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Eingeladener Vortrag
- nein (1)
The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits.
Sintering and foaming of barium and calcium silicate glass powder compacts have been studied for different powder milling. Sintering was measured by means of heating microscopy backed up by XRD, DTA, Vacuum Hot Extraction (VHE) and electron microscopy. Foaming intensity strongly increased with decreasing glass partiefe size. Although powder compacts were uniaxially pressed and sintered in ambient air, foaming was affected by the milling atmosphere and most intensive for milfing in C02. Conformingly, VHE studies revealed that foaming of fully sintered samples was mainly driven by C02, even for powders milled in technical air, Ar and N2. Prolonged storage of air milled barium silicate glass powders in ambient air before pressing and sintering caused further increase of foaming intensity. These findings indicate that carbonaceous species are preferentially trapped to or close beneath the powder surface during milling and later storage. The temperature range of C02 degassing from fully sintered barium and calcium silicate g/ass powder compacts fits the temperature ranges of decomposition of BaC03 and CaC03 mix-milled with the respective barium and calcium silicate glass powders.
A variety of methods used to prepare nano-objects for surface analysis are described along with information about when they might be best applied. Intrinsic properties of NPs which complicate their characterization and need to be considered when planning for surface or other analyses of NPs are identified, including challenges associated with reproducible synthesis and functionalization of the particles as well as their dynamic nature. The relevant information about the sample preparation processes, along with analysis details and data that need to be added to the collection of material provenance information is identified. Examples of protocols that have been successfully used for preparation of nano-objects for surface analysis are included in an annex.
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.
Since the beginnings of the European American Workshops (EAW) in 1997, the aim was to gather the experts in NDE reliability and discuss burning topics with the aim of identifying crucial problems and suggesting ways to move forward. This was usually achieved during the so-called break-out sessions, in which predetermined topics were discussed. During the 5th EAW, held in Berlin in 2013, this approach was replaced by an Open Space Technology (OST) approach. The benefit of this approach is seen in the freedom of topic choices, i. e., the topics are not predetermined but rather arise at that moment in that space and by the participants choice. The following topics arose: new reliability methods (Bayesian, MAPOD,
), structural health monitoring, definition of requirements of NDE by customer versus provider, what value of POD is good enough?, human factors, manual versus automated inspection, and basic concepts of reliability of NDE. The participants were encouraged to walk from one session to another and openly express their opinions. These were in the end summarized by a chosen group of moderators and presented in this paper.
This paper gives an introduction to the field of human factors with the focus on their influence on the reliability of NDT in the nuclear energy production (in-service inspections) and final storage of highly radioactive nuclear waste. A set of methodological tools has been developed in the scope of three projects, namely: 1) a theoretical model describing potential human factors influencing manual ultrasonic inspection performance during inservice inspections in nuclear power plants; 2) a method for identifying potential human errors during acquisition and evaluation of data gathered with mechanized ultrasonic, radiographic and eddy-current systems, as well as visual testing with a remote camera (Failure Modes and Effects Analysis, FMEA); and 3) use of eye tracking methodology to optimize existing procedures and practices. The experimental results have shown that time pressure, mental workload and experience influence the quality of the inspection performance. Noticeable were influences from the organization of the working schedule, communication, procedures, supervision and demonstration task. Implementing human redundancy in critical tasks, such as defect identification, as well as using an automated aid (software) to help operators in decision making about the existence and size of defects, could lead to other kinds of problems, namely social loafing (excerpting less effort when working on tasks collectively as compared to working alone) and automation bias (uncritical reliance on the proper function of an automated system without recognizing its limitations and the possibilities of automation failure) that might affect the reliability of NDT in an undesired manner.
Die übergeordnete Zielsetzung unserer Untersuchung bestand darin,
am Beispiel von Prüfungen mit Ultraschall eine belastbare Aussage zum Einfluss der Arbeitsbedingungen des Prüfers auf die Qualität der Ergebnisse von zerstörungsfreien Prüfungen zu ermitteln und Möglichkeiten zur Minimierung ungünstiger Einflussfaktoren aufzuzeigen.
Der Schwerpunkt der Untersuchung wurde auf die manuelle Ultraschallprüfung gelegt und der Faktor 'Zeitdruck' (in drei Stufen variiert) als die zu variierende physische Einflussgröße gewählt. Die Variation des Faktors Zeitdruck wurde gemäß dem Prozessmodell von der Erhebung psychologischer Faktoren, die das Individuum und die Organisation beschreiben, begleitet.
