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The thermal expansion of polymeric parts can be an issue in many applications where the available space is limited, or exact dimensions of the part are required. For this study, a device was designed and built that allowed measuring the thermal expansion simultaneously in all three spatial directions on cubic samples with real-scale dimensions (78 mm edge length). The results are shown between 25 °C and 125 °C for two PE materials, one HMWPE and one tempered UHMWPE, for non-irradiated samples as well as cubes that have been irradiated with 100 and 400 kGy. The results measured with the new device were very similar to those measured with conventional thermo-mechanical analysis equipment and to literature data of UHMWPE. The HMWPE material shows a much larger thermal expansion coefficient in one direction compared to the other two directions during the first heating due to frozen stresses from the pressing step during material manufacturing. These stresses are mostly released by the expansion during the first heating, so that the expansion during the second heating is more uniform. The overall volumetric expansion is the same for both heating runs. By contrast, the tempered UHMWPE material shows no significant difference between first and second heating run, as the stresses from processing could already relax in the tempering step. The irradiation treatment does not affect the values significantly for the given test set-up.
For the construction of hot water storage tanks, ultra high performance concrete proofed to be a suitable building material to ensure water tightness. Common storage tanks build with concrete are designed to endure temperatures up to 90 °C. To increase the energy efficiency however, modern tanks need to withstand temperatures above 100 °C. With increasing temperature and correlating water vapor pressures, the cement must meet new requirements. Thermodynamic modelling is a promising tool for predicting the phase stabilities of minerals in the cement within these temperature and pressure ranges (T/P). Thus, mixture designs can be investigated and optimized with regard to the expected mineral phases in selected T/P-ranges. Additionally, predictions of the long-term material behavior can be derived from thermodynamic data and subsequently the experimental effort can be reduced notably. On the other hand, validation of predictions is needed. The base for the thermodynamic model is a thermodynamic equilibrium and thus, the experimental data for validation should approach the presumed conditions of the equilibrium. This study investigates variable experimental conditions for the hydration of Portland cement at 100 °C to reach a sufficiently progressed development of the phase composition. In case of Portland cement, the highest degree of hydration achievable within a reasonable time span is the most significant parameter. Therefore, Portland cement pastes with w/c ratios from 0.4 to 0.6 and dwell times up to three weeks were examined with powder X-ray diffraction to identify mineral phase changes. At 100 °C and high humidity, Portland cement paste shows the expected mineral phases like portlandite, katoite, and remaining clinker phases. The cement pastes with high water content and long dwell time seem to have the highest degree of hydration, even though the AFm phases stabilize with increasing w/c ratio. A dwell time of two weeks and a w/c ratio of 0.5 was found to provide the mineral composition with the highest degree of hydration including the major phase transitions.
The adaption of the set-up for gas permeability measurements for ultra-high performance concrete
(2022)
In the framework of this project, a steam pressure vessel was to be developed from ultra-high perfor-mance concrete (UHPC) to withstand process temperatures of 200 °C and the respective steam pressure of 15,5 bar. To guarantee the long-term water vapour tightness of the system, the permeability of two UHPC mixtures were tested after long-term cyclic autoclaving. As UPHC shows a high density and therefore low permeability, measurements after the RILEM-Recommendation (TC 116-PCD) reached their detection limit. Therefore, the measurement set-up was adapted to measure the permeability of highly dense UHPC more reliably and quickly. This adaption includes measurements in a higher pres-sure range, the change of sample size thickness and the usage of Ar as a medium compared with the RILEM Recommendation. Additionally, the system was equipped with two pressure sensors and Ar-flowmeters to guarantee a continuous record of the experimental parameters. The new system was tested and evaluated by comparing measurements with the RILEM recommended system. Preliminary results show that the adapted system is capable to provide efficient and reliable results of concrete with low permeability.
