Observations of nanoindents via cross-sectional transmission electron microscopy: a survey of deformation mechanisms

Author(s):  
S.J Lloyd ◽  
A Castellero ◽  
F Giuliani ◽  
Y Long ◽  
K.K McLaughlin ◽  
...  

Examination of cross-sections of nanoindents with the transmission electron microscope has recently become feasible owing to the development of focused ion beam milling of site-specific electron transparent foils. Here, we discuss the development of this technique for the examination of nanoindents and survey the deformation behaviour in a range of single crystal materials with differing resistances to dislocation flow. The principal deformation modes we discuss, in addition to dislocation flow, are phase transformation (silicon and germanium), twinning (gallium arsenide and germanium at 400 °C), lattice rotations (spinel), shear (spinel), lattice rotations (copper) and lattice rotations and densification (TiN/NbN multilayers). The magnitude of the lattice rotation, about the normal to the foil, was measured at different positions under the indents. Indents in a partially recrystallized metallic glass Mg 66 Ni 20 Nd 14 were also examined. In this case a low-density porous region was formed at the indent tip and evidence of shear bands was also found. Further understanding of indentation deformation will be possible with three-dimensional characterization coupled with modelling which takes account of the variety of competing deformation mechanisms that can occur in addition to dislocation glide. Mapping the lattice rotations will be a particularly useful way to evaluate models of the deformation process.

2009 ◽  
Vol 17 (6) ◽  
pp. 20-23 ◽  
Author(s):  
Suhan Kim ◽  
Gao Liu ◽  
Andrew M. Minor

Focused ion beam (FIB) instrumentation has proven to be extremely useful for preparing cross-sectional samples for transmission electron microscopy (TEM) investigations. The two most widely used methods involve milling a trench on either side of an electron-transparent window: the “H-bar” and the “lift-out” methods [1]. Although these two methods are very powerful in their versatility and ability to make site-specific TEM samples, they rely on using a sacrificial layer to protect the surface of the sample as well as the removal of a relatively large amount of material, depending on the size of the initial sample. In this article we describe a technique for making thin film cross-sections with the FIB, known as Shadow FIBing, that does not require the use of a sacrificial layer or long milling times [2].


2013 ◽  
Vol 20 (1) ◽  
pp. 133-140 ◽  
Author(s):  
Filip Lenrick ◽  
Martin Ek ◽  
Daniel Jacobsson ◽  
Magnus T. Borgström ◽  
L. Reine Wallenberg

AbstractFocused ion beam is a powerful method for cross-sectional transmission electron microscope sample preparation due to being site specific and not limited to certain materials. It has, however, been difficult to apply to many nanostructured materials as they are prone to damage due to extending from the surface. Here we show methods for focused ion beam sample preparation for transmission electron microscopy analysis of such materials, demonstrated on GaAs–GaInP core shell nanowires. We use polymer resin as support and protection and are able to produce cross-sections both perpendicular to and parallel with the substrate surface with minimal damage. Consequently, nanowires grown perpendicular to the substrates could be imaged both in plan and side view, including the nanowire–substrate interface in the latter case. Using the methods presented here we could analyze the faceting and homogeneity of hundreds of adjacent nanowires in a single lamella.


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.


Author(s):  
T. Yaguchi ◽  
M. Konno ◽  
T. Kamino ◽  
M. Ogasawara ◽  
K. Kaji ◽  
...  

Abstract A technique for preparation of a pillar shaped sample and its multi-directional observation of the sample using a focused ion beam (FIB) / scanning transmission electron microscopy (STEM) system has been developed. The system employs an FIB/STEM compatible sample rotation holder with a specially designed rotation mechanism, which allows the sample to be rotated 360 degrees [1-3]. This technique was used for the three dimensional (3D) elemental mapping of a contact plug of a Si device in 90 nm technology. A specimen containing a contact plug was shaped to a pillar sample with a cross section of 200 nm x 200 nm and a 5 um length. Elemental analysis was performed with a 200 kV HD-2300 STEM equipped with the EDAX genesis Energy dispersive X-ray spectroscopy (EDX) system. Spectrum imaging combined with multivariate statistical analysis (MSA) [4, 5] was used to enhance the weak X-ray signals of the doped area, which contain a low concentration of As-K. The distributions of elements, especially the dopant As, were successfully enhanced by MSA. The elemental maps were .. reconstructed from the maps.


1987 ◽  
Vol 1 (2) ◽  
pp. 322-329 ◽  
Author(s):  
H. Warshawsky

The purpose of this paper is to review evidence which casts doubt on the interpretation universally applied to hexagonal images seen in sectioned enamel. The evidence is based on two possible models to explain the hexagonal profiles seen in mammalian enamel with transmission electron microscopy. The "hexagonal ribbon" model proposes that hexagonal profiles are true cross-sections of elongated hexagonal ribbons. The "rectangular ribbon" model proposes that hexagonal profiles are caused by three-dimensional segments that are parallelepipeds contained in the Epon section. Since shadow projections of such rectangular segments give angles that are inconsistent with the hexagonal unit cell, a model based on ribbons with rhomboidal cut ends and angles of 60 and 120° is proposed. The "rhomboidal ribbon" model projects shadows with angles that are predicted by the unit cell. It is suggested that segments of such crystallites in section project as opaque hexagons on the imaging plane in routine transmission electron microscopy. Morphological observations on crystallites in sections - together with predictions from the hexagonal, rectangular, and rhomboidal ribbon models - indicate that crystallites in rat incisor enamel are flat ribbons with rhomboidal cross-sectional shape. Hexagonal images in electron micrographs of thin-sectioned enamel can result from rhomboidal-ended, parallelepiped-shaped segments of these crystallites projected and viewed as two-dimensional shadows.


2000 ◽  
Vol 6 (3) ◽  
pp. 218-223
Author(s):  
Toshie Yaguchi ◽  
Takeo Kamino ◽  
Mitsumasa Sasaki ◽  
Gerard Barbezat ◽  
Ryoichi Urao

Abstract A focused ion beam (FIB) technique was applied to cross-sectional specimen preparation to observe an interface between a plasma sprayed coating and an aluminum (Al) substrate by transmission electron microscopy (TEM). The surface of the sprayed coating film has a roughness of several tens of microns. Sputter rates for the coating film and the substrate are greatly different. The rough surface and the difference in sputter rate cause problems in making TEM specimens with smooth side walls. The top surface of the coating film was planerized by the FIB before fabricating the TEM specimen. The interfaces were investigated by TEM and energy-dispersive X-ray (EDX) analysis. The TEM observation revealed that there is a 10 nm thick amorphous layer at the interface between the coating film and substrate. The coating film consists of two kinds of sublayers with bright and dark contrast. The bright contrast sublayers were amorphous layers with thickness of 2~10 nm. The Al/Fe X-ray intensity ratio was larger in bright contrast sublayers than that in dark contrast sublayers.


2013 ◽  
Vol 20 (1) ◽  
pp. 42-49 ◽  
Author(s):  
Jiangbo Lu ◽  
Maarten B.J. Roeffaers ◽  
Evelyne Bartholomeeusen ◽  
Bert F. Sels ◽  
Dominique Schryvers

AbstractScanning electron microscopy, focused ion beam (FIB), and transmission electron microscopy are combined to study the intergrowth of 90° rotational components and of ramps in coffin-shaped ZSM-5 crystals. The 90° rotational boundaries with local zig-zag features between different intergrowth components are observed in the main part of crystal. Also a new kind of displacement boundary is described. At the displacement boundary there is a shift of the unit cells along the boundary without a change in orientation. Based on lamellae prepared with FIB from different positions of the ramps and crystal, the orientation relationships between ramps and the main part of the crystal are studied and the three-dimensional morphology and growth mechanism of the ramp are illustrated.


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