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Eingeladener Vortrag
- nein (1)
27Al nuclear magnetic resonance spectra of polycrystalline aluminium borate 9Al2O3 · 2B2O3 have been measured in double rotation at 11.7 and 7.0 T and high-speed magic-angle spinning at 7.0, 9.4, 11.7, 14.1 and 17.6 T. Spinning sidebands from the satellite transitions were observed at 7.0 and 14.1 T. Each of the four structural aluminium sites [Al(IV), Al(V)(1), Al(V)(2) and Al(VI)] are observed, characterised and assigned in the spectra. The obtained parameter set gives a fully consistent interpretation in agreement with the crystal structure of the compound.
The applicability of excimer laser at 308 nm and Nd:YAG laser at 532 nm with fluences below 0.86 J/cm2 for cleaning of cellulose and paper materials was evaluated. The extent of degradation of purified cotton cellulose and Fabriano paper after laser treatment as well as after a period of accelerated humid oven ageing was determined by following the changes in the degree of polymerization. While irradiation of paper with the excimer laser at 308 nm results in depolymerization of cellulose accompanied by a decrease in ISO brightness, no detrimental effects of Nd:YAG laser treatments were observed.
We propose a model to describe the sintering kinetics of polydispersed glass particles, having no adjustable parameter. The model is based on three sintering stages: a pure Frenkel' (F) first step, a mixed Frenkel/MackenzieShuttleworth' stage, and a third, pure MackenzieShuttleworth' (MS) step. The model considers sample shrinkage as the sum of the partial shrinkage of several clusters, each consisting of equally sized particles and each showing independent F or MS behavior. The overall set of clusters mimics the specimen's real particle size distribution. We then introduce the concept of neck forming ability, which allows the formation of necks among particles of different sizes, relaxing the clustering condition. Using experimental physical parameters: particle size distribution, viscosity, surface energy, and the theoretical neck forming ability, the model describes well the sintering kinetics of an alumino-borosilicate glass powder having polydispersed, irregular shaped particles in a variety of temperatures. The sintering kinetics of the real powder is slower, but not far from the calculated kinetics of a monodispersed distribution containing only particles of average size. Thus the model provides a tool for estimating the sintering kinetics of real glass powders, for any size distribution and temperature, thus minimizing the number of laboratory experiments.
The reliability investigations are dedicated to throw light on the performance of the NDE system with respect to the required aim. This is especially of interest when it is looked for life damaging objects in the case of mine seeking and when it is even more difficult to distinguish between the different suppliers of methods concerning their actual capability.
In accordance with the conception of EFNDT WG5 and CEN BT 126 CW 07 the authors have the aim to transfer the knowledge in reliability measurement of NDE systems to the reliability measurement of mine detection systems. For this the three basic ways to investigate the reliability of NDE signals will be described. The first way of investigation, the performance demonstration, is preferred e.g. in the US American nuclear power industry. This is an integral consideration of the non destructive test as a system where the whole NDE system is packed in a black box and only the input in terms of the real existing flaws in the component is considered and compared to the output in terms of the indications of the human inspector or of the automated system. The second - the European tradition relies on a standardized description of physical/technical parameters of the NDE system which are preconditions for successful system performance. The third approach - the modular conception - is a marriage of both: The signal chain is cut into main modules.
Each module is assessed in a most appropriate individual way e.g. via modeling calculations. The single results are joint together according to the reliability theory of systems where the reliability of the total system is composed of the reliability of the subsystems. Separating criteria for the system were proposed through a reliability formula developed during a series of European-American workshops on NDE reliability. A further essential parameter especially for demining systems are the repeatability and reproducibility. Their affect on the reliability and its scatter will be investigated. Examples for the ROC/POD approach in terms of the investigation of the reliability of ultrasonic manual testing and for first attempts for the reliability investigation of demining data will be presented.
It will be strongly recommended to apply the ROC/POD and Modular Conceptions to the assessment and optimization of mine seeking systems.
Proposals for Performance Demonstration and Modular Reliability Assessment for Humanitarian Demining
(2003)
For safe and reliable demining it is necessary to determine the actual true performance of mine searching equipment in detecting mines. The subject to detect a hidden subject by penetrating physical interaction with the target is similar to that of non-destructive testing where it is looked for hidden cracks etc. in material via waves and rays. The non destructive testing profession is now about 100 years old and developed some procedures to check reliability of testing. Those principles like the performance demonstration where the successful detections are statistically evaluated against false calls rates and their implementation in an industrial standard (ASME section XI appendix VIII) are analysed. A first adoption to demining was accomplished in the prescription for blind trials in the CEN workshop agreement CEN BT 126
CWA07 for test and evaluation of metal detectors. A number of blind trials were accomplished within an ITEP project to learn about the necessary statistical layout of those trials to achieve true, reproducible and repeatable results to give guidance to selection and improvement of metal detectors. The special focus in these investigations was on the influence of the human factor due to the degree of experience of the operators and the infulence of uncooperative soil. The correlation of the results of the physical parameter measurement and the statistical results is analysed in a first attempt.
Because the demining process is always connected with a danger for human beings, it is necessary to make sure the proper functioning of mine searching equipment in detecting mines. Detecting a hidden target by penetrating physical interaction of rays or waves is similar to non-destructive testing. The non-destructive testing profession developed procedures to check the reliability of testing. These procedures, like the performance demonstration where the successful detections are statistically evaluated against false call rates and their implementation in an industrial standard (ASME section XI appendix VIII) are used as a template. A first adoption to demining was accomplished in the prescription for blind trials in the CEN workshop agreement CWA 14747: 2003 for test and evaluation of metal detectors. Within an ITEP project a number of blind trials were carried out to learn about the necessary statistical basis of those trials to achieve true, reproducible and repeatable results to give guidance for the selection and improvement of metal detectors. The special focus in this first investigation was on the influence of the human factor due to the different degree of experience of the operators and the influence of the soil.
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
Micro-computed tomography (µCT) provides quantitative three-dimensional information of bone around titanium implants similar to classical histology. The study, based on an animal model, using cuboid-shaped biofunctionalised Ti6Al4V implants with surrounding bone after 4 weeks, is performed using 3 µCT-systems with X-ray tubes, one synchrotron-radiation-based µCT-system (SRµCT), and classical histology. Although the spatial resolution of the µCTsystems is comparable, only the results of SRµCT agree with results of classical histology. The X-ray tube sources give rise to huge artefacts in the tomograms (interface scattering, beam hardening), which impaired the quantitative analysis of bone up to about 200 µm from the implant surface. Due to the non-destructive character of µCT the specimens can be subsequently examined by classical histology
without restriction. The quantitative comparison of bone formation uncovers the strong dependence of the detected amount of newly formed bone from the selected slice. This
implies the necessity of 3D analysis. SRµCT and classical histology prove that surface modifications of the titanium implant significantly influence the bone formation. Using SRµCT, the preparation artefacts due to cutting and polishing are excluded.