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Eingeladener Vortrag
- nein (250)
XTEM and TFXRD investigations of ohmic Ti/Al/Ti/Au/WSiN contacts on AlGaN/GaN HFET layer systems
(2002)
The microstructural features of the high-temperature-stable ohmic contact system Ti/Al/Ti/Au/WSiN on AlGaN/GaN were investigated using analytical transmission electron microscopy and thin film x-ray diffraction. For two typical rapid thermal annealing steps at 750 °C (non-ohmic behaviour) and 850 °C (ohmic behaviour) the intermetallic phases at the metal-semiconductor interface are presented. Increased annealing leads to the transformation of an Al2Au-AlAuTi phase mixture to a mixture of Al2Au-Al3Au8 phases and the formation of Ti-Al-nitride layers at the interfaces. In light of these results the electrical contact properties are discussed.
An attempt was undertaken to obtain a better understanding of the tribological properties of two wear-resistant coatings on tool steel by structural and microchemical analysis of wear particles using a transmission electron microscope. Coatings were deposited by physical vapor deposition and plasma-assisted chemical vapor deposition techniques and tribological properties were derived from reciprocating sliding tests of the coatings against alumina balls. Three types of wear particles were identified by electron diffraction and energy dispersive X-ray spectroscopy: nanocrystalline rutile (TiO2), nanocrystalline graphite and microcrystalline graphite. Low coefficients of friction, of the order of 0.2, were attributed to the formation of solid lubricant films of sub-stoichiometric TiO2-x Magnéli phases and/or graphite.
The focused ion beam technique - eine interessante Alternative, auch für konventionelle Werkstoffe
(2002)
The preparation and structural investigation of 17O-enriched xNa2O(100-x)P2O5 glasses (46.5<=x<=62.8) by nuclear magnetic resonance (NMR) is described. Enriched phosphoric acid was prepared by hydrolysis of PCl5 with 17O-enriched water and neutralized with sodium carbonate. The sodium metaphosphate was then melted at 800 °C for 15 h and quenched. Polyphosphate and ultraphosphate glass compositions were prepared by remelting the metaphosphate with sodium carbonate and phosphorus pentoxide, respectively. 31P magic angle sample spinning (MAS) NMR was used to determine the Na2O/P2O5 content in the glasses. 17O NMR spectra (quadrupole echo for non-rotating samples and multiple-quantum excitation for rotating samples (MQMAS)) show two oxygen sites in the samples with large quadrupolar coupling constants (4.7 and 7.7 MHz), in accordance with the high phosphorus electronegativity. According to the correlation of 17O quadrupolar constants with bond ionicity, these two components are attributed to bridging POP and non-bridging PO...Na oxygens. The average POP bond angle is estimated with the quadrupolar asymmetry derived from the fit of the static echo spectra. The MQMAS spectrum shows a distribution of non-bridging oxygen chemical shifts, attributed to a variation of bond length and angle.
Zeta potential as measured with the electrokinetic sonic amplitude (ESA) method has been compared to streaming potential as measured with the particle charge detection (PCD) method. The measurements have been carried out on identical suspensions of a-Al2O3, SiC and Si3N4 with a solids volume fraction of 1% and 10%. Zeta potential and streaming potential are related by a linear function. The correlation coefficients for this relationship are better than 0.99 for the suspensions with 1% solids loading. For the suspensions with 10% solids loading, correlation coefficients are slightly lower due to the influence of increasing viscosity. Regardless of lower correlation at the higher solids loading, the isoelectric pH is constant within the limits of accuracy of the pH measurements.
The isoelectric point is a material property for the characterization of acid-base behavior of the powder surface. The IEP of two alumina powders (AKP-30, Grade A) with different particle size characteristics in aqueous suspension has been determined by colloid vibration current (CVI) and particle charge detection (PCD) methods in moderately concentrated suspensions in order to qualify these methods for a future standardization. The solid loading of the suspensions were 1 and 5 vol%. The comparison of the IEP determined by PCD and CVI was in good agreement. However, the solid loading dependence of IEP and a large IEP hysteresis (at 1 vol%) were observed, which do not allow a proper determination of the IEP. The recording of the potential curve and therfore the determination of the IEP with CVI was difficult for the suspension of Grade A powder due to formation of agglomerates at pH values near the pHIEP.
