Thin-Film Microtensile-Test Structures for High-Throughput Characterization of Mechanical Properties.

A photolithographic process for the rapid fabrication of thin-film tensile-test structures is presented. The process is applicable to various physical vapor deposition techniques and can be used for the combinatorial fabrication of thin-film tensile-test structure materials libraries for the high-throughput characterization of mechanical properties. The functionality of the fabrication process and the feasibility of performing high-quality measurements with these structures are demonstrated with Cu tensile-test structures. In addition, the scalability from unary structures to libraries with compositional variations is demonstrated.

Development of a high-temperature micromechanics stage with a novel temperature measurement approach.

The study of mechanical properties of materials at high temperatures at the microstructural length regime requires dedicated setups for testing. Despite the advances in the instrumentation in these setups over the last decade, further optimization is required in order to extend the temperature range well-beyond 600 °C. Particularly, an improvement of the contact temperature measurement is required. A design with a novel approach of temperature measurement with independent tip and sample heating is developed to characterize materials at high temperatures. This design is realized by modifying a displacement controlled room temperature microstraining rig with the addition of two miniature hot stages, one each carrying the sample and indenter tip. The sample reaches temperatures of >600 °C with a 50 W diode laser system. The stages have slots for the working sample as well as a reference sample on both ends for precise temperature measurements, relying on the symmetry of the stage toward the ends. The whole setup is placed inside a custom-made steel chamber, capable of attaining a vacuum of 10-4 Pa. Alternatively, the apparatus can be operated under environmental conditions by applying various gases. Here, the unique design and its high temperature capabilities will be presented together with the first results of microtension experiments on freestanding copper thin films at 400 °C.

Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector.

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

Coccospheres confer mechanical protection: New evidence for an old hypothesis.

UNLABELLED: Emiliania huxleyi has evolved an extremely intricate coccosphere architecture. The coccosphere is comprised of interlocking coccoliths embedded in a polysaccharide matrix. In this work, we performed in-situ scanning electron microscopy based compression tests and conclude that coccospheres have a mechanical protection function. The coccosphere exhibits exceptional damage tolerance in terms of inelastic deformation, recovery and stable crack growth before catastrophic fracture, a feature, which is not found in monolithic ceramic structures. Some of the mechanical features of the coccospheres are due to their architecture, especially polysaccharide matrix that acts as a kind of bio-adhesive. Our data provide strong evidence for the mechanical protection-hypothesis of coccolithophore calcification, without excluding other functions of calcification such as various biochemical roles discussed in the literature. STATEMENT OF SIGNIFICANCE: Although bio-mechanics of shell structures like nacre have been studied over the past decade, coccospheres present an architecture that is quite distinct and complex. It is a porous cell structure evolved to protect the living algae cell inside it in the oceans, subjected to significant hydrostatic pressure. Despite being made of extremely brittle constituents like calcium carbonate, our study finds that coccospheres possess significant damage tolerance especially due to their interlocking coccolith architecture. This will have consequences in bio-mimetic design, especially relating to high pressure applications.

Measuring electro-mechanical properties of thin films on polymer substrates.

In order to advance flexible electronic technologies it is important to study the electrical properties of thin metal films on polymer substrates under mechanical load. At the same time, the observation of film deformation and fracture as well as the stresses that are present in the films during straining are also crucial to investigate. To address both the electromechanical and deformation behavior of metal films supported by polymer substrates, in-situ 4 point probe resistance measurements were performed with in-situ atomic force microscopy imaging of the film surface during straining. The 4 point probe resistance measurements allow for the examination of the changes in resistance with strain, while the surface imaging permits the visualization of localized thinning and crack formation. Furthermore, in-situ synchrotron tensile tests provide information about the stresses in the film and show the yield stress where the deformation initiates and the relaxation of the film during imaging. A thin 200 nm Cu film on 23 µm thick PET substrate will be used to illustrate the combined techniques. The combination of electrical measurements, surface imaging, and stress measurements allow for a better understanding of electromechanical behavior needed for the improvement and future success of flexible electronic devices.

A new method for polychromatic X-ray µLaue diffraction on a Cu pillar using an energy-dispersive pn-junction charge-coupled device.

µLaue diffraction with a polychromatic X-ray beam can be used to measure strain fields and crystal orientations of micro crystals. The hydrostatic strain tensor can be obtained once the energy profile of the reflections is measured. However, this remains a challenge both on the time scale and reproducibility of the beam position on the sample. In this review, we present a new approach to obtain the spatial and energy profiles of Laue spots by using a pn-junction charge-coupled device, an energy-dispersive area detector providing 3D resolution of incident X-rays. The morphology and energetic structure of various Bragg peaks from a single crystalline Cu micro-cantilever used as a test system were simultaneously acquired. The method facilitates the determination of the Laue spots' energy spectra without filtering the white X-ray beam. The synchrotron experiment was performed at the BM32 beamline of ESRF using polychromatic X-rays in the energy range between 5 and 25 keV and a beam size of 0.5 µm × 0.5 µm. The feasibility test on the well known system demonstrates the capabilities of the approach and introduces the "3D detector method" as a promising tool for material investigations to separate bending and strain for technical materials.

Ductile film delamination from compliant substrates using hard overlayers.

Flexible electronic devices call for copper and gold metal films to adhere well to polymer substrates. Measuring the interfacial adhesion of these material systems is often challenging, requiring the formulation of different techniques and models. Presented here is a strategy to induce well defined areas of delamination to measure the adhesion of copper films on polyimide substrates. The technique utilizes a stressed overlayer and tensile straining to cause buckle formation. The described method allows one to examine the effects of thin adhesion layers used to improve the adhesion of flexible systems.