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Paper des Monats
- ja (32)
The development of a robust hydrogen infrastructure poses challenges to materials exposed to high pressurized hydrogen environments. Polymeric materials, which are expected to perform as seals, gaskets, O-rings, hoses among other applications face high risk of damage due to rapid gas decompression (RGD) which might cause operational safety issues. In this study, we intend to assess the effects of a high pressurized hydrogen environment on carbon black filled (CB) elastomers. The materials were exposed to 100 MPa hydrogen atmosphere at room temperature and at 85°C. Ex-situ characterization was performed during the first 30 minutes after decompression and repeated two days after the exposure when total gas desorption has taken place. The physical and mechanical characteristics of the materials were determined by means of density and volume change, hardness and tensile tests, and dynamic mechanical analysis.
Intermittent microplasticity via dislocation avalanches indicates scale-invariance, which is a paradigm shift away from traditional bulk deformation. Recently, we have developed an experimental method to trace the spatiotemporal dynamics of correlated dislocation activity (dislocation avalanches) in microcrystals (Phys. Rev. Mat. 2 (2018) 120601; Phys. Rev. Mat. 3 (2019) 080601). Here we exploit the temperature sensitive deformation of bcc metals. A marked change of the slip-size distribution is observed in the studied microcrystals, with increasingly small event-sizes dominating with decreasing temperature. This shows how a reduction in thermal energy increasingly suppresses the length-scale of dislocation avalanches, indicating how long-range correlations become gradually limited to the scale of the lattice. Our results further show that the stress-strain response is composed of strain-increments that are either thermally activated or essentially athermal. Temperature-dependent small-scale testing in combination with state-of-the-art discrete dislocation dynamics (DDD) simulations of Nb microcrystals are used to reveal these insights.
Quenching a metallic liquid sufficiently fast can give rise to an amorphous solid, typically referred to as a metallic glass. This out-of-equilibrium material has a long suite of remarkable mechanical and physical properties but suffers from property deterioration via structural relaxation. As a function of time, relaxation may indeed constitute significant threads to safe applications. Consequently, relaxation of glasses has a long history across different amorphous materials and typical characterization methods promote a picture of gradually evolving and smooth relaxation, as for example obtained from mechanical spectroscopy. However, the true structural dynamics and underlying mechanisms remain far from understood and have hampered a physically informed atomic-scale picture of transport and physical aging of glasses.
Here we exploit the ability to track atomic-scale dynamics with x-ray photon correlation spectroscopy (XPCS) and resolve an unprecedented spectrum of short- and long-term relaxation time scales in metallic glasses. Conducted across temperatures and under the application of stress, the results reveal anything else than smooth aging and gradual energy minimization. In fact, temporal fluctuations persist throughout isothermal conditions over several hundred thousand of seconds, demonstrating heterogeneous dynamics at the atomic scale. In concert with microsecond molecular dynamic simulations, we identify possible mechanisms of correlated atomic-scale dynamics that can underly the temporal fluctuations and structural decorrelations. Despite temporally heterogeneous, the Kohlrausch-Williams-Watts functions is well suited to capture the average intermediate relaxation time regime, but at very long time scales an asymptotic power-law emerges. This indicates anomalous diffusion and gives overall strong evidence for temporal fractional diffusion in metallic glasses. We discuss these results in terms of the structural fast and slow relaxation modes as well as a true microstructure in metallic glasses.
Inspired by the ability to track atomic-scale dynamics with x-ray photon correlation spectroscopy (XPCS)1 and recent results of long-term atomistic simulations on material transport2, we reveal here an unprecedented spectrum of short- and long-term relaxation dynamics. Tracked along a 300 000 s long isotherm at 0.98Tg, a Zr-based bulk metallic glass exhibits temporal fluctuations that persist throughout the entire isotherm, demonstrating a continuous heterogeneous dynamics at the probed length scale. In concert with microsecond molecular dynamic simulations, we identify intermittent cluster dynamics as the origin for temporal signatures in the corresponding intensity cross-correlations. Despite temporally heterogeneous aging, the Kohlrausch-Williams-Watts functions is well suited to capture the average intermediate relaxation time regime, but at very long time scales an asymptotic power-law better describes the data. This indicates anomalous diffusion and gives overall strong evidence for temporal fractional diffusion in metallic glasses. We discuss these results in terms of the underlying structural fast and slow relaxation modes and their manifestation in the temporal form of the structural decorrelations.
