TY - JOUR A1 - Buzolin, R. H. A1 - Richter, Tim A1 - Pixner, F. A1 - Rhode, Michael A1 - Schroepfer, Dirk A1 - Enzinger, N. T1 - Microstructure characterisation of multi-principal element alloys welds produced by electron beam welding N2 - This work explores the feasibility of producing bead-on-plate welds of a CrCoNi medium entropy alloy and a CrMnFeCoNi high entropy alloy using electron beam welding. The alloys were welded in two states: one in an as-cold-rolled condition and the other in an annealed condition. In addition, the materials are welded with two different parameters. The FCC microstructure of the welds is investigated using scanning electron microscopy assisted by energy-dispersive X-ray spectroscopy and electron-backscattered diffraction. The impact of the weld on the microstructure is discussed. The heat-affected zone is negligible for the annealed condition of both medium and high entropy alloys since there is no driving force for recrystallisation and the exposure time to high temperature is insufficient for grain coarsening. The texture formed in the fusion zone is also discussed and compared to the texture in the base metal and the heat-affected zone. Although the grain growth along the (100) crystallographic direction is preferential in all cases, the crystallographic texture type differs from each weld. Higher hardness values are measured in the medium entropy alloy’s base metal and fusion zone than in the high entropy alloy. KW - Multi-principal element alloy KW - Electron backscattered diffraction KW - Electron beam welding KW - High-entropy alloy KW - Microstructure characterization PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568129 DO - https://doi.org/10.1016/j.matdes.2023.111609 SN - 1873-4197 VL - 225 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Can, S. Z. A1 - Engin, B. A. A1 - İşleyen, A. A1 - Jotanovic, A. A1 - Acosta, O. A1 - Prina, P. A1 - Schvartz, M. A1 - Savić, M. A1 - Stojanović, M. A1 - Ahumada, D. A. A1 - Abella, J. P. A1 - Näykki, T. A1 - Saro-Aho, T. A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Rienitz, O. A1 - Noordmann, J. A1 - Pape, C. A1 - Towara, J. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Ketrin, R. A1 - Mardika, E. A1 - Komalasari, I. A1 - Elishian, C. A1 - Naujalis, E. A1 - Knašienė, B. A1 - Uribe, C. A1 - Carrasco, E. A1 - Zoń, A. A1 - Warzywoda, B. A1 - Stakheev, A. A1 - Dobrovolskiy, V. A1 - Stolboushkina, T. A1 - Glinkova, A. A1 - Sobina, E. A1 - Tabatchikova, T. A1 - Gažević, L. A1 - Paunovic, M. A1 - Jaćimović, R. A1 - Zuliani, T. A1 - Zambra, R. P. A1 - Napoli, R. T1 - Determination of elements in river water N2 - The need for quality assessment of anthropogenic impact on environmental pollution is increasing due to discharge from various industries, the use of chemicals in agriculture and the consumption of fossil fuels. Diminishing resources such as natural waters used for the cultivation of agricultural products, plant and animal habitats are under severe pollution pressure and are at constant risk. Several parameters, such as Pb, Cd, Ni, Hg were listed by Water Framework Directive in Directive(2008/105/EC) in the priority substances. Cadmium and Hg were identified as priority hazardous substances whereas As is an important contaminant for its potential toxicological and carcinogenic effects. An inter-comparison study is organised in EURAMET TC-MC in order to demonstrate the capability participants for measuring five elements in river water. The participants carried out measurements for analytes: Pb, Cd, Ni and As as mandatory elements, and Se as an optional one. Participants were asked to perform the measurements with respect to the protocol provided. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - Metrology KW - Traceability KW - Toxic elements KW - River water PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08001 VL - 60 IS - 1a SP - 1 EP - 40 PB - BIPM & IOP Publishing Ltd AN - OPUS4-56786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stein, L. A1 - Wang, Cui A1 - Förster, C. A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Bulky ligands protect molecular ruby from oxygen quenching N2 - Chromium(III) complexes can show phosphorescence from the spin-flip excited doublet states 2E/2T1 in the near-infrared with high photoluminescence quantum yields and extremely long lifetimes in the absence of dioxygen. The prototype molecular ruby, [Cr(ddpd)2]3+ (ddpd = N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine), has a photoluminescence quantum yield and a luminescence lifetime of 13.7% and 1.1 ms in deaerated acetonitrile, respectively. However, its luminescence is strongly quenched by 3O2 via an efficient Dexter-type energy transfer process. To enable luminescence applications of molecular rubies in solution under aerobic conditions, we explored the potential of sterically demanding ddpd ligands to shield the chromium(III) center from O2 using steady state and time-resolved photoluminescence spectroscopy. The structures of the novel complexes with sterically demanding ligands were investigated by single crystal X-ray diffraction and quantum chemically by density functional theory calculations. The O2 sensitivity of the photoluminescence was derived from absolutely measured photoluminescence quantum yields and excited state lifetimes under inert and aerobic conditions and by Stern–Volmer analyses of these data. Optimal sterically shielded chromium(III) complexes revealed photoluminescence quantum yields of up to 5.1% and excited state lifetimes of 518 μs in air-saturated acetonitrile, underlining the large potential of this ligand design approach to broaden the applicability of highly emissive chromium(III) complexes. KW - Fluorescence KW - Synthesis KW - Production KW - Optical spectroscopy KW - Ligand KW - Photophysics KW - Cr(III) KW - Mechanism KW - NIR KW - Sensor KW - Oxygen PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570807 DO - https://doi.org/10.1039/d2dt02950b VL - 51 IS - 46 SP - 17664 EP - 17670 PB - The Royal Society of Chemistry CY - Berlin AN - OPUS4-57080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, T. A1 - Wang, J. A1 - Cheng, Z. A1 - Liu, Y. A1 - Qiao, X. A1 - Wen, J. A1 - Resch-Genger, Ute A1 - Long, W. A1 - Ou, J. T1 - NaYF4:Yb3+/Tm3+@NaYF4:Yb3+ Upconversion Nanoparticles for Optical Temperature Monitoring and Self-Heating in Photothermal Therapy N2 - The core−shell NaYF4:Yb3+/Tm3+@NaYF4:Yb3+ upconversion nanoparticles were successfully prepared by a solvothermal method, and a layer of mesoporous silica (mSiO2) was successfully coated on the periphery of the core−shell nanoparticles to transform their surface from lipophilic to hydrophilic, further expanding their applications in biological tissues. The physical phase, morphology, structure, and fluorescence properties were characterized by X-ray diffraction (XRD), field emission transmission electron microscopy (TEM), Fourier infrared spectroscopy (FT-IR), ζ potential analysis, and fluorescence spectroscopy. It was found that the material has a hexagonal structure with good hydrophilicity and emits intense fluorescence under 980 nm pump laser excitation. The non-contact temperature sensing performance of nanoparticles was evaluated by analyzing the upconversion fluorescence of Tm3+ (1G4 → 3F4 and 3F3 → 3H6) in the temperature range of 284−344 K. The absolute and relative sensitivities were found to be 0.0067 K−1 and 1.08 % K−1, respectively, with high-temperature measurement reliability and good temperature cycling performance. More importantly, its temperature measurement in phosphate-buffered saline (PBS) solution is accurate. In addition, the temperature of the cells can be increased by adjusting the laser power density and laser irradiation time. Therefore, an optical temperature sensing platform was built to realize the application of real-time monitoring of cancer cell temperature and the dual function of photothermal therapy. KW - Sensor KW - Temperature KW - Lanthanide KW - Tag KW - Fluorescence KW - Nanoparticles KW - Synthesis KW - Environment KW - Monitoring KW - Sensing KW - Nano KW - Life sciences KW - Upconversion PY - 2023 DO - https://doi.org/10.1021/acsanm.2c05110 VL - 6 IS - 1 SP - 759 EP - 771 PB - ACS Publications AN - OPUS4-57081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Koch, Matthias T1 - On-Site Detection of Volatile Organic Compounds (VOCs) N2 - Volatile organic compounds (VOCs) are of interest in many different fields. Among them are food and fragrance analysis, environmental and atmospheric research, industrial applications, security or medical and life science. In the past, the characterization of these compounds was mostly performed via sample collection and off-site analysis with gas chromatography coupled to mass spectrometry (GC-MS) as the gold standard. While powerful, this method also has several drawbacks such as being slow, expensive, and demanding on the user. For decades, intense research has been dedicated to find methods for fast VOC analysis on-site with time and spatial resolution. We present the working principles of the most important, utilized, and researched technologies for this purpose and highlight important publications from the last five years. In this overview, non-selective gas sensors, electronic noses, spectroscopic methods, miniaturized gas chromatography, ion mobility spectrometry and direct injection mass spectrometry are covered. The advantages and limitations of the different methods are compared. Finally, we give our outlook into the future progression of this field of research. KW - Volatile organic compounds KW - On-site detection KW - Mobile analytics KW - Sensors PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570885 DO - https://doi.org/10.3390/molecules28041598 VL - 28 IS - 4 SP - 1 EP - 19 PB - MDPI CY - Basel, Switzerland AN - OPUS4-57088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Wilsch, Gerd A1 - Gornushkin, Igor B. A1 - Kratochvilo, L. A1 - Pořízka, P. A1 - Kaiser, J. A1 - Millar, S. A1 - et al., T1 - Interlaboratory comparison for quantitative chlorine analysis in cement pastes with laser induced breakdown spectroscopy N2 - Concrete structures experience severe damage during service, for example due to pitting corrosion of rebars caused by the ingress of chlorine (Cl) into the porous concrete structure. The ingress can be monitored using laser-induced breakdown spectroscopy (LIBS), a recently introduced civil engineering technique used to detect Cl in concrete structures in addition to conventional wet chemistry methods. The key advantages of LIBS are high spatial resolution, which is important when analyzing heterogeneous concrete samples, as well as the almost complete absence of sample preparation. To assess LIBS as a reliable analytical method, its accuracy and robustness must be carefully tested. This paper presents the results of an interlaboratory comparison on the analysis of Cl in cement paste samples conducted by 12 laboratories in 10 countries. Two sets of samples were prepared with Cl content ranging from 0.06 to 1.95 wt% in the training set and 0.23–1.51 wt% in the test set, with additional variations in the type of cement and Cl source (salt type). The overall result shows that LIBS is suitable for the quantification of the studied samples: the average relative error was generally below 15%. The results demonstrate the true status quo of the LIBS method for this type of analysis, given that the laboratories were not instructed on how to perform the analysis or how to process the data. KW - LIBS KW - Interlaboratory comparison KW - Round robin test KW - Cement KW - Chlorine PY - 2023 DO - https://doi.org/10.1016/j.sab.2023.106632 SN - 0584-8547 VL - 202 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-57102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, T. A1 - Wang, J. A1 - Cheng, Z. A1 - Li, Z. A1 - Qiao, X. A1 - Wen, J. A1 - Resch-Genger, Ute A1 - Long, W. A1 - Ou, Jun T1 - Preparation of NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles and application of their fluorescence temperature sensing properties N2 - The NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles were successfully prepared by the solvothermal method, and the samples were pure hexagonal phase with good crystallinity and homogeneous size, asevidenced by XRD and TEM analysis. The FT-IR analysis shows that β-CD is successfully encapsulated on the surface of NaYF4: Yb3+/Tm3+@NaYF4 nanoparticles. The fluorescence intensity 3and lifetime were significantly increased after coating the inert layer on the surface of core nanoparticles. After further surface modification of β-CD, the fluorescence intensity and fluorescence lifetime were reduced, but the overall fluorescence was stronger. Temperature measurements using the fluorescence intensity ratio technique were found to have relatively low reliability and absolute sensitivity for temperature measurements using thermally coupled energy levels. However, the reliability of temperature measurements using non-thermally coupled energy levels is significantly higher and the absolute sensitivity is much higher than for measurements at thermally coupled levels. Since the maximum absolute sensitivity, maximum relative sensitivity and minimum temperature resolution are determined to be 0.1179 K-1, 2.19 %K􀀀 1 and 0.00019 K, respectively, NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles are expected to be widely used in the biomedical field due to their feasibility, reliability, non-toxicity and harmlessness. KW - Upconversion KW - Surface modification KW - Fluorescence intensity ratio KW - Thermally coupled levels KW - Non-thermally coupled levels PY - 2023 DO - https://doi.org/10.1016/j.optmat.2022.113389 SN - 0925-3467 VL - 136 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-57105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cheng, Z. A1 - Meng, M. A1 - Qiao, X. A1 - Liu, Y. A1 - Resch-Genger, Ute A1 - Ou, J. T1 - The synthesis of Er3+/Yb3+/K+ triple-doped NaYF4 phosphors and its high sensitivity optical thermometers at low power N2 - Optical Thermometry is popular among researchers because of its non-contact, high sensitivity, and fast measurement properties. In the present experiment, Er3+/Yb3+/K+ co-doped NaYF4 nanoparticles with different K+ concentrations were synthesized by solvothermal method, and the samples showed bright upconversion green emission under the excitation of a 980 nm laser. The powder X-ray diffractometer and transmission electron microscope were used to characterize the crystal structure and its surface morphology, respectively. The spectral characteristics of nanoparticles with K+ doping concentration from 10% to 30% (Molar ratio) were investigated by fluorescence spectroscopy, and it was observed that the fluorescence intensity reached the maximum at the K+ concentration of 20%, after which the intensity weakened when the K+ content continued to increase. According to the dependence between the luminescence intensity of the sample and the laser power density and fluorescence lifetime, the intrinsic mechanism was carefully investigated. Temperature-dependent spectra of the samples were recorded in the temperature range of 315–495 K, and the maximum values of absolute sensitivity (Sa) and relative sensitivity (Sr) were measured at 0.0041 K−1 (455 K) and 0.9220%K−1 (315 K). The experimental results show that K+/Er3+/Yb3+ triple-doped NaYF4 green fluorescent nanoparticles (GFNs) have good prospects for applications in display devices, temperature sensing, and other fields. KW - K+ doped KW - Upconversion luminescence KW - Optical temperature sensing KW - Thermal coupling energy level PY - 2023 DO - https://doi.org/10.1016/j.jallcom.2022.168299 VL - 937 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-57106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Machado Ferreira de Araujo, F. A1 - Duarte-Ruiz, D. A1 - Saßnick, H.-D. A1 - Gentzmann, Marie C. A1 - Huthwelker, T. A1 - Cocchi, C. T1 - Electronic Structure and Core Spectroscopy of Scandium Fluoride Polymorphs N2 - Microscopic knowledge of the structural, energetic, and electronic properties of scandium fluoride is still incomplete despite the relevance of this material as an intermediate for the manufacturing of Al−Sc alloys. In a work based on first-principles calculations and X-ray spectroscopy, we assess the stability and electronic structure of six computationally predicted ScF3 polymorphs, two of which correspond to experimentally resolved single-crystal phases. In the theoretical analysis based on density functional theory (DFT), we identify similarities among the polymorphs based on their formation energies, chargedensity distribution, and electronic properties (band gaps and density of states). We find striking analogies between the results obtained for the ow- and high-temperature phases of the material, indirectly confirming that the transition occurring between them mainly consists of a rigid rotation of the lattice. With this knowledge, we examine the X-ray absorption spectra from the Sc and F K-edge contrasting firstprinciples results obtained from the solution of the Bethe−Salpeter equation on top of all-electron DFT with high-energy-resolution fluorescence detection measurements. Analysis of the computational results sheds light on the electronic origin of the absorption maxima and provides information on the prominent excitonic effects that characterize all spectra. A comparison with measurements confirms that the sample is mainly composed of the high- and low-temperature polymorphs of ScF3. However, some fine details in the experimental results suggest that the probed powder sample may contain defects and/or residual traces of metastable polymorphs. KW - Scandium KW - X-ray spectroscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570727 DO - https://doi.org/10.1021/acs.inorgchem.2c04357 SN - 0020-1669 VL - 62 IS - 10 SP - 4238 EP - 4247 PB - ACS Publications CY - Washington DC AN - OPUS4-57072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, R. A1 - Faglioni, F. A1 - Bruno, Giovanni T1 - Synthetic Data Generation for Automatic Segmentation of X-ray Computed Tomography Reconstructions of Complex Microstructures N2 - The greatest challenge when using deep convolutional neural networks (DCNNs) for automatic segmentation of microstructural X-ray computed tomography (XCT) data is the acquisition of sufficient and relevant data to train the working network. Traditionally, these have been attained by manually annotating a few slices for 2D DCNNs. However, complex multiphase microstructures would presumably be better segmented with 3D networks. However, manual segmentation labeling for 3D problems is prohibitive. In this work, we introduce a method for generating synthetic XCT data for a challenging six-phase Al–Si alloy composite reinforced with ceramic fibers and particles. Moreover, we propose certain data augmentations (brightness, contrast, noise, and blur), a special in-house designed deep convolutional neural network (Triple UNet), and a multi-view forwarding strategy to promote generalized learning from synthetic data and therefore achieve successful segmentations. We obtain an overall Dice score of 0.77. Lastly, we prove the detrimental effects of artifacts in the XCT data on achieving accurate segmentations when synthetic data are employed for training the DCNNs. The methods presented in this work are applicable to other materials and imaging techniques as well. Successful segmentation coupled with neural networks trained with synthetic data will accelerate scientific output. KW - Automatic segmentation KW - 3D deep convolutional neural network (3D DCNN) KW - Dice score KW - Metal matrix composite (MMC) KW - Modified U-Net architectures KW - Multi-phase materials PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571243 DO - https://doi.org/10.3390/jimaging9020022 VL - 9 IS - 2 SP - 1 EP - 23 PB - MDPI AN - OPUS4-57124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -