Determination of reversible hydrogen adsorption site in Ni-nanoparticle-dispersed amorphous silica for hydrogenseparation at high temperature

2010 ◽  
Vol 25 (10) ◽  
pp. 2008-2014 ◽  
Author(s):  
Yumi H. Ikuhara ◽  
Tomohiro Saito ◽  
Yukichi Sasaki ◽  
Seiji Takahashi ◽  
Tsukasa Hirayama

The reversible hydrogen adsorption site in Ni-nanoparticle-dispersed amorphous silica (Si-O) was identified by analyzing the hydrogen adsorption behavior and the microstructure. The total amount of reversibly adsorbed hydrogen was evaluated from the total surface area of Ni and the Ni concentration in the composite. The total surface area of the Ni nanoparticles in each sample powder was calculated from the mean particle size of the Ni nanoparticles in the Si-O matrix using dark field images taken by transmission electron microscopy and high-angle annular dark-field images by scanning transmission electron microscopy. The estimated amount of reversibly adsorbed hydrogen was highly consistent with that obtained experimentally by hydrogen adsorption analysis, which suggested that reversible hydrogen adsorption occurred at the Ni/Si-O interface.

2005 ◽  
Vol 187 (11) ◽  
pp. 3814-3824 ◽  
Author(s):  
Jiamin Tian ◽  
Anthony J. Sinskey ◽  
JoAnne Stubbe

ABSTRACT Wautersia eutropha, formerly known as Ralstonia eutropha, a gram-negative bacterium, accumulates polyhydroxybutyrate (PHB) as insoluble granules inside the cell when nutrients other than carbon are limited. In this paper, we report findings from kinetic studies of granule formation and degradation in W. eutropha H16 obtained using transmission electron microscopy (TEM). In nitrogen-limited growth medium, the phenotype of the cells at the early stages of granule formation was revealed for the first time. At the center of the cells, dark-stained “mediation elements” with small granules attached were observed. These mediation elements are proposed to serve as nucleation sites for granule initiation. TEM images also revealed that when W. eutropha cells were introduced into nitrogen-limited medium from nutrient-rich medium, the cell size increased two- to threefold, and the cells underwent additional volume changes during growth. Unbiased stereology was used to analyze the two-dimensional TEM images, from which the average volume of a W. eutropha H16 cell and the total surface area of granules per cell in nutrient-rich and PHB production media were obtained. These parameters were essential in the calculation of the concentration of proteins involved in PHB formation and utilization and their changes with time. The extent of protein coverage of the granule surface area is presented in the accompanying paper (J. Tian, A. He, A. Lawrence, P. Liu, N. Watson, A. J. Sinskey, and J. Stubbe, J. Bacteriol. 187:3825-3832, 2005).


2020 ◽  
Vol 75 (11) ◽  
pp. 913-919
Author(s):  
Frank Krumeich

AbstractSince the 1970s, high-resolution transmission electron microscopy (HRTEM) is well established as the most appropriate method to explore the structural complexity of niobium tungsten oxides. Today, scanning transmission electron microscopy (STEM) represents an important alternative for performing the structural characterization of such oxides. STEM images recorded with a high-angle annular dark field (HAADF) detector provide not only information about the cation positions but also about the distribution of niobium and tungsten as the intensity is directly correlated to the local scattering potential. The applicability of this method is demonstrated here for the characterization of the real structure of Nb7W10O47.5. This sample contains well-ordered domains of Nb8W9O47 and Nb4W7O31 besides little ordered areas according to HRTEM results. Structural models for Nb4W7O31 and twinning occurring in this phase have been derived from the interpretation of HAADF-STEM images. A remarkable grain boundary between well-ordered domains of Nb4W7O31 and Nb8W9O47 has been found that contains one-dimensionally periodic features. Furthermore, short-range order observed in less ordered areas could be attributed to an intimate intergrowth of small sections of different tetragonal tungsten bronze (TTB) based structures.


2009 ◽  
Vol 24 (8) ◽  
pp. 2596-2604 ◽  
Author(s):  
Sašo Šturm ◽  
Makoto Shiojiri ◽  
Miran Čeh

The microstructure in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics is strongly affected by the formation of Ruddlesden-Popper fault–rich (RP fault) lamellae, which are coherently intergrown with the matrix of the perovskite grains. We studied the structure and chemistry of RP faults by applying quantitative high-resolution transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy analyses. We showed that the Sr2+ and Ca2+ dopant ions form RP faults during the initial stage of sintering. The final microstructure showed preferentially grown RP fault lamellae embedded in the central part of the anisotropic perovskite grains. In contrast, the dopant Ba2+ ions preferably substituted for Sr2+ in the SrTiO3 matrix by forming a BaxSr1−xTiO3 solid solution. The surplus of Sr2+ ions was compensated structurally in the later stages of sintering by the formation of SrO-rich RP faults. The resulting microstructure showed RP fault lamellae located at the surface of equiaxed BaxSr1-xTiO3 perovskite grains.


2017 ◽  
Vol 46 (1) ◽  
pp. 47-61 ◽  
Author(s):  
Uschi M. Graham ◽  
Robert A. Yokel ◽  
Alan K. Dozier ◽  
Lawrence Drummy ◽  
Krishnamurthy Mahalingam ◽  
...  

