In situ SEM indentation experiments: Instruments, methodology, and applications

Ghisleni, R.; Rzepiejewska-Malyska, Karolina; Philippe, Laëtitia; Schwaller, P.; Michler, Johann

doi:10.1002/jemt.20677

Cited by 47 publications

(23 citation statements)

References 27 publications

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“…However, due to the small sizes of the structures, observation and subsequent analysis can still be difficult and involve numerous assumptions. To address this, microscale compression tests are now being conducted inside high-resolution electron microscopes [13][14][15][16][17][18][19][20][21]. This enables the continuous observation of the structures during the compression and provides information concerning the deformation and failure modes including the moment and location where shear bands, cracks or buckling initially appear.…”

Section: Introductionmentioning

confidence: 99%

Quantitative stress/strain mapping during micropillar compression

Maeder

Mook

Niederberger

et al. 2011

Philosophical Magazine

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Micropillar compression is increasingly used as a method to examine small length-scale mechanical properties since it minimises the strain gradients that are unavoidable during nanoindentation into a flat surface. It also simplifies the data analysis since it is assumed that the compression is uniaxial. But how valid is this assumption when misalignments in the microscale setup are generally unavoidable? In order to investigate this, the stress and strain tensors of the micropillar should be measured during the compression. To accomplish this, electron backscatter diffraction (EBSD) mappings were obtained before, during and after consecutive compressions of a GaAs micropillar inside of a high-resolution scanning electron microscope. Elastic strain and the corresponding stress tensors were determined from the EBSD measurements using a cross-correlation technique. The results show that the von Mises stress compares well to the engineering stress determined from the nanoindenter load-displacement data. Even with rotations of almost 3 at maximum load, the negligible shear components in the strain tensor within the pillar indicates that the assumption of uniaxial compression can be made. Due to its high spatial resolution and strain sensitivity, in situ strain-stress mapping during micromechanical testing is a very promising route for the investigation of deformation phenomena on the sub-micron scale.

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Section: Introductionmentioning

confidence: 99%

Quantitative stress/strain mapping during micropillar compression

Maeder

Mook

Niederberger

et al. 2011

Philosophical Magazine

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“…Compared with conventional ex situ indentation and scratch testing, in situ indentation and scratch testing inside the scanning electron microscope (SEM) and the transmission electron microscope (TEM) have the function of dynamically observing the contact process between the indenter and the sample [11–18], which is meaningful to investigate deformation and damage mechanisms of materials during the indentation and scratch testing process and to explain discontinuous phenomena appearing in the penetration load-depth curves. The design of in situ indentation and scratch devices compatible with the SEM and TEM has limitations arising from the characteristics of the SEM and TEM, such as the small volume of the chamber, short working distance, electromagnetic sensing, the vacuum environment and vibration sensing [16]. Up to now, quantitative in situ SEM and TEM indentation devices have been presented by researchers and some of them can also carry out in situ scratch testing inside the SEM qualitatively [14,18].…”

Section: Introductionmentioning

confidence: 99%

A Novel Two-Axis Load Sensor Designed for in Situ Scratch Testing inside Scanning Electron Microscopes

Huang

Zhao

et al. 2013

Sensors

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Because of a lack of available miniaturized multiaxial load sensors to measure the normal load and the lateral load simultaneously, quantitative in situ scratch devices inside scanning electron microscopes and the transmission electron microscopes have barely been developed up to now. A novel two-axis load sensor was designed in this paper. With an I-shaped structure, the sensor has the function of measuring the lateral load and the normal load simultaneously, and at the same time it has compact dimensions. Finite element simulations were carried out to evaluate stiffness and modal characteristics. A decoupling algorithm was proposed to resolve the cross-coupling between the two-axis loads. Natural frequency of the sensor was tested. Linearity and decoupling parameters were obtained from the calibration experiments, which indicate that the sensor has good linearity and the cross-coupling between the two axes is not strong. Via the decoupling algorithm and the corresponding decoupling parameters, simultaneous measurement of the lateral load and the normal load can be realized via the developed two-axis load sensor. Preliminary applications of the load sensor for scratch testing indicate that the load sensor can work well during the scratch testing. Taking advantage of the compact structure, it has the potential ability for applications in quantitative in situ scratch testing inside SEMs.

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“…18 Today several sophisticated device concepts and improvements of already existing devices have been developed. [19][20][21] Further details on the history and recent developments of electron microscopy based in situ testing devices are given by Legros et al 8 In summary, the whole span of applications from tensile testing to in situ tribology for both organic and inorganic mater in amorphous and crystalline state is now being covered. [22][23][24][25][26][27][28][29][30][31][32][33][34][35][36][37] Even the first commercial solutions emerge for both SEM and TEM, mainly employing a patented three plate capacitor design for applying forces and measuring displacements at the same time.…”

Section: Introductionmentioning

confidence: 99%

“…[22][23][24][25][26][27][28][29][30][31][32][33][34][35][36][37] Even the first commercial solutions emerge for both SEM and TEM, mainly employing a patented three plate capacitor design for applying forces and measuring displacements at the same time. 7,19,38,39 MEMS technology integrated into electron microscopes currently offers the best force and displacement resolution. However, the routine application is not yet possible.…”

Section: Introductionmentioning

confidence: 99%

A novel apparatus for in situ compression of submicron structures and particles in a high resolution SEM

Romeis

Paul

Ziener

et al. 2012

Review of Scientific Instruments

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We report on the development and characterization of a novel in situ manipulation device to perform stressing experiments on the submicron scale inside a high resolution field emission scanning electron microscope. The instrument comprises two main assembly groups: an upper part for positioning and moving a mounted probe and a force sensor as well as a specimen support as lower part. The upper part consists of a closed loop tripod piezoelectric scanner mounted on a self-locking coarse positioning stage. Two interlocked steel springs and a linear variable differential transformer measuring the springs’ deflections compose the lower part of the instrument. This arrangement acts as force-sensor and sample support. In comparison to already well-established concepts a wide measuring range is covered by adjusting the spring constant between 30 N/m and 50000 N/m. Moreover, the new device offers striking advantages with respect to force calibration and sample deformation measurements. Force calibration is performed using the eigenfrequency of the force detection system directly inside the SEM. Deformation data are obtained with high accuracy by simultaneously recording displacements above and below the specimen. The detrimental apparatus compliance is determined, and the influence on measured data subsequently minimized: an easy to validate two-springs-in-series model is used for data correction. A force resolution in normal direction of 100 nN accompanied by a sample deformation resolution of 5 nm can be achieved with the instrument using an appropriate load cell stiffness. The capabilities and versatility of this instrument are exemplified by compression experiments performed on submicron amorphous silica particles.

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In situ SEM indentation experiments: Instruments, methodology, and applications

Cited by 47 publications

References 27 publications

Quantitative stress/strain mapping during micropillar compression

Quantitative stress/strain mapping during micropillar compression

A Novel Two-Axis Load Sensor Designed for in Situ Scratch Testing inside Scanning Electron Microscopes

A novel apparatus for in situ compression of submicron structures and particles in a high resolution SEM

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