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Additively manufactured (and in particular laser powder bed fused) materials represent a manyfold challenge for the materials scientist and engineer because of their distinctive microstructure. If laser powder bed fusion is used to produce components, the complexity level increases because meso-structures (e.g., overhanging features, surface and internal defects) gain importance. Furthermore, if the main advantage of additive manufacturing, i.e., the freedom of design, is to be fully exploited, and geometrically complex structures, such as lattices, are manufactured, then such structures become meta-materials. This means that the geometry and the materials properties become equally important.
This matryoshka-like (more literary than the dry “multi-scale”) complexity makes the characterization of the residual stress fields by means of diffraction methods so difficult with the current means, that new paradigms are necessary to tackle the challenge.
Indeed, classic open problems acquire an extra layer of difficulty, such that new solutions need to be found and the sometimes-dormant debate needs to be re-opened. Examples include the determination of: a- the unstrained reference: this reference can become location-dependent and needs to be carefully determined; b- the so-called diffraction elastic constants, which becomes immensely challenging since even the single-crystal elastic constants are not known for additively manufactured materials.
On top of this, other problems arise. The determination of the principal axes of stress becomes non-trivial because the hatching strategy sometimes dominates over the sample geometry. Even further, in complex structures, such as lattices, the textbook statement that the strain measurement in six independent directions uniquely identifies the strain tensor becomes simply invalid. The peculiar surface features of additively manufactured materials transform trivial tasks into formidable challenges: the precise alignment of a specimen in a beam or the determination of surface stresses with laboratory X-rays need to be thoroughly re-discussed and lay far from being routine tasks.
In this paper, we will show a few examples of the cases mentioned above. We will demonstrate that sometimes the classic approach works very well, but other times surprising conclusions can be drawn from in-depth studies of the residual stress in additively manufactured materials. In short, we predicate that classic methods cannot be used on additively manufactured materials and structures without a critical evaluation of their validity and application range.
In this seminar I present the microstructure and micromechanical properties of diesel particulate filter materials, and then particularize them to porous microcracked aluminum titanate.
I show that neutron diffraction is particularly suited for bulk studies, especially under applied load or at high temperatures. The combination of macroscopic and microscopic tests with modeling and simulation yields great added value to understand the mechanics of microcracking.
The effect of porosity and microcracking on the mechanical properties (strength, fracture toughness,Young’s modulus, and fracture energy) and thermal expansion of diesel particulate filter (DPF) gradecordierite materials has been investigated. A method to deconvolute the effect of porosity and microc-racking on Young’s modulus is proposed. In addition, the microcrack density and the pore morphologyfactor are calculated by applying a micromechanical differential scheme. The values of the investigatedmechanical properties are shown to decrease with an increase in porosity, but the thermal expansionvalues are insensitive to porosity. The variation in mechanical properties as a function of porosity leadsto distinct porosity dependence of thermal shock resistance for crack initiation and crack propagationfor DPF grade synthetic cordierite.
3D imaging techniques are very fashionable nowadays, and allow enormous progress in understanding ceramic microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this feature article, we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. While the techniques are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of process parameter influence or simply of microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography.
The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually called ANFO, is extensively used in the mining industry as a bulk industrial explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the porosity of the AN prills. Standardised tests routinely used to assess oil retention face several important limitations; the first being the difficulty to cover the wide range of porosity contents and morphologies from different types of ammonium nitrate prills; the second being the inability to evaluate the closed porosity, which is an important factor regarding the sensitivity of the explosive to detonation. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. XCT can therefore be employed to non-destructively and accurately evaluate and characterise porosity in ammonium nitrate prills.
Porosity in additively manufactured materials, such as laser powder bed fusion Ti-Al6-V4, can play an important role in their mechanical performance. Not only the total porosity but also the shape/morphology of the individual pores need to be considered. Therefore, it is necessary to determine the distributions of different defect types (especially fusing defects and keyhole pores) and their dependence on process parameters. We show that synchrotron X-ray refraction radiography allows analysis of large samples (up to several millimeters) without compromising the detectability of submicrometer defects. Correspondingly, a classification tool is introduced that is able to quantitatively distinguish defects such as keyhole pores and binding defects with a confidence level of 94 %, even when the shape cannot be discerned because of limited spatial resolution.
The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually referred to as ANFO, is extensively used in the mining industry as a bulk explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the complex pore structure of the AN prills. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. Importantly, oil retention measurements (qualifying the efficiency of ANFO as explosives) correlate well with the specific surface area determined by XCT. XCT can therefore be employed non-destructively; it can accurately evaluate and characterise porosity in ammonium nitrate prills, and even predict their efficiency.
Ammonium nitrate (AN) prills are commonly used as an ingredient in industrial explosives and in fertilisers. Conventional techniques (such as BET or mercury intrusion porosimetry) can measure the open porosity and specific surface area of AN prill, but the closed porosity is not obtainable. This work was focused on evaluating X-ray computed tomography (XCT) as a non-destructive technique for the assessment of porosity in AN prills. An advanced data processing workflow was developed so that the segmentation and quantification of the CT data could be performed on the entire 3D volume, yet allowing the measurements (e.g.; volume, area, shape factor…) to be extracted for each individual phase (prill, open porosity, closed porosity) of each individual prill, in order to obtain statistically relevant data. Clear morphological and structural differences were seen and quantified between fertiliser and explosive products. Overall, CT can provide a very wide range of parameters that are not accessible to other techniques, destructive or non-destructive, and thus offers new insights and complementary information.
In this Seminar cycle I will present first diffraction methods to determine residual stress and investigate micromechanical properties of complex materials, and then particularize the treatment with applications to porous microcracked ceramics for diesel particulate filter applications.
I will show that neutron diffraction is particularly suited for bulk studies, where 3D stresses are needed. The advantages to use Time-of-Flight or steady state sources will be discussed, together with the problematic of the determination of absolute RS values.
Finally, the behavior of DPF materials under applied load or at high temperatures will be discussed under the combination of macroscopic and microscopic tests.