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Paper des Monats
- ja (68)
Ergopeptides, like ergocornine and a-ergocryptine, exist in an S- and in an R-configuration. Kinetic experiments imply that certain configurations are preferred depending on the solvent. The experimental methods are explained in this article. Furthermore, computational methods are used to understand this configurational preference. Standard quantum chemical methods can predict the favored configurations by using minimum energy calculations on the potential energy landscape. However, the explicit role of the solvent is not revealed by this type of methods. In order to better understand its influence, classical mechanical molecular simulations are applied. It appears from our research that 'folding' the ergopeptide molecules into an intermediate state (between the S- and the R-configuration) is mechanically hindered for the preferred configurations.
Slicing - a new method for non destructive 3D elemental sensitive characterization of materials
(2014)
Recent advances in synchrotron sources and detector technology have led to substantial improvements in spatial resolution and detection limits for X-ray fluorescence analysis (XRF). However, the non-destructive three-dimensional elemental sensitive characterization of samples remains a challenge. We demonstrate the use of the so-called 'Color X-ray Camera' (CXC) for 3D measurements for the first time. The excitation of the sample is realized with a thin sheet-beam. The stepwise movement of the sample allows getting the elemental distribution for each layer with one measurement. These layers can be combined to a full 3D dataset for each element afterwards. Since the information is collected layer by layer, there is no need to apply reconstruction techniques, which quite often are the reason for artifacts in the results achieved by computed tomography (CT). The field of applications is wide, as the 3D elemental distribution of a material contains clues to processes inside the samples from a variety of origins. The technique is of special interest and well suited for biological specimens, because their light matrix minimizes restricting absorption effects. Measurement examples of a hornet and the teeth of a Sorex araneus are shown.
In this work an air-based sensor network for the localization of persons at extensive areas is presented. The developed network consists of a localization device which the person is wearing (BodyGuard-System), a mobile relay station in the air, and a base station. All three parts communicate with the same radio chip. The BodyGuard-System is an inertial navigation system which was developed for localization in difficult environments with high accuracy and low measurement uncertainty. To increase the range of the system, a multi-hop network was built up. The measured data of the BodyGuard-System and the mobile relay station is visualized on a PC in the base station. This multi-hop network is necessary for example for fire department missions.
The adsorption of porphyrin derivatives on a Au(111) surface was studied by scanning tunneling microscopy and spectroscopy at low temperatures in combination with density functional theory calculations. Different molecular appearances were found and could be assigned to the presence of single gold adatoms bonded by a coordination bond underneath the molecular monolayer, causing a characteristic change of the electronic structure of the molecules. Moreover, this interpretation could be confirmed by manipulation experiments of individual molecules on and off a single gold atom. This study provides a detailed understanding of the role of metal adatoms in surface–molecule bonding and anchoring and of the appearance of single molecules, and it should prove relevant for the imaging of related molecule–metal systems.
Bei der Abschätzung der Beständigkeit von Kunststoffen gegenüber niedermolekularen Flüssigkeiten ist die Kohäsionsenergiedichte CED ein wichtiger Parameter auf molekularer Ebene. Die Vernetzungsdichte ν eines polymeren Festkörpers bildet hierbei einen bedeutsamen Kennwert, der darüber hinaus neben der Löslichkeit wichtige Eigenschaften wie thermische Stabilität und Steifigkeit des Materials charakterisiert. Für die experimentelle Bestimmung von CED und ν eignet sich die Untersuchung des Quellverhaltens in unterschiedlichen Lösungsmitteln. Es werden zwei Messmethoden miteinander verglichen und die Ergebnisse unter Berücksichtigung des molekularen Aufbaus von Proben aus Polyurethan (PU) und hochmolekularem – (HMWPE) und ultrahochmolekularem Polyethylen (UHMWPE) diskutiert. Zum Verständnis des Quellverhaltens dieser Polymerproben in niedermolekularen Lösungsmitteln werden neben den Messergebnissen Literaturdaten zu Grunde gelegt.
We present a systematic study on the effect of surface ligands on the luminescence properties and colloidal stability of β-NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), comparing nine different surface coatings to render these UCNPs water-dispersible and bioconjugatable. A prerequisite for this study was a large-scale synthetic method that yields ~2 g per batch of monodisperse oleate-capped UCNPs providing identical core particles. These ~23 nm sized UCNPs display an upconversion quantum yield of ~0.35% when dispersed in cyclohexane and excited with a power density of 150 W cm-2, underlining their high quality. A comparison of the colloidal stability and luminescence properties of these UCNPs, subsequently surface modified with ligand exchange or encapsulation protocols, revealed that the ratio of the green (545 nm) and red (658 nm) emission bands determined at a constant excitation power density clearly depends on the surface chemistry. Modifications relying on the deposition of additional (amphiphilic) layer coatings, where the initial oleate coating is retained, show reduced non-radiative quenching by water as compared to UCNPs that are rendered water-dispersible via ligand exchange. Moreover, we could demonstrate that the brightness of the upconversion luminescence of the UCNPs is strongly affected by the type of surface modification, i.e., ligand exchange or encapsulation, yet hardly by the chemical nature of the ligand.
Quantitative determination of acidic surface sites is highly important for the characterization of solid acids because the activity of a catalyst is often related to the concentration of these sites. A recently developed method using 15N Nuclear Magnetic Resonance spectroscopy (NMR) for the quantification of acidic Lewis and Brønsted sites has been tested for a series of nanoscopic aluminum hydroxide fluorides. Comparison with other methods for the quantitative determination of acidic sites shows that this 15N NMR quantification method is a promising technique for the comprehensive investigation of acidic sites. Three different acidic sites, one Brønsted and two Lewis sites, can be distinguished by their 15N chemical shifts of pyridine and simultaneously quantified under conditions corresponding to catalytic reaction conditions. Determination of the individual concentrations of acidic sites allows further insight into the catalytic process. It was found that the concentration of Brønsted sites correlates with catalyzed conversion of citronellal to isopulegol in the investigated series of catalysts. Additionally, investigations indicate that one of the Lewis sites become blocked during the reaction of citronellal.
