Investigation of Copper Segregation to the Σ5(310)/[001] Symmetric Tilt Grain Boundary in Aluminum

1999 ◽  
Vol 589 ◽  
Author(s):  
Jürgen M. Plitzko ◽  
Geoffrey H. Campbell ◽  
Wayne E. King ◽  
Stephen M. Foiles

AbstractThe Σ5 (31O)/[001] symmetric tilt grain boundary (STGB) in the face centered cubic (FCC) metal aluminum with 1at% copper has been studied. The model grain boundary has been fabricated by ultra-high vacuum diffusion bonding of alloy single crystals. The segregation of the copper has been encouraged by annealing the sample after bonding at 200 °C. TEM samples of this FCCmaterial were prepared with a new low voltage ion mill under very low angles.The atomic structure of the Σ5(310)/[001] STGB for this system was modeled with electronic structure calculations. These theoretical calculations of the interface structure indicate that the Cu atoms segregate to distinct sites at the interface. High resolution electron microscopy (HRTEM) and analytical electron microscopy including electron energy spectroscopic imaging and X-ray energy dispersive spectrometry have been used to explore the segregation to the grain boundary. The HRTEM images and the analytical measurements were performed using different kinds of microscopes, including a Philips CM300 FEG equipped with an imaging energy filter. The amount of the segregated species at the interface was quantified in a preliminary way. To determine the atomic positions of the segregated atoms at the interface, HRTEM coupled with image simulation and a first attempt of a holographic reconstruction from a through-focal series have been used.

1990 ◽  
Vol 209 ◽  
Author(s):  
Wayne E. King ◽  
G. H. Campbell ◽  
A. Coombs ◽  
M. J. Mills ◽  
M. RüHle

ABSTRACTRecent atomistic simulations using interatomic potentials for Nb developed employing the embedded atom method (EAM) and the model generalized pseudopotential theory (MGPT) have indicated a possible cusp at the Σ5(310) orientation in the energy vs tilt angle curves for<001> symmetric tilt grain boundaries. In addition, the most stable structure predicted using EAM exhibits shifts of one crystal relative to the other along the tilt axis and along the direction perpendicular to the tilt axis lying in the boundary plane. The structure predicted using the MGPT was mirror symmetric across the plane of the grain boundary. This boundary has been prepared for experimental study using the ultra high vacuum diffusion bonding method. A segment of this boundary has been studied using high resolution electron microscopy.


Author(s):  
G. Shimaoka ◽  
J. W. Lane

Recent electron microscopy and diffraction studies of vacuum-deposited films have demonstrated the importance of temperature and surface condition of substrate in determining film structure and growth. Many interesting results of thin epitaxial films of face-centered cubic metals such as gold and silver have been reported. But, relatively few studies of copper have been made. The purpose of this study is to investigate structure and epitaxy of copper thin films evaporated onto various single-crystal substrates in an ultra-high vacuum.High purity copper was evaporated onto freshly cleaved (0001)MoS2, (100)NaC1, (001)mica and (11)CaF2 surfaces heated at temperatures between ∼25° and 200°C in a vacuum of ∼10-8 Torr. Average thickness of deposited films was about 90 Å. Deposition rate was about 0.4 Å/sec. The films were studied by reflection electron diffraction and transmission electron microscopy. Oxidation of copper films during preparation for electron microscopy and diffraction observation was minimized by deposition of thin layer of amorphous carbon upon freshly formed copper films.


2001 ◽  
Vol 7 (S2) ◽  
pp. 246-247
Author(s):  
J. M. Plitzko ◽  
G. H. Campbell ◽  
W. E. King ◽  
S. M. Foiles ◽  
C. Kisielowski

The phenomenon of segregation is of long standing scientific interest and has been studied extensively, both theoretically as well as experimentally. For our investigations we have chosen the Σ5 symmetric tilt grain boundaries (STGB) in two face-centered cubic (FCC) metals, aluminum and copper. Both metals were doped with only 1 at% of the impurity species (Cu and Ag). One of our major goals in this study was to investigate the size effect on segregation of an impurity to distinct sites at the grain boundary. Therefore we have selected the Ag as an impurity in Cu and Cu as an impurity in Al. The latter one is of special interest for applications like interconnects in microcircuits, where one of the major controlling factors of electromigration is expected to be the diffusion or segregation of Cu atoms at Al grain boundaries.The model grain boundaries have been fabricated with ultra-high vacuum diffusion bonding of single crystals which bonds the bicrystals under highly controlled environmental conditions.


Author(s):  
J. C. H. Spence ◽  
X. Zhang ◽  
J. M. Zuo ◽  
U. Weierstall ◽  
E. Munro ◽  
...  

The limited penetration of the low-voltage point-projection microscope (PPM) may be avoided by using the reflection geometry to image clean surfaces in ultra-high vacuum. Figure 1 shows the geometry we are using for experimental point-reflection (PRM) imaging. A nanotip field-emitter at about 100 - 1000 volts is placed above a grounded atomically flat crystalline substrate, which acts as a mirror and anode. Since most of the potential is dropped very close to the tip, trajectories are reasonably straight if the sample is in the far-field of the tip. A resolution of 10 nm is sought initially. The specular divergent RHEED beam then defines a virtual source S' below the surface, resulting in an equivalent arrangement to PPM (or defocused CBED). Shadow images of surface asperities are then expected on the distant detector, out of focus by the tip-to-sample distance. These images can be interpreted as in-line electron holograms and so reconstructed (see X. Zhang et al, these proceedings). Optical analog experiments confirm the absence of foreshortening when the detector is parallel to the surface.


Author(s):  
M. Gajdardziska-Josifovska ◽  
B. G. Frost ◽  
E. Völkl ◽  
L. F. Allard

Polar surfaces are those crystallographic faces of ionically bonded solids which, when bulk terminated, have excess surface charge and a non-zero dipole moment perpendicular to the surface. In the case of crystals with a rock salt structure, {111} faces are the exemplary polar surfaces. It is commonly believed that such polar surfaces facet into neutral crystallographic planes to minimize their surface energy. This assumption is based on the seminal work of Henrich which has shown faceting of the MgO(111) surface into {100} planes giving rise to three sided pyramids that have been observed by scanning electron microscopy. These surfaces had been prepared by mechanical polishing and phosphoric acid etching, followed by Ar+ sputtering and 1400 K annealing in ultra-high vacuum (UHV). More recent reflection electron microscopy studies of MgO(111) surfaces, annealed in the presence of oxygen at higher temperatures, have revealed relatively flat surfaces stabilized by an oxygen rich reconstruction. In this work we employ a combination of optical microscopy, transmission electron microscopy, and electron holography to further study the issue of surface faceting.


Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.


Author(s):  
Jean-Luc Rouvière ◽  
Alain Bourret

The possible structural transformations during the sample preparations and the sample observations are important issues in electron microscopy. Several publications of High Resolution Electron Microscopy (HREM) have reported that structural transformations and evaporation of the thin parts of a specimen could happen in the microscope. Diffusion and preferential etchings could also occur during the sample preparation.Here we report a structural transformation of a germanium Σ=13 (510) [001] tilt grain boundary that occurred in a medium-voltage electron microscopy (JEOL 400KV).Among the different (001) tilt grain boundaries whose atomic structures were entirely determined by High Resolution Electron Microscopy (Σ = 5(310), Σ = 13 (320), Σ = 13 (510), Σ = 65 (1130), Σ = 25 (710) and Σ = 41 (910), the Σ = 13 (510) interface is the most interesting. It exhibits two kinds of structures. One of them, the M-structure, has tetracoordinated covalent bonds and is periodic (fig. 1). The other, the U-structure, is also tetracoordinated but is not strictly periodic (fig. 2). It is composed of a periodically repeated constant part that separates variable cores where some atoms can have several stable positions. The M-structure has a mirror glide symmetry. At Scherzer defocus, its HREM images have characteristic groups of three big white dots that are distributed on alternatively facing right and left arcs (fig. 1). The (001) projection of the U-structure has an apparent mirror symmetry, the portions of good coincidence zones (“perfect crystal structure”) regularly separate the variable cores regions (fig. 2).


2018 ◽  
Vol 148 ◽  
pp. 141-148 ◽  
Author(s):  
Jian Yin ◽  
Yi Wang ◽  
Xiaohan Yan ◽  
Huaiyu Hou ◽  
Jing Tao Wang

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