Design and application of a novel microelectromechanical system for in situ SEM/TEM displacement controlled tensile testing of nanostructures

Abstract

Since the 1920s, different methodologies have been developed especially for mechanical characterization of material samples with characteristic length on the order of micro/nanometers. In the present manuscript, the main of such methodologies are presented and compared, in order to provide guidelines for mechanical characterization at the micro/nanoscale, and to identify the most versatile and effective among them. These are based on complete and miniaturized tensile testing stages, developed on proper microelectromechanical systems (MEMS). Because of their small size (they lie onto silicon wafers with area smaller than 1mm2 and thickness of only few micrometers), such testing devices are particularly suitable to handle micro/nanosized components, and can fit inside the tight chamber of scanning/ transmission electron microscopes (SEM/TEM), for real-time imaging of sample deformation. However, the effectiveness of the tests they allow to perform can be compromised by some disturbing phenomena, like onset of instability, as reported in a certain kind of tensile testing devices. In particular, these devices become unstable as soon as the sample under investigation shows stress relaxation, after some strain has been applied. Nevertheless, it is very important to be able to detect such singularities, since they may allow a deeper comprehen sion of materials’ behavior. In the present work, the above mentioned instability issue is overcome through the design of a novel device for in situ SEM/TEM tensile testing of nanostructures under true displacement control. Like other stages, also the one presented herein consists of two main components: an actuator and a sensor, which are separated by a small gap for positioning of the specimen. Actuation is performed by a thermal actuator, which pulls the end of the sample attached to it. The other end of the sample is instead connected to a displacement sensor, which moves from its equilibrium position, as a consequence of the force transmitted to it by the specimen. However, the main novelty of the present design is the introduction of a feedback control loop. In particular, a controller, implemented within a software routine, receives as input the sensor output, and computes the voltage to be applied to an electrostatic actuator, in order to generate a rebalance force of electrostatic nature, thus bringing the sensor back to equilibrium. In this way, the end ofand this boundary condition removes any potential source of instability. The MEMS sensing and actuating structures were designed by the means of both analytical and numerical approaches, in order to provide sufficiently high deformation (up to about 50% strain) and forces (up to 100μN) to break a variety of material samples. Fabrication was carried out by an external foundry on the basis of the masks drawings, reported in the present manuscript. In order to guarantee a correct functioning of the device, a proper experimental apparatus was developed. This allowed electrical connection of all of the actuating and sensing parts with external instrumentation, including current pre-amplifiers, power supplies, a lock-in amplifier, and a data acquisition card, which was used as interface between the controller and the MEMS device. The effectiveness of the present experimental apparatus was proven through an application on silver nanowires, with about 70 nm diameter and 3-4 μm gage length. The corresponding results, in terms of Young modulus, fracture and yield strength, showed good agreement with data already available in the literature, obtained for samples with comparable size. Also the device ability to detect singularities in the sample characteristic was demonstrated, as emerges from a load drop recorded after yielding of a nanowire. As a conclusion, the present experimental apparatus can be considered for future in situ SEM/TEM tensile tests on other material samples, as well as for electromechanical tests, since the specimen results to be electrically isolated from the remaining of the device. Thus, very interesting properties, like piezoresistivity and piezoelectricity, could be evaluated.