In Situ Dynamic Atomic-Level Investigation of a Weak Charge Transfer Lamellar Intercalation Process

1995 ◽  
Vol 404 ◽  
Author(s):  
L. Diebolt ◽  
R. Sharma ◽  
M. Mckelvy ◽  
W. S. Glaunsinger

AbstractEnvironmental-cell dynamic high-resolution transmission electron microscopy (DHRTEM) has been used to provide atomic-level insight into lamellar reaction processes for the model weak- charge-transfer intercalation reaction of NH3 with 2H-TaS2. In situ intercalation was induced by exposing 2H-TaS2 crystallites to controlled pressures of NH3(g) and recorded on videotape with 0.03 second time resolution. The intercalation processes observed possess a strong similarity to nucleation and growth processes. Onset occurs in either outermost or internal guest galleries, with further intercalation of the galleries progressing away from the onset layers. Randomly staged regions, containing occasional packages of short-range order, were observed to form during the growth process.

1993 ◽  
Vol 317 ◽  
Author(s):  
R. Sharma ◽  
Z. Atzmon ◽  
J. Mayer ◽  
S. Q. Hong

ABSTRACTCo-deposited Cu/Ti thin films were heated at various temperatures in an ammonia ambient in an environmental cell fitted in to the column of transmission electron Microscope (TEM). The reaction dynamics was observed in situ and recorded on video using a TV camera with 1/30 sec. time resolution. The nitridation of titanium accompanied by nucleation and growth of copper particles started at 370°C. Ti2N formed at lower temperatures while TiN was formed above 400°C. The nucleation of crystals occurred simultaneously (within a Minute) throughout the film indicating no effect of electron beam on reaction process. The growth rate of copper particles was observed to vary slightly from one particle to another indicating varying growth rate for different facets.


Author(s):  
D. A. Smith

The nucleation and growth processes which lead to the formation of a thin film are particularly amenable to investigation by transmission electron microscopy either in situ or subsequent to deposition. In situ studies have enabled the observation of island nucleation and growth, together with addition of atoms to surface steps. This paper is concerned with post-deposition crystallization of amorphous alloys. It will be argued that the processes occurring during low temperature deposition of one component systems are related but the evidence is mainly indirect. Amorphous films result when the deposition conditions such as low temperature or the presence of impurities (intentional or unintentional) preclude the atomic mobility necessary for crystallization. Representative examples of this behavior are CVD silicon grown below about 670°C, metalloids, such as antimony deposited at room temperature, binary alloys or compounds such as Cu-Ag or Cr O2, respectively. Elemental metals are not stable in the amorphous state.


Author(s):  
S. Q. Xiao ◽  
S. Baden ◽  
A. H. Heuer

The avian eggshell is one of the most rapidly mineralizing biological systems known. In situ, 5g of calcium carbonate are crystallized in less than 20 hrs to fabricate the shell. Although there have been much work about the formation of eggshells, controversy about the nucleation and growth mechanisms of the calcite crystals, and their texture in the eggshell, still remain unclear. In this report the microstructure and microchemistry of avian eggshells have been analyzed using transmission electron microscope (TEM) and energy dispersive spectroscopy (EDS).Fresh white and dry brown eggshells were broken and fixed in Karnosky's fixative (kaltitanden) for 2 hrs, then rinsed in distilled H2O. Small speckles of the eggshells were embedded in Spurr medium and thin sections were made ultramicrotome.The crystalline part of eggshells are composed of many small plate-like calcite grains, whose plate normals are approximately parallel to the shell surface. The sizes of the grains are about 0.3×0.3×1 μm3 (Fig.l). These grains are not as closely packed as man-made polycrystalline metals and ceramics, and small gaps between adjacent grains are visible indicating the absence of conventional grain boundaries.


Author(s):  
R-R. Lee

Partially-stabilized ZrO2 (PSZ) ceramics have considerable potential for advanced structural applications because of their high strength and toughness. These properties derive from small tetragonal ZrO2 (t-ZrO2) precipitates in a cubic (c) ZrO2 matrix, which transform martensitically to monoclinic (m) symmetry under applied stresses. The kinetics of the martensitic transformation is believed to be nucleation controlled and the nucleation is always stress induced. In situ observation of the martensitic transformation using transmission electron microscopy provides considerable information about the nucleation and growth aspects of the transformation.


