Matrix-Mediated Biomineralization in Marine Mollusks: A Combined Transmission Electron Microscopy and Focused Ion Beam Approach

2011 ◽  
Vol 17 (2) ◽  
pp. 220-225 ◽  
Author(s):  
Martin Saunders ◽  
Charlie Kong ◽  
Jeremy A. Shaw ◽  
Peta L. Clode

AbstractThe teeth of the marine mollusk Acanthopleura hirtosa are an excellent example of a complex, organic, matrix-mediated biomineral, with the fully mineralized teeth comprising layers of iron oxide and iron oxyhydroxide minerals around a calcium apatite core. To investigate the relationship between the various mineral layers and the organic matrix fibers on which they grew, sections have been prepared from specific features in the teeth at controlled orientations using focused ion beam processing. Compositional and microstructural details of heterophase interfaces, and the fate of the organic matrix fibers within the mineral layers, can then be analyzed by a range of transmission electron microscopy (TEM) techniques. Energy-filtered TEM highlights the interlocking nature of the various mineral phases, while high-angle annular dark-field scanning TEM imaging demonstrates that the organic matrix continues to exist in the fully mineralized teeth. These new insights into the structure of this complex biomaterial are an important step in understanding the relationship between its structural and physical properties and may help explain its high strength and crack-resistance behavior.

Metals ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 719
Author(s):  
Marija Korać ◽  
Željko Kamberović ◽  
Zoran Anđić ◽  
Srećko Stopić

This paper presents thermochemical synthesis of copper/alumina nanocomposites in a Cu-Al2O3 system with 1–2.5 wt.% of alumina and their characterization, which included: transmission electron microscopy: focused ion beam (FIB), analytical electron microscopy (AEM) and high resolution transmission electron microscopy (HRTEM). Thermodynamic analysis was used to study the formation mechanism of desirable products during drying, thermal decomposition and reduction processes. Upon synthesis of powders, samples were cold pressed (2 GPa) in tools dimension 8 × 32 × 2 mm and sintered at temperatures within the range 800–1000 °C for 15 to 120 min in a hydrogen atmosphere. Results of characterization showed that dispersion-strengthened compacts could be produced by sintering of thermo-chemically prepared Cu-Al2O3 powders with properties suitable for material application, such as a contact material exhibiting high strength and high electrical conductivity at the same time. Additional research was carried out in order to analyze the application of the obtained nanocomposite powders for the synthesis of copper/alumina nanocomposites by a new method, which is a combination of a thermochemical procedure and mechanical alloying. The measured values of an electric conductivity and hardness were compared with ones in literature, confirming an advantage of the proposed combined strategy.


2008 ◽  
Vol 23 (12) ◽  
pp. 3213-3221 ◽  
Author(s):  
Taro Sumitomo ◽  
Hideki Kakisawa ◽  
Yusuke Owaki ◽  
Yutaka Kagawa

The mechanical performance of nacre in seashells is generally described in terms of mesoscale mechanisms between mineral plates within the organic polymer matrix. However, recent work has reported nanostructures and organic material within individual plates and associated deformation mechanisms. In this work, we further investigated the nanoscale structure and mechanical behavior within individual plates of nacre by using two methods to induce fracture of plates: microindentation with focused ion beam preparation and ultramicrotomy. Using transmission electron microscopy, we observed deformation nanostructures and organic matrix within plates and identified nanoscale mechanisms, such as separation, shear, and matrix crack bridging.


2010 ◽  
Vol 16 (5) ◽  
pp. 604-613 ◽  
Author(s):  
T. Volkenandt ◽  
E. Müller ◽  
D.Z. Hu ◽  
D.M. Schaadt ◽  
D. Gerthsen

AbstractHigh-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) images of electron-transparent samples show dominant atomic number (Z-) contrast with a high lateral resolution. HAADF STEM at low electron energies <30 keV is applied in this work for quantitative composition analyses of InGaAs quantum wells. To determine the local composition, normalized experimental image intensities are compared with results of Monte Carlo simulations. For verification of the technique, InGaAs/GaAs quantum-well structures with known In concentration are used. Transmission electron microscopy samples with known thickness are prepared by the focused-ion-beam technique. The method can be extended to other material systems and is particularly promising for the analysis of materials that are sensitive toward knock-on damage.


2007 ◽  
Vol 1040 ◽  
Author(s):  
Luke Owuor Nyakiti ◽  
Jharna Chaudhuri ◽  
Ed A Kenik ◽  
Peng Lu ◽  
James H Edgar

AbstractIn the present study, the type and densities of defects in AlN crystals grown on 6H-SiC seeds by the sublimation-recombination method were assessed. The positions of the defects in AlN were first identified by defect selective etching (DSE) in molten NaOH-KOH at 400 °C for 2 minutes. Etching produced pits of three different sizes: 1.77 ìm, 2.35 ìm , and 2.86 ìm. The etch pits were either aligned together forming a sub-grain boundary or randomly distributed. The smaller etch pits were either isolated or associated with larger etch pits. After preparing cross-sections of the pits by the focused ion beam (FIB) technique, transmission electron microscopy (TEM) was performed to determine which dislocation type (edge, mixed or screw) produced a specific etch pit sizes. Preliminary TEM bright field and dark field study using different zone axes and diffraction vectors indicates an edge dislocation with a Burgers vector 1/3 is associated with the smallest etch pit size.


Author(s):  
Ching Shan Sung ◽  
Hsiu Ting Lee ◽  
Jian Shing Luo

Abstract Transmission electron microscopy (TEM) plays an important role in the structural analysis and characterization of materials for process evaluation and failure analysis in the integrated circuit (IC) industry as device shrinkage continues. It is well known that a high quality TEM sample is one of the keys which enables to facilitate successful TEM analysis. This paper demonstrates a few examples to show the tricks on positioning, protection deposition, sample dicing, and focused ion beam milling of the TEM sample preparation for advanced DRAMs. The micro-structures of the devices and samples architectures were observed by using cross sectional transmission electron microscopy, scanning electron microscopy, and optical microscopy. Following these tricks can help readers to prepare TEM samples with higher quality and efficiency.


Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang

Abstract The specimen preparation technique using focused ion beam (FIB) to generate cross-sectional transmission electron microscopy (XTEM) samples of chemical vapor deposition (CVD) of Tungsten-plug (W-plug) and Tungsten Silicides (WSix) was studied. Using the combination method including two axes tilting[l], gas enhanced focused ion beam milling[2] and sacrificial metal coating on both sides of electron transmission membrane[3], it was possible to prepare a sample with minimal thickness (less than 1000 A) to get high spatial resolution in TEM observation. Based on this novel thinning technique, some applications such as XTEM observation of W-plug with different aspect ratio (I - 6), and the grain structure of CVD W-plug and CVD WSix were done. Also the problems and artifacts of XTEM sample preparation of high Z-factor material such as CVD W-plug and CVD WSix were given and the ways to avoid or minimize them were suggested.


Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su

Abstract Focused ion beam (FIB) has become a useful tool in the Integrated Circuit (IC) industry, It is playing an important role in Failure Analysis (FA), circuit repair and Transmission Electron Microscopy (TEM) specimen preparation. In particular, preparation of TEM samples using FIB has become popular within the last ten years [1]; the progress in this field is well documented. Given the usefulness of FIB, “Artifact” however is a very sensitive issue in TEM inspections. The ability to identify those artifacts in TEM analysis is an important as to understanding the significance of pictures In this paper, we will describe how to measure the damages introduced by FIB sample preparation and introduce a better way to prevent such kind of artifacts.


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.


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