In-Situ TEM Studies of Sessile Dislocation Arrangements and N Vacancy Ordering in ZrN

2003 ◽  
Vol 779 ◽  
Author(s):  
P. Li ◽  
J.M. Howe

AbstractDissociation of perfect 1/2<110> single dislocations into two 1/6<112> Shockley partial dislocations in ZrN was observed by transmission electron microscopy (TEM). The 1/2<110> single dislocations have a super-jog character and are not coplanar with the dissociated Shockley partials. This sessile arrangement of dislocations may be responsible for the brittleness of ZrN. The wide separation of the partial dislocations bounding stacking faults indicates that the stacking-faults energy (SFE) is low in ZrN. The low SFE can be explained on the basis of a high vacancy concentration, which was confirmed by the appearance of diffuse intensity maxima in electron diffraction patterns due to short-range ordering (SRO) of N vacancies. In-situ heating experiments in the TEM revealed that the diffuse intensity maxima disappear during heating and reappear on cooling. This indicates that N (or N vacancy) diffusion scrambles the SRO arrangement of N vacancies during heating. The width of the stacking faults in ZrN increases with temperature, indicating that the SFE decreases as the vacancy concentration increases.

Author(s):  
Tai D. Nguyen ◽  
Ronald Gronsky ◽  
Jeffrey B. Kortright

Nanometer period Ru/C multilayers are one of the prime candidates for normal incident reflecting mirrors at wavelengths < 10 nm. Superior performance, which requires uniform layers and smooth interfaces, and high stability of the layered structure under thermal loadings are some of the demands in practical applications. Previous studies however show that the Ru layers in the 2 nm period Ru/C multilayer agglomerate upon moderate annealing, and the layered structure is no longer retained. This agglomeration and crystallization of the Ru layers upon annealing to form almost spherical crystallites is a result of the reduction of surface or interfacial energy from die amorphous high energy non-equilibrium state of the as-prepared sample dirough diffusive arrangements of the atoms. Proposed models for mechanism of thin film agglomeration include one analogous to Rayleigh instability, and grain boundary grooving in polycrystalline films. These models however are not necessarily appropriate to explain for the agglomeration in the sub-nanometer amorphous Ru layers in Ru/C multilayers. The Ru-C phase diagram shows a wide miscible gap, which indicates the preference of phase separation between these two materials and provides an additional driving force for agglomeration. In this paper, we study the evolution of the microstructures and layered structure via in-situ Transmission Electron Microscopy (TEM), and attempt to determine the order of occurence of agglomeration and crystallization in the Ru layers by observing the diffraction patterns.


2009 ◽  
Vol 1216 ◽  
Author(s):  
Akifumi Ono ◽  
Shigehito Isobe ◽  
Yongming Wang ◽  
Naoyuki Hashimoto ◽  
Somei Ohnuki

AbstractIn-situ observation on the catalytic effect of Nb2O5 in MgH2 was carried out by using transmission electron microscopy (TEM). We prepared two kinds of samples, because we tried to observe the reaction from two kinds of viewpoints. MgH2 catalyzed with 1 mol% of Nb2O5 was prepared for an overall viewpoint on the desorption process of MgH2 with catalyst by conventional TEM. The dehydrogenation of the 1 mol% sample started at 150 °C and Mg nano-size particles were formed. However, Nb2O5 was not confirmed in diffraction patterns and images, because it was highly dispersed by ball-milled. So MgH2 catalyzed with 10 mol% of Nb2O5 was prepared for local viewpoint to focus the boundary between the catalyst and the Mg phase by high voltage electron micro scope (HVEM). The sample mixed in mortar was prepared for this, because it was difficult to find the boundary in the sample ball-milled. The high resolution images of the 10 mol% sample revealed that the dehydrogenation started from the interface of MgH2 and Nb2O5. The result suggested that the dehydrogenation could proceed with hydrogen diffusion from MgH2 phase to the interface between Mg and Nb2O5.


Author(s):  
F. M. Ross ◽  
R. Hull ◽  
D. Bahnck ◽  
J. C. Bean ◽  
L. J. Peticolas ◽  
...  

We describe an investigation of the electrical properties of interfacial dislocations in strained layer heterostructures. We have been measuring both the structural and electrical characteristics of strained layer p-n junction diodes simultaneously in a transmission electron microscope, enabling us to correlate changes in the electrical characteristics of a device with the formation of dislocations.The presence of dislocations within an electronic device is known to degrade the device performance. This degradation is of increasing significance in the design and processing of novel strained layer devices which may require layer thicknesses above the critical thickness (hc), where it is energetically favourable for the layers to relax by the formation of misfit dislocations at the strained interfaces. In order to quantify how device performance is affected when relaxation occurs we have therefore been investigating the electrical properties of dislocations at the p-n junction in Si/GeSi diodes.


Author(s):  
Raja Subramanian ◽  
Kenneth S. Vecchio

The structure of stacking faults and partial dislocations in iron pyrite (FeS2) have been studied using transmission electron microscopy. Pyrite has the NaCl structure in which the sodium ions are replaced by iron and chlorine ions by covalently-bonded pairs of sulfur ions. These sulfur pairs are oriented along the <111> direction. This covalent bond between sulfur atoms is the strongest bond in pyrite with Pa3 space group symmetry. These sulfur pairs are believed to move as a whole during dislocation glide. The lattice structure across these stacking faults is of interest as the presence of these stacking faults has been preliminarily linked to a higher sulfur reactivity in pyrite. Conventional TEM contrast analysis and high resolution lattice imaging of the faulted area in the TEM specimen has been carried out.


Author(s):  
S. Hagège ◽  
U. Dahmen ◽  
E. Johnson ◽  
A. Johansen ◽  
V.S. Tuboltsev

Small particles of a low-melting phase embedded in a solid matrix with a higher melting point offer the possibility of studying the mechanisms of melting and solidification directly by in-situ observation in a transmission electron microscope. Previous studies of Pb, Cd and other low-melting inclusions embedded in an Al matrix have shown well-defined orientation relationships, strongly faceted shapes, and an unusual size-dependent superheating before melting.[e.g. 1,2].In the present study we have examined the shapes and thermal behavior of eutectic Pb-Cd inclusions in Al. Pb and Cd form a simple eutectic system with each other, but both elements are insoluble in solid Al. Ternary alloys of Al (Pb,Cd) were prepared from high purity elements by melt spinning or by sequential ion implantation of the two alloying additions to achieve a total alloying addition of up to lat%. TEM observations were made using a heating stage in a 200kV electron microscope equipped with a video system for recording dynamic behavior.


Author(s):  
M. Park ◽  
S.J. Krause ◽  
S.R. Wilson

Cu alloying in Al interconnection lines on semiconductor chips improves their resistance to electromigration and hillock growth. Excess Cu in Al can result in the formation of Cu-rich Al2Cu (θ) precipitates. These precipitates can significantly increase corrosion susceptibility due to the galvanic action between the θ-phase and the adjacent Cu-depleted matrix. The size and distribution of the θ-phase are also closely related to the film susceptibility to electromigration voiding. Thus, an important issue is the precipitation phenomena which occur during thermal device processing steps. In bulk alloys, it was found that the θ precipitates can grow via the grain boundary “collector plate mechanism” at rates far greater than allowed by volume diffusion. In a thin film, however, one might expect that the growth rate of a θ precipitate might be altered by interfacial diffusion. In this work, we report on the growth (lengthening) kinetics of the θ-phase in Al-Cu thin films as examined by in-situ isothermal aging in transmission electron microscopy (TEM).


2021 ◽  
Vol 10 (3) ◽  
pp. 578-586
Author(s):  
Lin-Kun Shi ◽  
Xiaobing Zhou ◽  
Jian-Qing Dai ◽  
Ke Chen ◽  
Zhengren Huang ◽  
...  

