Dark field imaging of semicrystalline polymers by scanning transmission electron microscopy

1981 ◽  
Vol 16 (1) ◽  
pp. 1-9 ◽  
Author(s):  
Edward S. Sherman ◽  
W. Wade Adams ◽  
Edwin L. Thomas
2012 ◽  
Vol 9 (73) ◽  
pp. 1774-1786 ◽  
Author(s):  
Benjamin Alexander ◽  
Tyrone L. Daulton ◽  
Guy M. Genin ◽  
Justin Lipner ◽  
Jill D. Pasteris ◽  
...  

The nanometre-scale structure of collagen and bioapatite within bone establishes bone's physical properties, including strength and toughness. However, the nanostructural organization within bone is not well known and is debated. Widely accepted models hypothesize that apatite mineral (‘bioapatite’) is present predominantly inside collagen fibrils: in ‘gap channels’ between abutting collagen molecules, and in ‘intermolecular spaces’ between adjacent collagen molecules. However, recent studies report evidence of substantial extrafibrillar bioapatite, challenging this hypothesis. We studied the nanostructure of bioapatite and collagen in mouse bones by scanning transmission electron microscopy (STEM) using electron energy loss spectroscopy and high-angle annular dark-field imaging. Additionally, we developed a steric model to estimate the packing density of bioapatite within gap channels. Our steric model and STEM results constrain the fraction of total bioapatite in bone that is distributed within fibrils at less than or equal to 0.42 inside gap channels and less than or equal to 0.28 inside intermolecular overlap regions. Therefore, a significant fraction of bone's bioapatite (greater than or equal to 0.3) must be external to the fibrils. Furthermore, we observe extrafibrillar bioapatite between non-mineralized collagen fibrils, suggesting that initial bioapatite nucleation and growth are not confined to the gap channels as hypothesized in some models. These results have important implications for the mechanics of partially mineralized and developing tissues.


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

2019 ◽  
Vol 104 (10) ◽  
pp. 1436-1443
Author(s):  
Guanyu Wang ◽  
Hejing Wang ◽  
Jianguo Wen

Abstract Interstratified clay minerals reflect the weathering degree and record climatic conditions and the pedogenic processes in the soil. It is hard to distinguish a few layers of interstratified clay minerals from the chlorite matrix, due to their similar two-dimensional tetrahedral-octahedral-tetrahedral (TOT) structure and electron-beam sensitive nature during transmission electron microscopy (TEM) imaging. Here, we used multiple advanced TEM techniques including low-dose high-resolution TEM (HRTEM), high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) imaging combined with energy-dispersive spectroscopic (EDS) mapping to study interstratified layers in a chlo-rite sample from Changping, Beijing, China. We demonstrated an interstratified mica or pyrophyllite monolayer could be well distinguished from the chlorite matrix by projected atomic structures, lattice spacings, and chemical compositions with advanced TEM techniques. Further investigation showed two different transformation mechanisms from mica or pyrophyllite to chlorite: either a 4 Å increase or decrease in the lattice spacing. This characterization approach can be extended to the studies of other electron-beam sensitive minerals.


Author(s):  
Ryosuke S. S. Maki ◽  
Peter E. D. Morgan

Many members of the complex crystalline fluorite supercell structures (e.g. zirconolite, pyrochlore and murataite polytypes) have been considered/studied for possible long-term radioactive-waste immobilization. The eight-coordinated sites in these crystals are of particular importance because they are preferred for the accommodation of trivalent rare earths and actinides present in radioactive waste from fuel element processing. The fluorite-type supercell structures include the murataites, M3, M5, M7, M8, having those numbers of repeating fluorite sub-cell units. One simple technique, as shown here, namely the substitution of Hf into the Zr site, is very helpful for structural analysis in these very complex cases in order to further illuminate the site preference of the Zr ion. Three M3 murataite samples, Ca-Mn-Ti-Zr-Al-Fe-O (regular M3), Ca-Ti-Zr-Al-Fe-O (Mn-free M3) and Ca-Mn-Ti-Hf-Al-Fe-O (Hf-substituted M3) are investigated and, through techniques described for larger cells, show that the Zr is very likely not to be hosted in the [6] Ti site in the M3 murataite structure, as suggested by Pakhomova et al. [(2013), Z. Kristallogr. Cryst. Mater. 228, 151–156], but more likely replaces the [8] Ca1 site and less likely the [8] Ca2 site. This adjusted site preference for each cation from the powder X-ray diffraction (PXRD) and scanning transmission electron microscopy electron energy-loss spectroscopy (STEM-EELS) methods, agrees well with the high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) image.


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