Bulk Liquid Electrochemistry
1490 series | |
Total Electrodes | 6 |
True Reference Electrode | Yes- drift rate less than 0.1 mV/min |
True Counter Electrode | Yes |
Counter Electrode Material | User’s choice of material |
Electrolytes | Aqueous, Wide range of organics* |
Spacer range | 100nm to 2 μm* |
Heating Capability | Yes |
EELS/ EDS Compatible | Yes |
TEM Compatibility | TFS/FEI, JEOL, Hitachi |
Fe incorporation into NiO particles resolved using in-situ TEM
Researchers at the Fritz-Haber-Institut der Max-Planck-Gesellschaft published recent work demonstrating the powerful capability of the Hummingbird Scientific Gen V In-situ Bulk Liquid-electrochemistry TEM sample holder to characterize the evolution of octahedral NiO catalyst particles under repeated high-cycle electrochemical cycling in a liquid cell infused with Fe-containing electrolyte. The electrochemical response for the holder re-produces the expected shift in OER onset potential due to Fe impurities in the electrolyte changing the chemistry of the catalyst. These results clarify the structural evolution of a NiO surface during OER and the critical role of Ni-Fe layered double hydroxide formation and degradation in determining the electrocatalytic performance.
Figure: (a-d) In-situ STEM images, combined Ni/Fe chemical EDS maps and STEM/Fe EDS maps of NiO octahedra during and after CV cycling. (e) Cyclic voltammograms collected before and after Fe addition and CV cycling. (f) Schematic of two-stage mechanism for Fe incorporation into NiO octahedra.
Image Copyright © 2023 The Authors. Published by American Chemical Society.
Reference: Yang et. al. J. Am. Chem. Soc. 145 (39) 21465-21474 (2023) DOI: 10.1021/jacs.3c07158
EditReplicating bulk electrochemistry experiments in-situ in the TEM
Hummingbird Scientific’s newest Generation V Bulk in-situ liquid-electrochemistry holder allows researchers for the first time to fully replicate bulk-level electrochemical details inside the transmission electron microscope. A newly developed hardware system allows quantitative measurements of electrochemical processes with details showing the complete cycle of the bulk.
As an illustration, a cyclic voltammetry (CV) study of a model compound CuSO4 solution showing plating and stripping of copper from the active electrode has been presented here. The copper plating and stripping occurs at the working electrode, replicating actual bulk behavior.
Video: In-situ liquid cell TEM copper plating and stripping from CuSO4 solution. Inset shows corresponding CV curve representing the video.
HBS internal data obtained in collaboration with Rui Filipe Serra Maia and Eric Stach at the University of Pennsylvania.
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Morgan Binggeli, Tzu-Hsien Shen, and Vasiliki Tileli. “Simulating Current Distribution of Oxygen Evolution Reaction in Microcells Using Finite Element Method.” J. Electrochem. Soc. (2021) | Abstract |
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See Wee Chee, Aram Yoon, Rosa Aran-Ais, Ruben Rizo, Philipp Grosse, and Beatriz Roldan Cuenya. “Investigating the Behavior of Cu-based Catalysts During Electrochemical CO2 Reduction with Liquid Cell Electron Microscopy.” Microscopy & Microanalysis (2020) | Abstract |
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Robin Girod, Nikolaos Nianias, and Vasiliki Tileli. “Electrochemical Behavior of Carbon Electrodes for In Situ Redox Studies in a Transmission Electron Microscope.” Microscopy & Microanalysis (2019) | Abstract |
