A FIB Micro-Sampling Technique and a Site Specific TEM Specimen Preparation Method

Abstract

Abstract:A FIB micro-sampling technique has been developed to facilitate TEM specimen preparation while allowing samples to remain intact. A deep trench is FIB-milled to remove a portion of the sample containing the region of interest. A micromanipulator is employed for the purpose of lifting out a small portion of the sample, i.e., the micro-sample. FIB assisted metal deposition is used to bond the micro-sample to the micromanipulator. The micro-sample is subsequently lifted out and mounted onto an edge of the micro-sample carrier using FIB assisted metal deposition. The micro-sample is then thinned to the thickness of about O.lpm for TEM observation. All of the above steps are accomplished under vacuum in the same FIB system. This procedure is a reliable TEM specimen preparation technique when the evaluation or failure analysis of a specific site is required. Both cross sectional and plan view TEM specimen preparations are feasible with this technique. In addition, a technique to prepare TEM specimens from a specific site has also been developed. In this technique, an FIB system equipped with a FIB/TEM(STEM) compatible specimen holder is used for thinning of the samples, e.g., a micro-sample. The compatible specimen holder permits repeated alternating FIB milling and TEM(STEM) observation, enabling TEM specimen preparation from a specific site.

Newly recognized hosts for uranium in the Hanford Site vadose zone

“…Fifteen elements (Na, Mg, Al, Si, P, K, Ca, Ti, V, Cr, Mn, Fe, Cu, Zr, and U) were analyzed. Uranium hosts were extracted and thinned for transmission electron microscopy (TEM) with an FEI Nova 600 DualBeam focused ion beam (FIB) instrument using an in-situ lift-out technique similar to the ones described by Giannuzzi et al (2005) and Kamino et al (2005). A Philips CM300 FEG TEM, operated at 300 kV, was used for imaging and EDS chemical analysis at a higher spatial resolution than that achievable in the electron microprobe.…”

A Small Spot, Inert Gas, Ion Milling Process as a Complementary Technique to Focused Ion Beam Specimen Preparation

“…The thinning and extraction of TEM specimens with accuracy and site-specificity is an advantage of FIB (Kirk et al, 1989;Young et al, 1990;Basile et al, 1991;Giannuzzi & Stevie, 1999;Anderson & Klepeis, 2005;Kamino et al, 2005;Jia et al, 2014). A significant fraction of the specimens produced at any given laboratory is now prepared using FIB technology.…”

The Total Release Method for FIB In-Situ TEM Sample Preparation

“…More recently, the method for performing the entire TEM sample preparation process within the FIB is known as "in-situ lift-out" and is based on the use of a chamber-mounted nanomanipulator and beam-induced material deposition. [1][2][3][4][5] The use of the FIB offers advantages over conventional mechanical TEM sample preparation. The dual-beam FIB offers the ability to locate the lift-out site with SEM resolution and then use the ion beam to excise the sample without sacrificing the wafer, followed by thinning the extracted sample to the thickness required for TEM inspection.…”