Metallic glasses (MGs) are disordered solids that exhibit a range of outstanding mechanical, thermomechanical, and functional properties. Whilst being a promising class of structural materials, well-defined and exploitable structure-property relationships are still lacking. This offsets them strongly from the crystalline counterparts, for which length-scale based property determination has been key for decades.
In recent years, both atomistic simulations and experiments have nurtured the view of heterogeneities that manifest themselves either as a structural partitioning into well-relaxed percolated network components and more frustrated domains in atomistic simulations, or as spatially-resolved property fluctuations revealed with atomic force microscopy. These signatures depend sensitively on the processing history and likely reflect emerging medium-range order fluctuations at the scale of 1-10 nanometers.
Here we demonstrate and discuss the emergence of spatially resolved property fluctuations at length scales that are one to two orders of magnitude larger. Such long-range decorrelation length scales are hard to reconcile in a monolithic glass but may offer the perspective of experimentally easy-to-access length-scale based structure-property relationships. Whilst long-range property fluctuations can be seen in both the plastic and elastic response, we focus here on high-throughput elastic nanoindentation mapping across the surface of a Zr-based model glass. After a deconvolution of surface topography and curvature effects, the spatially-resolved elastic response reveals an elastic microstructure with a correlation length of ca. 150-170 nm. Analytical scanning-transmission electron microscopy (STEM) is used to link the elastic property fluctuations to the chemistry and structure of the MG. In concert, nano-elastic mapping and STEM suggests that structural variations in the glass are responsible for the unexpectedly large length scales. We discuss these findings in terms of the materials processing history and the perspective of exploiting nanoindentation-based spatial mapping to uncover structural length scales in atomically disordered solids.
Compatibility of welded austenitic stainless steel (316L) tube for green hydrogen applications
(2024)
The increase in the energy demand and the need to comply to net zero carbon regulations, as per the Paris 2015 climate agreement by 2050, has necessitated the urgency to consider hydrogen as alternative energy carrier. Moreover, hydrogen interaction with metals tend to cause degradation of the mechanical properties in terms of the ductility of the materials. More concern is on the weldment and repair of tubes or pipelines of hydrogen transportation and storage systems. In this study, the heat inducted weld tubes of the cold drawn and annealed austenitic stainless steel (316L) were investigated by slow strain rate test. To achieve the most realistic component-related testing, hollow tube specimens have been fabricated from 1/2-inch Swagelok pipes filled with internal gaseous hydrogen or inert air for reference. The hydrogen concentration measurement is undertaken before and after the autoclave high-pressure pre-charging of the specimens using carrier gas hot extraction. SEM analysis was used to carry out fractographic analysis to determine the crack initiation sites, crack size and was compared for the base material and heat affected zone influence in the gaseous hydrogen. The effect of hydrogen on the material compatibility of the welded austenitic stainless steel is assessed and compared to none-welded tubes tested in defined testing parameters that contribute to Hydrogen Assisted Cracking. A better understanding on the impact of weldment on the structural integrity for stainless steel is elucidated for green hydrogen application.
A hybrid deterministic-probabilistic framework is presented that combines in-situ measurements and numerical analysis to predict the characteristic size of corrosion pits over extended periods of exposure to seawater. A probabilistic model, informed by corrosion current density and temperature data, applies a sampling method to a range of overpotential values to reflect the surface deterioration in terms of pitting. The model is calibrated and validated with pit size data obtained from corroded coupons. Results reveal a positively skewed truncated lognormal distribution of pit depths which implies a higher prevalence of smaller pit depths, corroborated both experimentally and numerically.
