Comptes Rendus
no. 2-3
Electron microscopy / Microscopie électronique
In situ mechanical TEM: Seeing and measuring under stress with electrons
[Voir et mesurer sous contrainte mécanique avec des électrons : La microscopie électronique à transmission (MET) in situ]
Marc Legros1
1 CEMES–CNRS, 29, rue Jeanne-Marvig, 31055 Toulouse, France
Comptes Rendus. Physique, Seeing and measuring with electrons: Transmission Electron Microscopy today and tomorrow, Volume 15 (2014) no. 2-3, pp. 224-240.

From the first observation of moving dislocations in 1956 to the latest developments of piezo-actuated sample holders and direct electron sensing cameras in modern transmission electron microscopes (TEM), in situ mechanical testing has brought an unequaled view of the involved mechanisms during the plastic deformation of materials. Although MEMS-based or load-cell equipped holders provide an almost direct measure of these quantities, deriving stress and strain from in situ TEM experiments has an extensive history. Nowadays, the realization of a complete mechanical test while observing the evolution of a dislocation structure is possible, and it constitutes the perfect combination to explore size effects in plasticity. New cameras, data acquisition rates and intrinsic image-related techniques, such as holography, should extend the efficiency and capabilities of in situ deformation inside a TEM.

Des premières observations du mouvement de dislocations en 1956 jusqu'aux derniers développements de porte-objets à commandes piézo-électriques et de caméras à détection d'électrons dans les microscopes électroniques à transmission (MET) modernes, les essais mécaniques in situ ont toujours permis une observation inégalée des mécanismes impliqués dans la déformation plastique. Bien que les porte-objets équipés d'une cellule de charge ou de MEMS offrent une visualisation presque directe de ces effets, l'élaboration des étapes nécessaires pour mesurer les relations entre contrainte et déformation à partir d'expériences réalisées in situ dans un MET a une longue histoire. Aujourd'hui, la réalisation d'un essai mécanique complet tout en observant l'évolution d'une structure de dislocations est possible ; ceci constitue la combinaison parfaite pour explorer les effets de taille dans la plasticité. Les nouvelles techniques intrinsèques d'imagerie (comme l'holographie en champ sombre) et l'accès à de nouveaux outils d'acquisition d'images (nouvelles caméras, taux d'acquisition rapides) vont étendre l'efficacité et les capacités de mesures sans entraver l'observation des mécanismes.

Publié le :
DOI : 10.1016/j.crhy.2014.02.002
Keywords: In situ TEM, Plastic deformation, Dislocation structure and dynamics
Mots-clés : Microscopie MET in situ, Déformation plastique, Structure et dynamique des dislocations

Marc Legros 1

1 CEMES–CNRS, 29, rue Jeanne-Marvig, 31055 Toulouse, France 
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Marc Legros. In situ mechanical TEM: Seeing and measuring under stress with electrons. Comptes Rendus. Physique, Seeing and measuring with electrons: Transmission Electron Microscopy today and tomorrow, Volume 15 (2014) no. 2-3, pp. 224-240. doi : 10.1016/j.crhy.2014.02.002. https://comptes-rendus.academie-sciences.fr/physique/articles/10.1016/j.crhy.2014.02.002/

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  • David Rodney; Pierre-Antoine Geslin; Sylvain Patinet; Vincent Démery; Alberto Rosso Does the Larkin length exist?, Modelling and Simulation in Materials Science and Engineering, Volume 32 (2024) no. 3, p. 035007 | DOI:10.1088/1361-651x/ad2543
  • Marc Legros; Frédéric Mompiou; Daniel Caillard Observing deformation in situ, Nature Materials, Volume 23 (2024) no. 1, p. 20 | DOI:10.1038/s41563-023-01739-2
  • Ying Han; Liqiang Wang; Ke Cao; Jingzhuo Zhou; Yingxin Zhu; Yuan Hou; Yang Lu In Situ TEM Characterization and Modulation for Phase Engineering of Nanomaterials, Chemical Reviews, Volume 123 (2023) no. 24, p. 14119 | DOI:10.1021/acs.chemrev.3c00510
  • Dominik Steinberger; Inas Issa; Rachel Strobl; Peter J. Imrich; Daniel Kiener; Stefan Sandfeld Data-mining of in-situ TEM experiments: Towards understanding nanoscale fracture, Computational Materials Science, Volume 216 (2023), p. 111830 | DOI:10.1016/j.commatsci.2022.111830
  • Mitsuhiro Murayama; Joshua Stuckner In situ electron microscopy: modalities of dynamic measurements to capture fundamental physical or chemical processes down to the atomic scale, Dynamic Processes in Solids (2023), p. 265 | DOI:10.1016/b978-0-12-818876-7.00007-6
  • Keqiang Li; Yeqiang Bu; Hongtao Wang Advances on in situ TEM mechanical testing techniques: a retrospective and perspective view, Frontiers in Materials, Volume 10 (2023) | DOI:10.3389/fmats.2023.1207024
  • Li Zhong; Lihua Wang; Jiangwei Wang; Yang He; Xiaodong Han; Zhiwei Shan; Xiuliang Ma In-Situ Nanomechanical TEM, In-Situ Transmission Electron Microscopy (2023), p. 53 | DOI:10.1007/978-981-19-6845-7_3
  • Runhao Han; Peizhen Hong; Shuai Ning; Qiang Xu; Mingkai Bai; Jing Zhou; Kaiyi Li; Fei Liu; Feng Shi; Feng Luo; Zongliang Huo The effect of stress on HfO2-based ferroelectric thin films: A review of recent advances, Journal of Applied Physics, Volume 133 (2023) no. 24, p. 240702 | DOI:10.1063/5.0146998
  • Jiabao Zhang; Xudong Yang; Zhipeng Li; Jixiang Cai; Jianfei Zhang; Xiaodong Han Novel Method for Image-Based Quantified In Situ Transmission Electron Microscope Nanoindentation with High Spatial and Temporal Resolutions, Micromachines, Volume 14 (2023) no. 9, p. 1708 | DOI:10.3390/mi14091708
  • Matteo Erbì; Hakim Amara; Riccardo Gatti Tuning Elastic Properties of Metallic Nanoparticles by Shape Controlling: From Atomistic to Continuous Models, Small, Volume 19 (2023) no. 47 | DOI:10.1002/smll.202302116
  • Zhongtao Ma; Waynah Lou Dacayan; Christodoulos Chatzichristodoulou; Kristian Speranza Mølhave; Francesco Maria Chiabrera; Wenjing Zhang; Søren Bredmose Simonsen Electrochemical Impedance Spectroscopy Integrated with Environmental Transmission Electron Microscopy, Small Methods, Volume 7 (2023) no. 7 | DOI:10.1002/smtd.202201713
  • Sandra Stangebye; Xing Liu; Lina Daza Llanos; Yichen Yang; Ting Zhu; Josh Kacher; Olivier Pierron Comparison of electrical sensing and image analysis for in situ transmission electron microscopy nanomechanical testing of thin films, Thin Solid Films, Volume 787 (2023), p. 140125 | DOI:10.1016/j.tsf.2023.140125
  • K. A. Mushankova; L. V. Stepanova Experience in modeling inclined cracks in materials with cubic crystal structure, Vestnik of Samara University. Natural Science Series, Volume 29 (2023) no. 4, p. 106 | DOI:10.18287/2541-7525-2023-29-4-106-116
  • Y. Cui; H.B. Chew Machine-Learning Prediction of Atomistic Stress along Grain Boundaries, Acta Materialia, Volume 222 (2022), p. 117387 | DOI:10.1016/j.actamat.2021.117387
  • Mohamed Amer; Qamar Hayat; Vit Janik; Nigel Jennett; Jon Nottingham; Mingwen Bai A Review on In Situ Mechanical Testing of Coatings, Coatings, Volume 12 (2022) no. 3, p. 299 | DOI:10.3390/coatings12030299
  • Shuang Li; Cynthia A. Powell; Suveen Mathaudhu; Bharat Gwalani; Arun Devaraj; Chongmin Wang Review of recent progress on in situ TEM shear deformation: a retrospective and perspective view, Journal of Materials Science, Volume 57 (2022) no. 26, p. 12177 | DOI:10.1007/s10853-022-07331-4
  • Christoph Gammer; Dayong An Conditions near a crack tip: Advanced experiments for dislocation analysis and local strain measurement, MRS Bulletin, Volume 47 (2022) no. 8, p. 808 | DOI:10.1557/s43577-022-00377-4
  • Shuang Li; Lei Li; Ayoub Soulami; Cynthia A. Powell; Suveen Mathaudhu; Arun Devaraj; Chongmin Wang In-situ observation of deformation twin associated sub-grain boundary formation in copper single crystal under bending, Materials Research Letters, Volume 10 (2022) no. 7, p. 488 | DOI:10.1080/21663831.2022.2057201
  • Thomas E. J. Edwards; Xavier Maeder; Johannes Ast; Luisa Berger; Johann Michler Mapping pure plastic strains against locally applied stress: Revealing toughening plasticity, Science Advances, Volume 8 (2022) no. 30 | DOI:10.1126/sciadv.abo5735
  • Nargisse Khiara; Fabien Onimus; Stéphanie Jublot-Leclerc; Thomas Jourdan; Thomas Pardoen; Jean-Pierre Raskin; Yves Bréchet In-situ TEM irradiation creep experiment revealing radiation induced dislocation glide in pure copper, Acta Materialia, Volume 216 (2021), p. 117096 | DOI:10.1016/j.actamat.2021.117096
  • Xin Yang; Chen Luo; Xiyue Tian; Fang Liang; Yin Xia; Xinqian Chen; Chaolun Wang; Steve Xin Liang; Xing Wu; Junhao Chu A revew of in situ transmission electron microscopy study on the switching mechanism and packaging reliability in non-volatile memory, Journal of Semiconductors, Volume 42 (2021) no. 1, p. 013102 | DOI:10.1088/1674-4926/42/1/013102
  • Meriem Ben Haj Slama; Vincent Taupin; Nabila Maloufi; Kaustubh Venkatraman; Anthony D. Rollett; Ricardo A. Lebensohn; Stéphane Berbenni; Benoît Beausir; Antoine Guitton Electron channeling contrast imaging characterization and crystal plasticity modelling of dislocation activity in Ti21S BCC material, Materialia, Volume 15 (2021), p. 100996 | DOI:10.1016/j.mtla.2020.100996
  • Juan A. de la Rosa Abad; Alejandra Londoño-Calderon; Eduardo M. Bringa; German J. Soldano; Sergio. A. Paz; Ulises Santiago; Sergio J. Mejía-Rosales; Miguel José Yacamán; Marcelo M. Mariscal Soft or Hard? Investigating the Deformation Mechanisms of Au–Pd and Pd Nanocubes under Compression: An Experimental and Molecular Dynamics Study, The Journal of Physical Chemistry C, Volume 125 (2021) no. 45, p. 25298 | DOI:10.1021/acs.jpcc.1c07685
  • Rituja B. Patil; Stephen D. House; Aayush Mantri; Judith C. Yang; James R. McKone Direct Observation of Ni–Mo Bimetallic Catalyst Formation via Thermal Reduction of Nickel Molybdate Nanorods, ACS Catalysis, Volume 10 (2020) no. 18, p. 10390 | DOI:10.1021/acscatal.0c02264
  • Pranjal Nautiyal; Benjamin Boesl; Arvind Agarwal In-Situ Mechanics: Introduction and Importance, In-situ Mechanics of Materials (2020), p. 1 | DOI:10.1007/978-3-030-43320-8_1
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  • T. Voisin; M.D. Grapes; T.T. Li; M.K. Santala; Y. Zhang; J.P. Ligda; N.J. Lorenzo; B.E. Schuster; G.H. Campbell; T.P. Weihs In situ TEM observations of high-strain-rate deformation and fracture in pure copper, Materials Today, Volume 33 (2020), p. 10 | DOI:10.1016/j.mattod.2019.11.001
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  • Josh Kacher; Ting Zhu; Olivier Pierron; Douglas E. Spearot Integrating in situ TEM experiments and atomistic simulations for defect mechanics, Current Opinion in Solid State and Materials Science, Volume 23 (2019) no. 3, p. 117 | DOI:10.1016/j.cossms.2019.03.003
  • Dalong Zhang; Lin Jiang; Xin Wang; Irene J. Beyerlein; Andrew M. Minor; Julie M. Schoenung; Subhash Mahajan; Enrique J. Lavernia Revealing deformation mechanisms in Mg–Y alloy by in situ deformation of nano-pillars with mediated lateral stiffness, Journal of Materials Research, Volume 34 (2019) no. 9, p. 1542 | DOI:10.1557/jmr.2019.124
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  • Sanjit Bhowmick; Horacio Espinosa; Katherine Jungjohann; Thomas Pardoen; Olivier Pierron Advanced microelectromechanical systems-based nanomechanical testing: Beyond stress and strain measurements, MRS Bulletin, Volume 44 (2019) no. 06, p. 487 | DOI:10.1557/mrs.2019.123
  • Cesar A. Sciammarella; Federico M. Sciammarella; Luciano Lamberti Determination of Displacement Fields at the Sub-Nanometric Scale, Materials, Volume 12 (2019) no. 11, p. 1804 | DOI:10.3390/ma12111804
  • Meriem Ben Haj Slama; Nabila Maloufi; Julien Guyon; Slim Bahi; Laurent Weiss; Antoine Guitton In Situ Macroscopic Tensile Testing in SEM and Electron Channeling Contrast Imaging: Pencil Glide Evidenced in a Bulk β-Ti21S Polycrystal, Materials, Volume 12 (2019) no. 15, p. 2479 | DOI:10.3390/ma12152479
  • K.H. Yano; S. Thomas; M.J. Swenson; Y. Lu; J.P. Wharry TEM in situ cube-corner indentation analysis using ViBe motion detection algorithm, Journal of Nuclear Materials, Volume 502 (2018), p. 201 | DOI:10.1016/j.jnucmat.2018.02.003
  • Giulio Guzzinati; Thomas Altantzis; Maria Batuk; Annick De Backer; Gunnar Lumbeeck; Vahid Samaee; Dmitry Batuk; Hosni Idrissi; Joke Hadermann; Sandra Van Aert; Dominique Schryvers; Johan Verbeeck; Sara Bals Recent Advances in Transmission Electron Microscopy for Materials Science at the EMAT Lab of the University of Antwerp, Materials, Volume 11 (2018) no. 8, p. 1304 | DOI:10.3390/ma11081304
  • Vahid Samaee; Riccardo Gatti; Benoit Devincre; Thomas Pardoen; Dominique Schryvers; Hosni Idrissi Dislocation driven nanosample plasticity: new insights from quantitative in-situ TEM tensile testing, Scientific Reports, Volume 8 (2018) no. 1 | DOI:10.1038/s41598-018-30639-8
  • Thomas Voisin; Michael D. Grapes; Yong Zhang; Nicholas J. Lorenzo; Jonathan P. Ligda; Brian E. Schuster; Melissa K. Santala; Tian Li; Geoffrey H. Campbell; Timothy P. Weihs DTEM In Situ Mechanical Testing: Defects Motion at High Strain Rates, Dynamic Behavior of Materials, Volume 1 (2017), p. 209 | DOI:10.1007/978-3-319-41132-3_29
  • M. Seita; J. P. Hanson; S. Gradečak; M. J. Demkowicz Probabilistic failure criteria for individual microstructural elements: an application to hydrogen-assisted crack initiation in alloy 725, Journal of Materials Science, Volume 52 (2017) no. 5, p. 2763 | DOI:10.1007/s10853-016-0568-2
  • Saurabh Gupta; Olivier N. Pierron A MEMS Tensile Testing Technique for Measuring True Activation Volume and Effective Stress in Nanocrystalline Ultrathin Microbeams, Journal of Microelectromechanical Systems, Volume 26 (2017) no. 5, p. 1082 | DOI:10.1109/jmems.2017.2708522
  • K.H. Yano; M.J. Swenson; Y. Wu; J.P. Wharry TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy, Journal of Nuclear Materials, Volume 483 (2017), p. 107 | DOI:10.1016/j.jnucmat.2016.10.049
  • L. Rigutti; L. Venturi; J. Houard; A. Normand; E. P. Silaeva; M. Borz; S. A. Malykhin; A. N. Obraztsov; A. Vella Optical Contactless Measurement of Electric Field-Induced Tensile Stress in Diamond Nanoscale Needles, Nano Letters, Volume 17 (2017) no. 12, p. 7401 | DOI:10.1021/acs.nanolett.7b03222
  • Thomas Voisin; Michael D. Grapes; Yong Zhang; Nicholas Lorenzo; Jonathan Ligda; Brian Schuster; Timothy P. Weihs TEM sample preparation by femtosecond laser machining and ion milling for high-rate TEM straining experiments, Ultramicroscopy, Volume 175 (2017), p. 1 | DOI:10.1016/j.ultramic.2016.12.001
  • N. Wieczorek; G. Laplanche; J.-K. Heyer; A.B. Parsa; J. Pfetzing-Micklich; G. Eggeler Assessment of strain hardening in copper single crystals using in situ SEM microshear experiments, Acta Materialia, Volume 113 (2016), p. 320 | DOI:10.1016/j.actamat.2016.04.055
  • Tobin Filleter; Allison M. Beese In Situ Transmission Electron Microscopy: Mechanical Testing, Encyclopedia of Nanotechnology (2016), p. 1543 | DOI:10.1007/978-94-017-9780-1_100990
  • Jiangwei Wang; Scott X. Mao Atomistic perspective on in situ nanomechanics, Extreme Mechanics Letters, Volume 8 (2016), p. 127 | DOI:10.1016/j.eml.2016.02.006
  • Saurabh Gupta; Olivier N. Pierron MEMS based nanomechanical testing method with independent electronic sensing of stress and strain, Extreme Mechanics Letters, Volume 8 (2016), p. 167 | DOI:10.1016/j.eml.2016.01.005
  • T Denneulin; M Hÿtch Four-wave dark-field electron holography for imaging strain fields, Journal of Physics D: Applied Physics, Volume 49 (2016) no. 24, p. 244003 | DOI:10.1088/0022-3727/49/24/244003
  • Nan Li; Jiangwei Wang; Scott Mao; Haiyan Wang In situ nanomechanical testing of twinned metals in a transmission electron microscope, MRS Bulletin, Volume 41 (2016) no. 4, p. 305 | DOI:10.1557/mrs.2016.66
  • Hosni Idrissi; Caroline Bollinger; Francesca Boioli; Dominique Schryvers; Patrick Cordier Low-temperature plasticity of olivine revisited with in situ TEM nanomechanical testing, Science Advances, Volume 2 (2016) no. 3 | DOI:10.1126/sciadv.1501671
  • Tobin Filleter; Allison M. Beese In Situ Transmission Electron Microscopy: Mechanical Testing, Encyclopedia of Nanotechnology (2015), p. 1 | DOI:10.1007/978-94-007-6178-0_100990-1
  • Peter J. Imrich; Christoph Kirchlechner; Daniel Kiener; Gerhard Dehm In Situ TEM Microcompression of Single and Bicrystalline Samples: Insights and Limitations, JOM, Volume 67 (2015) no. 8, p. 1704 | DOI:10.1007/s11837-015-1440-6
  • Q. Yu; M. Legros; A.M. Minor In situTEM nanomechanics, MRS Bulletin, Volume 40 (2015) no. 1, p. 62 | DOI:10.1557/mrs.2014.306
  • Peter J. Imrich; Christoph Kirchlechner; Daniel Kiener; Gerhard Dehm Internal and external stresses: In situ TEM compression of Cu bicrystals containing a twin boundary, Scripta Materialia, Volume 100 (2015), p. 94 | DOI:10.1016/j.scriptamat.2014.12.023
  • L. Farbaniec; G. Dirras; A. Krawczynska; F. Mompiou; H. Couque; F. Naimi; F. Bernard; D. Tingaud Powder metallurgy processing and deformation characteristics of bulk multimodal nickel, Materials Characterization, Volume 94 (2014), p. 126 | DOI:10.1016/j.matchar.2014.05.008

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