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Khim Karki, Daan Hein Alsem, and Norman Salmon. “Practical Electroanalytical Measurements in Liquid Cell TEM.” Microscopy & Microanalysis (2018) | Abstract |
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Feng Yan, Lili Liu, Tiffany R. Walsh, Yu Gong, Patrick Z. El-Khoury, Yanyan Zhang, Zihua Zhu, James J. De Yoreo, Mark H. Engelhard, Xin Zhang, and Chun-Long Chen. “Controlled synthesis of highly-branched plasmonic gold nanoparticles through peptoid engineering.” Nat. Commun. (2018) | Abstract |
Claudia Stauch, Christopher Hobbs, Aleksey Shmeliov, Valeria Nicolosi, Thomas Ballweg, Robert Luxenhofer, and Karl Mandel. “Colloidal Core–Satellite Supraparticles via Preprogramed Burst of Nanostructured Micro‐Raspberry Particles.” Particle & Particle Systems Characterization (2018) | Abstract |
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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 |
Jeung Hun Park, Nicholas M. Schneider, Daniel A. Steingart, Hariklia Deligianni, Suneel Kodambaka, and Frances M. Ross. “Control of Growth Front Evolution by Bi Additives during ZnAu Electrodeposition.” Nano Letters (2018) | Abstract |
Trevor H. Moser, Hardeep Mehta, Chiwoo Park, Ryan T. Kelly, Tolou Shokuhfar, and James E. Evans. “The role of electron irradiation history in liquid cell transmission electron microscopy,” Science Advances (2018) | Abstract |
Lili Liu, Shuai zhang, Mark E. Bowden, Jharna Chaudhuri, and James J. De Yoreo. “In-situ TEM and AFM investigation of morphological controls during the growth of single crystal BaWO4.” Crystal Growth & Design (2017) | Abstract |
Edward R. White, Jared J. Lodico, and B. C. Regan. “Intercalation events visualized in single microcrystals of graphite.” Nat. Commun. (2017) | Abstract |
Julio A. Rodriguez Manzo, Norman J. Salmon, and Daan Hein Alsem. “In Situ TEM Observation of Water Splitting.” Microscopy & Microanalysis (2017) | Abstract |
YuBo Wang, Shuai Wang, and Xing Lu. “In Situ Observation of the Growth of ZnO Nanostructures Using Liquid Cell Electron Microscopy,” The Journal of Physical Chemistry C (2017) | Abstract |
See Wee Chee, Shu Fen Tan, Zhaslan Baraissov, Michel Bosman, and Utkur Mirsaidov. “Direct observation of the nanoscale Kirkendall effect during galvanic replacement reactions.” Nat. Commun. (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 |
Jongwoo Lim, Yiyang Li, Daan Hein Alsem, Hongyun So, Sang Chul Lee, Peng Bai, Daniel A. Cogswell, Xuxhao Liu, Norman Jin, Young-sang Yu, Norman J. Salom, David A. Shapiro, Martin Z. Bazant, Tolek Tyliszczak, and William C. Chueh. “Origin and hysteresis of lithium compositional spatiodynamics within battery primary particles,” Science (2017) | Abstract |
Jongwoo Lim, Yiyang Li, Daan Hein Alsem, Hongyun So, Sang Chul Lee, Peng Bai, Daniel A. Cogswell, Xuzhao Liu, Norman Jin, Young-sang Yu, Norman J. Salmon, David Shapiro, Martin Z. Bazant, Tolek Tyliszczak, and William Chueh. “Using Scanning Transmission X-ray Microscopy to Reveal the Origin of Lithium Compositional Spatiodynamics in Battery Materials.” Microscopy & Microanalysis (2017) | Abstract |
Eli Fahrenkrug, Daan Hein Alsem, Norman Salmon, and Stephen Maldonado. “Electrochemical Measurements in In Situ TEM Experiments,” Journal of the Electrochemical Society (2017) | Abstract |
Eli Fahrenkrug, Daan Hein Alsem, Norman Salmon, and Stephen Maldonado. “Electrochemical Measurements during In Situ Liquid-Electrochemical TEM Experiments.” Microscopy & Microanalysis (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 |
