Preparation of H-bar cross-sectional specimen for in situ TEM straining experiments: A FIB-based method applied to a nitrided Ti–6Al–4V alloy

Castany, Philippe; Legros, Marc

doi:10.1016/j.msea.2010.10.025

Cited by 14 publications

(6 citation statements)

References 29 publications

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“…Signifi cant dislocation activity was observed during twin growth, specifi cally across the twin boundary. In Mg, ( ) 10 96 This wide variation in quantitative data demonstrates the stochastic nature of small-scale mechanical testing, as well as the signifi cant size effects associated with the twinning mechanism. In Yu et al's work, 94 signifi cant strain hardening was obtained after the formation of a nanotwinned structure, presumably resulting from the high density of twin boundaries, which serve as barriers to further dislocation motion.…”

Section: Observations Of Deformation Twinningmentioning

confidence: 99%

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In situTEM nanomechanics

Legros²,

Minor³

2015

MRS Bull.

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IntroductionThe mechanical properties of any material are highly correlated with its defect structure. Starting in the late 1950s, 1 in situ straining stages for use in transmission electron microscopes that could provide dynamic observations of dislocation motion in metals were developed. In the following years, research teams fabricated various transmission electron microscopy (TEM) straining holders, including some that could operate at low or high temperature. Since then, in situ TEM straining tests have been performed to study the behavior of dislocations and their interactions with other defects such as twins, grain boundaries (GBs), and interfaces.After early load sensor integration developments, 2 , 3 in situ TEM mechanical testing with quantitative load measurement expanded toward commercialization in the beginning of this century, including mechanical probing modes such as nanoindentation. 4 These developments are particularly useful for studying size effects in materials, whereby mechanical properties and microstructure can be tuned by the physical dimensions (internal such as grain size or external such as fi lm thickness) of materials. 5 -7 At the micrometer or nanometer scale, the sample dimensions can be of the same order as the defects that carry the deformation, such as the length of a dislocation line or the thickness or spacing of twins. When this occurs, strong size effects can change the deformation mechanisms and the corresponding mechanical properties. Quantitative in situ TEM mechanical testing is therefore an ideal tool for studying the origin and principles of these size effects. This review provides an overview of available in situ TEM techniques and recent studies performed on dislocation behavior, dislocation/boundary interactions, deformation twinning, and GB-mediated plasticity. We also provide a critical discussion of the effects of size on different deformation mechanisms and the correlated mechanical properties of materials. Some of these mechanisms are summarized in Figure 1 . In situ TEM straining techniquesVarious tools for mechanical testing by a transmission electron microscope that exist today 8 are briefl y detailed in this section. They span from simple motorized grips to elaborate mechanical testing units capable of returning values for load and displacement.In classical tensile holders for TEM, samples are attached to a pair of jaws, and one side is slowly pulled by an electric motor located in a housing unit outside the TEM instrument. A rigid shaft ensures strain transmission at speeds ranging from 10 nm/s to 10 µm/s. This simple technique 9 has various advantages because of its high versatility. Virtually any thin or thinned sample can be strained as soon as it is attached to In situ transmission electron microscopy (TEM) nanomechanical testing has benefi ted from a number of recent technical developments related to both how deformation is imaged and how deformation is induced and measured inside a TEM instrument. These developments have led to new insights into the ...

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Section: Observations Of Deformation Twinningmentioning

confidence: 99%

“…a stretchable grid. 10 Options for heating (up to 1200°C with a miniaturized furnace as shown in Figure 2 a) or cooling (down to liquid He or, more often, liquid N 2 temperatures) can be easily added. The very rigid strain transmission allows for the deformation of thin fi lms 12 , 13 or brittle alloys.…”

Section: Q Yu M Legros and Am Minormentioning

confidence: 99%

In situTEM nanomechanics

Legros²,

Minor³

2015

MRS Bull.

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“…This part is more dedicated to an overview of unusual but simple methods that can lead to well adapted TEM samples for in situ TEM. The old fashioned H-bar method (Castany and Legros, 2011) was progressively abandoned in favor of the lift-out method that is by far more convenient for most applications. However its extremely robustness (the TEM sample belongs to the micrometric scale) is a perfect asset regarding the moving probe system presented above.…”

Section: Focused Ion Beammentioning

confidence: 99%

In SituCharacterization Methods in Transmission Electron Microscopy

Masseboeuf¹

2012

Transmission Electron Microscopy in Micro‐Nanoelectronics

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HAL is a multi-disciplinary open access archive for the deposit and dissemination of scientific research documents, whether they are published or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers. L'archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d'enseignement et de recherche français ou étrangers, des laboratoires publics ou privés.

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“…FIB can realize site-specific extraction, transfer, mounting and machining of micron-sized material thanks to the integration of electron beam imaging, ion beam milling, micromanipulation and beam-induced deposition. This set of functions can well meet the high geometric and positioning requirements for in situ TEM samples [1,2].…”

Section: Introductionmentioning

confidence: 99%

FIB-shield: a structure to safely transfer and precisely mount beam-sensitive TEM specimens under focused ion beam

Zhang,

Yang,

et al. 2023

Phys. Scr.

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Focused ion beam (FIB) has been adopted extensively for transmission electron microscope (TEM) sample preparation during the past decades. However, ion beam- and deposition-induced damage during transferring and mounting of the sample cannot be effectively avoided, limiting the application of FIB in ion-beam illumination-sensitive samples. A transferring device called the FIB shield is designed and fabricated to greatly reduce the damage and contamination of the sample during transfer and mounting under Ga+ beam imaging, milling and Pt deposition. Nearly damage-free transfer and precise positioning and attachment of beam-sensitive in situ TEM nanoindentation samples are achieved. The effectiveness of the shielding plate to block Ga+ radiation damage during Ga+ beam imaging and milling and that of the buffer region to alleviate sputtering damage during Pt deposition are verified by corresponding experiments.

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Preparation of H-bar cross-sectional specimen for in situ TEM straining experiments: A FIB-based method applied to a nitrided Ti–6Al–4V alloy

Cited by 14 publications

References 29 publications

In situTEM nanomechanics

In situTEM nanomechanics

In SituCharacterization Methods in Transmission Electron Microscopy

FIB-shield: a structure to safely transfer and precisely mount beam-sensitive TEM specimens under focused ion beam

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