Enrico Salvati

A state-of-the-art review of micron-scale spatially resolved residual stress analysis by FIB-DIC ring-core milling and other techniques

Quantification of residual stress gradients can provide great improvements in understanding the complex interactions between microstructure, mechanical state, mode(s) of failure and structural integrity. Highly focused local probe non-destructive techniques such as X-ray diffraction, electron diffraction or Raman spectroscopy have an established track record in determining spatial variations in the relative changes in residual stress with respect to a reference state for many structural materials. However, the interpretation of these measurements in terms of absolute stress values requires a strain-free sample often difficult to obtain due to the influence of chemistry, microstructure or processing route. With the increasing availability of focused ion beam instruments, a new approach has been developed which is known as the micro-scale ring-core focused ion beam-digital image correlation technique. This technique is becoming the principal tool for quantifying absolute in-plane residual stresses. It can be applied to a broad range of materials: crystalline and amorphous metallic alloys and ceramics, polymers, composites and biomaterials. The precise nano-scale positioning and well-defined gauge volume of this experimental technique make it eminently suitable for spatially resolved analysis, that is, residual stress profiling and mapping. Following a summary of micro-stress evaluation approaches, we focus our attention on focused ion beam-digital image correlation methods and assess the application of micro-scale ring-core methods for spatially resolved residual stress profiling. The sequential ring-core milling focused ion beam-digital image correlation method allows micro- to macro-scale mapping at the step of 10–1000 μm, while the parallel focused ion beam-digital image correlation approach exploits simultaneous milling operation to quantify stress profiles at the micron scale (1–10 μm). Cross-validation against X-ray diffraction results confirms that these approaches represent accurate, reliable and effective residual stress mapping methods.

Strain softening of nano-scale fuzzy interfaces causes Mullins effect in thermoplastic polyurethane

The strain-induced softening of thermoplastic polyurethane elastomers (TPUs), known as the Mullins effect, arises from their multi-phase structure. We used the combination of small- and wide- angle X-ray scattering (SAXS/WAXS) during in situ repeated tensile loading to elucidate the relationship between molecular architecture, nano-strain, and macro-scale mechanical properties. Insights obtained from our analysis highlight the importance of the ‘fuzzy interface’ between the hard and soft regions that governs the structure evolution at nanometre length scales and leads to macroscopic stiffness reduction. We propose a hierarchical Eshelby inclusion model of phase interaction mediated by the ‘fuzzy interface’ that accommodates the nano-strain gradient between hard and soft regions and undergoes tension-induced softening, causing the Mullins effect that becomes apparent in TPUs even at moderate tensile strains.

Residual Stress Measurement on Shot Peened Samples Using FIB-DIC

Shot peening is an established technique for improving the fatigue resistance of mechanical components by performing a deformation treatment that causes local near surface plastic deformation and introduces a layer of compressive residual stress. The knowledge of the residual stress distribution plays a crucial role in the correct prediction of fatigue life during service in the context of engineering design. Reliable prediction of safe fatigue life requires knowing how the residual stress state obtained after shot peening depends on the sample geometry, e.g. the presence of notches, and how it evolves during cyclic loading. The Focused Ion Beam milling coupled with Digital Image Correlation (DIC) analysis of SEM images (the FIB-DIC method) has been shown to be an efficient technique for stress evaluation at the (sub)micron-scale. The residual stresses in the vicinity of shot-peened rounded notch tips in Al-7075-T651 samples were studied as a function of notch radii (ρ = 2, 0.5, 0.15 mm). The interpretation of the results is aided by comparison with a simple numerical model of eigenstrain cylinder.

Nanoscale Origins of the Size Effect in the Compression Response of Single Crystal Ni-Base Superalloy Micro-Pillars

Nickel superalloys play a pivotal role in enabling power-generation devices on land, sea, and in the air. They derive their strength from coherent cuboidal precipitates of the ordered γ’ phase that is different from the γ matrix in composition, structure and properties. In order to reveal the correlation between elemental distribution, dislocation glide and the plastic deformation of micro- and nano-sized volumes of a nickel superalloy, a combined in situ nanoindentation compression study was carried out with a scanning electron microscope (SEM) on micro- and nano-pillars fabricated by focused ion beam (FIB) milling of Ni-base superalloy CMSX4. The observed mechanical response (hardening followed by softening) was correlated with the progression of crystal slip that was revealed using FIB nano-tomography and energy-dispersive spectroscopy (EDS) elemental mapping. A hypothesis was put forward that the dependence of material strength on the size of the sample (micropillar diameter) is correlated with the characteristic dimension of the structural units (γ’ precipitates). By proposing two new dislocation-based models, the results were found to be described well by a new parameter-free Hall–Petch equation.

submitter : Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation.

Multiscale analysis of bamboo deformation mechanisms following NaOH treatment using X-ray and correlative microscopy

For hundreds of years, bamboo has been employed for a variety of applications ranging from load-bearing structures to textiles. Thanks to its hierarchical structure that is functionally graded and naturally optimised, bamboo displays a variation in properties across its stem that ensures exceptional flexural performance. Often, alkaline solutions are employed for the treatment of bamboo in order to alter its natural elastic behaviour and make it suitable for particular applications. In this work we study the effect of NaOH solutions of five different concentrations (up to 25%) on the elastic properties of bamboo. By exploiting the capabilities of modern experimental techniques such as in situ synchrotron X-ray scattering and Digital Image Correlation, we present detailed analysis of the deformation mechanisms taking place in the main constituents of bamboo, i.e. fibres and matrix (Parenchyma). The principal achievement of this study is the elucidation of the deformation mechanisms at the fibre scale, where the relative sliding of fibrils plays a crucial role in the property modification of the whole bamboo stem. Furthermore, we shed light on the parenchyma toughness variation as a consequence of alkali treatments. STATEMENT OF SIGNIFICANCE Alkaline solutions are often employed for the treatment of bamboo in order to alter its natural elastic behaviour. In this work we study the effect of alkaline solutions on the elastic properties of bamboo. Using state of the art experimental techniques allowed shedding light on the deformation mechanisms occurring in the bamboo main constituents, i.e. fibres and matrix (parenchyma cells). Enhancement of fibre stiffness was experienced when up to 20% NaOH solution was employed, while for higher concentration a decay was observed. This effect was imputed to the modification of adhesion between fibrils induced by disruption of ligand elements (e.g. lignin). Modification of the matrix toughness was also experienced, that indicated an improved resistance to cracking when the concentration of NaOH is 25%, while reduction of toughness was revealed for lower concentrations.

In situ monitoring and analysis of enamel demineralisation using synchrotron X-ray scattering

Dental caries is one of the most common chronic diseases that affect human teeth. It often initiates in enamel, undermining its mechanical function and structural integrity. Little is known about the enamel demineralisation process caused by dental caries in terms of the microstructural changes and crystallography of the inorganic mineral phase. To improve the understanding of the carious lesion formation process and to help identify efficient treatments, the evolution of the microstructure at the nano-scale in an artificially induced enamel erosion region was probed using advanced synchrotron small-angle and wide-angle X-ray scattering (SAXS and WAXS). This is the first in vitro and time-resolved investigation of enamel demineralisation using synchrotron X-ray techniques which allows in situ quantification of the microstructure evolution over time in a simulated carious lesion. The analysis revealed that alongside the reduction of mineral volume, a heterogeneous evolution of hydroxyapatite (HAp) crystallites (in terms of size, preferred orientation and degree of alignment) could be observed. It was also found that the rate and direction of dissolution depends on the crystallographic orientation. Based on these findings, a novel conceptual view of the process is put forward that describes the key structural parameters in establishing high fidelity ultrastructure-based numerical models for the simulation of the enamel demineralisation process. STATEMENT OF SIGNIFICANCE Hydroxyapatite (HAp) crystallites in the enamel dissolve during dental caries although little is known about the structural-chemical relationships that control the dynamic demineralisation process. For the first time this work investigated the in situ evolution of nano-scale morphology and the spatial distribution of ultrastructural HAp crystallites of human enamel during demineralisation in simulated caries. Advanced synchrotron SAXS and WAXS techniques showed that the heterogeneous evolution of crystallites (size, preferred orientation and degree of alignment) could be attributed to crystallographic-orientation-dependent anisotropic dissolution. Hence we propose a novel conceptual schematic diagram to describe the demineralisation process. These findings have important implications for understanding the detailed mechanisms of enamel demineralisation and provide insight into potential enamel remineralisation that could restore structural integrity and function.