2D Materials
| Biasing Manipulator TEM | Heating + Biasing TEM | Biasing TEM | Cryo-Biasing TEM | ||
| Stimuli |
Electrical |  |
|
|
|
| Thermal |  |
|
|
|
|
| Mechanical | |
 |
|
|
|
| Cryogenic | |
|
|
|
|
| Imaging | Higher resolution and diffraction | |
|
|
|
| EDS/EELS compatibility | |
|
|
|
|
| In-situ imaging | |
|
|
|
|
| Pre- and post-mortem analysis | |
|
|
|
|
| Sample Type |
Standard grid | |
|
|
|
| FIB lift-out | |
|
|
|
|
| MEMS chip | |
|
|
|
|
Excellent Good N/A
TEM Sample Holders for 2D Materials Research
 |
Biasing Manipulator HolderSee MoreOn-site electrical contacts with mobile probe |
 |
MEMS Biasing + Heating HolderSee MoreHigh temperature transport measurements—phase changes |
 |
Biasing HolderSee MoreWire-bonded samples to investigate functional electrical devices |
 |
Cryo-Biasing Holder See MoreElectrical biasing of cryo-cooled samples |
Edit
2D Materials Electrochemistry
Hummingbird Scientific’s in-situ electrical biasing holder can be used for electrochemically cycling thin film batteries while imaging the material microstructure. Representative battery cell can be thinned using FIB processing or attached to the substrate. The sample is a representative section of the real battery cell and the data obtained is representative of the real battery performance.
For example, a thin cross-section of a battery cell can be mounted, wire-bonded, and viewed in TEM while cycling. The image shown on the left is a 10 nm graphite flake folded onto itself after one complete intercalation/deintercalation cycle.
Reference: Edward R. White, Jared J. Lodico & B. C. Regan. “Intercalation events visualized in single microcrystals of graphite,” Nature Communications (2017).
Image (left) © 2017 Macmillan Publishers Limited, part of Springer Nature
Image (bottom right) © Materials Research Society 2010
2D Materials-Based Devices
Two-dimensional materials-based electronic devices are particularly well suited for in-situ microscopy studies. Is relatively easy to contact continuous films and large crystals of 2D materials with Hummingbird Scientific’s biasing platforms. The example shown here illustrates that 2D materials-based devices suited for TEM studies can also be studied with other characterization techniques, in a correlative manner. Dr. Marija Drndić’s group at the University of Pennsylvania developed a process to study the effects of electron beam irradiation on one-atom-thick MoS2 crystals by combining in-situ TEM and ex-situ Raman spectroscopy data—from the same sample.
Reference: William M. Parkin et al. Raman Shifts in Electron-Irradiated Monolayer MoS2. ACS Nano (2016).
Image © 2014 American Chemical Society
Edit
2D Materials at High Temperature
Hummingbird Scientific’s heating platforms allow researchers to heat 2D materials and—with some options—simultaneously apply voltages to the sample under observation. This example shows the segregation of MoS2 layers at high temperature. Researches at the University of Pennsylvania transformed few-layers of MoS2 with residual polymers from the transfer process into a 2D material with well segregated areas formed of either pure MoS2 or carbon based-composites. The segregation happens at temperature > 1000 °C. Energy-dispersive X-ray spectroscopy (EDS) confirmed the chemical content of each segregated area.
Data provided by Dr. Deep Jariwala and Dr. Eric Stach from the the University of Pennsylvania.
Edit
Biasing 2D Materials’ Edges
Hummingbird Scientific’s biasing-manipulator TEM holder’s movable biasing probe can be use to electrically contact 2D materials’ edges at specific locations with high spatial resolution. In this way, potential differences and electrical currents can be induced in the material locally. This examples shows a TEM image of contact between a metal probe of the biasing-manipulator TEM holder and the edge of a few-layers graphene sample.
Image courtesy of Dr. Yan Cheng from the Shanghai Institute of Microsystem and Information Technology.
EditTransport in Graphene Nanoribbons
In an electron microscope the electron beam’s main function is to act as an illumination source. However, in the right energy range the electron beam can displace atoms from a material. Marija Drndić’s group at the University of Pennsylvania developed a process to modify graphene sheets into graphene nanoribbons with the aid of a TEM’s electron beam. By having these modifications done in a Hummingbird Scientific in situ TEM biasing sample holder, the researchers were able to 1) fabricate graphene-based devices inside the TEM column and 2) characterize the devices electronically without the need to remove the sample from the microscope. This technique is well suited for any 2D material.
Reference: Marija Drndić et al. In Situ Transmission Electron Microscopy Modulation of Transport in Graphene Nanoribbons. ACS Nano (2016).
Edit
Image copyright © 2016 American Chemical Society Phase transformation of 2D transition metal (TM) dichalcogenides during the in-situ high-temperature heating
Two-dimensional (2D) TM dichalcogenides demonstrate exceptional electronic and optical properties. A previous study by researchers from the University of Pennsylvania on a few layers of 2D MoS2 has shown multiple phases with atoms occupying orientations within single/multiple layers (see npj 2D Materials and Applications here).
Here, the same group study different thin 2D dichalcogenide material and observe a unique conversion of phases from the parent crystalline substrate. The conversion is initiated when the temperature of the sample reaches around 500°C. The diffusion velocity of the new phase is dependent upon the stimulus applied to the sample.
Data provided by Pawan Kumar, Eric Stach and Deep Jariwala from the University of Pennsylvania.
Edit
| Gaurav Modi, Andrew C. Meng, Srinivasan Rajagopalan, Rangarajan Thiruvengadam, Peter K. Davies, Eric A. Stach, and Ritesh Agarwal. “Controlled self-assembly of nanoscale superstructures in phase-change Ge-Sb-Te nanowires” Nano Lett. (2024) | Abstract |
| M.J. Motala, X. Zhang, P. Kumar, E.F. Oliveira, A. Benton, P. Miesle, R. Rao, P.R. Stevenson, D. Moore, A. Alfieri, J. Lynch, D. Austin, S. Post, G. Gao, S. Ma, H. Zhu, Z. Wang, I. Petrov, E.A. Stach, W.J. Kennedy, S. Vangala, J.M. Tour, D.S. Galvao, D. Jariwala, C. Muratore, M. Snure, P.M. Ajayan, and N.R. Glavin. “Synthesis of two-dimensional van der waals superlattices, heterostructures, and alloys from conversion of sequentially layered sub-nanometer metal films,” Materials Today Nano (2023) | Abstract |
| Pawan Kumar, Andrew C. Meng, Kiyoung Jo, Eric A. Stach, and Deep Jariwala. “Interfacial Reaction and Diffusion at the One-Dimensional Interface of Two-Dimensional PtSe2,” Nano Letters (2022) | Abstract |
| Brian T. Zutter, Hyunseok Kim, William A. Hubbard, Dingkun Ren, Matthew Mecklenburg, Diana Huffaker, and B.C. Regan. “Mapping Charge Recombination and the Effect of Point-Defect Insertion in GaAs Nanowire Heterojunctions,” Physical Review Applied (2021) | Abstract |
| Pawan Kumar, James P. Horwath, Alexandre C. Foucher, Christopher C. Price, Natalia Acero, Vivek B. Shenoy, Eric A. Stach, and Deep Jariwala. “Direct visualization of out-of-equilibrium structural transformations in atomically thin chalcogenides,” npj 2D Materials and Applications (2020) | Abstract |
| Paul Masih Das and Marija Drndić, “In Situ 2D MoS2 Field-Effect Transistors with an Electron Beam Gate,” ACS Nano (2020) | Abstract |
| Pawan Kumar, James Horwath, Alexandre Foucher, Christopher Price, Natalia Acero, Vivek Shenoy, Deep Jariwala, Eric Stach, and Daan Hein Alsem. “Non-equilibrium Structural Phase Transformations in Atomically Thin Transition Metal Dichalcogenides,” Microscopy & Microanalysis (2020) | Abstract |
| William M. Parkin, Adrian Balan, Liangbo Liang, Paul Masih Das, Michael Lamparski, Carl H. Naylor, Julio A. Rodríguez-Manzo, A. T. Charlie Johnson, Vincent Meunier, and Marija Drndić. “Raman Shifts in Electron-Irradiated Monolayer MoS2,” ACS Nano (2016) |
Abstract |
| Julio A. Rodríguez-Manzo, Zhengqing John Qi, Alexander Crook, Jae-Hyuk Ahn, A. T. Charlie Johnson, and Marija Drndić. “In Situ Transmission Electron Microscopy Modulation of Transport in Graphene Nanoribbons,” ACS Nano (2016) | Abstract |
| Steffen Hartmann, Sascha Hermann, Jens Bonitz, Marc Heggen, Ole Hölck, Alexey Shaporin, Jan Mehner, Stefan E. Schulz, Thomas Gessner, and Bernhard Wunderle. “Towards nanoreliability of sensors incorporating interfaces between single-walled carbon nanotubes and metals: molecular dynamics simulations and in situ experiments using electron microscopy,” Mechatronics (2016) | Abstract |
| Julio A. Rodriguez-Manzo, Zhengqing John Qi, Matthew Puster, Adrian Balan, A. T. Charlie Johnson, and Marija Drndic. “Fabrication and Simultaneous Electrical Measurement of Graphene Nanoribbon Devices Inside a S/TEM,” Microscopy and Microanalysis (2015) |
Abstract |
| Matthew Puster, Julio A. Rodríguez-Manzo, Adrian Balan, and Marija Drndić. “Toward Sensitive Graphene Nanoribbon-Nanopore Devices by Preventing Electron Beam-Induced Damage,” ACS Nano (2013) | Abstract |
| Chong-Min Wang, Wu Xu, Jun Liu, Ji-Guang Zhang, Lax V. Saraf, Bruce W. Arey, Daiwon Choi, Zhen-Guo Yang, Jie Xiao, Suntharampillai Thevuthasan, Donald R. Baer. “In Situ Transmission Electron Microscopy Observation of Microstructure and Phase Evolution in a SnO2 Nanowire during Lithium Intercalation,” Nano Letters (2011) | Abstract |
| Seung Min Kim, Cary L. Pint, Placidus B. Amama, Robert H. Hauge, Benji Maruyama, and Eric A. Stach. “Catalyst and catalyst support morphology evolution in single-walled carbon nanotube supergrowth: Growth deceleration and termination,” Journal of Materials Research (2010) | Abstract |
| Avetik R. Harutyunyan, Gugang Chen, Tereza M. Paronyan, Elena Pigos, Oleg A. Kuznetsov, Kapila Hewaparakrama, Seung Min Kim, Dmitri Zakharov, Eric A. Stach, and Gamini U. Sumanasekera. “Preferential Growth of Single-Walled Carbon Nanotubes with Metallic Conductivity,” Science (2009) | Abstract |
| Stefan Meister, David T. Schoen, Mark A. Topinka, Andrew M. Minor, and Yi Cui. “Void Formation Induced Electrical Switching in Phase-Change Nanowires,” Nano Letters (2008) | Abstract |
| Hailin Peng, Chong Xie, David T. Schoen, and Yi Cui. “Large Anisotropy of Electrical Properties in Layer-Structured In2Se3 Nanowires,” Nano Letters (2008) | Abstract |
Read More