The digital photography has almost completely substituted the film photography. The film replacement is also fast progressing in medical X-ray radiography. This process is slower in NDT and especially in Europe. Reasons for the hesitating change to digital radiography (RT-D) in NDT are the necessary time for adoption of standards and the conservative request for film RT by auditors and NDT managers for applications in large plants and at construction areas. The fast serial inspection for small castings is already almost completely dominated by RT-D due to the cost effective short exposure and interpretation times. Standards were developed in parallel at CEN, ISO, ASTM and ASME. Unfortunately, the standard practices are different and the requirements on image quality and useable hardware are different too. The first standard series on Computed Radiography were developed and published by CEN and ASTM in 2005. Harmonized classification and qualification standards are available but the published practices are different. ASTM has developed the first standards for application of Digital Detector Arrays (DDA) in 2010. The first digital RT ISO standard practice is ISO 17636-2 (2013), which describes the practice for application of DDAs and Imaging Plates for weld inspection. At the first time this standard provides requirements for the selection of suitable hardware. Minimum image quality requirements are specified in analogy to film radiography and 3 Compensation Principles are defined to enable the application of a wider range of digital detectors. A comparison of the different international digital RT standards is given and first experiences with ISO 17636-2 are discussed. New standards on RT wall thickness and corrosion measurements (EN 16407, film and digital) have been developed recently.
A comparative study on the performance of digital detector systems for high energy applications
(2014)
For cast components reaching or exceeding total material thicknesses of 150mm, high energy sources such as linear accelerators or Betatrons are required in order to obtain reasonable exposure times. In this study, the performance of digital detector systems, involving imaging plates (IP) and digital detector arrays (DDA), was evaluated with respect to the testing class B requirements as formulated in the standard EN ISO 17636-2. As a reference, traditional radiographic film and a Cobalt-60 source was used. With film exposures, testing class B was achieved with Co-60 and Betatron (7.5 MV) at longer exposure times. The preliminary results show that the testing class B was not obtained with the examined digital detector arrays (DDA) and the high resolution imaging plates (IP) , even at 40, 60 and 80 minutes exposure time with a 7.5 MV Betatron. Class A was achieved using high resolution imaging plates with optimized metal filters between object and IPs and a high resolution DDA with intermediate Cu filters. Class A was also achieved applying a DDA with lower basic spatial resolution than required by Table B.13 of EN ISO 17636-2, but using the compensation principle as described in this standard. The next generation of digital detector arrays might potentially be able to obtain class B performance with the expected spatial resolution and sensitivity improvements.
The progress in X-ray detector electronics (sensitivity and speed) allows meanwhile fast single photon detection by a matrix detector. Combined photon counting and energy discrimination is implemented in the electronic circuit of each detector pixel. The company XCounter developed detectors based on CdTe single crystals, which can be tiled to larger areas and have a pixel size of 100ìm. The largest area available in beginning of 2014 is 50x75 mm². These detectors have very promising properties, which make them very suitable for NDT applications:
1. A CdTe attenuation layer of 750 µm thickness allows efficient X-ray detection up to ca. 300 keV. In counting mode only photon noise is important; no other detector noise sources need to be considered. There is no Offset signal without radiation.
2. Each of the detector pixels has two energy thresholds. These can be used for dual energy imaging for materials separation. Also the suppression of scattered radiation by energy thresholding will improve the image contrast sensitivity. First experiments will be presented which demonstrate the advantages of this new detector technology over the conventional charge integrating detectors.
A challenge is the development of a modified detector calibration procedure, which becomes critical at longer exposure times.
The objects of this investigation were sculptures taken from a ca. three hundred years old baroque epitaph of a church in Tonning, a town in Northern Germany. Around 1900 it was found in a disastrous state heavily damaged by wood-worm. At that time, the whole artwork was treated with the tar extract carbolineum as a remedy. Nowadays, this substance has been identified as carcinogenic, and its presence can be perceived by its stench and visually at certain spots on the surface where it has penetrated the covering paint.
A gold-painted sculpture of a massive wooden skull was interrogated with X-rays and fast neutrons to investigate the internal distribution of the carbolineum. The X-ray tomography, with its excellent spatial resolution revealed galleries left over from the worm infestation in the outer areas and cracks in the central region. The golden color coating appeared as a thick and dense layer. In comparison the tomography with fast neutrons, though being of lower resolution and yet unresolved artefacts revealed sections of slightly different densities in the bulk of the wood. These differences we attribute to the differences in the distribution of the impregnant in the wood, visible due to its higher hydrogen content making it less transparent for neutrons.
Using ultrafast X-ray diffraction, we study the coherent picosecond lattice dynamics of photoexcited thin films in the two limiting cases, where the photoinduced stress profile decays on a length scale larger and smaller than the film thickness. We solve a unifying analytical model of the strain propagation for acoustic impedance-matched opaque films on a semi-infinite transparent substrate, showing that the lattice dynamics essentially depend on two parameters: One for the spatial profile and one for the amplitude of the strain. We illustrate the results by comparison with high-quality ultrafast X-ray diffraction data of SrRuO3 films on SrTiO3 substrates.
Innovative X-ray backscatter technique for security applications: Detection of dangerous materials
(2014)
Radiological inspections, in general, are NDT&E methods to detect the bulk of explosives without invasion into the object of analysis. In contrast to personal luggage, cargo or structural components constitute a complexity that may significantly hamper the detection of a threat by conventional transmission radiography. A novel approach of interrogating a large object to a certain depth only with a single sided access will be presented. It consists of an X-ray backscatter camera with a special twisted slit collimator for imaging backscattered objects. The new X-ray backscatter camera is not only imaging the objects due to their densities but also by taking into account the influences of surrounding objects. Additionally, it does not only image illuminated features but also depicts shadows from absorbing materials. This is a unique characteristic of the developed X-ray backscatter camera. Experimental mock-ups are conducted imitating container with threats among a complex packing as they may be encountered in reality. At the end, the significant advantages of the presented X-ray backscatter camera in the context of aviation and port security will be discussed.
In this contribution, we present a dual high-energy X-ray imaging technique for cargo container inspection using the 'spectral high-energy X-ray attenuation method'. This method is based on attenuation of continuous highenergy spectra. The developed experimental technique consists of a betatron as high-energy (up to 7.5 MeV) X-ray source and a matrix detector with high spatial resolution (400 ìm) for digital X-ray imaging. In order to evaluate the material discrimination capability using dual high-energy X-ray imaging, a test specimen is proposed, comprising step wedges of different low and high atomic number (Z) materials. The selected X-ray spectra for the dual-energy experiments correspond to 3 MV and 7.5 MV acceleration potential of the betatron. We evaluated the ratio between low- and high-energy X-ray attenuation coefficients quantitatively based on simulated poly-energetic high-energy X-ray source spectra and the detector sensitivity using the 'analytical Radiographic Testing inspection simulation tool' (aRTist) developed at BAM. The simulated effective attenuation coefficients are compared with corresponding experimental results in order to establish a method for identification of low- and high-Z materials in the container. Finally, important applications of the proposed technique in the context of aviation security are discussed.
Critical parts in aircraft manufacturing such as stringers are very commonly used in modern aircraft structures to resist the compressive loads caused by the aerodynamic effects. They are generally made-up of thin aluminium (Al) metal sheets and are one of the key components in the aircraft wings. Any defects in the stringer leads to weakening of the stiffness of the whole wing structure and consequently, failures may occur. Hence, the structural integrity of the stringers should be evaluated using reliable non-destructive testing (NDT) methods. Due to the complex shaped structure of the stringer, the one-sided access NDT method such as X-ray backscatter technique is more preferable for the non-destructive imaging. In this paper, we present a new X-ray backscatter technique to image the internal sections of the stringer with only a single-sided access. The whole object was inspected by changing the viewing direction of the X-ray backscatter camera. For the first time, the X-ray backscatter measurements were conducted using high-energy (> 0.5MeV) X-rays and proved the applicability of the present technique to inspect thick carbon-fiber laminated components. In order to improve the inspection time and image quality of the backscatter image, we used high-resolution (180ìm) digital detector arrays (DDAs). At the end, important applications of the presented X-ray backscatter technique to the aerospace industry are discussed.
Genetic transformation of Knufia petricola A95 - a model organism for biofilm-material interactions
(2014)
We established a protoplast-based system to transfer DNA to Knufia petricola strain A95, a melanised rock-inhabiting microcolonial fungus that is also a component of a model sub-aerial biofilm (SAB) system. To test whether the desiccation resistant, highly melanised cell walls would hinder protoplast formation, we treated a melanin-minus mutant of A95 as well as the type-strain with a variety of cell-degrading enzymes. Of the different enzymes tested, lysing enzymes from Trichoderma harzianum were most effective in producing protoplasts. This mixture was equally effective on the melanin-minus mutant and the type-strain. Protoplasts produced using lysing enzymes were mixed with polyethyleneglycol (PEG) and plasmid pCB1004 which contains the hygromycin B (HmB) phosphotransferase (hph) gene under the control of the Aspergillus nidulans trpC. Integration and expression of hph into the A95 genome conferred hygromycin resistance upon the transformants. Two weeks after plating out on selective agar containing HmB, the protoplasts developed cell-walls and formed colonies. Transformation frequencies were in the range 36 to 87 transformants per 10 µg of vector DNA and 106 protoplasts. Stability of transformation was confirmed by sub-culturing the putative transformants on selective agar containing HmB as well as by PCR-detection of the hph gene in the colonies. The hph gene was stably integrated as shown by five subsequent passages with and without selection pressure.
Thermally reduced graphite oxide (TRGO), containing only four single carbon layers on average, was combined with ammonium polyphosphate (APP) and magnesium hydroxide (MH), respectively, in polypropylene (PP). The nanoparticle's influence on different flame-retarding systems and possible synergisms in pyrolysis, reaction to small flame, fire behavior and mechanical properties were determined. TRGO has a positive effect on the yield stress, which is decreased by both flame-retardants and acts as a synergist with regard to Young's modulus. The applicability and effects of TRGO as an adjuvant in combination with conventional flame-retardants depends strongly on the particular flame-retardancy mechanism. In the intumescent system, even small concentrations of TRGO change the viscosity of the pyrolysing melt crucially. In case of oxygen index (OI) and UL 94 test, the addition of increasing amounts of TRGO to PP/APP had a negative impact on the oxygen index and the UL 94 classification. Nevertheless, systems with only low amounts (≤1 wt%) of TRGO achieved V-0 classification in the UL 94 test and high oxygen indices (>31 vol%). TRGO strengthens the residue structure of MH and therefore functions as a strong synergist in terms of OI and UL 94 classification (from HB to V-0).
In this article, the high potential of the fluorolytic sol–gel process to synthesize nanoscopic rare earth-doped calcium fluoride sols is shown. Through a fluorolytic sol–gel process we manage to achieve spherical monodisperse ~5 nm sized nanoparticles using a simple and reproducible one-pot-wet chemical route at room temperature. The as-synthesized clear sols exhibit an intense red and green luminescence under UV excitation at room temperature. A spectroscopic study of the sols revealed the characteristic transitions 5D0 → 7FJ of Eu3+ and 5D4 → 7FJ of Tb3+, with 5D0 → 7F2 (611 nm) of Eu3+ and 5D4 → 7F4 (581 nm) of Tb3+ as the most prominent transitions. This facile synthetic strategy is also valuable for developing other luminescent nanoparticles.
