Fabrication and testing of an electrochemical microcell for in situ soft X-ray microspectroscopy measurements

Gianoncelli, Alessandra; Kaulich, Burkhard; Кискинова, М.; Mele, Claudio; Prasciolu, Mauro; Sgura, Ivonne; Bozzini, Benedetto

doi:10.1088/1742-6596/425/18/182010

Cited by 11 publications

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“…Of course, considering the limited penetration depth of soft X-rays special sample design is required to enable in situ work. In particular, as far as electrochemical cells are concerned, the developments are based on the following three concepts: (i) the pioneering two-electrode system with polymeric electrolyte described in ref ; (ii) the first version developed in our group, consisting of a Si-supported Si 3 N 4 film onto which an electrode system of four square metallic patches was evaporated; the cell was sealed by applying a second Si-supported Si 3 N 4 window and sealing it by gluing the sides of the assembly of the two Si frames; with this type of cell we performed a range of investigations in the field of fuel cells, corrosion, and electrodeposition; ,− (iii) the second fabricated by us displayed the same window concept, but the electrode system geometry was improved by using electron-beam lithography: this cell was operated quasi-in situ in an open configuration and used to complete a series of electrodeposition studies; − (iv) our third-generation cell was a variation of the second version, featuring a novel configuration of the microfabricated electrodes, allowing a Hull-cell type of current density (c.d.) distribution, suitable for insightful compositional and chemical-state studies of multielemental electrodeposition processes .…”

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confidence: 99%

“…distribution, suitable for insightful compositional and chemical-state studies of multielemental electrodeposition processes . In the present paper we describe the design and fabrication of a single-block cell, built around a solid microfabricated channel and implementing an innovative electrode design, featuring a discoidal working electrode, based on detailed computations and implemented by ultraviolet lithography, optimizing the current density distribution control and allowing all the types of electrochemical measurements that are typically carried out in conventional bulk cells. This new approach improves notably the sealed-cell concept adopted in refs − and in terms of seal reliability, electrolyte thickness control, and rapidity of electrolyte insertion, as well as transfer to sample stage.…”

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confidence: 99%

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Fabrication of a Sealed Electrochemical Microcell for in Situ Soft X-ray Microspectroscopy and Testing with in Situ Co-Polypyrrole Composite Electrodeposition for Pt-Free Oxygen Electrocatalysis

et al. 2013

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In this paper we report on the fabrication and testing of a novel concept of sealed electrochemical microcell for in situ soft X-ray microspectroscopy in transmission, dedicated for nonvacuum compatible electrolytes. The microcell, fabricated using ultraviolet lithography, at variance with previous versions of electrochemical wet cells, that featured an optical window glued on top of the electrode system and a very limited electrolyte volume, the device presented here is a single solid block based around a microfabricated channel with fixed optical windows and apt for microfluidic work. Moreover, this cell allows to employ an advanced electrodic geometry developed in our group - so far used only in open electrochemical cells for work with vacuum-compatible electrolytes - also with low-vapor pressure liquids, possibly saturated with the required gases. The cell optimal electrode design allows three-electrode electrochemical control typical of traditional electrochemical experiments. The first electrochemical experiments with this new cell explore the electrochemical growth of a Co-polypyrrole, a composite electrocatalyst material with promising performance to replace the expensive Pt catalyst in fuel-cell oxygen electrodes. Morphological and chemical-state distributions of Co codeposited with polypyrrole has been followed as a function of time and position, yielding unprecedented information on the processes relevant to the synthesis of this catalyst.

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confidence: 99%

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Fabrication of a Sealed Electrochemical Microcell for in Situ Soft X-ray Microspectroscopy and Testing with in Situ Co-Polypyrrole Composite Electrodeposition for Pt-Free Oxygen Electrocatalysis

et al. 2013

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“…The data from ptychographic scans recorded at 16 energies across the Co L 3 -edge were employed to generate these images. The selected region encompasses the electrode/electrolyte interface (electrolyte at the top of the images) and corresponds to the zone where the largest growth rate gradient develops (Gianoncelli et al 2013). Within this extended region, two sub-regions (of dimension ca.…”

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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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“…For this particular investigation, we fabricated a Hull-type flat cell (e.g. [49] The Hull-cell performance can be obtained in two ways: 1) by increasing the dimensions of the outer electrode, used as working electrode and 2) by spontaneous screening of the central, diskshaped counter electrode, which results from the hydrogen bubble that is formed in the highest cathodic current density zone in the water electrolysis reaction after the initial electrodeposition. [48]) based on the design proposed and described in detail elsewhere.…”

Section: Methodsmentioning

confidence: 99%

“…[29] This is part of a general class of transmission electrochemical cells that can be used for a range of in situ and quasi-in situ experiments. [49] The Hull-cell performance can be obtained in two ways: 1) by increasing the dimensions of the outer electrode, used as working electrode and 2) by spontaneous screening of the central, diskshaped counter electrode, which results from the hydrogen bubble that is formed in the highest cathodic current density zone in the water electrolysis reaction after the initial electrodeposition. In this way, a wide and space-resolved range of current densities can be obtained at the working electrode.…”

Section: Methodsmentioning

confidence: 99%

Electrodeposition of a Mn–Cu–ZnO Hybrid Material for Supercapacitors: A Soft X‐ray Fluorescence and Absorption Microspectroscopy Study

Bozzini¹,

Gianoncelli²,

Mele³

et al. 2013

ChemElectroChem

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Synchrotron‐based soft‐X‐ray imaging and microspectroscopy with sub‐micrometer spatial resolution are used to investigate the electrodeposition of Mn–Cu–ZnO, a prospective active material for supercapacitors. This study is focused on the correlation of the local current density and the spatial distribution of the composition and chemical‐state in electrodeposits grown potentiostatically at −0.7 V (vs a saturated calomel electrode), as well as the optimal potential for the achievement of high specific capacitance and cycling stability. The morphology, elemental distribution, and the local chemical state of both the electrode deposits and the grown dendrite structures are followed by using X‐ray imaging, X‐ray fluorescence mapping, and X‐ray absorption microspectroscopy. For transmission soft‐X‐ray measurements, a thin‐layer Hull‐type microcell is developed and fabricated by using electron‐beam lithography. The information obtained for the spatial distribution of the deposit is complemented by using electrochemical measurements and numerical simulations.

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Fabrication and testing of an electrochemical microcell for in situ soft X-ray microspectroscopy measurements

Cited by 11 publications

References 11 publications

Fabrication of a Sealed Electrochemical Microcell for in Situ Soft X-ray Microspectroscopy and Testing with in Situ Co-Polypyrrole Composite Electrodeposition for Pt-Free Oxygen Electrocatalysis

Fabrication of a Sealed Electrochemical Microcell for in Situ Soft X-ray Microspectroscopy and Testing with in Situ Co-Polypyrrole Composite Electrodeposition for Pt-Free Oxygen Electrocatalysis

Monitoring dynamic electrochemical processes with in situ ptychography

Electrodeposition of a Mn–Cu–ZnO Hybrid Material for Supercapacitors: A Soft X‐ray Fluorescence and Absorption Microspectroscopy Study

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