TY - CONF A1 - Bruno, Giovanni T1 - X-ray Absorption and Refraction techniques for characterization and non-destructive-testing of materials N2 - 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 show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials. T2 - ENSAM CY - Paris, France DA - 28.11.2019 KW - Additive Manufacturing KW - Computed Tomography KW - Neutron Diffraction KW - X-ray refraction techniques KW - Composites PY - 2019 AN - OPUS4-49927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Cong A1 - Müller, Bernd R. A1 - Lebedev, O. A1 - Giovannelli, F. A1 - Bruno, Giovanni A1 - Delorme, F. T1 - Effects of impurities on the stability of the low thermal conductivity in Fe2TiO5 ceramics N2 - The stability of the low thermal conductivity in Fe2TiO5 pseudobrookite ceramics has been studied. An increase in thermal diffusivity is observed after only three cycles of measurement. X-ray refraction shows an increase in the mean value of specific surface after the thermal diffusivity measurements. By using scanning electron microscopy and high‐angle annular dark‐field scanning transmission electron microscope equipped with energy dispersive X-ray spectroscopy, we observe a segregation of Ca- and F-rich nanocrystals at grain boundaries after three cycles of thermal diffusivity measurement. Therefore, impurities seem to be more efficient to scatter phonons as point defects in the pseudobrookite lattice rather than as nanocrystals at pseudobrookite grain boundaries. This emphasizes the importance of precursor purity and the influence of redistribution of impurities on thermoelectric properties: stability of micro-/nano-structures is a key point, and repeated thermoelectric measurements may allow detecting such metastable micro- /nano-structures and producing stable and reliable data. KW - Fe2TiO5 KW - Impurity segregation KW - Thermoelectrics KW - X-ray refraction KW - Scanning transmission electron microscopy PY - 2019 UR - http://www.sciencedirect.com/science/article/pii/S1044580318329309 DO - https://doi.org/10.1016/j.matchar.2019.01.021 SN - 1044-5803 SN - 1873-4189 VL - 149 SP - 111 EP - 117 PB - Elsevier Inc. AN - OPUS4-47255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hilgenberg, Kai A1 - Daum, Werner A1 - Maierhofer, Christiane A1 - Altenburg, Simon A1 - Bruno, Giovanni A1 - Heckel, Thomas A1 - Skrotzki, Birgit A1 - Zerbst, Uwe A1 - Kranzmann, Axel A1 - Bettge, Dirk A1 - Sommer, Konstantin A1 - Seeger, Stefan A1 - Nitsche, Michael A1 - Günster, Jens A1 - Evans, Alexander T1 - Additive manufacturing at the BAM: We focus on Safety N2 - In Germany, the Federal Institute for Materials Research and Testing (BAM) is addressing challenges in the implementation of additive manufacturing on the industrial landscape for safety-critical applications. KW - Process development KW - Additive Manufacturing KW - In-situ Process Monitoring KW - Non-destructive Materials KW - Characterisation KW - Safety KW - Fatigue KW - Environment KW - Standardisation PY - 2019 UR - https://static.asminternational.org/amp/201910/22/ SN - 0882-7958 VL - 177 IS - 7 SP - 22 EP - 26 PB - ASM International CY - Materials Park, OH, USA AN - OPUS4-49780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Engineering applications of neutrons at the ILL: retrospective, present, and future N2 - In this talk, the evolution of the demand for engineering applications of neutrons at the ILL in the last 10 years is presented. It is shown that small angle neutron scattering and diffraction are highly demanded by the materials science community. Further development in the field is foreseen, with the use of in-situ (furnace, tension/compression rig, humidity cells, etc.) techniques to associate to the neutron techniques. T2 - ILL 100th Scientific Council CY - Grenoble, France DA - 09.04.2019 KW - Neutron Diffraction KW - Residual Stress KW - Small Angle Neutron Scattering KW - Engineering applications KW - Institut Laue Langevin PY - 2019 AN - OPUS4-48396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Diffraction-based experimental determination of Residual Stress in AM parts: A critical discussion N2 - Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, not always paralleled by the knowledge about the materials properties and performance. In particular, residual stress (RS) has been soon recognized as an issue in AM parts, so that parts are always post-heat-treated. Moreover, much effort has been spent on simulating RS, especially using finite element methods. The experimental determination of RS has