Synthesis
| Gas-Heating TEM | Liquid-Heating-Optical TEM | Heating-Biasing TEM | Tomography TEM | Liquid X-Ray | ||
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TEM/SEM/X-Ray Holders for Synthesis Research
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Gas Flow HolderSee MoreHeating in reaction gas environments up to 1.5 atmosphere |
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Liquid Flow HolderSee MoreHeating, biasing and/or optical stimulation of samples reacting in liquid environments |
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Heating/Biasing HolderSee MoreHeating, biasing of samples reacting in vacuum environments |
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Tomography HolderSee MorePre or post-mortem material analysis |
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X-Ray/Synchrotron Liquid HolderSee MoreA complete in-situ x-ray lab system |
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Controlled Synthesis of Highly Branched Au Nanoparticles
Predictive synthesis of bio-inspired materials is desired for engineering proteins and other highly complex biomolecules. The researchers led by Pacific Northwest National Laboratory have used in-situ liquid TEM platform to design sequence-defined peptoids for systematically controlling the formation of gold nanomaterials.
The TEM image of the left shows time-series formation and evolution of gold nanoparticles from spherical to coral-shape. Scale bar 20 nm.
Reference: 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
Image Copyright © 2018 Springer Nature Limited.
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Synthesis and Optimization of Perovskite for Solar Cells
In-situ gas cell heating of FAPbI3 (FA-based perovskite) in argon leads to the formation (T<175˚C) and then segregation (T> 175˚C) of Pb precipitates at the grain boundaries (bright contrast). Upon optimization of synthesis procedures (e.g. stable T of 175˚C), device efficiencies of up to 17.09% obtained.
Left: Sequential atomic contrast STEM images accompanied by normalized histograms showing the evolution of grain interiors (blue curve) and multiple grain boundaries (red curve).
Reference: Jeffery A. Aguiar, Sarah Wozny, Terry G. Holesinger, Toshihiro Aoki, Maulik K. Patel, Mengjin Yang, Joseph J. Berry, Mowafak Al-Jassim, Weilie Zhou and Kai Zhu. “In situ investigation of the formation and metastability of formamidinium lead tri-iodide perovskite solar cells,” Energy & Environmental Science (2016) . Abstract
Image Copyright © The Royal Society of Chemistry 2016.
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Gas Delivery
Hummingbird Scientific’s gas-flow holder comes with either a single-channel or a multi-channel delivery system.
Single-channel gas delivery system
Hummingbird’s single-channel gas delivery system delivers a single pressure-controlled gas to the environmental cell.
Multi-channel gas delivery system
Hummingbird Scientific’s multi-channel gas delivery system is fully configurable and scalable, designed to deliver multiple pressure-controlled gases to an environmental cell at the same time.
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Heating
Our thin-film heating system for the gas holder discretely heats samples in the gas cell to > 1000ºC. Low-drift, high image stability and long lifetimes > 160 hours make the heating system not only robust, but allows tracking of the area of interest while imaging at high-magnification.
Heating is controlled via a custom-designed control box and software featuring closed-loop temperature control and four-point probe temperature sensing from an on-chip sensor.
Our liquid heating system is optimized for moderate temperature requirements. Heating is performed using a thin-film heater inside the liquid cell, which heats up to the boiling point of your solution (max 200˚C).
Read More About Liquid Heating
EditThe Origins of a Mineral
In a study published in Science, researchers at Lawrence Berkeley, Pacific Northwest National Laboratories, and the University of Washington used Hummingbird Scientific’s dual-flow liquid-TEM sample holder to directly observe calcium carbonate crystal nucleation. Their research reveals the presence of multiple simultaneously-operating nucleation pathways and calls into question traditional assumptions about the nature of the nucleation process. “For a decade, we’ve been studying the formation pathways of carbonates using high-powered microscopes,” explains Dr. Jim DeYoreo, the project lead, in a PNNL press release. “But we hadn’t had the tools to watch the crystals form in real time. Now we know the pathways are far more complicated than envisioned in the models established in the twentieth century.”
Because calcium carbonate is the largest global carbon sink, the results of this study have particular relevance to climatologists, who could use them to help explain the processes through which carbon dioxide is sequestered in rocks, minerals, shells, and reefs. In future work, Dr. DeYoreo and his fellow researchers hope to observe living organisms’ roles in calcium carbonate nucleation.
Reference: 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 345:6201 (2014) pp. 1158–1162 Abstract
Copyright © 2014, American Association for the Advancement of Science
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Concurrent formation of multiple phases. All scale bars are 500nm. Image courtesy of M.H. Nielson et al. Copyright © 2014, American Association for the Advancement of Science.
Self-Assembly of Branched Nanocrystals
Inverted dark-field STEM images showing the formation of ordered chains of CdSe/CdS octapods in toluene. The video shows the evolution of the system starting from single octapods dispersed in the entire liquid volume to interlocked chain-like structures.
Left: Total width and height of video frame is 3.64 μm x 3.64 μm
References: Eli Sutter, Peter Sutter, Alexei V. Tkachenko, Roman Krahne, Joost de Graaf, Milena Arciniegas and Liberato Manna. “In situ microscopy of the self-assembly of branched nanocrystals in solution,” Nature Communications (2016) Abstract
Video Copyright © 2018 Springer Nature Limited
Top page banner: Video Copyright © 2018 Springer Nature Limited
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| Shu Fen Tan, Geeta Bisht, Utkarsh Anand, Michel Bosman, Xin Ee Yong, and Utkur Mirsaidov. “In situ Kinetic and Thermodynamic Growth Control of Au-Pd Core-Shell Nanoparticles.” Journal of the American Chemical Society (2018) | Abstract |
| Jeffery A. Aguiar, Nooraldeen R. Alkurd, Sarah Wozny, Maulik K. Patel, Mengjin Yang, Weilie Zhou, Mowafak Al-Jassim, Terry G. Holesinger, Kai Zhu and Joseph J. Berry. “In situ investigation of halide incorporation into perovskite solar cells,” MRS Communications (2017) | Abstract |
| Jeffery A. Aguiar, Sarah Wozny, Terry G. Holesinger, Toshihiro Aoki,d Maulik K. Patel, Mengjin Yang, Joseph J. Berry, Mowafak Al-Jassim, Weilie Zhou and Kai Zhu. “In situ investigation of the formation and metastability of formamidinium lead tri-iodide perovskite solar cells,” Energy & Environmental Science (2016) | Abstract |
| Dongdong Xiao, Zhigang Wu, Miao Song, Jaehun Chun, Gregory K. Schenter, and Dongsheng Li. “Silver Nanocube and Nanobar Growth via Anisotropic Monomer Addition and Particle Attachment Processes,” Langmuir (2017) | 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 |
| 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 |
| Mingyuan Ge, Ming Lu, Yong Chu & Huolin Xin. “Anomalous Growth Rate of Ag Nanocrystals Revealed by in situ STEM,” Scientific Reports (2017) | Abstract |
| Lucas R. Parent, Evangelos Bakalis, Abelardo Ramírez-Hernández, Jacquelin K. Kammeyer, Chiwoo Park, Juan de Pablo, Francesco Zerbetto, Joseph P. Patterson, and Nathan C. Gianneschi.”Directly Observing Micelle Fusion and Growth in Solution by Liquid-Cell Transmission Electron Microscopy,” Journal of the American Chemical Society (2017) | Abstract |
| E. Sutter, P. Sutter, A. V. Tkachenko, R. Krahne, J. De Graff, M. Arciniegas and L. Manna. “In situ microscopy of the self-assembly of branched nanocrystals in solution,” Nature Communications (2016) | Abstract |
| J.H. Park, N.M. Schneider, J.M. Grogan, M.C. Reuter, H.H. Bau, S. Kodambaka & F.M. Ross. “Control of Electron Beam-Induced Au Nanocrystal Growth Kinetics through Solution Chemistry,” Nano Letters (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”, Nature Materials Letters, Published Online 01/26/2015. | 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 |
| S. Kashyap, T.J. Woehl, X. Liu, S.K. Mallapragada, T. Prozorov. ”Nucleation of Iron Oxide Nanoparticles Mediated by Mms6 Protein In Situ“ ACS Nano (2014) In Print. | Abstract |
| L.R. Parent, D.B. Robinson, P.J. Cappillino, R.J. Hartnett, P. Abellan, J.E. Evans, N.D Browning, and I. Arslan. “In-Situ Observation of Directed Nanoparticle Aggregation During the Synthesis of Ordered Nanoporous Metal in Soft Templates,” Chemistry of Materials 26:3 (2014) pp. 1426‒1433 | Abstract |
| T.J. Woehl, C. Park, J.E. Evans, I. Arslan, W.D. Ristenpart, N.D. Browning. “Direct Observation of Aggregative Nanoparticle Growth: Kinetic Modeling of the Size Distribution and Growth Rate,” Nano Lett. 14 (2014) pp. 373‒378 | 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 |
| 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 |
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