Der Large Hadron Collider (LHC) des europäischen Kernforschungszentrums CERN ist einer der weltweit größten und leistungsfähigsten Teilchenbeschleuniger. Um den Teilchenstrahl auf seiner Kreisbahn zu halten, werden mit Hilfe supraleitender Spulen sehr starke Magnetfelder erzeugt. Die hierzu benötigten hohen Ströme werden über Verbunddrähte aus Niob-Titan und Kupfer geleitet.
Die Drähte werden u.a. durch Ultraschallschweißungen miteinander verbunden. Eine mangelhafte Verbindung kann zur Erwärmung der Kontaktstelle und in Folge davon zum Zusammenbruch der Supraleitung führen. Auf Anfrage des CERN wurden an der BAM Untersuchungen zur Prüfbarkeit solcher Verbindungen bei Umgebungstemperatur durchgeführt. Es gelang, für einen Verbindungstypen einen Wirbelstromsensor für eine manuelle Prüfung zu entwickeln. Ein Prototyp des Sensors befindet sich beim CERN in der praktischen Erprobung. Das Sensorprinzip sowie Prüfergebnisse aus Labor und Praxis werden vorgestellt.
A flexible, sustainable, one-step thermal decomposition route for the synthesis of hierarchical, heteroatom doped carbon foams is presented. Task-specific semi-organic crystals combine functions for three different purposes: the carbon and heteroatom source, a foaming agent (CO2) and an in situ generable template (NaCl). Insights to the decomposition pathway were gained through FTIR/MS coupled TGA and an ultrafast out-of-furnace heating procedure and the products were analysed with (HR)SEM/TEM, EELS, FTIR, and N2 sorption. The resulting macroporous carbon foams are excellent supports for metallic nanoparticles due to their hierarchical structure, high surface area and tuneable heteroatom contents. This was demonstrated for catalytically active copper or the magnetic CoNi alloy for water purification.
Structural properties of iron-phosphate glasses: spectroscopic studies and ab initio simulations
(2014)
Vitrification is the most effective method for the immobilization of hazardous waste by incorporating toxic elements into a glass structure. Iron phosphate glasses are presently being considered as matrices for the storage of radioactive waste, even of those which cannot be vitrified using conventional borosilicate waste glass. In this study, a structural model of 60P2O5–40Fe2O3 glass is proposed. The model is based on the crystal structure of FePO4 which is composed of [FeO4][PO4] tetrahedral rings. The rings are optimized using the DFT method and the obtained theoretical FTIR and Raman spectra are being compared with their experimental counterparts. Moreover, the proposed model is in very good agreement with X-ray absorption fine structure spectroscopy (XANES/EXAFS) and Mössbauer spectroscopy measurements. According to the calculations the Fe3+ is in tetrahedral and five-fold coordination. The maximal predicted load of waste constituents into the glass without rebuilding of the structure is 30 mol%. Below this content, waste constituents balance the charge of [FeO4]- tetrahedra which leads to their strong bonding to the glass resulting in an increase of the chemical durability, transformation and melting temperatures and density.
Rigid rod-type metallo-supramolecular coordination polyelectrolytes with Fe(II) centres (Fe-MEPEs) are produced via the self-assembly of the ditopic ligand 1,4-bis(2,2':6',2''-terpyridine-4'-yl)benzene (tpy-ph-tpy) and Fe(II) acetate. Fe-MEPEs exhibit remarkable electrochromic properties; they change colour from blue to transparent when an electric potential is applied. This electrochemical process is generally reversible. The blue colour in the ground state is a result of a metal-to-ligand charge transfer at the Fe(II) centre ion in a quasi-octahedral geometry. When annealed at temperatures above 100 °C, the blue colour turns into green and the formerly reversible electrochromic properties are lost, even after cooling down to room temperature. The thermally induced changes in the Fe(II) coordination sphere are investigated in situ during annealing of a solid Fe-MEPE using X-ray absorption fine structure (XAFS) spectroscopy. The study reveals that the thermally induced transition is not accompanied by a redox process at the Fe(II) centre. From the detailed analysis of the XAFS spectra, the changes are attributed to structural changes in the coordination sphere of the Fe(II) site. In the low temperature state, the Fe(II) ion rests in a quasi-octahedral coordination environment surrounded by six nitrogen atoms of the pyridine rings. The axial Fe–N bond length is 1.94 Å, while the equatorial bond length amounts to 1.98 Å. In the high temperature state, the FeN6-site exhibits a distortion with the axial Fe–N bonds being shortened to 1.88 Å and the equatorial Fe–N bonds being elongated to 2.01 Å.
-Background-
Laboratory leaching tests on treated wood were performed during a European robustness study in the framework of the validation of a tank leaching test procedure that has been proposed for construction products in order to determine the potential release of dangerous substances which can be transferred to soil and groundwater. The release of substances has to be determined also for materials treated with biocidal products according to the requirements of the European Biocidal Products Regulation. A similar leaching test procedure was already harmonised for treated wood for this purpose. Both test procedures were applied in parallel to wood treated with the same preservative to investigate whether the results of these tests can replace each other. Additional experiments were performed to further investigate unexpected effects of L/A ratio on leaching of copper and duration of storage of treated test specimens.
-Results-
Both procedures generate similar results concerning cumulative emissions of tebuconazole, copper, dissolved organic carbon and total nitrogen. The emission rates with time are in comparable ranges for both leaching protocols. Emissions of copper increased with decreasing L/A ratios. Strong correlation of copper concentrations and dissolved organic carbon as well as total nitrogen concentrations in eluates indicates that this observation is caused by co-elution of copper with organic substances. Duration of storage of treated test specimens affected emissions for the investigated wood preservative.
