Liquid System Electrochemistry

Hummingbird Scientific was the first company to provide a commercially-available holder capable of supporting liquid-electrochemical experiments conducted inside the TEM.  In subsequent years, we have continued to refine the holder’s capabilities.  In its current configuration, the holder enables electrochemical research via integrated biasing contacts that connect to our specially-patterned electrochemical chips, which are available in a variety of materials. Among other topics, the system has been used for key research into battery materials (see Featured Research below).

The analytical electrochemistry tip features the sample basic capabilities of the standard electrochemistry liquid cell, but it also keeps the electrical contacts outside the experimental space. This option includes an optional low-noise potentiostat and fully shielded cabling for maximum analytical capabilities.

Wiring configurations

  • Standard configuration:  In the standard configuration, the system’s wires are not individually shielded. This configuration can connect to Hummingbird’s heater control box as well as a variety of electronic source and measurement devices.
  • Low current/noise:  For very small current or voltage values, we offer an individually-shielded, low-noise wiring system. In this system, a shielded coaxial cable runs through the holder shaft and connects through special micro-coax connectors in the holder.  The system can be configured for compatibility with a range of potentiostats and power supplies.  It is particularly well-suited for small-scale in-situ liquid electrochemistry measurements.

Biologic SP-200 potentiostat 

We are proud to collaborate with Bio-Logic to offer the Bio-Logic SP-200 potentiostat as a research-grade measurement tool for electrochemistry experiments. Hummingbird Scientific’s liquid-electrochemistry  and Biologic’s SP-200 potentiostat can be used in combination for corrosion experiments, electrochemistry, electrolysis, and battery and photovoltaic research.

 

Featured Research

 

Observation of redox product in lithium-oxygen battery

Lithium-oxygen batteries have exceptional higher energy densities. However, the byproduct lithium peroxide, cannot be easily decomposed during the charging cycle. Now, the work led by researchers from Johns Hopkins University have used Hummingbird Scientific’s liquid electrochemistry TEM holder to demonstrate that the decomposition of lithium peroxide can be improved by adding redox mediators as charge-transfer agents. Their findings are published in the recent issue of Advanced Materials. The fundamental understanding of the lithium-oxygen electrochemistry presented in this work may enable the development of better batteries

Formation of lithium peroxide during discharge. Image copyright © 2017 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim
Formation of lithium peroxide during discharge. Image copyright © 2017 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim

 

Reference: Mingwei Chen et al. Direct Observations of the Formation and Redox-Mediator-Assisted Decomposition of Li2O2 in a Liquid-Cell Li–O2 Microbattery by Scanning Transmission Electron Microscopy. Advanced Materials (2017). Abstract

