In-situ heating-and-electron tomography for materials research: from 3D (In-situ 2D) to 4D (In-situ 3D)

Hata, Satoshi; Ihara, Shiro; Saito, Hikaru; Murayama, Mitsuhiro

doi:10.1093/jmicro/dfae008

Title: In-situ heating-and-electron tomography for materials research: from 3D (In-situ 2D) to 4D (In-situ 3D)

Journal Article · 28 February 2024 · Microscopy

DOI: https://doi.org/10.1093/jmicro/dfae008 · OSTI ID:2471589

^[1]; Ihara, Shiro ^[1]; Saito, Hikaru ^[1]; Murayama, Mitsuhiro ^[2]

Kyushu University, Fukuoka (Japan)
Kyushu University, Fukuoka (Japan); Virginia Polytechnic Institute and State University (Virginia Tech), Blacksburg, VA (United States); Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)

In-situ observation has expanded the application of transmission electron microscopy (TEM) and has made a significant contribution to materials research and development for energy, biomedical, quantum, etc. Recent technological developments related to in-situ TEM have empowered the incorporation of three-dimensional observation, which was previously considered incompatible. In this review article, we take up heating as the most commonly used external stimulus for in-situ TEM observation and overview recent in-situ TEM studies. Then, we focus on the electron tomography (ET) and in-situ heating combined observation by introducing the authors’ recent research as an example. Assuming that in-situ heating observation is expanded from two dimensions to three dimensions using a conventional TEM apparatus and a commercially available in-situ heating specimen holder, the following in-situ heating-and-ET observation procedure is proposed: (i) use a rapid heating-and-cooling function of a micro-electro-mechanical system holder; (ii) heat and cool the specimen intermittently and (iii) acquire a tilt-series dataset when the specimen heating is stopped. This procedure is not too technically challenging and can have a wide range of applications. Essential technical points for a successful 4D (space and time) observation will be discussed through reviewing the authors’ example application.

View Accepted Manuscript (DOE)

Cite

Export

Save

Research Organization:: Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)

Sponsoring Organization:: Japan Science and Technology Agency (JST) Core Research for Evolutional Science and Technology (CREST); Japan Society for the Promotion of Science (JSPS) KAKENHI; National Science Foundation (NSF); USDOE

Grant/Contract Number:: AC05-76RL01830

OSTI ID:: 2471589

Journal Information:: Microscopy, Journal Name: Microscopy Journal Issue: 2 Vol. 73; ISSN 2050-5698

Publisher:: Oxford University PressCopyright Statement

Country of Publication:: United States

Language:: English

References (68)

Direct In Situ TEM Visualization and Insight into the Facet‐Dependent Sintering Behaviors of Gold on TiO ₂ Yuan, Wentao; Zhang, Dawei; Ou, Yang Angewandte Chemie, Vol. 130, Issue 51 https://doi.org/10.1002/ange.201811933	journal	December 2018
A MEMS-based heating holder for the direct imaging of simultaneous in-situ heating and biasing experiments in scanning/transmission electron microscopes : MEMS-BASED HEATING HOLDER Mele, Luigi; Konings, Stan; Dona, Pleun Microscopy Research and Technique, Vol. 79, Issue 4 https://doi.org/10.1002/jemt.22623	journal	January 2016
Conductive Nanomaterials for Printed Electronics Kamyshny, Alexander; Magdassi, Shlomo Small, Vol. 10, Issue 17 https://doi.org/10.1002/smll.201303000	journal	January 2014
Iterative methods for the three-dimensional reconstruction of an object from projections Gilbert, Peter Journal of Theoretical Biology, Vol. 36, Issue 1 https://doi.org/10.1016/0022-5193(72)90180-4	journal	July 1972
Limitations to significant information in biological electron microscopy as a result of radiation damage Glaeser, Robert M. Journal of Ultrastructure Research, Vol. 36, Issue 3-4 https://doi.org/10.1016/S0022-5320(71)80118-1	journal	August 1971
Quasi-four-dimensional analysis of dislocation interactions with grain boundaries in 304 stainless steel Kacher, Josh; Robertson, I. M. Acta Materialia, Vol. 60, Issue 19 https://doi.org/10.1016/j.actamat.2012.08.036	journal	November 2012
In situ transmission electron microscopy and scanning transmission electron microscopy studies of sintering of Ag and Pt nanoparticles Asoro, M. A.; Ferreira, P. J.; Kovar, D. Acta Materialia, Vol. 81 https://doi.org/10.1016/j.actamat.2014.08.028	journal	December 2014
Secondary phases in AlxCoCrFeNi high-entropy alloys: An in-situ TEM heating study and thermodynamic appraisal Rao, J. C.; Diao, H. Y.; Ocelík, V. Acta Materialia, Vol. 131 https://doi.org/10.1016/j.actamat.2017.03.066	journal	June 2017
Interfacial kinetics in nanosized Au/Ge films: An in situ TEM study Kryshtal, Aleksandr P.; Minenkov, Alexey A.; Ferreira, Paulo J. Applied Surface Science, Vol. 409 https://doi.org/10.1016/j.apsusc.2017.03.037	journal	July 2017
A review on CT image noise and its denoising Diwakar, Manoj; Kumar, Manoj Biomedical Signal Processing and Control, Vol. 42 https://doi.org/10.1016/j.bspc.2018.01.010	journal	April 2018
In situ TEM observation of calcium silicate hydrate nanostructure at high temperatures Zheng, Qi; Jiang, Jinyang; Li, Xinle Cement and Concrete Research, Vol. 149 https://doi.org/10.1016/j.cemconres.2021.106579	journal	November 2021
Electron tomography: An imaging method for materials deformation dynamics Hata, S.; Honda, T.; Saito, H. Current Opinion in Solid State and Materials Science, Vol. 24, Issue 4 https://doi.org/10.1016/j.cossms.2020.100850	journal	August 2020
Fast electron tomography: Applications to beam sensitive samples and in situ TEM or operando environmental TEM studies Koneti, Siddardha; Roiban, Lucian; Dalmas, Florent Materials Characterization, Vol. 151 https://doi.org/10.1016/j.matchar.2019.02.009	journal	May 2019
Deep learning denoising of SEM images towards noise-reduced LER measurements Giannatou, E.; Papavieros, G.; Constantoudis, V. Microelectronic Engineering, Vol. 216 https://doi.org/10.1016/j.mee.2019.111051	journal	August 2019
Advances in windowed gas cells for in-situ TEM studies Wu, Fan; Yao, Nan Nano Energy, Vol. 13 https://doi.org/10.1016/j.nanoen.2015.03.015	journal	April 2015
An in-situ TEM microreactor for real-time nanomorphology & physicochemical parameters interrelated characterization Li, Wei; Li, Ming; Wang, Xueqing Nano Today, Vol. 35 https://doi.org/10.1016/j.nantod.2020.100932	journal	December 2020
Transmission electron microtomography without the “missing wedge” for quantitative structural analysis Kawase, Noboru; Kato, Mitsuro; Nishioka, Hideo Ultramicroscopy, Vol. 107, Issue 1 https://doi.org/10.1016/j.ultramic.2006.04.007	journal	January 2007
Advanced microheater for in situ transmission electron microscopy; enabling unexplored analytical studies and extreme spatial stability van Omme, J. Tijn; Zakhozheva, Marina; Spruit, Ronald G. Ultramicroscopy, Vol. 192 https://doi.org/10.1016/j.ultramic.2018.05.005	journal	September 2018
Novel MEMS-Based Gas-Cell/Heating Specimen Holder Provides Advanced Imaging Capabilities for In Situ Reaction Studies Allard, Lawrence F.; Overbury, Steven H.; Bigelow, Wilbur C. Microscopy and Microanalysis, Vol. 18, Issue 4 https://doi.org/10.1017/S1431927612001249	journal	July 2012
A (S)TEM Gas Cell Holder with Localized Laser Heating for In Situ Experiments Mehraeen, Shareghe; McKeown, Joseph T.; Deshmukh, Pushkarraj V. Microscopy and Microanalysis, Vol. 19, Issue 2 https://doi.org/10.1017/S1431927612014419	journal	March 2013
Fast Improvement of TEM Images with Low-Dose Electrons by Deep Learning Katsuno, Hiroyasu; Kimura, Yuki; Yamazaki, Tomoya Microscopy and Microanalysis, Vol. 28, Issue 1 https://doi.org/10.1017/S1431927621013799	journal	December 2021
Stability and Reactivity: Positive and Negative Aspects for Nanoparticle Processing Xu, Liang; Liang, Hai-Wei; Yang, Yuan Chemical Reviews, Vol. 118, Issue 7 https://doi.org/10.1021/acs.chemrev.7b00208	journal	February 2018
Fast Electron Tomography for Nanomaterials Albrecht, Wiebke; Bals, Sara The Journal of Physical Chemistry C, Vol. 124, Issue 50 https://doi.org/10.1021/acs.jpcc.0c08939	journal	November 2020
Graphene Microheater Chips for In Situ TEM Zhao, Jie; Liang, Liang; Tang, Shiyi Nano Letters, Vol. 23, Issue 2 https://doi.org/10.1021/acs.nanolett.2c03510	journal	December 2022
Operando Transmission Electron Microscopy: A Technique for Detection of Catalysis Using Electron Energy-Loss Spectroscopy in the Transmission Electron Microscope Chenna, Santhosh; Crozier, Peter A. ACS Catalysis, Vol. 2, Issue 11 https://doi.org/10.1021/cs3004853	journal	September 2012
Sintering of Passivated Gold Nanoparticles under the Electron Beam Chen, Yu; Palmer, Richard E.; Wilcoxon, Jess P. Langmuir, Vol. 22, Issue 6 https://doi.org/10.1021/la0533157	journal	March 2006
Ambient Aqueous-Phase Synthesis of Copper Nanoparticles and Nanopastes with Low-Temperature Sintering and Ultra-High Bonding Abilities Kamikoriyama, Yoichi; Imamura, Hiroshi; Muramatsu, Atsushi Scientific Reports, Vol. 9, Issue 1 https://doi.org/10.1038/s41598-018-38422-5	journal	January 2019
A mild aqueous synthesis of ligand-free copper nanoparticles for low temperature sintering nanopastes with nickel salt assistance Imamura, Hiroshi; Kamikoriyama, Yoichi; Muramatsu, Atsushi Scientific Reports, Vol. 11, Issue 1 https://doi.org/10.1038/s41598-021-03707-9	journal	December 2021
Five-second STEM dislocation tomography for 300 nm thick specimen assisted by deep-learning-based noise filtering Zhao, Yifang; Koike, Suguru; Nakama, Rikuto Scientific Reports, Vol. 11, Issue 1 https://doi.org/10.1038/s41598-021-99914-5	journal	October 2021
Deep learning-based noise filtering toward millisecond order imaging by using scanning transmission electron microscopy Ihara, Shiro; Saito, Hikaru; Yoshinaga, Mizumo Scientific Reports, Vol. 12, Issue 1 https://doi.org/10.1038/s41598-022-17360-3	journal	August 2022
Direct visualization of out-of-equilibrium structural transformations in atomically thin chalcogenides Kumar, Pawan; Horwath, James P.; Foucher, Alexandre C. npj 2D Materials and Applications, Vol. 4, Issue 1 https://doi.org/10.1038/s41699-020-0150-2	journal	June 2020
Rapid low dose electron tomography using a direct electron detection camera Migunov, Vadim; Ryll, Henning; Zhuge, Xiaodong Scientific Reports, Vol. 5, Issue 1 https://doi.org/10.1038/srep14516	journal	October 2015
In situ electron tomography for the thermally activated solid reaction of anaerobic nanoparticles Ihara, Shiro; Yoshinaga, Mizumo; Miyazaki, Hiroya Nanoscale, Vol. 15, Issue 23 https://doi.org/10.1039/D3NR00992K	journal	January 2023
Printed electronics: the challenges involved in printing devices, interconnects, and contacts based on inorganic materials Perelaer, Jolke; Smith, Patrick J.; Mager, Dario Journal of Materials Chemistry, Vol. 20, Issue 39 https://doi.org/10.1039/c0jm00264j	journal	January 2010
Study of the Initial Stages of Sintering Solids by Viscous Flow, Evaporation‐Condensation, and Self‐Diffusion Kingery, W. D.; Berg, M. Journal of Applied Physics, Vol. 26, Issue 10 https://doi.org/10.1063/1.1721874	journal	October 1955
LXVIII. Direct observations of the arrangement and motion of dislocations in aluminium Hirsch, P. B.; Horne, R. W.; Whelan, M. J. Philosophical Magazine, Vol. 1, Issue 7 https://doi.org/10.1080/14786435608244003	journal	July 1956
Coalescence and sintering of Pt nanoparticles: in situ observation by aberration-corrected HAADF STEM Asoro, M. A.; Kovar, D.; Shao-Horn, Y. Nanotechnology, Vol. 21, Issue 2 https://doi.org/10.1088/0957-4484/21/2/025701	journal	December 2009
Three-dimensional electron tomography and recent expansion of its applications in materials science Baba, Norio; Hata, Satoshi; Saito, Hikaru Microscopy, Vol. 72, Issue 2 https://doi.org/10.1093/jmicro/dfac071	journal	December 2022
Development of temporal series 4D-STEM and application to relaxation time measurement Nakazawa, Katsuaki; Mitsuishi, Kazutaka Microscopy, Vol. 72, Issue 5 https://doi.org/10.1093/jmicro/dfad006	journal	January 2023
Development of a technique for high resolution electron microscopic observation of nano-materials at elevated temperatures Kamino, T. Journal of Electron Microscopy, Vol. 54, Issue 6 https://doi.org/10.1093/jmicro/dfi072	journal	December 2005
An in situ heating TEM analysis method for an interface reaction Tanigaki, T.; Ito, K.; Nagakubo, Y. Journal of Electron Microscopy, Vol. 58, Issue 5 https://doi.org/10.1093/jmicro/dfp020	journal	April 2009
Development of an analytical environmental TEM system and its application Kishita, K.; Sakai, H.; Tanaka, H. Journal of Electron Microscopy, Vol. 58, Issue 6 https://doi.org/10.1093/jmicro/dfp028	journal	June 2009
In-situ TEM studies of the sintering behavior of copper nanoparticles covered by biopolymer nanoskin Ida, K.; Sugiyama, Y.; Chujyo, Y. Journal of Electron Microscopy, Vol. 59, Issue S1 https://doi.org/10.1093/jmicro/dfq055	journal	June 2010
Development of an environmental high-voltage electron microscope for reaction science Tanaka, Nobuo; Usukura, Jiro; Kusunoki, Michiko Microscopy, Vol. 62, Issue 1 https://doi.org/10.1093/jmicro/dfs095	journal	January 2013
Atomic-resolution environmental TEM for quantitative in-situ microscopy in materials science Takeda, Seiji; Yoshida, Hideto Microscopy, Vol. 62, Issue 1 https://doi.org/10.1093/jmicro/dfs096	journal	January 2013
B11-P-14ISER, a new, compressed sensing based reconstruction algorithm for reducing image acquisition time Kamo, Katsumi; Horii, Noritaka; Furukawa, Hiromitsu Microscopy, Vol. 64, Issue suppl 1 https://doi.org/10.1093/jmicro/dfv218	journal	November 2015
Design of a 300-kV gas environmental transmission electron microscope equipped with a cold field emission gun Isakozawa, Shigeto; Nagaoki, Isao; Watabe, Akira Microscopy, Vol. 65, Issue 4 https://doi.org/10.1093/jmicro/dfw015	journal	May 2016
Thermal stability of laser-induced modified volumes in Si as studied by in situ and ex situ heating experiments Saka, Hiroyasu; Iwata, Hiroyuki; Kawaguchi, Daisuke Microscopy, Vol. 67, Issue 2 https://doi.org/10.1093/jmicro/dfy008	journal	February 2018
In situ transmission electron microscopic observations of redox cycling of a Ni–ScSZ cermet fuel cell anode Matsuda, Junko; Kawasaki, Tatsuya; Futamura, Shotaro Microscopy, Vol. 67, Issue 5 https://doi.org/10.1093/jmicro/dfy025	journal	May 2018
Evaluation of spatial and temporal resolution on in situ annealing aberration-corrected transmission electron microscopy with proportional–integral–differential controller Shimada, Yusuke; Yoshida, Kenta; Inoue, Koji Microscopy, Vol. 68, Issue 3 https://doi.org/10.1093/jmicro/dfz010	journal	March 2019
High-resolution in-situ transmission electron microscopy observation of a solid-liquid interface in the Al-Si system Arai, S.; Tsukimoto, S.; Miyai, H. Journal of Electron Microscopy, Vol. 48, Issue 4 https://doi.org/10.1093/oxfordjournals.jmicro.a023683	journal	January 1999
Analysis of Ni nanoparticle gas phase sintering Tsyganov, Sergej; Kästner, Jochen; Rellinghaus, Bernd Physical Review B, Vol. 75, Issue 4, Article No. 045421 https://doi.org/10.1103/PhysRevB.75.045421	journal	January 2007
In situ Transmission-Electron-Microscopy Investigation of Melting in Submicron Al-Si Alloy Particles under Electron-Beam Irradiation Yokota, Takeshi; Murayama, M.; Howe, J. M. Physical Review Letters, Vol. 91, Issue 26 https://doi.org/10.1103/PhysRevLett.91.265504	journal	December 2003
Parametric estimate of intensity inhomogeneities applied to MRI Styner, M.; Brechbuhler, C.; Szckely, G. IEEE Transactions on Medical Imaging, Vol. 19, Issue 3 https://doi.org/10.1109/42.845174	journal	March 2000
A Review on Development and Optimization of Microheaters for High-Temperature In Situ Studies Spruit, Ronald G.; van Omme, J. Tijn; Ghatkesar, Murali K. Journal of Microelectromechanical Systems, Vol. 26, Issue 6 https://doi.org/10.1109/JMEMS.2017.2757402	journal	December 2017
Technologies for Printing Sensors and Electronics Over Large Flexible Substrates: A Review Khan, Saleem; Lorenzelli, Leandro; Dahiya, Ravinder S. IEEE Sensors Journal, Vol. 15, Issue 6 https://doi.org/10.1109/JSEN.2014.2375203	journal	June 2015
Image Denoising by Sparse 3-D Transform-Domain Collaborative Filtering Dabov, Kostadin; Foi, Alessandro; Katkovnik, Vladimir IEEE Transactions on Image Processing, Vol. 16, Issue 8 https://doi.org/10.1109/TIP.2007.901238	journal	August 2007
Collaborative Filtering of Correlated Noise: Exact Transform-Domain Variance for Improved Shrinkage and Patch Matching Makinen, Ymir; Azzari, Lucio; Foi, Alessandro IEEE Transactions on Image Processing, Vol. 29 https://doi.org/10.1109/TIP.2020.3014721	journal	January 2020
A Threshold Selection Method from Gray-Level Histograms Otsu, Nobuyuki IEEE Transactions on Systems, Man, and Cybernetics, Vol. 9, Issue 1 https://doi.org/10.1109/TSMC.1979.4310076	journal	January 1979
Imaging of Transient Structures Using Nanosecond in Situ TEM Kim, Judy S.; LaGrange, Thomas; Reed, Bryan W. Science, Vol. 321, Issue 5895 https://doi.org/10.1126/science.1161517	journal	September 2008
In Situ TEM Observation of a Microcrucible Mechanism of Nanowire Growth Boston, R.; Schnepp, Z.; Nemoto, Y. Science, Vol. 344, Issue 6184 https://doi.org/10.1126/science.1251594	journal	May 2014
A Review of Image Denoising Algorithms, with a New One Buades, A.; Coll, B.; Morel, J. M. Multiscale Modeling & Simulation, Vol. 4, Issue 2 https://doi.org/10.1137/040616024	journal	January 2005
Study of Thin Crystalline Films by Universal Electron Diffraction Microscope Hashimoto, Hatsujiro Journal of the Physical Society of Japan, Vol. 9, Issue 2 https://doi.org/10.1143/JPSJ.9.150	journal	March 1954
Electron Microscopy of Biological Materials at the Nanometer Scale Kourkoutis, Lena Fitting; Plitzko, Jürgen M.; Baumeister, Wolfgang Annual Review of Materials Research, Vol. 42, Issue 1 https://doi.org/10.1146/annurev-matsci-070511-155004	journal	August 2012
Brief review of image denoising techniques Fan, Linwei; Zhang, Fan; Fan, Hui Visual Computing for Industry, Biomedicine, and Art, Vol. 2, Issue 1 https://doi.org/10.1186/s42492-019-0016-7	journal	July 2019
In Situ Heating Transmission Electron Microscopy Saka, Hiroyasu; Kamino, Takeo; Ara, Shigeo MRS Bulletin, Vol. 33, Issue 2 https://doi.org/10.1557/mrs2008.21	journal	February 2008
Direct Atomic-scale Observation Using Electron Diffraction Microscopy Hashimoto, Hatsujiro Journal of the Surface Finishing Society of Japan, Vol. 59, Issue 12 https://doi.org/10.4139/sfj.59.768	journal	January 2008
4D electron tomography of dislocations undergoing electron irradiation Mussi, Alexandre; Carrez, Philippe; Gouriet, Karine Comptes Rendus. Physique, Vol. 22, Issue S3 https://doi.org/10.5802/crphys.80	journal	December 2021

Similar Records

In-situ TEM Holder for Ultrafast, Multimodal Imaging

Technical Report · 2024 · OSTI ID:2435631

Grigoropoulos, Costas; Blankenship, Brian

In-situ nanoindentation specimen holder for a high-voltage transmission electron microscope

Conference · 1998 · OSTI ID:7726

Dahmen, ; U, ; Wall, M A

Dynamic observation of electrochemical etching in silicon

Technical Report · 1995 · OSTI ID:71306

Ross, F M; Searson, P C

Related Subjects

36 MATERIALS SCIENCE
3D
4D
Microscopy
heating
in-situ electron tomography
nanoparticle
sintering

Title: In-situ heating-and-electron tomography for materials research: from 3D (In-situ 2D) to 4D (In-situ 3D)

Citation Formats

References (68)

Similar Records

Related Subjects