TY - GEN A1 - Léonard, Fabien T1 - Overview of XCT data processing workflow for ammonium nitrate prills quantitative analysis N2 - This video presents the data processing workflow that was developed to perform the quantitative structural and morphological analysis of ammonium nitrate prills by x-ray computed tomography. KW - ANFO KW - Data processing KW - Explosives KW - Porosity KW - Surface area KW - XCT PY - 2020 DO - https://doi.org/10.5281/zenodo.3611339 PB - Zenodo CY - Geneva AN - OPUS4-51897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Evaluation of Advanced NDT-Methods for Measurement of Fibre Orientation in Concrete N2 - Integration of fibre reinforcement in high-performance cementitious materials has become widely applied in many fields of construction. One of the most investigated advantages of steel fibre reinforced concrete (FRC) is the deceleration of crack growth and hence it’s improved sustainability due to e.g. decrease of permeability of concrete by aggressive substances. Additional benefits are associated with the structural properties of FRC, where fibres can significantly increase the ductility and the tensile strength of concrete. In some applications, such as tunnel linings or industrial slabs, it is even possible to entirely replace the conventional reinforcement, leading to significant logistical and environmental benefits. Fibre reinforcement can, however, have critical disadvantages and even hinder the performance of concrete, since it can induce an anisotropic material behaviour of the mixture if the fibres are not appropriately oriented. For a safe use of FRC in the future, reliable non-destructive methods need to be identified to assess the fibres’ orientation in hardened concrete. In this study, ultrasonic material testing, electrical impedance testing, and X-ray computer tomography have been investigated for this purpose using specially produced samples with biased or random fibre orientations. This paper demonstrates the capabilities of each of these NDT techniques for fibre orientation measurements and draws conclusions based on these results about the most promising areas for future research and development using these techniques. T2 - fib2020 Shanghai CY - Online meeting DA - 22.11.2020 KW - Ultrasonic testing KW - Steel fibre reinforced concrete (FRC) KW - Fibre orientation KW - X-ray computed tomography (CT) KW - Electrical impedance PY - 2020 AN - OPUS4-51651 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Acoustic emission of fibre reinforced AlSi12CuMgNi alloy under compression N2 - Typically, the near-eutectic Al-Si alloys consist of highly interconnected three-dimensional network of the eutectic Silicon (Si) and intermetallics embedded into Aluminium (Al) matrix. For further improvement of the mechanical properties of such alloys, often, one single ceramic reinforcement phase, e.g. silicon carbide (SiC) or aluminium oxide (Al2O3) in the form of fibres or particles is added. However, hybrid reinforcements (fibres and particles) can further improve wear resistance and fracture toughness, and additionally, reduce anisotropy of the material. The engineering of metal matrix composites (MMC) for specific application requirements benefits from a comprehensive knowledge of the failure behaviour. Therefore, damage evolution under compression was investigated on: - pure near-eutectic AlSi12CuMgNi matrix alloy - type I: matrix reinforced with random-planar oriented Al2O3 short fibres (15 vol.%) - type II: matrix reinforced with random-planar oriented Al2O3 short fibres (7 vol.%) and additional SiC particles (15 vol.%) The analysis of damage mechanism was carried out in two rather independent but complementary studies. First, selected sister samples of every material were exposed to quasi-static compression (traverse control). The compression tests were interrupted at different strain levels. Miniature cylinders with a diameter of 1mm were extracted from the pre-strained samples and investigated by synchrotron computed tomography (SX-µCT) with a spatial resolution of about 0.7 µm. For the pure matrix alloy, microcracks are confined to the intermetallic particles and to the eutectic Si, hence no damage was observed in the Aluminium. The composite type II revealed a more effective strain accumulation (less damage) than type I at low plastic strain (up to 5 %), but a more catastrophic damage development due to cracking of the SiC clusters at higher strain levels. The second approach to study the damage initiation and accumulation in the materials subjected to compressive load was Acoustic Emission (AE) analysis. In this case the in-situ monitoring of the acoustic emission signal was performed during compression tests on specimens with dimension of several mm. For all three material types, AE activity set at 2% strain. Differences in AE behaviour of the three materials was proven based on AE hitrate, signal peak amplitudes as well as weighted peak frequencies (WPF). Future work focuses on combination of AE and SX-µCT aiming for more detailed knowledge on damage mechanism of metal matrix composites. T2 - Schall21 CY - Online meeting DA - 24.02.2021 KW - AlSi12CuMgNi KW - Al-Si alloys KW - Acoustic