Filtern
Erscheinungsjahr
- 2011 (345) (entfernen)
Dokumenttyp
- Zeitschriftenartikel (326)
- Beitrag zu einem Tagungsband (19)
Referierte Publikation
- ja (345) (entfernen)
Schlagworte
- Corrosion (9)
- Fluorescence (7)
- Steel (6)
- Flame retardancy (5)
- Hydrogen (5)
- LIBS (5)
- Nanoparticles (5)
- Sewage sludge ash (5)
- Simulation (5)
- Welding (5)
The introduction of carbon nanotubes (CNTs) modifies bulk polymer properties, depending on intrinsic quality, dispersion, alignment, interfacial chemistry and mechanical properties of the nanofiller. These effects can be exploited to enhance the matrices of conventional microscale fibre-reinforced polymer composites, by using primary reinforcing fibres grafted with CNTs. This paper presents a methodology that combines atomic force microscopy, polarised Raman spectroscopy, and nanoindentation techniques, to study the distribution, alignment and orientation of CNTs in the vicinity of epoxy-embedded micrometre-scale silica fibres, as well as, the resulting local mechanical properties of the matrix. Raman maps of key features in the CNT spectra clearly show the CNT distribution and orientation, including a parted morphology associated with long grafted CNTs. The hardness and indentation modulus of the epoxy matrix were improved locally by 28% and 24%, respectively, due to the reinforcing effects of CNTs. Moreover, a slower stress relaxation was observed in the epoxy region containing CNTs, which may be due to restricted molecular mobility of the matrix. The proposed methodology is likely to be relevant to further studies of nanocomposites and hierarchical composites.
The isotopic composition of boron is a well established tool in various areas of Science and industries. Boron isotope compositions are typically reported as 6"B values which indicate the isotopic difference of a sample relative to the internationally accepted isotope reference material NIST SRM 951. A significant drawback of all of the available boron isotope reference materials is that non covers a natural boron isotope composition apart from NIST SRM 951.
The variation of isotope abundance ratios is increasingly used to unravell natural and technical questions. In the past the investigation and interpretation of such variations was the field of a limited number of experts. With new upcoming techniques and research topics in the last decades, such as provenance and authenticity of food, the number of published isotope data strongly increased. The development of inductively coupled plasma mass spectrometers (ICPMS) from an instrument for simple quantitative analysis to highly sophisticated isotope abundance ratio machines influenced this process significantly. While in former times only experts in mass spectrometry were able to produce reproducible isotope data, nowadays many laboratories, never been in touch with mass spectrometry before, produce isotope data with an ICPMS. Especially for such user isotope reference materials (IRM) are indispensible to enable a reliable method validation. The fast development and the broad availability of ICPMS also lead to an expansion of the classical research areas and new elements are under investigation. Here all users require IRM to correct for mass fractionation or mass discrimination or at least to enable isotope data related to a common accepted basis. Despite this growing interest suitable IRM are still lacking for a number of isotope systems such as magnesium.
The wear behaviour of thin steel wires has been analyzed under oscillating sliding conditions in crossed cylinders contact geometry. The focus of this analysis was the influence of the crossing angle between the wires on the wear. The wires used had 0.45 mm in diameter and the material was cold-drawn eutectoid carbon steel (0.8% C) with a tensile strength higher than 2800 MPa. Two different types of tests were carried out, the first one representing the influence of the crossing angle for a constant load and the second one representing the influence of the crossing angle with constant contact pressure. In the first type of tests it was seen that as the contact angle decreases the contact pressure decreases too and hence less energy specific wear resistance is observed. As a consequence less wear is produced, thus increasing the life of the wires. In the second type of tests it was seen that with constant contact pressure but different crossing angles, nearly the same energy specific wear resistance was observed. This points at an identical wear behaviour in both type of tests but with a running-in and a steady state period as two different wear periods. The tests showed that the running in period may play an important role in the overall wear particle generation and hence the wear occurring in the steady state period is rather mild.
