scholarly journals ZrN Phase Formation, Hardening and Nitrogen Diffusion Kinetics in Plasma Nitrided Zircaloy-4

Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3572
Author(s):  
Robert Balerio ◽  
Hyosim Kim ◽  
Andres Morell-Pacheco ◽  
Laura Hawkins ◽  
Ching-Heng Shiau ◽  
...  

Plasma nitridation was conducted to modify the surfaces of Zircaloy-4. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman analysis were used to characterize microstructures and phases. Surface indentation and cross-sectional indentation were performed to evaluate mechanical property changes. Nitridation forms a thin layer of ZrN phase, followed by a much deeper layer affected by nitrogen diffusion. The ZrN phase is confirmed by both TEM and Raman characterization. The Raman peaks of ZrN phase show a temperature dependence. The intensity increases with increasing nitridation temperatures, reaches a maximum at 700 °C, and then decreases at higher temperatures. The ZrN layer appears as continuous small columnar grains. The surface polycrystalline ZrN phase is harder than the bulk by a factor of ~8, and the nitrogen diffusion layer is harder by a factor of ~2–5. The activation energy of nitrogen diffusion was measured to be 2.88 eV. The thickness of the nitrogen-hardened layer is controllable by changing the nitridation temperature and duration.

2010 ◽  
Vol 24 (01n02) ◽  
pp. 18-25 ◽  
Author(s):  
P. C. WO ◽  
P. R. MUNROE ◽  
Z. F. ZHOU ◽  
Z. H. XIE ◽  
K. Y. LI

The deformation microstructures generated by nanoindentation of multilayer coatings consisting of TiSiN layers alternating with ten TiN interlayers, were examined by cross-sectional transmission electron microscopy (XTEM). Two multilayered coatings were studied: a thin TiSiN coating interlayered with thick TiN interlayer and a thick TiSiN coating alternated with thin TiN layers. A monolithic TiSiN coating was also examined for comparison. Surface morphology of the samples was found to be variable. Both surface roughness and coating hardness increase with the thickness of the outermost TiSiN layer. All samples show columnar structures, and for the multilayer coatings, epitaxial growth of these columnar grains through the TiSiN / TiN multilayers was observed. Stair-shaped shear cracks can be seen in the multilayer coating alternated with thick TiN interlayers, whereas radial and edge cracks are observed in the coating multilayered with thin TiN layers and in the monolithic coating. TEM analysis also suggests that columnar grains help to resist the initiation of edge cracks. Compared to other studies on similar coating systems with fewer periods of interlayers, the deformation observed here appears less severe, indicating an improvement in the strength of the coating through increasing the number of interlayers.


Author(s):  
D. L. Callahan ◽  
Z. Ball ◽  
H. M. Phillips ◽  
R. Sauerbrey

Ultraviolet laser-irradiation can be used to induce an insulator-to-conductor phase transition on the surface of Kapton polyimide. Such structures have potential applications as resistors or conductors for VLSI applications as well as general utility electrodes. Although the percolative nature of the phase transformation has been well-established, there has been little definitive work on the mechanism or extent of transformation. In particular, there has been considerable debate about whether or not the transition is primarily photothermal in nature, as we propose, or photochemical. In this study, cross-sectional optical microscopy and transmission electron microscopy are utilized to characterize the nature of microstructural changes associated with the laser-induced pyrolysis of polyimide.Laser-modified polyimide samples initially 12 μm thick were prepared in cross-section by standard ultramicrotomy. Resulting contraction in parallel to the film surface has led to distortions in apparent magnification. The scale bars shown are calibrated for the direction normal to the film surface only.


Author(s):  
F. Shaapur

Non-uniform ion-thinning of heterogenous material structures has constituted a fundamental difficulty in preparation of specimens for transmission electron microscopy (TEM). A variety of corrective procedures have been developed and reported for reducing or eliminating the effect. Some of these techniques are applicable to any non-homogeneous material system and others only to unidirectionalfy heterogeneous samples. Recently, a procedure of the latter type has been developed which is mainly based on a new motion profile for the specimen rotation during ion-milling. This motion profile consists of reversing partial revolutions (RPR) within a fixed sector which is centered around a direction perpendicular to the specimen heterogeneity axis. The ion-milling results obtained through this technique, as studied on a number of thin film cross-sectional TEM (XTEM) specimens, have proved to be superior to those produced via other procedures.XTEM specimens from integrated circuit (IC) devices essentially form a complex unidirectional nonhomogeneous structure. The presence of a variety of mostly lateral features at different levels along the substrate surface (consisting of conductors, semiconductors, and insulators) generally cause non-uniform results if ion-thinned conventionally.


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.


1986 ◽  
Vol 76 ◽  
Author(s):  
L. Dori ◽  
M. Arienzo ◽  
Y. C. Sun ◽  
T. N. Nguyen ◽  
J. Wetzel

ABSTRACTUltrathin silicon dioxide films, 5 nm thick, were grown in a double-walled furnace at 850°C in dry O2. A consistent improvement in the electrical properties is observed following the oxidation either with a Post-Oxidation Anneal (POA) at 1000°C in N2 or with the same POA followed by a short re-oxidation (Re-Ox) step in which 1 nm of additional oxide was grown. We attribute these results to the redistribution of hydrogen and water related groups as well as to a change in the concentration of sub-oxide charge states at the Si-SiO2 interface. A further improvement observed after the short re-oxidation step had been attributed to the filling of the oxygen vacancies produced during the POA. High resolution Transmission Electron Microscopy cross-sectional observations of the Si-iSO2 interface have evidenced an increase in the interface roughness after the thermal treatment at high temperature. These results are in agreement with recent XPS data.


1998 ◽  
Vol 510 ◽  
Author(s):  
R. Jothilingam ◽  
T. Farrell ◽  
T.B. Joyce ◽  
P.J. Goodhew

AbstractWe report the photo modified growth of GaAs by chemical beam epitaxy at substrate temperatures in the range 335 to 670°C using triethygallium (TEG) and arsine. A mercury-xenon lamp (electrical power 200 W) provided the irradiation for the photoassisted growth. The growth was monitored in real time by laser reflectometry (LR) using a 670 nm semiconductor laser, and the optically determined growth rate agreed with that obtained from the layer thickness measured by cross sectional transmission electron microscopy. The observed photo-enhancement of the growth rate at low substrate temperatures and inhibition at high substrate temperatures is thermal in origin, consistent with raising the substrate temperature by 10±3°C. Cross sectional transmission electron microscopy showed that the photoassisted layers are essentially free from dislocations


2008 ◽  
Vol 8 (8) ◽  
pp. 4081-4085 ◽  
Author(s):  
Y. Batra ◽  
D. Kabiraj ◽  
D. Kanjilal

Germanium (Ge) nanoparticles have attracted a lot of attention due to their excellent optical properties. In this paper, we report on the formation of Ge nanoparticles embedded in GeO2 matrix prepared by electron beam evaporation and subsequent annealing. Transmission electron microscopy (TEM) studies clearly indicate the formation of Ge nanocrystals in the films annealed at 500 °C. Fourier transform infrared (FTIR) spectroscopic studies are carried out to verify the evolution of the structure after annealingat each stage. Micro-Raman analysis also confirms the formation of Ge nanoparticles in the annealed films. Development of Ge nanoparticles is also established by photoluminescence (PL) analysis. Surface morphology study is carried out by atomic force microscopy (AFM). It shows the evolution of granular structure of the films with increasing annealing temperature.


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