This is the first utilization of advanced analytical electron microscopy methods, including high-resolution transmission electron microscopy, high-angle annular dark field scanning transmission electron microscopy, electron energy loss spectroscopy, and energy-dispersive X-ray spectroscopy mapping to characterize the organ-specific bioprocessing of a relatively inert nanomaterial (nanoceria). Liver and spleen samples from rats given a single intravenous infusion of nanoceria were obtained after prolonged (90 days) in vivo exposure. These advanced analytical electron microscopy methods were applied to elucidate the organ-specific cellular and subcellular fate of nanoceria after its uptake. Nanoceria is bioprocessed differently in the spleen than in the liver.


1992 ◽  
Vol 7 (8) ◽  
pp. 2225-2229 ◽  
Author(s):  
Z.G. Li ◽  
P.F. Carcia ◽  
P.C. Donohue

The microstructure of LaB6-base thick film resistors was investigated by cross-sectional transmission electron microscopy. The specimens were prepared by a technique that polished them to a thin wedge, thus avoiding ion-milling and permitting imaging over a distance of tens of microns. The resistor microstructure contained a finely divided electrically conductive phase of TaB2 and nonconducting crystals of CaTa4O11, formed during high temperature processing of glass and LaB6 ingredients of the thick film ink. Using higher surface area ingredients virtually suppressed the formation of CaTa4O11 crystals, and the microstructure became more uniform. Resistors made with higher surface area intermediates also had better voltage withstanding properties.


2014 ◽  
Vol 47 (5) ◽  
pp. 1729-1735 ◽  
Author(s):  
Xin Nie ◽  
Yimin Guan ◽  
Dongshan Zhao ◽  
Yu Liu ◽  
Jianian Gui ◽  
...  

The crystallographic orientation relationships (ORs) of precipitated β-Mg2Sn particles in Mg–9.76 wt% Sn alloy aged at 573 K for 5 h, corresponding to its peak hardness, were investigated by advanced transmission electron microscopy (TEM). OR-3 of (110)β//(0001)αand [\overline 111]β//[1\overline 210]αand OR-4 of (110)β//(0001)αand [001]β//[2\overline 1\overline 10]αare the key ORs of β-Mg2Sn particles in the alloy. The proportions of β-Mg2Sn particles exhibiting OR-3 and OR-4 were determined as 75.1 and 24.3%, respectively. Crystallographic factors determined the predominance of OR-3 in the precipitated β-Mg2Sn particles. This mechanism was analyzed by a three-dimensional invariant line model constructed using a transformation matrix in reciprocal space. Models of the interface of precipitated β-Mg2Sn and the α-Mg matrix were constructedviahigh-resolution TEM and atomic resolution high-angle annular dark-field scanning TEM.


Materials ◽  
2021 ◽  
Vol 14 (16) ◽  
pp. 4531
Author(s):  
Maria Meledina ◽  
Geert Watson ◽  
Alexander Meledin ◽  
Pascal Van Der Voort ◽  
Joachim Mayer ◽  
...  

Ru catalyst nanoparticles were encapsulated into the pores of a Cr-based metal-organic framework (MOF)—MIL-101. The obtained material, as well as the non-loaded MIL-101, were investigated down to the atomic scale by annular dark-field scanning transmission electron microscopy using low dose conditions and fast image acquisition. The results directly show that the used wet chemistry loading approach is well-fitted for the accurate embedding of the individual catalyst nanoparticles into the cages of the MIL-101. The MIL-101 host material remains crystalline after the loading procedure, and the encapsulated Ru nanoparticles have a metallic nature. Annular dark field scanning transmission electron microscopy, combined with EDX mapping, is a perfect tool to directly characterize both the embedded nanoparticles and the loaded nanoscale MOFs. The resulting nanostructure of the material is promising because the Ru nanoparticles hosted in the MIL-101 pores are prevented from agglomeration—the stability and lifetime of the catalyst could be improved.


2008 ◽  
Vol 112 (6) ◽  
pp. 1759-1763 ◽  
Author(s):  
Norihiko L. Okamoto ◽  
Bryan W. Reed ◽  
Shareghe Mehraeen ◽  
Apoorva Kulkarni ◽  
David Gene Morgan ◽  
...  

2013 ◽  
Vol 393 ◽  
pp. 146-151 ◽  
Author(s):  
N.R. Nik Roselina ◽  
Aziz Azizan ◽  
Koay Mei Hyie ◽  
C.M. Mardziah ◽  
Salmiah Kasolang ◽  
...  

Manipulation of adding sequences have been found to influence the reaction rate, thus made it easier to produced controllable Ni nanoparticles. Hot-injection approach shown capability to significantly reduce the production time of Ni nanoparticles compared to the conventional one-pot synthesis. With minor modification on conventional polyol method, narrow, monodispersed and highly yield spherical nickel (Ni) nanoparticles were successfully produced at synthesis temperature of 60°C. Three mixing methods were investigated to study its efficiency towards producing rapid and narrower size distribution of Ni nanoparticles. Reduction processes were proposed each of the method. As-synthesized Ni nanoparticles were characterized with Transmission Electron Microscopy (TEM), Scanning Transmission Electron Microscopy (STEM) and Fourier transform infrared spectroscopy (FTIR) to analyze the size, morphology and interaction of reactants. Fine particles size distribution revealed that when hydrazine was first heated, reaction rate improved tremendously.


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