Die Ultraschallprüfungen erfolgten mit zehn Prüfern am Großbehälter und an Vergleichskörpern mit eingebrachten Testfehlern (Nuten, Risse). Die ausgewählten Fehler waren typisch für Prüfaufgaben, die bei wiederkehrenden Ultraschallprüfungen in Kernkraftwerken von den Prüfern zu lösen sind. Die Prüfaufgabe bestand darin, die in den vorgegebenen Prüfabschnitten vorhandenen Reflektoren aufzufinden und deren Amplituden, Ortskoordinaten und Längenerstreckungen zu ermitteln. Als Bewertungsmaßstab für die Qualität der Prüfaussage und für den Einfluss des menschlichen Faktors diente die Präzision der gemessenen Werte. Die Ergebnisse zeigen einen hohen Einfluss des menschlichen Faktors auf das Prüfergebnis und eine Einwirkung des Zeitdrucks besonders auf die Präzision der Messwerte. Hierbei war die Wirkung des individuell wahrgenommenen Zeitdrucks zusammen mit der psychischen Arbeitsbeanspruchung signifikant. Es wurde unter anderem herausgearbeitet, dass durch eine gute Vorbereitung auf die Prüfung, z.B. durch die sorgfältige Einweisung und ein vorgeschaltetes Fertigkeitstraining an Vergleichskörpern, die Zuverlässigkeit der Prüfergebnisse verbessert werden kann.
Insgesamt hatte der Faktor 'Organisation' neben der 'Erfahrung' einen hohen Einfluss auf das Leistungsvermögen der Prüfer.
Die Projektergebnisse wurden im Abschlussbericht des Forschungsvorhabens SR2514 dargestellt, es wurden drei Empfehlungen zur Vorbereitung und Einweisung der Prüfer, zur Stärkung der Verantwortung der Prüfaufsicht und zum 4-Augen-Prinzip formuliert. Die Empfehlungen wurden in der KTA- Regel 3201.4 'Komponenten des Primärkreises von Leichtwasserreaktoren; Teil 4: Wiederkehrende Prüfungen und Betriebsüberwachung (RÄE Fassung 2010-11)', umgesetzt.
The sintering of bioactive glasses allows for the preparation of complex structures, such as three‐dimensional porous scaffolds. Such 3D constructs are particularly interesting for clinical applications of bioactive glasses in bone regeneration, as the scaffolds can act as a guide for in‐growing bone cells, allowing for good Integration with existing and newly formed tissue while the scaffold slowly degrades. Owing to the pronounced tendency of many bioactive glasses to crystallize upon heat treatment, 3D scaffolds have not been much exploited commercially. Here, we investigate the influence of crystallization on the sintering behavior of several bioactive glasses. In a series of mixed‐alkali glasses an increased CaO/alkali metal oxide Ratio improved sintering compared to Bioglass 45S5, where dense sintering was inhibited.
Addition of small amounts of calcium fluoride helped to keep melting and sintering temperatures low. Unlike glass 13‐93, these new glasses crystallized during sintering but this did not prevent densification. Variation in bioactive glass particle size allowed for fine‐tuning the microporosity resulting from the sintering process.
Messung und Bewertung von Gerüchen aus Bauprodukten für den Innenraum gewinnen vor allem durch den zunehmenden Bau energieeffizienter Gebäude an Bedeutung. Intensive und unangenehme Gerüche werden von Bewohnerinnen, Bewohnern und Angestellten nicht akzeptiert und können auf Dauer krank machen. Bislang stand noch kein allgemein anerkanntes Messverfahren zur Verfügung. Dieses wurde nun in Forschungsprojekten entwickelt, wobei auch konkrete Bewertungsvorschläge zur Zumutbarkeit von Gerüchen gemacht wurden. Das Verfahren ist an die Messung der Emissionen flüchtiger organischer Verbindungen aus Bauprodukten gekoppelt und nutzt Probanden, um die Geruchsstärke (Intensität) und den Geruchseindruck (Hedonik) zu ermitteln. In der Praxis wird das Verfahren nun an verschiedenen Stellen erprobt. Die Bewertung der Geruchsemissionen gibt der Industrie die Möglichkeit, geruchsarme Produkte zu gestalten. Die Kennzeichnung geruchsarmer Bauprodukte mit dem Umweltzeichen Blauer Engel erleichtert Verbraucherinnen und Verbrauchern die Orientierung beim Einkauf.
Accurate and reproducible measurement of the structure and properties of high-value nanoparticles is extremely important for their commercialization. A significant proportion of engineered nanoparticle systems consist of some form of nominally core-shell structure, whether by design or unintentionally. Often, these do not form an ideal core-shell structure, with typical deviations including polydispersity of the core or shell, uneven or incomplete shells, noncentral cores, and others. Such systems may be created with or without intent, and in either case an understanding of the conditions for formation of such particles is desirable. Precise determination of the structure, composition, size, and shell thickness of such particles can prove challenging without the use of a suitable range of characterization techniques. Here, the authors present two such polymer core-shell nanoparticle systems, consisting of polytetrafluoroethylene cores coated with a range of thicknesses of either polymethylmethacrylate or polystyrene. By consideration of surface energy, it is shown that these particles are expected to possess distinctly differing coating structures, with the polystyrene coating being incomplete. A comprehensive characterization of these systems is demonstrated, using a selection of complementary techniques including scanning electron microscopy, scanning transmission electron microscopy, thermogravimetric analysis, dynamic light scattering, differential centrifugal sedimentation, and X-ray photoelectron spectroscopy. By combining the results provided by these techniques, it is possible to achieve superior characterization and understanding of the particle structure than could be obtained by considering results separately.
ISO Technical Report 23173 describes methods by which electron spectroscopies, including X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and synchrotron techniques, can be employed to calculate the Coating thicknesses and compositions of nanoparticles. The document has been developed to review and outline the current state-of-the-art for such measurements. Such analyses of core–shell nanoparticles are common within the literature, however the
methods employed are varied; the relative advantages and disadvantages of These methods, and the optimal usage of each may not be clear to the general analyst. ISO Technical Report 23173 aims to clarify the methods that are available, describe them in clear terms, exhibit examples of their use, and highlight potential issues users may face. The information provided should allow analysts of electron spectroscopy data to make clear choices regarding the appropriate analysis of electron spectroscopy data from coated nanoparticle systems and provide a basis for understanding and comparing results from different methods and systems.
Merocyanine–triarylamine bichromophores are readily synthesized by sequentially Pd-catalyzed insertion alkynylation–Michael–Suzuki four-component reactions. White-light emissive systems form upon aggregation in 1 : 99 and 0.1 : 99.9 vol% CH2Cl2–cyclohexane mixtures, ascribed to aggregation-induced dual emission (AIDE) in combination with partial energy transfer between both chromophore units as supported by spectroscopic studies.
Glass-ceramics are noted for their unusual combination of properties and manifold commercialized products for consumer and specialized markets. Evolution of novel glass and ceramic processing routes, a plethora of new compositions, and unique exotic nano- and microstructures over the past 60 years led us to review the Definition of glass-ceramics. Well-established and emerging processing methods, such as co-firing, additive manufacturing, and laser patterning are analyzed concerning the core requirements of processing glass-ceramics and the Performance of the final products. In this communication, we propose a revised, updated definition of glass-ceramics, which reads “Glass-ceramics are inorganic, non-metallic materials prepared by controlled crystallization of glasses via different processing methods. They contain at least one type of functional crystalline phase and a residual glass. The volume fraction crystallized may vary from ppm to almost 100%”.
Sugarcane bagasse is commonly combusted to generate energy. Unfortunately, recycling strategies rarely consider the resulting ash as a potential fertilizer. To evaluate this recycling strategy for a sustainable circular economy, we characterized bagasse ash as a fertilizer and measured the effects of co-gasification and co-combustion of bagasse with either chicken manure or sewage sludge: on the phosphorus (P) mass fraction, P-extractability, and mineral P phases. Furthermore, we investigated the ashes as fertilizer for soybeans under greenhouse conditions. All methods in combination are reliable indicators helping to assess and predict P availability from ashes to soybeans. The fertilizer efficiency of pure bagasse ash increased with the ash amount supplied to the substrate. Nevertheless, it was not as effective as fertilization with triple-superphosphate and K<sub>2</sub>SO<sub>4</sub>, which we attributed to lower P availability. Co-gasification and co-combustion increased the P mass fraction in all bagasse-based ashes, but its extractability and availability to soybeans increased only when co-processed with chicken manure, because it enabled the formation of readily available Ca-alkali phosphates. Therefore, we recommend co-combusting biomass with alkali-rich residues to increase the availability of P from the ash to plants.
In this contribution a Raman spectrometer based control structure for the heating of a desorption column is proposed. For this purpose calibration experiments for the absorption of carbon dioxide using monoethanolamine solutions are carried out and calibration models are developed to measure both carbon dioxide liquid loads and monoethanolamine mass fractions. The calibration experiments are supported by online NMR spectroscopy to accurately measure the appearance of all species in the electrolyte system. Both models are tested during the plant operation of a mini-plant for the oxidative coupling of methane and the proof of concept for the control structure is given. The Raman spectroscopy implemented in the ATEX conform mini-plant shows a reliable and robust performance being even indifferent to impurities hindering the GC analysis.
For absorption processes with fluctuating feed gas compositions it is vital to continuously adjust
the operation point to achieve energy efficiency. In this contribution a Raman-based advanced
process control (APC) is introduced for the absorption of carbon dioxide (CO2) using an aqueous
solution of monoethanolamine (MEA). The APC is based on a Raman spectroscopic analysis of
the composition and CO2 load of the scrubbing liquid and a non-linear model predictive control
(NMPC) to adjust the scrubbing liquid cycle. In addition, an outer real-time optimization loop is
set in place to update the set points for the absorption process depending on the current feed gas composition minimizing the energy consumption of the process. Implementation and testing of the APC have been carried out in a mini-plant at TU Berlin. During a plant operation of more than 160 hours robustness and stability of the APC were shown.