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X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, they can detect objects with size above a few wavelengths of the radiation.
Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads.
The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models.
We hereby show the application of non-destructive X-ray refraction radiography (SXRR, 2D mapping also called topography) to problems in additive manufacturing:
1) Porosity analysis in PBF-LM-Ti64. Through the use of SXRR, we could not only map the (very sparse) porosity distribution between the layers and quantify it, but also classify, and thereby separate, the filled porosity (unmolten powder) from the keyhole and gas pores (Figure 1).
2) In-situ heat treatment of laser powder bed fusion PBF-LM-AlSi10Mg to monitor microstructure and porosity evolution as a function of temperature (Figure 2). By means of SXRR we indirectly observed the initial eutectic Si network break down into larger particles as a function of increasing temperature. We also could detect the thermally induced porosity (TIP). Such changes in the Si-phase morphology upon heating is currently only possible using scanning electron microscopy, but with a much smaller field-of-view. SXRR also allows observing the growth of some individual pores, usually studied via X-ray computed tomography, but again on much smaller fields-of-view.
Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the defect distribution and the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
Additively manufactured (AM) triply periodic metallic minimum surface structures (TPMSS, from the English Triply Periodic Minimum Surface Structures) fulfill several requirements in both biomedical and engineering fields: tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some quality control challenges that may prevent their successful application. In fact, optimization of the AM process is impossible without considering structural features such as manufacturing accuracy, internal defects, and surface topography and roughness. In this study, quantitative nondestructive analysis of Ti-6Al-4V alloy TPMSS was performed using X-ray computed tomography (XCT). Several new image analysis workflows are presented to evaluate the effects of buildup direction on wall thickness distribution, wall degradation, and surface roughness reduction due to chemical etching of TPMSS. It is shown that the fabrication accuracy is different for the structural elements printed parallel and orthogonal to the fabricated layers. Different strategies for chemical etching showed different powder removal capabilities and thus a gradient in wall thickness. This affected the mechanical performance under compression by reducing the yield stress. A positive effect of chemical etching is the reduction of surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of powder retained with the pore size of the TPMSS, which can further improve the manufacturing process.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The challenges in the residual stress analysis of AM components are discussed on the basis on the show studies performed in BAM. Also, the synchrotron X-ray refraction technique, available in BAM, is presented, showing example of in-situ heating test of Al10SiMg AM material.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
An unusual microstructure, inherent residual stresses and void formation are the three key aspects to control when assessing metallic parts made by LPBF. This talk explains an experiment to unravel the interlinked influence of the two mechanisms for the formation of residual stresses in LPBF: the temperature gradient mechanism and constricted solidification shrinkage. The impact of each mechanism on the shape and magnitudes of the residual stress distribution is described. Combined results from neutron diffraction, X-ray diffraction, computed tomography and in-situ thermography are presented.
Also, influence of scan strategies as well as surface roughness of subjacent layers on void formation is shown. Results from computed tomography and in-situ thermography of a specimen dedicated to study the interaction of the melt pool with layers of powder underneath the currently illuminated surface are presented.
Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated.
Prior to Low Cycle Fatigue (LCF) tests at operating temperature (300°C), the microstructure (phases, crystallographic texture, and grain morphology), the mesostructure (defect shape and distribution), and subsurface RS on the LCF samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance.
To see and not to see - Möglichkeiten und Grenzen der Schadensanalyse mit CT an Kompositmaterialien
(2020)
Anhand von drei Beispielen (Datenfusion an CFK; Machine Learning an Metall-Matrix-Kompositen sowie Refraktion an CFK) wird gezeigt, wie die BAM mit neuen Analysemethoden mehr Informationen aus CT-Datensätzen extrahieren kann, sowie mit der Refraktion eine Analysemethode besitzt, die in Fällen eingesetzt werden kann, bei denen klassische Durchstrahlungsmethoden kein Ergebnis liefern.
Aluminum alloys are extensively used in the automotive industry. Particularly, squeeze casting production of Al-Si alloys is employed in the conception of metal matrix composites (MMC) for combustion engines. Such materials are of a high interest since they allow combining improved mechanical properties and reduced weight and hence improve efficiency. We investigate two types of MMCs, which can be potentially used for production of combustion engine pistons: 1) a near-eutectic cast AlSi12CuMgNi alloy reinforced with 15%vol. Al2O3 random planar oriented short fibers and 2) the same alloy reinforced with 7%vol. Al2O3 random planar oriented short fibers + 15%vol. SiC particles.
Complex 3D microstructure of the samples in as-cast condition, consisting of four and five phases (Al matrix, eutectic Si, intermetallics, Al2O3 fibers and SiC particles) was investigated by synchrotron computed tomography (CT). Advanced methods based on machine learning were applied for segmentation of all phases. This allowed extracting quantitative information such as volume fraction, shape and interconnectivity of every phase.
In-situ compression tests during neutron diffraction experiments were used to track the load transfer among phases, while CT on pre-strained samples to monitor and quantify damage. A micromechanical model was developed to simulate the evolution of the internal stress of each phase during uniaxial compression. We showed that in composites with the Al2O3 fiber mat plane perpendicular to the load axis the Al-alloy matrix presents a large hydrostatic stress component, i.e. undergoes compression also in the direction transverse to the external load. This feature holds with and without the addition of SiC ceramic reinforcement and is absent in the case when the Al2O3 fiber mat plane is parallel to the load axis. We show, that the intermetallics play a decisive role at very high loads, when all other reinforcement phases suffer (extensive) damage. The addition of SiC particles does alleviate the load on the Al2O3 fibers, on the eutectic Si, and on the intermetallic phases in both cases of parallel and orthogonal (to the load axis) Al2O3 fiber orientation. Apart from the beneficial addition of ceramic reinforcement, the presence of intermetallic phase and eutectic silicon, forming an interconnected network even at high loads, when single particles break, confers peculiar properties to these multi-phase composites.
The material and damage behaviour of additively manufactured polyamide 12 (PA12) under dynamic loading was characterized by cyclic tests and microstructure analysis. The results were used to develop a numerical material and damage model. In a recent study, it was shown that the material and damage behaviour of 3D printed PA12 under quasistatic loading is simulated in a realistic way by coupling the
material model by Chaboche and the damage model by Gurson-Tvergaard-Needleman (GTN).
Using microscopy, X-ray refraction, and computed tomography, a porosity of about 5% was evaluated. These results served as a starting point for the present work. For the dynamic load, both the previously used Chaboche model and the GTN model were extended. Furthermore, the temperature was measured during the experiment and the self-heating effect was observed. Therefore, a temperaturedependent material parameters for the simulation were introduced. Considering the results of mechanical experiments, microstructural investigations, and self-heating effects, a good agreement between Experiment and numerical simulation could be achieved.
Nominal-actual comparisons are routinely performed to compare a manufactured specimen to a reference specimen. X-ray Computed Tomography (CT) has brought a profound change in the way that tolerance verifications are performed in industry, by allowing the inner and outer geometries of an object to be measured, without the need for external access or destructive testing. As a results, CT is increasingly used in additive manufacturing applications, where a nominal-actual comparison performed between the digital model (CAD file), used as an input for the 3D printer, and the CT volume from the printed part, can provide invaluable information as to the accuracy of the printing process. However, the nominal-actual comparison process is somewhat different when applied to additively manufactured specimens by comparison to conventionally manufactured specimens.
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 or deformed 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.
Im Fokus dieser Arbeit steht die computertomographische (CT) Untersuchung (Synchrotron- und Labor-CT) von IN625-Pulver und den daraus gefertigten Streben, welche wiederum zu Gitterstrukturen zusammengesetzt werden. Aufgrund der Filigranität wurde zur Fertigung dieser Proben das pulverbettbasierte selektive Laserschmelzen verwendet.
Porositätsanalysen und Größenverteilungen wurden für das Pulver bei einer rekonstruierten Voxelgröße von 0,5µm ermittelt. 6,0mm lange Streben variierten im Aufbauwinkel von 30° bis 90° zur Bauplattform und zeigten so den Unterschied zwischen Up- und Down-Skin hinsichtlich der Rauigkeit und Porenverteilung. Die Gitterstrukturen konnten in-situ mit bis zu 5,0kN belastet werden, um deren Verformung computertomographisch zu erfassen.
Near eutectic cast Al–Si alloys are the basis of all Al-alloys used for pistons due to their high fluidity and relatively high strength-to-weight ratio. Their microstructure is characterized by the presence of eutectic-Si embedded in an age hardenable -Al matrix. During solution heat treatment, the eutectic Si network undergoes a process of gradual disintegration, reducing the load bearing capability and the strength of the alloy. The improvement of the high temperature strength is achieved by addition of transition elements such as Cu, Mg or Ni through the formation of stiff intermetallic (IM) phases.
In present study a near-eutectic AlSi12CuMgNi alloy produced by squeeze casting was investigated in as-cast condition. The in-situ neutron diffraction compression tests revealed the stress partitioning mechanism between phases of the alloy. Large stresses were found in IMs, showing their significant role as a reinforcement elements. After the failure of IM and Si phases the load is transferred back to the Al matrix, inducing further plastic deformation in it, yet without creating microcracking. The neutron diffraction experiments were coupled with assessment of internal damage after ex-situ compression tests by synchrotron radiation computed tomography. The quantitative analysis of CT data revealed that local tensile stresses in IM and Si phases induce microcracks with preferential orientation, parallel to the axis of applied load.
Altogether, present experimental data was used as an input for the developed micromechanical model based on Maxwell homogenization scheme. In contrast to the neutron diffraction experiment, which can only determine stress differences between the axial and radial sample directions, the model allows predicting the principal stresses in each phase of the alloy.
We investigated lattice structure manufactured by laser beam melting with computed tomography on difference scales, such as powder scale, strut scale and lattice scale.
The raw powder has been evaluated by means of synchrotron computed tomography (CT) at the BAM-Line (HZB Bessy II, Berlin). Therefore, the particle size distribution and even the pore size distribution was investigated and compared with results received by the producer by means of sieving. Studies with laboratory X-ray CT of porosity and roughness of manufactured struts in dependence of the build angle exhibited the tendency that elongated pores appear solely in a certain range near the edge. The integrity and load-bearing capacity of a lattice structure was investigated by means of in-situ CT during compression. The lattice structure was compressed by 10 % in height with an applied maximum force of 5 kN. We applied digital volume correlation algorithm on volumes of different load steps to quantifies the displacement within the structure.
Synchrotron X-ray diffraction is a powerful non-destructive technique for the analysis of the material stress-state. High cooling rates and heterogeneous temperature distributions during additive manufacturing lead to high residual stresses. These high residual stresses play a crucial role in the ability to achieve complex geometries with accuracy since they can promote distortion of parts during manufacturing. Furthermore, residual stresses are critical for the mechanical performance of parts in terms of durability and safety.
In the present study, Ti-6Al-4V bridge-like specimens were manufactured additively by selective laser melting (SLM) under different laser scanning speed conditions in order to compare the effect of process energy density on the residual stress state. Subsurface residual stress analysis was conducted by means of synchrotron X-ray diffraction in energy dispersive mode for three conditions: as-built on base plate, released from base plate, and after heat treatment on the base plate. The quantitative residual stress characterization shows a correlation with the qualitative bridge curvature method. Computed tomography (CT) was carried out to ensure that no stress relief took place owing to the presence of porosity. CT allows obtaining spatial and size pores distribution which helps in optimization of the SLM process.
High tensile residual stresses were found at the lateral surface for samples in the as-built conditions. We observed that higher laser energy density during fabrication leads to lower residual stresses. Samples in released condition showed redistribution of the stresses due to distortion.
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.
Defect recognition in CFRP components using various NDT methods within a smart manufacturing process
(2017)
The manufacturing process of carbon fiber reinforced polymer (CFRP) components is playing a more and more significant role when looking at the increasing amount of CFRPs used in industries today. The monitoring of the manufacturing process and hence the reliability of the manufactured products, is one of the major challenges we need to face in the near future. Common defects which arise during manufacturing are e.g. porosity and voids which may lead to delaminations during operation and under load. To find those defects in an early stage of the manufacturing process is of huge importance for the safety and reliability of the finished products, as well as of significant impact from an economical point of view. In this study we present various NDT methods which are applied to similar CFRP laminate samples in order to detect and characterize defective volume. Besides ultrasound, thermography and eddy current, different x-ray methods like radiography, laminography and computed tomography are used to investigate the samples. These methods are compared with the intention to evaluate their capability to reliably detect and characterize defective volume. Beyond the detection of flaws, we also investigate possibilities to combine various NDT methods within a smart manufacturing process in which the decision which method to apply is made by the process itself. Is it possible to design an in-line or at-line testing process which can recognize defects reliably and reduce testing time and costs? This study aims to show up opportunities of designing a smart NDT process synchronized to the production based on the ideas of smart production (Industry 4.0). A set of defective CFRP laminate samples and different NDT methods were used to demonstrate how effective defects are recognized and how communication between interconnected NDT sensors and the manufacturing process could be organized.
The evolution of the microstructure of multiphase metal matrix composite AlSi12CuNiMg with 7% vol. Al2O3 + 15% vol. SiC (short fibers and whiskers, respectively) was studied by synchrotron computed tomography. It comprehended as cast and after heat treatment conditions, as well as damage evaluation after ex-situ compression tests at room temperature. The volume fraction of different phases, their distribution, their orientation, and damage events are studied.
The influence on mechanical properties of the orientation of the planar random short fibres Al2O3 towards loading was investigated. Phase-specific load partition analysis for samples with fiber plane parallel and orthogonal to load, respectively, was performed by means of neutron diffraction (ND) during in-situ compression tests at room temperature. ND results proved that damage occurrence in the fillers strongly depends on the preferential orientation of those, playing a crucial role in the failure of the sample. The computed tomography observations confirm the damage observations from curves of load partition analysis of each phase.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component 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. This logic thread equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load.
The reinforcement of concrete with polymer fibers provides resistance to crack formation. The orientation distribution of these fibers has a significant influence on the mechanical behavior of the material. To optimize material performance, micromechanical models that are capable of making accurate predictions of the mechanical behavior of composite materials are needed. These models must be calibrated using experimental results from microstructural characterization. For the fiber orientation distribution analysis in the present study, computed tomography (CT) data were used to evaluate the properties of a fiber-reinforced cement mortar. The results have indicated that the fibers in this material have highly anisotropic orientation characteristics and that there is a clear tendency for the polymer fibers to agglomerate during mixing and casting. The incorporation of this experimental data into micromechanical models will increase the accuracy of those models for material simulation and optimization.
Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network.