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- Additive Manufacturing (49)
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- 7.6 Korrosion und Korrosionsschutz (114)
Eingeladener Vortrag
- nein (1102)
Using non-optimum combination of manufacturing parameters in selective laser melting (SLM) may lead to reduction of quality of component: defects generation, distortion of geometry and even cracking. Usually, the optimization of parameters is performed by changing volumetric energy density (Ev) and selecting parameters giving low porosity values. However, not only low porosity but also stable microstructure and low residual stresses will help to achieve advanced mechanical behavior of the component.
In present work, we investigated cuboid-shaped Ti-6Al-4V samples produced with different manufacturing parameters. The parameters leading to the same Ev were considered as well as parameters which are not included in Ev. Residual stresses in subsurface region were investigated by synchrotron X-ray diffraction, which allows to penetrate around 100 µm from the surface therefore overcome the problem of high roughness of SLM components without additional sample preparation. Only tensile stresses were found along the building direction, that can play critical role especially during cyclic loading. In parallel, using X-ray computed tomography we also observe that porosity is mainly concentrated in the contour region, except in case where the laser speed is small. However, by using some process parameters it was possible to decrease residual stresses and obtain uniform α+β Ti microstructure and relatively low porosity. Additionally, it was found that not included in Ev (e.g., base plate position, focus distance) should be considered as additional manufacturing parameters during SLM process.
The porosity and the surface roughness are recently discussed problems for SLM parts. The influence of SLM process parameters on porosity is well studied for different materials. Nevertheless, the build angle (i.e. the angle between part orientation and build plate) needs to be understood as an additional SLM process parameter, as it has been shown, that the microstructure and hence the mechanical performance of various materials depend on the build angle. The inherent build angle of each strut as a part of a lattice structure is the motivation to investigate the influence of the build angle on the porosity and roughness on round-shaped (1 mm diameter) struts by means of CT. Conventional Coordinate Measuring Machine (CMM) has the limitation towards small and round shaped samples. The need for Computed Tomography (CT) regarding investigations of SLM parts will increase because no other non-destructive technique allows the assessment of complex geometries with inner laying surfaces. We used CT to assess the pores and the strut surface. Seven struts out of the nickel alloy Inconel 625 with build angles from 30° to 90° were studied. It was found that the number of pores is smaller, and the size of pores is larger for the 90° strut. In case of 30° strut, the number of pores is increased towards down-skin side, additionally, this strut orientation showed to have the largest number of attached powder particles. The elongated pores exist exclusively near the strut surface. While the roughness at the down-skin surface is highly depending of the biud angle, the roughness at the up-skin surface is the same for all struts. The mechanisms of pore and surface roughness formation is not mainly driven by gravity.
Metallene Konstruktionswerkstoffe reagieren infolge ihres thermodynamisch instabilen Zustandes mehr oder weniger stark mit Stoffen aus der Umgebung. Eine große Rolle bei diesen Reaktionen spielt das Feuchtigkeitsangebot an der Metalloberfläche, welches nicht zwingend mit einem sichtbaren Wasserfilm einhergehen muss. An der Atmosphäre bilden sich an sauberen Metalloberflächen bei etwa 80 % relativer Luftfeuchte, bei versalzten Oberflächen auch schon ab etwa 25 % r. F., Feuchtfilme aus. Im Feuchtfilm laufen grundsätzlich die gleichen elektrochemischen Reaktionen ab, wie diese von wässrigen Medien bekannt sind. Dabei geht das Metall zunächst in Ionenform und in nachgelagerten Reaktionen in einen thermodynamisch stabilen Zustand in Form unterschiedlichster Oxid- und Hydroxidverbindungen über. Die so entstehenden Korrosionsprodukte können im Feuchtigkeitsfilm begrenzt löslich oder unlöslich sein und lagern sich auf den Oberflächen der Konstruktionswerkstoffe häufig als feste Korrosionsprodukte ab bzw. wachsen dort auf. Je nachdem wie die Korrosionsprodukte strukturell zum Untergrund passen, können sich dichte, sehr gut haftende Schichten ausbilden oder poröse, dicke Schichten ohne nennenswerte Haftung aufwachsen. Wachsen dichte, porenfreie Schichten mit guter Haftung auf, die im umgebenden Medium unlöslich sind, wird die weitere Auflösung des Metalls stark gehemmt. Man spricht dann von der Ausbildung schützender Deckschichten bzw. von Passivschichten auf welcher der Korrosionsschutz und damit die Dauerhaftigkeit vieler Konstruktionswerkstoffe beruhen. Kaesche bezeichnete die Passivität sehr treffend als „optimalen Grenzfall des Korrosionsschutzes durch Schichten von Korrosionsprodukten“. Aus technischer Sicht hält Kaesche eine Unterscheidung von Deckschichten bzw. Passivschichten für nicht zwingend erforderlich, da beide die Korrosionsgeschwindigkeit in gleichem Maß herabsetzen können. Die Übergänge zwischen den meist dickeren und dadurch sichtbaren Deckschichten und den meist dünnen, nicht sichtbaren Passivschichten sind fließend.
Due to its advantages of being a direct comparison method, quantitative NMR spectroscopy (qNMR) becomes more and more popular in industry. While conventional high-field NMR systems are often associated with high investment and operational costs, the upcoming market of permanent-magnet based benchtop NMR systems show a considerable option for a lot of applications. The mobility of these systems allows to bring them more closely to the real production environment, e.g. for at-line quality control.
In this work we present an interlaboratory comparison study investigating the qNMR performance of state-of-the-art benchtop NMR spectrometers. Therefore, BAM prepared two samples of a mixture of NMR reference standards tetramethylbenzene (TMB) and tetrachloronitrobenzene (TCNB) at concentration levels of 200 mM and 10 mM. These “ready-to-use” samples were sent to participant laboratories, which performed analysis on their benchtop NMR equipment of different vendors and fields from 43 to 80 MHz. Raw data was reported back and further investigated by using different data analysis methods at BAM.
After this very first qNMR comparison study of benchtop NMR spectrometers show promising results, following studies are planned to cover more parts of the qNMR process, e.g. sample preparation and weighing, but also data analysis, as commonly done in similar studies for high-field NMR spectroscopy in industry and metrology.
Improvement in deep process understanding is a mandatory prerequisite for the application of modern concepts like Industrial Internet of Things (IIoT) or “Industrie 4.0”. The direct hyphenation with online methods of process analytical technology (PAT) allows profound insights into the actual reactions within chemical and pharmaceutical production steps and provides necessary information for associated advanced control strategies.
While the industrial application of online Raman spectroscopy has already been successfully demonstrated, low-field NMR spectroscopy is not yet adequately developed as a robust online method for use in process industry. The high information content combined with the low calibration effort makes NMR spectroscopy a highly promising method for modern process automation with a high flexibility due to short set-up times and novel calibration concepts. This is a major advantage compared to other analytical methods, especially regarding multi-purpose plant strategies, as well as processes suffering from fluctuating quality of raw materials.
The work presented here focusses on the heterogeneous catalyzed hydrogenation of 2-butyne-1,4-diol, as a step of the synthesis of industrially important solvent tetrahydrofuran. This reaction is proceeding via an intermediate product and suffers from competitive reaction paths. In this application, online NMR and Raman spectroscopy were combined with data from classical process sensors, e.g., pressure, temperature, and flow transducers in a highly automated setup for the development of innovative control concepts.
The transition from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example.
Due to NMR spectroscopy as an “absolute comparison method”, independent of the matrix, it runs with very short set-up times in combination with “modular” spectral models. These are based on pure component NMR spectra without the need for tedious calibrations runs. We present approaches from statistical, (i.e., Partial Least Squares Regression) to physically motivated models (i.e., Indirect Hard Modelling).
Based on concentration measurements of reagents and products by the NMR analyser a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu).
Metallene Konstruktionswerkstoffe reagieren infolge ihres thermodynamisch instabilen Zustandes mehr oder weniger stark mit Stoffen aus der Umgebung. Eine große Rolle bei diesen Reaktionen spielt das Feuchtigkeitsangebot an der Metalloberfläche, welches nicht zwingend mit einem sichtbaren Wasserfilm einhergehen muss. An der Atmosphäre bilden sich an sauberen Metalloberflächen bei etwa 80 % relativer Luftfeuchte, bei versalzten Oberflächen auch schon ab etwa 25 % r. F., Feuchtfilme aus. Im Feuchtfilm laufen grundsätzlich die gleichen elektrochemischen Reaktionen ab, wie diese von wässrigen Medien bekannt sind. Dabei geht das Metall zunächst in Ionenform und in nachgelagerten Reaktionen in einen thermodynamisch stabilen Zustand in Form unterschiedlichster Oxid- und Hydroxidverbindungen über. Die so entstehenden Korrosionsprodukte können im Feuchtigkeitsfilm begrenzt löslich oder unlöslich sein und lagern sich auf den Oberflächen der Konstruktionswerkstoffe häufig als feste Korrosionsprodukte ab bzw. wachsen dort auf. Je nachdem wie die Korrosionsprodukte strukturell zum Untergrund passen, können sich dichte, sehr gut haftende Schichten ausbilden oder poröse, dicke Schichten ohne nennenswerte Haftung aufwachsen. Wachsen dichte, porenfreie Schichten mit guter Haftung auf, die im umgebenden Medium unlöslich sind, wird die weitere Auflösung des Metalls stark gehemmt. Man spricht dann von der Ausbildung schützender Deckschichten bzw. von Passivschichten auf welcher der Korrosionsschutz und damit die Dauerhaftigkeit vieler Konstruktionswerkstoffe beruhen. Kaesche bezeichnete die Passivität sehr treffend als „optimalen Grenzfall des Korrosionsschutzes durch Schichten von Korrosionsprodukten“. Aus technischer Sicht hält Kaesche eine Unterscheidung von Deckschichten bzw. Passivschichten für nicht zwingend erforderlich, da beide die Korrosionsgeschwindigkeit in gleichem Maß herabsetzen können. Die Übergänge zwischen den meist dickeren und dadurch sichtbaren Deckschichten und den meist dünnen, nicht sichtbaren Passivschichten sind fließend.
Seismic methods are increasingly used to improve ultrasonic imaging and monitoring of concrete. At BAM, we are research mainly the use of Reverse Time Migration to get better images from ultrasonic echo data of thick, complex concrete structures. Coda wave interferometry is used to detect subtle changes in concrete constructions, e. g. using embedded ultasonic transducers.
Additive manufacturing (AM) opens the route to a range of novel applications. However, the complexity of the manufacturing process poses a challenge to produce defect-free parts with a high reliability. Since process dynamics and resulting microstructures of AM parts are strongly influenced by the involved temperature fields and cooling rates, thermography is a valuable tool for process monitoring. Another approach to monitor the energy input into the part during process is the use of optical tomography.
Common visual camera systems reach much higher spatial resolution than infrared thermography cameras, whereas infrared thermography provides a much higher temperature dynamic. Therefore, the combined application increases the depth of information. Here, we present first measurement results using a laser beam melting setup that allows simultaneous acquisition of thermography and optical tomography from the same point of view using a beam splitter. A high-resolution CMOS camera operating in the visible spectral range is equipped with a near infrared bandpass filter and images of the build plate are recorded with long-term exposure during the whole layer exposing time. Thus, areas that reach higher maximum temperature or are at elevated temperature for an extended period of time appear brighter in the images. The used thermography camera is sensitive to the mid wavelength infrared range and records thermal videos of each layer exposure at an acquisition rate close to 1 kHz.
As a next step, we will use computer tomographic data of the built part as a reference for defect detection.
This research was funded by BAM within the focus area Materials.
Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds.
Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications.
In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals.
The thermoelectric properties of Sr1-xBixTiO3-δ (0 ≤ x ≤ 0.07) have been investigated. Dense ceramics of Sr1-xBixTiO3-δ and Sr0.95TiO3-δ have been prepared by solid-state reaction and conventional sintering in air followed by annealing in a reducing atmosphere. XRD and SEM analyses show that the rutile TiO2 in Sr0.95TiO3 formed after sintering becomes Magnéli phase of TinO2n-1 after annealing. Moreover, Bi resolves from Sr1-xBixTiO3 after annealing, resulting in the formation of Sr1-xBixTiO3-δ/Bi/TinO2n-1 composites. With increasing Bi content in Sr1-xBixTiO3-δ, the electrical conductivity increases while the absolute values of the Seebeck coefficient decrease as a result of increasing carrier concentration. The thermal conductivity of SrTiO3-δ is reduced by doping Bi up to x = 0.07. Highest ZT ~ 0.13 is obtained in Sr0.93Bi0.07TiO3-δ at 1000 K.
Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes).
Here, thin films with thicknesses down to few nanometers are prepared on different substrates as model systems for polymer composites. The thin films are investigated by a combination of surface analytical and volume sensitive methods. As surface analytical methods atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements (CAM) are employed. As volume sensitive broadband dielectric spectroscopy (BDS), specific heat spectroscopy (SHS), and ellipsometry are used. Especially attention is paid to understand the glass transition behavior of thin films because the glass transition is the key phenomenon determines the application of polymers also in thin films.
To understand the glass transition behavior of thin films, which is controversially discussed in literature, a three layer model is discussed. Firstly, a mobile surface layer is assumed at polymer air interface of the film due to missing of segment/segment interactions. Secondly, in the middle of the film a bulk-like layer should be expected. Thirdly, for polymers having non-repulsive interactions with the substrate an irreversibly adsorbed layer is expected to be formed. Due the adsorption the molecular mobility of the segments in this layer is slowed down. What is measured for the glass transition of thin films is a complicated average of all of these effects. The different layers are hardly to address separately. Therefore, in the presentation especially model systems are selected and investigated to verify the layer model.
The laser implantation technique bases on a localized dispersing of ceramic particles in metallic surface layers for changing their micro geometry as well as their material properties. Using TiB2 and NbC hard particles, tailored microtextures consisting of elevated dome-, ring-, or line-shaped Features can be manufactured. Especially TiB2 implants feature high hardness values up to 1800 HV1 and ceramic particle contents up to 55 %, indicating superior wear resistant properties.
Treatment and reusing of hazardous wastes have become significant issues of modern societies. Blast furnace sludge (BFS) and electric arc furnace dust (EAFD) are such typical wastes, because they usually contain high amounts of undesirable elements such as zinc (Zn) and lead (Pb).
These elements can cause operational problems in reusing of BFS and EAFD. In this study, the Ferro Duo GmbH and the Federal Institute for Materials Research and Testing have investigated a novel approach for eliminating and/or recovering Zn and Pb from both wastes. Applied was a selective chlorination and volatilization of Zn and Pb as chlorides at temperatures between 500 °C and 1100 °C. Both product obtained, Zn and Pb in the form of ZnCl2 and PbCl2 and the purified solid mineral compound are attractive materials for further use. Hydrochloric acid and iron(II) chloride were used as chlorination agents. Exceptionally high Zn and Pb removal efficiencies of >99.5 % could be achieved with both chlorination agents, whereby iron(II) chloride exhibited better performance.
Korrosionsschutzmethoden
(2019)
Der Vortrag thematisiert die Grundlagen des Korrosionsschutzes. Dieser kann planungs-,werkstoff oder mediumsseitig erfolgen oder mit elektrochemischen Methoden umgesetzt werden. Der Vortrag beschreit die Korrosivitäten der Atmosphären und welche Maßnahmen für den Korrosionsschutz daraus abgeleitet werden können.