288K. All the TEM-1 beta-lactamases were immobilized on the surface of the stationary phase in the mode of monolayer and there existed only one type of binding sites on them. Each TEM-1 beta-lactamase bound with only one beta-lactam antibiotic and hydrogen bond interaction and Van der Waals force were the main forces between them. This work provided an insight into the binding interactions between TEM-1 beta-lactamases and beta-lactam antibiotics, which may be beneficial for the designing and developing of new substrates resistant to TEM-1 beta-lactamases. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

2012-08-01

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

Automated SEM and TEM sample preparation applied to copper/low k materials

NASA Astrophysics Data System (ADS)

Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

2001-01-01

We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

TEM in situ cube-corner indentation analysis using ViBe motion detection algorithm

NASA Astrophysics Data System (ADS)

Yano, K. H.; Thomas, S.; Swenson, M. J.; Lu, Y.; Wharry, J. P.

2018-04-01

Transmission electron microscopic (TEM) in situ mechanical testing is a promising method for understanding plasticity in shallow ion irradiated layers and other volume-limited materials. One of the simplest TEM in situ experiments is cube-corner indentation of a lamella, but the subsequent analysis and interpretation of the experiment is challenging, especially in engineering materials with complex microstructures. In this work, we: (a) develop MicroViBE, a motion detection and background subtraction-based post-processing approach, and (b) demonstrate the ability of MicroViBe, in combination with post-mortem TEM imaging, to carry out an unbiased qualitative interpretation of TEM indentation videos. We focus this work around a Fe-9%Cr oxide dispersion strengthened (ODS) alloy, irradiated with Fe2+ ions to 3 dpa at 500 °C. MicroViBe identifies changes in Laue contrast that are induced by the indentation; these changes accumulate throughout the mechanical loading to generate a "heatmap" of features in the original TEM video that change the most during the loading. Dislocation loops with b = ½ <111> identified by post-mortem scanning TEM (STEM) imaging correspond to hotspots on the heatmap, whereas positions of dislocation loops with b = <100> do not correspond to hotspots. Further, MicroViBe enables consistent, objective quantitative approximation of the b = ½ <111> dislocation loop number density.

'How I do it': TEM for tumors of the rectum.

PubMed

Collinson, Rowan J; McC Mortensen, Neil J

2009-02-01

Transanal endoscopic microsurgery (TEM) has an established role in the management of benign rectal tumors. It also has an expanding role in the management of malignant tumors, which is more demanding for the clinician. It requires accurate histological and radiological assessment and draws on an expert understanding of the nature of local recurrence, metastasis, and the place of adjuvant therapies. A multidisciplinary approach is recommended. This paper discusses our institutional approach to TEM for benign and malignant tumors and covers some of the current management controversies.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Synthesis, Characterization, and Application of Gold Nanoparticles in Green Nanochemistry Dye-Sensitized Solar Cells

DTIC Science & Technology

2012-06-01

resolution tunneling electron microscopy (HR-TEM). 2.4 DSSC Assembly Annealed TiO2 nanoparticle photoanodes were placed into 10 mL each of the blackberry ...resolution tunneling electron microscopy, and ultraviolet-visible spectroscopy. After characterization, the NPs were found to vary in shape but had... Blackberry Anthocyanin Extraction Procedure ...............................................................3 2.3 Au Nanoparticle Synthesis

Effect of carbon coating on spontaneous C12A7 whisker formation

NASA Astrophysics Data System (ADS)

Zaikovskii, Vladimir I.; Volodin, Alexander M.; Stoyanovskii, Vladimir O.; Cherepanova, Svetlana V.; Vedyagin, Aleksey A.

2018-06-01

A carbon nanoreactor concept was applied to study the stabilization effect of carbon shell on phase composition and morphology of dodecacalcium hepta-aluminate Ca12Al14O33. The starting C12A7 powder was obtained using aluminum and calcium hydroxides as precursors. Carbon shell was formed by a chemical vapor deposition of divinyl at 550 °C. After the calcination at 1400 °C, the product was characterized by X-ray diffraction analysis (XRD) and high resolution transmission electron microscopy (HRTEM). It was observed for a first time that spontaneous formation of calcium aluminate whiskers take place under the conditions described. Each whisker consists of a 'head' (globular particle of 0.5 microns in diameter) and a 'tail' (prolonged whisker of few microns in length and 0.1-0.2 microns in diameter). According to HRTEM, the 'head' is characterized with microcrystal lattice of Ca12Al14O33 compound. XRD data show the presence of CaAl2O4 phase traces. The 'head' and 'tail' of the whisker are covered with structured graphene layers of 10 nm and 3 nm, correspondingly.

High temperature XRD of Cu2.1Zn0.9SnSe4

NASA Astrophysics Data System (ADS)

Chetty, Raju; Mallik, Ramesh Chandra

2014-04-01

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

Identification of TEM-135 β-Lactamase in Neisseria gonorrhoeae Strains Carrying African and Toronto Plasmids in Argentina

PubMed Central

Gianecini, R.; Oviedo, C.; Littvik, A.; Mendez, E.; Piccoli, L.; Montibello, S.

2014-01-01

One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin. PMID:25367903

TEM-72, a New Extended-Spectrum β-Lactamase Detected in Proteus mirabilis and Morganella morganii in Italy

PubMed Central

Perilli, Mariagrazia; Segatore, Bernardetta; Rosaria De Massis, Maria; Riccio, Maria Letizia; Bianchi, Ciro; Zollo, Alessandro; Rossolini, Gian Maria; Amicosante, Gianfranco

2000-01-01

A new natural TEM-2 derivative, named TEM-72, was identified in a Proteus mirabilis strain and in a Morganella morganii strain isolated in Italy in 1999. Compared to TEM-1, TEM-72 contains the following amino acid substitutions: Q39K, M182T, G238S, and E240K. Kinetic analysis showed that TEM-72 exhibits an extended-spectrum activity, including activity against oxyimino-cephalosporins and aztreonam. Expression of blaTEM-72 in Escherichia coli was capable of decreasing the host susceptibility to the above drugs. PMID:10952610

TEM Study of Internal Crystals in Supernova Graphites

NASA Astrophysics Data System (ADS)

Croat, T. K.; Bernatowicz, T.; Stadermann, F. J.; Messenger, S.; Amari, S.

2003-03-01

A coordinated TEM and isotopic study of ten supernova (SN) graphites from the Murchison meteorite has revealed many internal grains, mostly titanium carbides (TiCs) and TiC-kamacite composite grains, which were accreted during the graphite growth.

VES/TEM 1D joint inversion by using Controlled Random Search (CRS) algorithm

NASA Astrophysics Data System (ADS)

Bortolozo, Cassiano Antonio; Porsani, Jorge Luís; Santos, Fernando Acácio Monteiro dos; Almeida, Emerson Rodrigo

2015-01-01

Electrical (DC) and Transient Electromagnetic (TEM) soundings are used in a great number of environmental, hydrological, and mining exploration studies. Usually, data interpretation is accomplished by individual 1D models resulting often in ambiguous models. This fact can be explained by the way as the two different methodologies sample the medium beneath surface. Vertical Electrical Sounding (VES) is good in marking resistive structures, while Transient Electromagnetic sounding (TEM) is very sensitive to conductive structures. Another difference is VES is better to detect shallow structures, while TEM soundings can reach deeper layers. A Matlab program for 1D joint inversion of VES and TEM soundings was developed aiming at exploring the best of both methods. The program uses CRS - Controlled Random Search - algorithm for both single and 1D joint inversions. Usually inversion programs use Marquadt type algorithms but for electrical and electromagnetic methods, these algorithms may find a local minimum or not converge. Initially, the algorithm was tested with synthetic data, and then it was used to invert experimental data from two places in Paraná sedimentary basin (Bebedouro and Pirassununga cities), both located in São Paulo State, Brazil. Geoelectric model obtained from VES and TEM data 1D joint inversion is similar to the real geological condition, and ambiguities were minimized. Results with synthetic and real data show that 1D VES/TEM joint inversion better recovers simulated models and shows a great potential in geological studies, especially in hydrogeological studies.

Beyond the job exposure matrix (JEM): the task exposure matrix (TEM).

PubMed

Benke, G; Sim, M; Fritschi, L; Aldred, G

2000-09-01

The job exposure matrix (JEM) has been employed to assign cumulative exposure to workers in many epidemiological studies. In these studies, where quantitative data are available, all workers with the same job title and duration are usually assigned similar cumulative exposures, expressed in mgm(-3)xyears. However, if the job is composed of multiple tasks, each with its own specific exposure profile, then assigning all workers within a job the same mean exposure can lead to misclassification of exposure. This variability of exposure within job titles is one of the major weaknesses of JEMs. A method is presented for reducing the variability in the JEM methodology, which has been called the task exposure matrix (TEM). By summing the cumulative exposures of a worker over all the tasks worked within a job title, it is possible to address the variability of exposure within the job title, and reduce possible exposure misclassification. The construction of a TEM is outlined and its application in the context of a study in the primary aluminium industry is described. The TEM was found to assign significantly different cumulative exposures to the majority of workers in the study, compared with the JEM and the degree of difference in cumulative exposure between the JEM and the TEM varied greatly between contaminants.

TEM00 mode Nd:YAG solar laser by side-pumping a grooved rod

NASA Astrophysics Data System (ADS)

Vistas, Cláudia R.; Liang, Dawei; Almeida, Joana; Guillot, Emmanuel

2016-05-01

A simple TEM00 mode solar laser system with a grooved Nd:YAG rod pumped through a heliostat-parabolic mirror system is reported here. The radiation coupling capacity of a fused silica tube lens was combined with the multipass pumping ability of a 2 V-shaped cavity to provide efficient side-pumping along a 4.0 mm diameter grooved Nd:YAG single-crystal rod. TEM00 mode solar laser power of 3.4 W was measured by adopting an asymmetric large-mode laser resonant cavity. Record TEM00 mode solar laser collection efficiency of 3.4 W/m2and slope efficiency of 1.9% was achieved, which corresponds to 1.8 and 2.4 times more than the previous TEM00 mode Nd:YAG solar laser using the PROMES-CNRS heliostat-parabolic mirror system, respectively.

"One-sample concept" micro-combinatory for high throughput TEM of binary films.

PubMed

Sáfrán, György

2018-04-01

Phases of thin films may remarkably differ from that of bulk. Unlike to the comprehensive data files of Binary Phase Diagrams [1] available for bulk, complete phase maps for thin binary layers do not exist. This is due to both the diverse metastable, non-equilibrium or instable phases feasible in thin films and the required volume of characterization work with analytical techniques like TEM, SAED and EDS. The aim of the present work was to develop a method that remarkably facilitates the TEM study of the diverse binary phases of thin films, or the creation of phase maps. A micro-combinatorial method was worked out that enables both preparation and study of a gradient two-component film within a single TEM specimen. For a demonstration of the technique thin Mn x Al 1- x binary samples with evolving concentration from x = 0 to x = 1 have been prepared so that the transition from pure Mn to pure Al covers a 1.5 mm long track within the 3 mm diameter TEM grid. The proposed method enables the preparation and study of thin combinatorial samples including all feasible phases as a function of composition or other deposition parameters. Contrary to known "combinatorial chemistry", in which a series of different samples are deposited in one run, and investigated, one at a time, the present micro-combinatorial method produces a single specimen condensing a complete library of a binary system that can be studied, efficiently, within a single TEM session. That provides extremely high throughput for TEM characterization of composition-dependent phases, exploration of new materials, or the construction of phase diagrams of binary films. Copyright © 2018 Elsevier B.V. All rights reserved.

Identification of TEM-135 β-lactamase in Neisseria gonorrhoeae strains carrying African and Toronto plasmids in Argentina.

PubMed

Gianecini, R; Oviedo, C; Littvik, A; Mendez, E; Piccoli, L; Montibello, S; Galarza, P

2015-01-01

One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

A joint TEM-HLEM geophysical approach to borehole sitting in deeply weathered granitic terrains.

PubMed

Meju, M A; Fontes, S L; Ulugergerli, E U; La Terra, E F; Germano, C R; Carvalho, R M

2001-01-01

The accurate location of aquiferous fracture zones in granite beneath a > 50 m thick weathered mantle in semi-arid regions is a major hydrogeological problem. It is expected that the zone of intensive fracturing will be more susceptible to weathering and thus be characterized by the thickest development of saprolite, a good electrically conductive target for deep-probing electromagnetic systems. The single-loop transient electromagnetic (TEM) technique is well known to have the capability for detecting concealed steep mineralized targets in mining environments and can be adapted to this hydrogeological problem. We propose that combining the conventional frequency-domain horizontal-loop electromagnetic (HLEM) and single-loop TEM is an effective practical approach to locating concealed aquiferous fracture zones. In the supporting case studies presented here, we deployed multifrequency HLEM profiling (with 50 m transmitter-receiver separation) and TEM soundings with contiguous 10 or 20 m sided loops along the survey lines in a granitic terrain affected by deep (> 50 m) weathering in northeast Brazil. A somewhat layered structure consisting of resistive hardpan/leached zone, conductive saprolite, and resistive basement is identifiable in the typical TEM depth sounding data. We obtained coincident HLEM and TEM anomalies at all the sites, enabling a relatively straightforward selection of potential drilling positions. Simple resistivity-depth transformation of the TEM data was done for each site, yielding an approximate section from which drilling depths were estimated. All of the boreholes located were successful. Although our results appear to indicate that the single-loop TEM method could be used independently for borehole sitting in deeply weathered granitic terrains and that the weathering profile over granite can be mapped using TEM depth soundings of appropriate observational bandwidth, we recommend a joint electromagnetic approach for optimal well sitting.

Structure and Dynamics of Domains in Ferroelectric Nanostructures. In-situ TEM Studies

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

Pan, Xiaoqing

2015-06-30

The goal of this project was to explore the structure and dynamic behaviors of ferroelectric domains in ferroelectric thin films and nanostructures by advanced transmission electron microscopy (TEM) techniques in close collaboration with phase field modeling. The experimental techniques used include aberration-corrected sub-Å resolution TEM and in-situ TEM using a novel scanning tunneling microscopy (STM) - TEM holder that allows the direct observation of nucleation and dynamic evolution of ferroelectric domains under applied electric field. Specifically, this project was aimed to (1) to study the roles of static electrical boundary conditions and electrical charge in controlling the equilibrium domain structuresmore » of BiFeO 3 thin films with controlled substrate constraints, (2) to explore the fundamental mechanisms of ferroelectric domain nucleation, growth, and switching under an applied electric field in both uniform thin films and nanostructures, and to understand the roles of crystal defects such as dislocations and interfaces in these processes, (3) to understand the physics of ferroelectric domain walls and the influence of defects on the electrical switching of ferroelectric domains.« less

Microstructural analysis of 800H steel exposed at test operation in HTHL by using FIB-SEM and HRTEM techniques

NASA Astrophysics Data System (ADS)

Marušáková, Daniela; Bublíková, Petra; Berka, Jan; Vávrovcová, Zuzana; Burda, Jaroslav

2017-09-01

To understand the degradation process of metal materials which are used in power engineering, appropriate evaluation procedure is necessary to ensure. In that order, the degradation of alloy 800H during the first period of test operation in High Temperature Helium Loop (HTHL) was tested. Experiment was carried out in atmosphere of pure technical helium with purity 4.6 containing only residual concentration of moisture up to 300 vppm. Parameters during the operation test were not constant, process was interrupted several times. The maximum temperature on specimens during this period was 750 °C, average temperature was 460 °C, gas pressure ranged from 3 to 6 MPa and gas flow from 3 to 9 gs-1. Total duration of the test was 264 h. After the exposure the degradation of specimens was investigated by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). Using the technique of Focused Ion Beam (FIB) integrated within SEM the transparent samples with quality surface parameters were obtained for TEM analysis. FIB technique in combination with High Resolution TEM ensured the guaranteed methodology of exposed sample preparation and precise description of changes in this kind of material.

cisTEM, user-friendly software for single-particle image processing.

PubMed

Grant, Timothy; Rohou, Alexis; Grigorieff, Nikolaus

2018-03-07

We have developed new open-source software called cis TEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cis TEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k - 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cis TEM is available for download from cistem.org. © 2018, Grant et al.

cisTEM, user-friendly software for single-particle image processing

PubMed Central

2018-01-01

We have developed new open-source software called cisTEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cisTEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k – 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cisTEM is available for download from cistem.org. PMID:29513216

Probing the interaction of Rh, Co and bimetallic Rh-Co nanoparticles with the CeO2 support: catalytic materials for alternative energy generation.

PubMed

Varga, E; Pusztai, P; Óvári, L; Oszkó, A; Erdőhelyi, A; Papp, C; Steinrück, H-P; Kónya, Z; Kiss, J

2015-10-28

The interaction of CeO2-supported Rh, Co and bimetallic Rh-Co nanoparticles, which are active catalysts in hydrogen production via steam reforming of ethanol, a process related to renewable energy generation, was studied by X-ray diffraction (XRD), high resolution electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and low energy ion scattering (LEIS). Furthermore, diffuse reflectance infrared spectroscopy (DRIFTS) of adsorbed CO as a probe molecule was used to characterize the morphology of metal particles. At small loadings (0.1%), Rh is in a much dispersed state on ceria, while at higher contents (1-5%), Rh forms 2-8 nm particles. Between 473-673 K pronounced oxygen transfer from ceria to Rh is observed and at 773 K significant agglomeration of Rh occurs. On reduced ceria, XPS indicates a possible electron transfer from Rh to ceria. The formation of smaller ceria crystallites upon loading with Co was concluded from XRD and HRTEM; for 10% Co, the CeO2 particle size decreased from 27.6 to 10.7 nm. A strong dissolution of Co into ceria and a certain extent of encapsulation by ceria were deduced by XRD, XPS and LEIS. In the bimetallic system, the presence of Rh enhances the reduction of cobalt and ceria. During thermal treatments, reoxidation of Co occurs, and Rh agglomeration as well as oxygen migration from ceria to Rh are hindered in the presence of cobalt.

Crystal Face Distributions and Surface Site Densities of Two Synthetic Goethites: Implications for Adsorption Capacities as a Function of Particle Size.

PubMed

Livi, Kenneth J T; Villalobos, Mario; Leary, Rowan; Varela, Maria; Barnard, Jon; Villacís-García, Milton; Zanella, Rodolfo; Goodridge, Anna; Midgley, Paul

2017-09-12

Two synthetic goethites of varying crystal size distributions were analyzed by BET, conventional TEM, cryo-TEM, atomic resolution STEM and HRTEM, and electron tomography in order to determine the effects of crystal size, shape, and atomic scale surface roughness on their adsorption capacities. The two samples were determined by BET to have very different site densities based on Cr VI adsorption experiments. Model specific surface areas generated from TEM observations showed that, based on size and shape, there should be little difference in their adsorption capacities. Electron tomography revealed that both samples crystallized with an asymmetric {101} tablet habit. STEM and HRTEM images showed a significant increase in atomic-scale surface roughness of the larger goethite. This difference in roughness was quantified based on measurements of relative abundances of crystal faces {101} and {201} for the two goethites, and a reactive surface site density was calculated for each goethite. Singly coordinated sites on face {210} are 2.5 more dense than on face {101}, and the larger goethite showed an average total of 36% {210} as compared to 14% for the smaller goethite. This difference explains the considerably larger adsorption capacitiy of the larger goethite vs the smaller sample and points toward the necessity of knowing the atomic scale surface structure in predicting mineral adsorption processes.

Preparation of polyaniline/PbS core-shell nano/microcomposite and its application for photocatalytic H2 electrogeneration from H2O.

PubMed

Rabia, Mohamed; Mohamed, H S H; Shaban, Mohamed; Taha, S

2018-01-18

Lead sulfide (PbS) and polyaniline (PANI) nano/microparticles were prepared. Then, PANI/PbS core-shell nano/microcomposites (I, II, and III) were prepared by oxidative polymerization of different aniline concentrations (0.01, 0.03, and 0.05 M), respectively, in the presence of 0.05 M PbS. FT-IR, XRD, SEM, HR-TEM, and UV-Vis analyses were carried out to characterize the samples. From the FT-IR data, there are redshifts in PbS and PANI nano/microparticles bands in comparison with PANI/PbS nano/microcomposites. The average crystallite sizes of PANI/PbS core-shell nano/microcomposites (I, II, and III) from XRD analyses were 46.5, 55, and 42.16 nm, respectively. From the optical analyses, nano/microcomposite (II) has the optimum optical properties with two band gaps values of 1.41 and 2.79 eV. Then, the nano/microcomposite (II) membrane electrode supported on ITO glass was prepared and applied on the photoelectrochemical (PEC) H 2 generation from H 2 O. The characteristics current-voltage and current-time behaviors were measured at different wavelengths from 390 to 636 nm. Also, the incident photon-to-current conversion efficiency (IPCE) under monochromatic illumination condition was calculated. The optimum values for IPCE were 36.5 and 35.2% at 390 and 405 nm, respectively. Finally, a simple mechanism for PEC H 2 generation from H 2 O using the nano/microcomposite (II) membrane electrode was mentioned.

Synchronizing flash-melting in a diamond cell with synchrotron X ray diffraction (XRD)

NASA Astrophysics Data System (ADS)

Karandikar, Amol; Boehler, Reinhard; Meng, Yue; Rod, Eric; Shen, Guoyin

2013-06-01

The major challenges in measuring melting temperatures in laser heated diamond cells are sample instability, thermal runaway and chemical reactions. To circumvent these problems, we developed a ``flash heating'' method using a modulated CW fiber laser and fast X ray detection capability at APS (Pilatus 1M detector). As an example, Pt spheres of 5 micron diameter were loaded in a single crystal sapphire encapsulation in the diamond cell at 65 GPa and heated in a single flash heating event for 20 ms to reach a desired temperature. A CCD spectrometer and the Pilatus were synchronized to measure the temperature and the XRD signal, respectively, when the sample reached the thermal steady state. Each successive flash heating was done at a higher temperature. The integrated XRD pattern, collected during and after (300 K) each heating, showed no chemical reaction up to 3639 K, the highest temperature reached in the experiment. Pt111 and 200 peak intensity variation showed gradual recrystalization and complete diminishing at about 3600 K, indicating melting. Thus, synchronized flash heating with novel sample encapsulation circumvents previous notorious problems and enables accurate melting temperature measurement in the diamond cell using synchrotron XRD probe. Affiliation 2: Geowissenschaeften, Goethe-Universitaet, Altenhoeferallee 1, D-60438 Frankfurt a.M., Germany.

Preparation of high-quality planar FeRh thin films for in situ TEM investigations

NASA Astrophysics Data System (ADS)

Almeida, Trevor P.; McGrouther, Damien; Pivak, Yevheniy; Perez Garza, Hector Hugo; Temple, Rowan; Massey, Jamie; Marrows, Christopher H.; McVitie, Stephen

2017-10-01

The preparation of a planar FeRh thin film using a focused ion beam (FIB) secondary electron microscope (SEM) for the purpose of in situ transmission electron microscopy (TEM) is presented. A custom SEM stub with 45° faces allows for the transfer and milling of the sample on a TEM heating chip, whilst Fresnel imaging within the TEM revealed the presence of the magnetic domain walls, confirming the quality of the FIB-prepared sample.

1D Cole-Cole inversion of TEM transients influenced by induced polarization

NASA Astrophysics Data System (ADS)

Seidel, Marc; Tezkan, Bülent

2017-03-01

Effects of induced polarization (IP) can have an impact on time-domain electromagnetic measurements (TEM) and may lead to sign reversals in the recorded transients. To study these IP effects on TEM data, a new 1D inversion algorithm was developed for both, the central-loop and the separate-loop TEM configurations using the Cole-Cole relaxation model. 1D forward calculations for a homogeneous half-space were conducted with the aim of analyzing the impacts of the Cole-Cole parameters on TEM transients with respect to possible sign reversals. The forward modelings showed that the variation of different parameters have comparable effects on the TEM transients. This leads to an increasing number of equivalent models as a result of inversion calculations. Subsequently, 1D inversions of synthetic data were performed to study the potentials and limitations of the algorithm regarding the resolution of the Cole-Cole parameters. In order to achieve optimal inversion results, it was essential to error-weight the data points in the direct vicinity of sign reversals. The obtained findings were eventually adopted on the inversion of real field data which contained considerable IP signatures such as sign reversals. One field data set was recorded at the Nakyn kimberlite field in Western Yakutiya, Russia, in the central-loop configuration. Another field data set originates from a waste site in Cologne, Germany, and was measured utilizing the separate-loop configuration.

Coexistence of SHV-4- and TEM-24-Producing Enterobacter aerogenes Strains before a Large Outbreak of TEM-24-Producing Strains in a French Hospital

PubMed Central

Mammeri, H.; Laurans, G.; Eveillard, M.; Castelain, S.; Eb, F.

2001-01-01

In 1996, a monitoring program was initiated at the teaching hospital of Amiens, France, and carried out for 3 years. All extended-spectrum β-lactamase (ESBL)-producing Enterobacter aerogenes isolates recovered from clinical specimens were collected for investigation of their epidemiological relatedness by pulsed-field gel electrophoresis and enterobacterial repetitive intergenic consensus PCR (ERIC-PCR) and determination of the type of ESBL harbored by isoelectric focusing and DNA sequencing. Molecular typing revealed the endemic coexistence, during the first 2 years, of two clones expressing, respectively, SHV-4 and TEM-24 ESBLs, while an outbreak of the TEM-24-producing strain raged in the hospital during the third year, causing the infection or colonization of 165 patients. Furthermore, this strain was identified as the prevalent clone responsible for outbreaks in many French hospitals since 1996. This study shows that TEM-24-producing E. aerogenes is an epidemic clone that is well established in the hospital's ecology and able to spread throughout wards. The management of the outbreak at the teaching hospital of Amiens, which included the reinforcement of infection control measures, failed to obtain complete eradication of the clone, which has become an endemic pathogen. PMID:11376055

TEM Analysis of Interfaces in Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y.; Mori, S.; Asthana R.

2016-01-01

Silicon Carbide (SiC) is a promising material for thermo-structural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, and Mo-B. In this presentation, the result of microstructural analysis obtained by TEM observations and the influence of metallic interlayers and fiber orientation of SA-THX on the joint microstructure will be discussed.

Challenges in quantitative crystallographic characterization of 3D thin films by ACOM-TEM.

PubMed

Kobler, A; Kübel, C

2017-02-01

Automated crystal orientation mapping for transmission electron microscopy (ACOM-TEM) has become an easy to use method for the investigation of crystalline materials and complements other TEM methods by adding local crystallographic information over large areas. It fills the gap between high resolution electron microscopy and electron back scatter diffraction in terms of spatial resolution. Recent investigations showed that spot diffraction ACOM-TEM is a quantitative method with respect to sample parameters like grain size, twin density, orientation density and others. It can even be used in combination with in-situ tensile or thermal testing. However, there are limitations of the current method. In this paper we discuss some of the challenges and discuss solutions, e.g. we present an ambiguity filter that reduces the number of pixels with a '180° ambiguity problem'. For that an ACOM-TEM tilt series of nanocrystalline Pd thin films with overlapping crystallites was acquired and analyzed. Copyright © 2017. Published by Elsevier B.V.

Cross section TEM characterization of high-energy-Xe-irradiated U-Mo

DOE PAGES

Ye, B.; Jamison, L.; Miao, Y.; ...

2017-03-09

U-Mo alloys irradiated with 84 MeV Xe ions to various doses were characterized with transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) techniques. The TEM thin foils were prepared perpendicular to the irradiated surface to allow a direct observation of the entire region modified by ions. Furthermore, depth-selective microstructural information was revealed. Varied irradiation-induced phenomena such as gas bubble formation, phase reversal, and recrystallization were observed at different ion penetration depths in U-Mo.

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

Liu, Shuling, E-mail: liusl8888@yahoo.com.cn; Li, Honglin; Yan, Lu

Graphical abstract: - Highlights: • 3D urchin-like ZnS/CdS composites were synthesized via a two-step method. • The CdS nanoparticles were assembled on the thorns of 3D ZnS urchins. • The ZnS/CdS composites show excellent photocatalytic degradation activities. • The modification of CdS on ZnS is responsible for the enhanced property. - Abstract: Urchin-like ZnS/CdS semiconductor composites were successfully synthesized by combining solvothermal route with homogeneous precipitation process. The as-obtained samples were characterized by means of XRD, EDX, TEM, HR-TEM, ED and FE-SEM techniques. The results show that the as-obtained composites were comprised of the hexagonal structure ZnS and CdS, andmore » CdS nanoparticles were assembled on the surfaces of the thorns of urchin-like ZnS. In addition, the optical properties and photocatalytic activities of the as-prepared ZnS/CdS composites toward some organic dyes (such as Methyl Orange, Pyronine B, Rhodamine B and Methylene Blue) were separately investigated. It is found that the ZnS/CdS composites exhibit excellent photocatalytic degradation activity for these dyes under UV irradiation, as compared to corresponding pure ZnS urchins and commercial anatase TiO{sub 2} (P-25). This enhanced activity may be related to the modification of CdS nanoparticles on the surfaces of thorns of ZnS urchins and a tentative mechanism for the enhanced photocatalytic degradation activities of the ZnS/CdS composite catalyst was proposed.« less

Preparation method of Ni@Pt/C nanocatalyst affects the performance of direct borohydride-hydrogen peroxide fuel cell: Improved power density and increased catalytic oxidation of borohydride.

PubMed

Hosseini, Mir Ghasem; Mahmoodi, Raana

2017-08-15

The Ni@Pt/C electrocatalysts were synthesized using two different methods: with sodium dodecyl sulfate (SDS) and without SDS. The metal loading in synthesized nanocatalysts was 20wt% and the molar ratio of Ni: Pt was 1:1. The structural characterizations of Ni@Pt/C electrocatalysts were investigated by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HR-TEM). The electrocatalytic activity of Ni@Pt/C electrocatalysts toward BH 4 - oxidation in alkaline medium was studied by means of cyclic voltammetry (CV), chronopotentiometry (CP), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS). The results showed that Ni@Pt/C electrocatalyst synthesized without SDS has superior catalytic activity toward borohydride oxidation (22016.92Ag Pt -1 ) in comparison with a catalyst prepared in the presence of SDS (17766.15Ag Pt -1 ) in NaBH 4 0.1M at 25°C. The Membrane Electrode Assembly (MEA) used in fuel cell set-up was fabricated with catalyst-coated membrane (CCM) technique. The effect of Ni@Pt/C catalysts prepared with two methods as anode catalyst on the performance of direct borohydride-hydrogen peroxide fuel cell was studied. The maximum power density was obtained using Ni@Pt/C catalyst synthesized without SDS at 60°C, 1M NaBH 4 and 2M H 2 O 2 (133.38mWcm -2 ). Copyright © 2017 Elsevier Inc. All rights reserved.

Improvement of energy conversion efficiency and power generation in direct borohydride-hydrogen peroxide fuel cell: The effect of Ni-M core-shell nanoparticles (M = Pt, Pd, Ru)/Multiwalled Carbon Nanotubes on the cell performance

NASA Astrophysics Data System (ADS)

Hosseini, M. G.; Mahmoodi, R.

2017-12-01

In this study, core@shell nanoparticles with Ni as a core material and Pt, Pd and Ru as shell materials are synthesized on multiwalled carbon nanotube (MWCNT) as catalyst support using the sequence reduction method. The influence of Ni@Pt, Ni@Pd and Ni@Ru core@shell nanoparticles on MWCNT toward borohydride oxidation in alkaline solution is investigated by various three-electrode electrochemical techniques. Also, the impact of these anodic electrocatalysts on the performance of direct borohydride-hydrogen peroxide fuel cell (DBHPFC) is evaluated. The structural and morphological properties of electrocatalysts are studied by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). The results of three electrode investigations show that Ni@Pd/MWCNT has excellent catalytic activity since borohydride oxidation current density on Ni@Pd/MWCNT (34773.27 A g-1) is 1.37 and 9.19 times higher than those of Ni@Pt/MWCNT (25347.27 A g-1) and Ni@Ru/MWCNT (3782.83 A g-1), respectively. Also, the energy conversion efficiency and power density of DBHPFC with Ni@Pd/MWCNT (246.82 mW cm-2) increase to 34.27% and 51.53% respect to Ni@Pt/MWCNT (162.24 mW cm-2) and Ni@Ru/MWCNT (119.62 mW cm-2), respectively. This study reveals that Ni@Pd/MWCNT has highest activity toward borohydride oxidation and stability in fuel cell.

[Transanal endocopic microsurgery (TEM) in advanced rectal cancer disease treatment].

PubMed

Paci, Marcello; Scoglio, Daniele; Ursi, Pietro; Barchetti, Luciana; Fabiani, Bernardina; Ascoli, Giada; Lezoche, Giovanni

2010-01-01

After Heald's revolution in 1982, who introduced the total mesorectal excision, for improve the results in terms of recurrance and survival rate, there is a need to explore new therapeutic options in treatment of sub-peritoneal rectal cancer. In particular, local excision represent more often a valid technique for non advanced rectal cancer treatment in comparison with the more invasive procedure, especially in elderly and/or in poor health patients. The introduction of TEM by Buess (transanal endoscopy microsurgery), has extended the local treatment also to classes of patients who would normally have been candidates for TME. The author gives literature's details and his experience in the use of TEM for early rectal cancer sub-peritoneal. The aim of the study is to analyze short and long term results in terms of local recurrence and survival rate comparing TEM technique with the other transanal surgery in rectal cancer treatment. Preoperative Chemio-Radio therapy and rigorous Imaging Staging are the first steps to planning surgery. It's time, for local rectal cancer, has come to make the devolution a few decades ago has been accomplished in the treatment of breast cancer

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Hasegawa, Y.; Tsuda, H.; Mori, S.; Halbig, M. C.; Asthana, R.; Singh, M.

2017-01-01

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Effects of diagnostic ionizing radiation on pregnancy via TEM

NASA Astrophysics Data System (ADS)

Mohammed, W. H.; Artoli, A. M.

2008-08-01

In Sudan, X-rays are routinely used at least once for measurements of pelvis during the gestation period, though this is highly prohibited worldwide, except for a few life threatening cases. To demonstrate the effect of diagnostic ionizing radiation on uterus, fetus and neighboring tissues to the ovaries, two independent experiments on pregnant rabbits were conducted. The first experiment was a proof of concept that diagnostic ionizing radiation is hazardous throughout the gestation period. The second experiment was done through Transmission Electron Microscopy (TEM) to elucidate the morphological changes in the ultra structure of samples taken from irradiated pregnant rabbits. This study uses TEM to test the effect of diagnostic radiation of less than 0.6 Gray on the cellular level. Morphological changes have been captured and the images were analyzed to quantify these effects.

TEM1 expression in cancer-associated fibroblasts is correlated with a poor prognosis in patients with gastric cancer

PubMed Central

Fujii, Satoshi; Fujihara, Ayano; Natori, Kei; Abe, Anna; Kuboki, Yasutoshi; Higuchi, Youichi; Aizawa, Masaki; Kuwata, Takeshi; Kinoshita, Takahiro; Yasui, Wataru; Ochiai, Atsushi

2015-01-01

The cancer stroma, including cancer-associated fibroblasts (CAFs), is known to contribute to cancer cell progression and metastasis, suggesting that functional proteins expressed specifically in CAFs might be candidate molecular targets for cancer treatment. The purpose of the present study was to explore the possibility of using TEM1 (tumor endothelial marker 1), which is known to be expressed in several types of mesenchymal cells, as a molecular target by examining the impact of TEM1 expression on clinicopathological factors in gastric cancer patients. A total of 945 consecutive patients with gastric cancer who underwent surgery at the National Cancer Center Hospital East between January 2003 and July 2007 were examined using a tissue microarray approach. TEM1 expression in CAFs or vessel-associated cells was determined using immunohistochemical staining. Three items (CAF-TEM1-positivity, CAF-TEM1-intensity, and vessel-TEM1-intensity) were then examined to determine the correlations between the TEM1 expression status and the recurrence-free survival (RFS), overall survival (OS), cancer-related survival (COS), and other clinicopathological factors. Significant correlations between CAF-TEM1-positivity or CAF-TEM1-intensity and RFS, OS, or COS were observed (P < 0.001, Kaplan–Meier curves); however, no significant correlation between vessel-TEM1-intensity and RFS, OS, or COS was observed. A univariate analysis showed that CAF-TEM1-positivity and CAF-TEM1-intensity were each correlated with a scirrhous subtype, tumor depth, nodal status, distant metastasis, serosal invasion, lymphatic or venous vessel infiltrations, and pTMN stage. This study suggests that the inhibition of TEM1 expression specifically in the CAFs of gastric carcinoma might represent a new strategy for the treatment of gastric cancer. PMID:26336878

Technical Evaluation Motor 3 (TEM-3)

NASA Technical Reports Server (NTRS)

Garecht, Diane

1989-01-01

A primary objective of the technical evaluation motor program is to recover the case, igniter and nozzle hardware for use on the redesigned solid rocket motor flight program. Two qualification objectives were addressed and met on TEM-3. The Nylok thread locking device of the 1U100269-03 leak check port plug and the 1U52295-04 safe and arm utilizing Krytox grease on the barrier-booster shaft O-rings were both certified. All inspection and instrumentation data indicate that the TEM-3 static test firing conducted 23 May 1989 was successful. The test was conducted at ambient conditions with the exception of the field joints (set point of 121 F, with a minimum of 87 F at the sensors), igniter joint (set point at 122 F with a minimum of 87 F at sensors) and case-to-nozzle joint (set point at 114 F with a minimum of 87 F at sensors). Ballistics performance values were within specification requirements. Nozzle performance was nominal with typical erosion. The nozzle and the case joint temperatures were maintained at the heaters controlling set points while electrical power was supplied. The water and the CO2 quench systems prevented damage to the metal hardware. All other test equipment performed as planned, contributing to a successful motor firing. All indications are that the test was a success, and all expected hardware will be refurbished for the RSRM program.

Detecting single-electron events in TEM using low-cost electronics and a silicon strip sensor.

PubMed

Gontard, Lionel C; Moldovan, Grigore; Carmona-Galán, Ricardo; Lin, Chao; Kirkland, Angus I

2014-04-01

There is great interest in developing novel position-sensitive direct detectors for transmission electron microscopy (TEM) that do not rely in the conversion of electrons into photons. Direct imaging improves contrast and efficiency and allows the operation of the microscope at lower energies and at lower doses without loss in resolution, which is especially important for studying soft materials and biological samples. We investigate the feasibility of employing a silicon strip detector as an imaging detector for TEM. This device, routinely used in high-energy particle physics, can detect small variations in electric current associated with the impact of a single charged particle. The main advantages of using this type of sensor for direct imaging in TEM are its intrinsic radiation hardness and large detection area. Here, we detail design, simulation, fabrication and tests in a TEM of the front-end electronics developed using low-cost discrete components and discuss the limitations and applications of this technology for TEM.

Comprehensive analysis of TEM methods for LiFePO4/FePO4 phase mapping: spectroscopic techniques (EFTEM, STEM-EELS) and STEM diffraction techniques (ACOM-TEM).

PubMed

Mu, X; Kobler, A; Wang, D; Chakravadhanula, V S K; Schlabach, S; Szabó, D V; Norby, P; Kübel, C

2016-11-01

Transmission electron microscopy (TEM) has been used intensively in investigating battery materials, e.g. to obtain phase maps of partially (dis)charged (lithium) iron phosphate (LFP/FP), which is one of the most promising cathode material for next generation lithium ion (Li-ion) batteries. Due to the weak interaction between Li atoms and fast electrons, mapping of the Li distribution is not straightforward. In this work, we revisited the issue of TEM measurements of Li distribution maps for LFP/FP. Different TEM techniques, including spectroscopic techniques (energy filtered (EF)TEM in the energy range from low-loss to core-loss) and a STEM diffraction technique (automated crystal orientation mapping (ACOM)), were applied to map the lithiation of the same location in the same sample. This enabled a direct comparison of the results. The maps obtained by all methods showed excellent agreement with each other. Because of the strong difference in the imaging mechanisms, it proves the reliability of both the spectroscopic and STEM diffraction phase mapping. A comprehensive comparison of all methods is given in terms of information content, dose level, acquisition time and signal quality. The latter three are crucial for the design of in-situ experiments with beam sensitive Li-ion battery materials. Furthermore, we demonstrated the power of STEM diffraction (ACOM-STEM) providing additional crystallographic information, which can be analyzed to gain a deeper understanding of the LFP/FP interface properties such as statistical information on phase boundary orientation and misorientation between domains. Copyright © 2016 Elsevier B.V. All rights reserved.

Appendix B: Summary of TEM Particle Size Distribution Datasets

EPA Pesticide Factsheets

As discussed in the main text (see Section 5.3.2), calculation of the concentration of asbestos fibers in each of the bins of potential interest requires particle size distribution data derived using transmission electron microscopy (TEM).

Structural and morphological peculiarities of hybrid Au/nanodiamond engineered nanostructures

NASA Astrophysics Data System (ADS)

Matassa, Roberto; Orlanducci, Silvia; Reina, Giacomo; Cassani, Maria Cristina; Passeri, Daniele; Terranova, Maria Letizia; Rossi, Marco

2016-08-01

Nanostructured Au nano-platelets have been synthesized from an Au(III) complex by growth process triggered by nanodiamond (ND). An electroless synthetic route has been used to obtain 2D Au/ND architectures, where individual nanodiamond particles are intimately embedded into face-centered cubic Au platelets. The combined use of high resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), was able to reveal the unusual organization of these hybrid nanoparticles, ascertaining the existence of preferential crystallographic orientations for both nanocrystalline species and highlighting their mutual locations. Detailed information on the sample microstructure have been gathered by fast Fourier transform (FFT) and inverse fast Fourier transform (IFFT) of HR-TEM images, allowing us to figure out the role of Au defects, able to anchor ND crystallites and to provide specific sites for heteroepitaxial Au growth. Aggregates constituted by coupled ND and Au, represent interesting systems conjugating the best optoelectronics and plasmonics properties of the two different materials. In order to promote realistically the applications of such outstanding Au/ND materials, the cooperative mechanisms at the basis of material synthesis and their influence on the details of the hybrid nanostructures have to be deeply understood.

Structural and morphological peculiarities of hybrid Au/nanodiamond engineered nanostructures

PubMed Central

Matassa, Roberto; Orlanducci, Silvia; Reina, Giacomo; Cassani, Maria Cristina; Passeri, Daniele; Terranova, Maria Letizia; Rossi, Marco

2016-01-01

Nanostructured Au nano-platelets have been synthesized from an Au(III) complex by growth process triggered by nanodiamond (ND). An electroless synthetic route has been used to obtain 2D Au/ND architectures, where individual nanodiamond particles are intimately embedded into face-centered cubic Au platelets. The combined use of high resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), was able to reveal the unusual organization of these hybrid nanoparticles, ascertaining the existence of preferential crystallographic orientations for both nanocrystalline species and highlighting their mutual locations. Detailed information on the sample microstructure have been gathered by fast Fourier transform (FFT) and inverse fast Fourier transform (IFFT) of HR-TEM images, allowing us to figure out the role of Au defects, able to anchor ND crystallites and to provide specific sites for heteroepitaxial Au growth. Aggregates constituted by coupled ND and Au, represent interesting systems conjugating the best optoelectronics and plasmonics properties of the two different materials. In order to promote realistically the applications of such outstanding Au/ND materials, the cooperative mechanisms at the basis of material synthesis and their influence on the details of the hybrid nanostructures have to be deeply understood. PMID:27514638

A Study on Factors Affecting Strength of Solidified Peat through XRD and FESEM Analysis

NASA Astrophysics Data System (ADS)

Rahman, J. A.; Napia, A. M. A.; Nazri, M. A. A.; Mohamed, R. M. S. R.; Al-Geethi, A. S.

2018-04-01

Peat is soft soil that often causes multiple problems to construction. Peat has low shear strength and high deformation characteristics. Thus, peat soil needs to be stabilized or treated. Study on peat stabilization has been conducted for decades with various admixtures and mixing formulations. This project intends to provide an overview of the solidification of peat soil and the factors that affecting the strength of solidified peat soil. Three types of peats which are fabric, hemic and sapric were used in this study to understand the differences on the effect. The understanding of the factors affecting strength of solidified peat in this study is limited to XRD and FESEM analysis only. Peat samples were collected at Pontian, Johor and Parit Raja, Johor. Peat soil was solidified using fly ash, bottom ash and Portland cement with two mixing formulation following literature review. The solidified peat were cured for 7 days, 14 days, 28 days and 56 days. All samples were tested using Unconfined Compressive Strength Test (UCS), X-ray diffraction (XRD) and Field Emission Scanning Electron Microscope (FESEM). The compressive strength test of solidified peat had shown consistently increase of sheer strength, qu for Mixing 1 while decrease of its compressive strength value for Mixing 2. All samples were tested and compared for each curing days. Through XRD, it is found that all solidified peat are dominated with pargasite and richterite. The highest qu is Fabric Mixing 1(FM1) with the value of 105.94 kPa. This sample were proven contain pargasite. Samples with high qu were observed to be having fly ash and bottom ash bound together with the help of pargasite. Sample with decreasing strength showed less amount of pargasite in it. In can be concluded that XRD and FESEM findings are in line with UCS values.

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

NASA Astrophysics Data System (ADS)

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

2014-01-01

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

Quantitative energy-filtered TEM imaging of interfaces

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

Bentley, J.; Kenik, E.A.; Siangchaew, K.

Quantitative elemental mapping by inner shell core-loss energy-filtered transmission electron microscopy (TEM) with a Gatan Imaging Filter (GIF) interfaced to a Philips CM30 TEM operated with a LaB{sub 6} filament at 300 kV has been applied to interfaces in a range of materials. In sensitized type 304L stainless steel aged 15 h at 600{degrees}C, grain-boundary Cr depletion occurs between Cr-rich intergranular M{sub 23}C{sub 6} particles. Images of net Cr L{sub 23} intensity show segregation profiles that agree quantitatively with focused-probe spectrum-line measurements recorded with a Gatan PEELS on a Philips EM400T/FEG (0.8 nA in 2-nm-diam probe) of the same regions.more » Rare-earth oxide additives that are used for the liquid-phase sintering of Si{sub 3}N{sub 4} generate second phases of complex composition at grain boundaries and edges. These grain boundary phases often control corrosion, crack growth and creep damage behavior. High resolution imaging has been widely and with focused probes can be compromised by beam damage, but elemental mapping by EFTEM appears not to cause appreciable beam damage.« less

Prevalence of bla TEM-220 gene in Penicillinase-producing Neisseria gonorrhoeae strains carrying Toronto/Rio plasmid in Argentina, 2002 - 2011.

PubMed

Gianecini, Ricardo; Oviedo, Claudia; Guantay, Cristina; Piccoli, Laura; Stafforini, Graciela; Galarza, Patricia

2015-12-16

Penicillinase-producing Neisseria gonorroheae (PPNG) was first isolated in 1976. PPNG strains carrying bla TEM-1 and bla TEM-135 gene have been described in different countries. Recently, a novel bla TEM-220 allele was detected in PPNG isolates carrying Toronto/Rio plasmid. The prevalence and characteristics of TEM-220 strains worldwide are unknown, and therefore, it needs to be studied. The purpose of this study was to detect bla TEM-220 gene in PPNG strains possessing Toronto/Rio plasmid over a period of ten years in Argentina, and to evaluate the proportion of isolates producing non-TEM-220 containing the T539C substitution in the bla TEM allele. One hundred and fifty one PPNG isolates carrying Toronto/Rio plasmid were studied between 2002 and 2011. A mismatch amplification mutation assay (MAMA) PCR was used to identify the T539C substitution in the bla TEM allele and a MAMA-PCR protocol was developed to detect the G547A substitution in the bla TEM-220. The reference agar dilution method of the Clinical and Laboratory Standard Institute (CLSI) was used for susceptibility testing to five β-lactams antibiotics, ciprofloxacin, tetracycline and azithromycin. In all TEM-220-producing isolates, the whole bla TEM gene was sequenced and the isolates were typed using N. gonorroheae multiantigen sequence typing (NG-MAST). MAMA PCR successfully identified the G547A substitution in the bla TEM-220 allele. The proportion of isolates that possessed the bla TEM-220 allele was 2.6 %, and 93.2 % MAMA TEM-220 PCR-negative isolates showed the T539C substitution in the bla TEM gene. No differences in the susceptibility to five beta-lactam antibiotics tested were observed in PPNG isolates TEM-220-producing and PPNG isolates carrying the T539C substitution in the bla TEM gene. All TEM-220 isolates were indistinguishable by NG-MAST. This is the first study which shows the prevalence of bla TEM-220 in N. gonorrhoeae isolates carrying Toronto/Rio plasmid in Argentina. Although the bla

Distortion of DNA Origami on Graphene Imaged with Advanced TEM Techniques.

PubMed

Kabiri, Yoones; Ananth, Adithya N; van der Torre, Jaco; Katan, Allard; Hong, Jin-Yong; Malladi, Sairam; Kong, Jing; Zandbergen, Henny; Dekker, Cees

2017-08-01

While graphene may appear to be the ultimate support membrane for transmission electron microscopy (TEM) imaging of DNA nanostructures, very little is known if it poses an advantage over conventional carbon supports in terms of resolution and contrast. Microscopic investigations are carried out on DNA origami nanoplates that are supported onto freestanding graphene, using advanced TEM techniques, including a new dark-field technique that is recently developed in our lab. TEM images of stained and unstained DNA origami are presented with high contrast on both graphene and amorphous carbon membranes. On graphene, the images of the origami plates show severe unwanted distortions, where the rectangular shape of the nanoplates is significantly distorted. From a number of comparative control experiments, it is demonstrated that neither staining agents, nor screening ions, nor the level of electron-beam irradiation cause this distortion. Instead, it is suggested that origami nanoplates are distorted due to hydrophobic interaction of the DNA bases with graphene upon adsorption of the DNA origami nanoplates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ferric hydroxide supported gold subnano clusters or quantum dots: enhanced catalytic performance in chemoselective hydrogenation.

PubMed

Liu, Lequan; Qiao, Botao; Ma, Yubo; Zhang, Juan; Deng, Youquan

2008-05-21

An attempt to prepare ferric hydroxide supported Au subnano clusters via modified co-precipitation without any calcination was made. High resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) have been employed to study the structure and chemical states of these catalysts. No Au species could be observed in the HRTEM image nor from the XRD pattern, suggesting that the sizes of the Au species in and on the ferric hydroxide support were less than or around 1 nm. Chemoselective hydrogenation of aromatic nitro compounds and alpha,beta-unsaturated aldehydes was selected as a probe reaction to examine the catalytic properties of this catalyst. Under the same reaction conditions, such as 100 degrees C and 1 MPa H2 in the hydrogenation of aromatic nitro compounds, a 96-99% conversion (except for 4-nitrobenzonitrile) with 99% selectivity was obtained over the ferric hydroxide supported Au catalyst, and the TOF values were 2-6 times higher than that of the corresponding ferric oxide supported catalyst with 3-5 nm size Au particles. For further evaluation of this Au catalyst in the hydrogenation of citral and cinnamaldehyde, selectivity towards unsaturated alcohols was 2-20 times higher than that of the corresponding ferric oxide Au catalyst.

Isolation and characterisation of nanoparticles from tef and maize starch modified with stearic acid.

PubMed

Cuthbert, Wokadala O; Ray, Suprakas S; Emmambux, Naushad M

2017-07-15

Nanoparticles were isolated from tef and maize starch modified with added stearic acid after pasting at 90°C for 130min. This was followed by thermo-stable alpha-amylase hydrolysis of the paste. The resultant residues were then characterized using X-ray diffraction (XRD), differential scanning calorimetry (DSC), dynamic laser scattering particle size distribution (DLPSD), atomic force microscopy (AFM) and high-resolution transmission electron microscopy (HRTEM). XRD and DSC showed that the isolated residues consisted of amylose-lipid complexes. These complexes were type II with melting temperature above 104°C. DLPSD, AFM and HRTEM showed that the isolated tef and maize starch residues consisted of nanoparticles which became more distinct with increased hydrolysis time. The isolated tef and maize nanoparticles had distinct particles of about 3-10nm and 2.4-6.7nm, respectively and the yield was about 24-30%. The results demonstrated that distinct (physically separate) nanoparticles of less than 10nm can be isolated after formation during pasting of tef and maize starch with stearic acid. The production and isolation of the nanoparticles uses green chemistry principles and these nanoparticles can be used in food and non-food systems as nanofillers. Copyright © 2017 Elsevier Ltd. All rights reserved.

Revisiting the relevance of using a constant voltage step to improve electrochemical performances of Li-rich lamellar oxides

NASA Astrophysics Data System (ADS)

Pradon, A.; Caldes, M. T.; Petit, P.-E.; La Fontaine, C.; Elkaim, E.; Tessier, C.; Ouvrard, G.; Dumont, E.

2018-03-01

A Li-rich lamellar oxide was cycled at high potential and the relevance of using a constant voltage step (CVS) at the end of the charge, needed for industrial application, was investigated by electrochemical performance, X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). Electrochemical studies at 4.7 and 4.5 V with and without CVS showed that capacity and voltage fading occurred mostly when cells operated at high potential. After cycling, 3D-type defects involving transition metals trapped in lithium layer were observed by HRTEM into the electrode bulk. These defects are responsible for the voltage fading. XRD microstrain parameter was used to evaluate defects rate in aged materials subjected to a CVS, showing more 3D-type defects when cycled at 4.7 V than at 4.5 V. The time spent at high potential at the end of the charge as well as the value of the upper potential limit, are both relevant parameters to voltage decay. The use of a CVS at the end of the charge needs at the same time, a reduced upper potential window in order to minimize 3D-type defects occurrence. Unfortunately, this approach is still not sufficient to prevent voltage fading.

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

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

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

2013-11-13

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

Joint TEM and MT aquifer study in the Atacama Desert, North Chile

NASA Astrophysics Data System (ADS)

Ruthsatz, Alexander D.; Sarmiento Flores, Alvaro; Diaz, Daniel; Reinoso, Pablo Salazar; Herrera, Cristian; Brasse, Heinrich

2018-06-01

The Atacama Desert represents one of the driest regions on earth, and despite the absence of sustainable clean water reserves the demand has increased drastically since 1970 as a result of growing population and expanding mining activities. Magnetotelluric (MT) and Transient Electromagnetic (TEM) measurements were carried out for groundwater exploration in late 2015 in the area of the Profeta Basin at the western margin of the Chilean Precordillera. Both methods complement each other: While MT in general attains larger penetration depths, TEM allows better resolution of near surface layers; furthermore TEM is free from galvanic distortion. Data were collected along three profiles, enabling a continuous resistivity image from the surface to at least several hundred meters depth. TEM data were inverted in a 1-D manner, consistently yielding a poorly conductive near-surface layer with a thickness of approximately 30 m and below a well-conducting layer which we interpret as the aquifer with resistivities around 10 Ωm. At marginal sites of the main SW-NE-profile the resistive basement was found in 150 m. These depths are confirmed by interpretation of the MT soundings. Those were firstly inverted with a 2-D approach and then by 3-D inversion as clear indications of three-dimensionality exist. Several modeling runs were performed with different combinations of transfer functions and smoothing parameters. Generally, MT and TEM results agree reasonably well and an overall image of the resistivity structures in the Profeta Basin could be achieved. The aquifer reaches depths of more than 500 m in parts and, by applying Archie's law, resistivities of 1 Ωm can be assumed, indicating highly saline fluids from the source region of the surrounding high Andes under persisting arid conditions.

Investigating Processes of Materials Formation via Liquid Phase and Cryogenic TEM

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

De Yoreo, James J.; Sommerdijk, Nico

2016-06-14

The formation of materials in solutions is a widespread phenomenon in synthetic, biological and geochemical systems, occurring through dynamic processes of nucleation, self-assembly, crystal growth, and coarsening. The recent advent of liquid phase TEM and advances in cryogenic TEM are transforming our understanding of these phenomena by providing new insights into the underlying physical and chemical mechanisms. The techniques have been applied to metallic and semiconductor nanoparticles, geochemical and biological minerals, electrochemical systems, macromolecular complexes, and selfassembling systems, both organic and inorganic. New instrumentation and methodologies currently on the horizon promise new opportunities for advancing the science of materials synthesis.

Characterization of some biological specimens using TEM and SEM

NASA Astrophysics Data System (ADS)

Ghosh, Nabarun; Smith, Don W.

2009-05-01

The advent of novel techniques using the Transmission and Scanning Electron Microscopes improved observation on various biological specimens to characterize them. We studied some biological specimens using Transmission and Scanning Electron Microscopes. We followed negative staining technique with Phosphotungstic acid using bacterial culture of Bacillus subtilis. Negative staining is very convenient technique to view the structural morphology of different samples including bacteria, phage viruses and filaments in a cell. We could observe the bacterial cell wall and flagellum very well when trapped the negative stained biofilm from bacterial culture on a TEM grid. We cut ultra thin sections from the fixed root tips of Pisum sativum (Garden pea). Root tips were pre fixed with osmium tetroxide and post fixed with uranium acetate and placed in the BEEM capsule for block making. The ultrathin sections on the grid under TEM showed the granular chromatin in the nucleus. The protein bodies and large vacuoles with the storage materials were conspicuous. We followed fixation, critical point drying and sputter coating with gold to view the tissues with SEM after placing on stubs. SEM view of the leaf surface of a dangerous weed Tragia hispida showed the surface trichomes. These trichomes when break on touching releases poisonous content causing skin irritation. The cultured tissue from in vitro culture of Albizia lebbeck, a tree revealed the regenerative structures including leaf buds and stomata on the tissue surface. SEM and TEM allow investigating the minute details characteristic morphological features that can be used for classroom teaching.

Effect of particle size on the photochromic response of PWA/SiO2 nanocomposite

NASA Astrophysics Data System (ADS)

Huang, Feng-Hsi; Chen, Ching-Chung; Lin, Dar-Jong; Don, Trong-Ming; Cheng, Liao-Ping

2010-10-01

A series of photochromic phosphotungstic acid (PWA)/SiO2 composites were synthesized using the sol-gel method. Depending on the feeding schedule of PWA during synthesis, the size of the formed PWA/SiO2 particles varied considerably from as small as 1.2 nm to ca. 10 nm. With decreasing silica particle size, the total contact area/interaction between SiO2 and PWA increases, as revealed by FT-IR and solid-state 29Si-NMR analyses. Particularly, when the size of PWA/SiO2 is 1 nm, crystallization of PWA is inhibited, and PWA presents as amorphous molecular entities distributing uniformly in the SiO2 host, which is in evidence in the XRD spectroscopy and HR-TEM imaging. In contrast, substantial crystallization of PWA takes place when PWA/SiO2 particles are as large as 10 nm, in which case less amount of surface free Si-OH is available for PWA to make bonds with. Photochromism occurs activated by ultraviolet light irradiation. The rate of coloration/bleaching is found to depend strongly on the particle size of PWA/SiO2; specifically, the rate increases twice when the particle size is reduced from 10 nm to 1.2 nm.

Thermal stability, optical and Photoluminescence properties of spherical Ce x Zr1‑x O2 (x = 0.05) crystalline blue-emitting nanophosphors synthesized by microwave method

NASA Astrophysics Data System (ADS)

Manjunatha, S.; Dharmaprakash, M. S.

2018-03-01

Nanocrystalline ZrO2 based material is an impressive candidate for the various functional applications owing to their ease of preparation and high thermal stability. This paper reports the synthesis, structural and optical characterization of thermally stable monodispersed CexZr1‑xO2 (x = 0.05) nanoparticles. This method is based on the fact that, microwave irradiation allows the formation of size controlled and single phase cubic ZrO2 nanoparticles containing Ce+4 as a dopant. The XRD and Rietveld analysis revealed the formation of the crystalline cubic fluorite phase. The formation of nanoparticles was confirmed by FTIR. The morphology of the nanophosphors was characterised by FESEM and TEM. The optical band gap was calculated from the UV–visible absorption spectra and was found to vary from 3.93 to 4.25 eV with calcination temperature. It shows the decrease in the optical band gap from the pristine ZrO2. The particle size was measured by using HRTEM, and the average particle size was found to be 22 nm. Under the 268 nm Ultra Violet irradiation excitation a blue emission at 443 nm was observed at room temperature. The possible luminescence mechanism of CexZr1‑xO2 nanophosphor under UV excitation is discussed.

Silver nanoparticles synthesized with Rumex hymenosepalus extracts: effective broad-spectrum microbicidal agents and cytotoxicity study.

PubMed

Rodríguez-León, Ericka; Íñiguez-Palomares, Ramón A; Navarro, Rosa Elena; Rodríguez-Beas, César; Larios-Rodríguez, Eduardo; Alvarez-Cirerol, Francisco J; Íñiguez-Palomares, Claudia; Ramírez-Saldaña, Maricela; Hernández Martínez, Javier; Martínez-Higuera, Aarón; Galván-Moroyoqui, José Manuel; Martínez-Soto, Juan Manuel

2017-08-21

We synthesized silver nanoparticles using Rumex hymenosepalus root extract (Rh). Nanoparticles were subjected to a purification process and final product is a composite of Rh and silver nanoparticles (AgNPsC). Transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were used to perform a microstructure study. Additionally, two fractions (RhA and RhB) were obtained from the original extract by filtration with tetrahydrofuran (THF); both fractions were analyzed using UV-Vis spectroscopy, Fourier transform infrared spectroscopy (FT-IR), and 2,2-diphenyl-1-picrylhydrazyl (DPPH); total polyphenol content was also determined. Separate inhibition tests for AgNPsC and RhA and RhB were applied to Gram-positive bacteria, Gram-negative bacteria, and yeast (Candida albicans) using the well diffusion method. Extract fractions were found to have inhibitory effects only over Gram-positive bacteria, and silver nanoparticles showed inhibitory effects over all the evaluated microorganisms. Cytotoxicity was evaluated using the tetrazolium dye (MTT) assay in mononuclear peripheral blood cells. In addition, we assessment AgNPsC in THP-1 monocyte cell line, using the cell viability estimation by trypan blue dye exclusion test (TB) and Live/Dead (LD) cell viability assays by confocal microscopy.

Optimizing the synthesis conditions of silver nanoparticles using corn starch and their catalytic reduction of 4-nitrophenol

NASA Astrophysics Data System (ADS)

Salaheldin, Hosam I.

2018-06-01

In this study, silver nanoparticles (SNPs) were synthesised in an aqueous solution of corn starch. To fabricate the SNPs, reaction conditions, such as varying silver nitrate () concentration, time, temperature and solution pH of the reaction, were optimized. Since, the optimum reaction conditions were found 1 mmo l‑1, 15 min and , respectively. Then, to study the role of pH on SNP synthesis, varying pH values of the solution (3, 5, 7, 9 and 11) were investigated. Subsequently, the obtained silver/starch nanocomposites were characterised using different techniques. The x-ray diffraction (XRD) results revealed that the particles were face-centred cubic (FCC), and had an average particle size of 7.5 nm. This was confirmed by high-resolution transmission electron microscopy (HR-TEM) images. Moreover, the synthesised SNPs, at different pH values, were used as nanocatalyst for the reduction of 4-nitrophenol to 4-aminophenol in the presence of sodium borohydride. Under optimum reaction conditions, the higher catalytic activity was obtained with SNPs synthesised at pH 11 compared to lower pH of 7 or 9. Therefore, the rapid, reproducible, cost-effective silver/starch nanocomposite can be widely used for various applications such as drug manufacturing (e.g. analgesics and antipyretics) and the removal of pollutants from wastewater.

Enhanced magneto-optical and photo-catalytic properties of transition metal cobalt (Co2+ ions) doped spinel MgFe2O4 ferrite nanocomposites

NASA Astrophysics Data System (ADS)

Abraham, A. Godlyn; Manikandan, A.; Manikandan, E.; Vadivel, S.; Jaganathan, S. K.; Baykal, A.; Renganathan, P. Sri

2018-04-01

In this study, spinel magnesium cobalt ferrite (CoxMg1-xFe2O4: x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) nanocomposites were synthesized successfully by modified sol-gel combustion method. Magnesium nitrate, cobalt nitrate and iron nitrate were used as the source of divalent (Mg2+ and Co2+) and trivalent (Fe3+) cations, respectively and urea were used as the reducing (fuel) agent. The effects of cobalt ions on morphology, structural, optical, magnetic and photo-catalytic properties of spinel CoxMg1-xFe2O4 nanocomposites were investigated. Various characterization methods, including X-ray powder diffraction (XRD), high resolution scanning electron microscope (HR-SEM), transmission electron microscopy (HR-TEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transforms infrared (FT-IR) spectroscopy, vibrating sample magnetometer (VSM) and photo-catalytic degradation (PCD) activity were used to study the phase purity, microstructure, particle size, elemental composition, functional group determination, band gap calculation, magnetic properties and degradation efficiency of nanoparticles, respectively. The observed results showed that the final products consists cubic spinel phase with sphere-like nanoparticles morphologies. Furthermore, spinel Co0.6Mg0.4Fe2O4 nanocomposite showed highest PCD efficiency (98.55%) than other composition of ferrite nanoparticles.

Fabrication of Bi modified Bi2S3 pillared g-C3N4 photocatalyst and its efficient photocatalytic reduction and oxidation performances

NASA Astrophysics Data System (ADS)

Chen, Dongdong; Fang, Jianzhang; Lu, Shaoyou; Zhou, GuangYing; Feng, Weihua; Yang, Fan; Chen, Yi; Fang, ZhanQiang

2017-12-01

A novel efficient Bi modified Bi2S3 pillared g-C3N4 (BBC) plasmonic semiconductor photocatalyst has been successfully developed in a mixed solvothermal environment. The photocatalytic abilities of the as-prepared samples are examined by the photocatalytic reduction of Cr(VI) and oxidation of tetracycline (TC). And the chemical composition, structure, morphology and photo-absorption properties of the photocatalysts have been investigated by XRD, FT-IR, XPS, TEM, HRTEM and DRS methods, respectively. It is found that the addition of triethanolamine (TEA) results in the formation of the pillared-g-C3N4 (PG) nanostructure. The agglomeration of g-C3N4 nanosheets moiety and Bi2S3 nanorods moiety can be both hindered effectively by the special PG structure. And the photocatalytic results indicate that BBC exhibits the best photoreduction and photooxidation performances among all the samples, and meanwhile possesses superior photo-stability during the recycling runs. The enhanced photocatalytic activity of BBC could be ascribed to the furtherance of charge separation, localized surface plasma resonance (SPR) effect of metallic Bi and the excellent reaction interface. Finally, a tentative mechanism of BBC for photocatalytic reduction of Cr(VI) and oxidation of TC is discussed in detail.

Wavelength-Controlled Photodetector Based on Single CdSSe Nanobelt

NASA Astrophysics Data System (ADS)

Li, Xinmin; Tan, Qiuhong; Feng, Xiaobo; Wang, Qianjin; Liu, Yingkai

2018-06-01

CdSSe nanobelts (NBs) are synthesized by thermal evaporation and then characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), and cathodoluminescence (CL). It is found that the CdSSe NBs have a good morphology and microstructure without defects. CL is sensitive to the defects of CdSSe NBs; thus, we can select single nanobelt with homogeneous CL emission to prepare a detector. Based on it, the photodetector of single CdSSe NB was developed and its photoelectric properties were investigated in detail. It is found that under illumination of white light and at the bias voltage of 1 V, the photocurrent of a single CdSSe nanobelt device is 1.60 × 10-7 A, the dark current is 1.96 × 10-10 A, and the ratio of light current to dark one is 816. In addition, the CdSSe nanobelt detector has high photoelectric performance with spectral responsivity of 10.4 AW-1 and external quantum efficiency (EQE) of 19.1%. Its rise/decay time is about 1.62/4.70 ms. This work offers a novel strategy for design wavelength-controlled photodetectors by adjusting their compositions.

Coupled adsorption-photocatalytic degradation of crystal violet under sunlight using chemically synthesized grafted sodium alginate/ZnO/graphene oxide composite.

PubMed

Mohamed, S K; Hegazy, Sh H; Abdelwahab, N A; Ramadan, A M

2018-03-01

This research aimed to synthesize natural polymer nanocomposite and employ it for coupled adsorption- photocatalytic degradation of crystal violet. Sodium alginate-g-poly (acrylic acid-co-cinnamic acid) and its composites with ZnO nanorods and graphene oxide sheets were synthesized and characterized using FT-IR, XRD, SEM, HR-TEM and DR/UV-vis spectroscopy. The adsorption efficiency of samples for crystal violet has been studied in the dark. The effect of different parameters as pH, initial dye concentration, contact time and temperature on the adsorption efficiency of the synthesized sample has been examined. Kinetics studies showed that the adsorption of all samples was well described by the pseudo-second-order model and the equilibrium adsorption results fitted Freundlich model. The maximum adsorption capacity achieved at pH 5.0 was 13.85 mg g -1 . Thermodynamic studies exhibited that the adsorption is spontaneous, endothermic in nature and leads to higher entropy. Coupled adsorption-photocatalytic degradation studies under sunlight showed an enhancement in the removal efficiency by 10%. In the case of sodium alginate-g-poly (acrylic acid-co-cinnamic acid)/ZnO/graphene oxide composite, the removal efficiency after 5 h under sunlight was 94% versus 84% in the dark. Copyright © 2017 Elsevier B.V. All rights reserved.

Peculiar Li-storage mechanism at graphene edges in turbostratic carbon black and their application in high energy Li-ion capacitor

NASA Astrophysics Data System (ADS)

Anothumakkool, Bihag; Dupré, Nicolas; Moreau, Philippe; Guyomard, Dominique; Brousse, Thierry; Gaubicher, Joel

2018-02-01

We report experimental evidence for the specific Li-storage at turbostratic graphene edges of a well-known and cheap Super P® carbon black (Csp) material, which is usually used as a conductive additive in composite electrodes. Indeed, operando XRD and HR-TEM consistently demonstrate Li insertion occurs with zero expansion of graphene layer up to a composition of Li0.4C6 (150 mA h/g) that is reached at 0.01 V vs. Li+/Li. 7Li NMR substantiates these results and suggests that the weak electronic transfer from the carbon host to the intercalant could help local reorganization of the layer order as suggested by the unexpected reversible changes of the (002) Bragg peak intensity during the charge-discharge process. Our observations also indicate this insertion mechanism is kinetically favored resulting in remarkable cycling stability over 1000 cycles and power capability allowing to sustain 110 mA h/g at 8 A/g (21 C) in half cell. The capability of Csp as an efficient anode is ultimately demonstrated in a lithium hybrid capacitor against a positive electrode of activated carbon. The full cell delivers a maximum energy of 120 Wh/kg (4.3-2 V) and remarkable capacity retention over 1800 cycles.

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

Cingarapu, Sreeram; Yang, Zhiqiang; Sorensen, Christopher M.

We report synthesis of CdSe and CdTe quantum dots (QDs) from the bulk CdSe and CdTe material by evaporation/co-condensation using the solvated metal atom dispersion (SMAD) technique and refined digestive ripening. The outcomes of this new process are (1) the reduction of digestive ripening time by employing ligands (trioctylphosphine oxide (TOPO) and oleylamine (OA)) as capping agent as well as digestive ripening solvent, (2) ability to tune the photoluminescence (PL) from 410 nm to 670 nm, (3) demonstrate the ability of SMAD synthesis technique for other semiconductors (CdTe), (4) direct comparison of CdSe QDs growth with CdTe QDs growth based on digestivemore » ripening times, and (5) enhanced PL quantum yield (QY) of CdSe QDs and CdTe QDs upon covering with a ZnS shell. Further, the merit of this synthesis is the use of bulk CdSe and CdTe as the starting materials, which avoids usage of toxic organometallic compounds, eliminates the hot injection procedure, and size selective precipitation processes. It also allows the possibility of scale up. These QDs were characterized by UV-vis, photoluminescence (PL), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and powder XRD.« less

Synthesis of CdSe/ZnS and CdTe/ZnS Quantum Dots: Refined Digestive Ripening

DOE PAGES

Cingarapu, Sreeram; Yang, Zhiqiang; Sorensen, Christopher M.; ...

2012-01-01

We report synthesis of CdSe and CdTe quantum dots (QDs) from the bulk CdSe and CdTe material by evaporation/co-condensation using the solvated metal atom dispersion (SMAD) technique and refined digestive ripening. The outcomes of this new process are (1) the reduction of digestive ripening time by employing ligands (trioctylphosphine oxide (TOPO) and oleylamine (OA)) as capping agent as well as digestive ripening solvent, (2) ability to tune the photoluminescence (PL) from 410 nm to 670 nm, (3) demonstrate the ability of SMAD synthesis technique for other semiconductors (CdTe), (4) direct comparison of CdSe QDs growth with CdTe QDs growth based on digestivemore » ripening times, and (5) enhanced PL quantum yield (QY) of CdSe QDs and CdTe QDs upon covering with a ZnS shell. Further, the merit of this synthesis is the use of bulk CdSe and CdTe as the starting materials, which avoids usage of toxic organometallic compounds, eliminates the hot injection procedure, and size selective precipitation processes. It also allows the possibility of scale up. These QDs were characterized by UV-vis, photoluminescence (PL), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and powder XRD.« less

Carbon-coated copper nanoparticles prepared by detonation method and their thermocatalysis on ammonium perchlorate

NASA Astrophysics Data System (ADS)

An, Chongwei; Ding, Penghui; Ye, Baoyun; Geng, Xiaoheng; Wang, Jingyu

2017-03-01

Carbon-coated copper nanoparticles (CCNPs) were prepared by initiating a high-density charge pressed with a mixture of microcrystalline wax, hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), and copper nitrate hydrate (Cu(NO3)2.3H2O) in an explosion vessel filled with nitrogen gas. The detonation products were characterized by transmission electron microcopy (TEM), high resolution transmission electron microcopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and Raman spectroscopy. The effects of CCNPs on thermal decomposition of ammonium perchlorate (AP) were also investigated by differential scanning calorimeter (DSC). Results indicated that the detonation products were spherical, 25-40 nm in size, and had an apparent core-shell structure. In this structure, the carbon shell was 3-5 nm thick and mainly composed of graphite, C8 (a kind of carbyne), and amorphous carbon. When 5 wt.% CCNPs was mixed with 95 wt.% AP, the high-temperature decomposition peak of AP decreased by 95.97, 96.99, and 96.69 °Cat heating rates of 5, 10, and 20 °C/min, respectively. Moreover, CCNPs decreased the activation energy of AP as calculated through Kissinger's method by 25%, which indicated outstanding catalysis for the thermal decomposition of AP.

Manipulation of partially oriented hydroxyapatite building blocks to form flowerlike bundles without acid-base regulation.

PubMed

Wen, Zhenliang; Wang, Zihao; Chen, Jingdi; Zhong, Shengnan; Hu, Yimin; Wang, Jianhua; Zhang, Qiqing

2016-06-01

The application of hydroxyapatite (HAP) in different fields depends greatly on its morphology, composition and structure. Besides, the main inorganic building blocks of human bones and teeth are also HAP. Therefore, accurate shape and aggregation control and of hydroxyapatite particles will be of great interest. Herein, oriented bundles of flowerlike HAP nanorods were successfully prepared through hydrothermal treatment without acid-base regulation, with the mono-alkyl phosphate (MAP) and sodium citrate as surfactant and chelating agent, respectively. The prepared samples were characterized by the X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and zeta potential, the pH value and conductivity value of suspension were characterized by pH meter and conductivity measurement. The results showed that the MAP and citrate play an important role in assembly of HAP nanorods without acid-base regulation. Citrate calcium complex could decompose slowly and release citrate ions at hydrothermal conditions. Besides, the further decomposition of citrate ions could release aconitic acid as the reaction time prolongs. Moreover, the possible scheme for the formation process was discussed in detail. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis of inorganic fullerene-like WS2 nanoparticles and their lubricating performance

NASA Astrophysics Data System (ADS)

Yang, Haibin; Liu, Shikai; Li, Jixue; Li, Minghui; Peng, Gang; Zou, Guangtian

2006-03-01

A facile, large-scale and low-cost route was used to synthesize inorganic fullerene-like (IF) WS2 nanoparticles by the reaction of sulfur powder (S) and as-prepared WO3 nanoparticles in a hydrogen atmosphere at a heating temperature of 500-650 °C. The as-synthesized IF-WS2 nanoparticles are of a closed hollow cage structure with an average size of about 50 nm. The composition, morphology and structure of the products were characterized by XRD, TEM, FE-SEM, and HRTEM. The influences of the main reaction conditions were investigated and the possible growth mechanism are proposed. It is worth noting that through changing the amount of as-prepared composite powder (WO3 and S) and the content of hydrogen, yields of IF-WS2 in larger scales can accordingly be easily obtained, and such a synthetic route may also be used in the synthesis of other transition IF metal dichalcogenides. Furthermore, tribological experiments emphasized the important role played by these as-synthesized IF-WS2 nanoparticles in providing excellent lubricating performance, which may bring a much brighter future for their applications in the lubricating field, or even arouse great interest of both scientists and industrialists for their many other important applications.

Deposition of silver nanoparticles on multiwalled carbon nanotubes by chemical reduction process and their antimicrobial effects

NASA Astrophysics Data System (ADS)

Haider, Adawiya J.; Thamir, Amin D.; Ahmed, Duha S.; Mohammad, M. R.

2016-07-01

In this paper, the functionalization of raw-MWCNTs involves oxidation reaction using concentrated acid mixture of HNO3:H2SO4 (1:3), via ultrasonic bath (170 W, 50 kHz) to obtain functional groups. Then Ag nanoparticles are decorated the outside over the surface of functionalized MWCNTs using a chemical reduction process resulting in the formation of(Ag/ MWCNTs) hybrid material. The results showed that outer diameter functionalized F-MWCNTs andAg nanoparticles size was about (11-80) nm and (10 to 25) nm, respectively using TEM and HRTEM. The crystallographic structure of MWCNTs using X-ray diffraction (XRD) analysis proved diffraction peaks at 38.1°, 44.3°, 64.7° and 77.4° degrees namely, Ag (111), Ag (200), Ag (220), and Ag (311) of the face-centered cubic lattice of Ag, respectively, excepting the peak at 2θ =25.6°, which correspond to the (0 0 2) reflection of the MWNTs are corresponding to Ag/MWNTs. The antimicrobial activities of Ag/MWCNTs hybrid using plate count method showed that decreasing a large number of bacteria colonies of E. coli and S. aureu with increasing the hybrid concentrations after incubation for 24h in shaker incubator with percentage of inhibition approaching 100%.

Bird's nest-like nanographene shell encapsulated Si nanoparticles - Their structural and Li anode properties

NASA Astrophysics Data System (ADS)

Li, Beibei; Jiang, Yizhe; Jiang, Fan; Cao, Daxian; Wang, Hongkang; Niu, Chunming

2017-02-01

Bird's nest-like nanographene shell (NGS) encapsulated Si@SiO2 nanoparticles have been prepared by a simple chemical vapor deposition (CVD) method. The shell is comprised of a conformed coating with 4-10 layers of the nanographene, and nanographene spikes with the same thickness grown on the coating surface. The high crystallinity of the shell is demonstrated by XRD, HRTEM and Raman characterization. After SiO2 has been removed, distinctive void space is created between Si core and nested NGS. Statistical estimation from TEM images of 50 Si@void@NGS particles shows that the volume of void space is about 2.82 times of that of Si nanoparticle, sufficient to accommodate volume change from Si to Li15Si4. Evaluation of Si@void@NGS for Li ion anode reveals a specific capacity of 2634 mAh g-1 at a current density of 0.2 A g-1, and an excellent rate and cycling performance. The capacity decreases by 5.2%-2497 mAh g-1 after cycling at current densities of 0.5, 1, 2, 5 10, 20 A g-1. The excellent performance can be attributed to high conductivity and high stability of the shell, which remains intact after repeated cycling.

Synthesis of mesoporous Mn/TiO2 nanocomposites and investigating the photocatalytic properties in aqueous systems.

PubMed

Oseghe, Ekemena Oghenovoh; Ndungu, Patrick Gathura; Jonnalagadda, Sreekanth Babu

2015-01-01

Mesoporous 20 wt% Mn/TiO2 nanocomposites were synthesized adopting modified sol-gel method at different pH (pH = 2, 7 and 11) conditions and calcined at 400 °C. Based on the characteristics of the 20 wt% Mn/TiO2 nanocomposites synthesized at pH 11, same procedure was adopted for the synthesis of different wt% Mn/TiO2. The nanocomposite samples and their surface properties were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), mapping, inductively coupled plasma optical emission spectrometry (ICP-OES), Fourier transform infrared (FTIR), and fluorescence spectrometry. The nanocomposites existed in the anatase phase of TiO2 with no peak assigned to Mn on the diffractogram. The photocatalytic activities of the materials were evaluated by monitoring degradation of a model dye (methylene blue (MB)) in presence of visible light and ozone. The nanocomposite synthesized under neutral condition (pH = 7) exhibited the best photocatalytic activity resulting from its relatively smaller crystal size (5.98 nm) and larger pore volume (0.30 cm(3)/g). One percentage of weight Mn/TiO2 showed 100% decolouration of MB in the presence of O3 after 100 min.

Polyimide encapsulated lithium-rich cathode material for high voltage lithium-ion battery.

PubMed

Zhang, Jie; Lu, Qingwen; Fang, Jianhua; Wang, Jiulin; Yang, Jun; NuLi, Yanna

2014-10-22

Lithium-rich materials represented by xLi2MnO3·(1 - x)LiMO2 (M = Mn, Co, Ni) are attractive cathode materials for lithium-ion battery due to their high specific energy and low cost. However, some drawbacks of these materials such as poor cycle and rate capability remain to be addressed before applications. In this study, a thin polyimide (PI) layer is coated on the surface of Li1.2Ni0.13Mn0.54Co0.13O2 (LNMCO) by a polyamic acid (PAA) precursor with subsequently thermal imidization process. X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HR-TEM) results confirm the successful formation of a PI layer (∼3 nm) on the surface of LNMCO without destruction of its main structure. X-ray photoelectron spectroscopy (XPS) spectra show a slight shift of the Mn valence state from Mn(IV) to Mn(III) in the PI-LNMCO treated at 450 °C, elucidating that charge transfer takes place between the PI layer and LNMCO surface. Electrochemical performances of LNMCO including cyclic stability and rate capability are evidently improved by coating a PI nanolayer, which effectively separates the cathode material from the electrolyte and stabilizes their interface at high voltage.

Preparation of NiS/ZnIn2S4 as a superior photocatalyst for hydrogen evolution under visible light irradiation

PubMed Central

Wei, Liang; Chen, Yongjuan; Zhao, Jialin

2013-01-01

Summary In this study, NiS/ZnIn2S4 nanocomposites were successfully prepared via a facile two-step hydrothermal process. The as-prepared samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). Their photocatalytic performance for hydrogen evolution under visible light irradiation was also investigated. It was found that the photocatalytic hydrogen evolution activity over hexagonal ZnIn2S4 can be significantly increased by loading NiS as a co-catalyst. The formation of a good junction between ZnIn2S4 and NiS via the two step hydrothermal processes is beneficial for the directional migration of the photo-excited electrons from ZnIn2S4 to NiS. The highest photocatalytic hydrogen evolution rate (104.7 μmol/h), which is even higher than that over Pt/ZnIn2S4 nanocomposite (77.8 μmol/h), was observed over an optimum NiS loading amount of 0.5 wt %. This work demonstrates a high potential of the developing of environmental friendly, cheap noble-metal-free co-catalyst for semiconductor-based photocatalytic hydrogen evolution. PMID:24455453

Synthesis and characterization of nano-sized zirconia powder synthesized by single emulsion-assisted direct precipitation.

PubMed

Chandra, Navin; Singh, Deepesh Kumar; Sharma, Meenakshi; Upadhyay, Ravi Kant; Amritphale, S S; Sanghi, S K

2010-02-15

For the first time, single reverse microemulsion-assisted direct precipitation route has been successfully used to synthesize tetragonal zirconia nanoparticles in narrow size range. The synthesized powder was characterized using FT-IR, XRD and HRTEM techniques. The zirconia nanoparticles obtained were spherical in shape and has narrow particle size distribution in the range of 13-31nm and crystallite size in the range of 13-23nm. Copyright 2009 Elsevier Inc. All rights reserved.

Atom-counting in High Resolution Electron Microscopy:TEM or STEM - That's the question.

PubMed

Gonnissen, J; De Backer, A; den Dekker, A J; Sijbers, J; Van Aert, S

2017-03-01

In this work, a recently developed quantitative approach based on the principles of detection theory is used in order to determine the possibilities and limitations of High Resolution Scanning Transmission Electron Microscopy (HR STEM) and HR TEM for atom-counting. So far, HR STEM has been shown to be an appropriate imaging mode to count the number of atoms in a projected atomic column. Recently, it has been demonstrated that HR TEM, when using negative spherical aberration imaging, is suitable for atom-counting as well. The capabilities of both imaging techniques are investigated and compared using the probability of error as a criterion. It is shown that for the same incoming electron dose, HR STEM outperforms HR TEM under common practice standards, i.e. when the decision is based on the probability function of the peak intensities in HR TEM and of the scattering cross-sections in HR STEM. If the atom-counting decision is based on the joint probability function of the image pixel values, the dependence of all image pixel intensities as a function of thickness should be known accurately. Under this assumption, the probability of error may decrease significantly for atom-counting in HR TEM and may, in theory, become lower as compared to HR STEM under the predicted optimal experimental settings. However, the commonly used standard for atom-counting in HR STEM leads to a high performance and has been shown to work in practice. Copyright © 2017 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Dharmadhikari, Dipti V.; Athawale, Anjali A.

2013-06-01

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

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

NASA Technical Reports Server (NTRS)

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

2015-01-01

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

Ceftazidime-Resistant Enterobacteriaceae Isolates from Three Polish Hospitals: Identification of Three Novel TEM- and SHV-5-Type Extended-Spectrum β-Lactamases

PubMed Central

Gniadkowski, Marek; Schneider, Ines; Jungwirth, Renate; Hryniewicz, Waleria; Bauernfeind, Adolf

1998-01-01

Twelve ceftazidime-resistant isolates of the family Enterobacteriaceae (11 Klebsiella pneumoniae isolates and 1 Escherichia coli isolate) were collected in 1995 from three Polish hospitals located in different cities. All were identified as producers of extended-spectrum β-lactamases (ESBLs). Detailed analysis of their β-lactamase contents revealed that six of them expressed SHV-5-like ESBLs. The remaining six were found to produce three different TEM enzymes, each characterized by a pI value of 6.0 and specified by new combinations of amino acid substitutions. The amino acid substitutions compared to the TEM-1 β-lactamase sequence were Gly238Ser, Glu240Lys, and Thr265Met for TEM-47; Leu21Phe, Gly238Ser, Glu240Lys, and Thr265Met for TEM-48; and Leu21Phe, Gly238Ser, Glu240Lys, Thr265Met, and Ser268Gly for TEM-49. The new TEM β-lactamases, TEM-47, TEM-48, and TEM-49, belong to a subfamily of TEM-2-related enzymes. Genes coding for TEM-47 and TEM-49 could have originated from the TEM-48-encoding sequence by various single genetic events. The new TEM derivatives probably document the already advanced microevolution of ESBLs ongoing in Polish hospitals, in a majority of which no monitoring of ESBL producers was performed before 1996. PMID:9517925

Mineralogical composition of the meteorite El Pozo (Mexico): a Raman, infrared and XRD study.

PubMed

Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

2011-12-01

The Raman (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of El Pozo meteorite (an ordinary chondrite L5 type; village Valle of Allende, founded in State of Chihuahua, Mexico: 26°56'N and 105°24'W, 1998). RMP measurements in the range of 100-3500 cm(-1) revealed principal characteristic bands of the major minerals: olivine, two polymorph modifications of pyroxene (OPx and CPx) and plagioclase. Some bands of the minor minerals (hematite and goethite) were also identified. All these minerals were clearly distinguished using IR and XRD techniques. XRD technique has shown the presence of some metallic phases such as kamacite and taenite as well as troilite and chromite. These minerals do not have characteristic Raman spectra because Fe-Ni metals have no active modes for Raman spectroscopy and troilite is a weak Raman scatterer. Raman mapping microspectroscopy was a key part in the investigation of El Pozo meteorite's spatial distribution of the main minerals because these samples are structurally and chemically complex and heterogeneous. The mineral mapping by Raman spectroscopy has provided information for a certain spatial region on which a spatial distribution coexists of the three typical mineral assemblages: olivine; olivine+orthopyroxene; and orthopyroxene. Copyright © 2011 Elsevier B.V. All rights reserved.

Processing grounded-wire TEM signal in time-frequency-pseudo-seismic domain: A new paradigm

NASA Astrophysics Data System (ADS)

Khan, M. Y.; Xue, G. Q.; Chen, W.; Huasen, Z.

2017-12-01

Grounded-wire TEM has received great attention in mineral, hydrocarbon and hydrogeological investigations for the last several years. Conventionally, TEM soundings have been presented as apparent resistivity curves as function of time. With development of sophisticated computational algorithms, it became possible to extract more realistic geoelectric information by applying inversion programs to 1-D & 3-D problems. Here, we analyze grounded-wire TEM data by carrying out analysis in time, frequency and pseudo-seismic domain supported by borehole information. At first, H, K, A & Q type geoelectric models are processed using a proven inversion program (1-D Occam inversion). Second, time-to-frequency transformation is conducted from TEM ρa(t) curves to magneto telluric MT ρa(f) curves for the same models based on all-time apparent resistivity curves. Third, 1-D Bostick's algorithm was applied to the transformed resistivity. Finally, EM diffusion field is transformed into propagating wave field obeying the standard wave equation using wavelet transformation technique and constructed pseudo-seismic section. The transformed seismic-like wave indicates that some reflection and refraction phenomena appear when the EM wave field interacts with geoelectric interface at different depth intervals due to contrast in resistivity. The resolution of the transformed TEM data is significantly improved in comparison to apparent resistivity plots. A case study illustrates the successful hydrogeophysical application of proposed approach in recovering water-filled mined-out area in a coal field located in Ye county, Henan province, China. The results support the introduction of pseudo-seismic imaging technology in short-offset version of TEM which can also be an useful aid if integrated with seismic reflection technique to explore possibilities for high resolution EM imaging in future.

XRD and SEM study of alumina silicate porcelain insulator

NASA Astrophysics Data System (ADS)

Duddi, Dharmender; Singh, G. P.; Kalra, Swati; Shekhawat, M. S.; Tak, S. K.

2018-05-01

Higher strength electrical porcelain is a requirement of industry. This will be achieved by a specific composition of raw materials, which is consisted of clays and feldspars. Water absorption, particle size and insulating properties are of special interest now a day. China clay, Ball clay and Quartz are widely used by ceramic industries in Bikaner district of Rajasthan. Sample for present study were prepared by mixing of above clay, feldspar with MnO2, then shrinkage is observed. Bar shaped samples were prepared and heated up to a temperature of about 1185° C to observe shrinkage. For phase study of XRD and SEM are observed.

An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

NASA Technical Reports Server (NTRS)

Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

1993-01-01

By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

Ambient synthesis, characterization, and electrochemical activity of LiFePO₄ nanomaterials derived from iron phosphate intermediates

DOE PAGES

Patete, Jonathan M.; Wong, Stanislaus S.; Scofield, Megan E.; ...

2015-05-30

LiFePO₄ materials have become increasingly popular as a cathode material due to the many benefits they possess including thermal stability, durability, low cost, and long life span. Nevertheless, to broaden the general appeal of this material for practical electrochemical applications, it would be useful to develop a relatively mild, reasonably simple synthesis method of this cathode material. Herein, we describe a generalizable, 2-step methodology of sustainably synthesizing LiFePO₄ by incorporating a template-based, ambient, surfactantless, seedless, U-tube protocol in order to generate size and morphologically tailored, crystalline, phase-pure nanowires. The purity, composition, crystallinity, and intrinsic quality of these wires were systematicallymore » assessed using transmission electron microscopy TEM, HRTEM, SEM, XRD, SAED, EDAX and high-resolution synchrotron XRD. From these techniques, we were able to determine that there is an absence of defects present in our wires, supporting the viability of our synthetic approach. Electrochemical analysis was also employed to assess their electrochemical activity. Although our nanowires do not contain any noticeable impurities, we attribute their less than optimal electrochemical rigor to differences in the chemical bonding between our LiFePO₄ nanowires and their bulk-like counterparts. Specifically, we demonstrate for the first time experimentally that the Fe-O3 chemical bond plays an important role in determining the overall conductivity of the material, an assertion which is further supported by recent first principles calculations. Nonetheless, our ambient, solution-based synthesis technique is capable of generating highly crystalline and phase-pure energy-storage-relevant nanowires that can be tailored so as to fabricate different sized materials of reproducible, reliable morphology.« less

Rapid Extracellular Biosynthesis of Silver Nanoparticles by Cunninghamella phaeospora Culture Supernatant

PubMed Central

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

2016-01-01

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

Response to the comment by C. Kisielowski, H.A. Calderon, F.R. Chen, S. Helveg, J.R. Jinschek, P. Specht, D. Van Dyck on the article "On the influence of the electron dose-rate on the HRTEM image contrast" by J. Barthel, M. Lentzen, A. Thust, Ultramicroscopy 176 (2017) 37-45.

PubMed

Barthel, Juri; Lentzen, Markus; Thust, Andreas

2017-08-01

In a recent article [1] we examined the influence of the applied electron dose rate on the magnitude of the image contrast in high-resolution transmission electron microscopy (HRTEM). We concluded that the magnitude of the image contrast is not substantially affected by the applied electron dose rate. This result is in obvious contradiction to numerous earlier publications by Kisielowski and coworkers [2-7], who commented our recent article due to this contradiction. The present short communication is a response to the comment of Kisielowski and coworkers on our recent article, where we provide additional arguments supporting our initial findings and conclusions on the magnitude of the image contrast in HRTEM. Copyright © 2017 Elsevier B.V. All rights reserved.

Coordinated Isotopic and TEM Studies of Presolar Graphites from Murchison

NASA Astrophysics Data System (ADS)

Croat, T. K.; Stadermann, F. J.; Zinner, E.; Bernatowicz, T. J.

2004-03-01

TEM and NanoSIMS investigations of the same presolar Murchison KFC graphites revealed high Zr, Mo, and Ru content in refractory carbides within the graphites. Along with isotopically light carbon, these suggest a low-metallicity AGB source.

Helicopter TEM parameters analysis and system optimization based on time constant

NASA Astrophysics Data System (ADS)

Xiao, Pan; Wu, Xin; Shi, Zongyang; Li, Jutao; Liu, Lihua; Fang, Guangyou

2018-03-01

Helicopter transient electromagnetic (TEM) method is a kind of common geophysical prospecting method, widely used in mineral detection, underground water exploration and environment investigation. In order to develop an efficient helicopter TEM system, it is necessary to analyze and optimize the system parameters. In this paper, a simple and quantitative method is proposed to analyze the system parameters, such as waveform, power, base frequency, measured field and sampling time. A wire loop model is used to define a comprehensive 'time constant domain' that shows a range of time constant, analogous to a range of conductance, after which the characteristics of the system parameters in this domain is obtained. It is found that the distortion caused by the transmitting base frequency is less than 5% when the ratio of the transmitting period to the target time constant is greater than 6. When the sampling time window is less than the target time constant, the distortion caused by the sampling time window is less than 5%. According to this method, a helicopter TEM system, called CASHTEM, is designed, and flight test has been carried out in the known mining area. The test results show that the system has good detection performance, verifying the effectiveness of the method.

Quantitative strain and compositional studies of InxGa1-xAs Epilayer in a GaAs-based pHEMT device structure by TEM techniques.

PubMed

Sridhara Rao, Duggi V; Sankarasubramanian, Ramachandran; Muraleedharan, Kuttanellore; Mehrtens, Thorsten; Rosenauer, Andreas; Banerjee, Dipankar

2014-08-01

In GaAs-based pseudomorphic high-electron mobility transistor device structures, strain and composition of the In x Ga1-x As channel layer are very important as they influence the electronic properties of these devices. In this context, transmission electron microscopy techniques such as (002) dark-field imaging, high-resolution transmission electron microscopy (HRTEM) imaging, scanning transmission electron microscopy-high angle annular dark field (STEM-HAADF) imaging and selected area diffraction, are useful. A quantitative comparative study using these techniques is relevant for assessing the merits and limitations of the respective techniques. In this article, we have investigated strain and composition of the In x Ga1-x As layer with the mentioned techniques and compared the results. The HRTEM images were investigated with strain state analysis. The indium content in this layer was quantified by HAADF imaging and correlated with STEM simulations. The studies showed that the In x Ga1-x As channel layer was pseudomorphically grown leading to tetragonal strain along the [001] growth direction and that the average indium content (x) in the epilayer is ~0.12. We found consistency in the results obtained using various methods of analysis.

TEM measurement in a low resistivity overburden performed by using low temperature SQUID

NASA Astrophysics Data System (ADS)

Ji, Yanju; Du, Shangyu; Xie, Lijun; Chang, Kai; Liu, Yang; Zhang, Yi; Xie, Xiaoming; Wang, Yuan; Lin, Jun; Rong, Liangliang

2016-12-01

Exploration of areas with thick low resistivity overburden is still a challenge for time domain transient electromagnetic method (TEM). We report modeling of a sandwich-layered earth by simulating the B field response with different conductive target layer thicknesses, thus obtaining a relationship between the resolution of the B field and the exploration depth. A low temperature Superconducting Quantum Interference Device (SQUID) is an ideal sensor for measuring the secondary magnetic field B in TEM measurements, because its sensitivity of several fT/√Hz is independent of frequency. In our TEM experiments, we utilized two different coils as receivers, a simple SQUID system, and a large transmitter loop of 200 × 200 m2 to compare the detected decay curves. At some measurement points, a decay signal of more than 300 ms duration was obtained by using the SQUID. Apparent resistivity profiles of about 9 km length are presented.

Strain mapping in TEM using precession electron diffraction

DOEpatents

Taheri, Mitra Lenore; Leff, Asher Calvin

2017-02-14

A sample material is scanned with a transmission electron microscope (TEM) over multiple steps having a predetermined size at a predetermined angle. Each scan at a predetermined step and angle is compared to a template, wherein the template is generated from parameters of the material and the scanning. The data is then analyzed using local mis-orientation mapping and/or Nye's tensor analysis to provide information about local strain states.

Preparation and catalytic activities for H{sub 2}O{sub 2} decomposition of Rh/Au bimetallic nanoparticles

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

Zhang, Haijun, E-mail: zhanghaijun@wust.edu.cn; The State Key Laboratory of Refractory and Metallurgy, Wuhan University of Science and Technology, Wuhan 430081; Deng, Xiangong

2016-07-15

Graphical abstract: PVP-protected Rh/Au bimetallic nanoparticles (BNPs) were prepared by using hydrogen sacrificial reduction method, the activity of Rh80Au20 BNPs were about 3.6 times higher than that of Rh NPs. - Highlights: • Rh/Au bimetallic nanoparticles (BNPs) of 3∼5 nm in diameter were prepared. • Activity for H{sub 2}O{sub 2} decomposition of BNPs is 3.6 times higher than that of Rh NPs. • The high activity of BNPs was caused by the existence of charged Rh atoms. • The apparent activation energy for H{sub 2}O{sub 2} decomposition over the BNPs was calculated. - Abstract: PVP-protected Rh/Au bimetallic nanoparticles (BNPs) weremore » prepared by using hydrogen sacrificial reduction method and characterized by UV–vis, XRD, FT-IR, XPS, TEM, HR-TEM and DF-STEM, the effects of composition on their particle sizes and catalytic activities for H{sub 2}O{sub 2} decomposition were also studied. The as-prepared Rh/Au BNPs possessed a high catalytic activity for the H{sub 2}O{sub 2} decomposition, and the activity of the Rh{sub 80}Au{sub 20} BNPs with average size of 2.7 nm were about 3.6 times higher than that of Rh monometallic nanoparticles (MNPs) even the Rh MNPs possess a smaller particle size of 1.7 nm. In contrast, Au MNPs with size of 2.7 nm show no any activity. Density functional theory (DFT) calculation as well as XPS results showed that charged Rh and Au atoms formed via electronic charge transfer effects could be responsible for the high catalytic activity of the BNPs.« less

Facile synthesis of GO@SnO2/TiO2 nanofibers and their behavior in photovoltaics.

PubMed

Mohamed, Ibrahim M A; Dao, Van-Duong; Yasin, Ahmed S; Choi, Ho-Suk; Khalil, KhalilAbdelrazek; Barakat, Nasser A M

2017-03-15

Chemical doping is a widely-used strategy to improve the performance of TiO 2 for the dye-sensitized solar cells (DSCs). However, the effect of two efficient dopants has been rarely investigated. We present the synthesis of GO@SnO 2 /TiO 2 nanofibers (NFs) by a facile method using electrospinning and hydrothermal processes. The synthesized NFs are described in terms of morphology, crystallinity and chemistry through FESEM, TEM, HR-TEM, XRD, EDX, XPS, FT-IR and Raman spectra. As the results, the axial ratio and the average diameter of NFs decreased after the hydrothermal treatment and calcination process, respectively. The prepared Titania-based nanofibers have 81.82% anatase and 18.18% rutile-structure. The developed materials are applied as working electrodes of DSCs. The photovoltaic performances showed that the efficiency of the device employed GO@SnO 2 /TiO 2 photoanode gave 5.41%, which was higher than those of cells fabricated with SnO 2 /TiO 2 NFs (3.41%) and GO@TiO 2 NFs (4.52%) photoanodes. The photovoltaic parameters such as J sc , V oc , FF and R ct are calculated and found to be 11.19mAcm -2 , 0.72V, 0.67 and 9.26Ω, respectively. The high photovoltaic response of DSC based of GO@SnO 2 /TiO 2 NFs may be attributed to the large surface area of the NFs, and the low electron recombination. Furthermore, the start-stop switches of the cell devices with the developed photoanode affirmed the stability and photovoltaic performance of the cell. Copyright © 2016 Elsevier Inc. All rights reserved.

Green synthesis and characterization of Au@Pt core-shell bimetallic nanoparticles using gallic acid

NASA Astrophysics Data System (ADS)

Zhang, Guojun; Zheng, Hongmei; Shen, Ming; Wang, Lei; Wang, Xiaosan

2015-06-01

In this study, we developed a facile and benign green synthesis approach for the successful fabrication of well-dispersed urchin-like Au@Pt core-shell nanoparticles (NPs) using gallic acid (GA) as both a reducing and protecting agent. The proposed one-step synthesis exploits the differences in the reduction potentials of AuCl4- and PtCl62-, where the AuCl4- ions are preferentially reduced to Au cores and the PtCl62- ions are then deposited continuously onto the Au core surface as a Pt shell. The as-prepared Au@Pt NPs were characterized by transmission electron microscope (TEM); high-resolution transmission electron microscope (HR-TEM); scanning electron microscope (SEM); UV-vis absorption spectra (UV-vis); X-ray diffraction (XRD); Fourier transmission infrared spectra (FT-IR). We systematically investigated the effects of some experimental parameters on the formation of the Au@Pt NPs, i.e., the reaction temperature, the molar ratios of HAuCl4/H2PtCl6, and the amount of GA. When polyvinylpyrrolidone K-30 (PVP) was used as a protecting agent, the Au@Pt core-shell NPs obtained using this green synthesis method were better dispersed and smaller in size. The as-prepared Au@Pt NPs exhibited better catalytic activity in the reaction where NaBH4 reduced p-nitrophenol to p-aminophenol. However, the results showed that the Au@Pt bimetallic NPs had a lower catalytic activity than the pure Au NPs obtained by the same method, which confirmed the formation of Au@Pt core-shell nanostructures because the active sites on the surfaces of the Au NPs were covered with a Pt shell.

Mössbauer and XRD study of novel quaternary Sn-Fe-Co-Ni electroplated alloy

NASA Astrophysics Data System (ADS)

Kuzmann, E.; Sziráki, L.; Stichleutner, S.; Homonnay, Z.; Lak, G. B.; El-Sharif, M.; Chisholm, C. U.

2017-11-01

Constant current electrochemical deposition technique was used to obtain quaternary alloys of Sn-Fe-Co-Ni from a gluconate electrolyte, which to date have not been reported in the literature. For the characterization of electroplated alloys, 57Fe and 119Sn Conversion Electron Mössbauer Spectroscopy (CEMS), XRD and SEM/EDAX were used. XRD revealed the amorphous character of the novel Sn-Fe-Co-Ni electrodeposited alloys. 57Fe Mössbauer spectrum of quaternary deposit with composition of 37.0 at% Sn, 38.8 at% Fe, 16.8 at% Co and 7.4 at% Ni displayed a magnetically split sextet (B = 28.9T) with broad lines typical of iron bearing ferromagnetic amorphous alloys. Magnetically split 119Sn spectra reflecting a transferred hyperfine field (B = 2.3T) were also observed. New quaternary Sn-Fe-Co-Ni alloys were successfully prepared.

β-lactamases produced by amoxicillin-clavulanate-resistant enterobacteria isolated in Buenos Aires, Argentina: a new blaTEM gene.

PubMed

Di Conza, José A; Badaracco, Alejandra; Ayala, Juan; Rodríguez, Cynthia; Famiglietti, Angela; Gutkind, Gabriel O

2014-01-01

Resistance to β-lactam/β-lactamase inhibitors in enterobacteria is a growing problem that has not been intensively studied in Argentina. In the present work, 54/843 enterobacteria collected in a teaching hospital of Buenos Aires city were ampicillin-sulbactam-resistant isolates remaining susceptible to second- and third-generation cephalosporins. The enzymatic mechanisms present in the isolates, which were also amoxicillin-clavulanic acid (AMC)-resistant (18/54) were herein analyzed. Sequencing revealed two different variants of blaTEM-1, being blaTEM-1b the most frequently detected allelle (10 Escherichia coli, 3 Klebsiella pneumoniae, 2 Proteus mirabilis and 1 Raoultella terrigena) followed by blaTEM-1a (1 K. pneumoniae). Amoxicillin-clavulanate resistance seems to be mainly associated with TEM-1 overproduction (mostly in E. coli) or co-expressed with OXA-2-like and/or SHV β-lactamases (K. pneumoniae and P. mirabilis). A new blaTEM variant (TEM-163) was described in an E. coli strain having an AMC MIC value of 16/8μg/ml. TEM-163 contains Arg275Gln and His289Leu amino acid substitutions. On the basis of the high specific activity and low IC50 for clavulanic acid observed, the resistance pattern seems to be due to overproduction of the new variant of broad spectrum β-lactamase rather than to an inhibitor-resistant TEM (IRT)-like behavior. Copyright © 2014 Asociación Argentina de Microbiología. Publicado por Elsevier España. All rights reserved.

2.5D Modeling of TEM Data Applied to Hidrogeological Studies in PARANÁ Basin, Brazil

NASA Astrophysics Data System (ADS)

Bortolozo, C. A.; Porsani, J. L.; Santos, F. M.

2013-12-01

The transient electromagnetic method (TEM) is used all over the world and has shown great potential in hydrological, hazardous waste site characterization, mineral exploration, general geological mapping, and geophysical reconnaissance. However, the behavior of TEM fields are very complex and is not yet fully understood. Forward modeling is one of the most common and effective methods to understand the physical behavior and significance of the electromagnetics responses of a TEM sounding. Until now, there are a limited number of solutions for the 2D forward problem for TEM. More rare are the descriptions of a three-component response of a 3D source over 2D earth, which is the so-called 2.5D. The 2.5D approach is more realistic than the conventional 2D source previous used, once normally the source cannot be realistic represented for a 2D approximation (normally source are square loops). At present the 2.5D model represents the only way of interpreting TEM data in terms of a complex earth, due to the prohibitive amount of computer time and storage required for a full 3D model. In this work we developed a TEM modeling program for understanding the different responses and how the magnetic and electric fields, produced by loop sources at air-earth interface, behave in different geoelectrical distributions. The models used in the examples are proposed focusing hydrogeological studies, once the main objective of this work is for detecting different kinds of aquifers in Paraná sedimentary basin, in São Paulo State - Brazil. The program was developed in MATLAB, a widespread language very common in the scientific community.

Network Analysis of Sequence-Function Relationships and Exploration of Sequence Space of TEM β-Lactamases.

PubMed

Zeil, Catharina; Widmann, Michael; Fademrecht, Silvia; Vogel, Constantin; Pleiss, Jürgen

2016-05-01

The Lactamase Engineering Database (www.LacED.uni-stuttgart.de) was developed to facilitate the classification and analysis of TEM β-lactamases. The current version contains 474 TEM variants. Two hundred fifty-nine variants form a large scale-free network of highly connected point mutants. The network was divided into three subnetworks which were enriched by single phenotypes: one network with predominantly 2be and two networks with 2br phenotypes. Fifteen positions were found to be highly variable, contributing to the majority of the observed variants. Since it is expected that a considerable fraction of the theoretical sequence space is functional, the currently sequenced 474 variants represent only the tip of the iceberg of functional TEM β-lactamase variants which form a huge natural reservoir of highly interconnected variants. Almost 50% of the variants are part of a quartet. Thus, two single mutations that result in functional enzymes can be combined into a functional protein. Most of these quartets consist of the same phenotype, or the mutations are additive with respect to the phenotype. By predicting quartets from triplets, 3,916 unknown variants were constructed. Eighty-seven variants complement multiple quartets and therefore have a high probability of being functional. The construction of a TEM β-lactamase network and subsequent analyses by clustering and quartet prediction are valuable tools to gain new insights into the viable sequence space of TEM β-lactamases and to predict their phenotype. The highly connected sequence space of TEM β-lactamases is ideally suited to network analysis and demonstrates the strengths of network analysis over tree reconstruction methods. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Large-scale preparation of shape controlled SnO and improved capacitance for supercapacitors: from nanoclusters to square microplates

NASA Astrophysics Data System (ADS)

Wang, Lu; Ji, Hongmei; Zhu, Feng; Chen, Zhi; Yang, Yang; Jiang, Xuefan; Pinto, João; Yang, Gang

2013-07-01

Here, we first provide a facile ultrasonic-assisted synthesis of SnO using SnCl2 and the organic solvent of ethanolamine (ETA). The moderate alkalinity of ETA and ultrasound play very important roles in the synthesis of SnO. After the hydrolysis of the intermediate of ETA-Sn(ii), the as-synthesized SnO nanoclusters undergo assembly, amalgamation, and preferential growth to microplates in hydrothermal treatment. The as-synthesized SnO was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), ultraviolet-visible absorption spectroscopy (UV-vis) and X-ray diffraction (XRD). To explore its potential applications in energy storage, SnO was fabricated into a supercapacitor electrode and characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and galvanostatic charge-discharge measurements. The as-synthesized SnO exhibits remarkable pseudocapacitive activity including high specific capacitance (208.9 F g-1 at 0.1 A g-1), good rate capability (65.8 F g-1 at 40 A g-1), and excellent cycling stability (retention 119.3% after 10 000 cycles) for application in supercapacitors. The capacitive behavior of SnO with various crystal morphologies was observed by fitted EIS using an equivalent circuit. The novel synthetic route for SnO is a convenient and potential way to large-scale production of microplates which is expected to be applicable in the synthesis of other metal oxide nanoparticles.Here, we first provide a facile ultrasonic-assisted synthesis of SnO using SnCl2 and the organic solvent of ethanolamine (ETA). The moderate alkalinity of ETA and ultrasound play very important roles in the synthesis of SnO. After the hydrolysis of the intermediate of ETA-Sn(ii), the as-synthesized SnO nanoclusters undergo assembly, amalgamation, and preferential growth to microplates in hydrothermal treatment. The as-synthesized SnO was characterized by scanning

Validation of enhanced stabilization of municipal solid waste under controlled leachate recirculation using FTIR and XRD.

PubMed

Sethi, Sapna; Kothiyal, N C; Nema, Arvind K

2012-07-01

Leachate recirculation at neutral PH accompanied with buffer/nutrients addition has been used successfully in earlier stabilization of municipal solid waste in bioreactor landfills. In the present study, efforts were made to enhance the stabilization rate of municipal solid waste (MSW) and organic solid waste (OSW) in simulated landfill bioreactors by controlling the pH of recirculated leachate towards slightly alkaline side in absence of additional buffer and nutrients addition. Enhanced stabilization in waste samples was monitored with the help of analytical tools like Fourier Transform Infrared Spectroscopy (FTIR) and X-Ray Diffraction (XRD). Predominance of bands assigned to inorganic compounds and comparatively lower intensities of bands for organic compounds in the FTIR spectra of waste samples degraded with leachate recirculation under controlled pH confirmed higher rate of biodegradation and mineralization of waste than the samples degraded without controlled leachate recirculation. XRD spectra also confirmed to a greater extent of mineralization in the waste samples degraded under leachate recirculation with controlled pH. Comparison of XRD spectra of two types of wastes pointed out higher degree of mineralization in organic solid waste as compared to municipal solid waste.

[Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province].

PubMed

Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao

2014-12-01

Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

Studying dynamic processes in liquids by TEM/STEM/DTEM

NASA Astrophysics Data System (ADS)

Abellan, Patricia; Evans, James; Woehl, Taylor; Jungjohann, Katherine; Parent, Lucas; Arslan, Ilke; Ristenpart, William; Browning, Nigel; Mater. Sci. Group Team; Microsc. Group Team; Catal. Sci. Group Collaboration; Ristenpart Res. Group Collaboration

2013-03-01

In order to study dynamic phenomena such as corrosion or catalysis, extreme environmental conditions must be reproduced around the specimen - these include high-temperatures, high-pressures, specific oxidizing/reducing atmospheres or a liquid environment. The use of environmental stages specifically designed to fit in any transmission electron microscope (TEM) allows us to apply the distinct capabilities of each instrument to study dynamic processes. Localized gas/fluid conditions are created around the sample and separated from the high vacuum inside the microscope using hermetically sealed windowed-cells. Advanced capabilities of these techniques include spatial resolutions of ~1 Angstrom or better in aberration corrected instruments or temporal resolutions in the microsecond-nanosecond range in a dynamic TEM (DTEM). Here, unique qualities of the DTEM that benefit the in-situ experiments with gas/fluid environmental cells will be discussed. We also present our results with a liquid stage allowing atomic resolution imaging of nanomaterials in a colloidal suspension, core EEL spectra acquisition, continuous flow, controlled growth of nanocrystals and systematic calibration of the effect of the electron dose on silver nuclei formation.

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

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

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

2014-04-24

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

Pronounced effects of the nominal concentrations of WO3 and Ag: WO3 nano-plates (obtained by a co-precipitation method) on their structural, morphological and optical properties

NASA Astrophysics Data System (ADS)

Rajendran, V.; Deepa, B.

2018-03-01

Tungsten oxide and different concentration of silver (Ag)-doped tungsten oxide nano material were synthesized by co-precipitation technique. The functional vibrations, structure, and morphology of as-prepared nano material were studied by Fourier transmission infrared spectroscopy, X-ray diffraction, scanning electron microscopy (SEM) and High-resolution transmission electron microscopy (HR-TEM) techniques. The SEM and HR-TEM analysis revealed the formation of nano-plate/nano rods with an average diameter of 40-80 nm diameter and 1-1.5 mm length. Fluorescence (PL) and UV-visible absorption techniques have been used to study the optical properties of the prepared nanoparticles. The observed red shift in the visible absorption spectra confirmed the promoted electron-phonon interaction in WO3 and Ag: WO3 nanoparticles compared to bulk structures. The photoluminescence of nanocrystalline Ag2+ doped WO3 exhibited a strong violet-blue, blue-green emission. Concentration dependence of the emission intensity of Ag2+ in WO3 was studied, and the significant concentration was found to be 0.5% of Ag: WO3. The effluent dye degradation executed for the 0.5% of Ag: WO3 sample under the visible light which reveals the highest degradation efficiency in appropriate time.

The preparation of nanosized polyethylene particles via novel heterogeneous non-metallocene catalyst (m-CH3PhO)TiCl3/CNTs/AlEt3

NASA Astrophysics Data System (ADS)

Wang, J.; Guo, J. P.; Yi, J. J.; Huang, Q. G.; Li, H. M.; Li, Y. F.; Gao, K. J.; Yang, W. T.

2014-08-01

This paper reports the preparation of coral-shaped topological morphology nascent polyethylene (PE) particles promoted by the novel heterogeneous non-metallocene catalyst (m-CH3PhO)TiCl3/carbon nanotubes (CNTs), with AlEt3 used as a cocatalyst. Scanning electron microscope (SEM), high resolution transmission electron microscope (HR-TEM) and inductively coupled plasma (ICP) emission spectroscopy were used to determine the morphology of the catalyst particles and the content of (m-CH3PhO)TiCl3. The carbon nanotube surface was treated with Grignard Reagent prior to reacting with (m-CH3PhO)TiCl3. The catalyst system could effectively catalyze ethylene polymerization and ethylene with 1- hexene copolymerization, the catalytic activity could reach up to 5.8 kg/((gTi)h). Morphology of the obtained polymer particles by SEM and HR-TEM technique revealed that the nascent polyethylene particles looked like coral shape in micro-size. The multiwalled carbon nanotubes (MWCNTs) supported catalysts polymerized ethylene to form polymer nanocomposite in situ. The microscopic examination of this nanocomposite revealed that carbon nanoparticles in PE matrix had a good distribution and the cryogenically fractured surface was ductile-like when polymerization time was 2 min.

Superionic conductor PbSnF4 in the inner channel of SWNT

NASA Astrophysics Data System (ADS)

Zakalyukin, Ruslan Mikhalovich; Levkevich, Ekaterina Alexandrovna; Kumskov, Andrey Sergeevich; Orekhov, Andrey Sergeevich

2018-04-01

The nanocomposite PbSnF4@SWNT was obtained by capillary technique for the first time. This nanocomposite was investigated using X-ray diffraction phase analysis (XRD), high-resolution transmission electron microscopy (HRTEM) and scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDX). SWNT diameter is ˜2 nm. Lead tetrafluorostannate (PbSnF4) monoclinic modification (space group P2/n) was identified by XRD analysis. The periodicity of the crystal plane (201) along the tube axis is ˜3.2Å. The distortion of plane is 11° with respect to the nanotube axis. The model of PbSnF4 single crystal contains ˜168 atoms. The structure of 1D PbSnF4@SWNT nanocomposite and HREM image were modelled.

Synthesis of Silver and Gold Nanoparticles Using Antioxidants from Blackberry, Blueberry, Pomegranate, and Turmeric Extracts

EPA Science Inventory

Greener synthesis of Ag and Au nanoparticles is described using antioxidants from blackberry, blueberry, pomegranate, and turmeric extracts. The synthesized particles were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HR...

TEM-induced gene mutations at enzyme loci in the mouse.

PubMed

Soares, E R

1979-01-01

Strain DBA/2J male mice were treated with triethylenemelamine (TEM) and subsequently mated to strain C57BL/6J females. Tissues from F1 progeny produced in these crosses were then examined using starch gel electrophoresis for the presence of presumed induced mutations at a series of 11 specific enzyme loci. In the course of this study, four heritable mutations were identified at the following loci: Es-1, Ldh-1, Pgm-1, and Gpi-1. Of these four, the first two were apparently segregating in parental males and were not TEM-induced. Both of these are viable and fertile in the heterozygous and homozygous condition, and neither confers any readily apparent deleterious effect to the animal. The latter mutations (Pgm-1 and Gpi-1) are presumably induced. Although viable and fertile in the heterozygous state, we have not recovered any offsping homozygous for either of these two mutations.

Development of an analytical environmental TEM system and its application.

PubMed

Kishita, Keisuke; Sakai, Hisashi; Tanaka, Hiromochi; Saka, Hiroyasu; Kuroda, Kotaro; Sakamoto, Masayuki; Watabe, Akira; Kamino, Takeo

2009-12-01

Many automotive materials, such as catalysts and fuel cell materials, undergo significant changes in structure or properties when subjected to temperature change or the addition of a gas. For this reason, in the development of these materials, it is important to study the behavior of the material under controlled temperatures and gaseous atmospheres. Recently, a new environmental transmission electron microscope (TEM) has been developed for observation with a high resolution at high temperatures and under gaseous atmospheres, thus making it possible to analyze reaction processes in details. Also, the new TEM provides a high degree of reproducibility of observation conditions, thus making it possible to compare and validate observation of various specimens under a given set of conditions. Furthermore, easiness of gas condition and temperature control can provide a powerful tool for the studying of the mechanism of material change, such as oxidation and reduction reactions.

Mineralogical Composition of the Mexican Ordinary Chondrite Type Meteorite: A Raman, Infrared and XRD Study

NASA Astrophysics Data System (ADS)

Ostrooumov, M.

2016-08-01

The Raman microprobe (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of seven mexican meteorites: Aldama, Cosina, El Pozo, Escalon, Nuevo Mercurio,Pacula, Zapotitlan Salinas.

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

USDA-ARS?s Scientific Manuscript database

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

[NIR and XRD analysis of drill-hole samples from Zhamuaobao iron-graphite deposit, Inner Mongolia].

PubMed

Li, Ying-kui; Cao, Jian-jin; Wu, Zheng-quan; Dai, Dong-le; Lin, Zu-xu

2015-01-01

The author analyzed the 4202 drill-hole samples from Zhamuaobao iron-graphite deposit by using near infrared spectroscopy(NIR) and X-ray diffraction(XRD) measuring and testing techniques, and then compared and summarized the results of two kinds of testing technology. The results indicate that some difference of the mineral composition exists among different layers, the lithology from upper to deeper is the clay gravel layer of tertiary and quaternary, mudstone, mica quartz schist, quartz actinolite scarn, skarnization marble, iron ore deposits, graphite deposits and mica quartz schist. The petrogenesis in different depth also shows difference, which may indicate the geological characteristic to some extent. The samples had mainly undergone such processes as oxidization, carbonation, chloritization and skarn alteration. The research results can not only improve the geological feature of the mining area, but also have great importance in ore exploration, mining, mineral processing and so on. What's more, as XRD can provide preliminary information about the mineral composition, NIR can make further judgement on the existence of the minerals. The research integrated the advantages of both NIR and XRD measuring and testing techniques, put forward a method with two kinds of modern testing technology combined with each other, which may improve the accuracy of the mineral composition identification. In the meantime, the NIR will be more wildly used in geography on the basis of mineral spectroscopy.

Dopant concentration dependent growth of Fe:ZnO nanostructures

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

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

2016-05-23

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

Chemical effect of Si+ ions on the implantation-induced defects in ZnO studied by a slow positron beam

NASA Astrophysics Data System (ADS)

Jiang, M.; Wang, D. D.; Chen, Z. Q.; Kimura, S.; Yamashita, Y.; Mori, A.; Uedono, A.

2013-01-01

Undoped ZnO single crystals were implanted with 300 keV Si+ ions to a dose of 6 × 1016 cm-2. A combination of X-ray diffraction (XRD), positron annihilation, Raman scattering, high resolution transmission electron microscopy (HRTEM), and photoluminescence (PL) was used to study the microstructure evolution after implantation and subsequent annealing. A very large increase of Doppler broadening S parameters in Si+-implanted region was detected by using a slow positron beam, indicating that vacancy clusters or microvoids are induced by implantation. The S parameters increase further after annealing up to 700 °C, suggesting agglomeration of these vacancies or microvoids to larger size. Most of these defects are removed after annealing up to 1100 °C. The other measurements such as XRD, Raman scattering, and PL all indicate severe damage and even disordered structure induced by Si+ implantation. The damage and disordered lattice shows recovery after annealing above 700 °C. Amorphous regions are observed by HRTEM measurement, directly testifies that amorphous phase is induced by Si+ implantation in ZnO. Analysis of the S - W correlation and the coincidence Doppler broadening spectra gives direct evidence of SiO2 precipitates in the sample annealed at 700 °C, which strongly supports the chemical effect of Si ions on the amorphization of ZnO lattice.

Green synthesis of NiO nanoparticles using Moringa oleifera extract and their biomedical applications: Cytotoxicity effect of nanoparticles against HT-29 cancer cells.

PubMed

Ezhilarasi, A Angel; Vijaya, J Judith; Kaviyarasu, K; Maaza, M; Ayeshamariam, A; Kennedy, L John

2016-11-01

Green protocols for the synthesis of nickel oxide nanoparticles using Moringa oleifera plant extract has been reported in the present study as they are cost effective and ecofriendly, moreover this paper records that the nickel oxide (NiO) nanoparticles prepared from green method shows better cytotoxicity and antibacterial activity. The NiO nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), High resolution transmission electron microscopy (HRTEM), Energy dispersive X-ray analysis (EDX), and Photoluminescence spectroscopy (PL). The formation of a pure nickel oxide phase was confirmed by XRD and FTIR. The synthesized NiO nanoparticles was single crystalline having face centered cubic phase and has two intense photoluminescence emissions at 305.46nm and 410nm. The formation of nano- and micro-structures was confirmed by HRTEM. The in-vitro cytotoxicity and cell viability of human cancer cell HT-29 (Colon Carcinoma cell lines) and antibacterial studies against various bacterial strains were studied with various concentrations of nickel oxide nanoparticles prepared from Moringa oleifera plant extract. MTT assay measurements on cell viability and morphological studies proved that the synthesized NiO nanoparticles posses cytotoxic activity against human cancer cells and the various zones of inhibition (mm), obtained revealed the effective antibacterial activity of NiO nanoparticles against various Gram positive and Gram negative bacterial pathogens. Copyright © 2016 Elsevier B.V. All rights reserved.

On the structural affinity of macromolecules with different biological properties: molecular dynamics simulations of a series of TEM-1 mutants.

PubMed

Giampaolo, Alessia Di; Mazza, Fernando; Daidone, Isabella; Amicosante, Gianfranco; Perilli, Mariagrazia; Aschi, Massimiliano

2013-07-12

Molecular Dynamics simulations have been carried out in order to provide a molecular rationalization of the biological and thermodynamic differences observed for a class of TEM β-lactamases. In particular we have considered the TEM-1(wt), the single point mutants TEM-40 and TEM-19 representative of IRT and ESBL classes respectively, and TEM-1 mutant M182T, TEM-32 and TEM-20 which differ from the first three for the additional of M182T mutation. Results indicate that most of the thermodynamic, and probably biological behaviour of these systems arise from subtle effects which, starting from the alterations of the local interactions, produce drastic modifications of the conformational space spanned by the enzymes. The present study suggests that systems showing essentially the same secondary and tertiary structure may differentiate their chemical-biological activity essentially (and probably exclusively) on the basis of the thermal fluctuations occurring in their physiological environment. Copyright © 2013 Elsevier Inc. All rights reserved.

[Analysis of XRD spectral characteristics of soil clay mineral in two typical cultivated soils].

PubMed

Zhang, Zhi-Dan; Luo, Xiang-Li; Jiang, Hai-Chao; Li, Qiao; Shen, Cong-Ying; Liu, Hang; Zhou, Ya-Juan; Zhao, Lan-Po; Wang, Ji-Hong

2014-07-01

The present paper took black soil and chernozem, the typical cultivated soil in major grain producing area of Northeast, as the study object, and determinated the soil particle composition characteristics of two cultivated soils under the same climate and location. Then XRD was used to study the composition and difference of clay mineral in two kinds of soil and the evolutionary mechanism was explored. The results showed that the two kinds of soil particles were composed mainly of the sand, followed by clay and silt. When the particle accumulation rate reached 50%, the central particle size was in the 15-130 microm interval. Except for black soil profile of Shengli Xiang, the content of clay showed converse sequence to the central particle in two soils. Clay accumulated under upper layer (18.82%) in black soil profile while under caliche layer (17.41%) in chernozem profile. Clay content was the least in parent material horizon except in black profile of Quanyanling. Analysis of clay XRD atlas showed that the difference lied in not only the strength of diffraction peak, but also in the mineral composition. The main contents of black soil and chernozem were both 2 : 1 clay, the composition of black soil was smectite/illite mixed layer-illite-vermiculite and that of chernozem was S/I mixture-illite-montmorillonite, and both of them contained little kaolinite, chlorite, quartz and other primary mineral. This paper used XRD to determine the characteristics of clay minerals comprehensively, and analyzed two kinds of typical cultivated soil comparatively, and it was a new perspective of soil minerals study.

Cdc15 integrates Tem1 GTPase-mediated spatial signals with Polo kinase-mediated temporal cues to activate mitotic exit.

PubMed

Rock, Jeremy M; Amon, Angelika

2011-09-15

In budding yeast, a Ras-like GTPase signaling cascade known as the mitotic exit network (MEN) promotes exit from mitosis. To ensure the accurate execution of mitosis, MEN activity is coordinated with other cellular events and restricted to anaphase. The MEN GTPase Tem1 has been assumed to be the central switch in MEN regulation. We show here that during an unperturbed cell cycle, restricting MEN activity to anaphase can occur in a Tem1 GTPase-independent manner. We found that the anaphase-specific activation of the MEN in the absence of Tem1 is controlled by the Polo kinase Cdc5. We further show that both Tem1 and Cdc5 are required to recruit the MEN kinase Cdc15 to spindle pole bodies, which is both necessary and sufficient to induce MEN signaling. Thus, Cdc15 functions as a coincidence detector of two essential cell cycle oscillators: the Polo kinase Cdc5 synthesis/degradation cycle and the Tem1 G-protein cycle. The Cdc15-dependent integration of these temporal (Cdc5 and Tem1 activity) and spatial (Tem1 activity) signals ensures that exit from mitosis occurs only after proper genome partitioning.

3D TEM reconstruction and segmentation process of laminar bio-nanocomposites

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

Iturrondobeitia, M., E-mail: maider.iturrondobeitia@ehu.es; Okariz, A.; Fernandez-Martinez, R.

2015-03-30

The microstructure of laminar bio-nanocomposites (Poly (lactic acid)(PLA)/clay) depends on the amount of clay platelet opening after integration with the polymer matrix and determines the final properties of the material. Transmission electron microscopy (TEM) technique is the only one that can provide a direct observation of the layer dispersion and the degree of exfoliation. However, the orientation of the clay platelets, which affects the final properties, is practically immeasurable from a single 2D TEM image. This issue can be overcome using transmission electron tomography (ET), a technique that allows the complete 3D characterization of the structure, including the measurement ofmore » the orientation of clay platelets, their morphology and their 3D distribution. ET involves a 3D reconstruction of the study volume and a subsequent segmentation of the study object. Currently, accurate segmentation is performed manually, which is inefficient and tedious. The aim of this work is to propose an objective/automated segmentation methodology process of a 3D TEM tomography reconstruction. In this method the segmentation threshold is optimized by minimizing the variation of the dimensions of the segmented objects and matching the segmented V{sub clay} (%) and the actual one. The method is first validated using a fictitious set of objects, and then applied on a nanocomposite.« less

Covalent modification and exfoliation of graphene oxide using ferrocene

NASA Astrophysics Data System (ADS)

Avinash, M. B.; Subrahmanyam, K. S.; Sundarayya, Y.; Govindaraju, T.

2010-09-01

Large scale preparation of single-layer graphene and graphene oxide is of great importance due to their potential applications. We report a simple room temperature method for the exfoliation of graphene oxide using covalent modification of graphene oxide with ferrocene to obtain single-layer graphene oxide sheets. The samples were characterized by FESEM, HRTEM, AFM, EDAX, FT-IR, Raman and Mössbauer spectroscopic studies. HRTEM micrograph of the covalently modified graphene oxide showed increased interlayer spacing of ~2.4 nm due to ferrocene intercalation. The presence of single-layer graphene oxide sheets were confirmed by AFM studies. The covalently modified ferrocene-graphene oxide composite showed interesting magnetic behavior.Large scale preparation of single-layer graphene and graphene oxide is of great importance due to their potential applications. We report a simple room temperature method for the exfoliation of graphene oxide using covalent modification of graphene oxide with ferrocene to obtain single-layer graphene oxide sheets. The samples were characterized by FESEM, HRTEM, AFM, EDAX, FT-IR, Raman and Mössbauer spectroscopic studies. HRTEM micrograph of the covalently modified graphene oxide showed increased interlayer spacing of ~2.4 nm due to ferrocene intercalation. The presence of single-layer graphene oxide sheets were confirmed by AFM studies. The covalently modified ferrocene-graphene oxide composite showed interesting magnetic behavior. Electronic supplementary information (ESI) available: Magnetic data; AFM images; TEM micrographs; and Mössbauer spectroscopic data. See DOI: 10.1039/c0nr00024h

Scalable pumping approach for extracting the maximum TEM(00) solar laser power.

PubMed

Liang, Dawei; Almeida, Joana; Vistas, Cláudia R

2014-10-20

A scalable TEM(00) solar laser pumping approach is composed of four pairs of first-stage Fresnel lens-folding mirror collectors, four fused-silica secondary concentrators with light guides of rectangular cross-section for radiation homogenization, four hollow two-dimensional compound parabolic concentrators for further concentration of uniform radiations from the light guides to a 3 mm diameter, 76 mm length Nd:YAG rod within four V-shaped pumping cavities. An asymmetric resonator ensures an efficient large-mode matching between pump light and oscillating laser light. Laser power of 59.1 W TEM(00) is calculated by ZEMAX and LASCAD numerical analysis, revealing 20 times improvement in brightness figure of merit.

[Infrared spectroscopy and XRD studies of coral fossils].

PubMed

Chen, Quan-li; Zhou, Guan-min; Yin, Zuo-wei

2012-08-01

Coral fossil is an old remain of multicellular animal on the earth, and formed by various geological processes. The structural characteristics and compositions of the coral fossils with different color and radial texture on the surface were studied by infrared absorption spectroscopy and X-ray powder diffraction analyses. The results show that the studied coral fossils mainly are composed of SiO2, and the radial microstructure characterized by the calcareous coral cross-section is preserved. It is formed by metasomatism by SiO2. The infrared absorption spectra of the coral fossil with different color and texture are essentially the same, showing typical infrared absorption spectra of the quartz jade. XRD analysis shows that the main components of the coral fossils with different color and texture are consistent and mainly composed of SiO2 with a trace amount of other minerals and without CaCO3.

Bayesian resolution of TEM, CSEM and MT soundings: a comparative study

NASA Astrophysics Data System (ADS)

Blatter, D. B.; Ray, A.; Key, K.

2017-12-01

We examine the resolution of three electromagnetic exploration methods commonly used to map the electrical conductivity of the shallow crust - the magnetotelluric (MT) method, the controlled-source electromagnetic (CSEM) method and the transient electromagnetic (TEM) method. TEM and CSEM utilize an artificial source of EM energy, while MT makes use of natural variations in the Earth's electromagnetic field. For a given geological setting and acquisition parameters, each of these methods will have a different resolution due to differences in the source field polarization and the frequency range of the measurements. For example, the MT and TEM methods primarily rely on induced horizontal currents and are most sensitive to conductive layers while the CSEM method generates vertical loops of current and is more sensitive to resistive features. Our study seeks to provide a robust resolution comparison that can help inform exploration geophysicists about which technique is best suited for a particular target. While it is possible to understand and describe a difference in resolution qualitatively, it remains challenging to fully describe it quantitatively using optimization based approaches. Part of the difficulty here stems from the standard electromagnetic inversion toolkit, which makes heavy use of regularization (often in the form of smoothing) to constrain the non-uniqueness inherent in the inverse problem. This regularization makes it difficult to accurately estimate the uncertainty in estimated model parameters - and therefore obscures their true resolution. To overcome this difficulty, we compare the resolution of CSEM, airborne TEM, and MT data quantitatively using a Bayesian trans-dimensional Markov chain Monte Carlo (McMC) inversion scheme. Noisy synthetic data for this study are computed from various representative 1D test models: a conductive anomaly under a conductive/resistive overburden; and a resistive anomaly under a conductive/resistive overburden. In

Resolution Quality and Atom Positions in Sub-?ngstr?m Electron Microscopy

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

O'Keefe, Michael A.; Allard Jr, Lawrence Frederick; Blom, Douglas Allen

2005-01-01

John Cowley pioneered use of transmission electron microscopy (TEM) for high-resolution imaging and helped spur improvements in resolution that enabled researchers to pinpoint the positions of all but the lightest atoms within a crystal structure. Sub-{angstrom} capabilities allow imaging of even the lightest atoms. Initially achieved with software aberration correction (focal-series reconstruction of the specimen exit-surface wave), sub-{angstrom} imaging will become commonplace for next-generation electron microscopes with hardware-corrected lenses and monochromated electron beams. Currently, advanced HR-TEMs can image columns of light atoms (carbon, oxygen, nitrogen) in complex structures, including the lithium atoms present in battery materials. The ability to determinemore » whether an image peak represents one single atom (or atom column) instead of several depends on the resolution of the HR-(S)TEM. Rayleigh's resolution criterion, an accepted standard in optics, was derived as a means for judging when two image intensity peaks from two sources of light (stars) are distinguishable from a single source. Atom spacings closer than the Rayleigh limit have been resolved in HR-TEM, suggesting that it may be useful to consider other limits, such as the Sparrow resolution criterion. From the viewpoint of the materials scientist, it is important to be able to use the image to determine whether an image feature represents one or more atoms (resolution), and where the atoms (or atom columns) are positioned relative to one another (resolution quality). When atoms and the corresponding image peaks are separated by more than the Rayleigh limit of the HR-(S)TEM, it is possible to adjust imaging parameters so that relative peak positions in the image correspond to relative atom positions in the specimen. When atoms are closer than the Rayleigh limit, we must find the relationship of the peak position to the atom position by peak fitting or, if we have a suitable model, by

Development and Application of Operando TEM to a Ruthenium Catalyst for CO Oxidation

NASA Astrophysics Data System (ADS)

Miller, Benjamin Kyle

Operando transmission electron microscopy (TEM) is an extension of in-situ TEM in which the performance of the material being observed is measured simultaneously. This is of great value, since structure-performance relationships lie at the heart of materials science. For catalyst materials, like the SiO2-supported Ru nanoparticles studied, the important performance metric, catalyst activity, is measured inside the microscope by determining the gas composition during imaging. This is accomplished by acquisition of electron energy loss spectra (EELS) of the gas in the environmental TEM while catalysis is taking place. In this work, automated methods for rapidly quantifying low-loss and core-loss EELS of gases were developed. A new sample preparation method was also established to increase catalytic conversion inside a differentially-pumped environmental TEM, and the maximum CO conversion observed was about 80%. A system for mixing gases and delivering them to the environmental TEM was designed and built, and a method for locating and imaging nanoparticles in zone axis orientations while minimizing electron dose rate was determined. After atomic resolution images of Ru nanoparticles observed during CO oxidation were obtained, the shape and surface structures of these particles was investigated. A Wulff model structure for Ru particles was compared to experimental images both by manually rotating the model, and by automatically determining a matching orientation using cross-correlation of shape signatures. From this analysis, it was determined that most Ru particles are close to Wulff-shaped during CO oxidation. While thick oxide layers were not observed to form on Ru during CO oxidation, thin RuO2 layers on the surface of Ru nanoparticles were imaged with atomic resolution for the first time. The activity of these layers is discussed in the context of the literature on the subject, which has thus far been inconclusive. We conclude that disordered oxidized ruthenium

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Multivariate analysis of DSC-XRD simultaneous measurement data: a study of multistage crystalline structure changes in a linear poly(ethylene imine) thin film.

PubMed

Kakuda, Hiroyuki; Okada, Tetsuo; Otsuka, Makoto; Katsumoto, Yukiteru; Hasegawa, Takeshi

2009-01-01

A multivariate analytical technique has been applied to the analysis of simultaneous measurement data from differential scanning calorimetry (DSC) and X-ray diffraction (XRD) in order to study thermal changes in crystalline structure of a linear poly(ethylene imine) (LPEI) film. A large number of XRD patterns generated from the simultaneous measurements were subjected to an augmented alternative least-squares (ALS) regression analysis, and the XRD patterns were readily decomposed into chemically independent XRD patterns and their thermal profiles were also obtained at the same time. The decomposed XRD patterns and the profiles were useful in discussing the minute peaks in the DSC. The analytical results revealed the following changes of polymorphisms in detail: An LPEI film prepared by casting an aqueous solution was composed of sesquihydrate and hemihydrate crystals. The sesquihydrate one was lost at an early stage of heating, and the film changed into an amorphous state. Once the sesquihydrate was lost by heating, it was not recovered even when it was cooled back to room temperature. When the sample was heated again, structural changes were found between the hemihydrate and the amorphous components. In this manner, the simultaneous DSC-XRD measurements combined with ALS analysis proved to be powerful for obtaining a better understanding of the thermally induced changes of the crystalline structure in a polymer film.

Thinning of Large Biological Cells for Cryo-TEM Characterization by Cryo-FIB Milling

PubMed Central

Strunk, Korrinn M.; Ke, Danxia; Gray, Jennifer L.; Zhang, Peijun

2013-01-01

SUMMARY Focused ion beam milling at cryogenic temperatures (cryo-FIB) is a valuable tool that can be used to thin vitreous biological specimens for subsequent imaging and analysis in a cryo-transmission electron microscope (cryo-TEM) in their frozen-hydrated state. This technique offers the potential benefit of eliminating the mechanical artifacts that are typically found with cryo-ultramicrotomy. However, due to the additional complexity in transferring samples in and out of the FIB, contamination and devitrification of the amorphous ice is commonly encountered. In order to address these problems, we have designed a new sample cryo-shuttle that specifically accepts Polara TEM cartridges directly in order to simplify the transfer process between the FIB and TEM. We used the quality of the ice in the sample as an indicator to test various parameters used the process, and demonstrated with successful milling of large mammalian cells. By comparing the results from larger HeLa cells to those from E. coli cells, we discuss some of the artifacts and challenges we have encountered using this technique. PMID:22906009

TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy

NASA Astrophysics Data System (ADS)

Yano, K. H.; Swenson, M. J.; Wu, Y.; Wharry, J. P.

2017-01-01

The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe2+ ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

TEMs but not DKK1 could serve as complementary biomarkers for AFP in diagnosing AFP-negative hepatocellular carcinoma.

PubMed

Mao, Liping; Wang, Yueguo; Wang, Delin; Han, Gang; Fu, Shouzhong; Wang, Jianxin

2017-01-01

Hepatitis B virus (HBV)-related hepatocellular carcinoma (HCC) is prevalent worldwide. Despite its limitations, serum alpha-fetoprotein (AFP) remains the most widely-used biomarker for the diagnosis of HCC. This study aimed to assess whether measurement of peripheral plasma Dickkopf-1 (DKK1) and Tie2-expressing monocytes (TEMs) could overcome the limitations of AFP and improve the diagnostic accuracy of HCC. Plasma DKK1 level and the percentage of TEMs in peripheral CD14+CD16+ monocytes from HCC patients (n = 82), HBV-related liver cirrhosis (LC) patients (n = 29), chronic hepatitis B (CHB) infected patients (n = 28) and healthy volunteers (n = 31) were analyzed by ELISA and flow cytometry. Receiver operating characteristic (ROC) curves were used to analyze a single biomarker, or a combination of two or three biomarkers. Univariate and multivariate analyses were performed to assess the significance of each marker in prediction of HCC and AFP-negative HCC from LC patients. The percentage of TEMs in peripheral CD14+CD16+ monocytes and plasma level of DKK1 in HCC group were significantly higher than those in LC, CHB and healthy control groups (all P-values <0.05). The percentage of TEMs alone was also significantly higher in AFP-negative HCC group than that in LC, CHB and healthy control groups (all P-values <0.05). Plasma DKK1 level alone could not distinguish between AFP-negative HCC and LC patients. ROC curves showed that the optimal diagnostic cutoff value was 550.93 ng/L for DKK1 and 4.95% for TEMs. There was no significant difference in AUC of DKK1, TEMs and AFP in HCC diagnosis between the four groups (all P>0.05). A combination of DKK1, TEMs and AFP measurements increased the AUC for HCC diagnosis as compared with either marker alone (0.833; 95%CI 0.768-0.886). The AUC for TEMs was 0.692 (95% CI 0.564-0.819) in differentiating AFP-negative HCC from LC, with a sensitivity of 80.0% and a specificity of 65.52%. Only TEMs prevailed as a significant predictor for

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

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

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

2016-05-15

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

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

NASA Astrophysics Data System (ADS)

Johns, Steve; Shin, Wontak; Kane, Joshua J.; Windes, William E.; Ubic, Rick; Karthik, Chinnathambi

2018-07-01

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. To ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ∼60 μm. Discs 3 mm in diameter were then oxidized at temperatures between 575 °C and 625 °C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575 °C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

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

Johns, Steve; Shin, Wontak; Kane, Joshua J.

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

DOE PAGES

Johns, Steve; Shin, Wontak; Kane, Joshua J.; ...

2018-04-03

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

X-Ray Diffraction (XRD) Characterization Methods for Sigma=3 Twin Defects in Cubic Semiconductor (100) Wafers

NASA Technical Reports Server (NTRS)

Park, Yeonjoon (Inventor); Kim, Hyun Jung (Inventor); Skuza, Jonathan R. (Inventor); Lee, Kunik (Inventor); Choi, Sang Hyouk (Inventor); King, Glen C. (Inventor)

2017-01-01

An X-ray defraction (XRD) characterization method for sigma=3 twin defects in cubic semiconductor (100) wafers includes a concentration measurement method and a wafer mapping method for any cubic tetrahedral semiconductor wafers including GaAs (100) wafers and Si (100) wafers. The methods use the cubic semiconductor's (004) pole figure in order to detect sigma=3/{111} twin defects. The XRD methods are applicable to any (100) wafers of tetrahedral cubic semiconductors in the diamond structure (Si, Ge, C) and cubic zinc-blend structure (InP, InGaAs, CdTe, ZnSe, and so on) with various growth methods such as Liquid Encapsulated Czochralski (LEC) growth, Molecular Beam Epitaxy (MBE), Organometallic Vapor Phase Epitaxy (OMVPE), Czochralski growth and Metal Organic Chemical Vapor Deposition (MOCVD) growth.

Appraisal of an Array TEM Method in Detecting a Mined-Out Area Beneath a Conductive Layer

NASA Astrophysics Data System (ADS)

Li, Hai; Xue, Guo-qiang; Zhou, Nan-nan; Chen, Wei-ying

2015-10-01

The transient electromagnetic method has been extensively used for the detection of mined-out area in China for the past few years. In the cases that the mined-out area is overlain by a conductive layer, the detection of the target layer is difficult with a traditional loop source TEM method. In order to detect the target layer in this condition, this paper presents a newly developed array TEM method, which uses a grounded wire source. The underground current density distribution and the responses of the grounded wire source TEM configuration are modeled to demonstrate that the target layer is detectable in this condition. The 1D OCCAM inversion routine is applied to the synthetic single station data and common middle point gather. The result reveals that the electric source TEM method is capable of recovering the resistive target layer beneath the conductive overburden. By contrast, the conductive target layer cannot be recovered unless the distance between the target layer and the conductive overburden is large. Compared with inversion result of the single station data, the inversion of common middle point gather can better recover the resistivity of the target layer. Finally, a case study illustrates that the array TEM method is successfully applied in recovering a water-filled mined-out area beneath a conductive overburden.

Effectiveness of Shield Termination Techniques Tested with TEM Cell and Bulk Current Injection

NASA Technical Reports Server (NTRS)

Bradley, Arthur T.; Hare, Richard J.

2009-01-01

This paper presents experimental results of the effectiveness of various shield termination techniques. Each termination technique is evaluated by two independent noise injection methods; transverse electromagnetic (TEM) cell operated from 3 MHz 400 MHz, and bulk current injection (BCI) operated from 50 kHz 400 MHz. Both single carrier and broadband injection tests were investigated. Recommendations as to how to achieve the best shield transfer impedance (i.e. reduced coupled noise) are made based on the empirical data. Finally, the noise injection techniques themselves are indirectly evaluated by comparing the results obtained from the TEM Cell to those from BCI.

In situ assembly of well-dispersed Ni nanoparticles on silica nanotubes and excellent catalytic activity in 4-nitrophenol reduction

NASA Astrophysics Data System (ADS)

Zhang, Shenghuan; Gai, Shili; He, Fei; Ding, Shujiang; Li, Lei; Yang, Piaoping

2014-09-01

/SNTs makes it easy to recycle for reuse. Electronic supplementary information (ESI) available: XRD pattern and TEM image of SNTs after calcination, XRD pattern and EDS of NiSNTs, SEM images of a single SNT, NiSNTs and Ni/SNTs, enlarged HRTEM of Ni/SNTs, XRD pattern of NiO/SNTs, UV-vis spectra of the catalytic reduction of 4-NP to 4-AP over Ni/SNTs with different loading amounts, Ni/SNTs synthesized by wet impregnation and Ni/CNTs, TEM images of Ni/SNTs synthesized by wet impregnation and Ni/CNTs. See DOI: 10.1039/c4nr02096k

A Structural Study of Escherichia coli Cells Using an In Situ Liquid Chamber TEM Technology.

PubMed

Wang, Yibing; Chen, Xin; Cao, Hongliang; Deng, Chao; Cao, Xiaodan; Wang, Ping

2015-01-01

Studying cell microstructures and their behaviors under living conditions has been a challenging subject in microbiology. In this work, in situ liquid chamber TEM was used to study structures of Escherichia coli cells in aqueous solutions at a nanometer-scale resolution. Most of the cells remained intact under electron beam irradiation, and nanoscale structures were observed during the TEM imaging. The analysis revealed structures of pili surrounding the E. coli cells; the movements of the pili in the liquid were also observed during the in situ tests. This technology also allowed the observation of features of the nucleoid in the E. coli cells. Overall, in situ TEM can be applied as a valuable tool to study real-time microscopic structures and processes in microbial cells residing in native aqueous solutions.

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

PubMed

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

2013-12-01

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

TEM Pump With External Heat Source And Sink

NASA Technical Reports Server (NTRS)

Nesmith, Bill J.

1991-01-01

Proposed thermoelectric/electromagnetic (TEM) pump driven by external source of heat and by two or more heat pipe radiator heat sink(s). Thermoelectrics generate electrical current to circulate liquid metal in secondary loop of two-fluid-loop system. Intended for use with space and terrestrial dual loop liquid metal nuclear reactors. Applications include spacecraft on long missions or terrestrial beacons or scientific instruments having to operate in remote areas for long times. Design modified to include multiple radiators, converters, and ducts, as dictated by particular application.

Trace elemental analysis of Indian natural moonstone gems by PIXE and XRD techniques.

PubMed

Venkateswara Rao, R; Venkateswarulu, P; Kasipathi, C; Sivajyothi, S

2013-12-01

A selected number of Indian Eastern Ghats natural moonstone gems were studied with a powerful nuclear analytical and non-destructive Proton Induced X-ray Emission (PIXE) technique. Thirteen elements, including V, Co, Ni, Zn, Ga, Ba and Pb, were identified in these moonstones and may be useful in interpreting the various geochemical conditions and the probable cause of their inceptions in the moonstone gemstone matrix. Furthermore, preliminary XRD studies of different moonstone patterns were performed. The PIXE technique is a powerful method for quickly determining the elemental concentration of a substance. A 3MeV proton beam was employed to excite the samples. The chemical constituents of moonstones from parts of the Eastern Ghats geological formations of Andhra Pradesh, India were determined, and gemological studies were performed on those gems. The crystal structure and the lattice parameters of the moonstones were estimated using X-Ray Diffraction studies, trace and minor elements were determined using the PIXE technique, and major compositional elements were confirmed by XRD. In the present work, the usefulness and versatility of the PIXE technique for research in geo-scientific methodology is established. © 2013 Elsevier Ltd. All rights reserved.

Post Irradiation TEM Investigation of ZrN Coated U(Mo) Particles Prepared with FIB

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

Van Renterghem, W.; Leenaers, A.; Van den Berghe, S.

2015-10-01

In the framework of the Selenium project, two dispersion fuel plates were fabricated with Si and ZrN coated fuel particles and irradiated in the Br2 reactor of SCK•CEN to high burn-up. The first analysis of the irradiated plate proved the reduced swelling of the fuel plate and interaction layer growth up to 70% burn-up. The question was raised how the structure of the interaction layer had been affected by the irradiation and how the structure of the fuel particles had evolved. Hereto, samples from the ZrN coated UMo particles were prepared for transmission electron microscopy (TEM) using focused ion beammore » milling (FIB) at INL. The FIB technique allowed to precisely select the area of the interaction layer and/or fuel to produce a sample that is TEM transparent over an area of 20 by 20 µm. In this contribution, the first TEM results will be presented from the 66% burn-up sample.« less

GISAXS modelling of helium-induced nano-bubble formation in tungsten and comparison with TEM

NASA Astrophysics Data System (ADS)

Thompson, Matt; Sakamoto, Ryuichi; Bernard, Elodie; Kirby, Nigel; Kluth, Patrick; Riley, Daniel; Corr, Cormac

2016-05-01

Grazing-incidence small angle x-ray scattering (GISAXS) is a powerful non-destructive technique for the measurement of nano-bubble formation in tungsten under helium plasma exposure. Here, we present a comparative study between transmission electron microscopy (TEM) and GISAXS measurements of nano-bubble formation in tungsten exposed to helium plasma in the Large Helical Device (LHD) fusion experiment. Both techniques are in excellent agreement, suggesting that nano-bubbles range from spheroidal to ellipsoidal, displaying exponential diameter distributions with mean diameters μ=0.68 ± 0.04 nm and μ=0.6 ± 0.1 nm measured by TEM and GISAXS respectively. Depth distributions were also computed, with calculated exponential depth distributions with mean depths of 8.4 ± 0.5 nm and 9.1 ± 0.4 nm for TEM and GISAXS. In GISAXS modelling, spheroidal particles were fitted with an aspect ratio ε=0.7 ± 0.1. The GISAXS model used is described in detail.

Transmission Electron Microscopy of Single Wall Carbon Nanotube/Polymer Nanocomposites: A First-Principles Study

NASA Technical Reports Server (NTRS)

Sola, Francisco; Xia, Zhenhai; Lebrion-Colon, Marisabel; Meador, Michael A.

2012-01-01

The physics of HRTEM image formation and electron diffraction of SWCNT in a polymer matrix were investigated theoretically on the basis of the multislice method, and the optics of a FEG Super TWIN Philips CM 200 TEM operated at 80 kV. The effect of nanocomposite thickness on both image contrast and typical electron diffraction reflections of nanofillers were explored. The implications of the results on the experimental applicability to study dispersion, chirality and diameter of nanofillers are discussed.

Thermal behavior of polyhalite: a high-temperature synchrotron XRD study

DOE PAGES

Xu, Hongwu; Guo, Xiaofeng; Bai, Jianming

2016-09-17

As an accessory mineral in marine evaporites, polyhalite, K 2MgCa 2(SO 4) 4·2H 2O, coexists with halite (NaCl) in salt formations, which have been considered as potential repositories for permanent storage of high-level nuclear wastes. However, because of the heat generated by radioactive decays in the wastes, polyhalite may dehydrate, and the released water will dissolve its neighboring salt, potentially affecting the repository integrity. Thus, studying the thermal behavior of polyhalite is important. In this paper, a polyhalite sample containing a small amount of halite was collected from the Salado formation at the WIPP site in Carlsbad, New Mexico. Tomore » determine its thermal behavior, in situ high-temperature synchrotron X-ray diffraction was conducted from room temperature to 1066 K with the sample powders sealed in a silica-glass capillary. At about 506 K, polyhalite started to decompose into water vapor, anhydrite (CaSO 4) and two langbeinite-type phases, K 2Ca x Mg 2-x (SO 4) 3, with different Ca/Mg ratios. XRD peaks of the minor halite disappeared, presumably due to its dissolution by water vapor. With further increasing temperature, the two langbeinite solid solution phases displayed complex variations in crystallinity, composition and their molar ratio and then were combined into the single-phase triple salt, K 2CaMg(SO 4) 3, at ~919 K. Rietveld analyses of the XRD data allowed determination of structural parameters of polyhalite and its decomposed anhydrite and langbeinite phases as a function of temperature. Finally, from the results, the thermal expansion coefficients of these phases have been derived, and the structural mechanisms of their thermal behavior been discussed.« less

(S)TEM analysis of functional transition metal oxides

NASA Astrophysics Data System (ADS)

Chi, Miaofang

Perovskite vanadates (AVO3) form an ideal family to study the structure-property relationships in transition metal oxides because their physical properties can easily be tailored by varying the A-site cations. (S)TEM is an ideal tool for this type of study due to its capacity for simultaneous imaging and chemical analysis. Determination of the oxidation state of vanadium in complex oxides have been carried out by electron energy loss spectroscopy. SrVO3/LaAlO3 is then studied both experimentally and theoretically as a prototype system. Extra electrons have been detected on the interface layer, and further proven to originate mainly from a change in the local bonding configuration of V at the La-O terminated substrate surface. Cr-containing stainless steel deposited with a LaCrO3 thin-film layer is a promising interconnect material of Solid Oxide Fuel Cells (SOFC). Our investigation on its microstructural evolution reveals that the LaCrO 3 thin film plays a role in inhibiting the growth of an oxide layer on the metal surface and thus protects the surface of the stainless steel. Ca-doped LaCoO3 is a promising SOFC cathode material. The domain structures and the oxidation state of Co in Ca-doped LaCoO3, which are directly related to its mechanical properties and electronic conductivity, are investigated by in-situ TEM and EELS. The formation of microcracks is observed during thermal cycles. Ca-doping in LaCoO3 is shown to not only improve the electronic conductivity of the material, but is also likely to strengthen the grain boundaries. The realization of its application in SOFCs depends on depressing the ferroelastisity to reduce strain formation during thermal cycles. The application of the (S)TEM techniques used for studying the perovskite systems are further extended to other compounds containing transition metal elements. The refractory minerals from Comet 81 P/Wild-2 are studied to investigate the formation of the early solar system. A relatively high Ti3+/Ti 4

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

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

Catalyst-layer ionomer imaging of fuel cells

DOE PAGES

Guetaz, Laure; Lopez-Haro, M.; Escribano, S.; ...

2015-09-14

Investigation of membrane/electrode assembly (MEA) microstructure has become an essential step to optimize the MEA components and manufacturing processes or to study the MEA degradation. For these investigations, transmission electron microscopy (TEM) is a tool of choice as it provides direct imaging of the different components. TEM is then widely used for analyzing the catalyst nanoparticles and their carbon support. However, the ionomer inside the electrode is more difficult to be imaged. The difficulties come from the fact that the ionomer forms an ultrathin layer surrounding the carbon particles and in addition, these two components, having similar density, present nomore » difference in contrast. In this paper, we show how the recent progresses in TEM techniques as spherical aberration (Cs) corrected HRTEM, electron tomography and X-EDS elemental mapping provide new possibilities for imaging this ionomer network and consequently to study its degradation.« less

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

Guetaz, Laure; Lopez-Haro, M.; Escribano, S.

Investigation of membrane/electrode assembly (MEA) microstructure has become an essential step to optimize the MEA components and manufacturing processes or to study the MEA degradation. For these investigations, transmission electron microscopy (TEM) is a tool of choice as it provides direct imaging of the different components. TEM is then widely used for analyzing the catalyst nanoparticles and their carbon support. However, the ionomer inside the electrode is more difficult to be imaged. The difficulties come from the fact that the ionomer forms an ultrathin layer surrounding the carbon particles and in addition, these two components, having similar density, present nomore » difference in contrast. In this paper, we show how the recent progresses in TEM techniques as spherical aberration (Cs) corrected HRTEM, electron tomography and X-EDS elemental mapping provide new possibilities for imaging this ionomer network and consequently to study its degradation.« less

TEM characterization of a silorane composite bonded to enamel/dentin.

PubMed

Mine, Atsushi; De Munck, Jan; Van Ende, Annelies; Cardoso, Marcio Vivan; Kuboki, Takuo; Yoshida, Yasuhiro; Van Meerbeek, Bart

2010-06-01

The low-shrinking composite composed of combined siloxane-oxirane technology (Filtek Silorane, 3M ESPE, Seefeld, Germany) required the development of a specific adhesive (Silorane System Adhesive, 3M ESPE), in particular because of the high hydrophobicity of the silorane composite. The purpose of this study was to characterize the interfacial ultra-structure at enamel and dentin using transmission electron microscopy (TEM). Non-demineralized/demineralized 70-90 nm sections were prepared following common TEM specimen processing procedures. TEM revealed a typical twofold build-up of the adhesive resin, resulting in a total adhesive layer thickness of 10-20 microm. At bur-cut enamel, a tight interface without distinct dissolution of hydroxyapatite was observed. At bur-cut dentin, a relatively thin hybrid layer of maximum a few hundreds of nanometer was formed without clear surface demineralization. No clear resin tags were formed. At fractured dentin, the interaction appeared very superficial (100-200 nm). Distinct resin tags were formed due to the absence of smear plugs. Silver-nitrate infiltration showed a varying pattern of both spot- and cluster-like appearance of nano-leakage. Traces of Ag were typically detected along some part of the enamel-adhesive interface and/or between the two adhesive resin layers. Substantially more Ag-infiltration was observed along the dentin-adhesive interface of bur-cut dentin, as compared to that of fractured dentin. The nano-interaction of Silorane System Adhesive should be attributed to its relatively high pH of 2.7. The obtained tight interface at both enamel and dentin indicates that the two-step self-etch adhesive effectively bridged the hydrophilic tooth substrate with the hydrophobic silorane composite. Copyright (c) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Examination of the magnetic hyperthermia and other magnetic properties of CoFe2O4@MgFe2O4 nanoparticles using external field Mössbauer spectroscopy

NASA Astrophysics Data System (ADS)

Park, Jeongho; Choi, Hyunkyung; Kim, Sam Jin; Kim, Chul Sung

2018-05-01

CoFe2O4@MgFe2O4 core/shell nanoparticles were synthesized by high temperature thermal decomposition with seed-mediated growth. The crystal structure and magnetic properties of the nanoparticles were investigated using X-ray diffractometry (XRD), vibrating sample magnetometry (VSM), and Mössbauer spectrometry. The magnetic hyperthermia properties were investigated using a MagneTherm device. Analysis of the XRD patterns showed that CoFe2O4@MgFe2O4 had a cubic spinel crystal structure with space group Fd-3m and a lattice constant (a0) of 8.3686 Å. The size and morphology of the CoFe2O4@MgFe2O4 nanoparticles were confirmed by HR-TEM. The VSM measurements showed that the saturation magnetization (MS) of CoFe2O4@MgFe2O4 was 77.9 emu/g. The self-heating temperature of CoFe2O4@MgFe2O4 was 37.8 °C at 112 kHz and 250 Oe. The CoFe2O4@MgFe2O4 core/shell nanoparticles showed the largest saturation magnetization value, while their magnetic hyperthermia properties were between those of the CoFe2O4 and MgFe2O4 nanoparticles. In order to investigate the hyperfine interactions of CoFe2O4, MgFe2O4, and CoFe2O4@MgFe2O4, we performed Mössbauer spectrometry at various temperatures. In addition, Mössbauer spectrometry of CoFe2O4@MgFe2O4 was performed at 4.2 K with applied fields of 0-4.5 T, and the results were analyzed with sextets for the tetrahedral A-site and sextets for the octahedral B-site.

Synthesis and Structural Characterization of CdFe2O4 Nanostructures

NASA Astrophysics Data System (ADS)

Kalpanadevi, K.; Sinduja, C. R.; Manimekalai, R.

The synthesis of CdFe2O4 nanoparticles has been achieved by a simple thermal decomposition method from the inorganic precursor, [CdFe2(cin)3(N2H4)3], which was obtained by a simple precipitation method from the corresponding metal salts, cinnamic acid and hydrazine hydrate. The precursor was characterized by hydrazine and metal analyses, infrared spectral analysis and thermo gravimetric analysis. On appropriate annealing, [CdFe2(cin)3(N2H4)3] yielded CdFe2O4 nanoparticles. The XRD studies showed that the crystallite size of the particles was 13nm. The results of HRTEM studies also agreed well with those of XRD. SAED pattern of the sample established the polycrystalline nature of the nanoparticles. SEM images displayed a random distribution of grains in the sample.

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.

Coal emissions adverse human health effects associated with ultrafine/nano-particles role and resultant engineering controls.

PubMed

Oliveira, Marcos L S; Navarro, Orlando G; Crissien, Tito J; Tutikian, Bernardo F; da Boit, Kátia; Teixeira, Elba C; Cabello, Juan J; Agudelo-Castañeda, Dayana M; Silva, Luis F O

2017-10-01

There are multiple elements which enable coal geochemistry: (1) boiler and pollution control system design parameters, (2) temperature of flue gas at collection point, (3) feed coal and also other fuels like petroleum coke, tires and biomass geochemistry and (4) fuel feed particle size distribution homogeneity distribution, maintenance of pulverisers, etc. Even though there is a large number of hazardous element pollutants in the coal-processing industry, investigations on micrometer and nanometer-sized particles including their aqueous colloids formation reactions and their behaviour entering the environment are relatively few in numbers. X-ray diffraction (XRD), High Resolution-Transmission Electron microscopy (HR-TEM)/ (Energy Dispersive Spectroscopy) EDS/ (selected-area diffraction pattern) SAED, Field Emission-Scanning Electron Microscopy (FE-SEM)/EDS and granulometric distribution analysis were used as an integrated characterization techniques tool box to determine both geochemistry and nanomineralogy for coal fly ashes (CFAs) from Brazil´s largest coal power plant. Ultrafine/nano-particles size distribution from coal combustion emissions was estimated during the tests. In addition the iron and silicon content was determined as 54.6% of the total 390 different particles observed by electron bean, results aimed that these two particles represent major minerals in the environment particles normally. These data may help in future investigations to asses human health actions related with nano-particles. Copyright © 2017 Elsevier Inc. All rights reserved.

Efficient removal of atrazine from aqueous solutions using magnetic Saccharomyces cerevisiae bionanomaterial.

PubMed

Wu, Xin; He, Huijun; Yang, William L; Yu, Jiaping; Yang, Chunping

2018-06-17

A novel bionanomaterial comprising Saccharomyces cerevisiae (S. cerevisiae) and Fe 3 O 4 nanoparticles encapsulated in a sodium alginate-polyvinyl alcohol (SA-PVA) matrix was synthesized for the efficient removal of atrazine from aqueous solutions. The effects of the operating parameters, nitrogen source, and glucose and Fe 3+ contents on atrazine removal were investigated, and the intermediates were detected by gas chromatography-mass spectrometry (GC-MS). In addition, the synthesized Fe 3 O 4 particles were characterized by XRD, EDX, HR-TEM, FTIR, and hysteresis loops, and the bionanomaterial was characterized by SEM. The results showed that the maximum removal efficiency of 100% was achieved at 28 °C, a pH of 7.0, and 150 rpm with an initial atrazine concentration of 2.0 mg L -1 and that the removal efficiency was still higher than 95.53% even when the initial atrazine concentration was 50 mg L -1 . Biodegradation was demonstrated to be the dominant removal mechanism for atrazine because atrazine was consumed as the sole carbon source for S. cerevisiae. The results of GC-MS showed that dechlorination, dealkylation, deamination, isomerization, and mineralization occurred in the process of atrazine degradation, and thus, a new degradation pathway was proposed. These results indicated that this bionanomaterial has great potential for the bioremediation of atrazine-contaminated water.

Surface Properties and Photocatalytic Activities of the Colloidal ZnS:Mn Nanocrystals Prepared at Various pH Conditions

PubMed Central

Heo, Jungho; Hwang, Cheong-Soo

2015-01-01

Water-dispersible ZnS:Mn nanocrystals (NC) were synthesized by capping the surface with mercaptoacetic acid (MAA) molecules at three different pH conditions. The obtained ZnS:Mn-MAA NC products were physically and optically characterized by corresponding spectroscopic methods. The UV-Visible absorption spectra and PL emission spectra showed broad peaks at 310 and 590 nm, respectively. The average particle sizes measured from the HR-TEM images were 5 nm, which were also supported by the Debye-Scherrer calculations using the X-ray diffraction (XRD) data. Moreover, the surface charges and the degrees of aggregation of the ZnS:Mn-MAA NCs were determined by electrophoretic and hydrodynamic light scattering methods, indicating formation of agglomerates in water with various sizes (50–440 nm) and different surface charge values accordingly the preparation conditions of the NCs (−7.59 to −24.98 mV). Finally, the relative photocatalytic activities of the ZnS:Mn-MAA NCs were evaluated by measuring the degradation rate of methylene blue (MB) molecule in a pseudo first-order reaction condition under the UV-visible light irradiation. As a result, the ZnS:Mn-MAA NC prepared at the pH 7 showed the best photo-degradation efficiency of the MB molecule with the first-order rate constant (kobs) of 2.0 × 10−3·min−1. PMID:28347105

Deposition of silver nanoparticles on multiwalled carbon nanotubes by chemical reduction process and their antimicrobial effects

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

Haider, Adawiya J., E-mail: adawiyahaider@yahoo.com; Thamir, Amin D.; Ahmed, Duha S.

In this paper, the functionalization of raw-MWCNTs involves oxidation reaction using concentrated acid mixture of HNO{sub 3}:H{sub 2}SO{sub 4} (1:3), via ultrasonic bath (170 W, 50 kHz) to obtain functional groups. Then Ag nanoparticles are decorated the outside over the surface of functionalized MWCNTs using a chemical reduction process resulting in the formation of(Ag/ MWCNTs) hybrid material. The results showed that outer diameter functionalized F-MWCNTs andAg nanoparticles size was about (11-80) nm and (10 to 25) nm, respectively using TEM and HRTEM. The crystallographic structure of MWCNTs using X-ray diffraction (XRD) analysis proved diffraction peaks at 38.1°, 44.3°, 64.7° andmore » 77.4° degrees namely, Ag (111), Ag (200), Ag (220), and Ag (311) of the face-centered cubic lattice of Ag, respectively, excepting the peak at 2θ =25.6°, which correspond to the (0 0 2) reflection of the MWNTs are corresponding to Ag/MWNTs. The antimicrobial activities of Ag/MWCNTs hybrid using plate count method showed that decreasing a large number of bacteria colonies of E. coli and S. aureu with increasing the hybrid concentrations after incubation for 24 h in shaker incubator with percentage of inhibition approaching 100%.« less

Electrical and morphological properties of magnetocaloric nano ZnNi ferrite

NASA Astrophysics Data System (ADS)

Hemeda, O. M.; Mostafa, Nasser Y.; Abd Elkader, Omar H.; Hemeda, D. M.; Tawfik, A.; Mostafa, M.

2015-11-01

A series of Zn1-xNixFe2O4 nano ferrite (with x=0, 0.2, 0.4, 0.6, 0.8, and 1) compositions were synthesized using the combustion technique. The powder samples were characterized by XRD. The X-ray analysis showed that the samples were single phase spinel cubic structure. The AC resistivity decreases by increasing the frequency from 1 kHz to 10 kHz. As the frequency of the applied field increases the hopping of charge carrier also increase, thereby decreasing the resistivity. A shift in dielectric maximum is observed toward higher temperature with increasing the Ni content from 536 K to 560 K at 1 kHz. The HRTEM (high resolution TEM) images of four compositions have lattice spacing which confirms the crystalline nature of the samples. The surface morphology SEM of the sample consists of some grains with relatively homogenies distribution with an average size varying from 0.85 to 0.92 μm. The values for entropy change in this work are still small but are significally higher than the values that have been reported for iron oxide nanoparticle. The magnetic entropy change was calculated from measurements of M (H, T) where H is the magnetic field and T is the temperature. The maximum value of entropy change (ΔS) obtained near Curie temperature which makes these material candidates for magnetocaloric applications.

Microenvironment effects in electrocatalysis: ionic-liquid-like coating on carbon nanotubes enhances the Pd-electrocatalytic alcohol oxidation.

PubMed

Li, Shuwen; Dong, Zhengping; Yang, Honglei; Guo, Shujing; Gou, Galian; Ren, Ren; Zhu, Zhejun; Jin, Jun; Ma, Jiantai

2013-02-11

A new catalyst consisting of ionic liquid (IL)-functionalized carbon nanotubes (CNTs) obtained through 1,3-dipolar cycloaddition support-enhanced electrocatalytic Pd nanoparticles (Pd@IL(Cl(-))-CNTs) was successfully fabricated and applied in direct ethanol alkaline fuel cells. The morphology, structure, component and stability of Pd@IL(Cl(-))-CNTs were systematic characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Raman spectra, thermogravimetric analysis (TGA) and X-ray diffraction (XRD). The new catalyst exhibited higher electrocatalytic activity, better tolerance and electrochemical stability than the Pd nanoparticles (NPs) immobilized on CNTs (Pd@CNTs), which was ascribed to the effects of the IL, larger electrochemically active surface area (ECSA), and greater processing performance. Cyclic voltammograms (CVs) at various scan rates illustrated that the oxidation behaviors of ethanol at all electrodes were controlled by diffusion processes. The investigation of the different counteranions demonstrated that the performance of the IL-CNTs hybrid material was profoundly influenced by the subtly varied structures of the IL moiety. All the results indicated that the Pd@IL(Cl(-))-CNTs catalyst is an efficient anode catalyst, which has potential applications in direct ethanol fuel cells and the strategy of IL functionalization of CNTs could be available to prepare other carbonaceous carrier supports to enhance the dispersivity, stability, and catalytic performance of metal NPs as well. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Highly active carbon supported ternary PdSnPtx (x=0.1-0.7) catalysts for ethanol electro-oxidation in alkaline and acid media.

PubMed

Wang, Xiaoguang; Zhu, Fuchun; He, Yongwei; Wang, Mei; Zhang, Zhonghua; Ma, Zizai; Li, Ruixue

2016-04-15

A series of trimetallic PdSnPtx (x=0.1-0.7)/C catalysts with varied Pt content have been synthesized by co-reduction method using NaBH4 as a reducing agent. These catalysts were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV) and chronoamperometry (CA). The electrochemical results show that, after adding a minor amount of Pt dopant, the resultant PdSnPtx/C demonstrated more superior catalytic performance toward ethanol oxidation as compared with that of mono-/bi-metallic Pd/C or PdSn/C in alkaline solution and the PdSnPt0.2/C with optimal molar ratio reached the best. In acid solution, the PdSnPt0.2/C also depicted a superior catalytic activity relative to the commercial Pt/C catalyst. The possible enhanced synergistic effect between Pd, Sn/Sn(O) and Pt in an alloyed state should be responsible for the as-revealed superior ethanol electro-oxidation performance based upon the beneficial electronic effect and bi-functional mechanism. It implies the trimetallic PdSnPt0.2/C with a low Pt content has a promising prospect as anodic electrocatalyst in fields of alkali- and acid-type direct ethanol fuel cells. Copyright © 2016 Elsevier Inc. All rights reserved.

Kinetic and catalytic analysis of mesoporous Co3O4 on the oxidation of morin

NASA Astrophysics Data System (ADS)

Xaba, Morena. S.; Meijboom, Reinout

2017-11-01

Herein we report on the synthesis, characterization and catalytic evaluation of mesoporous cobalt oxides on the oxidation of morin. These mesoporous cobalt oxides were synthesized using an inverse surfactant micelle method, they are connected, well-defined with intra-particle voids. These materials were calcined to different final heating temperatures of 150, 250, 350, 450 and 550 °C, and each mesoporous cobalt oxide catalyst showed unique physical properties and catalytic behavior. Morin oxidation was used as a model reaction in the presence of hydrogen peroxide to evaluate the kinetic and catalytic activity of calcined mesoporous cobalt oxides. The adsorption-desorption equilibrium rate constants of morin and hydrogen peroxide were found to be inversely proportional to the crystallite size of the mesoporous cobalt oxide, and the characteristic path length in which the mass transfer takes place was found to be directly proportional to the crystallite size. The materials were characterized using powder X-Ray Diffraction (p-XRD), N2-sorption isotherms (BET), hydrogen temperature programmed reduction (H2-TPR) and High Resolution-Transmission Electron Microscopy (HR-TEM). UV-vis spectrophotometry was used to monitor the time-resolved absorbance of morin at λmax = 410 nm. The surface reaction in this system is described in terms of the well-established Langmuir-Hinshelwood model. The thermodynamic parameters, EA, ΔH#, ΔS# and ΔG# were calculated and catalyst recycling and reusability is demonstrated.

Manipulating the Temperature of Sulfurization to Synthesize α-NiS Nanosphere Film for Long-Term Preservation of Non-enzymatic Glucose Sensors

NASA Astrophysics Data System (ADS)

Lin, Hsien-Sheng; Shi, Jen-Bin; Peng, Cheng-Ming; Zheng, Bo-Chi; Cheng, Fu-Chou; Lee, Ming-Way; Lee, Hsuan-Wei; Wu, Po-Feng; Liu, Yi-Jui

2018-04-01

In this study, alpha nickel sulfide (α-NiS) nanosphere films have been successfully synthesized by electroplating the nickel nanosheet film on the indium tin oxide (ITO) glass substrate and sulfuring nickel-coated ITO glass substrate. First, we electrodeposited the nickel nanosheet films on the ITO glass substrates which were cut into a 0.5 × 1 cm2 size. Second, the nanosheet nickel films were annealed in vacuum-sealed glass ampoules with sulfur sheets at different annealing temperatures (300, 400, and 500 °C) for 4 h in vacuum-sealed glass ampoules. The α-NiS films were investigated by using X-ray diffraction (XRD), variable vacuum scanning electron microscopy (VVSEM), field emission scanning electron microscopy/energy dispersive spectrometer (FE-SEM/EDS), cyclic voltammogram (CV), electrochemical impedance spectroscopy (EIS), ultraviolet/visible/near-infrared (UV/Visible/NIR) spectra, and photoluminescence (PL) spectra. Many nanospheres were observed on the surface of the α-NiS films at the annealing temperature 400 °C for 4 h. We also used the high-resolution transmission electron microscopy (HR-TEM) for the analysis of the α-NiS nanospheres. We demonstrated that our α-NiS nanosphere film had a linear current response to different glucose concentrations. Additionally, our α-NiS nanosphere films were preserved at room temperature for five and a half years and were still useful for detecting glucose at low concentration.

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

Chen, Zhe; Cao, Minhua, E-mail: caomh@bit.edu.cn; Key Laboratory of Cluster Science, Ministry of Education of China, Department of Chemistry, Beijing Institute of Technology, Beijing 100081

Research highlights: {yields} Novel Bi{sub 2}S{sub 3} hierarchical nanostructures self-assembled by nanorods are successfully synthesized in mild benzyl alcohol system under hydrothermal conditions. {yields} The hierarchical nanostructures exhibit a flower-like shape. {yields} PVP plays an important role for the formation of the hierarchical nanostructures. {yields} Bi{sub 2}S{sub 3} film prepared from the flower-like hierarchical nanostructures exhibits good hydrophobic properties. -- Abstract: Novel Bi{sub 2}S{sub 3} hierarchical nanostructures self-assembled by nanorods are successfully synthesized in mild benzyl alcohol system under hydrothermal conditions. The hierarchical nanostructures exhibit a flower-like shape. X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), scanning electron microscopy (SEM), transmissionmore » electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED) were used to characterize the as-synthesized samples. Meanwhile, the effect of various experimental parameters including the concentration of reagents and reaction time on final product has been investigated. In our experiment, PVP plays an important role for the formation of the hierarchical nanostructures and the possible mechanism was proposed. In addition, Bi{sub 2}S{sub 3} film prepared from the flower-like hierarchical nanostructures exhibits good hydrophobic properties, which may bring nontrivial functionalities and may have some promising applications in the future.« less

Facile green synthesis of fluorescent N-doped carbon dots from Actinidia deliciosa and their catalytic activity and cytotoxicity applications

NASA Astrophysics Data System (ADS)

Arul, Velusamy; Sethuraman, Mathur Gopalakrishnan

2018-04-01

Green synthesis of fluorescent nitrogen doped carbon dots (N-CDs) using Actinidia deliciosa (A. deliciosa) fruit extract as a carbon precursor and aqueous ammonia as a nitrogen dopant is reported here. The synthesized N-CDs were characterized by high resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), UV-Visible spectroscopy (UV-Vis), fluorescence spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The average size of the N-CDs was approximately 3.59 nm and the calculated inter layer distance was found to be 0.21 nm. Raman spectroscopy and SAED pattern revealed the graphitic nature of the synthesized N-CDs. The N-CDs were found to emit intense blue color at 405 nm under the excitation of 315 nm. The doping of nitrogen over the surface of the N-CDs was confirmed by EDS, FT-IR and XPS studies. The synthesized N-CDs were found to exhibit excellent catalytic activity in the reduction of Rhodamine-B using sodium borohydrate. The MTT assay was used to evaluate the cytotoxicity and biocompatibility of N-CDs towards L-929 and MCF-7 cells. From the results obtained, it was found that the N-CDs exhibit low cytotoxicity and superior biocompatibility on both L-929 and MCF-7 cells.

Synthesis of Nanoscale TiO2 and Study of the Effect of Their Crystal Structure on Single Cell Response

PubMed Central

Ismagilov, Z. R.; Shikina, N. V.; Mazurkova, N. A.; Tsikoza, L. T.; Tuzikov, F. V.; Ushakov, V. A.; Ishchenko, A. V.; Rudina, N. A.; Korneev, D. V.; Ryabchikova, E. I.

2012-01-01

To study the effect of nanoscale titanium dioxide (TiO2) on cell responses, we synthesized four modifications of the TiO2 (amorphous, anatase, brookite, and rutile) capable of keeping their physicochemical characteristics in a cell culture medium. The modifications of nanoscale TiO2 were obtained by hydrolysis of TiCl4 and Ti(i-OC3H7)4 (TIP) upon variation of the synthesis conditions; their textural, morphological, structural, and dispersion characteristics were examined by a set of physicochemical methods: XRD, BET, SAXS, DLS, AFM, SEM, and HR-TEM. The effect of synthesis conditions (nature of precursor, pH, temperature, and addition of a complexing agent) on the structural-dispersion properties of TiO2 nanoparticles was studied. The hydrolysis methods providing the preparation of amorphous, anatase, brookite, and rutile modifications of TiO2 nanoparticles 3–5 nm in size were selected. Examination of different forms of TiO2 nanoparticles interaction with MDCK cells by transmission electron microscopy of ultrathin sections revealed different cell responses after treatment with different crystalline modifications and amorphous form of TiO2. The obtained results allowed us to conclude that direct contact of the nanoparticles with cell plasma membrane is the primary and critical step of their interaction and defines a subsequent response of the cell. PMID:22623903

VUV-Photocatalytic Degradation of Bezafibrate by Hydrothermally Synthesized Enhanced {001} Facets TiO2/Ti Film.

PubMed

Sayed, Murtaza; Fu, Pingfeng; Shah, Luqman Ali; Khan, Hasan M; Nisar, Jan; Ismail, M; Zhang, Pengyi

2016-01-14

In the present study, a novel TiO2/Ti film with enhanced {001} facets was synthesized by the hydrothermal technique followed by calcination for studying the removal of bezafibrate (BZF), from an aqueous environment. The synthesized photocatalyst was characterized by FE-SEM, XRD, HR-TEM, and PL-technique. The second-order rate constant of (•)OH with BZF was found to be 5.66 × 10(9) M(-1) s(-1). The steady state [(•)OH] was measured as 1.16 × 10(-11) M, on the basis of oxidation of terephthalic acid. The photocatalytic degradation of BZF followed pseudo-first-order kinetics according to the Langmuir-Hinshelwood model (k1 = 2.617 mg L(-1) min(-1) and k2 = 0.0796 (mg L(-1))(-1)). The effects of concentration and the nature of various additives including inorganic anions (NO3(-), NO2(-), HCO3(-), CO3(2-), Cl(-)) and organic species (fulvic acid) and initial solution pHs (2, 4, 6, 9) on photocatalytic degradation of BZF were investigated. It was found that the nature and concentration of studied additives significantly affected the photocatalytic degradation of BZF. The efficiency of the photocatalytic degradation process in terms of electrical energy per order was estimated. Degradation schemes were proposed on the basis of the identified degradation byproducts by ultraperformance liquid chromatography.

Wavelength-Controlled Photodetector Based on Single CdSSe Nanobelt.

PubMed

Li, Xinmin; Tan, Qiuhong; Feng, Xiaobo; Wang, Qianjin; Liu, Yingkai

2018-06-07

CdSSe nanobelts (NBs) are synthesized by thermal evaporation and then characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), and cathodoluminescence (CL). It is found that the CdSSe NBs have a good morphology and microstructure without defects. CL is sensitive to the defects of CdSSe NBs; thus, we can select single nanobelt with homogeneous CL emission to prepare a detector. Based on it, the photodetector of single CdSSe NB was developed and its photoelectric properties were investigated in detail. It is found that under illumination of white light and at the bias voltage of 1 V, the photocurrent of a single CdSSe nanobelt device is 1.60 × 10 -7  A, the dark current is 1.96 × 10 -10  A, and the ratio of light current to dark one is 816. In addition, the CdSSe nanobelt detector has high photoelectric performance with spectral responsivity of 10.4 AW -1 and external quantum efficiency (EQE) of 19.1%. Its rise/decay time is about 1.62/4.70 ms. This work offers a novel strategy for design wavelength-controlled photodetectors by adjusting their compositions.

Hierarchical Fe3O4@MoS2/Ag3PO4 magnetic nanocomposites: Enhanced and stable photocatalytic performance for water purification under visible light irradiation

NASA Astrophysics Data System (ADS)

Guo, Na; Li, Haiyan; Xu, Xingjian; Yu, Hongwen

2016-12-01

Novel hierarchical Fe3O4@MoS2/Ag3PO4 magnetic nanophotocatalyst with remarkable photocatalytic capability were prepared by simply depositing the Ag3PO4 onto the surface of crumpled Fe3O4@MoS2 nanosphere. The nanocomposites were characterized by XRD, TEM, HRTEM, XPS, BET, and UV-vis DRS. The outcome of the photocatalytic experiments demonstrated that Fe3O4@MoS2/Ag3PO4 with 6 wt% content of Ag3PO4 (FM/A-6%) showed the highest photocatalytic activity upon the degradation Congo red (CR) and Rhodamine B (RhB) under both visible light and simulated sunlight irradiation. In addition, FM/A-6% possessed larger specific surface area (76.56 m2/g) and excellent optical property. The possible Z-scheme charge carriers transfer mechanism for the enhanced photocatalytic properties of the FM/A-6% was also discussed. The Z-scheme charge carriers transfer mechanism established between MoS2 and Ag3PO4 facilitate the charge separation efficiency. Moreover, FM/A-6% can be separated and collected easily by external magnetic field and maintain high activity after five times photoreaction cycles. Given the remarkable photocatalytic performance and high stability of FM/A-6% nanocomposite, it is looking forward to exhibit great potential for applications in water purification.

Electrospinning preparation of one-dimensional Ce3+-doped Li4Ti5O12 sub-microbelts for high-performance lithium-ion batteries

NASA Astrophysics Data System (ADS)

Ji, Xueyang; Li, Dong; Lu, Qifang; Guo, Enyan; Yao, Linbing

2017-12-01

One-dimensional Ce3+-doped Li4Ti5O12 (Li4Ti5- x Ce x O12, x = 0, 0.01, 0.02, and 0.05) sub-microbelts with the width of approximately 500 nm and thickness of about 200 nm have been synthesized via the facile electrospinning method. The structure and morphology of the as-prepared samples are characterized by XRD, TEM, SEM, BET, HRTEM, XPS, and AFM. Importantly, one-dimensional Li4Ti5O12 sub-microbelts can be well preserved with the introduction of Ce3+ ions, while CeO2 impurity is obtained when x is greater than or equal to 0.02. The comparative experiments prove that Ce3+-doped Li4Ti5O12 electrodes exhibit the brilliant electrochemical performance than undoped counterpart. Particularly, the reversible capacity of Li4Ti4.98Ce0.02O12 electrode reaches up to 139.9 mAh g-1 and still maintains at 132.6 mAh g-1 even after 100 cycles under the current rate of 4 C. The superior lithium storage properties of Li4Ti4.98Ce0.02O12 electrode could be attributed to their intrinsic structure advantage as well as enhanced overall conductivity. [Figure not available: see fulltext.

Sol-gel thin-film based mesoporous silica and carbon nanotubes for the determination of dopamine, uric acid and paracetamol in urine.

PubMed

Canevari, Thiago C; Raymundo-Pereira, Paulo A; Landers, Richard; Benvenutti, Edilson V; Machado, Sérgio A S

2013-11-15

This work describes the preparation, characterization and application of a hybrid material composed of disordered mesoporous silica (SiO2) modified with multiwalled carbon nanotubes (MWCNTs), obtained by the sol-gel process using HF as the catalyst. This hybrid material was characterized by N2 adsorption-desorption isotherms, X-ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission microscopy (HR-TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). This new hybrid material was used for the construction of a thin film on a glassy carbon electrode. The modified electrode using this material was designated SiO2/MWCNT/GCE. The electrocatalytic properties of the electrode toward dopamine, uric acid and paracetamol oxidation were studied by differential pulse voltammetry. Well-defined and separated oxidation peaks were observed in phosphate buffer solution at pH 7.0, in contrast with the ill-defined peaks observed with unmodified glassy carbon electrodes. The electrode had high sensitivity for the determination of dopamine, uric acid and paracetamol, with the limits of detection obtained using statistical methods, at 0.014, 0.068 and 0.098 µmol L(-1), respectively. The electrode presented some important advantages, including enhanced physical rigidity, surface renewability by polishing and high sensitivity, allowing the simultaneous determination of these three analytes in a human urine sample. Crown Copyright © 2013 Published by Elsevier B.V. All rights reserved.

Gold nanoparticles mediated coloring of fabrics and leather for antibacterial activity.

PubMed

Velmurugan, Palanivel; Shim, Jaehong; Bang, Keuk-Soo; Oh, Byung-Taek

2016-07-01

Metal gold nanoparticles (AuNPs) were synthesized in situ onto leather, silk and cotton fabrics by three different modules, including green, chemical, and a composite of green and chemical synthesis. Green synthesis was employed using Ginkgo biloba Linn leaf powder extract and HAuCl4 with the fabrics, and chemical synthesis was done with KBH4 and HAuCl4. For composite synthesis, G. biloba extract and KBH4 were used to color and embed AuNPs in the fabrics. The colored fabrics were tested for color coordination and fastness properties. To validate the green synthesis of AuNPs, various instrumental techniques were used including UV-Vis spectrophotometry, HR-TEM, FTIR, and XRD. The chemical and composite methods reduce Au(+) onto leather, silk and cotton fabrics upon heating, and alkaline conditions are required for bonding to fibers; these conditions are not used in the green synthesis protocol. FE-SEM image revealed the binding nature of the AuNPs to the fabrics. The AuNPs that were synthesized in situ on the fabrics were tested against a skin pathogen, Brevibacterium linens using LIVE/DEAD BacLight Bacterial Viability testing. This study represents an initial route for coloring and bio-functionalization of various fabrics with green technologies, and, accordingly, should open new avenues for innovation in the textile and garment sectors. Copyright © 2016 Elsevier B.V. All rights reserved.

XRD and EBSD analysis of anisotropic microstructure development in cold rolled F138 stainless steel

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

De Vincentis, N.S., E-mail: devincentis@ifir-conic

The microstructural characteristics of deformation-processed materials highly influence their mechanical properties. For a complete characterization of a microstructure both local and global information must be gathered, which requires the combination of different analysis techniques. X-ray and Electron Backscatter Diffraction were used in the present paper to characterize the deformation induced in a cold rolled F138 austenitic stainless steel sample. The results obtained using laboratory and synchrotron X-ray sources were compared and combined with EBSD quantitative results, allowing the global and local characterization and orientation dependence of the deformation microstructure. A particular behavior was observed in the XRD data corresponding tomore » the planes with < 220 >∥ ND, likely due to a smaller amount of defects accumulated in the crystals with that particular orientation. EBSD was used to separate the scans data into partitions and to calculate misorientation variables and parameters, showing that this behavior can be attributed to a combination of larger grain sizes, lower local boundary misorientations and dislocation densities for crystals having < 220 >∥ ND. Several conclusions, of general validity for the evaluation of microstructure anisotropy, can be extracted from the results. - Highlights: •Combined XRD and EBSD for studying microstructure gave a superb insight on anisotropic accumulation of defects. •W-H and CMWP methods were applied for checking consistency of results. •XRD showed that a smaller accumulation of defects occurred in crystals with < 220 >∥ ND. •High brilliance X-ray beam allowed to study the anisotropy of defect accumulation.« less

Simulation and analysis of the effect of ungrounded rectangular loop distributed parameters on TEM response

NASA Astrophysics Data System (ADS)

Shi, Zongyang; Liu, Lihua; Xiao, Pan; Geng, Zhi; Liu, Fubo; Fang, Guangyou

2018-02-01

An ungrounded loop in the shallow subsurface transient electromagnetic surveys has been studied as the transmission line model for early turn-off stage, which can accurately explicate the early turn-off current waveform inconsistency along the loop. In this paper, the Gauss-Legendre numerical integration method is proposed for the first time to simulate and analyze the transient electromagnetic (TEM) response considering the different early turn-off current waveforms along the loop. During the simulation, these integral node positions along the loop are firstly determined by solving these zero points of Legendre polynomial, then the turn-off current of each node position is simulated by using the transfer function of the transmission line. Finally, the total TEM response is calculated by using the Gauss-Legendre integral formula. In addition, the comparison and analysis between the results affected by the distributed parameters and that generated by lumped parameters are presented. It is found that the TEM responses agree well with each other after current is thoroughly switched off, while the transient responses in turn-off stage are completely different. It means that the position dependence of the early turn-off current should be introduced into the forward model during the early response data interpretation of the shallow TEM detection of the ungrounded loop. Furthermore, the TEM response simulations at four geometric symmetry points are made. It shows that early responses of different geometric symmetry points are also inconsistent. The research on the influence of turn-off current position dependence on the early response of geometric symmetry point is of great significance to guide the layout of the survey lines and the transmitter location.

TEM-187, a new extended-spectrum β-lactamase with weak activity in a Proteus mirabilis clinical strain.

PubMed

Corvec, Stéphane; Beyrouthy, Racha; Crémet, Lise; Aubin, Guillaume Ghislain; Robin, Frédéric; Bonnet, Richard; Reynaud, Alain

2013-05-01

A Proteus mirabilis clinical strain (7001324) was isolated from urine sample of a patient hospitalized in a long-term-care facility. PCR and cloning experiments performed with this strain identified a novel TEM-type β-lactamase (TEM-187) differing by four amino acid substitutions (Leu21Phe, Arg164His, Ala184Val, and Thr265Met) from TEM-1. This characterization provides further evidence for the diversity of extended-spectrum β-lactamases (ESBL) produced by P. mirabilis and for their potential spread to other Enterobacteriaceae due to a lack of sensitive detection methods used in daily practice.

Composition and microstructure of MTA and Aureoseal Plus: XRF, EDS, XRD and FESEM evaluation.

PubMed

Cianconi, L; Palopoli, P; Campanella, V; Mancini, M

2016-12-01

The aim of this study was to determine the chemical composition and the phases' microstructure of Aureoseal Plus (OGNA, Italy) and ProRoot MTA (Dentsply Tulsa Dental, USA) and to compare their characteristics. Study Design: Comparing Aureoseal Plus and ProRoot MTA microstructure by means of several analyses type. The chemical analysis of the two cements was assessed following the UNI EN ISO 196-2 norm. X-Ray fluorescence (XRF) was used to determine the element composition. The crystalline structure was analysed quantitatively using x-ray diffraction (XRD). Powders morphology was evaluated using a scanning electron microscope (SEM) with backscattering detectors, and a field emission scanning electron microscope (FESEM). Elemental analysis was performed by energy dispersive x-ray analysis (EDS). The semi-quantitative XRF analysis showed the presence of heavy metal oxides in both cements. The XRD spectra of the two cements reported the presence of dicalcium silicate, tricalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and gypsum. SEM analysis showed that ProRoot MTA powder is less coarse and more homogeneous than Aureoseal. Both powders are formed by particles of different shapes: round, prismatic and oblong. The EDS analysis showed that some ProRoot MTA particles, differently from Aureoseal, contain Ca, Si, Al and Fe. Oblong particles in ProRoot and Aureoseal are rich of bismuth. The strong interest in developing new Portland cement-based endodontic sealers will create materials with increased handling characteristics and physicochemical properties. A thorough investigation on two cement powders was carried out by using XRF, XRD, SEM and EDS analysis. To date there was a lack of studies on Aureoseal Plus. This cement is similar in composition to ProRoot MTA. Despite that it has distinctive elements that could improve its characteristics, resulting in a good alternative to MTA.

In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

PubMed

Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

2017-06-12

The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

Synthesis of nano-sized ZnO particles by co-precipitation method with variation of heating time

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

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

Zinc oxide powders have been synthesized by a co-precipitation method at low temperature (85 °C), using zinc acetate dihydrate, ammonia, hydrochloric acid solutions as the reactants. A number of process parameters such as reaction temperature, solution basicity or pH and heating time are the main factors affecting the morphology and physical properties of the ZnO nanostructures. In this work the effect of heating time on the morphology and particles size were studied. The as-synthesized ZnO powders were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The samples were also analyzed using Fourier transform infrared (FTIR). Rietveld refinementmore » of XRD data confirms that ZnO crystallizes in the hexagonal wurtzite structure with high degree of purity and the (101) plane predominant. The XRD results show that the average crystallite sizes were about 66, 27 and 12 nm for 3, 4 and 5 h of heating times, respectively. The XRD analysis indicated that a fraction of nano-sized ZnO powders were in the form of aggregates, which was also verified by TEM image. The TEM photograph demonstrated that the nano-sized ZnO particles were a pseudo-spherical shape.« less

Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size

Treesearch

Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill

2017-01-01

Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...

NiCo2S4 nanorod embedded rGO sheets as electrodes for supercapacitor

NASA Astrophysics Data System (ADS)

Sarkar, Aatreyee; Bera, Supriya; Chakraborty, Amit Kumar

2018-04-01

We report the synthesis of a hybrid nanostructure based on NiCo2S4 and reduced graphene oxide (rGO) following a facile hydrothermal method. X-ray diffraction (XRD), and electron microscopy (FESEM and HRTEM) analyses showed rod-like NiCo2S4 nanostructures embedded in rGO sheets. The electrochemical analysis of the synthesized nanohybrid using cyclic voltammetry (CV) and galvanostatic charge discharge (GCD) revealed specific capacitance of 410 F/gm indicating its suitability as a good electrode material for supercapacitor.

New constraints on deformation processes in serpentinite from sub-micron Raman Spectroscopy and TEM

NASA Astrophysics Data System (ADS)

Smith, S. A. F.; Tarling, M.; Rooney, J. S.; Gordon, K. C.; Viti, C.

2017-12-01

Extensive work has been performed to characterize the mineralogical and mechanical properties of the various serpentine minerals (i.e. antigorite, lizardite, chrysotile, polyhedral and polygonal serpentine). However, correct identification of serpentine minerals is often difficult or impossible using conventional analytical techniques such as optical- and SEM-based microscopy, X-ray diffraction and infrared spectroscopy. Transmission Electron Microscopy (TEM) is the best analytical technique to identify the serpentine minerals, but TEM requires complex sample preparation and typically results in very small analysis areas. Sub-micron confocal Raman spectroscopy mapping of polished thin sections provides a quick and relatively inexpensive way of unambiguously distinguishing the main serpentine minerals within their in-situ microstructural context. The combination of high spatial resolution (with a diffraction-limited system, 366 nm), large-area coverage (up to hundreds of microns in each dimension) and ability to map directly on thin sections allows intricate fault rock textures to be imaged at a sample-scale, which can then form the target of more focused TEM work. The potential of sub-micron Raman Spectroscopy + TEM is illustrated by examining sub-micron-scale mineral intergrowths and deformation textures in scaly serpentinites (e.g. dissolution seams, mineral growth in pressure shadows), serpentinite crack-seal veins and polished fault slip surfaces from a serpentinite-bearing mélange in New Zealand. The microstructural information provided by these techniques has yielded new insights into coseismic dehydration and amorphization processes and the interplay between creep and localised rupture in serpentinite shear zones.

A novel functional domain of Cdc15 kinase is required for its interaction with Tem1 GTPase in Saccharomyces cerevisiae.

PubMed Central

Asakawa, K; Yoshida, S; Otake, F; Toh-e, A

2001-01-01

Exit from mitosis requires the inactivation of cyclin-dependent kinase (CDK) activity. In the budding yeast Saccharomyces cerevisiae, a number of gene products have been identified as components of the signal transduction network regulating inactivation of CDK (called the MEN, for the mitotic exit network). Cdc15, one of such components of the MEN, is an essential protein kinase. By the two-hybrid screening, we identified Cdc15 as a binding protein of Tem1 GTPase, another essential regulator of the MEN. Coprecipitation experiments revealed that Tem1 binds to Cdc15 in vivo. By deletion analysis, we found that the Tem1-binding domain resides near the conserved kinase domain of Cdc15. The cdc15-LF mutation, which was introduced into the Tem1-binding domain, reduced the interaction with Cdc15 and Tem1 and caused temperature-sensitive growth.The kinase activity of Cdc15 was not so much affected by the cdc15-LF mutation. However, Cdc15-LF failed to localize to the SPB at the restrictive temperature. Our data show that the interaction with Tem1 is important for the function of Cdc15 and that Cdc15 and Tem1 function in a complex to direct the exit from mitosis. PMID:11290702

High temperature XRD of Cu2GeSe3

NASA Astrophysics Data System (ADS)

Premkumar D., S.; Chetty, Raju; Malar, P.; Mallik, Ramesh Chandra

2015-06-01

The Cu2GeSe3 is prepared by solid state synthesis method. The high temperature XRD has been done at different temperature from 30 °C to 450 °C. The reitveld refinement confirms Cu2GeSe3 phase and orthorhombic crystal structure. The lattice constants are increasing with increase in the temperature and their rate of increase with respect to temperature are used for finding the thermal expansion coefficient. The calculation of the linear and volume coefficient of thermal expansion is done from 30 °C to 400 °C. Decrease in the values of linear expansion coefficients with temperature are observed along a and c axis. Since thermal expansion coefficient is the consequence of the distortion of atoms in the lattice; this can be further used to find the minimum lattice thermal conductivity at given temperature.

Photocatalytic activity of binary metal oxide nanocomposites of CeO2/CdO nanospheres: Investigation of optical and antimicrobial activity.

PubMed

Magdalane, C Maria; Kaviyarasu, K; Vijaya, J Judith; Siddhardha, Busi; Jeyaraj, B

2016-10-01

We report the synthesis of high quality CeO2-CdO binary metal oxide nanocomposites were synthesized by a simple chemical precipitation and hydrothermal method. Cerium nitrate and cadmium nitrate were used as precursors. Composition, structure and morphology of the nanocomposites were analyzed by X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). XRD pattern proves that the final product has cubic phase and the particle size diameter of the nanocomposites are 27nm, XRD results also indicated that the crystalline properties of the nanocomposite were improved without affecting the parent lattice, FESEM analysis indicates that the product is composed of spherical particles in clusters. The morphological and optical properties of CeO2-CdO nanosamples were characterized by HRTEM and DRS spectroscopy. The IR results showed high purity of products and indicated that the nanocomposites are made up of CeO2 and CdO bonds. Absorption spectra exhibited an upward shift in characteristic peaks caused by the addition of transition metal oxide, suggesting that crystallinity of both the metal oxide is improved due to specific doping level. TGA plots further confirmed the purity and stability of nanomaterials prepared. Hence the nanocomposite has cubic crystal lattice and form a homogeneous solid structure. From the result, Cd(2+) ions are embedded in the cubic crystal lattice of ceria. The growth rate increases which are ascribed to the cationic doping with a lower valence cation. Ce-Cd binary metal oxide nanocomposites showed antibacterial activity, it showed the better growth inhibition towards p.aeruginosa. Exploit of photodegradation and photocatalytic activity of large scale synthesis of CeO2-CdO binary metal oxide nanocomposites was reported. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of chitosan coating on the structural and magnetic properties of MnFe2O4 and Mn0.5Co0.5Fe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Mdlalose, W. B.; Mokhosi, S. R.; Dlamini, S.; Moyo, T.; Singh, M.

2018-05-01

We report the influence of polymer coatings on structural and magnetic properties of MnFe2O4 and Mn0.5Co0.5Fe2O4 nanoferrites synthesized by glycol thermal technique and then coated with chitosan viz. CHI-MnFe2O4 and CHI-Mn0.5Co0.5Fe2O4. The compounds were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), high-resolution scanning electron microscopy (HRSEM), Mössbauer spectroscopy and magnetization measurements. The powder XRD patterns of naked nanoferrites confirmed single-phase spinel cubic structure with an average crystallite size of 13 nm, while the coated samples exhibited an average particle size of 15 nm. We observed a reduction in lattice parameters with coating. HRTEM results correlated well with XRD results. 57Fe Mössbauer spectra showed ordered magnetic spin states in both nanoferrites. This study shows that coatings have significant effects on the structural and magnetic properties of Mn-nanoferrites. Magnetization studies performed at room temperature in fields up to 14 kOe revealed the superparamagnetic nature of both naked and coated nanoparticles with spontaneous magnetizations at room temperature of 49.2 emu/g for MnFe2O4, 23.6 emu/g for coated CHI-MnFe2O4 nanoparticles, 63.2 emu/g for Mn0.5Co0.5Fe2O4 and 33.2 emu/g for coated CHI-Mn0.5Co0.5Fe2O4 nanoparticles. We observed reduction in coercive fields due to coating. Overall, chitosan-coated manganese and manganese-cobalt nanoferrites present as suitable candidates for biomedical applications owing to physicochemical, and magnetic properties exhibited.

Guazuma ulmifolia bark-synthesized Ag, Au and Ag/Au alloy nanoparticles: Photocatalytic potential, DNA/protein interactions, anticancer activity and toxicity against 14 species of microbial pathogens.

PubMed

Karthika, Viswanathan; Arumugam, Ayyakannu; Gopinath, Kasi; Kaleeswarran, Periyannan; Govindarajan, Marimuthu; Alharbi, Naiyf S; Kadaikunnan, Shine; Khaled, Jamal M; Benelli, Giovanni

2017-02-01

In the present study, we focused on a quick and green method to fabricate Ag, Au and Ag/Au alloy nanoparticles (NPs) using the bark extract of Guazuma ulmifolia L. Green synthesized metal NPs were characterized using different techniques, including UV-Vis spectroscopy, FT-IR, XRD, AFM and HR-TEM analyses. The production of Ag, Au and Ag/Au alloy NPs was observed monitoring color change from colorless to brown, followed by pink and dark brown, as confirmed by UV-Vis spectroscopy characteristic peaks at 436, 522 and 510nm, respectively. TEM shed light on the spherical shapes of NPs with size ranges of 10-15, 20-25 and 10-20nm. Biosynthesized NPs showed good catalytic activity reducing two organic dyes, 4-nitrophenol (4-NP) and Congo red (CR). UV-vis spectroscopy, fluorescence, circular dichroism spectroscopy and viscosity analyses were used to investigate the NP binding with calf thymus DNA. The binding constant of NPs with DNA calculated in UV-Vis absorption studies were 1.18×10 4 , 1.83×10 4 and 2.91×10 4 M -1 , respectively, indicating that NPs were able to bind DNA with variable binding affinity: Ag/Au alloy NPs>Ag NPs>Au NPs. Ag/Au alloy NPs also showed binding activity to bovine serum albumin (BSA) over the other NPs. Ag and Ag/Au alloy NPs exhibited good antimicrobial activity on 14 species of microbial pathogens. In addition, the cytotoxic effects of Ag/Au alloy NPs were studied on human cervical cancer cells (HeLa) using MTT assay. Overall, our work showed the promising potential of bark-synthesized Ag and Ag/Au alloy NPs as cheap sources to develop novel and safer photocatalytic, antimicrobial and anticancer agents. Copyright © 2017. Published by Elsevier B.V.

NaYF{sub 4}:Er,Yb/Bi{sub 2}MoO{sub 6} core/shell nanocomposite: A highly efficient visible-light-driven photocatalyst utilizing upconversion

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

Sun, Yuanyuan; Wang, Wenzhong, E-mail: wzwang@mail.sic.ac.cn; Sun, Songmei

2014-04-01

Highlights: • Design and synthesis of NaYF{sub 4}:Er,Yb/Bi{sub 2}MoO{sub 6} based on upconversion. • NaYF{sub 4}:Er,Yb/Bi{sub 2}MoO{sub 6} nanocomposite was prepared for the first time. • Core–shell structure benefits the properties. • Upconversion contributed to the enhanced photocatalytic activity. • Helps to understand the functionality of new type photocatalysts. - Abstract: NaYF{sub 4}:Er,Yb/Bi{sub 2}MoO{sub 6} core/shell nanocomposite was designed and prepared for the first time based on upconversion. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HRTEM), energy dispersive X-ray spectroscopy (EDS) and diffuse reflectance spectra (DRS). The results revealed that the as-synthesizedmore » NaYF{sub 4}:Er,Yb/Bi{sub 2}MoO{sub 6} consisted of spheres with a core diameter of about 26 nm and a shell diameter of around 6 nm. The core was upconversion illuminant NaYF{sub 4}:Er,Yb and the shell was Bi{sub 2}MoO{sub 6} around the core, which was confirmed by EDS. The NaYF{sub 4}:Er,Yb/Bi{sub 2}MoO{sub 6} exhibited higher photocatalytic activity for the photodecomposition of Rhodamine B (RhB) under the irradiation of Xe lamp and green light emitting diode (g-LED). The mechanism of the high photocatalytic activity was discussed by photoluminescence spectra (PL), which is mainly attributed to upconversion of NaYF{sub 4}:Er,Yb in the NaYF{sub 4}:Er,Yb/Bi{sub 2}MoO{sub 6} nanocomposite and the core–shell structure.« less

Chemical synthesis and characterization of hollow dopamine coated, pentagonal and flower shaped magnetic iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Riasat, Rabia; Kaynat, Sumbal

2018-04-01

Iron oxide nanoparticles have gained attention recently in the field of nanoscience and technology due to their unique physicochemical properties. We hereby chemically synthesized novel pentagonal flower shaped iron oxide nanoparticles by thermal decomposition of iron penta-carbonyl in a two way annealing process. Controlled oxidation by acid etching was performed for these nanoparticles. At first 13 nm core shell nanoparticles of iron oxide (Fe/Fe3O4) were synthesized at 120°C annealing temperature that act as template material. The core shell nanoparticles then converted into porous hollow core shell nanoparticles (PH Fe/ Fe3O4) in a two way annealing process of heating, first at 100°C then at 250°C and heating rate of 5°C was kept constant throughout the reaction time. X-Ray diffraction (XRD) was done for the phase confirmation of as synthesized nanoparticles. Transmission electron microscopy (TEM) and higher resolution transmission electron microscopy (HRTEM) clearly shows the flower like nanoparticles that are approx. 16 nm-18 nm in size having the 4-5 nm core of Fe and 1-2 nm of the pores in the shell while the cavity between the shell and core is about 2 nm and the shell is 4-5 nm in diameter according to the TEM micrographs. The as prepared nanoparticles were then surface functionalized by dopamine polymer to make them water dispersible. Fourier transform Infrared spectroscopy confirmed the dopamine coating on the nanoparticles and the magnetic saturation of 38 emu/g of nanoparticles was analyzed by vibrating sample magnetometer (VSM). Magnetic saturation persists in the dopamine coated nanoparticles. These nanoparticles were surface functionalized with dopamine and show dispersity in the aqueous media and can further be exploited in many nano-biotechnological applications including target specific therapeutic applications for several diseases.