Correlative Nano‐Computed Tomography and Focused Ion‐Beam Sectioning: A Case Study on a Co‐Base Superalloy Oxide Scale

Lenz, Malte; Wirth, Janis; Englisch, Silvan; Rosiwal, Jan; Buchinger, Nadine; Weiser, M.; Virtanen, Sannakaisa; Zubiri, Benjamin Apeleo; Spiecker, Erdmann

doi:10.1002/adem.201900823

Cited by 4 publications

(2 citation statements)

References 58 publications

(128 reference statements)

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“…Several approaches for scale-bridging 3D analysis have been demonstrated. For instance, a semidestructive workflow combining nano-CT with FIB-SEM tomography enabled a superior segmentation of 3D datasets and thorough analysis of samples of several microns in size [39,40]. As a nondestructive approach, the combination of 360 • -ET and nano-CT proved to reliably reveal the structure of complex material systems [41,42], e.g., macroporous zeolite particle agglomerates, with nm resolution, while, at the same time, covering decently sized volumes up to (40 µm) 3 , enabling the acquisition of statistically relevant information [43].…”

Section: Introductionmentioning

confidence: 99%

Unraveling Structural Details in Ga-Pd SCALMS Systems Using Correlative Nano-CT, 360° Electron Tomography and Analytical TEM

et al. 2021

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We present a comprehensive structural and analytical characterization of the highly promising supported catalytically active liquid metal solutions (SCALMS) system. This novel catalyst shows excellent performance for alkane dehydrogenation, especially in terms of resistance to coking. SCALMS consists of a porous support containing catalytically active low-melting alloy particles (e.g., Ga-Pd) featuring a complex structure, which are liquid at reaction temperature. High-resolution 3D characterization at various length scales is required to reveal the complex pore morphology and catalytically active sites’ location. Nano X-ray computed tomography (nano-CT) in combination with electron tomography (ET) enables nondestructive and scale-bridging 3D materials research. We developed and applied a correlative approach using nano-CT, 360°-ET and analytical transmission electron microscopy (TEM) to decipher the morphology, distribution and chemical composition of the Ga-Pd droplets of the SCALMS system over several length scales. Utilizing ET-based segmentations of nano-CT reconstructions, we are able to reliably reveal the homogenous porous support network with embedded Ga-Pd droplets featuring a nonhomogenous elemental distribution of Ga and Pd. In contrast, large Ga-Pd droplets with a high Ga/Pd ratio are located on the surface of SCALMS primary particles, whereas the droplet size and the Ga/Pd ratio decreases while advancing into the porous volume. Our studies reveal new findings about the complex structure of SCALMS which are required to understand its superior catalytic performance. Furthermore, advancements in lab-based nano-CT imaging are presented by extending the field of view (FOV) of a single experiment via a multiple region-of-interest (ROI) stitching approach.

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Section: Introductionmentioning

confidence: 99%

Unraveling Structural Details in Ga-Pd SCALMS Systems Using Correlative Nano-CT, 360° Electron Tomography and Analytical TEM

et al. 2021

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“…Each expected mineral type can be unswervingly assigned to the particles by applying this approach. All particles from a respective mineral type are segmented in Arivis Vision4D by applying a machine-learning algorithm [3] and classified regarding their specific morphology, frequency and distribution, starting with the BSE/EDXS-informed Nano-CT virtual slices, according to Lenz, Wirth et al [4]. The segmentation routine transfers the chemical information to the entire Nano-CT volume, providing each mineral's morphology and distribution.…”

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Comprehensive, multidimensional and correlative particle characterization of a saxolite and talcum compound to support the understanding of complex separation processes

et al. 2021

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Correlative Laboratory Nano‐CT and 360° Electron Tomography of Macropore Structures in Hierarchical Zeolites

Zubiri

Wirth

Drobek

et al. 2020

Adv Materials Inter

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Hierarchical pore structures exhibit morphological features on several length scales, which govern important materials properties in catalysis, such as catalytic activity, diffusivity or selectivity. Correlative tomography offers unique opportunities for a comprehensive and scale‐bridging 3D characterization of such complex pore morphologies, which is crucial to further optimize materials design and synthesis routines. This study explores the capabilities of correlative 360° electron tomography (ET) and lab‐based nano X‐ray computed tomography (Nano‐CT) enabling 3D analyses of volumes of up to (60 µm)³ with down to nm resolution, as demonstrated for zeolite particles with embedded macropores. By first applying the two techniques to the same particle the higher resolution and fidelity of ET are used to improve the segmentation of pore space in the Nano‐CT reconstruction. Extended statistical relevance and access to interparticle pore space are obtained from reconstructions of larger particle agglomerates, using the large‐field‐of‐view mode of the Nano‐CT. The presented correlative approach enables real space analyses of important pore characteristics for comparison with complementary pore characterization techniques. Moreover, by investigating samples from different stages of the synthesis, 360°‐ET and Nano‐CT provide unique insights into the formation mechanism of porous materials, as demonstrated for the steam‐assisted crystallization of the macroporous zeolite particles.

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Correlative Nano‐Computed Tomography and Focused Ion‐Beam Sectioning: A Case Study on a Co‐Base Superalloy Oxide Scale

Cited by 4 publications

References 58 publications

Unraveling Structural Details in Ga-Pd SCALMS Systems Using Correlative Nano-CT, 360° Electron Tomography and Analytical TEM

Unraveling Structural Details in Ga-Pd SCALMS Systems Using Correlative Nano-CT, 360° Electron Tomography and Analytical TEM

Comprehensive, multidimensional and correlative particle characterization of a saxolite and talcum compound to support the understanding of complex separation processes

Correlative Laboratory Nano‐CT and 360° Electron Tomography of Macropore Structures in Hierarchical Zeolites

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