Inspired by the globule arc technique a new electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES) method was developed for the analysis of high-purity copper materials. The performance of the method was investigated for the analytes Ag, Al, As, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, S, Sb, Se, Si, Sn, Te, Ti, Zn and Zr. ETV parameters were optimized regarding the release of the analytes, the transport efficiency and the quality of analytical results in terms of precision, trueness and power of detection. The influence of CCl2F2, CHClF2, C2H2F4 and CHF3 as gaseous halogenation modifiers was investigated. A sufficient in situ analyte matrix separation was achieved by using CHF3 as halogenating reagent avoiding a high matrix input from the molten copper sample into the ETV system and the plasma. A complete release from the samples was obtained for all investigated analytes except Se and Te. Acceptable results for the determination of the trace elements Ag, Al, As, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, S, Sb, Si, Sn, Ti, Zn and Zr in high-purity copper were achieved. The method includes a preceding sample preparation step of oxidizing the surface of copper samples which results in a significantly enhanced sensitivity. In addition to the calibration with copper samples, the feasibility of the calibration with liquid multi-element solutions was investigated. Except for Ag, Mg and Ni all analytes could be analyzed using aqueous calibration solutions. The trueness of the method was tested by the determination of analyte contents of certified reference materials. Limits of quantification ranging from 0.6 ng g-1 to 29 ng g-1 were achieved. The developed direct solid sampling method is time and cost effective and well suited for the characterization of high-purity copper materials. The method can be automated to a large extent and is applicable for processes accompanying analyses. In contrast to all other investigated trace elements, Se and Te were not released from the matrix at measurable levels under the used conditions. The determination of these elements is still under investigation and will be reported in a succeeding publication.
Different types of lasers are used nowadays for a number of technological Solutions, Modem high power solid-state lasers with high brightness of Radiation like Fiber or disc lasers find ever more applications in welding technology. Apart from the replacement of the CC>2-iasers traditionaHy used fcr these purposes, they provide new technological possibilities of metal treatment, such as using industrial robots and remote welding with high power laser radiation. The possibility of flexible optical fiber delivery of the radiation to any point gives a great technological advantage and permits welding processes to be realized with complicated weld seam geomelries and different positions using a minimum of additional fixtures. The short wavelength of the high power solid state lasers (1.07 ’m) causes another advantage. The coefflcient of inverse 170
Bremsstrahlung absorption from free electrons in plasma for such radiation is about 100 times lower than for the COi-iaser radiation. Owing to this fact, using the solid state lasers allows it to avoid a negative influence of the welding plume.
However, a short wavelength can lead to another kind of laser Radiation attenuation, which is connected with the formation of a cloud consisting of small metal particles that absorb and scatter laser radiation. This cloud arises due to the condensation of hot metal vapor by flying out from the deep Penetration channel and broadening in relatively cold atmosphere over the metal Surface.
Some theoretical and experimental approaches were made in advance in Order to estimate the influence of the Condensed particles on laser radiation and welding quality.
In this paper a systematic study including the determination of the Cloud size and its dynamical characteristics is presented. The results were obtained within the scope of the first stage of the metal vapor condensation process Investigation during welding with high power fiber lasers.
Coda wave interferometry is a recent analysis method now widely used in seismology. It uses the increased sensitivity of multiply scattered elastic waves with long travel-times for monitoring weak changes in a medium. While its application for structural monitoring has been shown to work under laboratory conditions, the usability on a real structure with known material changes had yet to be proven. This article presents experiments on a concrete bridge during construction. The results show that small velocity perturbations induced by a changing stress state in the structure can be determined even under adverse conditions. Theoretical estimations based on the stress calculations by the structural engineers are in good agreement with the measured velocity variations.
