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- BAM-List (6)
- Dangerous goods (6)
- Compatibility evaluations (5)
- Corrosion tests (5)
- High-alloyed metallic tank materials (5)
- Deponieverordnung (4)
- Geokunststoffe (4)
- Zulassungsrichtlinien (4)
- XPS (3)
- BAM-Liste (2)
Organisationseinheit der BAM
- 6 Materialchemie (4)
- 8 Zerstörungsfreie Prüfung (3)
- 5 Werkstofftechnik (2)
- 5.1 Mikrostruktur Design und Degradation (2)
- 6.1 Oberflächen- und Dünnschichtanalyse (2)
- 6.3 Strukturanalytik (2)
- 8.5 Röntgenbildgebung (2)
- 9 Komponentensicherheit (2)
- 5.2 Metallische Hochtemperaturwerkstoffe (1)
- 7 Bauwerkssicherheit (1)
A cross-section sample of the friction film formed on top of a disc during a brake testing procedure against Polymer Matrix Composite pads was made using a Focused Ion Beam (FIB). The FIB-cut sampled the "third body" magnetite layer and the upper part of the cast iron disc containing a graphite flake. Images of the sample examined in a Energy Filtered Transmission Electron Microscope captured an instant view of the important role of the graphite flakes in magnetite formation, where few layer graphene batches interacted with the iron border promoting cracking and oxidation along the graphite–iron interface. The resulting nano-scale interlayer of magnetite and strongly disordered graphite formed a third body which yielded adequate brake performance.
Different, partly complementary and partly redundant characterization methods were applied to study the transition of magnetite, graphite and MoS2 powders to mechanically alloyed nanostructures. The applied methods were: Transmission electron microscopy (TEM), Mössbauer spectroscopy (MS), Raman spectroscopy (RS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The main objective was to prepare a model material providing the essential features of a typical tribofilm forming during automotive braking, and to assess the impact of different constituents on sliding behaviour and friction level. Irrespective of the initial grain size, the raw materials were transferred to a nanocrystalline structure and mixed on a nanoscopic scale during high energy ball milling. Whereas magnetite remained almost unchanged, graphite and molybdenum disulphide were transformed to a nanocrystalline and highly disordered structure. The observed increase of the coefficient of friction was attributed to a loss of lubricity of the latter ingredient due to this transformation and subsequent oxidation.
Measurement and data recording systems are important parts of a holistic Structural Health Monitoring (SHM) system.
New sensor technologies such as fiber-optic sensors are often used; however, standards (or at least guidelines) are not yet available or internationally approved. This lack in standardization makes the acceptance of FOS technologies in complex SHM systems substantially difficult. A standard family for different FOS technologies is therefore being developed that should help to design SHM systems in an optimal way. International standardization activities take place in several standardization bodies such as IEC and ASTM, and within SHM societies such as ISHMII.
The paper reports on activities in standardization of fiber-optic sensors, on results already achieved, and on newly started projects. Combined activities of fiber sensor experts and SHM experts from Civil Engineering are presented. These contributions should help owners of structures as well as developers of sensors and monitoring systems to select effective and validated sensing technologies. Using these standards, both parties find recommendations how to proceed in development of SHM systems to evaluate the structural behavior based on e.g. standardized fiber optic sensors, and to derive necessary measures, e.g. the optimal maintenance strategy.
