Three-dimensional mapping of nickel oxidation states using full field x-ray absorption near edge structure nanotomography

Nelson, George J.; Harris, William M.; Izzo, John R.; Grew, Kyle N.; Chiu, Wilson K. S.; Chu, Yong S.; Yi, Jaemock; Andrews, Joy C.; Liu, Yijin; Pianetta, P.

doi:10.1063/1.3574774

Cited by 65 publications

(54 citation statements)

References 22 publications

(25 reference statements)

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“…SRXTM methods may be complemented with nanoscale approaches such as focused-ion-beam scanning electron microscopy (Keller et al, 2011;Bera et al, 2011), transmission electron microscopy (Kanitpanyacharoen et al, 2011) and X-ray nanotomography (Nelson et al, 2011;Grew et al, 2010). Overall, this round-robin experiment of SRXTM documented that all three beamlines produce similar results with microstructural resolution of approximately 2 mm.…”

Section: Discussionmentioning

confidence: 69%

A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS

Kanitpanyacharoen

Parkinson

Carlo

et al. 2012

J Synchrotron Radiat

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Synchrotron radiation X-ray tomographic microscopy (SRXTM) was used to characterize the three-dimensional microstructure, geometry and distribution of different phases in two shale samples obtained from the North Sea (sample N1) and the Upper Barnett Formation in Texas (sample B1). Shale is a challenging material because of its multiphase composition, small grain size, low but significant amount of porosity, as well as strong shape-and lattice-preferred orientation. The goals of this round-robin project were to (i) characterize microstructures and porosity on the micrometer scale, (ii) compare results measured at three synchrotron facilities, and (iii) identify optimal experimental conditions of high-resolution SRXTM for fine-grained materials. SRXTM data of these shales were acquired under similar conditions at the Advanced Light Source (ALS) of Lawrence Berkeley National Laboratory, USA, the Advanced Photon Source (APS) of Argonne National Laboratory, USA, and the Swiss Light Source (SLS) of the Paul Scherrer Institut, Switzerland. The data reconstruction of all datasets was handled under the same procedures in order to compare the data quality and determine phase proportions and microstructures. With a 10Â objective lens the spatial resolution is approximately 2 mm. The sharpness of phase boundaries in the reconstructed data collected from the APS and SLS was comparable and slightly more refined than in the data obtained from the ALS. Important internal features, such as pyrite (high-absorbing), and low-density features, including pores, fractures and organic matter or kerogen (low-absorbing), were adequately segmented on the same basis. The average volume fractions of low-density features for sample N1 and B1 were estimated at 6.3 (6)% and 4.5 (4)%, while those of pyrite were calculated to be 5.6 (6)% and 2.0 (3)%, respectively. The discrepancy of data quality and volume fractions were mainly due to different types of optical instruments and varying technical set-ups at the ALS, APS and SLS.

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Section: Discussionmentioning

confidence: 69%

A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS

Kanitpanyacharoen

Parkinson

Carlo

et al. 2012

J Synchrotron Radiat

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“…Element-sensitive XNT measurements were performed at X-ray beam energies above and below elemental absorption edges, in order to invoke substantial elemental contrast in the absorption images. 25,28 For the materials in this study, tomographic imaging spanning the Fe K edge (7112 eV) and Gd L 3 edge (7243 eV) was performed by imaging at 7090, 7200, and 7280 eV, as shown in Fig. 3.…”

mentioning

confidence: 99%

“…[23][24][25] This technique addresses unexplored issues at the mesoscale; how do the phases, interfaces, resulting microstructure and potential changes during operation effect performance? Here we demonstrate the use of this technique to identify and map distinct phases in MIEC ceramic composite membranes.…”

mentioning

confidence: 99%

Characterization of 3D interconnected microstructural network in mixed ionic and electronic conducting ceramic composites

et al. 2014

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The microstructure and connectivity of the ionic and electronic conductive phases in composite ceramic membranes are directly related to device performance. Transmission electron microscopy (TEM) including chemical mapping combined with X-ray nanotomography (XNT) have been used to characterize the composition and 3-D microstructure of a MIEC composite model system consisting of a Ce 0.8 Gd 0.2 O 2 (GDC) oxygen ion conductive phase and a CoFe 2 O 4 (CFO) electronic conductive phase. The microstructural data is discussed, including the composition and distribution of an emergent phase which takes the form of isolated and distinct regions. Performance implications are considered with regards to the design of new material systems which evolve under non-equilibrium operating conditions.

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“…This rule of electrode design is obvious from Eqs. (16), (17), (20), and (21). Contour plot diagrams like Figure 7 are thus useful in designing and optimizing coordination numbers and percolation thresholds of binary particle aggregates.…”

Section: Coordination Numbers and Percolation Thresholdsmentioning

confidence: 97%

Design and Optimization of Composite Electrodes in Solid Oxide Cells

Fang

Chan

2012

Fuel Cells

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The performance of solid oxide cells (SOCs) heavily relies on the population of three‐phase boundaries (TPBs) in the composite electrodes. In this study, SOC composite electrodes are described by percolating binary particle aggregates that are constructed from random loose packing models and classical sintering theories. Summed perimeters of the sintering necks represent the total TPB lengths. A case study has been carried out on lanthanum strontium manganite (LSM)–yttria‐stabilized zirconia (YSZ) composite electrodes. By employing three‐dimensional data that are converted from relevant two‐dimensional data, the TPB length of baseline LSM–YSZ electrodes investigated in this study is 35.4 μm μm–3. The parametric and sensitivity analyses show the changes of TPB lengths in functions of the weight fraction of powders, particle size and particle size ratio of powders, void fraction of electrodes, and density of materials. In the case of baseline LSM–YSZ electrodes, proper electrode design and optimization would result in 2–3 times of the enlargement of TPBs. Technical guidelines on the design and optimization of SOC composite electrodes are proposed.

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Three-dimensional mapping of nickel oxidation states using full field x-ray absorption near edge structure nanotomography

Cited by 65 publications

References 22 publications

A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS

A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS

Characterization of 3D interconnected microstructural network in mixed ionic and electronic conducting ceramic composites

Design and Optimization of Composite Electrodes in Solid Oxide Cells

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