Morphological changes of poly(tetrafluoroethylene) by heat treatment on NaCl

1993 ◽  
Vol 8 (11) ◽  
pp. 2942-2947 ◽  
Author(s):  
Sadaatsu Yamaguchi ◽  
Masaki Tsuji

Fine granules of poly(tetrafluoroethylene) (PTFE) were heat-treated/annealed on NaCl near its melting temperature (Tm) and/or at a temperature (Tc) between upper and lower feet of the exothermic peak in the DSC cooling process from Tm. Morphological changes of the granules were examined in the bright- and dark-field modes by transmission electron microscopy. When the granules were heat-treated near Tm, microfibrils of 20–30 nm in width and fibrils of 70–120 nm in width came out of the granules. The microfibrils were also observed in the fibrils. The microfibrils formed by heat treatment near Tm seemed to be identified as microfibrils of 20–30 nm in width which were recognized outside the granules annealed at Tc. It is expected that such a microfibril will grow to be a band in the band structure observed on the surface of bulk PTFE. Since the 0015 dark-field images showed that the PTFE chains in such microfibrils and fibrils are set perpendicular to their fibril axis, the chains should fold back and forth repeatedly at both lateral side-surfaces of the microfibrils and fibrils.

2011 ◽  
Vol 172-174 ◽  
pp. 682-687 ◽  
Author(s):  
Remi Delville ◽  
Benoît Malard ◽  
Jan Pilch ◽  
Petr Šittner ◽  
Dominique Schryvers

Transmission electron microscopy and mechanical testing were employed to investigate the evolution of microstructure and functional superelastic properties of 0.1mm diameter as-drawn Ni-Ti wires subjected to a non-conventional heat treatment by controlled electric pulse current. This method enables a finer control of the recovery and recrystallisation processes taking place during the heat treatment and accordingly a better control on the final microstructure. The best functional properties were obtained for heat-treated Ni-Ti wires having a nanograined microstructure (20-50 nm) partially recovered through polygonization and partially recrystallized. Such microstructure is highly resistant against dislocation slip upon cycling, while microstructures annealed for longer time and showing mostly recrystallized grains were prone to dislocation slip, particularly as the grain size exceeds 100 nm. The density of dislocation defects increased significantly with increasing grain size of the microstructure. The activity of three <100>/{011} slip systems was identified in the largest grains of 500-1200 nm. An additional mode of plastic deformation, {114} compound austenite twinning, was observed in the largest grains of fully recrystallized microstructures. It is proposed that dislocation slip (and possibly deformation twinning) occurring in superelastic cycling is coupled with the stress-induced martensitic transformation.


2020 ◽  
Vol 2020 ◽  
pp. 1-9
Author(s):  
Chun Guo ◽  
Suhang Liu ◽  
Ruizhang Hu ◽  
Chunhui Liu ◽  
Feng Chen

Wire arc additive manufacturing (WAAM) technology was used to produce samples of a 2.25Cr1Mo0.25V heat-resistant steel. The phase composition, microstructure, and crystal structure of the investigated material in the as-cladded state and postcladding heat-treated (705°C × 1 h) state were analysed by optical emission spectrometry (OES), optical microscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The properties of the investigated material in the as-cladded state and postcladding heat-treated (705°C × 1 h) state were determined by a microhardness tester, mechanical properties tester, and Charpy impact tester. Through a study of the microstructure and properties, it is found that the investigated material produced by WAAM exhibits good forming quality and excellent metallurgical bonding properties, and no obvious defects are found. The microstructure consists mainly of Bg (granular bainite) and troostite precipitated at the grain boundaries. The results from high-resolution transmission electron microscopy observations show that the crystal structures of the 2.25Cr1Mo0.25V heat-resistant steel samples produced by WAAM in the as-cladded condition have many defects, such as dislocations and martensite-austenite (M-A) constituents, and their grain edges are sharp. There is a dramatic decrease in the dislocations in the 2.25Cr1Mo0.25V heat-resistant steel samples produced by the WAAM condition after the postcladding heat treatment (705°C × 1 h), and the grains become smooth. The distribution of the microhardness in the longitudinal and transverse cross sections of the samples is very uniform. The average longitudinal and transverse microhardness of the samples in the as-cladded state is 310 HV0.5 and 324 HV0.5, respectively. The average longitudinal and transverse microhardness of the samples after post-cladding heat treatment is 227 HV0.5 and 229 HV0.5, respectively. The yield strength of the samples without a postcladding heat treatment is 743 MPa, the tensile strength is 951 MPa, the elongation is 10%, and the Charpy impact value at -20°C is 15 J. After the postcladding heat treatment, the yield strength, tensile strength, elongation, and Charpy impact value of the samples are 611 MPa, 704 MPa, 14.5%, and 70 J, respectively.


Author(s):  
A. Garg ◽  
R. D. Noebe ◽  
J. M. Howe ◽  
A. W. Wilson ◽  
V. Levit

Three directionally solidified NiAl single-crystal alloys, NiAl-3Ti, NiAl-0.5Hf and NiAl-3Ti-0.5Hf (at.%), were grown by a Bridgeman technique using high purity alumina crucibles. The ingots were homogenized for 32h at 1644 K followed by aging for 6h at 1255 K and finally furnace cooled under an argon atmosphere. This heat treatment was found to be very effective in dissolving Hf-rich interdendritic particles that were present in the as-cast structure, and at the same time it produced fine second-phase precipitates in the alloy.Samples for transmission electron microscopy (TEM) were prepared from 3 mm diameter cylinders electro-discharge machined from the heat-treated ingots. Slices sectioned from the cylinders were mechanically ground and electrochemically thinned in a twin-jet Tenupol-3 polisher. Microstructural and energy-dispersive X-ray spectroscopy (EDXS) studies were conducted in a Philips 400T TEM equipped with a double tilt goniometer and a KEVEX Si/Li X-ray detector.


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.


1990 ◽  
Vol 38 (10) ◽  
pp. 1469-1478 ◽  
Author(s):  
D R Eisenmann ◽  
A H Salama ◽  
A M Zaki ◽  
S H Ashrafi

Colchicine is known to affect secretory, transport, and degradative functions of ameloblasts. The effects of colchicine on membrane-associated calcium and Ca2+,Mg2(+)-ATPase in secretory and maturation ameloblasts were investigated cytochemically. The pyroantimonate (PPA) method was used for localizing calcium and a modified Wachstein-Meisel medium was used to localize Ca2+,Mg2(+)-ATPase. Sections representing secretory and early maturation stages were examined by transmission electron microscopy. Morphological changes induced by colchicine included dislocated organelles and other well-established reactions to such anti-microtubule drugs. Calcium pyroantimonate (Ca-PA) deposits in most ameloblast types were markedly reduced, with the greater reduction occurring in those cells more severely altered morphologically. However, the cell membranes of both control and experimental smooth-ended maturation ameloblasts were essentially devoid of Ca-PA. The normal distribution and intensity of Ca2+,Mg2(+)-ATPase was not affected by colchicine. Because the observed reduction of membrane-associated calcium is apparently not mediated by Ca2+,Mg2(+)-ATPase in this case, other aspects of the calcium regulating system of ameloblasts are apparently targeted by colchicine.


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.


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.


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