Bulk Liquid Electrochemistry

Generation V: Introducing the world's first bulk liquid-electrochemistry TEM holder

Technical Specs

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 um*
Heating Capability Yes
EELS/ EDS Compatible Yes
TEM Compatibility TFS/FEI, JEOL, Hitachi

* Contact us for Custom Configurations

Features

Featured Research

Replicating 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.

The new Hummingbird Scientific’s liquid-cell hardware and cells allows, for the first time, for replication of bulk-level data in TEM.

Video  Right: 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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Video Spotlight

Electrochemical deposition of a conducting polymer on a gold electrode

Video on the left shows the methodological and controlled deposition of polyaniline – a conducting polymer – from solution into a gold electrode. The deposition starts at the interface between the working electrode and electrolyte solution. The electrode surface is heavily modified as the polymer deposits. This observation helps understanding the rate determining processes of nucleation and growth, which has an important application in corrosion protection of materials.

Hummingbird Scientific internal data.

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Customization & Service

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
Mei Sun, Xing Li, Zhiqiang Tang, Xianlong Wei and Qing Chen. “Constant-Rate Dissolution of InAs Nanowires in Radiolytic Water Observed by In situ Liquid Cell TEM.” Nanoscale (2018) Abstract
Khim Karki, Tyler Mefford, Daan Hein Alsem, Norman Salmon, and William C. Chueh. “Replicating Bulk Electrochemistry in Liquid Cell Microscopy,” Microscopy & Microanalysis (2018) Abstract
Khim Karki, Daan Hein Alsem, and Norman Salmon. “Practical Electroanalytical Measurements in Liquid Cell TEM,” Microscopy & Microanalysis (2018) Abstract
Jeung Hun Park, Tommy Watanabe, Ainsley Pinkowitz, David J. Duquette, Robert Hull, Daniel A. Steingart and Frances M. Ross. “In situ EC-TEM Studies of Metal Thin Film Corrosion in Liquid Solutions at Elevated Temperatures.” Microscopy & Microanalysis (2018) Abstract
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,” Nature Communications (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
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
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 & B. C. Regan. “Intercalation events visualized in single microcrystals of graphite,” Nature Communications (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 & Utkur Mirsaidov. “Direct observation of the nanoscale Kirkendall effect during galvanic replacement reactions,” 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
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
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. Advance Article (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 and Microanalysis (2015)   Abstract
J.P. Patterson, P. Abellan, M.S. Denny, C. Park, N.D. Browning, S.M. Cohen, J.E. Evans, 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, H. Park. “Materials processes observed using dynamical environmental TEM at University of Illinois,” Microscopy and Microanalysis (2015)  Abstract
T.J. Woehal, S. Kashyap, E. Firlar, T. Perez-Gonzalez, D. Faivre, D. Trubitsyn, D. Bazylinski, T. Prozorov. “Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In-Vivo Imaging,” Microscopy and Microanalysis (2015)  Abstract
T.J. Woehl, T. Prozorov. “Visualization of gold nanoparticle self-assembly kinetics,” Microscopy and Microanalysis (2015)  Abstract
N. Bhattarai, T. Prozorov. “In-situ STEM Investigation of Shape-Controlled Synthesis of Au-Pd Core-Shell Nanocube,” Microscopy and Microanalysis (2015)  Abstract
S.W. Chee, D. Loh, U Mirsaidov, P. Matsudaira, “Probing Nanoparticle Dynamics in 200 nm 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, 30, (2015) pp 326-339 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, Nature Materials Letters, Published Online 01/26/2015. Abstract
E. Sutter, K. Jungjohann, S. Bliznakov, A. Courty, E. Maisonhaute, S. Tenney & P. Sutter. “In situ liquid-cell electron microscopy of silver–palladium galvanic replacement reactions on silver nanoparticles.” Nature Communications, 5, Article number: 4946 doi:10.1038/ncomms5946 Abstract
 M.H. Nielsen, S. Aloni, J.J. De Yoreo.  “In situ TEM imaging of CaCO3 nucleation reveals coexistence of direct and indirect pathways”, Science vol. 345 iss. 6201 (2014) pp. 1158-1162 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. 14:3 (2014) 1293-1299
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 and Microanalysis 20:2 (2014) pp. 462‒468 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 and Microanalysis 20:4 (2014) pp.1029‒1037 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. 50 (2014) pp. 2104‒2107 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 and Microanalysis, 19 (Suppl. 2) , pp 476-477. (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. 13:12 (2013) pp. 6106‒6112 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 1525 (2013) Abstract
K.L. Jungjohann, S. Bliznakov, P.W. Sutter, E.A. Stach, E.A. Sutter. “In-Situ Liquid Cell Electron Microscopy of the Solution Growth of Au-Pd Core-Shell Nanostructures,” Nano. Lett. 13 (2013) pp. 2964–2970 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
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
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
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, 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
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

 

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