Welded steel structures used in the offshore wind industry are exposed to harsh marine environments, which can result in corrosion-induced fatigue damage. Of particular concern is the heat affected zone (HAZ) of welded joints, a region known for its altered microstructure and mechanical properties, which can significantly influence the initiation and propagation of fatigue cracks. This study investigates the short and long fatigue crack growth rates, and the effect of seawater exposure, for the HAZ in S355 steel weldments. Single-edge notch bend (SENB) specimens are used, with a shallow notch in the HAZ. A series of specimens is immersed in synthetic seawater that is continuously circulated at a controlled temperature to assess the synergistic effects of corrosion and fatigue. The experimental method integrates a novel application of front face strain compliance for monitoring short cracks, alongside an extended back-face strain compliance approach for monitoring long crack propagation. It is concluded that the short fatigue crack growth rate of the HAZ is 2.7 to 3.5 times higher in seawater as compared to air. As the crack propagates and enters into the long crack regime, the ratio decreases to 2.2 times at the transition point of the two-stage crack growth curve and further decreases to 1.5 times when the notch advances towards fracture. The findings indicate that the fatigue crack growth rates documented in standards tend to be on the conservative side. This study significantly enriches the fatigue crack growth data available in literature, which will contribute to a more accurate lifetime assessment offshore wind turbine structures.
Early detection of fatigue cracks and accurate measurements of the crack growth play an important role in the maintenance and repair strategies of steel and composite structures exposed to cyclic loads during their service life. Commonly used non-destructive techniques such as strain gauges, clip gauges, ultrasound, etc. used for detection and monitoring of fatigue damage are contact-based and perform local measurements. In addition, complex full-field techniques are commonly investigated, such as digital image correlation (DIC) and infrared thermography (IRT). In this work, a specific implementation of IRT, called lock-in IRT, is implemented for fatigue damage detection. This technique evaluates the thermal stress response of test specimens, specifically focusing or “locking-in” on the frequency of applied cyclic loads. Three different test scenarios are presented.
First, a section of a wind turbine rotor blade made of a glass fibre reinforced plastic (GFRP) shell structure under cyclic load was examined with Lock-In IRT along with DIC. The primary advantage of Lock-In IRT in this test setup was that it required no sample preparation, as compared to the painting and speckle pattern required for DIC. In the frequency domain, specifically the frequency of applied cyclic load, it was possible to extract local directional inhomogeneous loading within the shell structure due to progressive damage, confirmed with the deformation obtained from DIC results.
Second, thick welded specimens made of structural steel S355 were subjected to multiple NDT methods such as strain gauges, crack luminescence penetration (developed specifically at BAM), ultrasound, and IRT, with the aim of investigating the ability of each technique to detect fatigue damage initiation as early as possible in the total fatigue life of the specimen. Amongst the range of implemented techniques, Lock-In IRT provided the first indication of fatigue crack initiation at the weld toe of the specimens. This was validated with the other techniques as well as fractography.
Third, steel S355 specimens used to manufacture offshore wind turbine monopiles were tested. The specimens were extracted from a plate that was submerged in a marine environment, resulting in a corroded surface with corrosion pits. These specimens were subjected to cyclic tensile loads without removing the corrosion pits. The fatigue tests were monitored using IRT in a special full-field capturing setup that enables both sides of the specimen to be examined with one IRT camera. This allowed the entire pitted surface to be monitored for fatigue damage initiation at the same time. With the implementation of Lock In IRT, the surface stress distribution could be captured (the stress concentration at the pits), and fatigue crack initiation could be detected and linked with specific corrosion pits.
Passive infrared thermography as an inspection tool for operational wind turbine rotor blades
(2024)
The growing wind energy infrastructure presents a significant challenge in the maintenance and operation of wind turbines (WT) and their intricate components. An important aspect of WT maintenance is the inspection of wind turbine rotor blades (WTB) to ensure the overall health and safety of the turbine. This inspection process involves both visual and mechanical examinations of the blades to identify any indicators of damage or wear that could compromise their performance and, consequently, the structural integrity of the entire WT system. The complexity of WTBs is compounded by their ever-expanding dimensions, exceeding 100 meters in length for 16 MW WT systems, and their multi-material composition. Within this context, passive infrared thermography emerges as a potential alternative to conventional contact- or proximity-based inspection methods. Unlike active thermography, passive thermography uses solar radiation and ambient temperature variation for thermal contrast, eliminating the need for traditional heat lamps, flash, or laser-based techniques.
A novel inspection method has been developed to semi-autonomously assess wind turbine blades (WTBs) while the wind turbine (WT) is operational, from ground level. This approach leverages optimal thermal contrast, which depends on prevailing weather conditions during field measurements, enabling the visualization of both external and internal features of the WTBs through post-processing techniques. In this study, thermal data obtained through passive thermography is compared with contemporaneous visual imagery to definitively classify observed features in thermal images as either surface or sub-surface features. This analysis, coupled with corresponding weather conditions, provides valuable insights into the capabilities and limitations of the inspection technique. Additionally, finite-element-based (FE) thermal simulations of a WTB section are employed to parametrically assess the influence of weather conditions, beyond those observed during field measurements, based on a validated model.
In addition, the thermal images also consist of thermal signatures of leading-edge turbulence due to possible leading-edge erosion in WTBs. These are primarily vortices, and their shape and size depend on the morphology of the damage as well as the rotational speed of the WTBs. The inspections are accompanied by automatic data evaluation of the thermal signatures. To improve the precision of erosion damage identification, a fully convolutional network (FCN) is employed, trained, and tested using over 1000 annotated thermographic blade images. Additionally, the study introduces strategies for grouping smaller damage indications and simplification rules based on realistic thermal imaging resolutions. As leading-edge erosion could potentially lead to annual energy production (AEP) losses, this technique could prove to be a powerful tool in establishing the presence of damage and the resulting AEP loss.
Development of efficient portable sensors for accurately detecting biomarkers is crucial for early disease diagnosis, yet remains a significant challenge. To address this need, we introduce the enhanced luminescence lateral-flow assay, which leverages highly luminescent upconverting nanoparticles (UCNPs) alongside a portable reader and a smartphone app. The sensor’s efficiency and versatility were shown for kidney health monitoring as a proof of concept. We engineered Er3+- and Tm3+-doped UCNPs coated with multiple layers, including an undoped
inert matrix shell, a mesoporous silica shell, and an outer layer of
gold (UCNP@mSiO2@Au). These coatings synergistically enhance emission by over 40-fold and facilitate biomolecule conjugation, rendering UCNP@mSiO2@Au easy to use and suitable for a broad range of bioapplications. Employing these optimized nanoparticles in lateral-flow assays, we successfully detected two acute kidney injury-related biomarkers-kidney injury molecule-1 (KIM-1) and neutrophil gelatinase-associated lipocalin (NGAL)-in urine samples. Using our sensor platform, KIM-1 and NGAL can be accurately detected and quantified
within the range of 0.1 to 20 ng/mL, boasting impressively low limits of detection at 0.28 and 0.23 ng/mL, respectively. Validating our approach, we analyzed clinical urine samples, achieving biomarker concentrations that closely correlated with results obtained via ELISA. Importantly, our system enables biomarker quantification in less than 15 min, underscoring the performance of our novel UCNP-based approach and its potential as reliable, rapid, and user-friendly diagnostics.
Parameter studies are a common step in selecting process parameters for powder bed fusion of metals with laser beam (PBF-LB/M). Density cubes manufactured with varied process parameters exhibit distinguishable surface structures visible to the human eye. Industrial visual in-situ monitoring systems for PBF-LB/M currently have limited resolution and are incapable of reliably capturing differences in the surface structures. For this work, a 65 MPixel high resolution monochrome camera is integrated in an industrial PBF-LB/M machine together with a high intensity led bar. Post-exposure images are taken to analyze differences in light reflection on the specimen’s surface. The grey level co-occurrence matrix is used to quantify the in-situ measured visual surface structure of nickel-based super alloy IN939 density cubes. The properties of the grey level co-occurrence matrix correlate to the energy input and resulting porosity of specimens. Low energy samples with lack of fusion flaws show an increased contrast in the grey level co-occurrence matrix compared to specimens with an optimal energy input. The potential of high-resolution images as reference data in in-situ process monitoring in PBF-LB/M is discussed.
