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A sample preparation method is described for enabling direct correlation of site-specific plan-view and cross-sectional transmission electron microscopy (TEM) analysis of individual nanostructures by employing a dual-beam focused-ion beam (FIB) microscope. This technique is demonstrated using Si nanowires dispersed on a TEM sample support (lacey carbon or Si-nitride). Individual nanowires are first imaged in the plan-view orientation to identify a region of interest; in this case, impurity atoms distributed at crystalline defects that require further investigation in the cross-sectional orientation. Subsequently, the region of interest is capped with a series of ex situ and in situ deposited layers to protect the nanowire and facilitate site-specific lift-out and cross-sectioning using a dual-beam FIB microscope. The lift-out specimen is thinned to electron transparency with site-specific positioning to within ∼200 nm of a target position along the length of the nanowire. Using the described technique, it is possible to produce correlated plan-view and cross-sectional view lattice-resolved TEM images that enable a quasi-3D analysis of crystalline defect structures in a specific nanowire. While the current study is focused on nanowires, the procedure described herein is general for any electron-transparent sample and is broadly applicable for many nanostructures, such as nanowires, nanoparticles, patterned thin films, and devices.
The development of laser-assisted atom-probe tomography (APT) analysis and new sample preparation approaches have led to significant advances in the characterization of semiconductor materials and device structures by APT. The high chemical sensitivity and three-dimensional spatial resolution of APT makes it uniquely capable of addressing challenges resulting from the continued shrinking of semiconductor device dimensions, the integration of new materials and interfaces, and the optimization of evolving fabrication processes. Particularly pressing concerns include the variability in device performance due to discrete impurity atom distributions, the phase and interface stability in contacts and gate dielectrics, and the validation of simulations of impurity diffusion. This overview of APT of semiconductors features research on metal-silicide contact formation and phase control, silicon field-effect transistors, and silicon and germanium nanowires. Work on silicide contacts to silicon is reviewed to demonstrate impurity characterization in small volumes and indicate how APT can facilitate defect mitigation and process optimization. Impurity contour analysis of a pFET semiconductor demonstrates the site-specificity that is achievable with current APTs and highlights complex device challenges that can be uniquely addressed. Finally, research on semiconducting nanowires and nanowire heterostructures demonstrates the potential for analysis of materials derived from bottom-up synthesis methods.
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