2008 ◽  
Vol 1142 ◽  
Author(s):  
Hideto Yoshida ◽  
Seiji Takeda ◽  
Tetsuya Uchiyama ◽  
Hideo Kohno ◽  
Yoshikazu Homma

ABSTRACTNucleation and growth processes of carbon nanotubes (CNTs) in iron catalyzed chemical vapor deposition (CVD) have been observed by means of in-situ environmental transmission electron microscopy. Our atomic scale observations demonstrate that solid state iron carbide (Fe3C) nanoparticles act as catalyst for the CVD growth of CNTs. Iron carbide nanoparticles are structurally fluctuated in CVD condition. Growth of CNTs can be simply explained by bulk diffusion of carbon atoms since nanoparticles are carbide.


2007 ◽  
Vol 7 (12) ◽  
pp. 4378-4390 ◽  
Author(s):  
Anuradha Somayaji ◽  
Ramoun Mourhatch ◽  
Pranesh B. Aswath

Tribofilms with thickness ranging from 100–200 nm were developed in-situ during wear tests using a zinc dialkyl dithiophosphates (ZDDP) and fluorinated ZDDP (F-ZDDP). The influence of the antioxidant alkylated diphenyl amine on the formation and properties of these tribofilm is examined. Results indicate that the thickness of the tribofilms formed when F-ZDDP is used is always thicker than the tribofilm formed with ZDDP. In addition, in the presence of antioxidants the tribofilm thickness is increased. The hardness of these tribofilms in the absence of the antioxidants is significantly higher at the near surface region (0–30 nm) when compared to the films formed in the presence of antioxidant. Nanoscratch tests conducted to examine the abrasion resistance of the tribofilms also indicate that the tribofilms formed by F-ZDDP are more resistant to scratch compared to films formed by ZDDP. In the presence of antioxidant, tribofilms formed by F-ZDDP are significantly thicker while both films behave in a similar fashion in nanoscratch tests. Transmission electron microscopy of the wear debris formed during the tests were examined and results indicate the nucleation and growth of nanoparticles of Fe3O4 with an approximate size of 5–10 nm embedded within an otherwise amorphous tribofilm.


2001 ◽  
Vol 7 (6) ◽  
pp. 494-506 ◽  
Author(s):  
Renu Sharma

AbstractThe environmental transmission electron microscopy (E-TEM) is a budding technique for in situ study of gas–solid chemical reactions with numerous applications. Recent improvements in the design have made it possible not only to obtain atomic level information but also the chemical information during the reaction by incorporating an imaging filter or electron energy-loss spectrometer to an E-TEM. We have been involved in modifying a couple of microscopes to incorporate environmental cells in order to convert them into E-TEMs. These microscopes have been used to obtain atomic level information of the structural and chemical changes during dynamic processes by in situ electron diffraction, high-resolution imaging, and electron energyloss spectroscopy. The applications include, but are not limited to, oxidation, reduction, polymerization, nitridation, dehydroxylation, hydroxylation, chemical vapor deposition, etc. We report recent developments in the design and application along with the limitations of an E-TEM.


1996 ◽  
Vol 436 ◽  
Author(s):  
R.-M. Keller ◽  
W. Sigle ◽  
S. P. Baker ◽  
O. Kraft ◽  
E. Arzt

AbstractIn-situ transmission electron microscopy (TEM) was performed to study grain growth and dislocation motion during temperature cycles of Cu films with and without a cap layer. In addition, the substrate curvature method was employed to determine the corresponding stresstemperature curves from room temperature up to 600°C. The results of the in-situ TEM investigations provide insight into the microstructural evolution which occurs during the stress measurements. Grain growth occurred continuously throughout the first heating cycle in both cases. The evolution of dislocation structure observed in TEM supports an explanation of the stress evolution in both capped and uncapped films in terms of dislocation effects.


1993 ◽  
Vol 311 ◽  
Author(s):  
Robert Sinclair ◽  
Toyohiko J. Konno

ABSTRACTWe have studied the reactions at metal-metalloid interfaces using high resolution transmission electron microscopy, including in situ observation, and differential scanning calorimetry. There is contrasting behavior depending on the affinity for interaction or segregation. For reactive systems, compound formation ultimately results, but this can be preceded by solidstate amorphization. For non-reactive systems, crystallization of the metalloid is often achieved with nucleation and growth mediated by the metal phase.


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