In situ Tensile Testing of Nanoscale Freestanding Thin Films Inside a Transmission Electron Microscope

2005 ◽  
Vol 20 (7) ◽  
pp. 1769-1777 ◽  
Author(s):  
M.A. Haque ◽  
M.T.A. Saif
Keyword(s):  
Stress Measurement ◽  
Crystallographic Analysis ◽  
Uniaxial Tensile ◽  
In Situ Tem ◽  
Sensors And Actuators ◽  
Displacement Sensors ◽  
Thin Foils ◽  
Transmission Electron ◽  
Tensile Experiment

The unique capability of rendering opaque specimens transparent with atomic resolution makes transmission electron microscopy (TEM) an indispensable toolfor microstructural and crystallographic analysis of materials. Conventional TEM specimens are placed on grids about 3 mm in diameter and 10–100 μm thick. Such stringent size restriction has precluded mechanical testing inside the TEM chamber.So far, in situ testing of nanoscale thin foils has been mostly qualitative. Micro-electro-mechanical systems (MEMS) offer an unprecedented level of miniaturization to realize sensors and actuators that can add TEM visualization to nano-mechanical characterization. We present a MEMS-based uniaxial tensile experiment setup that integrates nanoscale freestanding specimens with force and displacement sensors, which can be accommodated by a conventional TEM straining stage. In situ TEM testing on 100-nm-thick freestanding aluminum specimens (with simultaneous stress measurement) show limited dislocation activity in the grain interior and consequent brittle mode of fracture. Plasticity at this size scale is contributed by grain boundary dislocations and partial dislocations.

In-situ TEM Observation of Formation-Retraction-Fracture Experiment of Liquid-Like Silicon Nanocontact

2011 ◽  
Vol 1318 ◽  
Author(s):  
Tadashi Ishida ◽  
Kuniyuki Kakushima ◽  
Hiroyuki Fujita
Keyword(s):  
Bias Voltage ◽  
Mechanical Characteristics ◽  
In Situ Tem ◽  
Mechanical Contact ◽  
Transmission Electron ◽  
Close Observation ◽  
High Bias ◽  
Pre Treatment ◽  
Tensile Experiment

ABSTRACTWe have examined the change of mechanical characteristics of silicon nanocontacts with and without the pre-treatment by flowing current through the contact. The silicon nanocontact formed between silicon tips by a mechanical contact was quickly deformed during its tensile test under a transmission electron microscope, after applying over 100 μA at a high bias voltage around 15 V between tips for a short duration. In the tensile experiment, the diameter of the nanocontact easily decreased from the initial diameter of 98 nm to 30 nm and the length increased from 11 nm to 66 nm. At 30 nm in diameter, it was suddenly fractured without further elongation and became round tips with smooth surfaces. According to the close observation, the silicon nanocontact seemed amorphous. In the retraction process of the silicon nanocontact, steps moved along the surface from the neck of the nanocontact to the tip side at the speed of 7.0 nm/s. Nano-scaled round step propagations were repeated from the neck to the tip. The step propagation caused the fast thinning of the nanocontact. On the other hand, the silicon nanocontact formed at 1 V in bias voltage was gradually thinned from 42.5 nm to 1.6 nm in diameter and elongated from 2.9 nm to 61.9 nm in length. From the comparison of silicon nanocontacts with and without the pre-treatment, the silicon nanocontact after flowing substantial current showed quick deformation and had different mechanical characteristics from the silicon nanocontact without the pre-treatment.

In situ TEM measurements of the electrical properties of interface dislocations

1992 ◽  
Vol 50 (2) ◽  
pp. 1338-1339
Author(s):  
F. M. Ross ◽  
R. Hull ◽  
D. Bahnck ◽  
J. C. Bean ◽  
L. J. Peticolas ◽  
...  
Keyword(s):  
Electrical Properties ◽  
Electronic Device ◽  
In Situ Tem ◽  
Device Performance ◽  
Misfit Dislocations ◽  
Electrical Characteristics ◽  
Strained Layer ◽  
Transmission Electron ◽  
Interfacial Dislocations

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.

In situ TEM Studies of agglomeration of sub-nanometer Ru layers in Ru/C multilayers

1992 ◽  
Vol 50 (1) ◽  
pp. 256-257
Author(s):  
Tai D. Nguyen ◽  
Ronald Gronsky ◽  
Jeffrey B. Kortright
Keyword(s):  
Layered Structure ◽  
Driving Force ◽  
High Energy ◽  
Superior Performance ◽  
In Situ Tem ◽  
Rayleigh Instability ◽  
Practical Applications ◽  
Transmission Electron ◽  
Diffraction Patterns

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.

In situ TEM observations of melting in nanosized eutectic Pb-Cd inclusions embedded in Al

1996 ◽  
Vol 54 ◽  
pp. 986-987
Author(s):  
S. Hagège ◽  
U. Dahmen ◽  
E. Johnson ◽  
A. Johansen ◽  
V.S. Tuboltsev
Keyword(s):  
Electron Microscope ◽  
Melt Spinning ◽  
Ternary Alloys ◽  
Solid Matrix ◽  
Eutectic System ◽  
In Situ Tem ◽  
In Situ Observation ◽  
Orientation Relationships ◽  
Transmission Electron

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.

Growth kinetics of Al2Cu in an Al-1.5Cu thin film by in Situ TEM

1993 ◽  
Vol 51 ◽  
pp. 1172-1173
Author(s):  
M. Park ◽  
S.J. Krause ◽  
S.R. Wilson
Keyword(s):  
Thin Film ◽  
In Situ Tem ◽  
Collector Plate ◽  
Transmission Electron ◽  
Device Processing ◽  
Corrosion Susceptibility ◽  
Precipitation Phenomena ◽  
Semiconductor Chips ◽  
Kinetics Of

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).

scholarly journals In-Situ TEM Annealing Observation of Helium Bubble Evolution in Pre-Irradiated FeCoNiCrTi0.2 Alloys

Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3727
Author(s):  
Huanhuan He ◽  
Zhiwei Lin ◽  
Shengming Jiang ◽  
Xiaotian Hu ◽  
Jian Zhang ◽  
...  
Keyword(s):  
Vacuum Arc ◽  
In Situ Tem ◽  
Face Centered Cubic ◽  
Helium Bubble ◽  
High Entropy ◽  
Helium Bubbles ◽  
Transmission Electron ◽  
Bubble Evolution ◽  
Face Centered

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.

scholarly journals In situ TEM thermal annealing of high purity Fe10wt%Cr alloy thin foils implanted with Ti and O ions

2019 ◽  
Vol 461 ◽  
pp. 219-225
Author(s):  
Martin Owusu-Mensah ◽  
Stéphanie Jublot-Leclerc ◽  
Aurélie Gentils ◽  
Cédric Baumier ◽  
Joël Ribis ◽  
...  
Keyword(s):  
Thermal Annealing ◽  
High Purity ◽  
In Situ Tem ◽  
Thin Foils

scholarly journals Fracture in Bulk Amorphous Alloys

1998 ◽  
Vol 554 ◽  
Author(s):  
J. A. Horton ◽  
J. L. Wright ◽  
J. H. Schneibel
Keyword(s):  
Crack Propagation ◽  
Crack Growth ◽  
Shear Bands ◽  
Bulk Amorphous Alloy ◽  
In Situ Tem ◽  
X Ray Diffraction ◽  
Transmission Electron ◽  
Crack Tips ◽  
Temperature Fracture

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.

scholarly journals Electron Microscopy Investigation of Magnetization Process in Thin Foils and Nanostructures

2007 ◽  
Vol 1026 ◽  
Author(s):  
Pascale Bayle-Guillemaud ◽  
Aurelien Masseboeuf ◽  
Fabien Cheynis ◽  
Jean-Christophe Toussaint ◽  
Olivier Fruchart ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Magnetic Anisotropy ◽  
Magnetic Induction ◽  
Perpendicular Magnetic Anisotropy ◽  
In Situ Observation ◽  
Magnetic Imaging ◽  
Thin Foils ◽  
Transmission Electron

AbstractThis paper presents investigations of magnetization configuration evolution during in-situ magnetic processes in materials exhibiting planar and perpendicular magnetic anisotropy. Transmission electron microscopy has been used to perform magnetic imaging. Fresnel contrasts in Lorentz Transmission Electron Microscopy (LTEM) and phase retrieval methods such as Transport of Intensity Equation (TIE) solving or electron holography have been implemented. These techniques are sensitive to magnetic induction perpendicular to the electron beam and can give access to a spatially resolved (resolution better than 10 nm) mapping of magnetic induction distribution and could be extended to dynamical studies during in-situ observation. Thin foils of FePd alloys with a strong perpendicular magnetic anisotropy (PMA) and self-assembled Fe dots are presented. Both are studied during magnetization processes exhibiting the capacities of in-situ magnetic imaging in a TEM.

In-Situ TEM Study of Plastic Stress Relaxation Mechanisms and Interface Effects in Metallic Films

2005 ◽  
Vol 875 ◽  
Author(s):  
Marc Legros ◽  
Gerhard Dehm ◽  
T. John Balk
Keyword(s):  
Thin Films ◽  
High Strength ◽  
Dislocation Motion ◽  
Dislocation Nucleation ◽  
Film Stress ◽  
In Situ Tem ◽  
Metallic Films ◽  
Cross Sectional ◽  
Thin Foils

AbstractTo investigate the origin of the high strength of thin films, in-situ cross-sectional TEM deformation experiments have been performed on several metallic films attached to rigid substrates. Thermal cycles, comparable to those performed using laser reflectometry, were applied to thin foils inside the TEM and dislocation motion was recorded dynamically on video. These observations can be directly compared to the current models of dislocation hardening in thin films. As expected, the role of interfaces is crucial, but, depending on their nature, they can attract or repel dislocations. When the film/interface holds off dislocations, experimental values of film stress match those predicted by the Nix-Freund model. In contrast, the attracting case leads to higher stresses that are not explained by this model. Two possible hardening scenarios are explored here. The first one assumes that the dislocation/interface attraction reduces dislocation mobility and thus increases the yield stress of the film. The second one focuses on the lack of dislocation nucleation processes in the case of attracting interfaces, even though a few sources have been observed in-situ.

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