-Conclusions-
Based on these findings, results from both test procedures can be used to describe leaching characteristics and avoid double testing of treated wood to fulfil the requirements of the European regulations for either biocides or construction products. Leaching of substances from treated wood is a complex process that depends on its chemical composition and ageing processes.
Ultrasonic testing of adhesively bonded joints using air-coupled cellular polypropylene transducers
(2014)
In air-coupled ultrasonic testing, the impedance mismatch between the transducer and the air is commonly being solved by adding matching layers to composite transducers. To avoid the difficult technological procedure regarding matching layers, some new piezoelectric materials have been proposed. Most promising are ferroelectrets, which are charged cellular polymers, having ferroelectric and consequently piezoelectric properties. In particular, the extreme softness of cellular polypropylene (cPP) leads to a high piezoelectric constant and to a good impedance match with the air, making matching layers redundant. Its elasticity modulus below 1 MPa causes an additional effect not observed with common piezoelectric materials: that is the electrostrictive effect, here defined as the thickness change due to the attractive force between the transducer electrodes. This effect exceeds the piezoelectric effect at excitation voltages over 1 kV. The extreme softness of cPP leads also to high flexibility, enabling easy focusing by bending the transducer.
We have developed air-coupled ultrasonic transducers based on cPP. This includes the electrical matching networks for the transmitter and for the receiver. The transmitter is excited with voltages up to 2.5 kV, so that the electrostrictive effect dominates, leading to sound pressure around 145dB at the transducer surface. These transducers have been applied for testing carbon-fiber-reinforced polymer plates, adhesive joints and other composite structures. Here we report about ultrasonic transmission of two types of adhesive joints. The first one is multi-layer aluminium components with some artificial disbonds, which are common in aerospace industry, and the second one is an aluminium-steel joint with polyurethane adhesive, which is used in automotive industry.
Pore annihilation was investigated in the single-crystal nickel-base superalloy CMSX-4. HIP tests at 1288 °C/103 MPa were interrupted at different times, then the specimens were investigated by TEM, metallography and density measurements. The kinetics of pore annihilation was determined. The pore closure mechanism was identified as plastic deformation on the octahedral slip systems. A model describing the kinetics of pore closure has been developed on the base of crystal plasticity and large strain theory. Mechanical tests with the superalloy CMSX-4 and the Ru-containing superalloy VGM4 showed, that HIP significantly increases the fatigue life at low temperatures but has no effect on creep strength.
The combination of complementary characterization techniques such as SEM (Scanning Electron Microscopy), T-SEM (Scanning Electron Microscopy in Transmission Mode), EDX (Energy Dispersive X-ray Spectroscopy) and SAM (Scanning Auger Microscopy) has been proven to be a powerful and relatively quick characterization strategy for comprehensive morphological and chemical characterization of individual silica and titania nanoparticles. The selected real life test materials, silica and titania, are listed in the OECD guidance manual as representative examples because they are often used as commercial nanomaterials. Imaging by high resolution SEM and in the transmission mode by T-SEM allows almost simultaneous surface and in-depth inspection of the same particle using the same instrument. EDX and SAM enable the chemical characterization of bulk and surface of individual nanoparticles. The core–shell properties of silica based materials are addressed as well. Titania nominally coated by silane purchased from an industrial source has been found to be inhomogeneous in terms of chemical composition.
The tribological and mechanical properties of niobium carbides (NbC) bonded with cobalt of Fe3Al
(2014)
The tribological and mechanical properties of niobium carbide bonded with 8 vol.-% (NbC-8Co), 12 vol.-% of cobalt (NbC-12Co) or 12 vol.-% of Fe3Al (NbC-12Fe3Al) are presented. Rotating discs made of metal-bonded niobium carbide were mated against alumina (99.7%) under unlubricated (dry) unidirectional sliding tests (0.1 m/s to 12.0 m/s; 22 °C and 400 C) as well as in oscillation tests (f=20 Hz, Δx=0.2 mm, 2/50/98% rel. humidity, n=105/106 cycles). Microstructure and phase compositions were determined as well. The tribological data obtained were benchmarked with different ceramics, cermets, hard metals and thermally sprayed coatings, where NbC bonded with 8% and 12% Co presented above 7 m/s the lowest wear rates so far in such a benchmark. Binderless NbC (HP-NbC1) and the metal-bonded NbCs exhibited low wear rates under dry sliding associated with P·V high load carrying capacities. NbC-based hard metal bonded with 12 vol.-% of Fe3Al resulted in a higher hardness level than for 12 vol.-% cobalt. The tribological profile established revealed a strong position of NbC-bearing materials under tribological considerations and for closed tribosystems against established reference tribo-couples.
Two design approaches for multifunctional information carriers are introduced. In the first one, quick response (QR) code carriers, which were composed of poly(ester urethane) (PEU) and microencapsulated thermochromic pigments (T-PIGs), differing in color and color switching temperature (CST), were prepared. The obtained material systems exhibited machine-readable QR codes at 23 °C and a two-stage decolorization when heated, culminating in unreadable QR codes at temperatures above the highest CST of the employed T-PIGs. In the second scenario, information carriers were sealed with a dark, thermochromic PEU layer. As a result, the QR codes were hidden at 23 °C and became readable upon heating due to color fading. Beyond the characterization of the employed components, preparation methods, functionality analyses and durability investigations are reported. When heated after thermo-mechanical programming, pronounced shape memory properties could be verified. The thermo-responsiveness of such multifunctional material systems may qualify them for usage in anti-counterfeiting applications.
The objective of this study was to investigate the influence of externally applied magnetic fields on the weld quality in laser beam welding. The optimization of the process parameters was performed using the results of computer simulations. Welding tests were performed with up to 20 kW laser beam power. It was shown that the AC magnet with 3 kW power supply allows for a prevention of the gravity drop-out for full penetration welding of 20 mm thick stainless steel plates. For partial penetration welding it was shown that an0.5 T DC magnetic field is enough for a suppression of convective flows in the weld pool. Partial penetration welding tests with 4 kW beam power showed that the application of AC magnetic fields can reduce weld porosity by a factor of 10 compared to the reference joints. The weld surface roughness was improved by 50%.
