TY - JOUR A1 - Kupsch, Andreas A1 - Laquai, René A1 - Müller, Bernd R. A1 - Paciornik, S. A1 - Horvath, J. A1 - Tushtev, K. A1 - Rezwan, K. A1 - Bruno, Giovanni T1 - Evolution of Damage in All-Oxide Ceramic Matrix Composite After Cyclic Loading N2 - While structural ceramics usually display a brittle mechanical behavior, their composites may show nonlinearities, mostly due to microcracking. Herein, the stiffness evolution of a sandwich-like laminate of an Al2O3 15%vol. ZrO2 matrix reinforced with Nextel 610 fibers is studied as a function of number of cycles N in tension. The stiffness of the composite degrades with increasing N, indicating microcracking. However, synchrotron X-ray refraction radiography shows that the internal specific surface of such cracks varies differently. A modeling strategy is developed for the calculation of the equivalent stiffness of mixtures (first the matrix and then the sandwich), based on the Voigt and Reuß schemes. The Bruno–Kachanov model is then used to estimate the initial microcrack density in the matrix (due to the thermal expansion mismatch) and the amount of microcracking increase upon cyclic loading. The stiffness in the composite degrades dramatically already after 20 000 cycles but then remains nearly constant. The combination of mechanical testing, quantitative imaging analysis, and modeling provides insights into the damage mechanisms acting: microcrack propagation is more active than microcrack initiation upon cyclic loading, but the second also occurs. This scenario is similar but not equal to previous results on porous and microcracked ceramics. KW - Ceramic matrix composites KW - Homogenization schemes KW - Microcracking KW - Nonlinear behavior KW - Synchrotron X-ray refraction radiography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534541 DO - https://doi.org/10.1002/adem.202100763 SN - 1527-2648 SN - 1438-1656 VL - 24 IS - 6 SP - 2100763 -1 EP - 2100763 -13 PB - VCH GmbH CY - Weinheim AN - OPUS4-53454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauzon, C. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Dubiez-Le Goff, S. A1 - Murugesan, S. A1 - Bruno, Giovanni A1 - Hryha, E. T1 - Residual stresses and porosity in Ti-6Al-4V produced by laser powder bed fusion as a function of process atmosphere and component design N2 - The influence of the process gas, laser scan speed, and sample thickness on the build-up of residual stresses and porosity in Ti-6Al-4V produced by laser powder bed fusion was studied. Pure argon and helium, as well as a mixture of those (30% helium), were employed to establish process atmospheres with a low residual Oxygen content of 100 ppm O2. The results highlight that the subsurface residual stresses measured by X-ray diffraction were significantly lower in the thin samples (220 MPa) than in the cuboid samples (645 MPa). This difference was attributed to the shorter laser vector length, resulting in heat accumulation and thus in-situ stress relief. The addition of helium to the process gas did not introduce additional subsurface residual stresses in the simple geometries, even for the increased scanning speed. Finally, larger deflection was found in the cantilever built under helium (after removal from the baseplate), than in those produced under argon and an argon-helium mixture. This result demonstrates that complex designs involving large scanned areas could be subjected to higher residual stress when manufactured under helium due to the gas’s high thermal conductivity, heat capacity, and thermal diffusivity. KW - Additive manufacturing KW - Ti-6Al-4V KW - Residual stress KW - Process atmosphere KW - Helium PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534209 DO - https://doi.org/10.1016/j.addma.2021.102340 VL - 47 SP - 2340 PB - Elsevier B.V. AN - OPUS4-53420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritsch, Tobias A1 - Farahbod-Sternahl, L. A1 - Serrano-Munoz, Itziar A1 - Léonard, F. A1 - Haberland, C. A1 - Bruno, Giovanni T1 - 3D Computed Tomography Quantifies the Dependence of Bulk Porosity, Surface Roughness, and Re-Entrant Features on Build Angle in Additively Manufactured IN625 Lattice Struts N2 - Layer-by-layer additive manufacturing (AM) by means of laser-powder bed Fusion (L-PBF) offers many prospects regarding the design of lattice structures used, for example, in gas turbines. However, defects such as bulk porosity, Surface roughness, and re-entrant features are exacerbated in nonvertical structures, such as tilted struts. The characterization and quantification of these kinds of defects are essential for the correct estimation of fracture and fatigue properties. Herein, cylindrical struts fabricated by L-PBF are investigated by means of X-ray computed tomography (XCT), with the aim of casting light on the dependence of the three kinds of defects (bulk porosity, surface roughness, and re-entrant features) on the build angle. Innovative analysis methods are proposed to correlate shape and position of pores, to determine the angular-resolved Surface roughness, and to quantify the amount of re-entrant surface features, q. A meshing of the XCT surface enables the correlation of q with the classical Surface roughness Pa. This analysis