Tribology of Advanced Ceramics III: Principles of solid lubrication - materials and mechanisms
(2002)
Promoting the infrastructure - prestandardisation endeavours for ceramic powders and green bodies
(2002)
Several colour-difference formulas such as CMC, CIE94, and CIEDE2000 have been developed by modifying CIELAB. These formulas give much better fits for experimental data based on small colour differences than does CIELAB. None of these has an associated uniform colour space (UCS). The need for a UCS is demonstrated by the widespread use of the a*b* diagram despite the lack of uniformity. This article describes the development of formulas, with the same basic structure as the DIN99 formula, that predict the experimental data sets better than do the CMC and CIE94 colour-difference formulas and only slightly worse than CIEDE2000 (which was optimized on the experimental data). However, these formulas all have an associated UCS. The spaces are similar in form to L*a*b*. © 2002 Wiley Periodicals, Inc. Col Res Appl, 27, 282-290, 2002; Published online in Wiley InterScience (www.interscience.wiley.com).
Raman spectroscopic and 35Cl-NMR scans of Hydro-Xan®, a preparation containing the biocatalytically effective Tetrachlorinedecaoxide anion (TCDO), are described. The spectroscopic analyses showed that HydroXan® does not contain chlorite initially used in the preparation anymore. Furthermore, a structure of four equal chlorate-like ClO3-groups was indicated for TCDO by the scans. Such a structure is supported by the long-term stability of HydroXan® found at tests over 267 days.
VOC/SVOC-Emissions from materials for flooring installation (primer, screed, adhesive, floor covering) were measured by means of emission test chambers and cells over a time period of at least 28 days at 23 C, 50 % relative humidity and an area specific air flow rate of q = 1.25 m³/m²h. Single components were tested in comparison to three complete structures (same concrete, primer, screed, adhesive) with different types of floor covering (PVC, carpet, linoleum). Sorption into concrete/screed and different sealing by the flooring materials affected the emissions from the complete structures. The complete structures with linoleum and PVC showed the same emissions and emission rates as the flooring materials alone. Emissions from the carpet-covered structure resulted mainly from the lower layers. For two adhesives the formation of secondary emissions (aldehydes and organic acids) was observed starting after the standard testing time of 28 days.
NDT of Concrete Structures
(2002)
NDT-CE in Civil Engineering
(2002)
NDT of Concrete Structures
(2002)
Super steels
(2002)
FAU membranes of type NaX and MFI membranes of type silicalite-1 which contain adsorbed azobenzene (AZB), have photoswitchable permeation properties due to the transcis photoisomerization of AZB. The change of gas permeation through these hostguest composite membranes depends on the irradiation wavelength, the quality of the membranes and the amount of adsorbed AZB. The permeances of the gases in the trans-form of the zeolite-encapsulated AZB were higher than those in the cis-form. The separation factors of equimolar mixtures of N2/CO2 and CH4/CO2 fed through the FAUAZB membrane were higher at trans-switching than at cis-switching. The changes of the permeances of single gases and of the separation factors of equimolar gas mixtures by photoinduced transcis switching were found to be reversible over numerous switching cycles. The experimental results are in agreement with predictions made by Monte Carlo simulations for passing of permeant gases through these hostguest systems with the zeolite-hosted AZB in the trans- and in the cis-configuration.
While artificial weathering is a long-established tool to investigate long-term behaviour of polymers at outdoor conditions, the use of chemiluminescence as a highly sensitive and broadly applicable sensor for the effected change is a recent addition. This combination of artificial weathering with chemiluminescence could already be successfully applied to differentiate and evaluate long-term stability of various real use polymeric building materials relatively to each other and promises to be a useful tool for a variety of other polymeric materials as well.
Monolayers of straight chain and 2-methyl branched chain alcohols with alkyl chain lengths of C10-C18 are experimentally studied by a conventional film balance technique combined with a Brewster angle microscope (BAM). The comparison of the surface pressure ()-area (A) isotherms with the corresponding BAM images provides information on the phase behavior and the first-order main phase transition of the monolayers. Striking differences in the dependence of the phase transition pressure on temperature of the straight chain and 2-methyl-substituted alcohols are correlated with differences in the molecular ordering. The general conditions for the main phase transition in the corresponding homologous alcohols can be derived. The effect of alkyl chain length and 2-methyl substitution on the general textural features of the condensed phase domains is determined under equilibrium and nonequilibrium conditions. n-Alcohol monolayers form defined and well-shaped condensed phase domains, often with inner texture in equilibrium. The long-range orientational order is strongly reduced in the condensed phase of 2-methyl-alcohols. Therefore, in the two-phase coexistence region of 2-methyl-alcohol monolayers only irregularly shaped domains without any inner structure are formed, which cannot be observed at the medium alkyl chain length C14 because of the low contrast. Model calculations of the two-dimensional lattice structure of the racemic 2-methyl-hexadecanol on the basis of the pg space group are performed and correspond well with the reduced ordering concluded from the experiments.
HIIRM final report
(2002)
Accurate analytical results have become more and more an absolute essential tool for further progresses in technology and science. Precision however, often used in this context as a quality criterion for analytical methods, is not a replacement for accuracy in any way. Therefore, analytical procedures are necessary, which will generate reliable and accurate results and can be used for evaluation of other analytical procedures and certification of reference materials (RM). Especially the certification of reference materials for the amount content of trace elements requires highly accurate results with a small combined uncertainty. The best example for an analytical procedure having this capability is undoubtedly Isotope Dilution Mass Spectrometry, for inorganic as well as for organic applications. Applied on Thermal Ionization Mass Spectrometry (TIMS) isotope dilution provides results of highest quality and proven high accuracy especially in the field of RM certifications for more than 30 years.
The major drawback of this approach often is the necessity for a complex chemical separation step. A major advantage of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is the potential to cope with a simplified or an on-line-carried-out sample preparation. A key requirement of isotope dilution analysis however is the accurate and precise determination of isotope ratios, because of its limiting factor for the accuracy and the total uncertainty of the result. Very precise isotope ratios can be determined in combination with a detection system that is capable of simultaneous detection of different isotopes, a so-called multi-collector system.
The objective of the presented project is to evaluate the advantages of such a multi-collector ICP-MS for the application of IDMS in the field of trace elemental analysis in reference materials. The focus is on the development of simple and fast procedures for isotope ratio measurements in general and IDMS analysis in particular. Furthermore, it is an objective to develop and evaluate on-line spiking procedures.
One of the first conclusions, which had a severe impact on the HIIRM project, arose during the early days of the project. Currently most certification experiments are accomplished by certification campaign based on a variety of participants’ results. The sample preparation, sending, analyzing and data evaluation however require lot of resources and the process may take a long time. An alternative way is given by using fewer participants with methods of higher metrological quality. For elemental amount contents such a method undoubtedly is isotope dilution analysis and multi-collector ICP-MS offers the necessary precision and matrix robustness and ruggedness as said above. Therefore, a multiple collector ICP-MS was manufactured as part of the project instead of the originally planned high-resolution instrument. Due to the novelty of the multicollector ICP-MS instrument, a lot of additional fundamental research became necessary. Especially interferences needed further attention. Fortunately, the IsoProbe is additionally equipped with a high-resolution option and with a brand new collison cell. The high-resolution option however can only be used to identify interferences but cannot be used to quantify them. On the other hand, the use of the collision cell proved to be a vital tool to overcome interferences. This is especially true because high resolution would have reduced the available sensitivity by a factor of ~100. Applying the collision cell technology the high sensitivity was maintained whilst most interferences were eliminated. However finding the right parameters of operation for the collision cell became a huge part of the method development process. A variety of gases like argon, helium, hydrogen, deuterium, nitrogen, krypton and xenon were tested for their suitability. Especially the tests accomplished for iron determinations revealed that carefully selected parameters have an incredible influence on the quality of the final results. Nonetheless collision cell technology will undoubtedly be widely used for newer ICP-MS instrumentation and contribute to eliminate wrong analytical values caused by interferences.