Dealing with first corrosion screening experiments to predict the reliability and safety of Germanys first Carbon Capture and Storage site in the northern Bassin of Germany, northwest of the Capital Berlin, laboratory experiments have been established to simulate the particular conditions at T=60 °C, highly saline aquifer water similar to 'Stuttgart Aquifer', but only at ambient pressure. With mounting 2 independent full 2-grade titanium autoclave systems (running up to 250 bar and 300 °C) pressures up to p=100 bar are possible. In 2010 a specific corrosion chamber of 2-grade titanium working up to 100 °C, flowing aqui fer water with different gas mixtures was designed to fit to a high cycle fatigue testing machine. Long term fatigue experiments simulating fatigue crack growth under corrosive environments will soon start. These experiments may not only help engineering a CCS site, but results can be used to improve the maintenance of geothermal energy production sites, especially moved parts such as pumps and shafts.
The CCS technique involves the compression of emission gasses in deep geological layers. To guarantee the safety of the site, CO2-corrosion of the injection pipe steels has to be given special attention when engineering CCS-sites. To get to know the corrosion behaviour samples of the heat treated steel 1.72252CrMo4, used for casing, and the stainless injection-pipe steel 1.4034 X46Cr13 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CC 2-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. The isothermal corrosion behaviour obtained by mass gain of the steels in the gas phase, the liquid phase and the intermediate phase gives surface corrosion rates around 0.1 to 0.8 mm/year at ambient pressure and much lower about 0.02 to 0.2 mm/year at 100 bar where the CO 2 is in its supercritical state. Severe pit corrosion with pit heights around 4.5 mm are only located on the 42CrMo4 steel. Main phase of the continuous complicated multi-layered carbonate/oxide structure is siderite FeCO 3 in both types of steel.
The main wood degraders in aerobic terrestrial ecosystems belong to the white- and brown-rot fungi, where their biomass can be created on wood decay only. However, total sulfur (S) concentration in wood is very low and only little is known about the different sulfur compounds in wood today. Sulfur-starved brown-rot fungi Gloeophyllum trabeum and Oligoporus placenta were incubated on sterilized pine wood blocks whereas Lentinus cyathiformis and the white-rot fungi Trametes versicolor were incubated on sterilized beech wood blocks. After 19 weeks of incubation, the S oxidation status was analyzed in wood, in degraded wood, and in biomass of wood-degrading fungi by synchrotron based S K-edge XANES, and total S and sulfate were quantified. Total sulfur and sulfate content in pine wood blocks were approximately 50 and 1 µg g-1, respectively, while in beech wood approximately 100 and 20 µg g-1 were found, respectively. Sulfur in beech was dominated by sulfate-esters. In contrast, pine wood also contained larger amounts of reduced S. Three out of four selected fungi caused a reduction of the S oxidation state in wood from oxidized S (sulfate-ester, sulfate) to intermediate S (sulfonate, sulfoxide) or reduced S (thiols, e.g., proteins, peptides, enzyme cofactors). Only O. placenta shifted thiol to sulfonate. Growth experiments of these fungi on selective minimal media showed that in particular cysteine (thiol), sulfonates, and sulfate enhanced total mycelium growth. Consequently, wood-degrading fungi were able to utilize a large variety of different wood S sources for growth but preferentially transformed in vivo sulfate-esters and thiol into biomass structures.
The presently active standards on Computed Radiography (CR) need a major revision. It was observed by many users that the image quality for class B of EN 14784-2 is not achievable under the same exposure conditions as used for film exposure. A mathematical model was developed and tested, which allows the calculation of the image quality, proven by image quality indicators (IQI), depending on the fixed pattern noise and the efficiency of the used imaging plate (IP) scanner system. All tested IP scanner systems provide a fixed correlation between the measured signal/noise ratio (SNR) and the grey values in the digital images. The maximum achievable SNRmax depends on the fixed pattern noise of the plate (high dose limit). Depending on the exposure dose an optimum visibility of IQIs can be predicted by calculation and measured considering the attenuation coefficient for calculation of the contrast/noise ratio (CNR). The diameter of the just visible wire is proportional to 1/sqrt(CNR). The optimum tube voltage for best visibility of IQIs and maximum CNR depend on the exposure dose. The optimum tube voltage for best visibility is achieved only at exposures with high dose. A dose dependant optimal tube voltage was not observed for film radiography.
Instrumented measurements on radioactive waste disposal containers during experimental drop testing
(2011)
In context with disposal container safety assessment of containers for radioactive waste the German Federal Institute for Materials Research and Testing (BAM) performed numerous drop tests in the last years. The tests were accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers. The instrumentation of a specimen is an important tool to evaluate its mechanical behavior during impact. Test results as deceleration-time and strain-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of calculations based on finite-element methods. Strain gauges are useful to determine the time dependent magnitude of any deformation and the associated stresses. Accelerometers are widely used for the measuring of motion i.e. speed or the displacement of the rigid cask body, vibration and shock events. In addition high-speed video technique can be used to visualize and analyze the kinematical impact scenario by motion analysis. The paper describes some selected aspects on instrumented measurements and motion analysis in context with low level radioactive waste (LLW) container drop testing
CCQM (Consultative Committee for Amount of Substance - Metrology in Chemistry) is an international body of the Meter Convention (BIPM) established as a framework of National Metrology Institutes running inter-laboratory of comparisons to demonstrate the international comparability of chemical measurements, with traceability to international or national reference standards. In 2003 the surface analysis working group (SAWG) was established at CCQM and since then several inter-laboratory comparisons in the field of EPMA have been carried out. In many cases the EPMA results deviated significantly from each other and the expanded uncertainties were greater than expected. Both methods EDS and WDS were employed. However, light elements such as carbon and nitrogen were the major elements analyzed and it is known that the corresponding lowenergy characteristic X-ray lines are more challenging to quantify by EPMA than the higher energy lines of elements with higher atomic numbers. Moreover, the standards selected and their qualities were variable, the quantification models were different, and the acquisition parameters were not specified sufficiently in the analysis instructions.
It is a latent wish of any SEM/EDS (scanning electron microscope with an energy dispersive spectrometer) analyst to “see more” of the analyzed specimen, i.e. to improve the existing analytical figures of merit.
One key issue are the relatively poor limits of detection (not below 0.1 mass-%) provided by energy dispersive X-ray spectrometry (EDX) with the conventional electron excitation (ED-EPMA). This is a consequence of relatively low peak-to-background ratios and reduced energy resolution when compared to wavelength dispersive spectrometry (WD-EPMA). Recent technological developments make possible to equip the SEM with a wavelength dispersive spectrometer (WDS), so that
significantly better energy resolution can be attained. Also a relative new product that can be easily attached to a SEM/EDS system is a micro-focus X-ray source. Hence, it is possible to perform (micro-focus) X-ray fluorescence spectrometry (μ-XRF) and take advantage of the enhanced peak-to-background ratios (well suited for trace analysis). However, there are also some disadvantages: an increased measurement time and excitation with a high current in the 10s of nA range are usually required for WDS. μ-XRF provides more bulk information and poor limits of detection for light elements. By combining the advantages of these analytical techniques “seeing more” becomes possible.
Simple procedures for specifying and checking the performance of energy dispersive X-ray spectrometers (EDS) have been since 2002 available in form of the international standard ISO 15632:2002 [1]. When specifying their spectrometers all major EDS manufacturers refer meanwhile to this standard. Main spectrometer parameters such as energy resolution can be determined as recommended in there. Just several years ago the Si-Li detector has been the mostly widespread type of detector. Since four-five years, silicon drift detector (SDD) EDS providing comparable (in many cases even better) energy resolutions at much higher count rates than the conventional Si-Li’s have got the breakthrough on the market.
The extremely low acoustic impedance of polypropylene ferroelectret combined with its piezoelectric properties makes this material suitable for construction of aircoupled ultrasonic transducers for non-destructive testing. For the fabrication of transducers with a stable quality, the reproducibility of their key parameters is of interest.