Richtlinie für die Zulassung von Geotextilien zum Filtern und Trennen für Deponieabdichtungen
(2010)
We report the results of a Versailles Project on Advanced Materials and Standards (VAMAS) interlaboratory study on the measurement of the shell thickness and chemistry of nanoparticle coatings. Peptide-coated gold particles were supplied to laboratories in two forms: a colloidal suspension in pure water and particles dried onto a silicon wafer. Participants prepared and analyzed these samples using either X-ray photoelectron spectroscopy (XPS) or low energy ion scattering (LEIS). Careful data analysis revealed some significant sources of discrepancy, particularly for XPS. Degradation during transportation, storage, or sample preparation resulted in a variability in thickness of 53%. The calculation method chosen by XPS participants contributed a variability of 67%. However, variability of 12% was achieved for the samples deposited using a single method and by choosing photoelectron peaks that were not adversely affected by instrumental transmission effects. The study identified a need for more consistency in instrumental transmission functions and relative sensitivity factors since this contributed a variability of 33%. The results from the LEIS participants were more consistent, with variability of less than 10% in thickness, and this is mostly due to a common method of data analysis. The calculation was performed using a model developed for uniform, flat films, and some participants employed a correction factor to account for the sample geometry, which appears warranted based upon a simulation of LEIS data from one of the participants and comparison to the XPS results.
The influence of the surface roughness of pearlitic grey cast iron discs on the formation of tribofilms and the evolution of the friction coefficient during a ring on disc tribotest with the addition of magnetite and magnetite–graphite nanopowders as interfacial media was investigated. The roughness parameters of the cast iron discs were varied by electro discharge machining (EDM) and grinding processes, producing four distinct surface roughness conditions. The evolution of the friction coefficient, however, did not reach the steady state for most of the samples and the role of the surface roughness on the friction coefficient could not be identified. Focused ion beam (FIB) microscopy on the cast iron discs was carried out to investigate the microstructure of the discs near the tribosurface. These results showed that the EDM process not only varied the surface roughness, but also changed the microstructure of the cast iron discs, promoting the incipient fusion of the cast iron surface, with the formation of ridges and casting defects (pores). As a result, a layer of rapidly solidified metal with a dendritic microstructure was formed near to the surface of the EDMed discs.
The study of protein corona formation on nanoparticles (NPs) represents an actual main issue in colloidal, biomedical and toxicological sciences. However, little is known about the influence of polymer shells on the formation and time evolution of protein corona onto functionalized NPs. Therefore, silicapoly(ethylene glycol) core–shell nanohybrids (SNPs@PEG) with different polymer molecular weights (MW) were synthesized and exhaustively characterized. Bovine serum albumin (BSA) at different concentrations (0.1–6 wt%) was used as model protein to study protein corona formation and time evolution. For pristine SNPs and SNPs@PEG (MW = 350 g/mol), zeta potential at different incubation times show a dynamical evolution of the nanoparticle–protein corona. Oppositely, for SNPs@PEG with MW ≥2000 g/mol a significant suppression of corona formation and time evolution was observed.
Furthermore, AFM investigations suggest a different orientation (side-chain or perpendicular) and Penetration depth of BSA toward PEGylated surfaces depending on the polymer length which may explain differences in protein corona evolution.
A facile and versatile synthetic route for controlling the size and surface potential of organic–inorganic hybrid silica nanoparticles (NPs) is introduced in this paper. For polymer-grafted NPs, the density of polymer chains on the surface is strongly affected by the concentration of precursor. Nevertheless, for condensed NPs, the precursor concentration determines the particle size but not the density of polymer chains on the surface or the adsorption of bovine serum albumin (BSA). Results presented here may have Major implications in biomedical and colloidal chemistry since interfacial and colloidal properties are known to drive several processes associated with nanoparticles in biological media.
A method is described for high-resolution label-free molecular imaging of human bone tissue. To preserve the lipid content and the heterogeneous structure of osseous tissue, 4 μm thick human bone sections were prepared via cryoembedding and tape-assisted cryosectioning, circumventing the application of organic solvents and a decalcification step. A protocol for comparative mass spectrometry imaging (MSI) on the same section was established for initial analysis with time-of-flight secondary ion mass spectrometry (TOF-SIMS) at a lateral resolution of 10 μm to <500 nm, followed by atmospheric pressure scanning microprobe matrix-assisted laser desorption/ionization (AP-SMALDI) Orbitrap MSI at a lateral resolution of 10 μm. This procedure ultimately enabled MSI of lipids, providing the lateral localization of major lipid classes such as glycero-, glycerophospho-, and sphingolipids. Additionally, the applicability of the recently emerged Orbitrap-TOF-SIMS hybrid system was exemplarily examined and compared to the before-mentioned MSI methods.
: Simvastatin is one of the most widely used active pharmaceutical ingredients for the treatment of hyperlipidemias. Because the compound is employed as a solid in drug formulations, particular attention should be given to the characterization of different polymorphs, their stability domains, and the nature of the phase transitions that relate them. In this work, the phase transitions delimiting the stability domains of three previously reported simvastatin forms were investigated from structural, energetics, and dynamical points of view based on single crystal X-ray diffraction (SCXRD), hot stage microscopy (HSM), and differential scanning calorimetry (DSC) experiments (conventional scans and heat capacity measurements), complemented with molecular dynamics (MD) simulations. Previous assignments of the crystal forms were confirmed by SCXRD: forms I and II were found to be orthorhombic (P212121, Z′/Z = 1/4) and form III was monoclinic (P21, Z′/Z = 2/4). The obtained results further indicated that (i) the transitions between different forms are observed at 235.9 ± 0.1 K (form III → form II) and at 275.2 ± 0.2 K (form II → form I) in DSC runs carried out at 10 K min−1 and close to these values when other types of techniques are used (e.g., HSM). (ii) They are enantiotropic (i.e., there is a transition temperature relating the two phases before fusion at which the stability order is reversed), fast, reversible, with very little hysteresis between heating and cooling modes, and occur under single crystal to single crystal conditions. (iii) A nucleation and growth mechanism seems to be followed since HSM experiments on single crystals evidenced the propagation of an interface, accompanied by a change of birefringence and crystal contraction or expansion (more subtle in the case of form III → form II), when the phase transitions are triggered. (iv) Consistent with the reversible and small hysteresis nature of the phase transitions, the SCXRD results indicated that the molecular packing is very similar in all forms and the main structural differences are associated with conformational changes of the “ester tail”. (v) The MD simulations further suggested that the tail is essentially “frozen” in two conformations below the III → II transition temperature, becomes progressively less hindered throughout the stability domain of form II, and acquires a large conformational freedom above the II → I transition. Finally, the fact that these transitions were found to be fast and reversible suggests that polymorphism is unlikely to be a problem for pharmaceutical formulations employing crystalline simvastatin because, if present, the III and II forms will readily convert to form I at ambient temperature.
Die nicht ionisierende elektromagnetische Strahlung im Bereich von Terahertz-Frequenzen ermöglicht berührungslose und zerstörungsfreie Mess- und Prüftechnik in zahlreichen Bereichen. Nach ersten Anwendungen in der Astronomie und der Atmosphärenforschung wurden in letzter Zeit Anwendungsfelder in der Sicherheitstechnik, der Medizintechnik, der Nachrichtentechnik und der zerstörungsfreien Prozess- und Qualitätskontrolle erschlossen. Dielektrische Materialien wie Kunststoffe und Keramiken können von Terahertz-Wellen durchdrungen werden. Das ermöglicht Untersuchungen des Objektinneren ohne spezielle Schutzmaßnahmen, wie sie z.B. beim Röntgen notwendig sind. Die Richtlinie erleichtert die Verständigung zwischen Nutzern, Herstellern und dem Vertrieb von Terahertz-Systemen. In der Richtlinie werden bekannte Einsatzgebiete sowie die eingesetzten Verfahren und Funktionsprinzipien aufgeführt, um den Leser bei der Auswahlentscheidung zu unterstützen. Nach einer kurzen Einführung in die physikalischen Grundlagen und Hinweisen zur elektromagnetischen Verträglichkeit, zum Strahlenschutz und zur regulierten Frequenzvergabe werden die verschiedenen Geräteklassen von Terahertz-Systemen ausführlich vorgestellt. Die Richtlinie gibt Hinweise zur messtechnischen Charakterisierung von Terahertz-Wellen. Einsatzgebiete von Terahertz-Systemen, wie die zerstörungsfreie Prüfung, die Dicken- und Abstandsmessung, die Tomografie und die chemische Analytik, werden mit ihren spezifischen Eigenschaften im Detail beschrieben. Umfangreiche Literaturverweise vereinfachen eine vertiefte Beschäftigung mit den Themen der Richtlinie. Eine tabellarische Übersicht mit einer Zusammenfassung, welche Terahertz-Systeme für welche Anwendungsfelder eingesetzt werden können, vervollständigt die Richtlinie.