The hydrogen economy is one of the most important solutions to achieve climate neutrality in Europe. It involves the production, storage, transport and use of large quantities of hydrogen in existing and new infrastructures. Components along this supply chain, such as pipelines and storage tanks, are made of various metallic materials, with steel being the most common construction material. The rapid introduction of hydrogen therefore brings with it major challenges, in particular the need for comprehensive qualification of components and materials to ensure the sustainable and safe use of hydrogen technologies. This article provides an overview of the state of the art in the testing of materials and components as well as corresponding future trends and developments for a successful transition to a hydrogen economy.
Antimicrobial resistance (AMR) is a global health problem. It is well known that antibiotics can drive evolutionary processes that underlie antimicrobial resistance (AMR) evolution and spread in clinical and environmental settings. In contrast, less is known about the effects of antimicrobial substances that are used as biocides (i.e. disinfectants and preservatives) on AMR evolution and spread. Biocides are present in various settings, interacting with diverse microbial communities. Therefore, it is crucial to evaluate their role in the evolution and dissemination of antimicrobial resistance. Biocides occur in a wide range of concentrations in various environmental settings. By examining how the various concentrations affect selection mechanisms, we gain insights into potential developments related to antimicrobial resistance. The aim of this PhD thesis is to investigate the effects of biocides on processes underlying resistance evolution. Specifically, the work focused on key mechanisms for resistance spread, resistance evolution, and the effect of selection pressures on evolved resistance mechanisms. The thesis is structured around three major objectives: (i) to determine the effect of biocides on the evolution of resistance by affecting the rate of occurrence of de novo mutations, (ii) to determine the effect of biocides on the spread of resistance genes by modifying the rate of horizontal gene transfer (HGT) processes, and (iii) to investigate the selective drivers of the emergence of antimicrobial resistance in adaptive laboratory evolution (ALE) experiments. De-novo mutations are spontaneous mutations that occur at a certain rate in microorganisms. The effect of biocides at subinhibitory environmentally relevant concentrations on the mutation rate in Acinetobacer baylyi, Bacillus subtilis and Escherichia coli was assessed with the fluctuation assay. The results showed that biocides affected mutation rates in a species and substance dependent matter. The bisbiguanide chlorhexidine digluconate, the quaternary ammonium compound didecyldimethylammonium chloride, the metal copper, the pyrethroid-insecticide permethrin, and the azole-fungicide propiconazole increase mutation rates in E. coli, whereas no increases were identified for B. subtilis and A. baylyi. Horizontal gene transfer refers to diverse mechanisms that mediate the transfer of mobile genetic elements between microorganisms. This work focused on conjugation and transformation. Conjugation is a process whereby a conjugative plasmid is transferred from a donor cell to a recipient cell. Transformation is a process whereby exogenous donor DNA is taken up into a recipient cell and integrated into the recipient’s’ genome. The effects of subinhibitory environmentally relevant biocide concentrations on the conjugation rate of E. coli and the transformation rate of the naturally competent organisms A. baylyi in were assessed. The results showed that benzalkonium chloride (BAC), chlorhexidine and permethrin increased conjugation in E. coli, while none of the biocides increased transformation rates in A. baylyi. To further understand the molecular mechanisms underlying the effects on mutation and conjugation rates, I investigated the induction of the RpoS-mediated general stress and the RecA-linked SOS response upon biocide exposure. The results show a link between the general stress and the SOS response with increased rates of mutation and conjugation, but not for all biocides. One major approach to study the evolutionary response of bacteria to antimicrobials are ALE experiments with growth at subinhibitory concentrations linked to serial subculturing over many generations. Such experiments have been used to study resistance evolution to antibiotics and biocides. However, previous work showed that adaptation to biocide stress may be mediated by different evolutionary drivers. Here, I investigated the contributions of evolution for increased survival as opposed to improved growth in ALE experiments with E. coli exposed to subinhibitory BAC concentrations. Two distinct evolutionary treatments selecting for survival only or survival and growth led to specific evolutionary adaptations apparent in the phenotypes and genotypes of the evolved populations. Populations growing in the presence of BAC evolved increased fitness in the presence of BAC associated with higher resistance to BAC and cross-resistance to antibiotics, while this was not the case for populations evolving for increased survival only. Genotypic characterization by whole genome sequencing of the evolved populations revealed parallelism in mutated genes among replicate populations and distinct differences across treatments. Treatments selecting for survival and growth showed mutations in stress response related genes (hslO and tufA), while selection for survival led to mutations in genes for metabolic regulation (cyaA) and cellular structure (flagella fliJ). In summary, this thesis shows that biocides affect AMR evolution and emphasizes the importance of understanding of how biocides impact the molecular and evolutionary process that underlie AMR evolution.
The application of an external magnetic field has been found to significantly mitigate the porosity ratio in laser beam welded joints of AlMg3 aluminum alloy. To investigate the suppression mechanism, a 3D transient multi-physics coupled numerical model of laser beam welding (LBW), including laser propagation, laser-material interaction, and magnetohydrodynamic effects, has been developed to calculate the keyhole dynamics and weld pool behaviors during the welding process. The induced time-averaged Lorenz force is directed downward. Under the effects of the external magnetic field, the fluid flow pattern and the weld pool profile are both affected. The keyhole geometry reconstruction algorithm is proposed to calculate the keyhole diameter and its fluctuation, which is used to evaluate the keyhole stability. The results indicate that the oscillating magnetic field does not affect keyhole stability obviously in the LBW of aluminum alloy. Moreover, an electromagnetic expulsive force is induced on the bubble because of the time-averaged downward Lorentz force. This electromagnetic expulsive force can accelerate the bubble escape speed considerably. An analytical model is developed for investigating the bubble escape window, which shows that the bubble escape window is expanded by 45% under the effect of the external magnetic field. The calculated results based on the developed model agree well with the experimental results.
Advanced light weight applications like aircrafts and wind turbine blades are made of fibre reinforced plastics (FRP) with continuous fibre reinforcement and must withstand a high thermo-mechanical cyclic loading. The quality of the fibre matrix interface has a high impact on the fatigue life and was continuously improved over the years since the 50th. The fatigue life of glass fibre reinforced plastics (GFRP) used in aircraft industry is 10 to 100 times higher compared to glass fibre non crimp fabrics used for wind turbine blades.
To assure a constant and reliable high quality and strength of reinforcement fibres, synthetic fibre production is state of the art (CF, GF). There is a need for recycling GFRP and CFRP waste due to the upcoming use. Pyrolysis and solvolysis are more expensive than the mechanical route however enable a more sustainable recycling. Natural fibres and recycled synthetic fibres have a high scatter in quality and strength. Hence it is a challenge to optimize the production / recycling processes to get a reliable quality for any demanding (second life) application.
Chemical routes for using renewables resources and recycling, is going to be a good approach especially for polymer-matrix systems to get 100% quality (back) compared to the state of the art.
Finally, a proper design, life-time extension and repair is preferable to recycling to keep the carbon footprint as low as possible.
The Modified Varestraint Transvarestraint test is a local variant of the globally used Varestraint test. With these tests, measuring solidification cracking susceptibility as a function of welding parameters is possible. A wide range of welding parameters for four high-strength steel filler wires, including three solid wires and one-flux cored metal wire, were tested. All wires do show a very low solidification cracking susceptibility, regardless of the paramaters. On a low level, it could be shown that solidification cracking susceptibility increases with heat input and welding speed.
Testing of highly restraint high-strength fillet welds with regards to solidification cracking susceptibility. The Controlled Thermal Severity test was used to apply a high amount of strain to solidifying welds. Test welds were cut and observed under an optical light microscope. A clear positive correlation between restraint intensity and measured crack sizes, as well as heat input and measured crack sized could be observed.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.