thereby become increasingly important, and even simple data constitute (to date) a piece of knowledge to fill the above-mentioned gap. In particular, diffraction methods, which are basically non-destructive, offer enormous possibilities to gain knowledge on real components, since neutrons and synchrotron radiation can penetrate even heavy metals up to several millimeters (or even centimeters). Indeed, some success has been obtained, and the knowledge about the origins of the RS fields, as well as their variation as a consequence of heat or mechanical treatments, has been greatly expanded. In this talk, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with focus on those produced by laser powder bed fusion) has even allowed showing that process parameters that were considered unimportant play a major role in the onset of stress. However, while RS is starting to be considered in the part design, deposition strategy (e.g. build plate temperature), and even in the definition of the relevant metric to assess the quality of a part, much is still to be investigated about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even to date unclear will also be discussed, such as the determination of the reference unstrained samples and of the principal axes of stress. All these aspects will draw the path towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts. T2 - MSTAM 2019 CY - Bremen, Germany DA - 10.12.2019 KW - Elastic Constants KW - Residual Stress KW - Additive Manufacturing KW - Neutron Diffraction PY - 2019 AN - OPUS4-50020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Artzt, K. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Exploring the correlation between subsurface residual stresses and manufacturing parameters in laser powder bed fused Ti-6Al-4V N2 - Subsurface residual stresses (RS) were investigated in Ti-6Al-4V cuboid samples by means of X-ray synchrotron diffraction. The samples were manufactured by laser powder bed fusion (LPBF) applying different processing parameters, not commonly considered in open literature, in order to assess their influence on RS state. While investigating the effect of process parameters used for the calculation of volumetric energy density (such as laser velocity, laser power and hatch distance), we observed that an increase of energy density led to a decrease of RS, although not to the same extent for every parameter variation. Additionally, the effect of support structure, sample roughness and LPBF machine effects potentially coming from Ar flow were studied. We observed no influence of support structure on subsurface RS while the orientation with respect to Ar flow showed to have an impact on RS.We conclude recommending monitoring such parameters to improve part reliability and reproducibility. KW - Additive manufacturing KW - Synchrotron X-ray diffraction KW - Residual stress KW - Ti-6Al-4V PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474281 DO - https://doi.org/10.3390/met9020261 SN - 2075-4701 VL - 9 IS - 2 SP - 261, 1 EP - 13 PB - MDPI AN - OPUS4-47428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Gouraud, F. A1 - Müller, Bernd R. A1 - Huger, M. A1 - Chotard, T. A1 - Antou, G. A1 - Bruno, Giovanni T1 - Evolution of Thermal Microcracking in Refractory ZrO2-SiO2 after Application of External Loads at High Temperatures N2 - Zirconia-based cast refractories are widely used for glass furnace applications. Since they have to withstand harsh chemical as well as thermo-mechanical environments, internal stresses and microcracking are often present in such materials under operating conditions (sometimes in excess of 1700 °C). We studied the evolution of thermal (CTE) and mechanical (Young’s modulus) properties as a function of temperature in a fused-cast refractory containing 94 wt.% of monoclinic ZrO2 and 6 wt.% of a silicate glassy phase. With the aid of X-ray refraction techniques (yielding the internal specific surface in materials), we also monitored the evolution of microcracking as a function of thermal cycles (crossing the martensitic phase transformation around 1000 °C) under externally applied stress. We found that external compressive stress leads to a strong decrease of the internal surface per unit volume, but a tensile load has a similar (though not so strong) effect. In agreement with existing literature on -eucryptite microcracked ceramics, we could explain These phenomena by microcrack closure in the load direction in the compression case, and by microcrack propagation (rather than microcrack nucleation) under tensile conditions. KW - Electro-fused zirconia KW - Microcracking KW - Synchrotron x-ray refraction radiography (SXRR) KW - Thermal expansion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477431 DO - https://doi.org/10.3390/ma12071017 VL - 12 IS - 7 SP - 1 EP - 15 PB - MDPI AN - OPUS4-47743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiede, Tobias A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Serrano-Munoz, Itziar A1 - Gollwitzer, Christian A1 - Bruno, Giovanni T1 - 3D shape analysis of powder for laser beam melting by synchrotron X-ray CT N2 - The quality of components made by laser beam melting (LBM) additive manufacturing is naturally influenced by the quality of the powder bed. A packing density <1 and porosity inside the powder particles lead to intrinsic voids in the powder bed. Since the packing density is determined by the particle size and shape distribution, the determination of these properties is of significant interest to assess the printing process. In this work, the size and shape distribution, the amount of the particle’s intrinsic porosity, as well as the packing density of micrometric powder used for LBM, have been investigated by means of synchrotron X-ray computed tomography (CT). Two different powder batches were investigated: Ti–6Al–4V produced by plasma atomization and stainless steel 316L produced by gas atomization. Plasma atomization particles were observed to be more spherical in terms of the mean anisotropy compared to particles produced by gas atomization. The two kinds of particles were comparable in size according to the equivalent diameter. The packing density was lower (i.e., the powder bed contained more voids in between particles) for the Ti–6Al–4V particles. The comparison of the tomographic results with laser diffraction, as another particle size measurement technique, proved to be in agreement. KW - Additive manufacturing KW - Laser beam melting KW - Synchrotron computed tomography KW - Powder analysis KW - Imaging PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474070 DO - https://doi.org/10.3390/qubs3010003 SN - 2412-382X VL - 3 IS - 1 SP - 3, 1 EP - 12 PB - MDPI AN - OPUS4-47407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khrapov, D. A1 - Surmeneva, M. A1 - Koptioug, A. A1 - Evsevleev, Sergei A1 - Léonard, Fabien A1 - Bruno, Giovanni A1 - Surmenev, R. T1 - X-ray computed tomography of multiple-layered scaffolds with controlled gradient cell lattice structures fabricated via additive manufacturing N2 - In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively. KW - Additive manufacturing KW - Lattice structure KW - Multiple-layered scaffold KW - Coating KW - Medical implants KW - Computed tomography KW - Polycaprolactone KW - Calcium phosphate PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471931 UR - http://stacks.iop.org/1742-6596/1145/i=1/a=012044 DO - https://doi.org/10.1088/1742-6596/1145/1/012044 SN - 1742-6596 VL - 1145 SP - 012044, 1 EP - 7 PB - IOP AN - OPUS4-47193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mack, D. E. A1 - Laquai, René A1 - Müller, Bernd R. A1 - Helle, O. A1 - Sebold, D. A1 - Vaßen, R. A1 - Bruno, Giovanni T1 - Evolution of porosity, crack density, and CMAS penetration in thermal barrier coatings subjected to burner rig testing N2 - Degradation of thermal barrier coatings (TBCs) in gas‐turbine engines due to calcium–magnesium–aluminosilicate (CMAS) glassy deposits from various sources has been a persistent issue since many years. In this study, state of the art electron microscopy was correlated with X‐ray refraction techniques to elucidate the intrusion of CMAS into the porous structure of atmospheric plasma sprayed (APS) TBCs and the formation and growth of cracks under thermal cycling in a burner rig. Results indicate that the sparse nature of the infiltration as well as kinetics in the burner rig are majorly influenced by the wetting behavior of the CMAS. Despite the obvious attack of CMAS on grain boundaries, the interaction of yttria‐stabilized zirconia (YSZ) with intruded CMAS has no immediate impact on structure and density of internal surfaces. At a later stage the formation of horizontal cracks is observed in a wider zone of the TBC layer. KW - Characterization KW - CMAS KW - Synchrotron X‐ray refraction radiography KW - Thermal barrier coatings PY - 2019 DO - https://doi.org/10.1111/jace.16465 SN - 0002-7820 SN - 1551-2916 VL - 102 IS - 10 SP - 6163 EP - 6175 PB - Wiley CY - Oxford AN - OPUS4-47804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -