High-resolution TEM studies of mullite formation in metakaolinite

Author(s):  
Mehmet Sarikaya ◽  
IInan A. Aksay

Studies on the compressive fracture strength (759 MPa at 15000°C) and the flexural strength (700MPaat 1300°C) of polycrystalline mullite (3Al2O3•2SiO2-2Al2O3•SiO2) illustrate its potential for high temperature applications. In the processing of these high strength mullites, molecularly mixed Al2O3-SiO2 precursors are used to enhance mullite formation rates and to achieve microstructural homogeneity in the submicrometer range. Reaction steps leading to the formation of mullite in molecularly mixed systems are not adequately understood. The prevailing problems center around (i) the composition of a spinel phase that forms at around a 980°C exothermic reaction, and (ii) the concurrent or subsequent formation and growth of mullite. Here, we report our high resolution TEM results on the formation of the spinel and mullite phases in a molecularly mixed precursor, metakaolinite (Al2O3•2SiO2).

2011 ◽  
Vol 110-116 ◽  
pp. 991-996
Author(s):  
Lee Siang Chuah ◽  
A. Mahyudin ◽  
Z. Hasan ◽  
C.W. Chin

A high-quality crack-free AlN cap layer on GaN layer has been achieved using an AlN buffer layer directly grown on a silicon substrate at high temperature by radio frequency (RF) plasma-assisted molecular beam epitaxy. A two dimensional (2D) growth process guide to AlN cap layer of high grade crystal quality. The nucleation and the growth dynamics have been studied by in situ reflection high energy electron diffraction (RHEED) and ex situ by high resolution transmission electron microscopy (HR-TEM). The microstructure was investigated by energy-dispersive X-ray spectroscopy (EDX). It was disclosed that AlN is single crystalline with low defect. High densities of V-shaped pits were not detected at the interface between AlN and GaN layers. Contradictory the earlier reported V-shaped defects in nitride-based alloys; these V-shaped pits were condensed on top of the AlN layer because of H2 etching of the surface when a high temperature growth discontinuity between AlN and GaN layers.


1990 ◽  
Vol 209 ◽  
Author(s):  
Donald H. Galvàn ◽  
M. Avalos-Borja ◽  
L. Cota-Araiza ◽  
J. Cruz-Reyes ◽  
E. A. Early

ABSTRACTRecently Ogushi et al reported a La-Sr-Nb-O compound with a superconducting temperature of about 225 K. The possibility of having superconductors with such a high temperature is certainly technologically relevant. We prepared specimens with the same nominal stoichiometry and performed characterization by SEM, high resolution TEM, Scanning Auger and X-rays.


2005 ◽  
Vol 892 ◽  
Author(s):  
Jie Bai ◽  
J. Bai ◽  
V.L. Tassev ◽  
M. Lal Nakarmi ◽  
W. Sun ◽  
...  

AbstractThe evolution of stress during the MOCVD growth of AlN thin films on sapphire substrates under both low and high temperature conditions has been evaluated. The final stress state of the films is assumed to consist of the summation of stresses from three different sources: (1) the stress which arises from residual lattice mismatch between film and substrate i.e. that which persists after partial relaxation by misfit dislocation formation. The extent of relaxation is determined from High Resolution TEM analysis of the substrate/film interface; (2) the stress arising from the coalescence of the 3D islands nucleated in this high mismatch epitaxy process. This requires knowledge of the island sizes just prior to coalescence and this was provided by AFM studies of samples grown under the conditions of interest; and (3) the stress generated during post-growth cooling which arises from the differences in thermal expansion coefficient between AlN and sapphire. The final resultant stress, comprising the summation of stresses arising from these three sources, is found to be tensile in the sample grown at lower temperature and compressive in the sample grown at higher temperature. These results are in general qualitative agreement with results of TEM and High resolution X-ray diffraction (HRXRD) studies, which show evidence for tensile and compressive stresses in the low temperature and high temperature cases, respectively.


2011 ◽  
Vol 60 (3) ◽  
pp. 217-225 ◽  
Author(s):  
T. Yaguchi ◽  
M. Suzuki ◽  
A. Watabe ◽  
Y. Nagakubo ◽  
K. Ueda ◽  
...  

Author(s):  
D. F. Blake ◽  
L. F. Allard ◽  
D. R. Peacor

Echinodermata is a phylum of marine invertebrates which has been extant since Cambrian time (c.a. 500 m.y. before the present). Modern examples of echinoderms include sea urchins, sea stars, and sea lilies (crinoids). The endoskeletons of echinoderms are composed of plates or ossicles (Fig. 1) which are with few exceptions, porous, single crystals of high-magnesian calcite. Despite their single crystal nature, fracture surfaces do not exhibit the near-perfect {10.4} cleavage characteristic of inorganic calcite. This paradoxical mix of biogenic and inorganic features has prompted much recent work on echinoderm skeletal crystallography. Furthermore, fossil echinoderm hard parts comprise a volumetrically significant portion of some marine limestones sequences. The ultrastructural and microchemical characterization of modern skeletal material should lend insight into: 1). The nature of the biogenic processes involved, for example, the relationship of Mg heterogeneity to morphological and structural features in modern echinoderm material, and 2). The nature of the diagenetic changes undergone by their ancient, fossilized counterparts. In this study, high resolution TEM (HRTEM), high voltage TEM (HVTEM), and STEM microanalysis are used to characterize tha ultrastructural and microchemical composition of skeletal elements of the modern crinoid Neocrinus blakei.


Author(s):  
P.M. Mul ◽  
B.J.M. Bormans ◽  
L. Schaap

The first Field Emission Guns (FEG) on TEM/STEM instruments were introduced by Philips in 1977. In the past decade these EM400-series microscopes have been very successful, especially in analytical electron microscopy, where the high currents in small probes are particularly suitable. In High Resolution Electron Holography, the high coherence of the FEG has made it possible to approach atomic resolution.Most of these TEM/STEM systems are based on a cold field emitter (CFE). There are, however, a number of disadvantages to CFE’s, because of their very small emission region: the maximum current is limited (a strong disadvantage for high-resolution TEM imaging) and the emission is unstable, requiring special measures to reduce the strong FEG-induced noise. Thermal field emitters (TFE), i.e. a zirconiated field emitter source operating in the thermal or Schottky mode, have been shown to be a viable and attractive alternative to CFE’s. TFE’s have larger emission regions, providing much higher maximum currents, better stability, and reduced sensitivity to vacuum conditions as well as mechanical and electrical interferences.


Author(s):  
H. Kung ◽  
A.J. Griffin ◽  
Y.C. Lu ◽  
K.E. Sickafus ◽  
T.E. Mitchell ◽  
...  

Materials with compositionally modulated structures have gained much attention recently due to potential improvement in electrical, magnetic and mechanical properties. Specifically, Cu-Nb laminate systems have been extensively studied mainly due to the combination of high strength, and superior thermal and electrical conductivity that can be obtained and optimized for the different applications. The effect of layer thickness on the hardness, residual stress and electrical resistivity has been investigated. In general, increases in hardness and electrical resistivity have been observed with decreasing layer thickness. In addition, reduction in structural scale has caused the formation of a metastable structure which exhibits uniquely different properties. In this study, we report the formation of b.c.c. Cu in highly textured Cu/Nb nanolayers. A series of Cu/Nb nanolayered films, with alternating Cu and Nb layers, were prepared by dc magnetron sputtering onto Si {100} wafers. The nominal total thickness of each layered film was 1 μm. The layer thickness was varied between 1 nm and 500 nm with the volume fraction of the two phases kept constant at 50%. The deposition rates and film densities were determined through a combination of profilometry and ion beam analysis techniques. Cross-sectional transmission electron microscopy (XTEM) was used to examine the structure, phase and grain size distribution of the as-sputtered films. A JEOL 3000F high resolution TEM was used to characterize the microstructure.


Author(s):  
W. Lo ◽  
J.C.H. Spence ◽  
M. Kuwabara

Work on the integration of STM with REM has demonstrated the usefulness of this combination. The STM has been designed to replace the side entry holder of a commercial Philips 400T TEM. It allows simultaneous REM imaging of the tip/sample region of the STM (see fig. 1). The REM technique offers nigh sensitivity to strain (<10−4) through diffraction contrast and high resolution (<lnm) along the unforeshortened direction. It is an ideal technique to use for studying tip/surface interactions in STM.The elastic strain associated with tunnelling was first imaged on cleaved, highly doped (S doped, 5 × 1018cm-3) InP(110). The tip and surface damage observed provided strong evidence that the strain was caused by tip/surface contact, most likely through an insulating adsorbate layer. This is consistent with the picture that tunnelling in air, liquid or ordinary vacuum (such as in a TEM) occurs through a layer of contamination. The tip, under servo control, must compress the insulating contamination layer in order to get close enough to the sample to tunnel. The contaminant thereby transmits the stress to the sample. Elastic strain while tunnelling from graphite has been detected by others, but never directly imaged before. Recent results using the STM/REM combination has yielded the first direct evidence of strain while tunnelling from graphite. Figure 2 shows a graphite surface elastically strained by the STM tip while tunnelling (It=3nA, Vtip=−20mV). Video images of other graphite surfaces show a reversible strain feature following the tip as it is scanned. The elastic strain field is sometimes seen to extend hundreds of nanometers from the tip. Also commonly observed while tunnelling from graphite is an increase in the RHEED intensity of the scanned region (see fig.3). Debris is seen on the tip and along the left edges of the brightened scan region of figure 4, suggesting that tip abrasion of the surface has occurred. High resolution TEM images of other tips show what appear to be attached graphite flakes. The removal of contamination, possibly along with the top few layers of graphite, seems a likely explanation for the observed increase in RHEED reflectivity. These results are not inconsistent with the “sliding planes” model of tunnelling on graphite“. Here, it was proposed that the force due to the tunnelling probe acts over a large area, causing shear of the graphite planes when the tip is scanned. The tunneling current is then modulated as the planes of graphite slide in and out of registry. The possiblity of true vacuum tunnelling from the cleaned graphite surface has not been ruled out. STM work function measurements are needed to test this.


2003 ◽  
Vol 762 ◽  
Author(s):  
Hwang Huh ◽  
Jung H. Shin

AbstractAmorphous silicon (a-Si) films prepared on oxidized silicon wafer were crystallized to a highly textured form using contact printing of rolled and annealed nickel tapes. Crystallization was achieved by first annealing the a-Si film in contact with patterned Ni tape at 600°C for 20 min in a flowing forming gas (90 % N2, 10 % H2) environment, then removing the Ni tape and further annealing the a-Si film in vacuum for2hrsat600°C. An array of crystalline regions with diameters of up to 20 μm could be formed. Electron microscopy indicates that the regions are essentially single-crystalline except for the presence of twins and/or type A-B formations, and that all regions have the same orientation in all 3 directions even when separated by more than hundreds of microns. High resolution TEM analysis shows that formation of such orientation-controlled, nearly single crystalline regions is due to formation of nearly single crystalline NiSi2 under the point of contact, which then acts as the template for silicide-induced lateral crystallization. Furthermore, the orientation relationship between Si grains and Ni tape is observed to be Si (110) || Ni (001)


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