DNA origami nanostructures allow for the arrangement of different functionalities such as proteins, specific DNA structures, nanoparticles, and various chemical modifications with unprecedented precision. The arranged functional entities can be visualized by atomic force microscopy (AFM) which enables the study of molecular processes at a single-molecular level. Examples comprise the investigation of chemical reactions, electron-induced bond breaking, enzymatic binding and cleavage events, and conformational transitions in DNA. In this paper, we provide an overview of the advances achieved in the field of single-molecule investigations by applying atomic force microscopy to functionalized DNA origami substrates.
The most successful additive manufacturing (AM) technologies are based on the layer-by-layer deposition of a flowable powder. Although considered as the third industrial revolution, one factor still limiting these processes to become completely autonomous is the often necessary build-up of support structures. Besides the prevention of lateral shifts of the part during the deposition of layers, the support assures quality and stability to the built process. The loose powder itself surrounding the built object, or so-called powder-bed, does not provide this sustenance in most existent technology available. Here we present a simple but effective and economical method for stabilizing the powder-bed, preventing distortions in the geometry with no need for support structures. This effect, achieved by applying an air flow through the powder-bed, is enabling an entirely autonomous generation of parts and is a major contribution to all powder-based additive manufacturing technologies. Moreover, it makes powder-based AM independent of gravitational forces, which will facilitate crafting items in space from a variety of powdery materials.
Geführte Ultraschallwellen bieten eine Vielzahl von Einsatzmöglichkeiten in der Zerstörungsfreien Prüfung, der Zustandsüberwachung sowie der Materialcharakterisierung. Insbesondere für Rohrleitungen und ausgedehnte Plattenstrukturen ist eine Vielzahl von auf geführten Wellen basierenden Verfahren in der Entwicklung und teilweise bereits im Einsatz. Aufgrund des komplexen Ausbreitungsverhaltens geführter Wellen werden numerische Verfahren (etwa die Finite Elemente Methode (FEM) oder die Randelementemethode (BEM)) zur Simulation der Wellenausbreitung sowie der Wechselwirkung mit Defekten in Wellenleitern angewendet. Diese Methoden sind für große Strukturen extrem rechenintensiv und umständlich in der Anwendung. Ein ungleich effizienteres Verfahren wurde kürzlich von den Autoren auf Grundlage der Scaled Boundary Finite Element Method entwickelt. Ein semi-analytischer Ansatz erlaubt die Modellierung beliebig ausgedehnter Strukturen bei extrem kurzen Rechenzeiten. Die Wechselwirkung geführter Wellen mit Rissen kann auf besonders elegante und exakte Weise beschrieben werden. Mit dieser Methode können die komplexen Vorgänge in Wellenleitern innerhalb weniger Sekunden modelliert werden.
Fourier-Spektroskopische Untersuchungen von hochmolekularem Polyethylen (HMW-PE) und ultrahochmolekularem Polyethylen (UHMW-PE) im Mittleren - und Fernen Infrarotbereich können Veränderungen der molekularen Strukturen nachweisen, die durch Co60 γ-Strahlung und Rekristallisationsprozesse initiiert werden. UHMW-PE und HMW-PE sind im gewählten IR-Bereich unterscheidbar. Die integrale Absorption der B1u – Gitterschwingungen im Fernen Infrarotbereich (THz-Bereich) ermöglichen die quantitative Beschreibung des Kristallinitätsgrades und dessen Abbau. Die Bildung ungesättigter Vinylengruppen und der Abbau ungesättigter Methylengruppen können im Mittleren Infrarotbereich nachgewiesen werden.
The synthesis of the polymorphic cocrystal caffeine:anthranilic acid was investigated to obtain a better understanding of the processes leading to the formation of different polymorphic forms. In the case of these cocrystal polymorphs synthesized by liquid-assisted grinding a distinct influence of the dipole moment of the solvent was found. A pre-coordination between the solvent molecules and the caffeine:anthranilic acid cocrystal could be identified in the formation of form II. In the case of form II the solvent can be regarded as a catalyst. The formation pathway of each polymorph was evaluated using synchrotron X-ray diffraction.
Bikontinuierliche poröse Keramiken für Filteranwendungen weisen eine komplizierte Mikrostruktur auf, in der Poren und Festkörperphase 'vermischt' sind. Mechanische, thermische sowie Filtereigenschaften können nur präzise bestimmt werden, wenn die Morphologie beider Phasen quantitativ angegeben werden kann. Hier werden unter Anwendung von 3D Computertomographie (CT) und verschiedenen Techniken, die auf der Röntgenrefraktion basieren, die Porosität und die Porenorientierung in keramischen Cordierit-Dieselpartikelfiltern bewertet. Dabei werden zur Auswertung der Tomogramme die Fouriertransformierten sowie eine neu entwickelte richtungssensitive Bildanalyse (DIVA, directional interface variance analysis) angewandt. Sowohl die genannten Messtechniken als auch der statistische Ansatz gestatten die Extraktion optional ortsaufgelöster oder gemittelter Werte. Es ergeben sich sehr gute Übereinstimmungen der experimentell ermittelten Porositätswerte mit Ergebnissen aus Quecksilberintrusionsversuchen als auch der ermittelten Porenorientierung im Vergleich zu publizierten Angaben zur kristallographischen Textur. Dies legt den Schluss nahe, dass die Kenntnis der Grenzflächen (zwischen Poren und Materie) genügt, die morphologischen Eigenschaften solcher Materialien hinreichend zu beschreiben.
The determination of the fatigue life in technical alloys containing large and small defects must rely on a propagation model which accounts for short and long crack growth. Recently an analytical model which incorporates propagation in the short crack regime and plastic correction for the crack driving force has been presented by two of the authors.
This work is intended to show further validation of the model, taking into account data sets for different materials with different testing conditions.
Despite the assumptions about missing parameters, the value of which had to be taken from the literature, the predictions showed a fairly good approximation of the fatigue lives. A possible interpretation of the results in terms of multiple crack initiation and propagation at higher loads is proposed.
A micromechanical model of creep induced grain boundary damage is proposed, which allows for the simulation of creep damage in a polycrystal with the finite element method. Grain boundary cavitation and sliding are considered via a micromechanically motivated cohesive zone model, while the grains creep following the slip system theory. The model has been calibrated with creep test data from pure Cu single crystals and a coarse-grained polycrystalline Cu-Sb alloy. The test data includes porosity measurements and estimates of grain boundary sliding. Finally, the model has been applied to Voronoi models of polycrystalline structures. In particular the influence of grain boundary sliding on the overall creep rate is demonstrated.
Recently, C K-edge Near Edge X-ray Absorption Fine Structure (NEXAFS) spectra of graphite (HOPG) surfaces have been measured for the pristine material, and for HOPG treated with either bromine or krypton plasmas (Lippitz et al., Surf. Sci., 2013, 611, L1). Changes of the NEXAFS spectra characteristic for physical (krypton) and/or chemical/physical modifications of the surface (bromine) upon plasma treatment were observed. Their molecular origin, however, remained elusive. In this work we study by density functional theory, the effects of selected point and line defects as well as chemical modifications on NEXAFS carbon K-edge spectra of single graphene layers. For Br-treated surfaces, also Br 3d X-ray Photoelectron Spectra (XPS) are simulated by a cluster approach, to identify possible chemical modifications. We observe that some of the defects related to plasma treatment lead to characteristic changes of NEXAFS spectra, similar to those in experiment. Theory provides possible microscopic origins for these changes.
Hemocompatible materials are needed for internal and extracorporeal biomedical applications, which should be realizable by reducing protein and thrombocyte adhesion to such materials. Polyethers have been demonstrated to be highly efficient in this respect on smooth surfaces. Here, we investigate the grafting of oligo- and polyglycerols to rough poly(ether imide) membranes as a polymer relevant to biomedical applications and show the reduction of protein and thrombocyte adhesion as well as thrombocyte activation. It could be demonstrated that, by performing surface grafting with oligo- and polyglycerols of relatively high polydispersity (>1.5) and several reactive groups for surface anchoring, full surface shielding can be reached, which leads to reduced protein adsorption of albumin and fibrinogen. In addition, adherent thrombocytes were not activated. This could be clearly shown by immunostaining adherent proteins and analyzing the thrombocyte covered area. The presented work provides an important strategy for the development of application relevant hemocompatible 3D structured materials.
Über die Entwicklung von Anwendungsregeln für reaktive Brandschutzsysteme auf Stahlzuggliedern
(2014)
Der vorliegende Beitrag stellt den Entwicklungsstand von Anwendungsregeln für reaktive Brandschutzsysteme auf Stahlzuggliedern zusammenfassend dar. Dabei wird insbesondere auf die jüngsten Veränderungen in den normativen Grundlagen und bauaufsichtlichen Regelungen eingegangen und im Hinblick auf Sicherheitsaspekte bewertet.
Die Verringerung der Teilsicherheit für den Bauteilwiderstand nicht stabilitätsgefährdeter Bauteile im Regelwerk für die Kaltbemessung von Stahltragwerken ist hier als besonders kritisch anzusehen, da hierdurch ein systematisches Sicherheitsdefizit für den Brandfall verursacht wird.
Weiterhin werden neuste Forschungsergebnisse bei der Entwicklung von Bewertungsregeln von reaktiven Brandschutzsystemen auf Vollkreisprofilen unter Zugbeanspruchung vorgestellt und diskutiert. Die Untersuchungen behandeln die Fragestellung, inwieweit Prüfungen mit Zugbeanspruchungen an Kreisvollprofilen erforderlich sein werden.
Sollten CT Aufnahmen quantitativ und automatisch ausgewertet werden, ist die Qualität der Tomogramme ein wesentlicher Punkt. Außerdem steht bei Serienmessungen nur eine begrenzte Meßzeit für jede Probe. Es werden die verschiedenen Mikrofokusröhren in Bezug auf die Parameter Orts- und Dichteauflösung, sowie Meßzeit verglichen, CT Beispiele dazu gezeigt.
In order to investigate molecular recognition on surfaces, an azide-functionalized monolayer was deposited on gold. The monolayer was characterized by X-ray photoelectron spectroscopy (XPS) and angle-resolved near-edge X-ray absorption fine structure (NEXAFS) experiments and the decomposition of the azide upon irradiation with X-ray beams was investigated. Subsequently, various alkyne-functionalized host and guest molecules were attached to the azide by 1,3-dipolar cycloaddition. These modified surfaces and their host–guest chemistry were analysed by XPS and angle-resolved NEXAFS. The reversibility of guest binding was shown for one example as a proof of principle.
The mechanochemical synthesis of two model compounds, a metal organic framework ([Bi(1,4-bdc)2]*(Im) (bdc = benzene dicarboxylate, Im = imidazole cation)) and a cocrystal (Carbamazepine:Indometacin 1:1) were followed ex situ by combined analytical methods. Powder X-ray diffraction (XRD) and Raman spectroscopy data were evaluated for the synthesis of the metal organic framework. XRD measurements and REM images were analysed for the synthesis of the cocrystal. The measurements revealed that both model compounds were synthesised within minutes. The metal organic framework [Bi(1,4-bdc)2]*(Im) is synthesised via an intermediate structure. The cocrystal Carbamazepine:Indometacin 1:1 is formed within few seconds and afterwards the crystallite size decreases extremely.
Two metal organic structures composed of the ligands benzene-1,4-dicarboxylate and pyridine-2,5-dicarboxylate and bismuth cations are presented: (H2Im)[Bi(1,4-bdc)2] (1) and [Bi(pydc)(NO3)2(H2O)2]*H2O (2) (bdc = benzenedicarboxylate, H2Im = imidazole cation, pydc = pyridinedicarboxylate). Both compounds were synthesised via grinding and the crystal structure of compound (2) was solved based on its powder diffraction pattern. Compound 1 crystallises isostructurally to the dimethyl ammonium containing compound (dma)[(Bi(1,4-bdc)2]. Raman spectroscopy and Extended X-ray absorption fine structure (EXAFS)
measurements provided additional information about the two mechanochemically synthesised metal organic compounds.
The current furfural production yield is low due to the use of non-selective homogeneous catalysts and expensive separation. In this work, partially hydroxylated MgF2 catalysts, synthesized using different water contents, were screened during xylose dehydration in watertoluene at 160 °C. The different Lewis/Brønsted ratios on the MgF2 catalysts showed that under-coordinated Mg can isomerize xylose to xylulose, whilst the surface OH-groups were responsible for the dehydration reactions. The presence of glucose as a co-carbohydrate reduced the furfural selectivity from 86 to 81%, whilst it also led to high 5-hydroxymethylfurfural selectivity. The tests catalyzed by MgF2 in combination with simultaneous N2-stripping showed that a furfural selectivity of 87% could be achieved using low xylose loadings. Moreover, the catalysts regenerated by H2O2 showed high activity during the dehydration tests in watertoluene at 160 °C.
Recent advances in vacuum sciences and applications are reviewed. Novel optical interferometer cavity devices enable pressure measurements with ppm accuracy. The innovative dynamic vacuum standard allows for pressure measurements with temporal resolution of 2 ms. Vacuum issues in the construction of huge ultra-high vacuum devices worldwide are reviewed. Recent advances in surface science and thin films include new phenomena observed in electron transport near solid surfaces as well as novel results on the properties of carbon nanomaterials. Precise techniques for surface and thin-film characterization have been applied in the conservation technology of cultural heritage objects and recent advances in the characterization of biointerfaces are presented. The combination of various vacuum and atmospheric-pressure techniques enables an insight into the complex phenomena of protein and other biomolecule conformations on solid surfaces. Studying these phenomena at solid–liquid interfaces is regarded as the main issue in the development of alternative techniques for drug delivery, tissue engineering and thus the development of innovative techniques for curing cancer and cardiovascular diseases. A review on recent advances in plasma medicine is presented as well as novel hypotheses on cell apoptosis upon treatment with gaseous plasma. Finally, recent advances in plasma nanoscience are illustrated with several examples and a roadmap for future activities is presented.
The vibrational density of states of a series of homologous triphenylene-based discotic liquid crystals HATn (n = 5, 6, 8, 10, 12) depending on the length of the aliphatic side chain is investigated by means of inelastic neutron scattering. All studied materials have a plastic crystalline phase at low temperatures, followed by a hexagonally ordered liquid crystalline phase at higher temperatures and a quasi isotropic phase at the highest temperatures. The X-ray scattering pattern for the plastic crystalline phase of all materials shows a sharp Bragg reflection corresponding to the intercolumnar distance in the lower q-range and a peak at circa 17 nm-1 related to intracolumnar distances between the cores perpendicular to the columns as well as a broad amorphous halo related to the disordered structure of the methylene groups in the side chains in the higher q-range. The intercolumnar distance increases linearly with increasing chain length for the hexagonal columnar ordered liquid crystalline phase. A similar behaviour is assumed for the plastic crystalline phase. Besides n = 8 all materials under study exhibit a Boson peak. With increasing chain length, the frequency of the Boson peak decreases and its intensity increases. This can be explained by a self-organized confinement model. The peaks for n = 10, 12 are much narrower than for n = 5, 6 which might imply the transformation from a rigid system to a softer one with increasing chain length. Moreover the results can also be discussed in the framework of a transition from an uncorrelated to a correlated disorder with increasing n where n = 8 might be speculatively considered as a transitional state.
This paper presents a finite element model of an overhead transmission line using so called cable elements which allow reproducing the cable's nonlinear characteristics accurately employing only a few elements. Aerodynamic damping is considered in the equation of motion by taking into account the relative velocity between the flow of the wind and the moving structure. The wind flow itself is simulated by wave superposition making necessary assumptions on the lateral correlation between the wind velocities along the cable length. As result from the simulation, the following conclusions can be drawn. The first natural frequency of generally used wide spanning cables lies well below 1 Hz where also most of the energy content of the wind excitation is to be expected. Aerodynamic damping is significant for the moving cables holding very low structural damping which leads to a suppression of resonant amplification. This is particularly of interest regarding the support reaction which is dominated by the mean value and the so called background response. The latter is mostly influenced by the randomness of the wind flow, especially lateral to the main wind direction.
A mechanical structure supported by nonlinear springs subjected to an external load is considered. If all mechanical parameters of the system were known, the displacement of the system subjected to this load could be easily calculated. If not all of the parameters are known, but the load and the displacement are measured at one location, an inverse problem exists. In the presented problem the nonlinear springs are unknown and have to be determined. At first glance a problem needs to be solved, which is underdetermined due to the number of unknown variables. However, evolutionary computing can be applied to solve this inverse, nonlinear and multimodal problem. Sometimes a prior knowledge exists on certain system properties, which is difficult to implement into analytical or numerical solver. This knowledge can play a decisive role in identifying the system properties and it can be easily included as boundary condition when applying evolutionary algorithm. This article examines how and under what conditions the spring resistances can be identified. The procedure is exemplified at a mechanical system of a pile foundation.