FIB Specimen Preparation for STEM and EFTEM Tomography

Schwarz, Stephen; Giannuzzi, Lucille A.

doi:10.1017/s143192760488752x

Cited by 8 publications

(7 citation statements)

References 2 publications

(2 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The microsampling technique has also been used to prepare cylindrical samples with diameters from hundreds of nanometers to micrometers for STEM and energy-filtered tomography (Schwarz and Giannuzzi, 2004) and 3-D observations (Kamino et al, 2002). Instead of milling a lamella from the piece of material a pillar is prepared.…”

Section: -D Techniquesmentioning

confidence: 99%

Focused ion beams techniques for nanomaterials characterization

Langford

2006

Microscopy Res & Technique

111

View full text Add to dashboard Cite

Focused ion beam and dual platform systems have, over the last 10 years, become a main stay of sample preparation for material analysis. In this article the merits of using these systems are discussed and the three main techniques used to prepare cross-section specimens for transmission electron microscopy (TEM) are both discussed and compared with emphasis being placed on the tricks that users do to make the lamellae as thin as possible and with a minimum of damage at their sidewalls. Other techniques such as serial slicing for three-dimensional reconstruction and the preparation of plan-view specimens are also summarized.

show abstract

Section: -D Techniquesmentioning

confidence: 99%

Focused ion beams techniques for nanomaterials characterization

Langford

2006

Microscopy Res & Technique

111

View full text Add to dashboard Cite

show abstract

“…Reference points in the bulk sample are lost as the TEM specimen is lifted out and transferred to the grid for final thinning, which means that they cannot be used as stop points in specimens with low contrast. It should also be noted that these methods were neither applied to low contrast materials nor to very tiny electronic structures (Dai et al, 2001; Stevie et al, 2001; Schwarz & Giannuzzi, 2004; van Leer & Giannuzzi, 2008; Unocic et al, 2008; Felfer et al, 2011). Nanometer scale FIB sample extraction of carbon nanotube interconnects has been reported (Ke et al, 2009).…”

Section: Introductionmentioning

confidence: 99%

A Method for Producing Site-Specific TEM Specimens from Low Contrast Materials with Nanometer Precision

et al. 2013

View full text Add to dashboard Cite

A method that enables high precision extraction of transmission electron microscope (TEM) specimens in low contrast materials has been developed. The main idea behind this work is to produce high contrast markers on both sides of and close to the area of interest. The markers are filled during the depositing of the protective layer. The marker material can be of either Pt or C depending on which one gives the highest contrast. It is thereby possible to distinguish the location of the area of interest during focused ion beam (FIB) milling and ensure that the TEM sample is extracted precisely at the desired position. This method is generally applicable and enables FIB/scanning electron microscope users to make high quality TEM specimens from small features and low contrast materials without a need for special holders. We explain the details of this method and illustrate its potential by examples from three different types of materials.

show abstract

“…Spectral imaging, where complete x-ray spectra are acquired from 2D or 3D arrays of points, is a powerful microanalytical technique, especially when combined with multivariate statistical analysis [1]. Chemical imaging, typically spectroscopic imaging or mapping with energy-loss electrons or x rays has been performed on flat [2][3] or pillar-shaped specimens [4] in the TEM to achieve 3D chemical images. In this paper we describe results from acquisition and analysis, via multivariate statistical analysis (MSA), of x-ray spectral images acquired from a needle-shaped FIB specimen, tilted from -90 to +90 in a newly available TEM specimen holder from Fischione Instruments [5], with full EDS coverage and constant thickness throughout the tomographic series.…”

mentioning

confidence: 99%

Computed Tomographic Spectral Imaging: 3D STEM-EDS Spectral Imaging

Kotula

Brewer

Michael

et al. 2007

MAM

View full text Add to dashboard Cite

Spectral imaging, where complete x-ray spectra are acquired from 2D or 3D arrays of points, is a powerful microanalytical technique, especially when combined with multivariate statistical analysis [1]. Chemical imaging, typically spectroscopic imaging or mapping with energy-loss electrons or x rays has been performed on flat [2][3] or pillar-shaped specimens [4] in the TEM to achieve 3D chemical images. In this paper we describe results from acquisition and analysis, via multivariate statistical analysis (MSA), of x-ray spectral images acquired from a needle-shaped FIB specimen, tilted from -90 to +90 in a newly available TEM specimen holder from Fischione Instruments [5], with full EDS coverage and constant thickness throughout the tomographic series.A needle-shaped specimen of aluminum oxide (~10-20nm particles) dispersion-strengthened Ni (matrix) was prepared by FIB to a thickness of ~100nm near the tip and ~200nm near the base, and extracted in situ and placed upon a special cartridge designed originally for atom-probe tips. The cartridge was then placed in the Fischione Model 2050 On-Axis Tomography holder [5]. Figure 1a shows the tip of the holder while Figure 1b is an SEM image of the needle-shaped specimen. The specimen was imaged in a FEI Tecnai F-30ST operated at 300kV in STEM mode (3nm-diameter FWTM electron probe) with an EDAX SUTW Si (Li) EDS. Drift-corrected spectral images were then acquired at 10° intervals over the range from -90° to +90° from a 400 nm by 2000 nm area and 100 by 500 pixels (4nm/pixel). The dwell time per pixel was 50 msec, resulting in a spectral image acquisition time of about one hour or a total acquisition time of about 19 hours. After acquisition, the series of spectral images, consisting of a total of almost one million spectra, were analyzed with Sandia's Automated eXpert Spectral Image Analysis (AXSIA) software [1] in one minute on a dual Itanium 64-bit computer equipped with 6Gb RAM. Three components resulted from the analysis of the 0-2kV region of the series of spectral images: Ni, Al 2 O 3 , and an absorption component reflecting the use of soft x-rays for this analysis. Figure 2a are the Ni (red) and alumina (green) component images overlaid for +90°, 0°, and 90°. Figure 2b shows the corresponding spectral shapes. Ni and alumina components are clearly deconvolved in the MSA analysis shown, even though the x rays used are soft (<1.5kV). Reconstruction of the tilt-series data into 3D renderings is underway.

show abstract

FIB Specimen Preparation for STEM and EFTEM Tomography

Abstract: Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Cited by 8 publications

References 2 publications

Focused ion beams techniques for nanomaterials characterization

Focused ion beams techniques for nanomaterials characterization

A Method for Producing Site-Specific TEM Specimens from Low Contrast Materials with Nanometer Precision

Computed Tomographic Spectral Imaging: 3D STEM-EDS Spectral Imaging

Contact Info

Product

Resources

About