Alexander J.G. Lunt

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.

In situ X-ray scattering evaluation of heat-induced ultrastructural changes in dental tissues and synthetic hydroxyapatite.

Human dental tissues consist of inorganic constituents (mainly crystallites of hydroxyapatite, HAp) and organic matrix. In addition, synthetic HAp powders are frequently used in medical and chemical applications. Insights into the ultrastructural alterations of skeletal hard tissues exposed to thermal treatment are crucial for the estimation of temperature of exposure in forensic and archaeological studies. However, at present, only limited data exist on the heat-induced structural alterations of human dental tissues. In this paper, advanced non-destructive small- and wide angle X-ray scattering (SAXS/WAXS) synchrotron techniques were used to investigate the in situ ultrastructural alterations in thermally treated human dental tissues and synthetic HAp powders. The crystallographic properties were probed by WAXS, whereas HAp grain size distribution changes were evaluated by SAXS. The results demonstrate the important role of the organic matrix that binds together the HAp crystallites in responding to heat exposure. This is highlighted by the difference in the thermal behaviour between human dental tissues and synthetic HAp powders. The X-ray analysis results are supported by thermogravimetric analysis. The results concerning the HAp crystalline architecture in natural and synthetic HAp powders provide a reliable basis for deducing the heating history for dental tissues in the forensic and archaeological context, and the foundation for further development and optimization of biomimetic material design.

Hierarchical modelling of in situ elastic deformation of human enamel based on photoelastic and diffraction analysis of stresses and strains

Human enamel is a typical hierarchical mineralized tissue with a two-level composite structure. To date, few studies have focused on how the mechanical behaviour of this tissue is affected by both the rod orientation at the microscale and the preferred orientation of mineral crystallites at the nanoscale. In this study, wide-angle X-ray scattering was used to determine the internal lattice strain response of human enamel samples (with differing rod directions) as a function of in situ uniaxial compressive loading. Quantitative stress distribution evaluation in the birefringent mounting epoxy was performed in parallel using photoelastic techniques. The resulting experimental data was analysed using an advanced multiscale Eshelby inclusion model that takes into account the two-level hierarchical structure of human enamel, and reflects the differing rod directions and orientation distributions of hydroxyapatite crystals. The achieved satisfactory agreement between the model and the experimental data, in terms of the values of multidirectional strain components under the action of differently orientated loads, suggests that the multiscale approach captures reasonably successfully the structure-property relationship between the hierarchical architecture of human enamel and its response to the applied forces. This novel and systematic approach can be used to improve the interpretation of the mechanical properties of enamel, as well as of the textured hierarchical biomaterials in general.

Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

Understanding nature's residual strain engineering at the human dentine-enamel junction interface.

UNLABELLED Human dental tissue is a hydrated biological mineral composite. In terms of volume and mass, a human tooth mainly consists of dentine and enamel. Human dental tissues have a hierarchical structure and versatile mechanical properties. The dentine enamel junction (DEJ) is an important biological interface that provides a durable bond between enamel and dentine that is a life-long success story: while intact and free from disease, this interface does not fail despite the harsh thermo-mechanical loading in the oral cavity. The underlying reasons for such remarkable strength and durability are still not fully clear from the structural and mechanical perspectives. One possibility is that, in an example of residual stress engineering, evolution has led to the formation of a layer of inelastic strain adjacent to the DEJ during odontogenesis (tooth formation). However, due to significant experimental and interpretational challenges, no meaningful quantification of residual stress in the vicinity of the DEJ at the appropriate spatial resolution has been reported to date. In this study, we applied a recently developed flexible and versatile method for measuring the residual elastic strain at (sub)micron-scale utilising focused ion beam (FIB) milling with digital image correlation (DIC). We report the results that span the transition from human dentine to enamel, and incorporate the material lying at and in the vicinity of the DEJ. The capability of observing the association between internal architecture and the residual elastic strain state at the micrometre scale is useful for understanding the remarkable performance of the DEJ and may help the creation of improved biomimetic materials for clinical and engineering applications. STATEMENT OF SIGNIFICANCE We studied the micron-scale residual stresses that exist within human teeth, between enamel (outer tooth shell, hardest substance in the human body) and dentine (soft bone-like vascularised tooth core). The dentine-enamel junction (DEJ) is an extremely interesting example of natures design in terms of hierarchical structuring and residual stress management. Key developments reported are systematic focused ion beam (FIB) milling and digital image correlation (DIC) micrometre scale residual strain evaluation, and the determination of principal strain direction near DEJ, correlated with internal architecture responsible for remarkable strength. This work helps understanding DEJ performance and improving biomimetic materials design for clinical and engineering applications.

Microscale resolution fracture toughness profiling at the zirconia-porcelain interface in dental prostheses

The high failure rate of the Yttria Partially Stabilized Zirconia (YPSZ)-porcelain interface in dental prostheses is influenced by the micro-scale mechanical property variation in this region. To improve the understanding of this behavior, micro-scale fracture toughness profiling by nanoindentation micropillar splitting is reported for the first time. Sixty 5 μm diameter micropillars were machined within the first 100 μm of the interface. Berkovich nanoindentation provided estimates of the bulk fracture toughness of YPSZ and porcelain that matched the literature values closely. However, the large included tip angle prevented precise alignment of indenter with the pillar center. Cube corner indentation was performed on the remainder of the pillars and calibration between nanoindentation using different tip shapes was used to determine the associated conversion factors. YPSZ micropillars failed by gradual crack propagation and bulk values persisted to within 15 μm from the interface, beyond which scatter increased and a 10% increase in fracture toughness was observed that may be associated with grain size variation at this location. Micropillars straddling the interface displayed preferential fracture within porcelain parallel to the interface at a location where nano-voiding has previously been observed and reported. Pure porcelain micropillars exhibited highly brittle failure and a large reduction of fracture toughness (by up to ~90%) within the first 50 μm of the interface. These new insights constitute a major advance in understanding the structure-property relationship of this important bi-material interface at the micro-scale, and will improve micromechanical modelling needed to optimize current manufacturing routes and reduce failure.

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.

Characterisation of nanovoiding in dental porcelain using small angle neutron scattering and transmission electron microscopy

OBJECTIVES Recent studies of the yttria partially stabilised zirconia-porcelain interface have revealed the presence of near-interface porcelain nanovoiding which reduces toughness and leads to component failure. One potential explanation for these nanoscale features is thermal creep which is induced by the combination of the residual stresses at the interface and sintering temperatures applied during manufacture. The present study provides improved understanding of this important phenomenon. METHODS Transmission electron microscopy and small angle neutron scattering were applied to a sample which was crept at 750°C and 100MPa (sample C), a second which was exposed to an identical heat treatment schedule in the absence of applied stress (sample H), and a reference sample in the as-machined state (sample A). RESULTS The complementary insights provided by the two techniques were in good agreement and log-normal void size distributions were found in all samples. The void number density was found to be 1.61μm-2, 25.4μm-2 and 98.6μm-2 in samples A, H and C respectively. The average void diameter in sample A (27.1nm) was found to be more than twice as large as in samples H (10.2nm) and C (11.6nm). The crept data showed the highest skewness parameter (2.35), indicating stress-induced growth of larger voids and void coalescence that has not been previously observed. SIGNIFICANCE The improved insight presented in this study can be integrated into existing models of dental prostheses in order to optimise manufacturing routes and thereby reduce the significant detrimental impact of this nanostructural phenomenon.