emission KW - Tension PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534268 UR - https://www.dgzfp.de/seminar/schall21 AN - OPUS4-53426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Oesch, T. A1 - Mielentz, Frank A1 - Meinel, Dietmar A1 - Spyridis, P. T1 - Non-Destructive Multi-Method Assessment of Steel Fiber Orientation in Concrete N2 - Integration of fiber reinforcement in high-performance cementitious materials has become widely applied in many fields of construction. One of the most investigated advantages of steel Fiber reinforced concrete (SFRC) is the deceleration of crack growth and hence its improved sustainability. Additional benefits are associated with its structural properties, as fibers can significantly increase the ductility and the tensile strength of concrete. In some applications it is even possible to entirely replace the conventional reinforcement, leading to significant logistical and environmental benefits. Fiber reinforcement can, however, have critical disadvantages and even hinder the Performance of concrete, since it can induce an anisotropic material behavior of the mixture if the fibers are not appropriately oriented. For a safe use of SFRC in the future, reliable non-destructive testing (NDT) methods need to be identified to assess the fibers’ orientation in hardened concrete. In this study, ultrasonic material testing, electrical impedance testing, and X-ray computed tomography have been investigated for this purpose using specially produced samples with biased or random Fiber orientations. We demonstrate the capabilities of each of these NDT techniques for fiber orientation measurements and draw conclusions based on these results about the most promising areas for future research and development. KW - Spectral induced polarization KW - Steel fiber reiniforced concrete KW - Fiber orientation KW - Non-destructive testing KW - Micro-computed tomography KW - Ultrasound PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543520 DO - https://doi.org/10.3390/app12020697 VL - 12 IS - 2 SP - 1 EP - 14 PB - MDPI CY - Basel Switzerland AN - OPUS4-54352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - 3D imaging and residual stress analysis of AM materials at BAM N2 - The overview of the activity of group 8.5 Micro-NDT (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). T2 - Seminar at Chalmers University and Centre for Additive Manufacture (CAM2) CY - Gothenburg, Sweden DA - 19.05.2022 KW - Additive manufacturing KW - Laser powder bed fusion KW - Residual stress KW - Computed tomography KW - Synchrotron X-ray diffraction KW - X-ray refraction PY - 2022 AN - OPUS4-55019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roveda, Ilaria T1 - Investigation of residual stresses and microstructure effects on the fatigue behaviour of a L-PBF AlSi10Mg alloy N2 - Laser Powder Bed Fusion (L-PBF) allow the fabrication of lightweight near net shape AlSi10Mg components attractive to the aerospace, automotive, biomedical and military industries. During the build-up process, high cooling rates occur. Thus, L-PBF AlSi10Mg alloys exhibit a Si-nanostructure in the as-built condition, which leads to superior mechanical properties compared to conventional cast materials. At the same time, such high thermal gradients generally involve a deleterious residual stress (RS) state that needs to be assessed during the design process, before placing a component in service. To this purpose post-process heat treatments are commonly performed to relieve detrimental RS. In this contribution two low-temperature stress-relief heat treatments (SRHT) are studied and compared with the as-built state: a SRHT at 265°C for 1 hour and a SRHT at 300°C for 2 hours. At these temperatures microstructural changes occur. In the as-built state, Si atoms are supersaturated in the α-aluminium matrix, which is enveloped by a eutectic Si-network. At 265°C the Si precipitation from the matrix to the pre-existing network is triggered. Thereafter, above 295°C the fragmentation and spheroidization of the Si branches takes place, presumably by Al–Si interdiffusion. After 2 hours the original eutectic network is completely replaced by uniformly distributed blocky particles. The effect of the heat and the microstructure modification on the RS state and the fatigue properties is investigated. Energy dispersive x-ray and neutron diffraction are combined to investigate the near-surface and bulk RS state of a L-PBF AlSi10Mg material. Differences in the endurance limit are evaluated experimentally by high cycle fatigue (HCF) tests and cyclic R-curve determination. T2 - 43rd Materials Mechanics Seminar CY - Sani, Chalkidiki, Greece DA - 05.06.2022 KW - AlSi10Mg KW - Fatigue KW - Neutron diffraction KW - X-ray diffraction PY - 2022 AN - OPUS4-55090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - 3D Imaging and residual stress analysis of additively manufactured materials N2 - The focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of additively manufactured (AM) materials in BAM (Berlin, Germany). The manufacturing defects and high RS are inherent of AM techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads. T2 - The International Symposium