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One-part-geopolymers, produced by addition of water to a mixture of solid silica and sodium alumi-nate, are a less exhaustively studied approach to form geopolymeric binders. Depending on the silica source, the reaction products show significant amounts of zeolite Na-A besides amorphous compounds. Previously, 29Si MAS NMR has been used to analyze the chemical structure of such one-part geopolymers, having crystalline structures and amorphous phases (Q2, Q3, Q4).
In this work, pure zeolites and three different one-part-geopolymers cured for 1 day were investigated by 29Si-27Al TRAPDOR NMR. It was used to identify aluminum phases in overlapping silicon sites. Zeolites Na-X (Si/Al=1.4) and Na-Y (Si/Al=2.7) served as model systems to measure the TRAPDOR effect of the structural units Q4(mAl). Both materials show several Q4(mAl) signals, which are all separated by their chemical shifts. The more aluminum surrounds the silicon tetrahedron the higher are the normalized TRAPDOR difference signals (S0/∆S). The intensity ratios between Q4(mAl) to Q4({m-1}Al) of these signals is fixed but vary slightly between both zeolites. These results are transferred to the complex geopolymer structure.
Most crucial for components of complex shape or heterogeneous micro structure, precise control of sintering has decisive influence on dimensional accuracy, mechanical integrity and reliability of sintered components. In these cases, only in situ 3D high-temperature shape screening during shrinkage would allow revealing temporary sinter warpage and hereby caused potential defects. Against this background, nokra Optische Prüftechnik und Automation GmbH, HTM Reetz GmbH and BAM developed a testing device for in situ 3D shape screening for ceramic and glass-ceramic tapes up to 1000°C by means of high-temperature laser profilometry. The local repeatability of the sample-sensor distance (sample height profile) is 10 µm at 1000°C. Current work is focused on dropping these restrictions in sample shape and temperature. In a second testing device, currently being in development, samples up to 5 cm x 5 cm x 5 cm can be measured at temperatures up to 1500°C.The presentation illustrates the current state of this work and possible applications of the method.
To better understand the mechanism of hydrogen assisted cracking (HAC), it is important to investigate the 3D structure of the cracks non-destructively. Since, cracks introduced by HAC are usually very small, conventional x-ray imaging methods often lack the required spatial resolution.
However, the detection of those cracks can be enhanced by taking advantage of refraction at interfaces within the sample.
To image this refractive deflection we employ analyser based imaging (ABI). In this work we aim at proving the enhanced crack detection of ABI by investigating an alluminum alloy weld.
Application of 4Q-BSE detector and dedicated software enables 3D surface measurements of fracture samples in SEM. 3D surface measurement is independent from magnification and material invariant. Quantitative height measurements require careful detector adjustment and system calibration. Live 3D view allows a fast assessment of topographical features. In addition to SE and BSE imaging, 3D surface data help to analyse and interpret fracture samples.
In this poster we will present some results of a research projects dealing with Arabic recipes of black inks [1-2]. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed.
We will show procedures and problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on squid ink [3] and mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [4]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol, the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts.
[1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004
[2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013
[3] S. Centeno, J. Shamir Journal of Molecular Structure, 873 (2008), 149-159
[4] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50
In this poster we will present some results of a research projects dealing with Arabic recipes of black inks. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed.
First, we will provide an overview of the sources [1-2] employed in the study – dating from 9th to 14th century, although the manuscripts in which they can be found dates up to the 20th century – with an eye on the ink typologies (real and perceived by the compilers). Then we will show how, by reproducing the recipes, it was possible to shed light on some oddities in the procedures and the choice of ingredients. In the end we will discuss problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [3]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol and the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts.
[1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004
[2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013
[3] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50
A comparison between the results obtained from a Computational Fluid Dynamic (CFD) simulation and from the application of an empirical formula for determining the temperature distribution inside a tunnel in case of fire is presented. The temperature is measured and calculated at different distances from the location of the fire and at different time intervals. The fire considered varies with time following a time-heat release rate curve which has a parabolic growing phase, a constant period and a linear decay. The comparison reveals differences in the results. The temperatures calculated with the empirical formula resulted higher than the temperatures obtained by means of the CFD simulation. A list of possible reasons for this limited correspondence is also presented and commented. A proposal for further studies to better define the limitations of both the procedures and to define the influence of each parameter involved is finally presented.
The Kemnitz et al. developed a fluorolytic route to access metal fluorides 1 such as AlF3 2 and MgF2 3 which possess a high surface area. In aluminium-based systems, the synthetic approach led to amorphous xerogels that can be further converted into Lewis superacids.2 Still, despite zirconium oxide being described as a stronger Lewis acid than other metal oxides4 zirconium fluoride-based materials have only recently been reported or investigated. In this work we extend the class of amorphous Lewis acidic heterogeneous catalysts to an amorphous ZrF4 that is active in C-F bond activation.
Kemnitz et al. developed a fluorolytic route to access metal fluorides 2 such as AlF3 3 and MgF2 4 which possess a high surface area. In aluminium-based systems, the synthetic approach led to amorphous xerogels that can be further converted into Lewis superacids.3 Still, despite zirconium oxide being described as a stronger Lewis acid than other metal oxides 4 zirconium fluoride-based materials have only recently been reported or investigated. 6 In this work we extend the class of amorphous Lewis acidic heterogeneous catalysts to an amorphous ZrF4 that is active in C-F bond activation.
The main solidification parameters, namely the crystal axis, the growth rate, and the cross-sectional area of the columnar crystal control the primary microstructure and thus the final weld seam properties.
Limited understanding of solidification parameters due to complexities in experimental and theoretical weld pool boundary determination and
its mathematical description.
Application of local Lamé curves for efficient weld pool boundary reconstruction Derivation of general analytical solutions for the main solidification parameters of a two-dimensional columnar crystal growth during laser beam welding of thin steel sheets.
The Lamé curves approximation technique was successfully applied for the reconstruction of the rear part of the two-dimensional steady-state weld pool boundary. General analytical expressions for the main solidification parameters, namely the crystal axis, the growth rate and the cross-sectional area of the crystal were derived.
The derived expressions and herewith obtained results were verified and validated by comparing them to known theoretical solutions and experimental measurements. Dimensionless analysis of the influence of the size and shape of the rear weld pool boundary on the solidification parameters was provided.
The derived general solutions and the analysis provided allow for critical welding parameters to be estimated and adapted accordingly to improve the welding process.