MEMS for in situ mechanical characterization

MEMS for in situ mechanical characterization refers to microelectromechanical systems (MEMS) used to measure the mechanical properties (such as the Young’s modulus and fracture strength) of nanoscale specimens such as nanowires, nanorods, whiskers, nanotubes and thin films. They distinguish themselves from other methods of nanomechanical testing because the sensing and actuation mechanisms are embedded and/or co-fabricated in the microsystem, providing—in the majority of cases—greater sensitivity and precision. This level of integration and miniaturization allows carrying out the mechanical characterization in situ, i.e., testing while observing the evolution of the sample in high magnification instruments such as optical microscopes, scanning electron microscopes (SEM), transmission electron microscopes (TEM) and X-ray setups. Furthermore, analytical capabilities of these instruments such as spectroscopy and diffraction can be used to further characterize the sample, providing a com

Transfer of Graphene under Ultra-High Vacuum

Darius Constantin Merk

This thesis reports on a novel method for graphene transfer that is fully UHV compatible, which has remained a challenge for a long time due to the necessity of supporting graphene for transfer and most often requiring supporting layer removal post-transfer. Our graphene transfer method is based on the wafer-bonding approach, where graphene is stamped onto a target surface, from a support to which it is weakly bound. We use a bilayer of graphene supported by a teflon tape for the low adhesion between graphene layers and the flexibility of teflon tape to allow adaptability to the target surface.We demonstrate successful transfer onto Cu(100) and Ir(111) single crystal surfaces as well as on gr/Ir(111), thus forming a (partial) graphene bilayer on Ir(111). For in-situ characterization, we use Auger electron spectroscopy and STM. Auger measurements confirm that we are able to transfer an average 0.8-0.9 ML of carbon, by comparison to CVD grown samples. After transfer onto Ir(111), we show that by annealing to 1000 °C, we are able to observe by STM the characteristic moiré pattern formed by CVD grown graphene on Ir(111). Auger spectra show that the graphene-Iridium interaction undergoes a change from physisorption to chemisorption upon annealing. XAS and Raman spectroscopy demonstrate that the annealing step taken post transfer to observe the moiré by STM is only necessary to induce a change in interaction strength but not to heal graphene defects, to increase its domain size, or to make it flat. After transfer onto Cu(100), Raman spectra show that the transferred graphene is of the same quality as the CVD grown graphene before transfer, without further annealing. Comparison of synchrotron based high resolution XAS spectra of transferred gr/Ir(111) to CVD grown samples confirms that the transferred graphene is flat on top of the Ir(111) crystal surface.This enables sample and device fabrication, usually hampered by impurities, to be carried out in UHV leading to fully reproducible results. Clean twisted bilayer graphene samples can be made and studied in UHV. Further, surface science can be extended to the third dimension, by capping layers and continuing growth, etc., all under clean conditions.

EPFL2022

In-situ Laue diffraction to follow dislocation patterning during fatigue

Ainara Irastorza Landa

The macroscopic strength of metals is determined by the dislocation arrangements that are formed when dislocations slip in the crystal lattice in response to the applied stress. Despite the extensive research carried out, the transition from uniform to non-uniform dislocation structures is not yet fully understood. This information is however essential to support the development of computational models that aim to predict dislocation patterning. Lattice rotation caused by the presence of dislocations is, for instance, a parameter that is often not taken into account in computational models although it plays a role in the development of dislocation ensembles. Experimentally following in-situ dislocation patterning including involved lattice rotations at lengthscales comparable to those in simulations is not straightforward. In fact, the current available techniques that have the necessary spatial and angular resolution are either destructive (3D-EBSD) or very time consuming (3D X-ray Laue diffraction). In this dissertation we present a new experimental approach that allows following lattice rotation and dislocation ensembles time-resolved during deformation. The technique is based on X-ray Laue diffraction scanning in transmission mode, which provides a sub-micron spatial resolution in 2D and statistical information on orientation spread in the third dimension. The in-situ mechanical tests are performed at the microXAS beamline of the Swiss Light Source Synchrotron. The method has been applied to understand dislocation pattering of copper single crystals occurring in the earlier phases of low cycle fatigue. Samples with different crystal orientations (single crystal, coplanar and collinear) have been cyclically deformed up to a maximum of 120 cycles. A dedicated miniaturized shear-fatigue device compatible with Laue diffraction has been constructed for that purpose and a sample preparation based on picosecond laser ablation has been developed. The developed procedure analyzes the evolving dislocation microstructures in terms of lattice rotation, lattice curvature and geometrically necessary dislocation densities at lengthscales similar to those addressable in computational models. It sacrifices on the fully 3D aspect but it brings the time resolution required to validate ongoing simulations. It has been shown that the error made by integration depends on the dislocation network expected. For instance, the technique can be used to validate 3DDD models or density based dislocation dynamics models when applied in deformation geometries where the formation of 2D dislocation patterns are expected (e.g. vein-channel structure in single slip oriented fatigued samples). The greatest advantage of this technique is that the evolving regions are easy to follow due to the high rotational sensitivity and time resolution of the method. What is more, the influence of the initial microstructure can be evaluated and quantitative values can be provided. On the other hand, the principal drawbacks are related to the gauge thickness of the samples. Even if the technique can estimate the orientation spread along the third direction, the approach cannot physically resolve the integrated signal along the thickness. This is source of uncertainty when providing actual values of lattice curvatures and geometrically necessary dislocation densities. Another shortcoming is the sensitivity of the method to the energy distribution of the X-ray beam provided in the beamline, which determines the collected signal - the principal basis of the subsequent analysis and interpretation.

EPFL2016