Analytische Chemie
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Complex materials (e.g., porous ceramics) need high resolution techniques at multi-scale levels. Microstructure is intimately linked to properties and performance. One technique (or even a few techniques) is not enough. X-ray refraction and CT are very powerful tools. Non-destructive characterisation and quantitative image analysis techniques (2D and 3D) are necessary to understand the anisotropy.
One of the great strengths of X-ray computed tomography over conventional inspection methods (ultrasound, thermography, radiography) is that it can image damage in 3D. However for curved ordeformed composite panels it can be difficult to automatically ascribe the damage to specific plies or inter-ply interfaces. An X-ray computed tomography (CT) data processing methodology is developed to extract the through-thickness distribution of damage in curved or deformed composite panels. The method is applied to [(0°/90°)2]s carbon fibre reinforced polymer (CFRP) panels subjected low velocity impact damage (5 J up to 20 J) providing 3D ply-by-ply damage visualisation and analysis. Our distance transform approach allows slices to be taken that approximately follow the composite curvature allowing the impact damage to be separated, visualised and quantified in 3D on a ply-by-ply basis. In this way the interply delaminations have been mapped, showing characteristic peanut shaped delaminations with the major axis oriented with the fibres in the ply below the interface. This registry to the profile of the panel constitutes a significant improvement in our ability to characterise impact damage in composite laminates and extract relevant measurements from X-ray CT datasets.
The use of novel multi-scale correlative methods, which involve the coordinated characterisation of matter across a range of length scales, are becoming of increasing value to materials scientists. Here, we describe for the first time how a multi-scale correlative approach can be used to investigate the nature of ductile fracture in metals. Specimens of a nuclear pressure vessel steel, SA508 Grade 3, are examined following ductile fracture using medium and high-resolution 3D X-ray computed tomography (CT) analyses, and a site-specific analysis using a dual beam plasma focused ion beam scanning electron microscope (PFIB-SEM). The methods are employed sequentially to characterise damage by void nucleation and growth in one volume of interest, allowing for the imaging of voids that ranged in size from less than 100 nm to over 100 mm. This enables the examination of voids initiated at carbide particles to be detected, as well as the large voids initiated at inclusions. We demonstrate that this multi-scale correlative approach is a powerful tool, which not only enhances our understanding of ductile failure through detailed characterisation of microstructure, but also provides quantitative information about the size, volume fractions and spatial distributions of voids that can be used to inform models of failure. It isfound that the vast majority of large voids nucleated at MnS inclusions, and that the volume of a void varied according to the volume of its initiating inclusion raised to the power 3/2. The most severe voiding was concentrated within 500 mm of the fracture surface, but measurable damage was found to extend to a depth of at least 3 mm. Microvoids associated with carbides (carbide-initiated voids) were found to be concentrated around larger inclusion-initiated voids at depths of at least 400 mm. Methods for quantifying X-ray CT void data are discussed, and a procedure for using this data to calibrate parameters in the Gurson-Tvergaard Needleman (GTN) model for ductile failure is also introduced.
Photon counting detectors (PCD) offer new possibilities for x-ray micro computed tomography (CT) in the field of non-destructive testing. For large and/or dense objects with high atomic numbers the problem of scattered radiation and beam hardening severely influences the image quality. This work shows that using an energy discriminating PCD based on CdTe allows to address these problems by intrinsically reducing both the influence of scattering and beam hardening.
Based on 2D-radiographic measurements it is shown that by energy thresholding the influence of scattered radiation can be reduced by up to in case of a PCD compared to a conventional energy-integrating detector (EID).
To demonstrate the capabilities of a PCD in reducing beam hardening, cupping artefacts are analyzed quantitatively. The PCD results show that the higher the energy threshold is set, the lower the cupping effect emerges. But since numerous beam hardening correction algorithms exist, the results of the PCD are compared to EID results corrected by common techniques. Nevertheless, the highest energy thresholds yield lower cupping artefacts than any of the applied correction algorithms.
As an example of a potential industrial CT application, a turbine blade is investigated by CT. The inner structure of the turbine blade allows for comparing the image quality between PCD and EID in terms of absolute contrast, as well as normalized signal-to-noise and contrast-to-noise ratio. Where the absolute contrast can be improved by raising the energy thresholds of the PCD, it is found that due to lower statistics the normalized contrast-to-noise-ratio could not be improved compared to the EID. These results might change to the contrary when discarding pre-filtering of the x-ray spectra and thus allowing more low-energy photons to reach the detectors.
Despite still being in the early phase in technological progress, PCDs already allow to improve CT image quality compared to conventional detectors in terms of scatter and beam hardening reduction.
Time-dependent in situ measurement of atmospheric corrosion rates of duplex stainless steel wires
(2018)
Corrosion rates of strained grade UNS S32202 (2202) and UNS S32205 (2205) duplex stainless steel wires have been measured, in situ, using time-lapse X-ray computed tomography. Exposures to chloride-containing (MgCl2) atmospheric environments at 50 °C (12–15 M Cl− and pH ~5) with different mechanical elastic and elastic/plastic loads were carried out over a period of 21 months. The corrosion rates for grade 2202 increased over time, showing selective dissolution with shallow corrosion sites, coalescing along the surface of the wire. Corrosion rates of grade 2205 decreased over time, showing both selective and pitting corrosion with more localised attack, growing preferentially in depth. The nucleation of stress corrosion cracking was observed in both wires.
A composite material is a combination of two or more materials with very different mechanical, thermal and electrical properties. The various forms of composite materials, due to their high material properties, are widely used as structural materials in the aviation, space, marine, automobile, and sports industries. However, some defects like voids, delamination, or inhomogeneous fiber distribution that form during the fabricating processes of composites can seriously affect the mechanical properties of the composite material. In this study, several imaging NDE techniques such as: thermography, high frequency eddy current, ultrasonic, x-ray radiography, x-ray laminography, and high resolution x-ray CT were conducted to characterize the microstructure of carbon fiber composites. Then, a 3D analysis was implemented by the destructive technique of serial sectioning for the same sample tested by the NDE methods. To better analyze the results of this work and extract a clear volume image for all features and defects contained in the composite material, an intensive comparison was conducted among hundreds of 3D-NDE and multi serial sections’ scan images showing the microstructure variation.
For the first time, X-ray refraction techniques are proven for the identification of void formation in Ti-6Al-4V parts produced by selective laser melting. The topology and volume fraction of pores are measured in samples produced with different laser energy density. Unique X-ray refraction methods identify different kinds of defects, characteristic to the regions below and above the Optimum laser energy density, namely unprocessed powder (unmolten powder particles, balling effect, and Fusion defects) from empty keyhole pores. Furthermore, it is possible to detect small inhomogeneities (voids or cracks) with sizes below the spatial resolution of optical microscopy and X-ray computed tomography.
During their life cycle, composite structures used in aircraft structures can be subjected to high- and low-velocity impact loading. High velocity impact damage is usually easy to detect as it creates visible external damage. Low-velocity impacts are more complex to assess because, although significant damage can be generated internally, there can be little indication of external damage on the impacted surface, leading to the term BVID. Impact damage, especially barely visible impact damage, is therefore of primary concern for design and maintenance of modern aircraft composite structures. As a result there is a concerted research effort to improve the damage resistance and tolerance of these materials.
One of the great strengths of X-ray computed tomography over conventional inspection methods (ultrasound, thermography, radiography) is that it can image damage in 3D. or inter-ply interfaces. An X-ray computed tomography (CT) data processing methodology is developed to extract the through-thickness distribution of damage in curved or deformed composite panels. The method is applied to [(0°/90°)2]s carbon fibre reinforced polymer (CFRP) panels subjected to low velocity impact damage (5 J up to 20 J) providing 3D ply-by-ply damage visualisation and analysis. Our distance transform approach allows slices to be taken that approximately follow the composite curvature allowing the impact damage to be separated, visualised and quantified in 3D on a ply-by-ply basis. In this way the interply delaminations have been mapped, showing characteristic peanut shaped delaminations with the major axis oriented with the fibres in the ply below the interface. This registry to the profile of the panel constitutes a significant improvement in our ability to characterise impact damage in composite laminates and extract relevant measurements from X-ray CT datasets.
Additive manufacturing (AM) offers an effective solution to the medical sector. It enables the production, on demand, of customised implants which match the patient’s anatomy, with grafts that promote bone growth, as well as surgical guides that help the surgeons.
The objective of this project is to provide a comprehensive basis to enable the safe use of medical AM products with traceable and reliable dimensionalmeasurements. This will guarantee the reliability of medical AM products to notified bodies and facilitate acceptance of AM in the medical sector for a better quality of life.