Abstract:The focused ion beam~FIB! tool has been successfully used as both a stand alone analytical instrument and a means to prepare specimens for subsequent analysis by SEM, TEM, SIMS, XPS, and AUGER.In this work, special emphasis is given to TEM specimen preparation by the FIB lift-out technique. The fundamental ion/solid interactions that govern the FIB milling process are examined and discussed with respect to the preparation of electron transparent membranes. TRIM, a Monte Carlo simulation code, is used to physically model variables that influence FIB sputtering behavior. The results of such computer generated models are compared with empirical observations in a number of materials processed with an FEI 611 FIB workstation. The roles of incident ion attack angle, beam current, trench geometry, raster pattern, and target-material-dependent removal rates are considered. These interrelationships are used to explain observed phenomena and predict expected milling behaviors, thus increasing the potential for the FIB to be used more efficiently with reproducible results.
Particles of Zn powder have been studied to show that high-quality scanning electron microscope (SEM) and transmission electron microscope (TEM) specimens can be rapidly produced from a sitespecific region on a chosen particle by the focused ion beam (FIB) lift-out technique. A TEM specimen approximately 20-m long by 5-m wide was milled to electron transparency, extracted from the bulk particle, and micromanipulated onto a carbon coated copper mesh TEM grid. Using the FIB lift-out method, we were able to prepare a site-specific TEM specimen from a difficult material in under 3 hours. The TEM analysis of the lift-out specimen revealed a large amount of thin area free from characteristic signs of damage that may be observed as a result of conventional argon ion milling. The overall microstructure of the specimen prepared by the FIB lift-out method was consistent with samples prepared by conventional metallographic methods. A grain size of ϳ10 to 20 m was observed in all specimens by both TEM and SEM analysis. Light optical microscopy revealed the presence of internal voids in ϳ10 to 20 pct of all particles. The SEM analysis showed the voids to extend over ϳ70 pct of the particle volume in some cases.
Commercially available focused ion beam (FIB) workstations with spatial resolution of 5-7 nm can prepare specimens with excellent lateral resolution. This capability has been utilized extensively by the semiconductor industry to obtain materials characterization from continually smaller areas. The FIB has been adopted generally as a preparation tool for scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The ability to prepare site-specific specimens that can be removed from the bulk of a sample provides enhanced SEM and TEM analyses and new approaches for other analytical tools. Dedicated scanning transmission electron microscopy (STEM) can provide images through samples several micrometers thick. Auger electron spectroscopy (AES) can analyze with improved ability to identify a small particle. Secondary ion mass spectrometry (SIMS) can provide trace analysis at high mass resolution. Automatic operation of FIB workstations permits the creation of multiple lift-out samples without the presence of an operator.
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Localized plan view TEM samples have been prepared from silicon semiconductor wafers using the focused ion beam lift-out technique. Two different methods of sample preparation before FIB machining were found to be successful: mounting cleaved samples sandwiched together or adding silver paint and cleaving through paint and samples. The plan view technique offers site specific TEM capability from a horizontal section rather than a vertical cross section. The sections can be taken from any layer and can be angled if desired. Results have been obtained from metal layers in a semiconductor device structure. TEM micrographs of tungsten plug arrays show non-uniform barrier layer coverage and tungsten grain size across the via. Hundreds of plugs have been cut through in one sample, thereby offering statistical as well as specific structural information. Metal and polysilicon lines have been examined for grain size and uniformity in a single micrograph. Plan view samples from continuous metal layers can also be made.
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