An ultra-high vacuum electrochemical flow cell for <i>in situ</i>/<i>operando</i> soft X-ray spectroscopy study

Bora, Debajeet K.; Glans, Per‐Anders; Pepper, John; Liu, Yi‐Sheng; Du, Chun; Wang, Dunwei; Guo, Jinghua

doi:10.1063/1.4870795

Cited by 43 publications

(30 citation statements)

References 28 publications

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“…The cell was also adapted for the investigation of the interaction between water and graphene depending on the incidence X‐ray angle under static conditions . Such flow‐cell designs are being further optimized at ALS . Besides to Si 3 N 4 , polyimide films with deposited electrodes also served as membranes for such kind of cells …”

Section: Progress In Analytical Techniques Observed In Electrochemicmentioning

confidence: 99%

Probing Operating Electrochemical Interfaces by Photons and Neutrons

et al. 2015

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The operation of all electrochemical energy-related systems, such as supercapacitors, batteries, fuel cells, etc. depends largely on the processes occurring at electrochemical interfaces at which charge separation and chemical reactions occur. Evolution of structure and composition at the interface between electrodes and electrolytes affects all the device′s functional parameters including power and long-term performance stability. The analytical techniques capable of exploring the interfaces are still very limited, and more often only ex situ studies are performed. This sometimes leads to a loss of important pieces of the puzzle, hindering the development of novel technologies, as in many cases intermediates and electrochemical reaction products cannot be “quenched” for post-process analyses. Techniques capable of operando probing of electrochemical interfaces by photons and neutrons have become an extensively growing field of research. This review aims at highlighting approaches and developing ideas on the adaptation of photoelectron, X-ray absorption, vibrational spectroscopy, nuclear magnetic resonance, and X-ray and neutron reflectometry in electrochemical studies

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Section: Progress In Analytical Techniques Observed In Electrochemicmentioning

confidence: 99%

Probing Operating Electrochemical Interfaces by Photons and Neutrons

et al. 2015

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“…It is therefore of great interest to combine XAS and the liquid cell technique for in situ/operando investigations on liquid-based materials. [9][10][11][12] When a sample's thickness exceeds the penetration depth of soft X-rays, which is the case for the liquid cell adopted in this study, detection of XA spectra in the transmission mode is not applicable. Therefore, fluorescence yield (FY) or electron yield (EY) must be employed to acquire XA spectra.…”

mentioning

confidence: 99%

Introducing Ionic-Current Detection for X-ray Absorption Spectroscopy in Liquid Cells

Schön

Xiao

Golnak

et al. 2017

J. Phys. Chem. Lett.

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Photons and electrons are two common relaxation products upon X-ray absorption, enabling fluorescence yield and electron yield detections for X-ray absorption spectroscopy (XAS).The ions that are created during the electron yield process are relaxation products too, which are exploited in this study to produce ion yield for XA detection. The ionic currents measured in a liquid cell filled with water or iron(III) nitrate aqueous solutions exhibit characteristic O K-edge and Fe L-edge absorption profiles as a function of excitation energy. Application of two electrodes installed in the cell is crucial for obtaining the XA spectra of the liquids behind membranes. Using a single electrode can only probe the species adsorbed on the membrane surface. The ionic-current detection, termed as total ion yield (TIY) in this study, also produces an undistorted Fe L-edge XA spectrum, indicating its promising role as a novel detection method for XAS studies in liquid cells.Key words: total ion yield (TIY), ionic current, liquid flow-cell, total electron yield (TEY), X-ray absorption spectroscopy (XAS) TOC GraphicPage 2 of 17 ACS Paragon Plus EnvironmentThe Journal of Physical Chemistry Letters 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 3 Studying the electronic structure of liquid water and aqueous solutions by soft X-rays has attracted much attention in recent years, 1-6 and continues to be a vital research field. Resonant excitation by X-rays is highly element-specific, which makes X-ray absorption spectroscopy (XAS) a widely used tool in many scientific disciplines. Due to the vacuum requirement for soft X-ray propagation, detection of XA spectra for liquid (volatile) samples in vacuum is very challenging. One of the most applied techniques to introduce liquid samples into a vacuum chamber is a liquid flow-cell with an ultra-thin membrane separating the liquid from the vacuum. 7,8 When equipped with multiple electrodes, such a liquid cell can act as a standard electrochemical cell. It is therefore of great interest to combine XAS and the liquid cell technique for in situ/operando investigations on liquid-based materials. [9][10][11][12] When a sample's thickness exceeds the penetration depth of soft X-rays, which is the case for the liquid cell adopted in this study, detection of XA spectra in the transmission mode is not applicable. Therefore, fluorescence yield (FY) or electron yield (EY) must be employed to acquire XA spectra. Due to the significant thickness of typical membranes, e.g. Si 3 N 4 and SiC membranes (~ 100 nm), the electrons created within liquid solutions cannot penetrate the membrane and escape into vacuum. The FY was thus considered the only feasible way to probe the liquid-phase species behind membranes. However, EY has been recently realized in liquid cell studies, thanks to the newly developed graphene membra...

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“…X-ray region are easily measured in transmission or fluorescence mode due to the high transmission character of hard X-rays. On the other hand, in the soft X-ray region, several groups have developed electrochemical cells for XAS of light elements such as C, N, and O (1s), and Mn and Fe (2p) in fluorescence yields [222,223]. The in situ spatial measurement by scanning transmission X-ray microscope (STXM) is applied to the electrochemical reaction [224][225][226].…”

Section: Electrochemical Reactionsmentioning

confidence: 99%