on Nondestructive Characterization of Materials 2023 CY - Zurich, Switzerland DA - 15.08.2023 KW - Additive manufacturing KW - Residual stress KW - X-ray computed tomography PY - 2023 AN - OPUS4-58113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khrapov, D. A1 - Kozadayeva, M. A1 - Koptyug, A. A1 - Mishurova, Tatiana A1 - Meinel, Dietmar A1 - Surmenev, R. A1 - Surmeneva, M. T1 - Geometrical features and mechanical properties of the sheet-based gyroid scaffolds with functionally graded porosity manufactured by electron beam melting N2 - Functionally graded porous scaffolds (FGPS) constructed with pores of different size arranged as spatially continuous structure based on sheet-based gyroid with three different scaling factors of 0.05, 0.1 and 0.2 were produced by electron beam powder bed fusion. The pore dimensions of the obtained scaffolds satisfy the values required for optimal bone tissue ingrowth. Agglomerates of residual powder were found inside all structures, which required post-manufacturing treatment. Using X-ray Computed Tomography powder agglomerations were visualized and average wall thickness, wall-to-wall distances, micro- and macro-porosities were evaluated. The initial cleaning by powder recovery system (PRS) was insufficient for complete powder removal. Additional treatment by dry ultrasonic vibration (USV) was applied and was found successful for gyroids with the scaling factors of 0.05 and 0.1. Mechanical properties of the samples, including quasi-elastic gradients and first maximum compressive strengths of the structures before and after USV were evaluated to prove that additional treatment does not produce structural damage. The estimated quasi-elastic gradients for gyroids with different scaling factors lie in a range between 2.5 and 2.9 GPa, while the first maximum compressive strength vary from 52.5 for to 59.8 MPa, compressive offset stress vary from 46.2 for to 53.2 MPa. KW - Additive manufacturing KW - Electron beam KW - Powder bed fusion KW - Triply periodic minimal surfaces KW - Functionally graded porous scaffolds KW - X-ray computed tomography PY - 2023 DO - https://doi.org/10.1016/j.mtcomm.2023.106410 SN - 2352-4928 VL - 35 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-57682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obaton, A.-F. A1 - Fain, J. A1 - Meinel, Dietmar A1 - Tsamos, Athanasios A1 - Léonard, F. A1 - Lécuelle, B. A1 - Djemaï, M. T1 - In Vivo Bone Progression in and around Lattice Implants Additively Manufactured with a New Titanium Alloy N2 - The osseointegration in/around additively manufactured (AM) lattice structures of a new titanium alloy, Ti–19Nb–14Zr, was evaluated. Different lattices with increasingly high sidewalls gradually closing them were manufactured and implanted in sheep. After removal, the bone–interface implant (BII) and bone–implant contact (BIC) were studied from 3D X-ray computed tomography images. Measured BII of less than 10 µm and BIC of 95% are evidence of excellent osseointegration. Since AMnaturally leads to a high-roughness surface finish, the wettability of the implant is increased. The new alloy possesses an increased affinity to the bone. The lattice provides crevices in which the biological tissue can jump in and cling. The combination of these factors is pushing ossification beyond its natural limits. Therefore, the quality and speed of the ossification and osseointegration in/around these Ti–19Nb–14Zr 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. Thus, this new titanium alloy and such laterally closed lattice structures are appropriate candidates to be implemented in a new generation of implants. KW - Osseointegration KW - X-ray computed tomography KW - Additive manufacturing KW - Machine learning segmentation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-577066 DO - https://doi.org/10.3390/app13127282 VL - 13 IS - 12 SP - 1 EP - 18 PB - MDPI CY - Basel, Switzerland AN - OPUS4-57706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - Applications of x-ray computed tomography in material science N2 - The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field material characterization by X-ray imaging is presented. The principle of X-ray Computed Tomography (XCT) is explained. The multiple examples of application of quantitative analysis by XCT are reported, such as additive manufacturing, Li-ion battery, concrete research. T2 - Lecture for PhD students at Politecnico di Torino CY - Turin, Italy DA - 14.03.2024 KW - X-ray computed tomography KW - Additive manufacturing PY - 2024 AN - OPUS4-59689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Barzegar, M. A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Mishurova, Tatiana A1 - Pasadas, Dario J. A1 - Ribeiro, Artur L. A1 - Ramos, Helena G. T1 - Adhesive Porosity Analysis of Composite Adhesive Joints Using Ultrasonic Guided Waves N2 - Adhesively bonded composite joints can develop voids and porosity during fabrication, leading to stress concentration and a reduced load-carrying capacity. Hence, adhesive porosity analysis during the fabrication is crucial to ensure the required quality and reliability. Ultrasonic-guided wave (UGW)-based techniques without advanced