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- ItemSolid carbon active screen plasma nitrocarburizing of AISI 316L stainless steel in cold wall reactor: influence of plasma conditions(Rio de Janeiro : Elsevier, 2020) Jafarpour, Saeed M.; Puth, Alexander; Dalke, Anke; Böcker, Jan; Pipa, AndreiV.; Röpcke, Jürgen; van Helden, Jean-Pierre H.; Biermann, HorstLow temperature plasma nitrocarburizing processes are widely used surface treatment techniques to improve the surface hardness and wear resistance of stainless steels without loss of their excellent corrosion resistance. In the present study, plasma nitrocarburizing based on the active screen technology was applied in an industrial-scale cold wall reactor for the treatment of AISI 316L. Different technological aspects of a cold wall active screen plasma nitrocarburizing (ASPNC) reactor are addressed. The current study compiles recent achievements for the ASPNC treatment using an active screen made of carbon fibre-reinforced carbon under varying plasma conditions. In addition, it is shown that utilizing an active screen made of carbon opens up the possibility to control the structural properties of expanded austenite by the variation of the plasma conditions. It is revealed that for the ASPNC treatment using an active carbon screen, the high reactivity of the generated plasma at the carbon surface suppresses the requirement to apply a bias discharge.
- ItemStudy of TiAl thin films on piezoelectric CTGS substrates as an alternative metallization system for high-temperature SAW devices(Rio de Janeiro : Elsevier, 2021) Seifert, Marietta; Lattner, Eric; Menzel, Siegfried B.; Oswald, Steffen; Gemming, ThomasTi/Al multilayer films with a total thickness of 200 nm were deposited on the high-temperature (HT) stable piezoelectric Ca3TaGa3Si2O14 (CTGS) as well as on thermally oxidized Si (SiO2/Si) reference substrates. The Ti–Al films were characterized regarding their suitability as an alternative metallization for electrodes in HT surface acoustic wave devices. These films provide the advantage of significantly lower costs and in addition also a significantly lower density as compared to Pt, which allows a greater flexibility in device design. To realize a thermal stability of the films, AlNO cover as well as barrier layers at the interface to the substrate were applied. The samples were annealed for 10 h at up to 800 °C in high vacuum (HV) and at 600 °C in air and analyzed regarding the γ-TiAl phase formation, film morphology, and possible degradation. The Ti/Al films were prepared either by magnetron sputtering or by e-beam evaporation and the different behavior arising from the different deposition method was analyzed and discussed. For the evaporated Ti/Al films, AlNO barriers with a lower O content were used to evaluate the influence of the composition of the AlNO on the HT stability. The sputter-deposited Ti/Al films showed an improved γ-TiAl phase formation and HT stability (on SiO2/Si up to 800 °C in HV and 600 °C in air, on CTGS with a slight oxidation after annealing at 800 °C in HV) as compared to the evaporated samples, which were only stable up to 600 °C in HV and in air.
- ItemApplication of machine learning to object manipulation with bio-inspired microstructures(Rio de Janeiro : Elsevier, 2023) Samri, Manar; Thiemecke, Jonathan; Hensel, René; Arzt, EduardBioinspired fibrillar adhesives have been proposed for novel gripping systems with enhanced scalability and resource efficiency. Here, we propose an in-situ optical monitoring system of the contact signatures, coupled with image processing and machine learning. Visual features were extracted from the contact signature images recorded at maximum compressive preload and after lifting a glass object. The algorithm was trained to cope with several degrees of misalignment and with unbalanced weight distributions by off-center gripping. The system allowed an assessment of the picking process for objects of various mass (200, 300, and 400 g). Several classifiers showed a high accuracy of about 90 % for successful prediction of attachment, depending on the mass of the object. The results promise improved reliability of handling objects, even in difficult situations.
- ItemAluminum based high temperature thin film electrode system for wireless sensors(Rio de Janeiro : Elsevier, 2023) Seifert, Marietta; Leszczynska, Barbara; Menzel, Siegfried B.; Schmidt, Hagen; Gemming, ThomasSelf-sustained, wireless high-temperature stable sensors are developed, which are based on an aluminum alloy as the electrode metallization. Due to its cost-effectiveness accompanied by a high-temperature stability, this alloy substitutes and outperforms the commonly applied expensive Pt- and Ir-based metals. For the first time, a comprehensive structural, electrical and high-frequency characterization of these surface acoustic wave (SAW) sensors is shown. They are based on Catangasite (Ca3TaGa3Si2O14, CTGS) in combination with properly structured cover and barrier layers for the metallization. The frequency characteristics is determined up to 700 °C by ex situ and in situ methods. In addition, the morphology of the AlRu electrodes is analyzed after the thermal loadings and the temperature dependent sheet resistance is measured. The results reveal a reproducible and linear correlation between the applied temperature and the sheet resistance as well as the resonant frequency. In addition, hardly any degradation of the electrodes is detected after the thermal loadings. The observed high-temperature stability of the devices up to at least 700 °C demonstrates the large potential of the AlRu based SAW sensors as a cost-efficient alternative to expensive noble metal based sensors in industrial applications for the support of energy efficient operation.
- ItemNovel low modulus beta-type Ti–Nb alloys by gallium and copper minor additions for antibacterial implant applications(Rio de Janeiro : Elsevier, 2022) Alberta, Ludovico Andrea; Vishnu, Jithin; Hariharan, Avinash; Pilz, Stefan; Gebert, Annett; Calin, MarianaThis study aims to develop novel low-modulus, corrosion-resistant Ti-based alloys with enhanced antimicrobial properties for bone-related implant applications. Novel β-type (Ti–45Nb)-based alloys with minor additions of the antibacterial elements Ga and/or Cu (up to 4 wt.%) were produced by a two-step casting process followed by homogenization treatment. Three nominal compositions (Ti–45Nb)96-4 Ga, (Ti–45Nb)96–4Cu and (Ti–45Nb)96-2 Ga–2Cu (wt.%) were prepared based on alloy design approach using [Mo]eq and electron per atom (e/a) ratio. The influence of Ga and/or Cu addition on the phase constitution, mechanical response and corrosion characteristics in simulated body fluids (PBS, 37.5 °C) has been investigated. X-ray diffraction studies displayed a single β phase structure for all alloys, with an observed lattice contraction evidenced by the reduction of lattice parameters during Rietveld analysis. Homogenous equiaxed microstructures with grain sizes ranging from 55 μm up to 323 μm were observed for (Ti–45Nb)96-4 Ga, (Ti–45Nb)96-2 Ga–2Cu and (Ti–45Nb)96–4Cu alloys. The alloys displayed excellent plasticity with no cracking, or fracturing during compression tests. Their tensile strength, Young's modulus, maximum tensile strain and elastic energy were measured in the ranges of 544–681 MPa, 73–78 GPa, 17–28% and 2.5–3.7 MJ/m3, in the order (Ti–45Nb)96-4 Ga > (Ti–45Nb)96-2 Ga–2Cu > (Ti–45Nb)96–4Cu. In addition, it has been observed that micro-alloying Ti–Nb alloy with Ga and/or Cu posed no deleterious effect on the corrosion resistance in simulated body fluid conditions. The improvement in strength of the developed alloys has been discussed based on grain boundary and solid-solution strengthening, whereas the improved plasticity is attributed to work hardening.
- ItemMicro-mechanical response of ultrafine grain and nanocrystalline tantalum(Rio de Janeiro : Elsevier, 2021) Yang, Wen; Ruestes, Carlos J.; Li, Zezhou; Torrents Abad, Oscar; Langdon, Terence G.; Heiland, Birgit; Koch, Marcus; Arzt, Eduard; Meyers, Marc A.In order to investigate the effect of grain boundaries on the mechanical response in the micrometer and submicrometer levels, complementary experiments and molecular dynamics simulations were conducted on a model bcc metal, tantalum. Microscale pillar experiments (diameters of 1 and 2 μm) with a grain size of ~100–200 nm revealed a mechanical response characterized by a yield stress of ~1500 MPa. The hardening of the structure is reflected in the increase in the flow stress to 1700 MPa at a strain of ~0.35. Molecular dynamics simulations were conducted for nanocrystalline tantalum with grain sizes in the range of 20–50 nm and pillar diameters in the same range. The yield stress was approximately 6000 MPa for all specimens and the maximum of the stress–strain curves occurred at a strain of 0.07. Beyond that strain, the material softened because of its inability to store dislocations. The experimental results did not show a significant size dependence of yield stress on pillar diameter (equal to 1 and 2 um), which is attributed to the high ratio between pillar diameter and grain size (~10–20). This behavior is quite different from that in monocrystalline specimens where dislocation ‘starvation’ leads to a significant size dependence of strength. The ultrafine grains exhibit clear ‘pancaking’ upon being plastically deformed, with an increase in dislocation density. The plastic deformation is much more localized for the single crystals than for the nanocrystalline specimens, an observation made in both modeling and experiments. In the molecular dynamics simulations, the ratio of pillar diameter (20–50 nm) to grain size was in the range 0.2–2, and a much greater dependence of yield stress to pillar diameter was observed. A critical result from this work is the demonstration that the important parameter in establishing the overall deformation is the ratio between the grain size and pillar diameter; it governs the deformation mode, as well as surface sources and sinks, which are only important when the grain size is of the same order as the pillar diameter.
- ItemLong-term high-temperature behavior of Ti–Al based electrodes for surface acoustic wave devices(Rio de Janeiro : Elsevier, 2022) Seifert, Marietta; Leszczynska, Barbara; Menzel, Siegfried; Gemming, ThomasThe long-term high-temperature behavior of Ti–Al based electrodes for the application in surface acoustic wave (SAW) sensor devices was analyzed. The electrodes were obtained by e-beam evaporation of Ti/Al multilayers on the high-temperature stable piezoelectric Ca3TaGa3Si2O14 (CTGS) substrates and structuring via the lift-off process. AlNO (25 at.% Al; 60 at.% N and 15 at.% O) cover and barrier layers were applied as protection against oxidation from the surrounding atmosphere and to prohibit a chemical reaction with the substrate. The samples were annealed at temperatures up to 600 °C in air for a duration of up to 192 h. Scanning and transmission electron microscopy were used to evaluate the morphology and degradation of the electrodes as well as of the extended contact pads. The results revealed that the Ti–Al based electrodes remained unoxidized after annealing for 192 h at 400 and 500 °C and for 24 h at 600 °C. After the heat treatment for 192 h at 600 °C, a strong oxidation of the structured electrodes occurred, which was less pronounced within the pads. In summary, the investigation showed that Ti–Al based SAW devices are a cost efficient alternative for long-term applications up to at least 500 °C and short- and medium-term applications up to 600 °C.
- ItemDurability of TiAl based surface acoustic wave devices for sensing at intermediate high temperatures(Rio de Janeiro : Elsevier, 2023) Seifert, Marietta; Leszczynska, Barbara; Weser, Robert; Menzel, Siegfried; Gemming, Thomas; Schmidt, HagenTiAl based surface acoustic wave (SAW) devices, which offer a promising cheap and easy to handle wireless sensor solution for intermediate high temperatures up to 600 °C, were prepared and investigated with respect to their durability. To obtain the devices, Ti/Al multilayers were deposited on high-temperature stable piezoelectric catangasite (CTGS) substrates and structured as electrodes via the lift-off technique. AlNO cover layers and barrier layers at the substrate site served as an oxidation protection. The devices were characterized regarding their electrical behavior by ex-situ measurements of their frequency characteristics after heat treatments up to 600 °C in air. In addition, long-term in situ measurements up to 570 °C were performed to analyze a possible drift of the resonant frequency in dependence on the temperature and time. Scanning electron microscopy of the surfaces of the devices and scanning transmission electron microscopy of cross sections of TiAl interdigital transducer electrode fingers and the contact pads were conducted to check the morphology of the electrode metallization and to reveal if degradation or oxidation processes occurred during the heat treatments. The results demonstrated a sufficient high-temperature stability of the TiAl based devices after a first conditioning of system. A linear dependence of the resonant frequency on the temperature of about −37 ppm/K was observed. In summary, the suitability of TiAl based SAW sensors for long-term application at intermediate temperatures was proven.
- ItemTribocorrosion behaviour of additively manufactured β-type Ti–Nb alloy for implant applications(Rio de Janeiro : Elsevier, 2024) Akman, Adnan; Douest, Yohan; Alberta, Ludovico Andrea; Perrin, Kevin; Trunfio Sfarghiu, Ana-Maria; Courtois, Nicolas; Ter-Ovanessian, Benoit; Pilz, Stefan; Zimmermann, Martina; Calin, Mariana; Gebert, Annettβ-type Ti–Nb alloys are promising materials for load-bearing implant applications with improved mechanical biofunctionality and biocompatibility. In this work, the electrochemical and tribo-electrochemical behaviour of laser powder bed fusion (LPBF) produced β-type Ti–42Nb alloy processed via Gaussian and top hat laser was investigated and compared with commercial grade β-type Ti–45Nb and α+β-type Ti–6Al–4V ELI. Electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization experiments were performed in phosphate-buffered saline (PBS) for corrosion behaviour. Tribocorrosion behaviour was studied under open circuit potential (OCP) conditions in PBS by using a reciprocating pin-on-disk tribometer. The passivation nature of the LPBF alloys is more decisive than the microstructural particularities for electrochemical behaviour. The overall corrosion response is similar due to the protective nature of the passive films formed on Ti alloys. Ti–6Al–4V ELI exhibits the best corrosion performance among all tested alloys with lower corrosion and passivation current density values. However, LPBF-produced alloys exhibit less reactive surfaces with better passive film properties compared to Ti–45Nb. In addition, EIS results revealed that passive film resistance values are higher for LPBF-produced alloys than conventionally produced Ti–45Nb. LPBF-produced alloys exhibit better tribo-electrochemical behaviour compared to Ti–45Nb. The differences in volume loss are mainly attributed to the microhardness of the alloys and the volume loss is dominated by mechanical wear. The alloys produced with LPBF show promising corrosion and tribocorrosion performance to be a potential candidate for load-bearing implant applications.
- ItemDesigning materials by laser powder bed fusion with machine learning-driven bi-objective optimization(Rio de Janeiro : Elsevier, 2024) Kononenko, Denys Y.; Chernyavsky, Dmitry; King, Wayne E.; Hufenbach, Julia Kristin; van den Brink, Jeroen; Kosiba, KonradTo exploit the full industrial potential of additive manufacturing (AM) beyond prototyping, the resource-consuming identification of the optimal processing conditions needs to be minimized. This task becomes more challenging when multiple properties of the part shall be simultaneously optimized. We utilize machine learning (ML) methods in a case study on laser powder bed fusion (LPBF) of a Zr-based glass-forming alloy. Our experiments show that processing parameters affect density and amorphicity opposingly, demonstrating the efficacy of our ML-based approach. We employ multi-objective optimization using Gaussian Process Regression to model and predict target properties and their uncertainties of parts fabricated by LPBF – a widely used metal AM technology. With density and amorphicity as target parameters, we optimize models using the Pareto front facilitated by the Non-Dominated Sorting Genetic Algorithm II. Despite deviations in the amorphicity data, we demonstrate this method to identify the high-performance region of the process parameters and its ability to be iteratively enhanced with additional experimental data. This bi-objective optimization approach provides a robust toolset for navigating LPBF processing. It can be easily extended to a larger set of target properties and transferred to further AM technologies.