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Eingeladener Vortrag
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Determination of short carbon fiber orientation in zirconium diboride ceramic matrix composites
(2024)
In fiber-reinforced components, the fiber alignment and orientation have paramount influence on the thermomechanical properties of the resulting composite, for both short and continuous fiber. Here we present the case of an ultra-refractory matrix intended for extreme environment applications, ZrB2, reinforced with 20 vol% and 50 vol% short carbon fibers. In both cases, fibers tend to align perpendicular to the uniaxial pressure applied during shaping and sintering of a pellet, although the fiber tilt across the pellet thickness is difficult to determine. Moreover, for high volume fractions of reinforcement, the spatial distribution of the fibers is heterogeneous and tends to have domains of preferential orientations. We compare the information on the fiber distribution as collected by scanning electron microscopy images, X-ray computed tomography and synchrotron X-ray refraction radiography (SXRR). The three techniques prove to be complementary. Importantly, we demonstrate that SXRR yields the most statistically significant information due to the largest field of view, yet with a sensitivity down to the nanometer, and that can be successfully applied also to heavy matrix materials, such as zirconium boride.
AbstractIn this study, we compare the residual stress state in a laser powder bed fusion (PBF‐LB/M) AlSi10Mg alloy in the as‐built (AB) condition with that after two different heat treatments (265 °C for 1 h, HT1; and 300 °C for 2 h, HT2). The bulk residual stress (RS) is determined using synchrotron X‐ray diffraction (SXRD), and near‐surface profiles are determined using laboratory energy‐dispersive X‐ray diffraction (EDXRD). The EDXRD results do not reveal any notable difference between the conditions at a depth of 350 μm, suggesting that the machining process yields a comparable residual stress state in the near‐surface regions. On the other hand, the SXRD results show that HT1 is more effective in relieving the bulk RS. It is observed that HT1 reduces the RS state in both the aluminium matrix and the silicon network. In addtion, HT2 does not have a significant impact on relaxing the RS as‐built state of the matrix, although it does induce a reduction in the RS magnitudes of the Si phase. It is concluded that the heat treatment stress relieving is effective as long as the Si‐network is not disaggregated.
A new titanium alloy improving the operation of implants additively manufactured and including laterally closed lattice structures is proposed. The new alloy possesses an increased affinity to the bone. The measured bone–interface implant (BII) of less than 10 mm and bone–implant contact (BIC) of 95% demonstrated an excellent osseointegration. Furthermore, since additive manufacturing naturally leads to a high-roughness surface finish, the wettability of the implant is increased. The combination of these factors is pushing ossification beyond its natural limits. In addition, the quality and speed of the ossification and osseointegration in/around laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required.
Powder Bed Fusion – Laser Beam (PBF-LB) of high γ’ strengthened Ni-base superalloys, such as CM247LC, is of great interest for high temperature applications in gas turbines. However, PBF-LB of CM247LC is challenging due to the high cracking susceptibility during PBF-LB processing (solidification cracking) and heat treatment (strain age cracking, mostly caused by residual stresses). This study focuses on understanding the impact of process parameters on microstructure, residual stresses and solidification cracking. Laser power (P), speed (v) and hatch spacing (h) were varied while the layer thickness (t) was fixed. The melt pool size and shape were found to be key factors in minimizing solidification cracking. Narrower and shallower melt pools, achieved using a low line energy density (LED = P/v ≤ 0.1 J/mm), gave low crack densities (0.7 mm/mm2). A tight hatch spacing (h = 0.03 mm) resulted in reduced lack of fusion porosity. Electron backscatter diffraction investigations revealed that parameters giving finer microstructure with 〈100〉crystallographic texture had low crack densities provided they were processed with a low LED. Atom probe tomography elucidated early stages of spinodal decomposition in the as-built condition, where Cr and Al cluster separately. The extent of spinodal decomposition was found to be affected by the LED and the hatch spacing. Samples with low LED and small hatch spacing showed higher degrees of spinodal decomposition. X-ray diffraction residual stress investigations revealed that the residual stress is proportional to the volumetric energy density (VED = P/(v. h. t)). Although low residual stresses can be achieved by using low VED, there is a high risk of lack of fusion. Hence, other parameters such as modified scan strategy, build plate pre-heating and pulsed laser mode, must be further explored to minimize the residual stresses to reduce the strain age cracking susceptibility.
Efficient density evolution during sintering of the as-printed component is vital to reach full densification and required properties of binder jet (BJT) components. However, due to the high porosity and brittle nature of the green compact, analysis of the microstructure development during sintering is very difficult, resulting in lack of understanding of the densification process. Density development from green state (57 ± 1.6 %) up to full density (99 ± 0.3 %) was characterized by high-resolution synchrotron X-Ray computed tomography (SXCT) on BJT 316L samples from ex-situ interrupted sintering tests. Periodicity of density fluctuations along the building direction was revealed for the first time and was related to the layer thickness of ~ 42 μm during printing that decreased down to ~ 33 μm during sintering. Sintering simulations, utilizing a continuum sintering model developed for BJT, allowed to replicate the density evolution during sintering with a mean error of 2 % and its fluctuation evolution from green (1.66 %) to sintered (0.56 %) state. Additionally, simulation of extreme particle size segregation (1 μm to 130 μm) suggested that non-optimized printing could lead to undesirable density fluctuation amplitude rapid increase (~10 %) during sintering. This might trigger the nucleation of defects (e.g., layer delamination, cracking, or excessive residual porosity) during the sintering process.
Large temperature gradients inherent to additive manufacturing (AM) processes induce large residual stress (RS) in the final part. Because RS can influence the tribological properties, this study focuses on the relationship between wear sliding properties and RS in IN718 coatings. Such coatings were deposited with a Laser metal deposition (LMD) machine using two different scanning strategies.
The wear resistance and RS state were investigated after surface milling. RS were measured before and after wear tests on a reciprocating sliding test apparatus.
Two different X-ray diffraction techniques were employed to measure the surface and subsurface state RS: Laboratory Energy Dispersive X-ray Diffraction (LEDXD) and Synchrotron X-ray Energy Dispersive Diffraction (SXEDD). Due to the milling process, the coatings show similar depth distributions of RS from 22 to 92 μm depth, but exhibit different magnitudes depending on the scanning strategy used. Reciprocating sliding wear tests induced high compressive residual stresses that erased the initial RS state, and a similar wear behavior was observed in the two samples. These samples possess similar texture and grain morphology. This demonstrates that the influence of RS on wear resistance is a second-order effect. Nevertheless, it was observed that RS can still impact the wear performance at the early testing stages of the repaired parts.
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). Also, two successful research project in collaboration with CAM2, Sweden are presented.
In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate.
Electron backscatter diffraction (EBSD) images of extruded pure aluminum were statistically analyzed to investigate creep-induced subgrain structures after applying two different levels of creep stress, corresponding to the power law (PL) and power-law breakdown (PLB) regimes. Kernel average misorientation analysis of EBSD measurements revealed 2D morphologies, which were subdivided by a multi-step segmentation procedure into subgranular arrangements. Various descriptors were employed to characterize the “subgrains” quantitatively, including their size, shape, spatial arrangement, and crystallographic orientation. In particular, the analysis of the orientations of subgrains was conducted by neglecting rotations around the loading axis. This approach facilitated the individual investigation of the {001} and {111} subgrain families with respect to the loading axis for two investigated stress levels plus a reference specimen. For the PL regime, the statistical analysis of subgrain descriptors computed from segmented image data revealed a similar degree of strain accumulation for {111} and {001} subgrains. In contrast, for the PLB regime, the analyzed descriptors indicate that {111} subgrains tend to accumulate significantly more strain than {001} ones. These observations suggest that the mechanisms leading to PLB may be associated with strain localization dependent on intergranular stress, hindering the recovery process within {111} grains.