leads to the conclusion that there is a linear correlation between q and Pa. However, it is conjectured that there must be a threshold of surface roughness, below which no re-entrant features can be build. KW - Additive manufacturing KW - Laser powder bed fusion KW - Computed tomography KW - Surface roughness analysis KW - Re-entrant surface feature PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534728 DO - https://doi.org/10.1002/adem.202100689 IS - 2100689 SP - 1 EP - 8 PB - Wiley-VCH Verlag AN - OPUS4-53472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Serrano-Munoz, Itziar A1 - Evans, Alexander A1 - Mishurova, Tatiana A1 - Sprengel, Maximilian A1 - Pirling, T. A1 - Kromm, Arne A1 - Bruno, Giovanni T1 - The importance of subsurface residual stress in laser powder bed fusion IN718 N2 - The residual stress (RS) in laser powder bed fusion (LPBF) IN718 alloy samples produced using a 67°-rotation scan strategy is investigated via laboratory X-ray diffraction (XRD) and neutron diffraction (ND). The location dependence of the strain-free (d₀) lattice spacing in ND is evaluated using a grid array of coupons extracted from the far-edge of the investigated specimen. No compositional spatial variation is observed in the grid array. The calculated RS fields show considerable non-uniformity, significant stress gradients in the region from 0.6 to 2 mm below the surface, as well as subsurface maxima that cannot be accounted for via XRD. It is concluded that failure to determine such maxima would hamper a quantitative determination of RS fields by means of the stress balance method. KW - Laser powder bed fusion KW - Neutron and X-ray diffraction KW - Residual stress analysis KW - Strain-free lattice references KW - Stress balance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532707 DO - https://doi.org/10.1002/adem.202100895 SN - 1615-7508 SN - 1527-2648 VL - 24 IS - 6 SP - 1 EP - 7 PB - Wiley-VCH CY - Weinheim AN - OPUS4-53270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - Separation of the impact of residual stress and microstructure on the fatigue performance of LPBF Ti-6Al-4V at elevated temperature (Keynote) N2 - 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 fatigue tests at elevated temperature, the microstructure, the mesostructure, and subsurface RS on the fatigue 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. T2 - EUROMAT 2021 CY - Online meeting DA - 12.09.2021 KW - Additive manufacturing KW - Ti-6Al-4V KW - Residual stress KW - Fatigue performance PY - 2021 AN - OPUS4-53278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Micromechanics of internal stresses in multiphase materials Part I- Residual Stress analysis by Diffraction N2 - 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. T2 - ATHOR webinar "Micromechanics of internal stresses in multiphase materials" CY - Online meeting DA - 12.01.2021 KW - Porosity KW - Neutron Diffraction KW - Residual Stress KW - Non-linear stress-strain KW - Anisotropy KW - Microcracking KW - Imaging PY - 2021 AN - OPUS4-52125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Mishurova, Tatiana A1 - Fritsch, Tobias A1 - Serrano-Munoz, Itziar A1 - Evans, Alexander A1 - Sprengel, Maximilian A1 - Klaus, M. A1 - Genzel, C. A1 - Schneider, J. A1 - Bruno, Giovanni T1 - On the influence of heat treatment on microstructure and mechanical behavior of laser powder bed fused Inconel 718 N2 - A range of heat treatments have been developed for wrought Inconel 718 to obtain desired properties. For additively manufactured Inconel 718, the recently developed standard ASTM F3301 provides guidance for heat treatment of powder bed fusion specimens. Although this standard is based on standards developed for wrought Inconel 718, it does not include direct aging. Since direct aging reduces the number of processing steps, it can result in a post processing cost reduction if the desired properties are obtained. In this study, we characterized the microstructure and tensile behavior of Inconel 718 specimens produced by a laser powder bed fusion process. The specimens were heat treated according to two different routines after stress relieving: a full heat Treatment versus a one-step direct aging process. Differences in the resulting texture and grain morphology were observed. The ex-situ stress-strain behavior was broadly similar. However, a slight increase in yield strength was observed for the direct aged specimen. In order to understand this behavior, investigations with in-situ synchrotron Energy dispersive X-ray diffraction tensile testing revealed differences in the load partitioning among different Crystal directions. Importantly, the elastic anisotropy expressed by the magnitude of the diffraction elastic constants showed a dependency on the microstructures. KW - Electron microscopy KW - X-ray analysis KW - Inconel 718 KW - Additive Manufacturing KW - Mechanical behavior KW - Diffraction elastic constants PY - 2021 DO - https://doi.org/10.1016/j.msea.2020.140555 VL - 805 SP - 40555 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-52142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Artzt, K. A1 - Rehmer, Birgit A1 - Haubrich, J. A1 - Ávila Calderón, Luis A1 - Schoenstein, F. A1 - Serrano-Munoz, Itziar A1 - Requena, G. A1 - Bruno, Giovanni T1 - Separation of the impact of residual stress and microstructure on the fatigue performance of LPBF Ti-6Al-4V at elevated temperature N2 - Manufacturing defects, high residual stress (RS), and microstructures affect the structural integrity of laser powder bed fusion (LPBF) Ti-6Al-4V. In this study, the individual effect of these factors on fatigue performance at elevated temperature (300 °C) was evaluated. Material in as-built condition and subjected to post-processing, including two heat treatments and hot isostatic pressing, was investigated. It was found that in the absence of tensile RS, the fatigue life at elevated temperature is primary controlled by the defects; and densification has a much stronger effect than the considered heat treatments on the improvement of the mechanical performance. KW - Additive manufacturing KW - Ti-6Al-4V KW - Residual stress KW - Fatigue performance KW - Computed tomography PY - 2021 DO - https://doi.org/10.1016/j.ijfatigue.2021.106239 SN - 0142-1123 VL - 148 SP - 106239 PB - Elsevier Ltd. AN - OPUS4-52369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Micromechanics of internal stresses in multiphase materials, Part II- Mechanical properties of microcracked and porous materials N2 - 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. T2 - ATHOR webinar "Micromechanics of internal stresses in multiphase materials" CY - Online meeting DA - 26.01.2021 KW - Porosity KW - Neutron Diffraction KW - Residual Stress KW - Non-linear stress-strain KW - Anisotropy KW - Microcracking KW - Imaging PY - 2021 AN - OPUS4-52126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Assessing the safety of new technologies: Summary of Project AGIL N2 - In Additive Manufacturing everybody is talking about Free Form, Unconventional Design, Re-thinking Components, “Think out of the box”. However, there are a few outstanding question: a) What are the material properties ? They certainly differ from literature values for conventional materials; b) How about the microstructure? It is different from conventional materials. Does it stay so with ageing? How does it form? c) Do we properly take residual stress into account? We often blame them for our ignorance about failure scenarios. d) Do we apply tailored heat treatments? Very often, we follow conventional schedules… This talk describes the summary of the efforts carried out within the BAM Project AGIL. At BAM, we aimed to thoroughly investigate the microstructure and how it evolves as a function of load and temperature (service), to determine the material properties after different process and service conditions, to properly determine residual stress and the way it impacts mechanical properties and component performance, to properly quantify the impact of (unavoidable?) defects, and to determine heat treatments tailored to the process-specific material (stress relieve, microstructure homogenization etc.). The Project AGIL was and is intimately coupled with the project ProMoAM, dealing with online monitoring of AM processes. T2 - Workshop In-situ Monitoring and Microstructure Development in Additive Manufactured Alloys CY - Online meeting DA - 19.04.2021 KW - Mechanical properties KW - Additive manufacturing KW - Residual Stress KW - Microstructure KW - Fatigue KW - Creep PY - 2021 AN - OPUS4-52581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khimich, M. A. A1 - Prosolov, K. A. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Monforte, X. A1 - Teuschl, A. H. A1 - Slezak, P. A1 - Ibragimov, E. A. A1 - Saprykin, A. A. A1 - Kovalevskaya, Z. G. A1 - Dmitriev, A. I. A1 - Bruno, Giovanni A1 - Sharkeev, Y. P. T1 - Advances in Laser Additive Manufacturing of Ti-Nb Alloys: From Nanostructured Powders to Bulk Objects N2 - The additive manufacturing of low elastic modulus alloys that have a certain level of porosity for biomedical needs is a growing area of research. Here, we show the results of manufacturing of porous and dense samples by a laser powder bed fusion (LPBF) of Ti-Nb alloy, using two distinctive fusion strategies. The nanostructured Ti-Nb alloy powders were produced by mechanical alloying and have a nanostructured state with nanosized grains up to 90 nm. The manufactured porous samples have pronounced open porosity and advanced roughness, contrary to dense samples with a relatively smooth surface profile. The structure of both types of samples after LPBF is formed by uniaxial grains having micro- and nanosized features. The inner structure of the porous samples is comprised of an open interconnected system of pores. The volume fraction of isolated porosity is 2 vol. % and the total porosity is 20 vol. %. Cell viability was assessed in vitro for 3 and 7 days using the MG63 cell line. With longer culture periods, cells showed an increased cell density over the entire surface of a porous Ti-Nb sample. Both types of samples are not cytotoxic and could be used for further in vivo studies. KW - Additive manufacturing KW - Biomaterials KW - Ti-Nb alloy KW - Nanostructured powder KW - Laser methods KW - Powder methods KW - Laser powder bed fusion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525344 DO - https://doi.org/10.3390/nano11051159 VL - 11 IS - 5 SP - 1159 PB - MDPI AN - OPUS4-52534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peruzzi, N. A1 - Galli, S. A1 - Helmholz, H. A1 - Kardjilov, N. A1 - Krüger, D. A1 - Markötter, Henning A1 - Moosmann, J. A1 - Orlov, D. A1 - Prgomet, Z. A1 - Willumeit-Römer, R. A1 - Wennerberg, A. A1 - Bech, M. T1 - Multimodal ex vivo methods reveal that Gd-rich corrosion byproducts remain at the implant site of biodegradable Mg-Gd screws N2 - Extensive research is being conducted on magnesium (Mg) alloys for bone implant manufacturing, due to their biocompatibility, biodegradability and mechanical properties. Gadolinium (Gd) is among the most promising alloying elements for property control in Mg alloy implants; however, its toxicity is contro- versial. Investigating Gd behavior during implant corrosion is thus of utmost importance. In this study, we analyzed the degradation byproducts at the implant site of biodegradable Mg-5Gd and Mg-10Gd implants after 12 weeks healing time, using a combination of different imaging techniques: histology, energy-dispersive x-ray spectroscopy (EDX), x-ray microcomputed tomography (μCT) and neutron μCT. The main finding has been that, at the healing time in exam, the corrosion appears to have involved only the Mg component, which has been substituted by calcium and phosphorus, while the Gd remains localized at the implant site. This was observed in 2D by means of EDX maps and extended to 3D with a novel application of neutron tomography. X-ray fluorescence analysis of the main excretory organs also did not reveal any measurable accumulation of Gd, further reinforcing the conclusion that very limited or no removal at all of Gd-alloy happened during degradation. KW - Magnesium-gadolinium alloy KW - Biodegradable implant KW - Multimodal analysis KW - Energy-dispersive x-ray spectroscopy KW - Micro-computed tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535910 DO - https://doi.org/10.1016/j.actbio.2021.09.047 SN - 1742-7061 SP - 1 EP - 10 PB - Elsevier Ltd. AN - OPUS4-53591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprengel, Maximilian A1 - Ulbricht, Alexander A1 - Evans, Alexander A1 - Kromm, Arne A1 - Sommer, Konstantin A1 - Werner, Tiago A1 - Kelleher, J. A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - Towards the optimization of post-laser powder bed fusion stress-relieve treatments of stainless steel 316L N2 - This study reports on the stress relaxation potential of stress-relieving heat treatments for laser powder bed fused 316L. The residual stress is monitored non-destructively using neutron diffraction before and after the heat treatment. Moreover, the evolution of the microstructure is analysed using scanning electron microscopy. The results show, that a strong relaxation of the residual stress is obtained when applying a heat treatment temperature at 900°C. However, the loss of the cellular substructure needs to be considered when applying this heat treatment strategy. KW - Residual stress KW - Additive manufacturing KW - Neutron diffraction KW - Projekt AGIL - Alterung additiv gefertigter metallischer Materialien und Komponenten PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536045 DO - https://doi.org/10.1007/s11661-021-06472-6 SN - 1543-1940 VL - 52 IS - 12 SP - 5342 EP - 5356 PB - Springer CY - Boston AN - OPUS4-53604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Mrkwitschka, Paul A1 - Moos, R. A1 - Rabe, Torsten T1 - Glass-ceramic composites as insulation material for thermoelectric oxide multilayer generators N2 - Thermoelectric generators can be used as energy harvesters for sensor applications. Adapting the ceramic multilayer technology, their production can be highly automated. In such multilayer thermoelectric generators, the electrical insulation material, which separates the thermoelectric legs, is crucial for the performance of the device. The insulationmaterial should be adapted to the thermoelectric regarding its averaged coefficient of thermal expansion α and its sintering temperature while maintaining a high resistivity. In this study, starting from theoretical calculations, a glass-ceramic Composite material adapted for multilayer generators fromcalciummanganate and Calcium cobaltite is developed. The material is optimized towards an α of 11 × 10−6 K−1 (20–500◦C), a sintering temperature of 900◦C, and a high resistivity up to 800◦C. Calculated and measured α are in good agreement. The chosen glass-ceramic composite with 45 vol.% quartz has a resistivity of 1 × 107 Ωcm and an open porosity of <3%. Sintered multilayer samples from tape-cast thermoelectric oxides and screen-printed insulation show only small reaction layers. It can be concluded that glass-ceramic composites are a well-suited material class for insulation layers as their physical properties can be tuned by varying glass composition or dispersion phases. KW - Electrical insulators KW - Glass-ceramics KW - Multilayers KW - Thermal expansion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538898 DO - https://doi.org/10.1111/jace.18235 SN - 0002-7820 SP - 1 EP - 10 PB - Wiley Online Library AN - OPUS4-53889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -