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Paper des Monats
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We synthesized and characterized a set of ultrasmall hexagonal-phase NaGdF4: 20% Yb3+, 2% Er3+ upconversion nanoparticles with core diameters of 3.7 ± 0.5 nm. In order to assess passivation effects and the influence of possible core−shell intermixing and to identify optimum particle structures for combined imaging in the visible and near-infrared (vis−NIR: 410−850 nm) and short-wave infrared (SWIR: 1520 nm), NaYF4 shells of varying thicknesses (monolayer to 10 nm) were introduced and the influence of this parameter on the upconversion and downshifting photoluminescence of these particles was studied at different excitation power densities. This included excitation power-dependent emission spectra, slope factors, quantum yields, and excited state decay kinetics. These measurements revealed enhancement factors of the upconversion quantum yield of >10 000 in the low power region and an excitation power density-independent quantum yield of the downshifted emission at 1520 nm between 0.1 and 14%. The optimized shell thickness for combined vis and SWIR imaging was identified as 5 nm. Moreover, lifetimes and quantum yields can be continuously tuned by shell thickness which can be exploited for lifetime multiplexing and encoding. The fact that we did not observe a saturation of the upconversion quantum yield or the excited state decay kinetics with increasing shell thickness is ascribed to a strong intermixing of the active core with the inert shell during the shelling procedure. This indicates the potential of spectroscopic tools to detect cation intermixing.
Systematic errors in the evaluation of uncorrected data from thermographic lock-in measurements
(2018)
Lock-in thermography (LT) is based on the correct evaluation of phase differences between the temperature oscillations at different surface regions of the object under test during periodic heating. Since the usual heating procedures contain a DC component, the actual heating pattern achieved is not harmonic. This causes systematic deviations when phase differences are determined by means of harmonic analysis, e.g. with FFT analysis. The resulting errors depend clearly on the ratio between DC and AC amplitude, which is demonstrated at simulated and experimentally recorded temperature transients. Further experimental LT data obtained by different oscillating energy inputs showed a variety of possible shapes of transients with different DC components.
In order to test their suitability different non-destructive methods were performed to inspect a GFRP plate with artificial defects. These defects were manufactured by means of thin PTFE sheets inserted between two plies in three different depth. The inspection methods were microwave reflection, flash thermography and phased array ultrasonics, all applied to the same specimen. Selected results are shown for all methods demonstrating opportunities and limits of the particular inspection methods. The achieved detection limits and further application aspects are compared directly to provide a useful information for the planning of inspection tasks.
Foundations
(2018)
IAPR participates in the EMPIR 16SRT02, entitled ‘Certified forensic alcohol reference materials - ALCOREF’ funded by EURAMET as an external funded partner. The Research in this project will address the needs for better enforcement of drink-driving legislation in several European countries, by building up long-term capacities for the production and certification of forensic alcohol reference materials, suitable for the calibration of evidential breath alcohol analyzers. The certification procedure includes characterization of the materials, assessment of homogeneity, stability, and uncertainty estimation. An interlaboratory comparison will be conducted to test the materials and capabilities developed. EMPIR 16SRT02-ALCOREF project is coordinated by BAM (DE).
Monitoring of the absolute water content in porous materials based on embedded humidity sensors
(2018)
Moisture transport monitoring may indicate the onset of deterioration in porous building materials Prior to damage occurring. Most moisture measurement systems provide only qualitative values, require extensive calibration, or are destructive. Thus, non-destructive and calibration-free monitoring Systems are required. Our approach of moisture monitoring is to embed sensors that measure the relative humidity.
In our experiment, screed samples are monitored during the Hydration and evaporation process. Every test sample is equipped with 10 embedded sensors which measure the relative humidity across the sample thickness. Based on Hillerborg’s approach, the relative humidity is converted into the corresponding pore saturation. In our study, the free water is computed without knowledge of the Sorption isotherm. The free water in the pore system is predicted and validated. The predicted weight decrease corresponds conclusively to gravimetrically measured weights. The embedded sensors yield the absolute liquid water content and enable an experimental, non-destructive monitoring of liquid water in porous materials.
An improved algorithm for calibration-free laser induced breakdown spectroscopy (CF LIBS) is presented which includes several novel features in comparison with previously proposed similar algorithms. In particular, it allows using spectral lines with arbitrary optical thickness for the construction of Saha-Boltzmann plots, retrieves the absorption path length (plasma diameter) directly from a spectrum, replaces the Lorentzian line profile function by the Voigt function, and allows for self-absorption correction using pre-calculated and tabulated data rather than approximating functions. The tabulated data embody the solutions of the radiative transfer equation for numerous combinations of optical thicknesses and line widths. The algorithm is thoroughly verified with synthetic spectra.
Laser-induced plasmas are widely used in many areas of science and technology; examples include spectrochemical analysis, thin film deposition, material processing, and even jet propulsion. Several topics will be addressed. First, general phenomenology of laser-induced plasmas will be discussed. Then, a chemical model will be presented based on a coupled solution of Navier-Stokes, state, radiative transfer, material transport, and chemical (Guldberg-Waage) equations. Results of computer simulations for several chemical systems will be shown and compared to experimental observations obtained by optical imaging, spectroscopy, and tomography. The latter diagnostic tools will also be briefly discussed. Finally, a prospective application of laser-induced plasma and plasma modeling will be illustrated on the example of calibration-free MC LIBS (Monte Carlo Laser Induced Breakdown Spectroscopy), in which concentrations of elements in materials are found by fitting model-generated and experimental spectra.
Moisture testing and mapping
(2018)
Selected resonance states of the deuterated formyl radical in the electronic ground state X^2A´ are computed using our recently introduced dynamically pruned discrete variable representation [H. R. Larsson, B. Hartke, and D. J. Tannor, J. Chem. Phys. 145, 204108 (2016)]. Their decay and asymptotic distributions are analyzed and, for selected resonances, compared to experimental results obtained by a combination of stimulated emission pumping and velocity-map Imaging of the product D atoms.
The theoretical results show good agreement with the experimental kinetic energy distributions. The intramolecular vibrational energy redistribution is analyzed and compared with previous results from an effective polyad Hamiltonian. Specifically, we analyzed the part of the wavefunction that remains in the interaction region during the decay. The results from the polyad Hamiltonian could mainly be confirmed. The C=O stretch quantum number is typically conserved, while the D-C=O bend quantum number decreases. Differences are due to strong anharmonic coupling such that all resonances have major contributions from several zero-order states. For some of the resonances, the coupling is so strong that no further zero-order states appear during the dynamics in the interaction region, even after propagating for 300 ps.
Accuracy of calibration-free (CF) methods in laser-induced breakdown spectroscopy (LIBS) depends on experimental conditions and instrumental parameters that must match a CF LIBS model. Here, the numerical study is performed to investigate effects of various factors, such as the optical density, plasma uniformity, line overlap, noise, spectral resolution, electron density and path length on the results of CF-LIBS analyses. The effects are examined one-by-one using synthetic spectra of steel slag samples that fully comply with the mathematical model of the method. Also, the algorithm includes several new features in comparison with previously proposed CF algorithms. In particular, it removes limits on the optical thickness of spectral lines that are used for the construction of the Saha-Boltzmann plot; it retrieves the absorption path length (Plasma diameter) directly from spectral lines; it uses the more realistic Voigt line profile function instead of the Lorentzian function; and it employs the pre-calculated and tabulated thin-to-thick line ratios instead of approximating functions for selfabsorption correction.
Minimally invasive injection of calcium phosphate cement into bone defects in aged sheep vertebrae has been used as a model for the treatment of osteoporotic vertebral fractures. One of the therapeutic criteria is a compression test of non-treated or treated vertebral bodies. In the present study, an in situ compression test with a stepwise load increase was performed with small spongiosa cylinders from the vertebrae under continuous monitoring by μCT. This allows localization of bone cracks and the visualization of correct placement and form of the bone cylinder. In addition, the effects of an uneven load distribution on the sample due to an irregular shape and a subsequent underperformance of the test sample can be excluded by controlling its shape under increasing load. There was a good agreement between the measured data and those obtained by simulated load-dependent transformation on the basis of a digital volume correlation between consecutive compression tests on the bone surface under the assumption of homogeneous bone material. Mechanic simulation was executed by directly using structural voxel data, resulting in maps of Von Mise stresses and predicted displacements.
Statistic process control as well as process capability demand for calibrated determination of layer thicknesses in various industries, e.g. automotive, aerospace, microelectronics manufacturing. Calibration requires well know and well characterized samples. A calibration laboratory accredited according to DIN EN ISO 17025 has the objective to distribute standards traceable to SI units to industrial laboratories for quality control of manufacturing of various products. Especially, the thickness determination of thin metallic coatings e.g. from galvanic processes or layer deposition using X-Ray Fluorescence can be significantly improved by customized calibration samples. This is essential as the measurement uncertainty directly correlates to the capability performing reliable control of processes with high yield. For calibration laboratories, the validation of results using round robins and the direct comparison to national metrology institutes is a prerequisite to demonstrate the competence to perform calibration services.
In this paper a strategy to obtain traceability and validation for thin alloy layers as well as first results are presented. The combined use of the accredited method for determination of mass per area from measurement of mass and area combined with standard free X-Ray Fluorescence as well as chemical analysis of dissolved samples with thin layers is deployed for material systems as NixZn1-x as well as NixP1-x. The obtained results are compared to reference free X-Ray Fluorescence at the BESSY II laboratories of Physikalisch-Technische Bundesanstalt. An excellent agreement of the obtained measured values as mass per unit area and alloy concentrations from the different applied methods within the measurement uncertainty was observed for NixP1-x showing the successful performed traceability of the calibration samples to SI units in combination with a validation of results by national metrology institutes and the round robin approach.
Due to the increasing consumption of cereals worldwide, monitoring of growth, storage and processing is becoming more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sampling and procedures for mycotoxin analysis are complex and contain invasive and cost intensive steps.
A possible approach to avoid sampling inaccuracies is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with more than 180 compounds. Due to its non-functionalized sesquiterpene structure, quantification of trichodiene using Headspace GC-MS methods is possible (e.g. [1]). Thereby, it could be used as biomarker for trichothecene contamination in foodstuff.
However, further studies are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the trichothecene content in samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals.
Air-coupled ultrasonic testing (ACUT) has experienced rapid growth within the last years. It is especially well suited to inspection of lightweight structures consisting of composite materials and adhesive joints. Uniform coupling and easy maintenance are its advantages compared to contact technique. However, the impedance mismatch between the transducer and air poses a major challenge to the development of ACUT transducers. Commercially available air-coupled transducers consist of a piezocomposite material and matching layers. Their fabrication is difficult in handling and their signal-to-noise ratio sometimes not sufficient for various testing requirements. However, there are several innovative approaches using other materials and other physical principles to transmit and receive an ultrasonic pulse. We present a review of the latest advances in research on air-coupled transducers for non-destructive testing, including previously unpublished results. We recognize two major directions as most promising: ferroelectrets and thermoacoustic transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties. Their small acoustic impedance is matched to air better than matching layers applied in conventional air-coupled transducers. Applying bias voltage to a ferroelectret receiver is the latest development in this field, which increased the received signal by 12 to 15 dB. Thermoacoustic transducers use heat to initiate an ultrasonic wave, acting as transmitters. The working principle is known from nature as thunder and lightning: thermal energy of an electrically heated material, which can also be air, is converted into acoustic energy. Some thermoacoustic transmitters consist of a conductive layer with a thickness in the nanometer range deposited on a solid substrate. Another possibility is to use an electric spark. For the first time, measurements of the sound field of an electric spark up to 500 kHz were performed. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing.
Composite pressure vessels consist of an internal liner (Steel, aluminum, or plastic) which stores the liquid or gas and CFRP (carbon fiber reinforced plastics) which serves as pressure resistance. These vessels comprise some advantages compared with conventional vessels made of steel or aluminum and their application grew strongly over the last decade. The reason for this trend is the tremendous weight saving.
However, the long-time behavior for filling and discharging cycles and the creep strength of composite vessels is not fully understood. Therefore, BAM started an internal project to investigate degradation of these material systems. Normally, high-frequency eddy current testing (HF-ET, f > 10 MHz) is deployed for CFRP due to the low conductivity of the fibers, which is in the order of 0.01 MS/s, and the capacitive coupling between them. Nevertheless, in some cases conventional ET can be applied.
Some first results using conventional ET for detecting leakages in the internal liners are already presented. This contribution gives an update of our investigation using both conventional and high-frequency ET. Therefore, we developed an ET equipment based on a vector network analyzer using frequencies between 300 kHz and 2 GHz. The focus concerns the study of the aging effects.
Alternariol (AOH) and Alternariol monomethylether (AME) are two secondary metabolites of Alternaria fungi which can be found in various foodstuffs like tomatoes, nuts and grains. Due to their toxicity and potential mutagenic activity the need for the development of high-throughput methods for the supervision of AOH- and AME-levels is of increasing interest. As the availability of both native and labelled AOH and AME analytical standards is very limited we herein wish to present a novel concise approach towards their synthesis employing a ruthenium-catalyzed ortho-arylation4 as the key step.
Singlet oxygen generation potential of two novel free-base-porphyrin photocatalysts was investigated. The freebase-porphyrin-sensitized Fe3O4 magnetic nanoparticles (MNPs) were tested for the degradation of the model pollutant Bisphenol A (BPA) in aqueous solution, for the first time. MNPs with either cubic or spherical shape were synthesized using the sonochemical approach, followed by sensitizing with photoactive 4,4′,4′′,4′′′- (Porphine-5,10,15,20-tetrayl)tetrakis(benzoic acid) (TCPP). The resulted photocatalysts were characterized in detail by scanning and transmission electron microscopy, Brunauer–Emmett–Teller analysis, spectral techniques and vibrating sample magnetometry. The electron spin resonance experiments have confirmed the high activity of the photocatalysts through the efficient formation of singlet oxygen in solution. The optimum operational parameters for BPA degradation were established as follows: 1.0 μmol L−1 BPA, 1.0 g L−1 of photocatalyst, 100 μmol L−1 H2O2, under UVA irradiation. In these conditions, the results for both photocatalysts revealed that after only 10 min of reaction, over 64% and ca. 90% of BPA have been removed from solution in the absence and presence of H2O2, respectively. Whereas after 60 minutes of treatment, only 24% of BPA in real wastewater effluent samples were removed under UVA irradiation in the absence of H2O2, showing the high complexity of real wastewater. Moreover, both photocatalysts were successfully used for BPA removal in three consecutive runs, without significant loss of catalytic features.
The Scaled Boundary Finite Element Method (SBFEM) for prismatic structures is an efficient method for the simulation of acoustic behavior. Hence a further development of the method is of great interest. The wave propagation can be calculated for isotropic and anisotropic materials in solids. As for many applications the acoustic behavior in fluids and the behavior in case of fluid-structure interaction (FSI) is subject of research, the implementation of a fluid model in SBFEM for prismatic structures is needed. In case of FSI the coupling between fluid and solid domains can be performed without additional effort when describing both domains in the same variables. Hence a displacement-based fluid description is used. As the discretized formulation leads to spurious modes, a penalty method to suppress the unphysical behavior is chosen. To validate the derived model a comparison with analytical solutions of purely fluid domains is made. As to verify that in case of FSI the model shows the right behavior, dispersion curves of water-filled pipes are calculated and compared to results obtained with Comsol.