This study examines the relationship between the magnetic mesostructure with the microstructure of low carbon steel tungsten inert gas welds. Optical microscopy revealed variation in the microstructure of the parent material, in the heat affected and fusion zones, correlating with distinctive changes in the local magnetic stray fields measured with high spatial resolution giant magneto resistance sensors. In the vicinity of the heat affected zone high residual stresses were found using neutron diffraction.
Notably, the gradients of von Mises stress and triaxial magnetic stray field modulus follow the same tendency transverse to the weld. In contrast, micro-X-ray fluorescence characterization indicated that local changes in element composition had no independent effect on magnetic stray fields.
A gray cast iron disc, which had been submitted to a heavy duty automotive brake test, was examined with energy filtered transmission electron microscopy. A graphite flake in a convenient angular position showed the shear interaction of graphite layers with the iron matrix in nano-scale resolution. Atomic layers of graphite were wedged into the ferritic bulk, allowing the entrance of oxygen and the subsequent formation of magnetite. The exfoliated few-layer graphene batches deformed heavily when forced into the matrix. When Raman spectra from the disc surface, which show distinctive carbonaceous bands, were compared with Raman spectra from graphite subjected to deformation in a shaker mill with different milling times, it could be seen that the shear stress on the brake surface was much more effective to induce disorder than the milling, where compressive and impact forces had been additionally exerted on the sample. During shear load the high anisotropy of elastic modulus in the graphite crystalline structure and the low adhesion between graphite basal planes allowed the exfoliation of wrinkled few-layer grapheme batches, causing the formation of more defect related Raman bands than the mechanical stress during high-energy milling.
To start the large-scale deployment of offshore wind in German waters, the German Federal Ministry for the Environment (BMU) supports the offshore test site "alpha ventus" in the North Sea with a research budget of about 50 million Euro in the next years. The overall objective of the research is to reduce the costs of offshore wind energy deployment in deep water. In order to provide all participating research projects with detailed data, the test site will be equipped with extensive measurement instrumentation.
This research initiative was named RAVE Research at Alpha VEntus and consists of a variety of projects in connection with the installation and operation of alpha ventus. As part of the RAVE initiative, so far the participating institutes and companies have prepared projects on the following topics:
Realization of the joint measurements and data management
Analysis of loads, modelling and further development of the different components of offshore wind turbines
Loads at offshore foundations and structures
Further development of LIDAR wind measuring techniques
Grid integration of offshore wind energy
Monitoring of the offshore wind energy deployment in Germany "Offshore WMEP"
Measurement of the operating noises and modelling of the sound propagation between tower and water
Ecologic research
In Germany the BAM-List Requirements for Tanks for the Transport of Dangerous
Goods is the basis for substance-related prototype approvals for tank containers designed for
the carriage of dangerous goods. Such approval is undertaken by the Federal Institute for
Materials Research and Testing (BAM). Compatibility evaluations of selected metallic
material groups as well as of polymeric gasket and lining materials under the influence of
dangerous goods and water-polluting substances are published in section 5 of the BAM-List.
According to the relevant regulations for rail, road and sea transportation a compulsory
internal inspection after certain intervals is required. The required corrosion resistance
depends on the length of the inspection interval.
There is a large number of dangerous goods with a high corrosivity to metals, where the standard
steels are not corrosion resistant. Chemical companies, transportation providers and tank
producers need tanks made of corrosion-resistant materials in order to protect the tank shell
and prevent contamination of high-value cargo as well as the environment. One solution is to
line the tank with a polymeric material, an alternative solution to corrosion problems is the
application of high-alloyed materials.
