In situ Transmission Electron Microscopy Observations of Toughening Mechanisms in Ultra-fine Grained Columnar Aluminum Thin Films

2005 ◽  
Vol 20 (7) ◽  
pp. 1869-1877 ◽  
Author(s):  
K. Hattar ◽  
J. Han ◽  
M.T.A. Saif ◽  
I.M. Robertson

A unique straining device, fabricated using microlithographic techniques, has been developed to permit real-time investigation in the transmission electron microscope (TEM) of the deformation and failure mechanisms in ultrafine-grained aluminum. The tensile specimen is a freestanding thin film with a columnar microstructure that has a uniform cross-section (100 × 0.125 μm) and a gauge length of 300 μm. In situ TEM straining experiments show the fracture mode is intergranular with no accompanying general plasticity. Propagating cracks were halted at large grains, and crack blunting occurred through grain-boundary-mediated processes. The blunting process was accompanied by dislocation emission and deformation twinning in the grain responsible for arresting the crack. Voids or microcracks nucleated and grew on grain boundaries ahead of the arrested crack, and crack advance occurred through linkage of the microcracks and the primary crack.

2005 ◽  
Vol 907 ◽  
Author(s):  
Khalid Hattar ◽  
J H Han ◽  
D M Follstaedt ◽  
S J Hearne ◽  
T A Saif ◽  
...  

AbstractThe deformation and failure processes in ultra-fine and nanograined metals over different length scales have been probed using transmission electron microscopy (TEM) and scanning electron microscopy (SEM) in combination with a micromechanical in situ straining device. This novel straining device affords the opportunity to directly correlate the macroscopic mechanical properties with the microscopic deformation and failure mechanisms. Through use of this device it has been shown that increased film thickness results in a transition between limited plasticity and intergranular fracture to global plasticity and shear failure for deposited aluminum samples of similar grain size but different thickness.


Author(s):  
P. Nagpal ◽  
I. Baker

The purpose of this paper is to present a comparison of the dislocation structures that are present in polycrystalline samples of the B2 (ordered body-centered cubic) compound NiAI after straining in bulk and after in-situ straining of thin foils in the TEM.A dumbell-shaped tensile specimen (gauge length ∼ 10mm; diameter ∼ 3mm) of ∼15μm grain-sized stoichiometric NiAl which had a low initial dislocation density was strained to fracture under tension. The fracture strain was ∼ 2%. Discs were cut from the gauge and thin foils were prepared as described elsewhere. (Processing conditions to obtain this fine-grained material are also described elsewhere.) TEM in-situ straining samples (7mm long; 3 mm wide; 0.25 mm thick, with 1mm diameter loading holes located 1.5mm from the ends, see reference 4 for details) were prepared from the same material and strained in a modified JEOL straining holder. Both sets of samples were viewed in a JEOL 2000FX operated at 200 KeV. For the in-situ experiments images were recorded either on film after a given strain increment or dynamically during straining using a Gatan camera, an image intensifier and a VCR.


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):  
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.


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).


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.


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.


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