Automated three-dimensional X-ray analysis using a dual-beam FIB

Schaffer, Miroslava; Wagner, Julian; Schaffer, Bernhard; Schmied, Mario; Mulders, Hans

doi:10.1016/j.ultramic.2006.11.007

Cited by 84 publications

(71 citation statements)

References 17 publications

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“…From the series of data created in this way, a 3D volume model can be reconstructed. The fully automated 3D-EDXS method [36] is performed using the Nanolab Nova200 DB-FIB (FEI) and the Genesis EDXS detector (EDAX). The DB-FIB is operated with an ion beam current of 1 nA at 30 kV acceleration voltage during milling, and with an electron beam current of 2.2 nA at 15 kV acceleration voltage during SEM and EDXS analysis.…”

Section: Methodsmentioning

confidence: 99%

“…The right part of this image shows a very homogeneous distribution of precipitates with almost identical diameter, which is the result of a two-dimensional projection of a three-dimensional array of tubular precipitates in the normal to the growth direction of the precipitates. Figure 2 shows a corresponding microstructure reproduction performed with sequential sectioning using the FIB (focused ion beam) technique [36].…”

Section: Precipitate Morphologymentioning

confidence: 99%

See 1 more Smart Citation

Evolution of Size and Morphology of γ' Precipitates in UDIMET 720 Li during Continuous Cooling

Radis¹,

Schaffer²,

Albu³

et al. 2008

Superalloys 2008 (Eleventh International Symposium)

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In this work, an analysis of the evolution of precipitates in the nickel-base superalloy UDIMET 720 Li during continuous cooling is carried out. Starting from the solution-annealed condition, the precipitation kinetics, the distribution and the morphology of particles during continuous cooling is studied experimentally by SEM, EFTEM and FIB. The results are compared to simulations using the software MatCalc. Depending on the cooling rate, discontinuous precipitation as well as monomodal and multi-modal distributions are observed. The precipitate microstructure of various samples is investigated and evaluated quantitatively to determine the precipitate distribution parameters. The experimental results are discussed and compared with the results of the simulation. Finally, two parameter studies are carried out which indicate the sensitivity of the simulation results on the input data, i.e. the thermodynamic and diffusion databases.

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Section: Methodsmentioning

confidence: 99%

Section: Precipitate Morphologymentioning

confidence: 99%

Evolution of Size and Morphology of γ' Precipitates in UDIMET 720 Li during Continuous Cooling

Radis¹,

Schaffer²,

Albu³

et al. 2008

Superalloys 2008 (Eleventh International Symposium)

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show abstract

“…A freshly milled section was obtained perpendicular to the surface. The electron beam images the section with an angle of 36°and the resulting take-off angle for the EDS detector is 27° [6]. During the 3-D acquisition, layers were etched away sequentially through the whole volume.…”

Section: -D Eds By Fib/semmentioning

confidence: 99%

“…Using a focused ion beam (FIB) combined with SEM/EDS, 2-D mapping can be extended to three dimensions: using an FIB to sequentially mill away thin layers of material through the volume of interest, each section is characterized with SEM images and EDS maps. This technique is called 3-D EDS by FIB/ SEM [5,6].…”

Section: Introductionmentioning

confidence: 99%

“…Two segmentation methods adapted to 3-D EDS were reported: (i) a straightforward method most commonly used to isolate one phase is to set up a threshold value for one of the elements [6,8,9] and (ii) a segmentation method developed by Kotula et al [10] based on multivariate statistical analysis-this method provides a set of statistically dominant phases with their corresponding spectrum. Both of these methods rely only on EDS measurements, without using the high spatial information given by SE images.…”

Section: Introductionmentioning

confidence: 99%

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Three-dimensional chemical analysis of laser-welded NiTi–stainless steel wires using a dual-beam FIB

et al. 2013

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The biomedical industry has an increasing demand for processes to join dissimilar metals, such as laser welding of NiTi and stainless steel wires. A region of the weld close to the NiTi interface, which previously was shown to be prone to cracking, was further analyzed by energy dispersive spectrometry (EDS) extended in the third dimension using a focused ion beam. As the spatial resolution of EDS analysis is not precise enough to resolve the finest parts of the microstructure, a new segmentation method that uses in addition secondaryelectron images of higher spatial resolution was developed. Applying these tools, it is shown that this region of the weld close to the NiTi interface does not comprise a homogeneous intermetallic layer, but is rather constituted by a succession of different intermetallics, the composition of which can be directly correlated with the solidification path in the ternary Fe-Ni-Ti Gibbs simplex.

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Three‐dimensional characterization of Ni‐Sm0.2Ce0.8O2 ‐δ cermet for SOFC anodes by high‐resolution FIB ‐ SEM Tomography

Kapun

Šturm

Marinšek

et al. 2016

European Microscopy Congress 2016: Proceedings

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A solid oxide fuel cells (SOFC) technology is one of the most promising energy conversion device due to its high conversion efficiency, low environmental pollution and high flexibility to various fuel types (1). To overcome all challenges concerning materials' long term stability at operating temperatures, current research efforts are aimed at intermediate temperature SOFCs (IT‐SOFCs) (2). From this point of view samaria‐doped ceria (SDC) is a promising ceramic material, with superb ionic conductivity, which can be used as an anode material when combined with Ni in Ni‐SDC cermet (2). To ensure electronic and ionic conductivity as well as gas permeability, anode cermet should exhibit carefully tailored microstructure where metallic Ni, ceramic SDC and pores form continuous phases. In an operating cell fuel gas is electrochemically oxidized at the Ni/SDC/fuel interface, called the triple phase boundary (TPB) region. Therefore, both the activity of Ni‐SDC and their stability are strongly influenced by the cermet's morphology and microstructures such as volume fractions, grain connectivity, grain size, pore size, pore distribution and TPB length (3). For this purpose, exact and accurate microstructural determination is crucial in predicting material's performances in an operating cell. In such a cermet composite critical topological features such as connectivity and the tortuosity of transport pathways in the pores can only be established based on 3D microstructural information (4). In this work we present quantitative characterization of Ni‐Sm 0.2 Ce 0.8 O 2‐δ cermets, sintered at 1400°C, using high‐resolution FIB‐SEM tomography. Initially, a layer of platinum was deposited ontop the region of interest to protect the surface and prevent rounding of top edges of cross section during milling. The volume of interest was separated using an optimised U‐pattern pre‐milling procedure to prevent material redeposition and shadowing of the signals used for imaging and microanalysis. The sample was then serial sectioned using an automated slicing procedure with drift correction algorithms to obtain a series of 2D images with narrow and reproducible spacing between the individual image planes (5). Experimental milling and imaging parameters have been optimised in order to obtain a high quality 3D reconstruction with phase contrast information. Individual phases were identified from EDXS elemental maps and further segmented according to their grey level. 3D reconstructed volume is a base for determination of: volume fractions of individual phases, grain connectivity, porosity, tortuosity and TPB length. The presented analytical method will serve as a tool for quantitative characterization of primary microstructural parameters and complex topological features, during microstructure evolution of Ni‐Sm 0.2 Ce 0.8 O 2‐δ anode cermets using various sintering procedure.

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Automated three-dimensional X-ray analysis using a dual-beam FIB

Cited by 84 publications

References 17 publications

Evolution of Size and Morphology of γ' Precipitates in UDIMET 720 Li during Continuous Cooling

Evolution of Size and Morphology of γ' Precipitates in UDIMET 720 Li during Continuous Cooling

Three-dimensional chemical analysis of laser-welded NiTi–stainless steel wires using a dual-beam FIB

Three‐dimensional characterization of Ni‐Sm0.2Ce0.8O2 ‐δ cermet for SOFC anodes by high‐resolution FIB ‐ SEM Tomography

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Automated three-dimensional X-ray analysis using a dual-beam FIB

Cited by 84 publications

References 17 publications

Evolution of Size and Morphology of &#947;' Precipitates in UDIMET 720 Li during Continuous Cooling

Evolution of Size and Morphology of &#947;' Precipitates in UDIMET 720 Li during Continuous Cooling

Three-dimensional chemical analysis of laser-welded NiTi–stainless steel wires using a dual-beam FIB

Three‐dimensional characterization of Ni‐Sm0.2Ce0.8O2 ‐δ cermet for SOFC anodes by high‐resolution FIB ‐ SEM Tomography

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Evolution of Size and Morphology of γ' Precipitates in UDIMET 720 Li during Continuous Cooling

Evolution of Size and Morphology of γ' Precipitates in UDIMET 720 Li during Continuous Cooling