TY - CONF A1 - Müller, Bernd R. 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. T2 - Eleventh Joint BER II and BESSY II User Meeting CY - Wilhelm-Conrad-Roentgen-Campus, Berlin-Adlershof, Germany DA - 04.12.2019 KW - Characterization KW - CMAS KW - Synchrotron X-ray refraction radiography KW - Thermal arrier coatings PY - 2019 AN - OPUS4-49857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Serrano-Munoz, Itziar T1 - Influence of scanning strategies on the development of residual stresses in a LPBF IN718 alloy N2 - This presentation is a brief summary on the activites that 8.5 division has been carrying out on the measurements of residual stresses of a Laser Power Bed Fusion IN718 alloy. T2 - Euromat 2019 CY - Stockholm, Sweden DA - 02.09.2019 KW - Laser Powder Bed Melting KW - AM IN718 alloy KW - Residual stresses KW - Neutron diffraction KW - Synchrotron Energy Dispersive Diffraction PY - 2019 AN - OPUS4-48895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - CONF A1 - Ulbricht, Alexander T1 - How Temperature Gradient Influences the Formation of Residual Stresses in Metallic Parts Made by L-PBF N2 - Rapid cooling rates and steep temperature gradients are characteristic of additively manufactured (AM) parts and important factors for residual stress formation which have implications on structural integrity. This study examined the influence of heat input on the distribution of residual stresses in two prisms produced by laser powder bed fusion (L-PBF) of austenitic stainless steel 316L. The layers of the prisms were exposed using two distinct helix scanning strategies: one scanned from the centre to the perimeter and the other from the perimeter to the centre. Residual stresses were characterised at one plane perpendicular to the building direction at half of its build height using neutron diffraction. In addition, the defect distribution was analysed via micro X-ray computed tomography (µCT) in a twin specimen. Both scanning strategies reveal residual stress distributions typical for AM: compressive stresses in the bulk and tensile stresses at the surface. However, temperature gradients and maximum stress levels differ due to the different heat input. Regarding the X-ray µCT results, they show an accumulation of defects at the corners where the laser direction turned through 90°. The results demonstrate that neutron diffraction and X-ray µCT can be successfully used as non-destructive methods to analyse through-thickness residual stress and defect distribution in AM parts, and in the presented case, illustrate the influence of scanning strategies. This approach contributes to deeper assessment of structural integrity of AM materials and components. T2 - First European Conference on Structural Integrity of Additively Manufactured Materials (ESIAM19) CY - Trondheim, Norwegen DA - 09.09.2019 KW - AGIL KW - Neutron diffraction KW - Thermography KW - Additive manufacturing KW - Residual stress PY - 2019 AN - OPUS4-49805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander T1 - Influence of manufacturing parameters on microstructure and subsurface residual stress in SLM Ti-6Al-4V N2 - Using non-optimum combination of manufacturing parameters in selective laser melting (SLM) may lead to reduction of quality of component: defects generation, distortion of geometry and even cracking. Usually, the optimization of parameters is performed by changing volumetric energy density (Ev) and selecting parameters giving low porosity values. However, not only low porosity but also stable microstructure and low residual stresses will help to achieve advanced mechanical behavior of the component. In present work, we investigated cuboid-shaped Ti-6Al-4V samples produced with different manufacturing parameters. The parameters leading to the same Ev were considered as well as parameters which are not included in Ev. Residual stresses in subsurface region were investigated by synchrotron X-ray diffraction, which allows to penetrate around 100 µm from the surface therefore overcome the problem of high roughness of SLM components without additional sample preparation. Only tensile stresses were found along the building direction, that can play critical role especially during cyclic loading. In parallel, using X-ray computed tomography we also observe that porosity is mainly concentrated in the contour region, except in case where the laser speed is small. However, by using some process parameters it was possible to decrease residual stresses and obtain uniform α+β Ti microstructure and relatively low porosity. Additionally, it was found that not included in Ev (e.g., base plate position, focus distance) should be considered as additional manufacturing parameters during SLM process. T2 - ISAM Konferenz 2019 CY - Dresden, Germany DA - 29.01.2019 KW - Computed Tomography KW - Additive Manufacturing KW - Metals KW - Microstructure PY - 2019 AN - OPUS4-47328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geyler, Paul T1 - Machine learning assisted evaluation of the shape of VIAs in a LTCC multilayer N2 - The introduction of the 5G technology and automotive radar applications moving into higher frequency ranges trigger further miniaturization of LTCC technology (low temperature co-fired ceramics). To assess dimensional tolerances of inner metal structures of an industrially produced LTCC multilayer, computer tomography (CT) scans were evaluated by machine learning segmentation. The tested multilayer consists of several layers of a glass ceramic substrate with low resistance silver-based vertical interconnect access (VIA). The VIAs are punched into the LTCC green tape and then filled with silver-based pastes before stacking and sintering. These geometries must abide by strict tolerance requirements to ensure the high frequency properties. This poster presents a method to extract shape and size specific data from these VIAs. For this purpose, 4 measurements, each containing 3 to 4 samples, were segmented using the trainable WEKA segmentation, a non-commercial machine learning tool. The dimensional stability of the VIA can be evaluated regarding the edge-displacement as well as the cross-sectional area. Deviation from the ideal tubular shape is best measured by aspect ratio of each individual layer. The herein described method allows for a fast and semi-automatic analysis of considerable amount of structural data. This data can then be quantified by shape descriptors to illustrate 3-dimensional information in a concise manner. Inter alia, a 45 % periodical change of cross-sectional area is demonstrated. T2 - DKG Jahrestagung 2019 CY - Leoben, Austria DA - 06.05.2019 KW - Machine Learning KW - LTCC multilayer KW - 5G PY - 2019 AN - OPUS4-48289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiede, Tobias T1 - µCT Surface Analysis of LBM Struts - Influence of the Build Angle N2 - In this work, the structural integrity of LBM fabricated IN625 small cylinders (d = 1 mm, h = 6 mm) was investigated regarding the porosity and the surface roughness by means of computed tomography. The measurements were carried out on a GE v|tome|x L 300/180 with a reconstructed voxel size of 2 µm. The pores were analyzed for size, shape and spatial distribution. The correlation between compactness C and spatial distribution showed that elongated pores (C < 0.2) appear exclusively within a distance of 80 µm to the sample surface. The reconstructed surface was digitally meshed and unwrapped to evaluate the mean roughness Ra. Since the gravity correlates linearly with the sine of the build angle, the influence of gravity on porosity and surface roughness was determined. T2 - iCT 2019 CY - Padua, Italien DA - 13.02.2019 KW - Additive Manufacturing KW - Laser Beam Melting KW - Selective Laser Melting KW - Computed Tomography KW - Roughness KW - Porosity KW - Build Angle PY - 2019 AN - OPUS4-47775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Buljak, V. T1 - Modeling of elastic modulus evolution in porous ceramics due to thermally induced cracking N2 - Within polycrystalline porous ceramics used in automotive applications as diesel particulate filters, it is evidenced that during cooling from firing temperature micro cracks are gradually formed. The cracks are formed as a consequence of strong thermal anisotropy of grains. Typically these micro cracks are granting better thermal shock resistance, with respect to dense materials, but reduce stiffness. The reduction can be quantified by measuring the drop in elastic properties of bulk material which, depending on the level of porosity, can decrease even by 50% with respect to its value at high temperature. It is further observed that upon subsequent heating these cracks are closing and partially or totally healing at very high temperatures. Such peculiar behavior results in partial or complete recovery of the elastic properties of bulk material upon completing one thermal cycle. Despite its evident practical application, still there is no constitutive description of this phenomenon, capable of predicting the evolution of Young's modulus as a function of temperature history. For reliable numerical simulation of this phenomenon, it is required to model fracture. To model inter-crystalline fracture, an effective strategy is to use cohesive elements, since crack patterns are a priori known. Major limitation of this approach is that the cohesive elements already implemented within commercial codes cannot take into account crack healing upon subsequent heating. In this study new cohesive element is developed and numerically implemented within ABAQUS commercial finite element code, capable to model crack opening, closing and healing. Further on, a computer code is generated to build numerical model of porous ceramic specimens that takes into account experimentally measured crystallographic orientation and porosity, and models the microstructure by using Voronoi polygons. The developed numerical tools serve as a framework for more realistic simulations, required to study the hysteresis in elastic properties within porous ceramics provoked by thermal cyclic. In a subsequent phase, an inverse analysis procedure is developed, in which macroscopic properties are used to calibrate parameters entering into micro crack model. The approach is centered on a minimization of a discrepancy function designed to quantify the difference between experimentally measured quantities and their computed counterpart. The model is calibrated on the basis of experimental data regarding the drop of bulk Young's modulus with decrease of temperature. Developed procedure is tested with porous cordierite sample, and obtained results are quit promising despite the current limitation of using only two-dimensional model. T2 - European Ceramic Society Conference 2019 CY - Turin, Italy DA - 16.06.2019 KW - Microcracking KW - Cordierite KW - Inverse Problems KW - Finite elements KW - Cohesive Elements KW - Young's modulus PY - 2019 AN - OPUS4-48926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Design and fabrication of ceramic springs N2 - Ceramic springs offer versatile possibilities for load bearing or sensor applications in challenging environments. Although it may appear unexpected, a wide range of spring constants can be implemented by material selection and especially by the design of the spring. Based on a rectangular cross-section of the windings, it is possible to design a spring geometry that generates the desired spring constant simply by choosing appropriate diameter, height, widths, and number of windings. In a recent research project the calculation of helical compression springs made of rectangular steel (German standard DIN 2090) was applied for the design of ceramic springs. A manufacturing technology has been worked out to fabricate such springs from hollow cylinders of several highly dense technical ceramics by milling. Ceramic springs with precise rectangular section, without edge damage, and mean surface roughness smaller than 0.2 µm were produced after parameter optimization. Tolerances of less than 10 µm were achieved regarding spring diameter, height, and width of cross section. It is shown that the calculations outlined in the standard are valid for a variety of ceramic materials as well. Demonstrator springs with a wide range of spring constants have been fabricated, including zirconia springs with 0.02 N/mm, alumina springs with 1 N/mm and Si3N4 springs with 5 N/mm. A reproducibility study of six zirconia springs with a constant of 0.3 N/mm showed a relative difference in spring constants of less than +/- 1 %. This combination of a valid calculation approach for spring geometry and a reliable manufacturing technology allows for purposeful development and fabrication of ceramic springs with precise mechanical properties and superior chemical stability. T2 - EUROMAT 2019 CY - Stockholm, Sweden DA - 01.09.2019 KW - Ceramic spring KW - Hard machining KW - Spring constant PY - 2019 AN - OPUS4-48870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Evaluation of a multi-purpose measurement cell for standardized volume resistivity measurements at high temperatures N2 - The ProboStat is a multi-purpose measurement cell suitable for various electrical and physical measurements under different atmospheres and at high temperatures. Disc and bar shaped samples are sandwiched between platinum electrodes at the top of the tubular cell. The gas tight assembly can be inserted into a furnace. Different gases can be flushed through the tube. For this study, a ProboStat was adapted to measure volume resistivity of ceramic insulators at high temperatures according to standards. The standardized measurement of volume resistivity of ceramic insulators requires the consideration of many specifications including sample diameter, thickness, electrode design, and the proportion of these characteristics. Measurements are ideally performed in a state of dielectric equilibrium. The time-related slope of resistivity of a specific sample follows a power function. Thus, care must be taken when choosing a charge time or defining the duration of a measurement. As fringing of the guarded electrode occurs under high voltage, the effective electrode area for evaluation of the results should be corrected with respect to sample thickness and electrode design. The demands of effective standards on sample geometry and electrode design are stricter for room temperature measurements than for high temperature measurements. To perform high temperature measurements on ceramic samples that also fulfill the demands on room temperature measurements, a ProboStat was equipped with a dedicated large sample setup for discs with diameters of up to 60 mm. The volume resistivity of different alumina samples was first measured at room temperature in a standard test fixture and then compared to results obtained with the ProboStat. All measurements were performed for at least 100 min using a 26 mm guarded electrode. High temperature measurements at 500 °C were performed using the same samples. Room temperature values obtained with the standard test fixture are in the order of 10^17 Ohm·cm. The quantitative effect of electrode area correction is presented. Practical issues related to the use of the multi-purpose cell are addressed. These include electrode material selection, application of electrodes, and compensation of leakage currents. High temperature results of volume resistivity of the different alumina samples are presented. The validity is discussed with respect to the suitability of the multi-purpose cell for such measurements. T2 - XVI Conference and Exhibition of the European Ceramic Society (ECerS 2019) CY - Torino, Italy DA - 16.06.2019 KW - ceramics KW - alumina KW - volume resistivity PY - 2019 AN - OPUS4-48270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -