FRACTURE AND FATIGUE BEHAVIOR OF ADDITIVELY MANUFACTURED MAR-M 509 CO-BASED SUPERALLOYS

Mar-M 509 is a Cobalt-based superalloy suitable for elevated temperature applications like nozzle guide vanes and blades in aero engines and gas turbines. Short cycle aging heat treatment of laser powder-bed-fusion processed Mar-M 509 is a novel route explored in this study to enhance the mechanical properties of this alloy, especially tensile ductility and fracture toughness, while retaining room and elevated temperature strengths. A detailed microstructural analysis is carried out using advanced characterisation tools and correlated to miniature, small volume, room temperature tensile tests and fracture toughness and fatigue tests using clamped beam geometry combined with digital image correlation-based in-situ strain mapping across the longitudinal and transverse directions, before and after heat treatment. Mechanisms leading to corresponding changes in fracture and fatigue properties will be discussed.
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INTEGRATING SIMULATION, MACHINE LEARNING, AND EXPERIMENTAL APPROACHES FOR HIGH-THOUGHPUT SMALL-SCALE FRACTURE INVESTIGATIONS

From Da Vinci to Galileo to modern experimentalists a variety of characterization methods have been introduced for investigating the fracture of materials. Determining fracture properties of materials at small length scales, with complex shapes, under extreme environmental conditions, is still extremely challenging. We will show how this gap is addressed by introducing two novel methods to investigate fracture. The first one involves light for contactless mechanical testing, while the second method integrates experiments with data-driven approaches to address issues related to complex shapes.
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OPERANDO EXPERIMENTS TO CHARACTERISE BRITTLE FRACTURE-LIKE EVENTS IN CERAMIC ELECTROLYTES VIA PHOTOELASTICITY

Solid electrolytes at current densities that are relevant to real battery operating conditions are prove to the penetration of lithium metal protrusions, also known as “dendritic” events, that are formed during battery charging. In this work, we show via operando photoelasticity experiments that the dendritic events at high current densities can be understood by the classic Griffith – Irwin fracture theory.
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QUANTIFICATION OF INTERFACE STRENGTH OF A THIN FILM USING A NEW MICROCANTILEVER GEOMETRY.

Interfaces failure occurs not only in structural materials but also in functional material systems including systems for energy conversion and storage. Such failures lead to degradation of mechanical and functional properties, such as battery capacity or electrical conductivity. In bulk scale, there are various experimental methods to investigate the interface strength and its failure mechanisms, for instance, peeling test, superlayer test, or indentation test. One of the disadvantages of these approaches is that it can be applied only to relatively thick coatings [1,2]. Small-scale mechanical testing is a powerful tool for studying interface properties because it can quantify micro- and nanometer-sized thin films, and individual interfaces of interest can be tested by isolating them using focused ion beam (FIB). Single and double cantilever beams have been used to investigate fracture/delamination properties of single interfaces [3,4], however, these methods are prone to experimental imperfections arising from testing geometries.
In this talk, we propose a new in situ scanning electron microscope (SEM) microcantilever design that provides reliable and quantitative interface toughness. In addition, the optimized geometry can promote a pre-notch (or crack) to propagate in a stable manner, which is important to generate a natural crack front without FIB-induced damage/artifacts.
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EVALUATING THE INTERFACIAL TOUGHNESS OF GAN-ON-DIAMOND USING BLISTERING METHOD WITH NANO-INDENTATION

An improved analysis of the interfacial toughness using nanoindentation induced blistering of thin films on stiff substrates is demonstrated on GaN-on-diamond. The Hutchinson-Suo analysis requires accurate measurement of blister dimensions, conventionally measured using 2-D line-scans from 3-D topographical maps. The new meteorology overcomes shortcomings of this technique by fitting the 3-D analytical solution of a clamped Kicrchoff plate to the topological map of the blister. This allowed for quantification of interfacial toughness of smaller blisters in GaN-on-diamond, previously assumed invalid for analysis due to inadequacies of the line-scan analysis. Three samples were investigated and found to have interfacial toughness ranging from 0.6–1 J m−2. Additionally, the relationship between residual stress in the GaN and interfacial toughness was investigated using photoluminescence spectroscopy. In all cases, the GaN was found to be under increased compression at the diamond interface by up to -0.81 GPa, although no correlation with interfacial toughness was observed.
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IMPACT OF GRAIN BOUNDARY MODIFICATIONS ON FRACTURE TOUGHNESS OF TUNGSTEN BASED NANOMATERIALS [Keynote]

Nanostructured materials commonly excel with respect to their strength, but their ductility and toughness remain limiting factors for deployment in safety related applications. In this work, using grain boundary engineering concepts in conjunction with severe plastic deformation for microstructural refinement, we aim to develop nanostructured and nanocomposite materials that overcome these limitations. Since material volumes are limited, we utilize small scale testing approaches to examine the respective material properties such as strength, ductility and fracture toughness. We detail on the one hand challenges and recent advancements in small scale fracture experiments, and on the other hand the effectiveness of the mentioned grain boundary engineering approaches to design outstanding nanomaterials overcoming strength-ductility-toughness limitations.
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A NOVEL SMALL-SCALE BEND GEOMETRY CREEP TEST TO EVALUATE DEFORMATION AND CAVITATION DAMAGE IN POLYCRYSTALLINE AND BI CRYSTAL COPPER

Understanding the mechanisms of creep deformation and damage (cavitation) in engineering components materials is important, but despite the significant research that has been conducted over the past 50 years, there is still a lack of understanding of the microstructural processes that influence and control the development of damage. To provide further insights into this, in the present work a novel small-scale constant load cantilever beam geometry test specimen is used. The materials selected for the tests are polycrystalline and bi-crystals of high purity copper. The copper provides a simple model material for exploring initiation and early growth of creep cavitation and allows comparison with crystal-based model predictions.
In this study, both creep deformation and creep cavitation were measured. For the latter, a range of higher spatial resolution techniques were adopted including scanning electron microscopy, electron backscattered diffraction and focused gallium ion beam serial section milling. Creep cavity number density and size measurements were made using advanced image analysis procedures. Polycrystalline and bi-crystal results are compared, with particular attention given to the role of Schmid factor and misorientation on the initiation and early growth of the creep cavities. These experimental results inform the development of microstructural based models of cavitation.
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ANALYSIS OF FRACTURE BEHAVIOUR OF MULTILAYERS BY CANTILEVER AND CLAMPED BEAM BENDING GEOMETRY

Multilayering of metal/ceramic combinations can help to achieve better strength and toughness than the individual material constituents. The effect of elastic-plastic mismatch in multilayers on the crack driving force and eventually on fracture resistance has been analyzed in this work. The enhancement in fracture toughness by decreasing layer spacing has been predicted from finite element calculations and verified by micro-cantilever fracture tests. Further, calculations have been carried out for a more stable clamped beam bend geometry to determine R-curve behavior in such multilayers.
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OPTIMIZATION AND USE OF HIGH-THROUGHPUT MICROMECHANICAL TESTING DESIGN FOR 3D-PRINTED POLYMERS

Modern materials behave differently on a micro-scale level than in bulk applications. Therefore, with ever present miniaturization, the materials’ testing on a micron-level is gaining importance. 3D printing with a sub micron precision, such as direct laser writing by two-photon lithography, allows for relatively fast manufacturing of miniaturized specimens for micromechanical testing. In combination with precise loading by a nanoindenter tip, high throughput micromechanical testing is enabled. Presented research shows design process of miniaturized cantilever and push to pull device specimens for fracture mechanics testing, aided finite element modelling, together with high throughput testing of polymeric materials with varied printing parameters and loading conditions. Such in situ and ex situ experimental setup allows for systematic fracture mechanics testing on the small scale for common materials used in small-scale 3D printing.
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MICRO-BENDING FOR MULTI-SCALE FRACTURE CHARACTERIZATION OF CEMENT-BASED MATERIALS AND CERAMICS

The last few years have seen the development of several testing techniques at the micro-scale to characterize the mechanical properties of multi-scale materials. One such novel methods are micro-cantilever bending tests to assess mechanical properties of materials. Micro-cantilever tests allow for a variety of test configurations, including scaled chevron-notch geometry allowing controlled crack-growth prior to critical failure load. Chevron notches are convenient at such length scales since they allow for ex-situ measurements of crack length – avoiding the need to directly measure crack length, which could be a challenge at such scale. The test approach provides access to R-curve behavior for quasi-brittle materials on the micro-scale and opens the door to investigate more sophisticated topics, i.e., creep crack growth. Moreover, the technique complemented with visualization and scanning tools, such as Scanning Electron Microscopy and Microtomography, allows for a proper and extensive analysis of the crack growth phenomena.
The motivation of this work revolves around expanding currently available knowledge on multiscale characterization of cement-based materials with the focus on fracture testing at the micro- and mesoscale through the novel micro-bending technique. This test opens the door to understanding fracture, toughening mechanisms, and evolution of these properties regarding processing variables.
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