Dynamic low-dose electron diffraction and imaging of phase transitions in polymers

Author(s):  
David C. Martin ◽  
Jun Liao

By careful control of the electron beam it is possible to simultaneously induce and observe the phase transformation from monomer to polymer in certain solid-state polymcrizable diacetylenes. The continuous change in the crystal structure from DCHD diacetylene monomer (a=1.76 nm, b=1.36 nm, c=0.455 nm, γ=94 degrees, P2l/c) to polymer (a=1.74 nm, b=1.29 nm, c=0.49 nm, γ=108 degrees, P2l/c) occurs at a characteristic dose (10−4C/cm2) which is five orders of magnitude smaller than the critical end point dose (20 C/cm2). Previously we discussed the progress of this phase transition primarily as observed down the [001] zone (the chain axis direction). Here we report on the associated changes of the dark field (DF) images and selected area electron diffraction (SAED) patterns of the crystals as observed from the side (i.e., in the [hk0] zones).High resolution electron micrographs (HREM), DF images, and SAED patterns were obtained on a JEOL 4000 EX HREM operating at 400 kV.

2013 ◽  
Vol 456 ◽  
pp. 533-536
Author(s):  
Yan Zhi Lou

In this paper, high resolution electron microscopy (HREM) was used to observe nanosized Fe2M precipitates in M50NiL steel, and crystal structure of which was also investigated by selected area electron diffraction (SAED). At the same time, the orientation relationship between the Fe2M and the martensite matrix was also studied. The results suggested that crystal structure of Fe2M is close-packed hexagonal, and lattice parameters about a=b=0.473nm, c=0.772nm, α=β=90°, γ=120°. The orientation relationship between the nanoprecipitates Fe2M and martensite is and .


Author(s):  
John P. Langmore ◽  
Brian D. Athey

Although electron diffraction indicates better than 0.3nm preservation of biological structure in vitreous ice, the imaging of molecules in ice is limited by low contrast. Thus, low-dose images of frozen-hydrated molecules have significantly more noise than images of air-dried or negatively-stained molecules. We have addressed the question of the origins of this loss of contrast. One unavoidable effect is the reduction in scattering contrast between a molecule and the background. In effect, the difference in scattering power between a molecule and its background is 2-5 times less in a layer of ice than in vacuum or negative stain. A second, previously unrecognized, effect is the large, incoherent background of inelastic scattering from the ice. This background reduces both scattering and phase contrast by an additional factor of about 3, as shown in this paper. We have used energy filtration on the Zeiss EM902 in order to eliminate this second effect, and also increase scattering contrast in bright-field and dark-field.


Author(s):  
Andrew J. Lovinger ◽  
Bernard Lotz ◽  
Don D. Davis

In contrast to its isotactic isomer, syndiotactic polypropylene has received only little attention. Our main source of understanding of its structure is the X-ray study by Conradini et al., who found the chains to have a (t2g2)2 conformation (corresponding to a 4∗2/1 helix with molecular repeat 0.74 nm), and to be packed in a C-centered unit cell as shown in the left side of Fig. 1. We have recently begun a study of the structure, crystallization, and morphology of syndiotactic polypropylene using electron microscopy and diffraction. Here we concentrate specifically on the electron-diffraction evidence as a function of temperature, in order to obtain an understanding of the evolution and variation of structure in this polymer.Thin films of syndiotactic polypropylene (synthesized by Dr. R. E. Cais as reported previously) were prepared by casting from dilute solution in xylenes at ca. 140°c onto freshly cleaved mica substrates. Following evaporation of the solvent, they were melted and then isothermally crystallized at a variety of temperatures. After shadowing with Pt/C and coating with carbon, they were floated off their substrates for examination by transmission electron microscopy (bright- and dark-field) and selected-area electron diffraction at 100-200 keV.


RSC Advances ◽  
2015 ◽  
Vol 5 (94) ◽  
pp. 76957-76962 ◽  
Author(s):  
Hongqiang Ma ◽  
Kun Lin ◽  
Laijun Liu ◽  
Baoling Yang ◽  
Yangchun Rong ◽  
...  

The crystal structure and electrical property of a tetragonal tungsten bronze ceramic, BaCeFeNb4O15, were investigated by synchrotron X-ray powder diffraction, selected area electron diffraction, and AC impedance spectroscopy.


2007 ◽  
Vol 561-565 ◽  
pp. 243-246 ◽  
Author(s):  
Junya Nakamura ◽  
Kenji Matsuda ◽  
Yoshio Nakamura ◽  
Tatsuo Sato ◽  
Susumu Ikeno

The purpose of this study is to identify the crystal structure of metastable phase in Ag added Al-Mg-Si alloy to compare the formation of β’-phases in Al-Mg-Si alloys without Ag, using images of high resolution transmission electron microscope (HRTEM), selected area electron diffraction (SAED) patterns and an energy dispersive X-ray spectroscopy (EDS). The result of SAED patterns and HRTEM images have been simulated and compared with images then SAED patterns obtained from actual precipitates. SAED patterns and HRTEM images obtained from metastable phase in the Ag added Al-Mg-Si alloy showed similar to those of β’-phase in Al-Mg-Si alloy without Ag and the lattice spacings changed because of the effect of Ag.


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