AbstractA nano-laminated Y3Si2C2 ceramic material was successfully synthesized via an in situ reaction between YH2 and SiC using spark plasma sintering technology. A MAX phase-like ternary layered structure of Y3Si2C2 was observed at the atomic-scale by high resolution transmission electron microscopy. The lattice parameters calculated from both X-ray diffraction and selected area electron diffraction patterns are in good agreement with the reported theoretical results. The nano-laminated fracture of kink boundaries, delamination, and slipping were observed at the tip of the Vickers indents. The elastic modulus and Vickers hardness of Y3Si2C2 ceramics (with 5.5 wt% Y2O3) sintered at 1500 °C were 156 and 6.4 GPa, respectively. The corresponding values of thermal and electrical conductivity were 13.7 W·m-1·K-1 and 6.3×105 S·m-1, respectively.


Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3727
Author(s):  
Huanhuan He ◽  
Zhiwei Lin ◽  
Shengming Jiang ◽  
Xiaotian Hu ◽  
Jian Zhang ◽  
...  

The FeCoNiCrTi0.2 high-entropy alloys fabricated by vacuum arc melting method, and the annealed pristine material, are face centered cubic structures with coherent γ’ precipitation. Samples were irradiated with 50 keV He+ ions to a fluence of 2 × 1016 ions/cm2 at 723 K, and an in situ annealing experiment was carried out to monitor the evolution of helium bubbles during heating to 823 and 923 K. The pristine structure of FeCoNiCrTi0.2 samples and the evolution of helium bubbles during in situ annealing were both characterized by transmission electron microscopy. The annealing temperature and annealing time affect the process of helium bubbles evolution and formation. Meanwhile, the grain boundaries act as sinks to accumulate helium bubbles. However, the precipitation phase seems have few effects on the helium bubble evolution, which may be due to the coherent interface and same structure of γ’ precipitation and matrix.


1998 ◽  
Vol 554 ◽  
Author(s):  
J. A. Horton ◽  
J. L. Wright ◽  
J. H. Schneibel

AbstractThe fracture behavior of a Zr-based bulk amorphous alloy, Zr-10 Al-5 Ti-17.9 Cu-14.6Ni (at.%), was examined by transmission electron microscopy (TEM) and x-ray diffraction forany evidence of crystallization preceding crack propagation. No evidence for crystallizationwas found in shear bands in compression specimens or at the fracture surface in tensile specimens.In- situ TEM deformation experiments were performed to more closely examine actualcrack tip regions. During the in-situ deformation experiment, controlled crack growth occurredto the point where the specimen was approximately 20 μm thick at which point uncontrolledcrack growth occurred. No evidence of any crystallization was found at the crack tips or thecrack flanks. Subsequent scanning microscope examination showed that the uncontrolledcrack growth region exhibited ridges and veins that appeared to have resulted from melting. Performing the deformations, both bulk and in-situ TEM, at liquid nitrogen temperatures (LN2) resulted in an increase in the amount of controlled crack growth. The surface roughness of the bulk regions fractured at LN2 temperatures corresponded with the roughness of the crack propagation observed during the in-situ TEM experiment, suggesting that the smooth-appearing room temperature fracture surfaces may also be a result of localized melting.


Further experiments by transmission electron microscopy on thin sections of stainless steel deformed by small amounts have enabled extended dislocations to be observed directly. The arrangement and motion of whole and partial dislocations have been followed in detail. Many of the dislocations are found to have piled up against grain boundaries. Other observations include the formation of wide stacking faults, the interaction of dislocations with twin boundaries, and the formation of dislocations at thin edges of the foils. An estimate is made of the stacking-fault energy from a consideration of the stresses present, and the properties of the dislocations are found to be in agreement with those expected from a metal of low stacking-fault energy.


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