Jeung Hun Park, Daniel A. Steingart, Suneel Kodambaka, and Frances M. Ross. “Electrochemical electron beam lithography: Write, read, and erase metallic nanocrystals on demand,” Science Advances (2017) | Abstract |
Jianbo Wu, Wenpei Gao, Hong Yang, and Jian-Min Zuo. “Dissolution Kinetics of Oxidative Etching of Cubic and Icosahedral Platinum Nanoparticles Revealed by in Situ Liquid Transmission Electron Microscopy,” ACS Nano (2017) | 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 |
Ainsley Pinkowitz, See Wee Chee, Brent J. Engler, David J. Duquette, and Robert Hull. “An In Situ Transmission Electron Microscopy Study of Localized Corrosion on Aluminum.” MRS Adv. (2016) | Abstract |
Colm O’Regan, Xi Zhu, Jun Zhong, Utkarsh Anand, Jingyu Lu, Haibin Su, and Utkur Mirsaidov. “CTAB-Influenced Electrochemical Dissolution of Silver Dendrites.” Langmuir (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. Commun. (2015) | Abstract |
R.R. Unocic. “In-situ Liquid S/TEM: Practical Aspects, Challenges, and Opportunities.” Microscopy & Microanalysis (2015) | Abstract |
W. Zhang, D.H. Alsem, F. Wang, and N. Salmon. “In-Situ Liquid Cell TEM Studies of Electrochemical Reaction in Lithium-Ion Batteries.” Microscopy and Microanalysis (2015) | Abstract |
J.P. Patterson, P. Abellan, M.S. Denny, C. Park, N.D. Browning, S.M. Cohen, J.E. Evans, and N.C. Gianneschi. “Observing the Self-assembly of Metal-Organic Frameworks by In-Situ Liquid Cell TEM.” Microscopy and Microanalysis (2015) | Abstract |
J.-M. Zuo, A. Yoon, W. Gao, J. Wu, and H. Park. “Materials processes observed using dynamical environmental TEM at University of Illinois.” Microscopy & Microanalysis (2015) | Abstract |
T.J. Woehal, S. Kashyap, E. Firlar, T. Perez-Gonzalez, D. Faivre, D. Trubitsyn, D. Bazylinski, and T. Prozorov. “Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In-Vivo Imaging.” Microscopy & Microanalysis (2015) | Abstract |
Feng Wang, Wei Zhang, Peng Gao, and Khim Karki. “Tracking Ionic Transport and Electrochemical Dynamics in Battery Electrodes Using in situ TEM-EELS.” Microscopy & Microanalysis (2015) | Abstract |
Jeung Hun Park, See Wee Chee, Suneel Kodambaka, and Frances M. Ross. “In Situ LC-TEM Studies of Corrosion of Metal Thin Films in Aqueous Solutions.” Microscopy & Microanalysis (2015) | Abstract |
T.J. Woehl, and T. Prozorov. “Visualization of gold nanoparticle self-assembly kinetics.” Microscopy & Microanalysis (2015) | Abstract |
See Wee Chee, Jeung-Hun Park, Ainsley Pinkowitz, Brent Engler, Frances M. Ross, David Duquette, and Robert Hull. “Liquid Cell TEM of Al Thin Film Corrosion under Potentiostatic Polarization.” Microscopy & Microanalysis (2015) | Abstract |
N. Bhattarai, and T. Prozorov. “In-situ STEM Investigation of Shape-Controlled Synthesis of Au-Pd Core-Shell Nanocube.” Microscopy & Microanalysis (2015) | Abstract |
S.W. Chee, D. Loh, U Mirsaidov, and P. Matsudaira. “Probing Nanoparticle Dynamics in 200nm Thick Liquid Layers at Millisecond Time Resolution.” 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. J. M. Smeets, K. R. Cho, R. G. E. Kempen, N. A. J. M. Sommerdijk, and J. J. De Yoreo. “Calcium carbonate nucleation driven by ion binding in a biomimetic matrix revealed by in situ electron microscopy.” Nat. Mater. Letters (2015) | Abstract |
E. Sutter, K. Jungjohann, S. Bliznakov, A. Courty, E. Maisonhaute, S. Tenney, and P. Sutter. “In situ liquid-cell electron microscopy of silver–palladium galvanic replacement reactions on silver nanoparticles.” Nat. Commun. (2014) | Abstract |
M.H. Nielsen, S. Aloni, and J.J. De Yoreo. “In situ TEM imaging of CaCO3 nucleation reveals coexistence of direct and indirect pathways.” Science (2014) | Abstract |
B. Layla Mehdi, Meng Gu, Lucas R. Parent, Wu Xu, Eduard N. Nasybulin, Xilin Chen, Raymond R. Unocic, Pinghong Xu, David A. Welch, Patricia Abellan, Ji-Guang Zhang, Jun Liu, Chong-Min Wang, Ilke Arslan, James Evans, and Nigel D. Browning. “In-Situ Electrochemical Transmission Electron Microscopy for Battery Research.” Microscopy & Microanalysis (2014) | Abstract |
Nicholas M. Schneider, Jeung Hun Park, Joseph M. Grogan, Suneel Kodambaka, Daniel A. Steingart, Frances M. Ross, and Haim H. Bau. “Visualization of Active and Passive Control of Morphology during Electrodeposition.” Microscopy & Microanalysis (2014) | 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 Lett. (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. Commun. (2014) | Abstract |
D.A. Fischer, D.H. Alsem, B. Simon, T. Prozorov, and N. Salmon. “Development of an Integrated Platform for Cross-Correlative Imaging of Biological Specimens in Liquid using Light and Electron Microscopies.” Microscopy & Microanalysis (2013) | 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 Lett. (2013) | Abstract |
S.W. Chee, F.M. Ross, D. Duquette, and R. Hull. “Studies of Corrosion of Al Thin Films using Liquid-Cell Transmission Electron Microscopy.” MRS Proceedings (2013) | Abstract |
K.L. Jungjohann, S. Bliznakov, P.W. Sutter, E.A. Stach, and E.A. Sutter. “In-Situ Liquid Cell Electron Microscopy of the Solution Growth of Au-Pd Core-Shell Nanostructures.” Nano. Lett. (2013) | Abstract |
Lucas R. Parent, Volker Presser, Yury Gogotsi, Raymond R. Unocic, Robert L. Sacci, James E. Evans, Nigel D. Browning, Emilie Perre, Bruce Dunn, and Ilke Arslan. “Direct Observation of Pseudocapacitor Electrode Behavior During Electrochemical Biasing using in-situ Liquid Stage Electron Microscopy.” Microscopy & Microanalysis (2013) | Abstract |
Robert L. Sacci, Nancy J. Dudney, Karren L. More, and Raymond R. Unocic. “Quantitative In Situ Electrochemical Liquid Cell Characterization of SEI Formation in Lithium Ion Batteries.” Microscopy & Microanalysis (2013) | Abstract |
Y.Z. Liu, X.M. Lin, Y.G. Sun, and T. Rajh. “In-Situ Visualization of Self-Assembly of Charged Gold Nanoparticles.” J. Am. Chem. Soc. (2013) | 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 (2012) | Abstract |
T.J. Woehl, J. E. Evans, I. Arslan, W.D. Ristenpart, and N.D. Browning. “Direct in-situ determination of the mechanisms controlling nanoparticle nucleation and growth.” ACS Nano (2012) | 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 & Microanalysis (2012) | 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 (2012) | Abstract |
K.L. Jungjohann, J.E. Evans, I. Arslan, and N.D. Browning. “Electron Energy Loss Spectroscopy for Aqueous in-Situ Scanning Transmission Electron Microscopy.” Microscopy & Microanalysis (2011) | Abstract |
R. R. Unocic, L. A. Adamczyk, N. J. Dudney, D. H. Alsem, N. J. Salmon, and K. L. More. “In-situ TEM Characterization of Electrochemical Processes in Energy Storage Systems.” Microscopy & Microanalysis (2011) | 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 |
Raymond R. Unocic, Leslie A. Adamczyk, N. Dudney, Karren L. More, Daan Hein Alsem, and Norman Salmon. “In-Situ TEM Characterization of the SEI in Li-Ion Batteries.” ECS Meet. Abstr. (2010) | Abstract |
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