A variety of materials of technological interest change their properties through contact with reactive media. Solid-gas reactions lead to a variety of reaction products on the surfaces and internal interfaces. The observation of nucleation and growth processes in the environment where they occur (in situ) from a chemical-structural perspective is especially challenging for aggressive atmospheres. The talk presents innovative approaches to study corrosion mechanisms using advanced X-ray methods. Using energy dispersive X-ray diffraction and X-ray absorption spectroscopy in different tailor made environmental reaction chambers, valuable insights into high temperature oxidation and sulfidation processes were gained. Fe-based alloys were exposed to hot and reactive atmospheres containing gases like SO2, H2O and O2 at 650°C. During the gas exposure the tailor made reaction chambers were connected to a high energy diffraction end station at the synchrotron. The crystallization and growth of oxide and sulfide reaction products at the alloy surfaces were monitored by collecting full diffraction pattern every minute. Careful examination of shape and intensity of phase-specific reflections enabled to a detailed view on growth kinetics. These studies showed, oxides are the first phases occurring immediately after experimental start. As soon as reactive gas media enter the chamber, the conditions change and different reaction products, such as sulfides start to grow. A comparison of different gas environments applied, illustrated the differences in the type of reaction products. The in situ observation of high temperature material degradation by corrosion made it possible to study the contribution of phases, which are not stable at room temperature. For instance, wuestite (Fe1-xO), was frequently observed at high temperatures in humid gases on Fe with 2 wt.% and 9 wt.% chromium, but not at room temperature. The strength of the occurrence of this phase additionally explains why, despite a higher Cr content, ferritic alloys with 9 wt.% Cr in a challenging atmosphere prevent the intrinsic formation of protective layers. The in situ observations were supplemented by careful considerations of thermodynamic boundary conditions and detailed post characterization by classical metallographic analysis. Additionally, the structure and chemistry of the dominant oxide layers were evaluated using X-ray absorption near edge structure spectroscopy. The talk will give an overview about chances and challenges for studying high temperature corrosion phenomena by advanced X-ray methods.
The ferritic steel 13CrMo4-5 due to good properties with relation to attractive price is frequently use in power plants industry. According EN10028-2 this steel can be used up to 570 °C because of its creep behavior but its corrosion resistance limits the use frequently to lower temperatures, depending on gas temperature and slag formation. The corrosion test were performed in environment containing mixture of gases like: O2, COx, SOx and ashes, with elements e.g. Na, Cl, Ca, Si, C, Fe, Al. Exposure time was respectively 240 h, 1000 h and 4500 h in temperature 600 °C. The oxide scale on the 13CrMo4-5 steel was significant thicker than for In686 coating and the difference increase according for longer exposure time.
The microstructure, chemical and phase composition of the oxide scales were investigated by means of a light microscope, the electron scanning and transmission microscopes (SEM,TEM) equipped with the EDS detectors.
All in all, practicing professionals as well as researchers can read this book with pleasure and great benefit. It presents a comprehensive collection of data and practical examples manifested in about 100 graphs, 80 schemes of processes and devices, a manifold of images showing the microstructure of alloys or details of components and several phase diagrams. Tables containing data on commercially available coatings, alloys, compositions of corrosive salts, function of constituents of coatings add further important pieces of information. Thus, this book is a valuable source of information for anyone engaged in work with or research on high temperature coatings.
Abstract Investigations on metal halide systems carried out by Knudsen effusion mass spectrometry in the period 1990-2014 are reviewed in the present paper.163 original papers were published focused on metal halides showing still considerable activity in this area. The fundamentals of the Knudsen effusion mass spectrometry method and thermodynamic background of the investigation are briefly reported. Data to the system studied, temperature ranges, Knudsen cell materials, vapor species identified in the equilibrium vapors and the thermodynamic properties obtained in the study are presented. The important issues of metal halide vaporization studies are briefly discussed and commented. The studies of the vaporization of metal halogens by Knudsen effusion mass spectrometry aimed firstly atthe determination of gaseous complexes species in the vapor and determination of its thermodynamic data like sublimation enthalpy etc. and secondly at the determination of negative ions formation and various ion-molecule equilibria reactions of metal halide systems. Many of the studied materials have a crucial role for modern technologies, for example metal halide lamps, hot corrosion caused by halide salts, phosphorus recovery technologies or gas assisted separation of lanthanides. The investigation of such systems gives information on mechanisms of vaporization, volatility of the systems under various conditions (temperature, pressure etc.), reactivity, thermal stability, resistance etc. that could be further applied for various calculations and to predict the behavior of various components under various technological aspects.