Electrochemistry Selected Publications

Nikhilendra Singh, Timothy S. Arthur, Oscar Tutusaus, Jing Li, Kim Kisslinger, Huolin L. Xin, Eric A. Stach, Xudong Fan, and Rana Mohtadi. “Achieving High Cycling Rates via In-situ Generation of Active Nanocomposite Metal Anodes.” ACS Applied Energy Materials (2018) Abstract
Chen Houa, Jiuhui Hanb, Pan Liua, Chuchu Yangb, Gang Huangb, Takeshi Fujitab, Akihiko Hiratab, and Mingwei Chen. “Operando observations of RuO2 catalyzed Li2O2 formation and decomposition in a Li-O2 micro-battery,” Nano Energy (2018) Abstract
Pan Liu, Jiuhui Han, Xianwei Guo, Yoshikazu Ito, Chuchu Yang, Shoucong Ning, Takeshi Fujita, Akihiko Hirata and Mingwei Chen. “Operando characterization of cathodic reactions in a liquid-state lithium-oxygen micro-battery by scanning transmission electron microscopy,” Scientific Reports (2018) Abstract
Edward R. White, Jared J. Lodico & B. C. Regan. “Intercalation events visualized in single microcrystals of graphite,” Nature Communications (2017) Abstract
Chuchu Yang, Jiuhui Han, Pan Liu, Chen Hou, Gang Huang, Takeshi Fujita, Akihiko Hirata, and Mingwei Chen. “Direct Observations of the Formation and Redox-Mediator-Assisted Decomposition of Li2O2 in a Liquid-Cell Li–O2 Microbattery by Scanning Transmission Electron Microscopy,” Advanced Materials (2017) Abstract
Timothy S. Arthur, Per-Anders Glans, Nikhilendra Singh, Oscar Tutusaus, Kaiqi Nie, Yi-Sheng Liu, Fuminori Mizuno, Jinghua Guo, Daan Hein Alsem, Norman J. Salmon, and Rana Mohtadi. “Interfacial insight from operando sXAS/TEM for magnesium metal deposition with borohydride electrolytes,” Chemistry of Materials (2017) Abstract
J. R. Vance  and  S. J. Dillon. “Thermally driven bubble evolution at a heater wire in water characterized by high-speed transmission electron microscopy,”  Chemical Communications (2017) Abstract
J. P.  Patterson, L. R. Parent, J. Cantlona, H. Eickhoffa, G. Bareda, J. E. Evansa and N.C. Gianneschia. “Picoliter Drop-On-Demand Dispensing for Multiplex Liquid Cell Transmission Electron Microscopy,” Microscopy & Microanalysis (2016) Abstract
Omid Sadeghi, Clément Falaise, Pedro I. Molina, Ryan Hufschmid, Charles F. Campana, Bruce C. Noll, Nigel D. Browning, and May Nyman. “Chemical Stabilization and Electrochemical Destabilization of the Iron Keggin Ion in Water,” Inorganic Chemistry (2016) Abstract
R. R. Unocic, L. Baggetto, G. M. Veith, J. A. Aguiar, K. A. Unocic, R. L. Sacci, N. J. Dudneyb and K. L. Morea. “Probing battery chemistry with liquid cell electron energy loss spectroscopy,” Chem. Communication (2015) Abstract
R.R. Unocic. “In-situ Liquid S/TEM: Practical Aspects, Challenges, and Opportunities,” Microscopy and Microanalysis (2015)  Abstract
W. Zhang, D.H. Alsem, F. Wang, N. Salmon. “In-Situ Liquid Cell TEM Studies of Electrochemical Reaction in Lithium-Ion Batteries,” Microscopy & Microanalysis (2015)   Abstract
C. Wang. “In situ transmission electron microscopy and spectroscopy studies of rechargeable batteries under dynamic operating conditions: A retrospective and perspective view.” Journal of Materials Research (2015) Abstract
P. Abellan, B. L. Mehdi, L.R. Parent, M. Gu, C. Park, W. Xu, Y. Zhang, I. Arslan, J.G. Zhang, C.M. Wang, J.E. Evans, and N.D. Browning ”
Probing the Degradation Mechanisms in Electrolyte Solutions for Li-Ion Batteries by in Situ Transmission Electron Microscopy” Nano Letter (2014)
Abstract
S.W. Chee, D.J. Duquette, F.M. Ross, and R. Hull. “Metastable Structures in Al Thin Films Before the Onset of Corrosion Pitting as Observed using Liquid Cell Transmission Electron Microscopy,” Micoscopy & Microanalysis (2014) Abstract
R.R. Unocic, X.G. Sun, R.L. Sacci, L.A. Adamczyk, D.H. Alsem, S. Dai, N.J. Dudney, and K.L. More. “Direct Visualization of Solid Electrolyte Interphase Formation in Lithium-Ion Batteries with In Situ Electrochemical Transmission Electron Microscopy,” Microscopy & Microanalysis (2014) Abstract
R.L. Sacci, N. Dudney, K. More, L.R. Parent, I. Arslan, N.D. Browning, and R.R. Unocic. “Direct Visualization of Initial SEI Morphology and Growth Kinetics During Lithium Deposition by In-Situ Electrochemical Transmission Electron Microscopy,” Chem. Communication (2014) Abstract
J.M. Miller, D.H. Alsem, N. Salmon, N.E. Johnson and J.E. Hutchison. “Functionalized Surfaces to Improve Imaging Conditions in Liquid Cell Transmission Electron Microscopy. ” Microscopy & Microanalysi (2014) Abstract
