Investigation of Energy‐Relevant Materials with Synchrotron X‐Rays and Neutrons

Manke, Ingo; Markötter, Henning; Tötzke, Christian; Kardjilov, Nikolay; Grothausmann, Roman; Dawson, Martin; Hartnig, Christoph; Haas, Sylvio; Thomas, D.; Hoell, Armin; Genzel, Christoph; Banhart, John

doi:10.1002/adem.201000284

Cited by 69 publications

(28 citation statements)

References 151 publications

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“…In particular, imaging and structural methods based on X-rays, such as absorption near-edge spectroscopy, fluorescence, diffraction and scattering, are regarded as the cutting-edge tools for the study of buried electrochemical interfaces (Ebner et al 2013;Lin et al 2017;Sun et al 2017). Pioneering investigations in the field, thriving on the complementarity of the approaches, have disclosed a wealth of morphological and chemical modifications of active materials resulting from growth and dissolution processes and have provided unprecedented insight at the submicron scale into complex dynamic interfacial phenomena (e.g., Nagy 2011; Manke et al 2011;Bozzini et al 2012aBozzini et al , 2015a. Moreover, advances in lithographic fabrication of cells has allowed the technical limitations of in situ experiments to be overcome, enabling observations of electrode/electrolyte interfaces at normal incidence to the photon beam .…”

Section: Introductionmentioning

confidence: 99%

Monitoring dynamic electrochemical processes with in situ ptychography

et al. 2018

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The present work reports novel soft X-ray Fresnel CDI ptychography results, demonstrating the potential of this method for dynamic in situ studies. Specifically, in situ ptychography experiments explored the electrochemical fabrication of Codoped Mn-oxide/polypyrrole nanocomposites for sustainable and cost-effective fuel-cell air-electrodes. Oxygen-reduction catalysts based on Mn-oxides exhibit relatively high activity, but poor durability: doping with Co has been shown to improve both reduction rate and stability. In this study, we examine the chemical state distribution of the catalytically crucial Co dopant to elucidate details of the Co dopant incorporation into the Mn/polymer matrix. The measurements were performed using a custom-made three-electrode thin-layer microcell, developed at the TwinMic beamline of Elettra Synchrotron during a series of experiments that were continued at the SXRI beamline of the Australian Synchrotron. Our time-resolved ptychography-based investigation was carried out in situ after two representative growth steps, controlled by electrochemical bias. In addition to the observation of morphological changes, we retrieved the spectroscopic information, provided by multiple ptychographic energy scans across Co L 3 -edge, shedding light on the doping mechanism and demonstrating a general approach for the molecular-level investigation complex multimaterial electrodeposition processes.

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Section: Introductionmentioning

confidence: 99%

Monitoring dynamic electrochemical processes with in situ ptychography

et al. 2018

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“…Several imaging techniques were employed in PEMFC research to extend the understanding of physical phenomena related to fuel‐cell performance . Imaging techniques have various objectives in the field of energy‐related materials such as characterization of the dynamic behavior under varied operating conditions as well as revealing structural properties of these materials .…”

Section: Introductionmentioning

confidence: 99%

“…[8][9][10][11][12][13][14][15][16][17] Several imaging techniques were employed in PEMFCr esearcht oe xtend the understandingo fp hysical phenomena related to fuel-cell performance. [18,19] Imaging techniques have variouso bjectives in the field of energy-related materials such as characterization of the dynamic behavior under varied operating conditions as wella sr evealing structural properties of these materials. [20,21] Amongt he techniques used for water-managements tudies of PEMFCs are X-ray and synchrotron X-ray imaging, [22][23][24][25][26][27][28][29][30][31] magnet resonancet omography, [32][33][34] and neutron imaging.…”

Section: Introductionmentioning

confidence: 99%

Improved Performance of Polymer Electrolyte Membrane Fuel Cells with Modified Microporous Layer Structures

et al. 2017

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A possible method to improve membrane humidity conditions in polymer electrolyte membrane fuel cells and, therefore, the cell performance is the optimization of microporous layer (MPL) structures. In this work, water transport in modified MPL materials in polymer electrolyte membrane fuel cells (PEMFCs) was investigated by in operando synchrotron X‐ray tomography. Three different types of MPLs are compared: A reference standard MPL material, an MPL material with a special wavy structure, and an MPL with randomly distributed holes. We found a strong impact of the modified MPL structure on the water distribution at operating temperatures of 40 and 55 °C and an increase of cell performance up to 14 % compared to the reference cell. We assume the water distribution at the membrane to be responsible for the performance increase and provide a detailed discussion.

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“…On the other hand, synchrotron X‐ray beams are more compatible with liquid‐phase reactions because of the increased penetration power of X‐rays in liquids and air. Synchrotron X‐ray techniques have been widely used for studying solids in liquid and gas environments, but exploring their capabilities for real‐time monitoring colloidal nanoparticle synthesis represents a very new area emerged recently. In this review, the advances in developing in situ synchrotron X‐ray techniques will be highlighted to show their promising potentials in real‐time probing the complex nanophase evolution involved in the synthesis of colloidal nanoparticles.…”

Section: Introductionmentioning

confidence: 99%

In Situ Synchrotron X‐Ray Techniques for Real‐Time Probing of Colloidal Nanoparticle Synthesis

Sun

Ren

2013

Part & Part Syst Charact

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Solution‐phase synthesis of colloidal nanoparticles with precisely tailored properties is one of the fastest growing research topic and represents the most critical foundation to implant nanotechnology in a variety of areas to boost performance of traditional systems. Comprehensive understanding of the nucleation and growth mechanisms involved in the formation of colloidal nanoparticles is very important to realize rational design and synthesis of well‐tailored nanoparticles and requires appropriate in situ techniques to probe the kinetics of the synthetic reactions. Synchrotron hard X‐rays represent a class of promising probes for solution‐phase reactions due to their strong penetration in ambient environment and solutions. This review completely summarizes the in situ synchrotron X‐ray techniques emerged in the recent years for real‐time probing nanophase evolution of colloidal nanoparticles. Typical examples of colloidal nanoparticle syntheses are discussed in detail to shed the light on the advantages and disadvantages of individual techniques.

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Investigation of Energy‐Relevant Materials with Synchrotron X‐Rays and Neutrons

Cited by 69 publications

References 151 publications

Monitoring dynamic electrochemical processes with in situ ptychography

Monitoring dynamic electrochemical processes with in situ ptychography

Improved Performance of Polymer Electrolyte Membrane Fuel Cells with Modified Microporous Layer Structures

In Situ Synchrotron X‐Ray Techniques for Real‐Time Probing of Colloidal Nanoparticle Synthesis

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