TY - JOUR A1 - Meyer, Andreas A1 - Weidner, Steffen A1 - Kricheldorf, Hans R. T1 - Star-shaped poly(l-lactide)s based on pentaerythritol: About crystallization and polycondensation plus disproportionation and ring formation in the solid state N2 - Star-shaped poly( L-lactide)s (s-PLAs), were prepared by ring-opening polymerization of with pentaerythritol and catalyzed by tin(II) 2-ethylhyexanoate (SnOct out in bulk at either 120 ◦ C or 160 ◦ L-lactide (LA) initiated 2 ). Two small series of ROPs were carried C with variation of the LA/initiator ratio. Matrix-assisted laser desorption/ ionization time-of-flight (MALDI-TOF) mass spectra revealed traces of cycles in 120 ◦ C samples only at low initiator/catalyst ratios. In contrast, higher fractions of cycles were detected in samples prepared at 160 C, suggesting a "back-biting" origin. The influence of arm length and thermal history on crystallinity was investigated by differential scanning calorimetry (DSC) and wide-angle x-ray scattering (WAXS). It was shown that annealing increased the melting temperature (T ◦ ◦ m ) and crystallinity. However, annealing at 140 ◦ C for 14 d also caused significant solid-state transesterification. In addition, crystallites composed of s-PLAs with extended arms and, simultaneously, crystallites composed exclusively of extended rings were formed, identified by their typical "sawtooth" pattern in the MALDI mass spectra. Small angle x-ray scattering (SAXS) indicated that the crystal thickness was lower than that of linear PLAs annealed under identical conditions, but increased upon annealing at 140 C. KW - MALDI-TOF MS KW - Polylactide KW - Crystallisation KW - AStar-shaped polymers PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636832 DO - https://doi.org/10.1016/j.polymer.2025.128709 SN - 0032-3861 VL - 334 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-63683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Miccoli, Lorenzo A1 - Silva, R. A. A1 - Oliveira, D. V. A1 - Müller, U. T1 - Static behavior of cob: Experimental testing and finite-element modeling N2 - The aim of this paper is to implement a numerical model to reproduce the nonlinear behavior of cob walls under shear loading. Axial compression, pull-off, and diagonal compression tests were carried out to derive the mechanical parameters. In addition, the stressstrain relationships, the nonlinear behavior, and the failure modes were defined. The experimental results were then used to calibrate a finiteelement model. The material behavior was simulated through a macromodeling approach adopting the total strain rotating crack model. A sensitivity analysis was conducted to assess the effects of varying the parameters with higher uncertainty on the structural behavior. The numerical model achieved good correspondence with the experimental results in terms of simulation of the shear stress–shear strain relationship and of damage pattern. KW - Cob KW - Compression behavior KW - Shear behavior KW - Digital image correlation KW - Finite-element method PY - 2019 DO - https://doi.org/10.1061/(ASCE)MT.1943-5533.0002638 SN - 0899-1561 SN - 1943-5533 VL - 31 IS - 4 SP - 04019021-1 EP - 04019021-13 PB - ASCE American Society of Civil Engineers AN - OPUS4-47316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieder, Philipp A1 - Petrich, Lukas A1 - Serrano-Munoz, Itziar A1 - Mouiya, Mossaab A1 - Markötter, Henning A1 - Huger, Marc A1 - Bruno, Giovanni A1 - Schmidt, Volker T1 - Statistical analysis of grains and pores within polycrystalline Al2TiO5 ceramics, based on X-ray computed tomography N2 - Advanced statistical image analysis workflows were developed to segment and quantitatively evaluate 2D electron-backscatter diffraction (EBSD) maps and 3D synchrotron X-ray computed tomography (SXCT) volumes of a polycrystalline Al2TiO5 refractory composite that contains microcracks and pores. Several size, shape, and further geometric descriptors were determined for both the solid phase (Al2TiO5 grains) and the pore space. The resulting pore-size distribution is distinctly bimodal: coarse pores (tens to hundreds of micrometers), traced to incomplete powder compaction, coexist with fine pores generated during sintering. The two pore populations appear to be correlated with grain growth and crystallographic orientation in different ways. Finally, the descriptors obtained from the 2D EBSD and 3D SXCT data sets are internally consistent but complementary, highlighting the value of characterizations based on EBSD and SXCT in the microstructural study of refractory ceramics. KW - Synchrotron X-ray computed tomography KW - Electron-backscatter diffraction KW - Aluminum titanate KW - Morphological reconstruction KW - Image Segmentation KW - Statistical image analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643918 DO - https://doi.org/10.1016/j.matchar.2025.115602 SN - 1044-5803 VL - 229 SP - 1 EP - 13 PB - Elsevier Inc. AN - OPUS4-64391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kiefer, P. A1 - Deubener, J. A1 - Müller, Ralf A1 - Behrens, H. T1 - Statistical analysis of propagation rates of indentation-induced radial cracks N2 - Due to the stochastic nature of crack nucleation by Vickers indentation, a statistical analysis of propagation rates of 185 radial cracks was performed. Crack growth was observed directly using a video camera with high Image acquisition rate. It is found that propagation rates are controlled by the environmental reactions at the crack-tip shortly after their initiation (< 1 s). Calibration of the stress intensity KI showed that the residual stress factor χ and the exponent n of the equation KI==χPc−n (with P==load and c==crack length) are broadly distributed among the 185 analyzed cracks, ranging from 10−16 to 104 and from 0.1 to 5, respectively. For the most frequent crack, the equation KI==0.052Pc−1.47 holds. The results show that correlations of indentation-induced crack length to stress intensity necessitate the use of statistical significant data that are calibrated by the environmental reactions at the crack-tip. KW - Stress intensity factor KW - Vickers indentation KW - Subcritical crack growth KW - Soda-lime-silica glass PY - 2019 DO - https://doi.org/10.1016/j.jnoncrysol.2019.119739 VL - 527 SP - 119739 PB - Elsevier B.V. AN - OPUS4-50393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marko, A. A1 - Graf, B. A1 - Rethmeier, Michael T1 - Statistical analysis of weld bead geometry in Ti6Al4V laser cladding N2 - The process of laser cladding has become more important during recent years because of its broad application for cladding, repair or additive manufacturing. In the field of mechanical engineering, one use is the repair of turbine blades. For high quality and reliability of the repaired components, it is necessary to adjust the weld bead geometry to the specific repair task. The bead geometry influences the metallurgical bonding and the degree of dilution as well as the formation of defects like pores or cracks. Therefore, it is important to know the effects of the different parameters on the welding bead. A valuable tool to meet this industrial challenge is the design of experiments (DoE). In this context, the user can choose between a huge number of test plans. Greater Profit of information is expected by a larger test range. In order to confirm the acceptance, a five-step full factorial test plan is compared to a central composite design in this paper. Moreover, the limits of the experimental range are indicated and restrictions can be derived. As the results show, the essential effects are detected with a full factorial test plan as well as with a central composite design. Merely the effect strength could not always be specified unambiguously. On this account and in consideration of cost efficiency, the use of central compound design is recommended in industrial applications. KW - Laser metal deposition KW - Design of experiments KW - Laser cladding KW - Cladding parameter KW - Additive manufacturing PY - 2017 DO - https://doi.org/10.3139/120.111077 SN - 0025-5300 SN - 2195-8572 VL - 59 IS - 10 SP - 837 EP - 843 PB - Carl Hanser Verlag CY - München AN - OPUS4-42882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieder, Philipp A1 - Petrich, Lukas A1 - Serrano-Munoz, Itziar A1 - Fernández, Ricardo A1 - Bruno, Giovanni A1 - Schmidt, Volker T1 - Statistical Comparison of Substructures in Pure Aluminum Before and After Creep Deformation, Based on EBSD Image Data N2 - 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. KW - Crystallographic descriptor KW - Dislocation-climb-controlled creep KW - Electron backscatter diffraction (EBSD) KW - Geometric descriptor KW - Ernel average misorientation (KAM) KW - pure aluminum KW - Qquantification and segmentation KW - Statistical image analysis KW - subgrain PY - 2023 DO - https://doi.org/10.1093/micmic/ozad121 SN - 1431-9276 SP - 1 EP - 12 PB - Oxford University Press AN - OPUS4-58730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Salzmann, Christoph A1 - Pellegrino, Francesco A1 - Hodoroaba, Vasile-Dan T1 - STEM-in-SEM versus SE-InLens-type-SEM as a Reliable Analytical Pair-Tool for Measurement of Nanoparticle Size and Shape Distribution N2 - Following points are addressed in this contribution: Advantages of correlative analysis in electron microscopy; Measurement principle of the different electron microscopy modes used; Presentation of the nanomaterials used for this study; Role of sample preparation; and, with particular description, the Sequence kV-variation with InLens SE & transmission SEM detection of the same field-of-view. KW - Nanoparticles KW - Electron microscopy KW - Metrology KW - Particle size distribution PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.308 VL - 30 IS - Supplement_1 SP - 650 EP - 651 PB - Oxford University Press (OUP) AN - OPUS4-61042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, A. A1 - Weidner, Steffen A1 - Kricheldorf, H. T1 - Stereocomplexation of cyclic polylactides with each other and with linear poly(L-lactide)s N2 - Two kinds of cyclic poly(D- and L-lactide)s were synthesized, namely CI labeled samples mainly consisting of even-numbered cycles with low dispersity and CII, CIII or CIV-labeled ones consisting of equal amounts of even and odd-numbered cycles with high dispersity and igher molecular weights (Mw up to 300 000). Furthermore, linear poly L-lactide)s were prepared by initiation with ethanol and in both series the molecular weight was varied. The formation of stereocomplexes from cyclic poly(D-lactide)s and all kinds of poly L-lactide)s was performed in dichloromethane/toluene mixtures. The stereocomplexes crystallized from the reaction mixture were characterized in the virgin state and after annealing at 205 °C. Stereocomplexes free of stereohomopolymers with crystallinities up to 80% were obtained from all experiments in yields ranging from 60 to 80%. Despite the high annealing temperature (maintained for 1 h), little transesterification was observed and the crystallinity slightly increased. KW - Polylactide KW - MALDI-TOF MS KW - Stereocomplex KW - Cyclic PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496693 DO - https://doi.org/10.1039/c9py01236b VL - 10 SP - 6191 EP - 6199 PB - Royal Society for Chemistry AN - OPUS4-49669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zerbst, Uwe A1 - Madia, Mauro A1 - Kiyak, Yusuf A1 - Breidung, Marc A1 - Baer, Wolfram A1 - Küppers, M. ED - Madia, Mauro T1 - Stiffness/constraint effects in analytical flaw assessment - A technical note N2 - Using the case study of a fail-safe design criterion for a steering knuckle of a commercial vehicle, the effect of stiffness/constraint on the crack driving force in the component is discussed. The problem arises when assessment procedures such as R6, BS 7910 or SINTAP/FITNET are applied in conjunction with substitute geometries for determining the model parameters K-factor and limit load (or a substitute for the latter), as it is common practice. In the example, the conservatism was so pronounced that this procedure was in fact unusable. A way out could be the finite element-based determination of the model parameters and their use in the analytical framework. This procedure is useful and effective if the finite element-based calculations are used in parameter sensitivity analyses. KW - Fail-safe design KW - Fracture resistance KW - Fracture assessment KW - Stiffness KW - Constraint PY - 2022 DO - https://doi.org/10.1016/j.engfracmech.2022.108728 SN - 0013-7944 IS - 273 SP - 1 EP - 15 PB - Elsevier Science CY - Kidlington AN - OPUS4-55544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huo, W. A1 - Bakir, Nasim A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael A1 - Wolter, K. T1 - Strain Prediction Using Deep Learning during Solidification Crack Initiation and Growth in Laser Beam Welding of Thin Metal Sheets N2 - The strain field can reflect the initiation time of solidification cracks during the welding process. The traditional strain measurement is to first obtain the displacement field through digital image correlation (DIC) or optical flow and then calculate the strain field. The main disadvantage is that the calculation takes a long time, limiting its suitability to real-time applications. Recently, convolutional neural networks (CNNs) have made impressive achievements in computer vision. To build a good prediction model, the network structure and dataset are two key factors. In this paper, we first create the training and test sets containing welding cracks using the controlled tensile weldability (CTW) test and obtain the real strain fields through the Lucas–Kanade algorithm. Then, two new networks using ResNet and DenseNet as encoders are developed for strain prediction, called StrainNetR and StrainNetD. The results show that the average endpoint error (AEE) of the two networks on our test set is about 0.04, close to the real strain value. The computation time could be reduced to the millisecond level, which would greatly improve efficiency. KW - Convolutional neural network KW - Strain fields prediction KW - Laser beam welding KW - Solidification cracking PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570565 DO - https://doi.org/10.3390/app13052930 VL - 13 IS - 5 SP - 1 EP - 15 PB - MDPI AN - OPUS4-57056 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -