In-Situ TEM Observation of Electromigration Damage by Surface or Interface Diffusion in Al and Al Alloy Films

1991 ◽  
Vol 225 ◽  
Author(s):  
C. Y. Chang ◽  
R. W. Vook

ABSTRACTIn-situ transmission electron microscope (TEM) electromigration damage (EMD) tests were performed on pure Al films which were thermally evaporated onto oxidized silicon wafers under different deposition conditions. Three different aluminum alloy films, Al-2wt%Cu, Al-8wt%Cu, and Al-2wt%Cu-lwt%Si were also examined. TEM images were recorded photographically and by a video camcorder. The sample stripes were stressed by a high DC current density (≈1.5 MA/cm2). A linear temperature ramp (5°C/min) was supplied by an external, computer controlled heater. The morphology of EMD-induced voids was found to be strongly dependent on microstructure. In small grain size Al stripes, EMD occurred by the formation of void “fingers” which propagated in an almost random manner. In large grain size Al and Al alloy stripes, the EMD-elongated voids propagated approximately parallel to each other and along the field direction. They were preceded with clearly identifiable local thinning. The thinned regions often had crystallographic edges. Contrary to the commonly held belief that EMD occurs only by a grain boundary diffusion mechanism, the present study clearly shows that surface or interface diffusion was the dominant, latter stage EMD failure mode in large grain size films.

2002 ◽  
Vol 721 ◽  
Author(s):  
A. Gungor ◽  
K. Barmak ◽  
A. D. Rollett ◽  
C. Cabral ◽  
J. M. E. Harper

AbstractAnnealing Cu and dilute Cu(Ti), Cu(Sn) and Cu(Al) alloy films resulted in the strengthening of film texture, with the strongest <111> fiber texture being found for Cu(Ti). Annealing also resulted in a decrease of electrical resistivity and the growth of grains, with the largest grain size and lowest resistivity being seen for pure Cu itself. Among the alloy films, the lowest resistivity was found for Cu(Ti) and the largest grain size for Cu(Al). Electron beam evaporated films with compositions in the range of 2.0-3.0 at% and thicknesses in the range of 420-540 nm were annealed at 400°C for 5 hours. Four point probe resistance measurement, xray diffraction and transmission electron microscopy were used to follow the changes in film resistivity, texture and grain size.


CORROSION ◽  
10.5006/3457 ◽  
2020 ◽  
Vol 76 (5) ◽  
pp. 464-475 ◽  
Author(s):  
Shravan K. Kairy ◽  
Nick Birbilis

The role of magnesium silicide (Mg2Si) and silicon (Si) particles in the localized corrosion of aluminum (Al) alloys was investigated herein. Sub-micrometer-sized Mg2Si and Si particles were grown in the Al matrix of Al-Mg-Si and Al-Si alloys, respectively, and characterized by transmission electron microscopy (TEM). A quasi in situ TEM technique was used to study an identical location containing Mg2Si or Si particle in the Al matrix, prior to and following a period of immersion in 0.1 M NaCl at pH 6, 2, and 12. At pH 6 and 2, Mg2Si was initially “anodic,” preferentially dealloying via selective dissolution of Mg, resulting in the development of SiO-rich remnants that are electrochemically inert. The SiO-rich remnants at pH 2 physically detached from the Al matrix. Silicon particles were electrochemically inert at pH 6, while “cathodic” at pH 2, dissolving the Al matrix at their periphery. It was observed that copper (Cu) was redeposited on Si particles at pH 2. At pH 12, Mg2Si and Si were “cathodic” to the Al matrix. This study clarifies, and provides new insights into, the characteristics of Al alloy physical manifestation of corrosion associated with Mg2Si and Si at the nanoscale.


1995 ◽  
Vol 382 ◽  
Author(s):  
Toshio Itoh ◽  
Robert Sinclair

ABSTRACTReactions between Fe and amorphous carbon (a-C) below 600ºC have been investigated. In situ annealing in a transmission electron microscopy (TEM) was performed on a-C/Fe/a-C trilayer films deposited by DC sputtering. As-deposited films showed a well defined tri-layered structure and an average Fe grain size of about 50Å. Cementite (Fe3C) grains appeared in the Fe layer by annealing around 300ºC. As the annealing temperature was raised, the number and size of the cementite grains increased. When the annealing temperature reached 500ºC, the Fe layer completely turned into cementite with an average grain size of 1000Å. At this point the film still kept a well defined tri-layered structure even though some parts of the cementitelayer agglomerated. Above 500ºC, the cementite layer started to “move” into the a-C leaving graphite behind. Graphite formed in this process is strongly textured with the (0002) graphite basal planes parallel to the surface of the moving cementite. This process is concluded to be carbide mediated crystallization of a-C, similar to silicide mediated crystallization of silicon in Ni-Si and Pd-Si systems.


2017 ◽  
Vol 62 (1) ◽  
pp. 5-9 ◽  
Author(s):  
T. Bončina ◽  
F. Zupanič

Abstract Precipitation kinetics and mechanisms within an Al-Mn-Be-Cu quasicrystal strengthened alloy at 300°C were studied using in-situ transmission electron microscopy. The alloy was cast into a copper mould. Quasicrystalline precipitates formed throughout the Al-rich solid solution, whilst heterogeneous formations of Al2Cu and T-phase occurred on icosahedral quasicrystalline particles formed during solidification. The formation of quasicrystalline particles and T-phase was limited by manganese diffusivity, whilst that of Al2Cu by copper diffusivity. The precipitation produced only a small hardening effect.


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.


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