signal processing often provide low-resolution imaging and can be ineffective for detecting small-size defects. This article proposes a damage imaging process for adhesive porosity analysis of bonded composite plates using UGWs measured by scanning laser Doppler vibrometer (LDV). To implement this approach, a piezoelectric transducer is mounted on the composite joint specimen to generate UGWs, which are measured over a densely sampled area. The signals obtained from the scan are processed using the proposed signal processing in different domains. Through the utilization of filter banks in frequency and wavenumber domains, along with the root-mean-square calculation of filtered signals, damage images of the adhesive region are obtained. It has been observed that different filters provide information related to different void sizes. Combining all the images reconstructed by filters, a final image is obtained which contains damages of various sizes. The images obtained by the proposed method are verified by radiography results and the porosity analysis is presented. The results indicate that the proposed methodology can detect the pores with the smallest detectable pore area of 2.41 mm^2, corresponding to a radius of 0.88 mm, with an overall tendency to overestimate the pore size by an average of 11%. KW - Adhesives KW - Damage imaging KW - Nondestructive testing (NDT) KW - Porosity analysis KW - Signal processing KW - Ultrasonic guided waves (UGWs) PY - 2024 DO - https://doi.org/10.1109/TUFFC.2024.3371671 VL - 71 IS - 4 SP - 485 EP - 495 PB - Institute of Electrical and Electronics Engineers (IEEE) AN - OPUS4-59970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - In-situ hot isostatic pressing combined with x-ray imaging and diffraction of laser powder bed fusion ti-6al-4v N2 - Hot Isostatic Pressing (HIP) is often introduced to tackle the porosity issue in additively manufactured (AM) materials. For instance, HIP post-processing is recommended to improve fatigue resistance of Laser powder bed fusion (PBF-LB) manufactured parts [1, 2]. Even though HIP cannot completely remove porosity, it significantly decreases the defect population and its average size below the critical threshold value leading to early crack initiation. In the present study, in-situ investigation of HIP procedure of PBF-LB Ti-6Al-4V parts was carried out to gain further insights into the densification mechanism occurring during HIP. The in-situ observations at high pressure and high temperature are uniquely possible at the PSICHE beamline of the Soleil synchrotron (France), thanks to the Ultrafast Tomography on a Paris-Edinburgh Cell (UToPEC) and the combination of the fast phase-contrast tomography and energy-dispersive diffraction [3, 4]. A detailed methodology was developed to ensure that the correct pressure and temperature were maintained during the experiments. The results allowed an estimation of the global dentification rate during HIP of PBF-LB Ti-Al-4V material, as well as a detailed quantitative characterization of the influence of pore size and shape on the densification process, thereby understanding the effectiveness of HIP process on different pore categories. After 20 mins, 75% of porosity can be considered as closed or has size below the resolution of the XCT reconstruction. We also observed that the smallest defects showed higher densification rate, while the defect shape did not have significant effect on such rate. The current development of in-situ HIP experiment allows experimental quantification and validation of the simulation work. Ultimately it paves the road to tailoring the HIP procedure for different materials depending on the porosity and microstructure. T2 - AAMS 2023 CY - Madrid, Spain DA - 26.09.23 KW - Additive manufacturing KW - HIP KW - X-ray computed tomography PY - 2023 AN - OPUS4-58482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - 3D imaging and residual stress analysis for AM Materials N2 - 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). T2 - Seminar at Integrated Additive Manufacturing center, Politecnico Torino CY - Turin, Italy DA - 14.02.2023 KW - Additive manufacturing KW - Laser powder bed fusion KW - Residual stress KW - Computed tomography KW - Synchrotron X-ray diffraction PY - 2023 AN - OPUS4-57047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kinne, R. W. A1 - Gunnella, F. A1 - Kunisch, E. A1 - Heinemann, S. A1 - Nies, B. A1 - Maenz, S. A1 - Horbert, V. A1 - Illerhaus, Bernhard A1 - Huber, R. A1 - Firkowska-Boden, I. A1 - Bossert, J. A1 - Jandt, K. D. A1 - Sachse, A. A1 - Bungartz, M. A1 - Brinkmann, O. T1 - Performance of calcium phosphate cements in the augmentation of sheep vertebrae - An ex vivo study N2 - Oil-based calcium phosphate cement (Paste-CPC) shows not only prolonged shelf life and injection times, but also improved cohesion and reproducibility during application, while retaining the advantages of fast setting, mechanical strength, and biocompatibility. In addition, poly(L-lactideco-glycolide) (PLGA) fiber reinforcement may decrease the risk for local extrusion. Bone defects (diameter 5 mm; depth 15 mm) generated ex vivo in lumbar (L) spines of female Merino sheep (2–4 years) were augmented using: (i) water-based CPC with 10% PLGA fiber reinforcement (L3); (ii) Paste-CPC (L4); or (iii) clinically established polymethylmethacrylate (PMMA) bone cement (L5). Untouched (L1) and empty vertebrae (L2) served as controls. Cement performance was analyzed using micro-computed tomography, histology, and biomechanical testing. Extrusion was comparable for Paste-CPC(-PLGA) and PMMA, but significantly lower for CPC + PLGA. Compressive strength and Young’s modulus were similar for Paste-CPC and PMMA, but significantly higher compared to those for empty defects and/or CPC + PLGA. Expectedly, all experimental groups showed significantly or numerically lower compressive strength and Young’s modulus than those of untouched controls. Ready-to-use Paste-CPC demonstrates a performance similar to that of PMMA, but improved biomechanics compared to those of water-based CPC + PLGA, expanding the therapeutic arsenal for bone defects. O, significantly lower extrusion of CPC + PLGA fibers into adjacent lumbar spongiosa may help to reduce the risk of local extrusion in spinal surgery. KW - Sheep KW - PMMA KW - Calcium phosphate bone cement KW - Oil-based KW - Ready-to-use KW - Water-based KW - Micro-CT KW - Compressive strength KW - Young’s modulus PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569072 DO - https://doi.org/10.3390/ma14143873 SN - 1996-1944 VL - 14 IS - 14 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-56907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hohendorf, Stefan T1 - Medea und Jason, Eine Radiologische Untersuchung im Neuen Palais Potsdam N2 - Seit der Antike gehört die Medea-Sage zu den bekanntesten Geschichten der Weltliteratur. Der berühmte französische Künstler Carle Van Loo hat sich dieses Epos um 1759 angenommen und ein beeindruckendes Ölgemälde mit Abmessungen von 2,30x3,28m² erschaffen. Mit Mademoiselle Clairon als Medea und Henri Louis Le Kain als Jason ist ein Kunstwerk entstanden, das seitdem einige Veränderungen und Restaurierungen erfahren hat. Die Bundesanstalt für Materialforschung und -prüfung (BAM) hatte 2020 die Möglichkeit, dieses und ein zweites Kunstwerk, im Neuen Palais in Potsdam, für die Stiftung Preußische Schlösser und Gärten Berlin-Brandenburg, radiografisch zu untersuchen. Hierbei wurden sowohl technologisch als auch kunsthistorisch einige interessante Entdeckungen gemacht, die im vorliegenden Beitrag vorgestellt werden. T2 - DGZfP Jahrestatung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Röntgen KW - X-Ray KW - Kunsstechnologisch KW - Gemälde KW - Untermalung KW - Speicherfolie KW - Strahlenschutz PY - 2022 AN - OPUS4-56577 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pavasarytė, Lina A1 - Azevedo do Nascimento, Allana A1 - Cysne Barbosa, Ana Paula A1 - Trappe, Volker A1 - Melo, Daniel T1 - Effects of particle size and particle concentration of poly (ethylene-co-methacrylic acid) on properties of epoxy resin N2 - Self-healing polymers have been developed to improve durability and reduce costs associated with maintenance during service. The addition of thermoplastics to thermosets to produce mendable polymers appears as a promising selfhealing technique. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was added to epoxy resin and the effects of EMAA addition on epoxy properties were evaluated. Specimens with two different contents of thermoplastic and particles sizes were manufactured. A two-level full factorial experimental design was used to evaluate the effect of particle size and particle content on properties of epoxy modified with addition of EMAA. Tensile tests and dynamic mechanical analysis (DMA) were used and the evaluated responses were tensile strength, modulus of elasticity, and glass transition temperature (Tg). X-ray computed tomography (XCT) was used to investigate particle size and concentration after manufacturing. It was found that the particle concentration has greater effects on stress–strain behavior of epoxy while Tg was not significantly affected by neither of the analyzed entrance variables. KW - Fracture KW - Self-healing KW - Epoxy KW - Thermoplastic PY - 2024 DO - https://doi.org/10.1002/app.55677 SN - 0021-8995 SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-60205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, André A1 - Hasenbein, Ines A1 - Hortschansky, Peter A1 - Schmuck, Klaus D. A1 - Maenz, Stefan A1 - Illerhaus, Bernhard A1 - Kuehmstedt, Peter A1 - Ramm, Roland A1 - Huber, René A1 - Kunisch, Elke A1 - Horbert, Victoria A1 - Gunnella, Francesca A1 - Roth, Andreas A1 - Schubert, Harald A1 - Kinne, Raimund W. T1 - BMP-2 (and partially GDF-5) coating significantly accelerates and augments bone formation close to hydroxyapatite/tricalcium-phosphate/brushite implant cylinders for tibial bone defects in senile, osteopenic sheep N2 - Bilateral defects (diameter 8 mm) in the medial tibial head of senile, osteopenic female sheep (n = 48; 9.63 ± 0.10 years; mean ± SEM) were treated with hydroxyapatite (HA)/beta-tricalcium phosphate (β-TCP)/dicalcium phosphate dihydrate (DCPD; brushite) cylinders coated with BMP-2 (25 or 250 micrograms) or growth differentiation factor (GDF)-5 (125 or 1250 micrograms; left side); cylinders without BMP served as controls (right side). Three, 6, and 9 months post-operation (n = 6 each group), bone structure and formation were analyzed in vivo by X-ray and ex vivo by osteodensitometry, histomorphometry, and micro-computed tomography (micro-CT) at 3 and 9 months. Semi-quantitative X-ray evaluation showed significantly increasing bone densities around all implant cylinders over time. High-dose BMP-2-coated cylinders (3 and 9 months) and low-dose GDF-5-coated cylinders (3 and 6 months) demonstrated significantly higher densities than controls (dose-dependent for BMP-2 at 3 months). This was confirmed by osteodensitometry at 9 months for high-dose BMP-2-coated cylinders (and selected GDF-5 groups), and was again dose-dependent for BMP-2. Osteoinduction by BMP-2 was most pronounced in the adjacent bone marrow (dynamic histomorphometry/micro-CT). BMP-2 (and partially GDF-5) significantly increased the bone formation in the vicinity of HA/TCP/DCPD cylinders used to fill tibial bone defects in senile osteopenic sheep and may be suitable for surgical therapy of critical size, non-load-bearing bone defects in cases of failed tibial head fracture or defect healing. KW - Bone morphogenetic protein (BMP) KW - Growth differentiation factor (GDF) KW - Bone replacement material PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623923 DO - https://doi.org/10.1007/s10856-023-06734-2 SN - 1573-4838 VL - 34 IS - 7 SP - 1 EP - 15 PB - Springer Science and Business Media LLC CY - Dordrecht AN - OPUS4-62392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Weise, Frank A1 - Oesch, T. A1 - Wilsch, Gerd A1 - Sigmund, S. A1 - Hünger, K.-J. A1 - Kositz, M. T1 - Analyse des gefügeabhängigen Löslichkeitsverhaltens potenziell AKR-empfindlicher Gesteinskörnungen T1 - Analysis of the microstructure depending solubility behavior of potential ASR sensitive aggregates N2 - Das gefügeabhängige Löslichkeitsverhalten wurde an folgenden vier Gesteinskörnungen unterschiedlicher Alkaliempfindlichkeitsklassen untersucht: • GK1 (EIII-S): quarzreicher Kies • GK2 (EIII-S): Grauwacke (Splitt) • GK3 (EI-S): Quarz-Feldspat-Porphyr (Splitt) • GK4 (EI-S): sandsteinreicher Kies DiePorenstrukturanalyse erfolgte sowohl an Einzelkörnern mittels vergleichender 3D-CT und BET- Untersuchungen als auch an Korngemengen der einzelnen Kornfraktionen (außer Fraktion 16/22 mm) über die Wasseraufnahme und mit BET. Für die Visualisierung und Quantifizierung der von außen zugänglichen Oberflächenanteile der Einzelkörner wurde ein Softwaretool entwickelt, erprobt und erfolgreich angewandt. Es gelang so u.a. den Nachweis zu erbringen, dass die gebrochenen Einzelkörner der Grauwacke und des Rhyoliths einen deutlich geringeren von außen zugänglichen Oberflächenanteil als die gleichartigen Gesteinskörner aus dem Kies besitzen. Aufgrund der limitierten Ortsauflösung der 3D-CT von 11 bis 16,5 μm wurde mit BET eine um drei Zehnerpotenzen höhere spezifische Oberfläche ermittelt. Zu den Porositätsuntersuchungen an den Korngemengen sei angemerkt, dass zum Teil gegenläufige Trends zwischen offener Porosität und spezifischer Oberfläche festgestellt wurden. Dieses ist beim Bezug des bei den Löseversuchen in 0,1 M KOH mit definierter NaCl-Zugabe aus der Gesteinskörnung gelösten SiO2 und Al2O3 von zentraler Bedeutung. Bei den Löseversuchen an den fraktionsspezifischen Korngemengen selbst zeigte sich, dass die stufenweise Erhöhung des NaCl-Gehalts von 0 auf 10 M.-% im Eluat eine erhöhte SiO2-Löslichkeit und eine verminderte Auslaugung von Al2O3 zur Folge hat. Auffallend war hierbei, dass die Al2O3-Löslichkeit bei GK4 ohne und mit geringer NaCl-Zugabe die mit Abstand höchsten Werte annimmt. Bei den zusätzlich durchgeführten Löseversuchen an den tomografierten Einzelkörnern in 1 M KOH-Lösung mit Zugabe von 1 M.-% NaCl zeigte sich, dass nur vereinzelt bei den untersuchten Gesteinsarten eine Korrelation zwischen dem SiO2- bzw. Al2O3-Gehalt im Eluat und der absoluten BET-Oberfläche nachweisbar ist. Dies ist vermutlich darauf zurückzuführen, dass neben der Oberfläche weitere Parameter (z.B. die mineralogische Zusammensetzung der Einzelkörner) das Löseverhalten maßgebend beeinflussen. Bei den parallel zu den Löseversuchen durchgeführten Betonversuchen nach dem ARS 04/2013 zeigte sich, dass die Alkaliempfindlichkeit der GK4 bei beiden Betonversuchen mit Alkalizufuhr unterschiedlich zu bewerten ist. So ist unabhängig von der vorgegebenen pessimalen Betonrezeptur des Fahrbahndeckenbetons ausschließlich bei der Klimawechsellagerung die GK4 als alkaliempfindlich einzustufen. Allerdings konnte der Befund der stark ausgeprägten AKR bei der GK4 mit der Dünnschliffmikroskopie nicht bestätigt werden. Analoges gilt für die Bewertung der Alkaliempfindlichkeit von GK2 mit den Betonversuchen nach der Alkalirichtlichtlinie des DAfStb. So ist auch hier die GK2 nicht im 60 °C-Betonversuch sondern ausschließlich im 40 °C-Betonversuch als alkaliempfindlich einzustufen. Dienach den verschiedenartigen Betonversuchen durchgeführten LIBS-Analysen am Vertikalschnitt der Prüfkörper zeigen, dass im Kernbereich nach dem 60 °C-Betonversuch mit 10 %iger NaCl-Lösung und nach der Klimawechsellagerung mit NaCl-Beaufschlagung annähernd gleich hohe Natrium- und Chloridgehalte vorgefunden werden. Wider Erwarten treten an den beaufschlagten Prüfflächen Abreicherungen von Natrium und Anreicherungen von Chlorid auf. Im 40°C- und 60 °C-Betonversuch wurde das Natrium bis in eine maximale Tiefe von ca. 30 mm bzw. 20 mm ausgelaugt. Die aufbauenden korrelativen Betrachtungen zwischen den Ergebnissen des 60°C Betonversuchs mit Alkalizufuhr und der Löseversuche an den fraktionsspezifischen Korngemengen in 1 M KOH-Lösung mit definierter NaCl-Zugabe sind durchaus vielversprechend. So zeigt sich beispielsweise beim Waschbeton, dass der fraktionsspezifisch gewichtete SiO2-Überschuss im Eluat nach 56 Tagen mit Zugabe von 0,5 M.-% NaCl ohne Bezug auf die BET-Oberfläche zur gleichen Einstufung der vier betrachteten Gesteinskörnungen wie bei den Dehnungen im 60 °C-Betonversuch mit 3 %-iger NaCl-Lösung führt. Außerdem korrelieren die im 60 °C-Betonversuch mit 10 %-iger NaCl-Lösung ermittelten Dehnungen mit dem gewichteten SiO2-Überschuss im Eluat bei Zugabe von 2 M.-% NaCl ohne Bezug auf die BET-Oberfläche. Ausschließlich bei den Betonversuchen nach der Alkali-Richtlinie erwies sich der Bezug des im Eluat ermittelten SiO2-Überschusses auf die BET-Oberfläche als zielführend. Aufgrund des Potenzials der Löseversuche mit NaCl-Zugabe für die Bewertung der Alkaliempfindlichkeit der Gesteinskörnung im Fahrbahndeckenbeton wird empfohlen, die vergleichenden Untersuchungen zwischen den Löseversuchen an Korngemischen der einzelnen Fraktionen und den Betonversuchen nach dem ARS 04/2013 mit einer möglichst hohen Anzahl an Gesteinskörnungen und einem präzisierten Untersuchungsumfang fortzuführen. N2 - The following four aggregates (GK) of varying grades of alkali sensitivity were examined for their microstructure-dependent solubility behavior: • GK1 (EIII-S) gravel with high quarz content • GK2 (EIII-S) greywacke (crushed stone) • GK3 (EI-S) quarz-feldspar-porphyry (crushed stone) • GK4 (EI-S) gravel with high sandstone content Pore structure analysis was carried out both on single grains using comparative 3D-CT and BET tests, and on grain samples of individual grain fractions (excluding the 16/22 mm fraction) using water absorption and BET. A software tool for visualizing and quantifying the externally accessible surfaces of single grains was developed, tested and successfully applied. This enabled us, among other things, to prove that single broken grains of greywacke and rhyolite have a much smaller externally accessible surface than grains of gravel of the same aggregate fraction. Due to the 3D-CT’s limited spatial resolution of 11 to 16.5 μm, BET was used to determine a two to three powers of ten higher specific surface. In relation to the porosity tests of the grain samples, it should be noted that in some cases, counterdirectional trends between open porosity and specific surface were determined. This is of central importance in relation to the SiO2 and Al2O3 dissolved from the aggregate in the solubility tests in 1 M KOH with defined addition of NaCl. The solubility tests on the grain samples of specific fractions showed that the gradual increase of the NaCl content in the eluate from 0 to 10 M.-% resulted in increased SiO2 solubility and reduced leaching of Al2O3. It was striking in this context that the solubility of Al2O3 in GK4 with no or little addition of NaCl gives by far the highest values. The additional solubility tests carried out on single grains, that were previously subjected to CT testing, in 1 M KOH solution with 1 M.-% added NaCl showed that in the types of aggregate examined, a correlation between the SiO2 and Al2O3 in eluate and the absolute BET surface is only occasionally demonstrable. This is probably due to the fact that solubility behavior is decisively influenced by other parameters in addition to the surface (e.g. by the mineralogical composition of individual grains). The concrete tests according to ARS 04/2013 carried out parallel to the solubility tests showed that GK4’s alkali sensitivity in both concrete tests with added alkali must be evaluated differently. For example, independent of the prescribed pessimal road surface concrete formula, GK4 can only be classified as alkali sensitive under cyclic storage. However petrographic microscopy could not confirm the findings of very marked ASR in GK4. The same applies to the evaluation of alkali sensitivity in GK2 with the concrete tests according to the German Committee for Structural Concrete (DAfStb)’s Alkali Guidelines. In this case too, GK2 should not be classified as alkali sensitive in 60 °C concrete testing, but only in 40 °C concrete testing. The LIBS analyses carried out on the vertical cross-section of the test specimens after the various concrete tests showed that almost equally high sodium and chloride levels were found in the core area after the 60 °C concrete prism test with 10 % NaCl solution and after cyclic storage with NaCl application. Contrary to expectations, the surfaces of samples after NaCl application showed a decrease in sodium and an increase in chloride. In the 40°C and 60°C concrete prism tests, sodium was depleted up to a maximum depth of approx. 