The enhanced sensitivity of the instrument revealed also problems not detectable by other means. The control of contaminations seems to be one of the major analytical challenges in the future. Sector field based ICP-MS will give the user an opportunity to trace sources of contamination back to their origin and eliminate them. Even lower limits of detection will be the result as well as an enhanced reliability for analysts dealing with higher amount contents. The analyst will also benefit in controlling blank levels when the method of isotopically spiked procedure blanks is used as demonstrated in this project.
Another main part of the project was the validation of the developed procedures. The first validation step was successfully accomplished by applying these procedures on the standard solutions provided by NRG. The main part of this validation however consisted of the evaluation of the fundamental parameters of the isotope dilution process and related measurements. This approach turned out to be superior compaired to the first step as a highly reliable uncertainty calculation can be easily performed. The best reputation and acceptance of the methods can however only be accomplished by participating in certification campaigns or in interlaboratory comparisons on highest metrological level. The results of the participations in general were brilliant. Not only the results but also the obtained realistic uncertainties were of superior quality. Direct comparisons at BAM with the results obtained by a multicollector TIMS applying the same calculation schemes showed the benefits of using multicollector ICP-MS. The main benefits of ICP-MS were identified, of which the first one is the enhanced precision of the isotope ratio measurement. For a variety of elements the values obtained by multicollector ICP-MS are even more precise than the ones obtainable by multicollector TIMS. The second important advantage identified was the simplified sample preparation. The laborious and time consuming analyte-matrix-separation step as necessary for TIMS measurements can either be omitted or at least be drastically reduced. Therefore, the advantages regarding time and enhanced sample throughput will result in further spread of ICP-MS in general and multicollector ICP-MS in particular.
The third major part in terms of the method development process was mainly focused on developing an online isotope dilution system. The volumetric instead of the gravimetric IDMS approach proved difficult, if the high demands necessary for RM definition measurements are to be fulfilled. The major obstacle in this case is the missing stability and precision in terms of mass flow. Consequently, the initial development failed as the system made up of two piezoelectric droplet injectors was unable to reach the required stability as well as precision. The thereupon-created system consisting of two HPLC pumps proved to be far more valuable regarding automation and particularly the quantification of transient signals. Nevertheless, such a system will probably be rarely used in certification campaigns, as the gain of time is too small compared to the loss of reliability. However, this system proved most valuable in terms of species-specific elemental analysis as preliminary investigations showed. In this context this system will be suitable for certification measurements, as the major uncertainty contributions derive from sampling, sample treatment and species distribution and as moreover all availabel methods demonstrate far beyond.
During the whole project, one of the main concerns regarding the multicollector ICP-MS instrument were software issues caused by the early development state of the original control programs. A lot of effort was necessary to accomplish the necessary data manipulations externally. The development of a new software suite by Micromass for the HIIRM project has solved this issue almost completely. With the new software suite and the validated parameters of measurement a step forward for institutes dealing with reference material certifications was achieved.
Future certifications campaigns for minor elemental contents in different matrices should be performed by a small number of participants from highly qualified institutes. These institutes should apply very reliable methods of measurement like the ones developed in the HIIRM project. Many resources may be saved that way while the outcome of the certifications may easily be improved. ICP-MC-MS has the potential to be an important method in this context. Stable isotope dilution analysis in combination with a multi-detector ICP-MS, equipped with a hexapole collision cell for the suppression of important spectral interferences and for enhanced sensitivity, proved to be an advanced method of elemental analysis with a high potential for matrix independent measurements. Since ICP mass spectrometers of this type have only recently been introduced, no systematic evaluation of the capabilities of this specific application of the ICP-IDMS method has yet been made.
The role of 1,1-diphenylethylene (DPE) in radical emulsion polymerization of methyl methacrylate is investigated. The presence of DPE causes a strong decrease in both the rate of polymerization and the molecular weight. According to the results of structure analysis by means of MALDI-TOF mass spectrometry, UVvis spectroscopy, and 1HNMR spectroscopy, DPE is incorporated in the copolymer chain exclusively as a reactive recombinant ?,p-dimer, underlining the peculiar role of DPE in radical polymerizations.
This paper discusses the results and the consequences of the results obtained in a finished project on fretting
testing at very small amplitudes. In this project a crossed cylinders model contact (radius 2.5 mm) was tested
mainly in tangential oscillatory modes with strokes 2-100 µm, with forces between 0.5 and 5 N and frequencies
of 1 and 10 Hz, financed by the European Commission.
For non-noble contact platings it has been shown that very small amplitudes (< 10 µm) result in surface damage
and contact failure. For noble platings it results in surface damage, only followed by contact failure after wear
causes exposure of the non-noble underlayer.
The most important conclusion from the project work was that the contact resistance remains low and stable in
partial slip, while gross slip causes electrical failure(>0.5 .).
In this paper the following items are discussed: i) The application of the Mindlin theory to predict the transition
from partial to gross slip ii) Aspects of tribo simulation testing of electrical contacts iii) The methods of extending
the allowable external displacement amplitude by additional springs that absorb part of the motion, and iv)
The options if large vibrations at the contact interface can not be avoided.
Laboratory model test for monitoring the new main railway station of Berlin - The Lehrter Bahnhof
(2002)
Part 3 of the ISO 14577 ¡°Instrumented indentation test for hardness and materials parameters¡° (IIT) concerns the calibration of reference blocks. Besides the widely spread activities for supplying reference blocks in the nano and micro range it is needed to be taken into account the macro range too. The paper reports on test results on ceramic materials which are tailored for reference blocks. The specimens made of Si3N4, SiC, or Al2O3 ceramics are highly homogenous and exhibit an increased quality with a roughness Ra ¡Ü 0.005 ¦Ìm. They are successfully used for reference blocks of the traditional Vickers and Knoop hardness. In comparison, the capability of hardened steel which is used for traditional hardness techniques is studied.
The standard for advanced technical ceramics ENV 843-4 of 1995 (Vickers, Knoop and Rockwell superficial hardness tests) was validated within the framework of the CERANORM EC-project. The paper reports on depth sensing hardness measurements done for comparison with the other hardness tests. The instrumented indentation test is a modern technique (recent issue ISO/DIS 14577) that has the potential to take into account the specific response of materials in a much better way. An evaluation has been made to establish whether the instrumented hardness technique is a appropriate method for advanced technical ceramics and offers potential for additional applications.
Dielectric investiations of photochromic copolymers with azobenzene moities in the side group
(2002)
Apparently that the type testing procedure should be conducted under the conditions ensuring reproducibility of its outcomes. We investigated various factors effecting upon the reproducibility. To obtain quantitative characteristics of indications visibility the image-processing hard-and software were used. It was established that there are two main groups of these factors. The first depends on the differences between various test panels, which are used for type testing. The second one concerns the reproducibility of some stages of penetrant testing procedure (excess penetrant removing and developer application). The recommendations to increase the reproducibility of type testing are developed and illustrated experimentally.
The determination of penetrant system sensitivity as a part of type testing should be conducted ensuring reproducibility of the result. We investigated some factors effecting the reproducibility. To obtain quantitative characteristics of indications visibility, an image processing system was used [1]. We used 3 different sets of reference blocks (rb1, rb2, rb3) corresponding to type 1 of EN ISO 3452-3 [2]. Two fluorescent penetrants with different sensitivities and the same wet solvent developer were used.
It was established that the reproducibility of type testing is influenced by mainly two principal factors. First there are the differences between reference blocks. Second one concerns the reproducibility of penetrant testing procedure, especially excess penetrant removal and developer application.
According to EN ISO 3452-3 a reference block for determination of sensitivity level of fluorescent penetrants consists of a set of three nickel-chrome plated panels with 10, 20 and 30 µm plating thickness. Transverse cracks are made in each panel by stretching the panels in the longitudinal direction and width to depth ratio of the cracks should be approximately 1/20. Each panel presents a certain sensitivity level, which is characterised by the level of visibility of the indication. The highest level 3 corresponds to the panel with 10 µm thickness plating. Each panel is cut longitudinally (perpendicular to the crack) so that 2 sheets (panels A and B) with nearly the same cracks will be produced. These panels A and B of a reference block are used for relative evaluation, for example to compare sensitivities of two penetrants. It is considered that the application of the same penetrant to both panels with subsequent adequate development results in the same visibility of the indications on these panels.
Quantitative correlations between the abilities of the reference blocks used for determining of the sensitivity were obtained in our investigations. We used the relations between the measured values of light-fluxes from the indications of similar comparing areas on two panels. These indications correspond to certain cracks parts of the same total length on both comparing areas. The relations of the steps between the panel are responsible for the definition of the sensitivity groups. From our investigations it follows that the steps of the different sets are different. Besides it was established that the indications visibility for the same penetrant applied on different reference blocks might have a considerable difference depending on the penetrant sensitivity: the higher penetrant sensitivity, the smaller is such a difference between the steps 30/20 and 20/10. For example, for rb3 the relations 30/20 and 20/10 for lower sensitive penetrant (I1) reached factor 3 comparing with factor 2 for higher sensitive penetrant (I2).
Some results of the comparison between the 3 sets (rb1, rb2, rb3) investigations are summarised in Table 1 with rb1 as a reference.
Thermal shock cycle experiments between room and cryogenic temperatures on polymer composites
(2002)
This paper presents investigations on the tribological behaviour of PTFE composites against steel at cryogenic temperatures. The results showed that the friction coefficient decreases with temperature down to 77 K, but did not follow a linear evolution further down to extreme low temperatures. It can be stated that the cryogenic environment has a significant influence on the tribological performance of the polymer composites. The effect of low temperatures was more clearly detected at low sliding speed, where friction heat is reduced. A change in wear mechanism from adhesive to abrasive was observed in this case. SEM and AFM analyses showed that the PTFE matrix composites investigated under these experimental conditions have transferred material onto the disc down to very low temperatures. Chemical analyses indicate the presence of iron fluorides.
The gelcasting process was used for manufacturing porous ceramic bodies from nano sized powders. 3 different powders with specific surface areas between 12 and 30 m²/g were used. Solid content of the corresponding slurries was dependent on the milling procedure and the use of a suitable dispersant. For bimodal GradeA powder solid content was as high as 58 vol%. For sintering temperatures between 1250 and 1600°C the porosity varied between 45 and 20%, whereas the pore radii varied between 50 and 91nm. The grain size of crystallites in the sintered microstructures was about 1um. The reflection ratio for visible light increased in comparison to a reference sample made from conventional powder from 0.8 to 0.95 in the wavelenght range around 400nm.
Fabrication of carbon/silica hybrid materials using cationic polymerization and the sol-gel process
(2002)
Long-term performance of permeable reactive barriers has been investigated in laboratory experiments using elemental iron and hydroxyapatite as reactive materials and uranium as contaminant. Accelerated testing has been performed by applying elevated pollutant concentration and an increased flow velocity. The spatial distribution of uranium in the test columns has been investigated using a radioactive tracer. The results show that the migration pattern exhibits a linear behaviour.