The reproducibility was evaluated by means of (i) impedance spectroscopy and (ii) pulse-echo measurements. (i) Impedance spectroscopy was applied to identify the resonance frequency, the coupling factor and the acoustic impedance of several nominally identical transducers. (ii) Pulse-echo measurements yielded the signal form of these transducers.
The variation of the signal amplitude measured with pulseecho technique was about 10 dB. A part of this variation Comes from the deposition of transducer electrodes and another part from local variations of ferroelectret properties. The variation of the signal amplitude was caused by the observed variation of the coupling factor, which was also about 10 dB. The variation of the acoustic impedance was only about 1 dB, thus having no effect on the variation of the signal amplitude.
These results indicate that the variability can be reduced by improving the control of electrode deposition and by optimizing the production technology affecting the reproducibility of material properties.
This paper studies the dielectric dispersion of high frequency radar wave in concrete in early-aged and hardened concrete specimens. Frequency-dependent spectra of phase velocity ν(ω) were measured to deduce the spectra of real part of dielectric permittivity ε'(ω). The dispersion was measured by three high nominal ground penetrating radar frequencies (1.5, 1.6 and 2.6 GHz), experimenting on two steel bars with concrete cover 50 and 100 mm. It was found that ν(ω) and ε'(ω) dispersed at lower frequency, but became stable at high frequency regions, which agrees with the classical GPR plateau. The same frequency components at different nominal antenna frequencies show a close range of ν(ω) and ε'(ω) in concrete of different ages. The results in this paper warrant further investigation of using GPR wave to study material properties.
Using ground penetrating radar and time-frequency analysis to characterize construction materials
(2011)
For decades, applications of nondestructive evaluation-civil engineering (NDE-CE) focus on object identifications (such as steel bars, tendon ducts and backwall reflections) in infrastructures. Because of the advantage of efficient visualization of internal structure, utilization of these methods can probably be extended to material characterization (MC) of aging and adversely exposed infrastructures. However, two factors yield a big gap between NDE and MC. First, for the ease of visualization, the primary focus of NDE-signal processing is object identification, which usually alters the originality of the signal. Second, there is lack of relationship and inverse models bridging the NDE-derived and conventional material properties compared to other disciplines of science, such as geophysics. These disadvantages make laboratory and field-scale NDE-MC still a far-reaching holy grail and is possibly the greatest hurdle to be regularly adopted in CE structures. This paper attempts to address this gap from object identification to MC using ground penetrating radar (GPR) as one of the most frequently used NDE-CE methods, and signal processing with joint timefrequency domain (JTFA) analysis. Three examples of material property characterization regarding the individual effects of steel bar corrosion in concrete, hydration and moisture content distribution of construction materials are given.
This study reports three new crystalline aluminum isopropoxide oxide fluorides with molar ratios of Al:F equal to 1:1 and 1:1.25. These are the first three representatives isolated without the incorporation of external donor molecules. Compound 1 Al4F4(µ4-O)(µ-O'Pr)5[H(O'Pr)2] contains a tetranuclear unit consisting of two different five fold coordinated AlFO4-units, with F exclusively in the terminal position. Compound 2, Al4F4(µ4-O)(µ-O'Pr)5[H(O'Pr)2]·Al5F5(µ5-O)(µ-O'Pr)8, contains both a tetranuclear unit (as in 1) and a pentanuclear Al-unit. Al-atoms in the latter are five- and six fold coordinated. Compound 3, Al16F20(µ4-O)4(µ-O'Pr)20·2('PrOH), exhibits a slightly higher fluorination degree and contains an oligomeric chain of four F-linked tetranuclear Al-units. In addition to X-ray structure analysis, compound 1 was characterized by different solid state MAS NMR techniques, including 27Al triple quantum MAS NMR and 1H, 1H→13C CP, 19F and 27Al MAS NMR. On the basis of the collected data, a reliable decomposition of 27Al single pulse MAS NMR spectra and an unambiguous assignment of the resonances to the respective structural AlFO4-units are given. The new crystalline aluminum isopropoxide oxide fluorides are direct evidence of the fluorolytic sol–gel mechanism previously discussed.