Only a narrow limited number of corrosion test results of these high-alloyed materials under
the influence of corrosive dangerous goods are available. In order to change this situation and
include the superaustenitic steels X1NiCrMoCuN25-20-7 (Alloy 926), X1NiCrMoCu32-28-7
(Alloy 31) and the nickel-based alloy NiCr23Mo16Al (Alloy 59) in the BAM-List, BAM,
IKS Dresden and ThyssenKrupp VDM started an comprehensive test program with welded
specimens made. The program comprises corrosion resistance evaluations of the high-alloyed
materials in substances representing 12 major groups of corrosive dangerous goods (e.g.
inorganic halogenides, organic acidic halogenides, halogenic carbonic acids, chlorosilanes,
chlorates, perchlorates, chlorites, hypochlorites and hydrogen sulphates).
The test results, presented in this paper, will be included in the upcoming 8th edition of the
BAM-List and therefore available for the costumer.
Use of Corrosion Resistant High-Alloyed Metallic Materials for Transport Tanks of Dangerous Goods
(2005)
To properly understand and assess the long-term behaviour of geosynthetic materials it is necessary to investigate the various types of possible degradation mechanims. This includes both chemical and mechanical behaviour, and sometimes even their interactions with one another. Clearly, chemical degradation of geosynthetics depends on the polymer type. For example, polyolefins are vulnerable to oxidation; polyesters are susceptible to hydrolysis; and plasticizers can leach from polyvinyl chloride. This paper describes the concept of these three types of degradation, but focuses on the oxidation of polyolefins since the majority of the geosynthetics is made from this type of polymer. The methods used to predict the lifetime of antioxidants and service life of the geosynthetic material will be illustrated. Furthermore, the influence of temperature, pressure, and ultraviolet light on the service life are also demonstrated. Finally, the current specifications targeting the longevity of different geosynthetics are presented.
Regarding mechanical degradation, the paper mainly focuses upon the creep deformation of geogrids and stress crack resistance (SCR) of polyethylene geomembranes and geopipe. The method to assess stress crack resistance is described, and the microscopic mechanisms that lead to such failure are explained. For creep evaluation, different acceleration tests are presented and their applicability with respect to the different types of polymers is illustrated. In addition, the long-term shear behaviour of geocomposites and geosynthetic clay liners is presented.
A new type of test sample for the determination of lateral resolution in surface analysis is presented. The certified reference material BAM-L002 Nanoscale strip pattern for length calibration and testing of lateral resolution is an embedded cross-section of epitaxially grown layers of AlxGa1-xAs and InxGa1-xAs on GaAs substrate. The surface of the sample provides a flat pattern with strip widths of 0.4-500 nm. The combination of gratings, isolated narrow strips and sharp edges of wide strips offers improved possibilities for the calibration of a length scale, the determination of lateral resolution and the optimization of instrument settings. The feasibility of the reference material for an analysis of lateral resolution is demonstrated for SIMS.
Cell cultures form the basis of most biological assays conducted to assess the cytotoxicity of nanomaterials.
Since the molecular environment of nanoparticles exerts influence on their physicochemical properties, it can have an impact on nanotoxicity. Here, toxicity of silica nanoparticles upon delivery by fluid-phase uptake is studied in a 3T3 fibroblast cell line. Based on XTT viability assay, cytotoxicity is shown to be a function of (1) particle concentration and (2) of fetal calf serum (FCS) content in the cell culture medium.
Application of dynamic light scattering shows that both parameters affect particle agglomeration. The DLS Experiments verify the stability of the nanoparticles in culture medium without FCS over a wide range of particle concentrations.
The related toxicity can be mainly accounted for by single silica nanoparticles and small agglomerates. In contrast, agglomeration of silica nanoparticles in all FCS-containing media is observed, resulting in a decrease of the associated toxicity. This result has implications for the evaluation of the cytotoxic potential of silica nanoparticles and possibly also other nanomaterials in standard cell culture.