30 mm and 20 mm respectively. Subsequent correlative observations between the findings of the 60°C concrete prism test with alkali application, and the solubility tests on the samples of specific grain fractions in 1 M KOH solution with defined NaCl addition, are very promising. In the case of exposed aggregate concrete, for example, the fraction-specific weighted excess SiO2 to in the eluate after 56 days with added 0.5 M.-% NaCl unrelated to the BET surface results in the same classification of the four aggregates examined as the expansions in the 60 °C concrete prism test with 3% NaCl solution. In addition, the expansions found in the 60 °C concrete prism test with 10% NaCl solution correlated with the weighted excess SiO2 in eluate with added 2 M.-% NaCl without relation to the BET surface. Only in the case of the concrete test in accordance with the Alkali Guidelines did the relationship of the excess SiO2 in the eluate to the BET surface prove to be productive. Due to the potential of the solubility test with added NaCl for the evaluation of alkali sensitivity of aggregates in road surface concrete, we recommend continuing with comparative tests between solubility tests of grain samples of the various fractions and the concrete tests in accordance with ARS O4/13 with the greatest possible number of aggregates and a precisely defined investigation scope. KW - LIBS KW - Betonfahrbahndecke KW - Alkali-Kieselsäure-Reaktion KW - Gesteinskörnung KW - Alkaliempfindlichkeit KW - 3D-CT KW - Tausalzeintrag PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:hbz:opus-bast-25832 UR - https://bast.opus.hbz-nrw.de/frontdoor/index/index/docId/2583 SN - 978-3-95606-648-1 SN - 0943-9323 VL - S 165 SP - 1 EP - 111 PB - Fachverlag NW in der Carl Ed. Schünemann KG CY - Bremen AN - OPUS4-54755 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andrade, C. A1 - Saucedo, L. A1 - Rebolledo, N. A1 - Cabeza, S. A1 - Meinel, Dietmar T1 - X-Ray computed tomography and traditional analysis of a capillary absorption test in cement pastes N2 - Water absorption testing has the attraction of being simple, relatively quick and use water as a fluid which is the key substance in the possible concrete deterioration. However, in spite of the advantages its application has remained empirical, except for the testing of resistance to frost, through the identification of the critical degree of saturation. Rilem TC-116 studied this test, among others, for the characterization of concrete resistance against transport through the concrete pore network. Results indicated a low discriminating ability of the absorbency for qualifying concrete resistance and then, it seemed necessary to try to move forward by making the link between the absorption testing and the concrete pore microstructure. In the present work, thanks to the X-Ray computed tomography, it is described the evolution of the water front in three paste-specimen with different w/c ratios (different pore radius distributions). The observations allowed us to deduce that all the pores start to fill simultaneously, but the bigger ones fill quicker and rise less. The saturation degree is measured along the height of the sample, showing that each pore size has a different rate which becomes constant after the first hour. Washburn’s equation was applied to the progressive advance of the water front, resulting in a pore radius much smaller than the one expected. KW - Capillary absorption KW - Pore size distribution KW - X-ray CT KW - Gravimetry PY - 2020 DO - https://doi.org/10.1016/j.cemconcomp.2020.103634 VL - 113 SP - 103634 PB - Elsevier Ltd. CY - London AN - OPUS4-51487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hashemi, Seyedreza A1 - Zscherpel, Uwe T1 - Measurement of Focal Spots of X-ray Tubes Using a CT Reconstruction Approach on Edge Images of Large Holes and Comparison to Pinhole Imaging N2 - The first Non-destructive testing (NDT) method which evolved in the industrial age was radiographic testing (RT). Among all NDT methods, RT is no exception, so there are still many issues for optimizations even today. One of them is the measurement of the focal spot of X-ray tubes. The size of the focal spot is critical for imaging, because it determines the spatial resolution in the X-ray image. The classical way to evaluate focal spots of X-ray tubes is by pinhole imaging using a camera obscura. But this method has a natural lower limit, which is defined by the diameter of the pinhole used (today min. 10 µm). Therefore, focal spot sizes lower than 50 µm diameter cannot be imaged and measured correctly. An alternative approach, which permits this, was investigated here using the edge unsharpness of holes much larger than the focal spot size. The results of both methods were compared using 3 different X-ray tubes. KW - Reconstruction method KW - Radiographic testing (RT) using X-rays KW - Focal spot measurement KW - Edge unsharpness KW - X-ray tubes KW - Pinhole imaging KW - Computed Tomography (CT) KW - Focal Spot (FS) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608646 DO - https://doi.org/10.58286/29556 SN - 2941-4989 SP - 1 EP - 9 PB - NDT.net CY - Berlin, Germany AN - OPUS4-60864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -