TY - JOUR A1 - Tammas-Williams, S. A1 - Zhao, H. A1 - Léonard, Fabien A1 - Derguti, F. A1 - Todd, I. A1 - Prangnell, P.B. T1 - XCT analysis of the influence of melt strategies on defect population in Ti-6Al-4V components manufactured by Selective Electron Beam Melting N2 - Selective Electron Beam Melting (SEBM) is a promising powder bed Additive Manufacturing technique for near-net-shape manufacture of high-value titanium components. However without post-manufacture HIPing the fatigue life of SEBM parts is currently dominated by the presence of porosity. In this study, the size, volume fraction, and spatial distribution of the pores in model samples have been characterised in 3D, using X-ray Computed Tomography, and correlated to the process variables. The average volume fraction of the pores (b0.2%) was measured to be lower than that usually observed in competing processes, such as selective laser melting, but a strong relationship was found with the differentbeamstrategies used to contour ,and infill by hatching, a part section. The majority of pores were found to be small spherical gas pores, concentrated in the infill hatched region; this was attributed to the lower energy density and less focused beam used in the infill strategy allowing less opportunity for gas bubbles to escape the melt pool. Overall, increasing the energy density or focus of the beam was found to correlate strongly to a reduction in the level of gas porosity. Rarer irregular shaped pores were mostly located in the contour region and have been attributed to a lack of fusion between powder particles. KW - Titanium KW - Additive Manufacture KW - Selective Electron Beam Melting KW - Pores KW - X-ray computed tomography PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-416577 UR - http://www.sciencedirect.com/science/article/pii/S104458031500039X?via%3Dihub DO - https://doi.org/10.1016/j.matchar.2015.02.008 VL - 102 SP - 47 EP - 61 CY - Materials Characterization AN - OPUS4-41657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mushtaq, S. A1 - Steers, E.B.M. A1 - Barnhart, D. A1 - Churchill, G. A1 - Kasik, M. A1 - Richter, Silke A1 - Pfeifer, Jens A1 - Putyera, K. T1 - The production of doubly charged sample ions by “charge transfer and ionization” (CTI) in analytical GD-MS N2 - Normally, in analytical GD-MS, the doubly charged metallic ion signals from the sample are several orders of magnitude less than the corresponding singly charged signals. However, we have observed that using a neon plasma, the M++ signals of some elements, which have double ionization energies close to the first ionization energy of neon, are of the same order as the M+ signal. Doubly charged ions may be produced directly in the discharge cell by electron ionization (EI), and also by two electron Penning ionization (TEP), but these processes cannot explain the above effect. In this paper, we suggest that an additional process named as ‘Charge Transfer and Ionization’ (CTI) produces such ions either in their ionic ground state or in an excited state. To confirm that this process is typical of the discharges used in GD-MS and not an artefact of any particular form of cell and ion extraction system, we have carried out comprehensive experimental measurements using three different GD-MS instruments, viz., Nu Astrum, VG9000 and ELEMENT GD and our results provide clear evidence for CTI. This is the first time the process has been identified as an ionization process in analytical GD-MS. CTI must be differentiated from Asymmetric Charge Transfer (ACT), which is a “selective” process and requires a close energy match (e.g. ΔE < 0.5 eV for a strong effect). On the other hand, CTI is “non-selective” in the sense that a close energy match is not required (e.g. a strong effect is observed with ΔE ∼ 2 eV), although the process only occurs for a limited number of elements, depending on the plasma gas used and the total energy required to doubly ionize the metallic atom. KW - Titanium KW - Glow discharge processes KW - Doubly charged ions KW - The charge transfer and ionization process (CTI) KW - Krypton KW - Neon PY - 2017 DO - https://doi.org/10.1039/C6JA00415F SN - 0267-9477 SN - 1364-5544 VL - 32 IS - 9 SP - 1721 EP - 1729 PB - Royal Society of Chemistry AN - OPUS4-41108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silverstein, R. A1 - Eliezer, D. A1 - Böllinghaus, Thomas T1 - Hydrogen-trapping mechanisms of TIG-welded 316L austenitic stainless steels N2 - The interaction of hydrogen with various tungsten-inert-gas-welded austenitic stainless steels’ (AUSS) microstructure is studied by means of desorption/absorption analysis and microstructure observations. One of the limitations of welding is created by the presence of hydrogen in the weld, which can shorten the steel’s service life. The local hydrogen concentration, trapping, and its distribution along the welded samples were studied by thermal desorption spectrometry and were supported by X-ray diffraction (XRD) and electronic microstructural observations. Hydrogen content demonstrated a dependence on the welding zone. It was found that hydrogen distribution, and accepted microstructure during welding, played a significant role in the trapping mechanism of 316L AUSS. XRD analysis revealed residual stresses which were caused due to the presence of hydrogen in c-phase. It was shown that the austenite microconstituents inside 316L can have a crucial effect in preventing hydrogen-assisted cracking phenomenon. The effects of AUSS microstructure on hydrogen absorption and desorption behavior are discussed in detail. KW - Thermal-desorption spectroscopy KW - Ferritic steels KW - Strain rates KW - Duplex KW - Embrittlement KW - Diffusion KW - Titanium KW - Alloys KW - Behavior PY - 2018 DO - https://doi.org/10.1007/s10853-018-2349-6 SN - 1573-4803 SN - 0022-2461 VL - 53 IS - 14 SP - 10457 EP - 10468 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-46833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kirner, Sabrina A1 - Wirth, Thomas A1 - Sturm, Heinz A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Nanometer-resolved chemical analyses of femtosecond laser-induced periodic surface structures on titanium N2 - The chemical characteristics of two different types of laser-induced periodic surface structures (LIPSS), so-called high and low spatial frequency LIPSS (HSFL and LSFL), formed upon irradiation of titanium surfaces by multiple femtosecond laser pulses in air (30 fs, 790 nm, 1 kHz), are analyzed by various optical and electron beam based surface analytical techniques, including micro-Raman spectroscopy, energy dispersive X-ray analysis, X-ray photoelectron spectroscopy, and Auger electron spectroscopy. The latter method was employed in a high-resolution mode being capable of spatially resolving even the smallest HSFL structures featuring spatial periods below 100 nm. In combination with an ion sputtering technique, depths-resolved chemical information of superficial oxidation processes was obtained, revealing characteristic differences between the two different types of LIPSS. Our results indicate that a few tens of nanometer shallow HSFL are formed on top of a ∼150 nm thick graded superficial oxide layer without sharp interfaces, consisting of amorphous TiO2 and partially crystallized Ti2O3. The larger LSFL structures with periods close to the irradiation wavelength originate from the laser-interaction with metallic titanium. They are covered by a ∼200 nm thick amorphous oxide layer, which consists mainly of TiO2 (at the surface) and other titanium oxide species of lower oxidation states underneath. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser KW - Oxidation KW - Titanium KW - Auger electron spectroscopy PY - 2017 DO - https://doi.org/10.1063/1.4993128 SN - 0021-8979 VL - 122 IS - 10 SP - 104901, 1 EP - 9 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-41905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kirner, Sabrina V. A1 - Slachciak, Nadine A1 - Elert, Anna Maria A1 - Griepentrog, Michael A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Sahre, Mario A1 - Dörfel, Ilona A1 - Sturm, Heinz A1 - Pentzien, Simone A1 - Koter, Robert A1 - Spaltmann, Dirk A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Tribological performance of titanium samples oxidized by fs-laser radiation, thermal heating, or electrochemical anodization N2 - Commercial grade-1 titanium samples (Ti, 99.6%) were treated using three alternative methods, (i) femtosecond laser processing, (ii) thermal heat treatment, and (iii) electrochemical anodization, respectively, resulting in the formation of differently conditioned superficial titanium oxide layers. The laser processing (i) was carried out by a Ti:sapphire laser (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz) in a regime of generating laser-induced periodic surface structures (LIPSS). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning setup for the processing of several square-millimeters large surface areas covered homogeneously by these nanostructures. The differently oxidized titanium surfaces were characterized by optical microscopy, micro Raman spectroscopy, variable angle spectroscopic ellipsometry, and instrumented indentation testing. The tribological performance was characterized in the regime of mixed friction by reciprocating sliding tests against a sphere of hardened steel in fully formulated engine oil as lubricant. The specific tribological performance of the differently treated surfaces is discussed with respect to possible physical and chemical mechanisms. KW - Femtosecond laser KW - Titanium KW - Oxidation KW - Friction PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-445609 DO - https://doi.org/10.1007/s00339-018-1745-8 SN - 0947-8396 SN - 1432-0630 VL - 124 IS - 4 SP - 326, 1 EP - 10 PB - Springer-Verlag AN - OPUS4-44560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwibbert, Karin A1 - de Eulate Pérez, Elisa García A1 - Wen, Keqing A1 - Voss, Heike A1 - Thiele, Dorothea A1 - Richter, Anja M. A1 - Bonse, Jörn T1 - Escherichia coli repellence via laser-induced periodic surface structures (LIPSS) on titanium: Critical role of biofilm-associated gene expression N2 - The inconsistency in the observed bacteria-repellent effects of laser-induced surface textures remains a subject of scientific debates. With E. coli TG1 as test strain, we performed biofilm formation assays on ultrashort pulse laser textured titanium. Samples covered with low spatial frequency LIPSS (LSFL) of periods around 750 nm or with high spatial frequency LIPSS (HSFL) featuring smaller periods around 100 nm were processed on polished samples. While LSFL significantly reduce the number of adhering bacteria compared to the polished reference, HSFL do not. Simultaneously, we concentrate our study on bacterial strategies employed for biofilm formation, that is the transcription of the biofilm-associated genes csgB, involved in primary adhesion to a surface, and wza, participating in biofilm maturation. Promoter regions of these genes were cloned into a promotor probe plasmid with the green fluorescent protein GFP+ as reporter and transferred into the test strain. As indicated by the fluorescence intensity of the reporter protein, among the bacteria colonizing LSFL-covered areas, a markedly higher proportion of cells transcribing csgB or wza were detected, compared to the bacterial populations colonizing the polished or HSFL-covered areas. To our knowledge, this is the first study indicating that the antifouling effect of LSFL topographies can be counteracted when bacteria activate biofilm-associated genes. KW - Laser-induced periodic surface structures (LIPSS) KW - Titanium KW - Biofilm KW - Antifouling KW - Gene expression KW - Fluorescence microscopy PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655572 DO - https://doi.org/10.1016/j.apsusc.2026.166363 SN - 0169-4332 VL - 730 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-65557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Fritsch, Tobias A1 - Ferrari, Bruno A1 - Altmann, Mika León A1 - Bruno, Giovanni A1 - Toenjes, Anastasiya T1 - Laser powder bed fusion: Defect type influences critical porosity re-growth during reheating after hot isostatic pressing N2 - Despite the remarkable product design flexibility offered by additive manufacturing (AM) techniques, such as laser powder bed fusion, AM processes are susceptible to the formation of defects. In this context, the control of process parameters and the application of post-processing treatments, such as hot isostatic pressing (HIP), are of paramount importance to achieve the desired mechanical properties. The present study investigates the effectiveness of HIP as a function of process parameters in laser powder bed fused Ti-6V-4Al (PBF-LB/Ti64) using X-ray computed tomography. The process parameters are modified to obtain reference samples with low porosity, lack of fusion defects, or keyhole porosity. In all instances, subsurface keyhole porosity was observed in the as-built parts. Moreover, it was found that the efficacy of pore closure is dependent on the specific defect type. In the case of low porosity and keyhole pores, HIP resulted in effective closure. Conversely, larger lack of fusion defects were not closed due to their interconnectivity and the entrapment of argon gas. Subsequent heat treatments above the β-transus temperature allowed the investigation of the impact of defect type on porosity re-growth. For the first time, we reveal that lack of fusion defects are affected by considerable pore re-growth during post-HIP heat treatments of PBF-LB/Ti64. Such phenomenon is driven by the increasing internal pore pressure and local creep deformation at high temperatures. In contrast, re-growth is limited in samples with low porosity or keyhole pores. KW - Additive Manufacturing KW - Hot Isostatic Pressing KW - Titanium KW - Laser Powder Bed Fusion KW - X-ray Computed Tomography KW - Heat Treatment KW - Porosity PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629289 DO - https://doi.org/10.1016/j.jmatprotec.2025.118839 VL - 340 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-62928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -