Synthesis and Microstructural Analysis of Benzylthiol-functionalized Au Nanocrystals

2006 ◽  
Vol 959 ◽  
Author(s):  
Floriana Vitale ◽  
Luciana Mirenghi ◽  
Emanuela Piscopiello ◽  
Maria Lucia Protopapa ◽  
Leander Tapfer ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Au Nanoparticles ◽  
Microstructural Analysis ◽  
High Resolution Electron Microscopy ◽  
Phase Method ◽  
Two Phase ◽  
X Ray ◽  
Resolution Electron ◽  
Phase Liquid ◽  
Ir Emission

ABSTRACTWe report on the synthesis and microstructural and microanalytical analysis of dodecanethiol and benzylthiol-stabilized Au nanoparticles (diameter range between 2 nm and 10 nm). Stable functionalized gold nanoparticles were synthesized by using two different routes: a two-phase liquid-liquid method and a one-phase method. The size, strain, shape and crystalline structure of the nanocrystals were determined by a full-pattern X-ray powder diffraction analysis and high-resolution electron microscopy. The chemical environment of the Au nanocrystals and their interaction with the thiols was investigated by X-ray photoelectron spectroscopy. Photoluminescence spectroscopy measurements show a characteristic IR emission at λ=960 nm of small sized Au nanocrystals (∼3 nm). The origin of this IR emission line seems to be correlated to the Au-S bonding and the size of the nanoparticles.

scholarly journals Protected Gold Nanoparticles with Thioethers and Amines As Surrogate Ligands

2013 ◽  
Vol 2013 ◽  
pp. 1-4 ◽  
Author(s):  
M. Rafiq H. Siddiqui
Keyword(s):  
Gold Nanoparticles ◽  
Variable Temperature ◽  
Size Control ◽  
Analytical Techniques ◽  
High Resolution Electron Microscopy ◽  
Phase Method ◽  
Two Phase ◽  
H Nmr ◽  
Resolution Electron ◽  
Vis Spectroscopy

Dodecyl sulfide, dodecyl amine, and hexylamine were shown to act as surrogate ligands (L) via metastable gold nanoparticles. By collating analytical and spectroscopic data obtained simultaneously, empirical formula Au24L was assigned. These impurity-free nanoparticles obtained in near quantitative yields showing exceptional gold assays (up to 98%Au) were prepared by a modification of the two-phase method. Replacement reactions on the Au24L showed that Au:L ratios may be increased (up to Au55:L (L= (H25C12)2S)) or decreased (Au12:L (L= H2NC12H25and H2NC6H13)) as desired. This work encompassing the role of analytical techniques used, that is, elemental analysis, variable temperature1H NMR, FAB mass spectrometry, UV-Vis spectroscopy, thin film X-ray diffraction, and high-resolution electron microscopy (HREM) has implications in the study of size control, purity, stability, and metal assays of gold nanoparticles.

Silica-protein composite layers of the giant basal spicules from Monorhaphis: Basis for their mechanical stability

2010 ◽  
Vol 82 (1) ◽  
pp. 175-192 ◽  
Author(s):  
Xiaohong Wang ◽  
Ute Schloßmacher ◽  
Klaus Peter Jochum ◽  
Lu Gan ◽  
Brigitte Stoll ◽  
...  
Keyword(s):  
Mechanical Stability ◽  
High Resolution Electron Microscopy ◽  
Hybrid Fibers ◽  
Protein Scaffold ◽  
X Ray ◽  
Composite Layers ◽  
Resolution Electron ◽  
Ft Ir ◽  
Ir Emission ◽  
Solid Glass

The hexactinellid sponge Monorhaphis chuni possesses with its giant basal spicules the largest biosilica structure on Earth. The approximately 8.5-mm-thick spicules are composed of up to 800 lamellae. By application of high-resolution electron microscopy (HR-SEM), it is shown that within the siliceous lamellae a proteinaceous scaffold exists which is composed of one protein of a size of 27 kDa. Analyses with Fourier transform infrared (FT-IR) emission and energy-dispersive X-ray (EDX) spectroscopy support this localization of the protein. No evidence for the presence of protein on the surfaces of the lamellae could be obtained. Heating the giant basal spicule to 600 °C destroys and eliminates the protein scaffold. At a temperature of 1600 °C, the lamellae fuse to solid glass via a nonstructured, foamed-up molten transition state. Elevation of the temperature to 2700 °C results in the formation of silica drops (Euplectella aspergillum). After the elimination of the protein scaffold from the silica lamellae, the spicules lose their mechanical characteristics of the original hydrated silica/protein composite to be flexible and simultaneously stiff and tough. The data presented here are expected to contribute to technologies suited to fabricate novel organic/inorganic (silica) hybrid fibers.

scholarly journals Fast and Straightforward Synthesis of Luminescent Titanium(IV) Dioxide Quantum Dots

2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Václav Štengl ◽  
Jiří Henych ◽  
Martin Šťastný ◽  
Martin Kormunda
Keyword(s):  
Quantum Dots ◽  
Photoelectron Spectroscopy ◽  
High Resolution Electron Microscopy ◽  
Fast Method ◽  
X Ray ◽  
Force Microscopy ◽  
Selected Area Electron Diffraction ◽  
Atomic Force ◽  
Resolution Electron ◽  
Close Range

The nucleus of titania was prepared by reaction of solution titanium oxosulphate with hydrazine hydrate. These titania nuclei were used for titania quantum dots synthesis by a simple and fast method. The prepared titanium(IV) dioxide quantum dots were characterized by measurement of X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), high-resolution electron microscopy (HRTEM), and selected area electron diffraction (SAED). The optical properties were determined by photoluminescence (PL) spectra. The prepared titanium(IV) dioxide quantum dots have the narrow range of UV excitation (365–400 nm) and also a close range of emission maxima (450–500 nm).

New ways of characterizing layered silicates and their intercalates

1984 ◽  
Vol 311 (1517) ◽  
pp. 271-285 ◽  
Keyword(s):  
Photoelectron Spectroscopy ◽  
High Resolution Electron Microscopy ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
X Ray ◽  
Photoelectron Diffraction ◽  
Organic Species ◽  
New Methods ◽  
Resolution Electron ◽  
Angle Spinning

Four new methods of probing the atomic and microstructural characteristics of the clay minerals are described: solid-state, magic-angle-spinning 27 Al and 29 Si n.m.r. (along with 18 C n.m.r. of mobile, intercalated organic species); X-ray induced photoelectron studies encompassing photoelectron diffraction as a complement to conventional photoelectron spectroscopy; high-resolution electron microscopy either alone or in association with electron-stimulated X-ray emission microanalysis; and neutron scattering techniques. In reviewing the principles, scope and application of these methods specific case histories are selected from representative minerals belonging to the serpentines, kandites, smectites, micas, vermiculites, chloritoids, zeolites and intergrowths of these with one another or with other silicate minerals. Emphasis is placed on problems not readily amenable to solution by traditional, X-ray based procedures.

Electron microscopy of rabbit FC crystals

1983 ◽  
Vol 41 ◽  
pp. 730-731
Author(s):  
Robert A. Grant ◽  
Laura L. Degn ◽  
Wah Chiu ◽  
John Robinson
Keyword(s):  
Electron Microscopy ◽  
High Resolution ◽  
High Resolution Electron Microscopy ◽  
Molecular Replacement ◽  
X Ray ◽  
X Ray Crystallography ◽  
Resolution Electron ◽  
Replacement Technique ◽  
Hydrated Crystal ◽  
Molecular Structure Analysis

Proteolytic digestion of the immunoglobulin IgG with papain cleaves the molecule into an antigen binding fragment, Fab, and a compliment binding fragment, Fc. Structures of intact immunoglobulin, Fab and Fc from various sources have been solved by X-ray crystallography. Rabbit Fc can be crystallized as thin platelets suitable for high resolution electron microscopy. The structure of rabbit Fc can be expected to be similar to the known structure of human Fc, making it an ideal specimen for comparing the X-ray and electron crystallographic techniques and for the application of the molecular replacement technique to electron crystallography. Thin protein crystals embedded in ice diffract to high resolution. A low resolution image of a frozen, hydrated crystal can be expected to have a better contrast than a glucose embedded crystal due to the larger density difference between protein and ice compared to protein and glucose. For these reasons we are using an ice embedding technique to prepare the rabbit Fc crystals for molecular structure analysis by electron microscopy.

Nano-probe x-ray analysis and high-resolution imaging on planar defects in high-pressure synthesized infinite-layer superconductor

1994 ◽  
Vol 52 ◽  
pp. 728-729
Author(s):  
Y. Y. Wang ◽  
H. Zhang ◽  
V. P. Dravid ◽  
H. Zhang ◽  
L. D. Marks ◽  
...  
Keyword(s):  
High Pressure ◽  
High Resolution ◽  
Atomic Structure ◽  
Emission Spectra ◽  
High Resolution Electron Microscopy ◽  
Planar Defects ◽  
X Ray ◽  
Infinite Layer ◽  
Resolution Electron ◽  
Resolution Imaging

Azuma et al. observed planar defects in a high pressure synthesized infinitelayer compound (i.e. ACuO2 (A=cation)), which exhibits superconductivity at ~110 K. It was proposed that the defects are cation deficient and that the superconductivity in this material is related to the planar defects. In this report, we present quantitative analysis of the planar defects utilizing nanometer probe xray microanalysis, high resolution electron microscopy, and image simulation to determine the chemical composition and atomic structure of the planar defects. We propose an atomic structure model for the planar defects.Infinite-layer samples with the nominal chemical formula, (Sr1-xCax)yCuO2 (x=0.3; y=0.9,1.0,1.1), were prepared using solid state synthesized low pressure forms of (Sr1-xCax)CuO2 with additions of CuO or (Sr1-xCax)2CuO3, followed by a high pressure treatment.Quantitative x-ray microanalysis, with a 1 nm probe, was performed using a cold field emission gun TEM (Hitachi HF-2000) equipped with an Oxford Pentafet thin-window x-ray detector. The probe was positioned on the planar defects, which has a 0.74 nm width, and x-ray emission spectra from the defects were compared with those obtained from vicinity regions.

Characterisation of planar crystal defects in Y2Fe17Cx (0.6 ≤ x ≤ 1.6) magnetic material by High Resolution Electron Microscopy

1990 ◽  
Vol 48 (4) ◽  
pp. 774-775
Author(s):  
W. Coene ◽  
F. Hakkens ◽  
T.H. Jacobs ◽  
K.H.J. Buschow
Keyword(s):  
Electron Microscopy ◽  
High Resolution ◽  
Permanent Magnets ◽  
Annealing Treatment ◽  
High Resolution Electron Microscopy ◽  
Crystal Defects ◽  
Ordered Structure ◽  
X Ray ◽  
Planar Crystal ◽  
Resolution Electron

Intermetallic compounds of the type RE2Fe17Cx (RE= rare earth element) are promising candidates for permanent magnets. In case of Y2Fe17Cx, the Curie temperature increases from 325 K for x =0 to 550 K for x = 1.6 . X ray and electron diffraction reveal a carbon - induced structural transformation in Y2Fe17Cx from the hexagonal Th2Ni17 - type (x < 0.6 ) to the rhombohedral Th2Zn17 - type ( x ≥ 0.6). Planar crystal defects introduce local sheets of different magnetic anisotropy as compared with the ordered structure, and therefore may have an important impact on the coercivivity mechanism .High resolution electron microscopy ( HREM ) on a Philips CM30 / Super Twin has been used to characterize planar crystal defects in rhombohedral Y2Fe17Cx ( x ≥ 0.6 ). The basal plane stacking sequences are imaged in the [100] - orientation, showing an ABC or ACB sequence of Y - atoms and Fe2 - dumbbells, for both coaxial twin variants, respectively . Compounds resulting from a 3 - week annealing treatment at high temperature ( Ta = 1000 - 1100°C ) contain a high density of planar defects.

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