In-Situ X-Ray Bulk Liquid Electrochemistry

Introducing the world's first bulk liquid-electrochemistry X-ray holder

Technical Specs

Hummingbird Scientific X-Ray Synchrotron Holder - ElectroChemistry Liquid Flow Cell
1470 Series X-Ray
Total Electrodes 6
True Reference Electrode  Yes*
True Counter Electrode Yes*
Electrolytes  Aqueous, Wide range of organics
Spacer Range  100 nm to 2 um*
Heating Compatibility Yes
X-ray Microscope Compatibility Custom integration

* Different Configurations and Materials Available


Featured Research

Operando STXM demonstration of critical surface catalytic activity for hydrogen generation

William Chueh et al. from Stanford University, in collaboration with Hummingbird Scientific, Advanced Light Source (Lawrence Berkeley National Laboratory) and the University of Warwick used the operando STXM cell to demonstrate for the first time the surface site activity of transition metal (oxy) hydroxides with an electrochemical stimulus for developing a promising electrocatalyst for the oxygen evolution reaction (OER). This reaction is key in water splitting to generate hydrogen that can be used to store energy.

The data from the STXM electrochemical shows heterogeneity in the distribution of Co3+ species in the β-Co(OH)2 particles with an increase in the voltage. However, the electrochemical current is primarily restricted to the particle edge facets. The local concentration of higher Co oxidation state (Co3+) compared to the bulk of the particles suggests that layered oxides’ OER activity can be improved by improvising the surface morphology.

Figure: Cyclic voltammogram in 0.1M KOH of β-Co(OH)2 in the STXM electrochemical flow cell at a scan rate of 10 mV s-1 and a flow rate of 30 μL min-1. The voltage-dependent Co oxidation state phasemap of β-Co(OH)2 is also shown.

Image Copyright © 2021 Springer Nature Limited

Reference: Mefford et al., Nature,  2020 Full Paper


Video Spotlight

Operando liquid-electrochemical microscopy reveals the origin of Li charging and discharging of battery primary particles

Hummingbird Scientific supported and collaborated in a study lead by Stanford University in which LixFePO4 battery material particles were charged and discharged in-situ while recording the special charge state using STXM (Scanning Transmission X-ray Microscopy) at Lawrence Berkeley Lab’s Advanced Light Source. This data showed that spatial heterogeneities in reaction rates account for domains with the charging process significantly less uniform than the discharging process. These results highlight the crucial role of surface reaction rate for lithiation, observing these inconsistencies of ion insertion have implications for electrode engineering and battery management for future generation battery technology.

Video: LixFePO4 battery material particles are shown here charging (red to green) and discharging (green to red) in-situ in the X-ray liquid-electrochemical cell. The video shows regions of faster and slower charge.

Video Copyright © 2016 American Association for the Advancement of Science

Reference: Lim et al. Science 2016, 1353 (6299), pp. 566-571. Full Paper

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Customization & Service

Selected Publications

J. Tyler Mefford, Andrew R. Akbashev, Minkyung Kang, Cameron L. Bentley, William E. Gent, Daan Hein Alsem, Norman Salmon, David A. Shapiro, Patrick R. Unwin, William C. Chueh. “Correlative operando microscopy of oxygen evolution electrocatalysts,” Nature (2021)  Abstract
Shapiro, David A., Sergey Babin, Richard S. Celestre, Weilun Chao, Raymond P. Conley, Peter Denes, Bjoern Enders et al. “An ultrahigh-resolution soft x-ray microscope for quantitative analysis of chemically heterogeneous nanomaterials.” Science Advances (2020) Abstract
Mi Yoo, Young-Sang Yu, Hyunwoo Ha, Siwon Lee, Jin-Seok Choi, Sunyoung Oh, Eunji Kang, Hyuk Choi, Hyesung An, Kug-Seung Lee, Jeong Young Park, Richard Celestre, Matthew A. Marcus, Kasra Nowrouzi, Doug Taube, David A. Shapiro, WooChul Jung, Chunjoong Kim and Hyun You Kim . “A tailored oxide interface creates dense Pt single-atom catalysts with high catalytic activity,” Energy & Environmental Science (2020) Abstract
Yimin A. Wu, Ian McNulty, Cong Liu, Kah Chun Lau, Qi Liu, Arvydas P. Paulikas, Cheng-Jun Sun, Zhonghou Cai, Jeffrey R. Guest, Yang Ren, Vojislav Stamenkovic, Larry A. Curtiss, Yuzi Liu & Tijana Rajh, “Facet-dependent active sites of a single Cu2O particle photocatalyst for CO2 reduction to methanol” Nature Energy (2019) Abstract
J. Tyler Mefford, Khim Karki, Daan Hein Alsem, David Shapiro, Norman Salmon and William C. Chueh. ” Operando Scanning Transmission X-ray Microscopy of Co(OH)2 Oxygen Evolution Electrocatalysts,” Microscopy & Microanalysis (2019) Abstract
Khim Karki, Tyler Mefford, Daan Hein Alsem, Norman Salmon, William C Chueh. “Replicating bulk electrochemistry in liquid cell microscopy,” Microscopy & Microanalysis (2018) Abstract
J. Lim,Y. Li, D. H. Alsem, H. So, S. C. Lee, P. Bai, D.A. Cogswell, X. Liu, N. Jin, Y. Yu, N. J. Salmon, D. A. Shapiro, M. Z. Bazant, T.Tyliszczak, W. C. Chueh, “Origin and Hysteresis of Lithium Compositional Spatiodynamics Within Battery Primary Particles”, Science (2016) Abstract
A. Kammers, D.H. Alsem, J. Lim, Y. Li, W. Chueh, N. Salmon. “Accelerating Next Generation Battery Development Through the Application of Cross-Correlative In-Situ Microscopy,” Microscopy & Microanalysis (2015) Abstract
B. Stripe, V. Rose, M. Misek, S.W. Chee, D.H. Alsem, N. Salmon. “Applications of In-Situ Synchrotron Radiation Techniques in Nanomaterials Research,” MRS Spring (2014) Abstract


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