Structural Evolution During the Sol to Gel Transition of Silicon-Alkoxide Based Sols Observed by Cryogenic Transmission Electron Microscopy (CRYO-TEM)

1988 ◽  
Vol 121 ◽  
Author(s):  
Joseph K. Bailey ◽  
Martha L. Mecartney

ABSTRACTThe gelation reaction for tetraethoxysilane in both acid and base catalyzed environments was studied using cryogenic transmission electron microscopy. The evolution of the gel structure was observed in wet samples by the technique of fast-freeze vitrification, in which the three dimensional gel structure is preserved in vitreous solvent. The sample is then observed in the electron microscope using a cold stage. Samples were prepared and allowed to react until a specific point of gelation was reached, then were vitrified at that point. Results from this technique show a coarse network structure for base catalyzed gels. This network is composed of silica clusters ≈40Å in size. The acid catalyzed gels show an extremely fine texture (<10Å) at end point of gelation. The structures at intermediate stages of gelation were also determined.

Author(s):  
W. D. Cooper ◽  
C. S. Hartley ◽  
J. J. Hren

Interpretation of electron microscope images of crystalline lattice defects can be greatly aided by computer simulation of theoretical contrast from continuum models of such defects in thin foils. Several computer programs exist at the present time, but none are sufficiently general to permit their use as an aid in the identification of the range of defect types encountered in electron microscopy. This paper presents progress in the development of a more general computer program for this purpose which eliminates a number of restrictions contained in other programs. In particular, the program permits a variety of foil geometries and defect types to be simulated.The conventional approximation of non-interacting columns is employed for evaluation of the two-beam dynamical scattering equations by a piecewise solution of the Howie-Whelan equations.


2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Bing Han ◽  
Yucheng Zou ◽  
Zhen Zhang ◽  
Xuming Yang ◽  
Xiaobo Shi ◽  
...  

AbstractCryogenic transmission electron microscopy (cryo-TEM) is a valuable tool recently proposed to investigate battery electrodes. Despite being employed for Li-based battery materials, cryo-TEM measurements for Na-based electrochemical energy storage systems are not commonly reported. In particular, elucidating the chemical and morphological behavior of the Na-metal electrode in contact with a non-aqueous liquid electrolyte solution could provide useful insights that may lead to a better understanding of metal cells during operation. Here, using cryo-TEM, we investigate the effect of fluoroethylene carbonate (FEC) additive on the solid electrolyte interphase (SEI) structure of a Na-metal electrode. Without FEC, the NaPF6-containing carbonate-based electrolyte reacts with the metal electrode to produce an unstable SEI, rich in Na2CO3 and Na3PO4, which constantly consumes the sodium reservoir of the cell during cycling. When FEC is used, the Na-metal electrode forms a multilayer SEI structure comprising an outer NaF-rich amorphous phase and an inner Na3PO4 phase. This layered structure stabilizes the SEI and prevents further reactions between the electrolyte and the Na metal.


Soft Matter ◽  
2021 ◽  
Vol 17 (11) ◽  
pp. 3096-3104
Author(s):  
Valeria Castelletto ◽  
Jani Seitsonen ◽  
Janne Ruokolainen ◽  
Ian W. Hamley

A designed surfactant-like peptide is shown, using a combination of cryogenic-transmission electron microscopy and small-angle X-ray scattering, to have remarkable pH-dependent self-assembly properties.


1990 ◽  
Vol 110 (4) ◽  
pp. 883-894 ◽  
Author(s):  
R Reichelt ◽  
A Holzenburg ◽  
E L Buhle ◽  
M Jarnik ◽  
A Engel ◽  
...  

Nuclear pore complexes (NPCs) prepared from Xenopus laevis oocyte nuclear envelopes were studied in "intact" form (i.e., unexposed to detergent) and after detergent treatment by a combination of conventional transmission electron microscopy (CTEM) and quantitative scanning transmission electron microscopy (STEM). In correlation-averaged CTEM pictures of negatively stained intact NPCs and of distinct NPC components (i.e., "rings," "spoke" complexes, and "plug-spoke" complexes), several fine structural features arranged with octagonal symmetry about a central axis could reproducibly be identified. STEM micrographs of unstained/freeze-dried intact NPCs as well as of their components yielded comparable but less distinct features. Mass determination by STEM revealed the following molecular masses: intact NPC with plug, 124 +/- 11 MD; intact NPC without plug, 112 +/- 11 MD; heavy ring, 32 +/- 5 MD; light ring, 21 +/- 4 MD; plug-spoke complex, 66 +/- 8 MD; and spoke complex, 52 +/- 3 MD. Based on these combined CTEM and STEM data, a three-dimensional model of the NPC exhibiting eightfold centrosymmetry about an axis perpendicular to the plane of the nuclear envelope but asymmetric along this axis is proposed. This structural polarity of the NPC across the nuclear envelope is in accord with its well-documented functional polarity facilitating mediated nucleocytoplasmic exchange of molecules and particles.


2008 ◽  
Vol 47 (1) ◽  
pp. 394-399 ◽  
Author(s):  
Hirotoshi Furusho ◽  
Yumiko Mishima ◽  
Norihiro Kameta ◽  
Mitsutoshi Masuda ◽  
Ichiro Yamashita ◽  
...  

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.


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