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Zusammenfassung Im Rahmen des Themenfeldprojektes „Process Monitoring of AM“ (ProMoAM) evaluiert die Bundesanstalt für Materialforschung und -prüfung (BAM) gegenwärtig die Anwendbarkeit verschiedenster ZfP-Verfahren zur in-situ Prozessüberwachung in der additiven Fertigung (AM) von Metallen in Hinblick auf die Qualitätssicherung. Einige der wichtigsten Messgrößen sind hierbei die Temperatur des Schmelzbades und die Abkühlrate, welche starken Einfluss auf das Gefüge und die Eigenspannung haben. Aufgrund der Zugänglichkeit zum Werkstück während des Bauprozesses bieten sich optische Verfahren zu Temperaturbestimmung an. Hierbei stellen jedoch u. a. die hohe Bandbreite der zu messenden Temperaturen, die Bestimmung der Emissivität und ihre Änderung bei Phasenübergängen der verwendeten Legierung große experimentelle Herausforderungen dar. Eine weitere Herausforderung stellt für die IR-Spektroskopie die Absorption durch das Schutzgas und weitere optische Elemente dar. Um diese auch in einem industriellen Umfeld kompensieren zu können, wurde eine Methode entwickelt, die das gemessene Spektrum bei der Verfestigung des Werkstoffes als Referenz nutzt. In diesem Beitrag wird die Anwendung dieser Methode für die IR-Spektrometrie als auch Thermografische Messungen beim Laser-Pulver-Auftragschweißen von 316L gezeigt, wobei beide Methoden weiterhin in Hinblick auf ihre individuellen Vor- und Nachteile miteinander verglichen werden.

Material qualification for laser powder bed fusion (L-PBF) processes are often based on results derived from additively manufactured (AM) bulk material or small density cubes, although it is well known that the part geometry has a tremendous influence on the heat flux and, therefore, on the thermal history of an AM component. This study shows experimentally the effect of simple geometrical obstructions to the heat flux on cooling behavior and solidification conditions of 316L stainless steel processed by L-PBF. Additionally, it respects two distinct inter layer times (ILT) as well as the build height of the parts. The cooling behavior of the parts is in-situ traced by infrared (IR) thermography during the built-up. The IR signals reveal significant differences in cooling conditions, which are correlated to differences in melt pool geometries. The acquired data and results can be used for validation of computational models and improvements of quality assurance.

Additive manufacturing of metals offers the opportunity to build parts with a high degree of complexity without additional costs, opening a new space for design optimization. However, the processes are highly complex and due to the rapid thermal cycles involved, high internal stresses and peculiar microstructures arise, which influence the parts mechanical properties. To systematically examine the formation of internal stresses and the microstructure, in-process spatially resolved measurements of the part temperature are needed. Usually, thermography is used to measure temporally resolved thermal fields. The thermal cameras are calibrated at black body reference radiators (unity emissivity) for the conversion of the measured thermal radiation intensity to temperatures. If the emissivity of the inspected part is known, its thermodynamic temperature can be reconstructed by a suited radiometric model. However, in additive manufacturing of metals, the emissivity of the part surface is strongly inhomogeneous and rapidly changing due to variations of, e.g., the degree of oxidation, the material state and temperature. However, measuring the process thermal radiation at different wavelengths simultaneously enables one to separate temperature and emissivity spatially resolved to obtain further insight into the process. Here, we present results of a study using multispectral thermography to obtain real temperatures and emissivities in the laser metal deposition (LMD) process. For a better understanding of the basic processes, the measurements have been performed first without powder supply and by recording images at different wavelength in subsequent runs.

Thermography is one on the most promising techniques for in-situ monitoring of metal additive manufacturing processes. Especially in laser powder bed fusion processes, the high process dynamics and the strong focus of the laser beam cause a very complex thermal history within the produced specimens, such as multiple heating cycles within single layer expositions. This complicates data interpretation, e.g., in terms of cooling rates. A quantity that is easily calculated is the time a specific area of the specimen is at a temperature above a chosen threshold value (TOT). Here, we discuss variations occurring in time-over-threshold-maps during manufacturing of an almost defect free cuboid specimen.

Remote gas sensors mounted on mobile robots enable the mapping of gas distributions in large or hardly accessible areas. A challenging task, however, is the generation of three-dimensional distribution maps from these gas measurements. Suitable reconstruction algorithms can be adapted, for instance, from the field of computed tomography (CT), but both their performance and strategies for selecting optimal measuring poses must be evaluated. For this purpose simulations are used, since, in contrast to field tests, they allow repeatable conditions. Although several simulation tools exist, they lack realistic models of remote gas sensors. Recently, we introduced a model for a Tunable Diode Laser Absorption Spectroscopy (TDLAS) gas sensor taking into account the conical shape of its laser beam. However, the novel model has not yet been validated with experiments. In this paper, we compare our model with a real sensor device and show that the assumptions made hold.

Herein, we have developed a systematic study on the oxidation and passivation of mechanically exfoliated black phosphorus (BP). We analyzed the strong anisotropic behavior of BP by scanning Raman microscopy providing an accurate method for monitoring the oxidation of BP via statistical Raman spectroscopy. Furthermore, different factors influencing the environmental instability of the BP, i.e., thickness, lateral dimensions or visible light illumination, have been investigated in detail. Finally, we discovered that the degradation of few-layer BP flakes of

Thinning out MoS2 crystals to atomically thin layers results in the transition from an indirect to a direct bandgap material. This makes single layer MoS2 an exciting new material for electronic devices. In MoS2 devices it has been observed that the choice of materials, in particular for contact and gate, is crucial for their performance. This makes it very important to study the interaction between ultrathin MoS2 layers and materials employed in electronic devices in order to optimize their performance. In this work we used NC-AFM in combination with quantitative KPFM to study the influence of the substrate material and the processing on single layer MoS2 during device fabrication. We find a strong influence of contaminations caused by the processing on the surface potential of MoS2. It is shown that the charge transfer from the substrate is able to change the work function of MoS2 by about 40 meV. Our findings suggest two things. First, the necessity to properly clean devices after processing as contaminations have a great impact on the surface potential. Second, that by choosing appropriate materials the work function can be modified to reduce contact resistance.

We present photoluminescence and resonant Raman measurements of atomically thin layers of molybdenum disulfide (MoS2) in the energy range of the A and B optical transitions. We found a Stokes shift of the transition energies in the resonant Raman measurements compared to the photoluminescence. The Stokes shift increases for the bilayer compared to the single layer. Furthermore, in resonance with the A transition, the Raman intensity of the A1g mode of the bilayer is six times larger than that of the single layer. Schematic crystal structure of molybdenum disulfide. (a) Top view (slightly tilted). (b) Side view.

Two new first-order Raman-active modes are experimentally observed in few-layer MoS${}_{2}$ samples. The authors of this paper show that these modes should appear in virtually all few-layer systems. Since these new modes are symmetry-forbidden in single-layer structures, the results are going to be useful for metrology of layered thin films.

We present Raman measurements of mono- and few-layer ${\mathrm{WS}}_{2}$. We study the monolayer ${A}_{1}^{\ensuremath{'}}$ mode around $420{\mathrm{cm}}^{\ensuremath{-}1}$ and its evolution with the number of layers. We show that with increasing layer number there are an increasing number of possible vibrational patterns for the out-of-plane Raman mode: in $N$-layer ${\mathrm{WS}}_{2}$ there are $N$ $\mathrm{\ensuremath{\Gamma}}$-point phonons evolving from the ${A}_{1}^{\ensuremath{'}}$ monolayer mode. For an excitation energy close to resonance with the $A$ excitonic transition energy, we were able to observe all of these $N$ components, irrespective of their Raman activity. Density functional theory calculations support the experimental findings and make it possible to attribute the modes to their respective symmetries. The findings described here are of general importance for all other phonon modes in ${\mathrm{WS}}_{2}$ and other layered transition-metal dichalcogenide systems in the few-layer regime.

Graphene nanostructures are an important building block to make use of the properties of graphene for applications in integrated devices. It is important to study edge roughness and defects in such nanostructures for further device improvement as they become important when downscaling structures. Recent Raman studies focused mainly on the D mode to characterize the defects in graphene and graphene nanoribbons (GNR) whereas not much attention has been paid to the D′ mode that is smaller in Raman intensity. In this work we show by comparison with AFM measurements of the GNR width that both defect-induced Raman modes have different scattering length scales. Furthermore the size and quality of lithographically defined GNRs can be estimated by a close analysis of the defect-induced Raman modes and the width of the well-studied 2D mode of graphene. The findings are explained by the different vibration pattern for both Raman modes and the differences in the matrix elements determining the Raman intensity, i.e. the electron-phonon coupling and the phonon density of states.

We present a photoluminescence study of freestanding and Si/${\text{SiO}}_{2}$ supported single- and few-layer ${\text{MoS}}_{2}$. The single-layer exciton peak (A) is only observed in freestanding ${\text{MoS}}_{2}$. The photoluminescence of supported single-layer ${\text{MoS}}_{2}$ instead originates from the A${}^{\ensuremath{-}}$ (trion) peak as the ${\text{MoS}}_{2}$ is $n$-type doped from the substrate. In bilayer ${\text{MoS}}_{2}$, the van der Waals interaction with the substrate decreases the indirect band gap energy by up to $\ensuremath{\approx}80$ meV. Furthermore, the photoluminescence spectra of suspended ${\text{MoS}}_{2}$ can be influenced by interference effects.

Two-dimensional nanomaterials such as MoS2 are of great interest both because of their novel physical properties and their applications potential. Liquid exfoliation, an important production method, is limited by our inability to quickly and easily measure nanosheet size, thickness or concentration. Here we demonstrate a method to simultaneously determine mean values of these properties from an optical extinction spectrum measured on a liquid dispersion of MoS2 nanosheets. The concentration measurement is based on the size-independence of the low-wavelength extinction coefficient, while the size and thickness measurements rely on the effect of edges and quantum confinement on the optical spectra. The resultant controllability of concentration, size and thickness facilitates the preparation of dispersions with pre-determined properties such as high monolayer-content, leading to first measurement of A-exciton MoS2 luminescence in liquid suspensions. These techniques are general and can be applied to a range of two-dimensional materials including WS2, MoSe2 and WSe2.

We have investigated the deterioration of field effect transistors based on twodimensional materials due to irradiation with swift heavy ions. Devices were prepared with exfoliated single layers of MoS2 and graphene, respectively. They were characterized before and after irradiation with 1.14 GeV U228+2 ions using three different fluences. By electrical characterization, atomic force microscopy and Raman spectroscopy we show that the irradiation leads to significant changes of structural and electrical properties. At the highest fluence of 4 x 102^11 ions/cm^2, the MoS2 transistor is destroyed, while the graphene based device remains operational, albeit with an inferior performance.

Single layer regions of MoS2 on SiO2 and SrTiO3 were identified by Raman spectroscopy and μ-photoluminescence before Kelvin probe force microscopy was performed. For the already known system MoS2/SiO2 we find 1.839 eV for the direct bandgap, in good agreement with earlier results. On MoS2/SrTiO3 the direct bandgap was determined to be 1.829 eV. From our Kelvin probe data we infer that the SrTiO3 substrate leads to a dipole layer at the interface of the MoS2 single layer. The corresponding μ-PL measurements however show no significant decrease of the bandgap. This shows, that in the case of MoS2 the carrier type as well as concentration is not significantly influenced by the choice of SrTiO3 as the substrate compared to SiO2.

We demonstrate that it is possible to mechanically exfoliate graphene under ultra high vacuum conditions on the atomically well defined surface of single crystalline silicon. The flakes are several hundred nanometers in lateral size and their optical contrast is very faint in agreement with calculated data. Single layer graphene is investigated by Raman mapping. The G and 2D peaks are shifted and narrowed compared to undoped graphene. With spatially resolved Kelvin probe measurements we show that this is due to p-type doping with hole densities of n_h \simeq 6x10^{12} cm^{-2}. The in vacuo preparation technique presented here should open up new possibilities to influence the properties of graphene by introducing adsorbates in a controlled way., Comment: 8 pages, 7 figures