Michaël Coulombier

New On-Chip Nanomechanical Testing Laboratory - Applications to Aluminum and Polysilicon Thin Films

The measurement of the mechanical properties of materials with submicrometer dimensions is extremely challenging, from the preparation and manipulation of specimens to the application of small loads and extraction of accurate stresses and strains. A new on-chip nanomechanical testing concept has been developed in order to measure the mechanical properties of submicrometer freestanding thin films allowing various loading configurations and specimen geometries. The basic idea is to use internal stress present in one film to provide the actuation for deforming another film attached to the first film on one side and to the substrate on the other side. The measurement of the displacement resulting from the release of both films gives access to the stress and the strain applied to the test specimen provided the Youngs modulus and mismatch strain of the actuator film are known. Classical microelectromechanical-systems-based microfabrication procedures are used to pattern the test structures and release the films from the substrate. The design procedures, data reduction scheme, and a generic fabrication strategy are described in details and implemented in order to build a suite of test structures with various combinations of dimensions. These structures allow the characterization of different materials and mechanical properties and enable high throughputs of data while avoiding any electrical signal or external actuation. Results obtained on ductile aluminum and brittle polysilicon films demonstrate the potential of the method to determine the Youngs modulus, yield stress or fracture stress, fracture strain, and strain hardening in ductile materials.

On-chip stress relaxation testing method for freestanding thin film materials.

A stress relaxation method for freestanding thin films is developed based on an on-chip internal stress actuated microtensile testing set-up. The on-chip test structures are produced using microfabrication techniques involving cleaning, deposition, lithography, and release. After release from the substrate, the test specimens are subjected to uniaxial tension. The applied load decays with the deformation taking place during relaxation. This technique is adapted to strain rates lower than 10(-6)∕s and permits the determination of the strain rate sensitivity of very thin films. The main advantage of the technique is that the relaxation tests are simultaneously performed on thousands of specimens, pre-deformed up to different strain levels, for very long periods of time without monopolizing any external mechanical loading equipment. Proof of concept results are provided for 205-nm-thick sputtered AlSi(0.01) films and for 350-nm-thick evaporated Pd films showing unexpectedly high relaxation at room temperature.

Point Defect Clusters and Dislocations in FIB Irradiated Nanocrystalline Aluminum Films: An Electron Tomography and Aberration-Corrected High-Resolution ADF-STEM Study

Focused ion beam (FIB) induced damage in nanocrystalline Al thin films has been characterized using advanced transmission electron microscopy techniques. Electron tomography was used to analyze the three-dimensional distribution of point defect clusters induced by FIB milling, as well as their interaction with preexisting dislocations generated by internal stresses in the Al films. The atomic structure of interstitial Frank loops induced by irradiation, as well as the core structure of Frank dislocations, has been resolved with aberration-corrected high-resolution annular dark-field scanning TEM. The combination of both techniques constitutes a powerful tool for the study of the intrinsic structural properties of point defect clusters as well as the interaction of these defects with preexisting or deformation dislocations in irradiated bulk or nanostructured materials.

Overcurvature describes the buckling and folding of rings from curved origami to foldable tents

Daily-life foldable items, such as popup tents, the curved origami sculptures exhibited in the Museum of Modern Art of New York, overstrained bicycle wheels, released bilayered microrings and strained cyclic macromolecules, are made of rings buckled or folded in tridimensional saddle shapes. Surprisingly, despite their popularity and their technological and artistic importance, the design of such rings remains essentially empirical. Here we study experimentally the tridimensional buckling of rings on folded paper rings, lithographically processed foldable microrings, human-size wood sculptures or closed arcs of Slinky springs. The general shape adopted by these rings can be described by a single continuous parameter, the overcurvature. An analytical model based on the minimization of the energy of overcurved rings reproduces quantitatively their shape and buckling behaviour. The model also provides guidelines on how to efficiently fold rings for the design of space-saving objects.

MEMS-based microstructures for nanomechanical characterization of thin films

The measurement of mechanical properties of thin films is a major issue for the design of reliable microelectronic devices, microsensors or thin coatings. New simple microstructures actuated through the release of internally stressed long beams made of high temperature, low pressure chemical vapour deposition silicon nitride have been developed to test under uniaxial tension submicron thin film material specimens. The relative displacement between a fixed and a moving cursor is used to determine the strain applied to the specimen. The stress is inferred based on the mismatch strain and Youngs modulus of the silicon nitride actuator beam. By multiplying the tensile test microstructures with different lengths, the full stress-strain curve characterizing the thin material sample is generated from which the elastic stiffness, yield strength, ductility and fracture stress can be extracted. The potential of the method is demonstrated through applications on both brittle and ductile thin films. The Youngs modulus of 238 GPa for a 373 nm thick silicon nitride film is extracted and size effects are observed for the yield strength of pure aluminium with a value of 220 and 550 MPa, respectively, for 373 and 205 nm thick films. An original variant of the procedure based on this new test microstructure for measuring Youngs modulus is also presented.

Plasticity mechanisms in ultrafine grained freestanding aluminum thin films revealed by in-situ transmission electron microscopy nanomechanical testing

In-situ bright field transmission electron microscopy (TEM) nanomechanical tensile testing and in-situ automated crystallographic orientation mapping in TEM were combined to unravel the elementary mechanisms controlling the plasticity of ultrafine grained Aluminum freestanding thin films. The characterizations demonstrate that deformation proceeds with a transition from grain rotation to intragranular dislocation glide and starvation plasticity mechanism at about 1% deformation. The grain rotation is not affected by the character of the grain boundaries. No grain growth or twinning is detected.

Automatic Crystallographic Characterization in a Transmission Electron Microscope: Applications to Twinning Induced Plasticity Steels and Al Thin Films

A new automated crystallographic orientation mapping tool in a transmission electron microscope technique, which is based on pattern matching between every acquired electron diffraction pattern and precalculated templates, has been used for the microstructural characterization of nondeformed and deformed aluminum thin films and twinning-induced plasticity steels. The increased spatial resolution and the use of electron diffraction patterns rather than Kikuchi lines make this tool very appropriate to characterize fine grained and deformed microstructures.

Study of creep/relaxation mechanisms in thin freestanding nanocrystalline palladium films through the lab-on-chip technology

A nanomechanical lab-on-chip set-up has been used to study the creep/relaxation response of thin palladium films with temperature. The basic idea is to use residual stresses present in a silicon nitride thin beam to load the test film after etching the underneath sacrificial layer. The main advantage of this experimental method is that we can simultaneously perform thousands of creep/relaxation tests without monopolizing any external actuating/loading equipment and without using any time consuming calibration procedures. A signature of the dominant relaxation mechanism is given by the activation volume which has been determined for different levels of plastic deformation and different temperatures. The activation volume is equal to 15-40 b3 at room temperature and tends to decrease with increasing plastic deformation. The activation volume decreases when relaxation takes place at 50 C down to 7-20 b3. These variations of the activation volume indicate the competition between two different thermally activated deformation mechanisms in the temperature range between 20 C and 50 C.

Ductility of thin metallic films

Depending on the loading conditions, geometry and material characteristics, the ductility of thin metallic films is controlled either by the resistance to plastic localization or by the resistance to internal damage. New on-chip tensile tests performed on submicron aluminium films show significant strain hardening capacity leading to relatively good resistance to necking, while damage occurs through void nucleation at grain boundaries followed by their growth and coalescence. These results are discussed in the light of several other studies presented in the recent literature in order to unravel the origins of the frequently reported poor ductility of thin metallic films, and the various means existing to improve it.

Low Complexity Testing Micromachines Revealing Size-Dependent Mechanical Properties of Thin Al Films

The mechanical properties measurement of materials with submicron dimensions is extremely challenging, from the preparation and manipulation of specimens, to the application of small loads and extraction of accurate stresses and strains. Here, we describe a novel, versatile concept of micro and nano- machines to test films or beams with characteristic dimensions ranging between 10 nm to 1 mum, allowing multiple loading configurations and geometries. This testing method has been applied to thin, pure aluminium films. The yield strength linearly increases with the inverse of the film thickness, reaching 625 MPa for 150 nm thickness which is 10 times larger than for macroscopic samples.