M. Gu, L.R. Parent, B.L. Mehdi, R.R. Unocic, M.T. McDowell, R.L. Sacci, W. Xu, J.G. Connell, P. Xu, P. Abellan, X. Chen,Y. Zhang, D.E. Perea, J.E. Evans, L.J. Lauhon, J.G. Zhang, J. Liu, N.D. Browning, Y. Cui, I. Arslan, and C.M. Wang. “Demonstration of an Electrochemical Liquid Cell for Operando Transmission Electron Microscopy Observation of the Lithiation/Delithiation Behavior of Si Nanowire Battery Anodes.” Nano Letter (2013) Abstract
Y.Z. Liu, X.M. Lin, Y.G. Sun, T. Rajh. “In-Situ Visualization of Self-Assembly of Charged Gold Nanoparticles.” J. Am. Chem. Soc. 135:10 (2013) pp. 3764–3767 Abstract
G. Zhu, Y. Jiang, W. Huang, H. Zhang, F. Lin, and C. Jin. “Atomic Resolution Liquid-Cell Transmission Electron Microscopy Investigations of the Dynamics of Nanoparticles in Ultrathin Liquids,” Chem. Commun. 49 (2013) pp. 10944‒10946 Abstract
M.H. Nielsen, J.R.I. Lee, Q. Hu, T. Y.-J. Han, and J.J. De Yoreo, “Structural evolution, formation pathways and energetic controls during template-directed nucleation of CaCO3,” Faraday Discuss. 159 (2012) pp. 105–121 Abstract
D. Li, M.H. Nielsen, J.R.I. Lee, C. Frandsen, J.F. Banfield, and J.J. De Yoreo. “Direction-Specific Interactions Control Crystal Growth by Oriented Attachment,” Science 336:6084 (2012) pp. 1014–1018 Abstract
E.R. White, M. Mecklenburg, B. Shevitski, S.B. Singer, and B.C. Regan, “Charged nanoparticle dynamics in water induced by scanning transmission electron microscopy,” Langmuir 28:8 (2012) pp. 3695–3698 Abstract
E.R. White, S.B. Singer, V. Augustyn, W.A. Hubbard, M. Mecklenburg, B. Dunn, and B.C. Regan,“In-Situ Transmission Electron Microscopy of Lead Dendrites and Lead Ions in Aqueous Solution” ACS Nano 6:7 (2012) pp. 6038–6317 Abstract
K.L. Jungjohann, J.E. Evans, J.A Aguiar , I. Arslan, N.D. Browning. “Atomic-scale imaging and spectroscopy for in-situ liquid scanning transmission electron microscopy.” Microscopy & Microanalysis 18:03 (2012) pp. 621–627  Abstract
L.R. Parent, D.B. Robinson, T.J. Woehl, W.D. Ristenpart, J.E. Evans, N.D. Browning, I. Arslan “Direct in-situ observation of nanoparticle synthesis in a liquid crystal surfactant template,” ACS Nano 6:4 (2012) pp. 3589–3596  Abstract
T.J. Woehl , J. E. Evans, I. Arslan, W.D. Ristenpart , N.D. Browning “Direct in-situ determination of the mechanisms controlling nanoparticle nucleation and growth,” ACS Nano 6:10 (2012) pp. 8599–8610  Abstract
J.E. Evans, K.L. Jungjohann, P.C.K. Wong, P.L. Chiua, G.H. Dutrowa, I. Arslan, N.D. Browning. “Visualizing macromolecular complexes with in-situ liquid scanning transmission electron microscopy” Micron 43:11 (2012) pp. 1085–1090  Abstract
R.R. Unocic, L. Baggetto, K.A. Unocic, G.M. Veith, N.J. Dudney, and K.L. More. “Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy.” Microscopy and Microanalysis 18 (Suppl 2), (2012) 1104-1105 Abstract
K.L. Jungjohann, J.E. Evans, J.A Aguiar , I. Arslan, N.D. Browning. “Atomic-scale imaging and spectroscopy for in-situ liquid scanning transmission electron microscopy.” Microscopy & Microanalysis 18:03 (2012) pp. 621–627. Abstract
K.L. Jungjohann, J.E. Evans, I. Arslan, N.D. Browning. “Electron Energy Loss Spectroscopy for Aqueous in-Situ Scanning Transmission Electron Microscopy.” Microscopy & Microanaysis 17:S2 (2011) pp. 778–779. Abstract
J.E. Evans, K.L. Jungjohann, N.D. Browning and I. Arslan. “Controlled Growth of Nanoparticles from Solution with In-Situ Liquid Transmission Electron Microscopy,” Nano Lett. 11:7 (2011) pp. 2809–2813  Abstract
N. de Jonge, D.B. Peckys, G.J. Kremers, D.W. Piston. “Electron microscopy of whole cells in liquid with nanometer resolution,” PNAS 106:7 (2009) pp. 2159–2164  Abstract
J.E. Evans, N.D. Browning, “Enabling Direct Nanoscale Observations of Biological Reactions with Dynamic TEM,” Microscopy 62:1 (2013) pp. 147–156  Abstract
E.R. White, M. Mecklenburg, B. Shevitski, S.B. Singer, and B.C. Regan, “Charged nanoparticle dynamics in water induced by scanning transmission electron microscopy,” Langmuir 28:8 (2012) pp. 3695–3698  Abstract
R.R. Unocic, L.A. Adamczyk, N.J. Dudney, D.H. Alsem, N.J. Salmon, and K.L. More. “In-Situ Electron Microscopy of Electrical Energy Storage Materials,” ECS Fall Meeting 2010 Abstract
C.M. Wang, W. Xu, J. Liu, D.W. Choi, B. Arey, L.V. Saraf, J.G. Zhang, Z.G. Yang, S. Thevuthasan, D.R. Baer, and N. Salmon. “In-situ transmission electron microscopy and spectroscopy studies of interfaces in Li ion batteries: Challenges and opportunities,” J. Mater. Res. 25:8 (2010) pp. 1541–1547 Abstract

 

Read More