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Eingeladener Vortrag
- nein (23)
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material that exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). Therefore, it can be used to create composites with controllable expansion coefficients and prevent thermal stress, fatigue, cracking, and deformation at interfaces. We implement interdisciplinary research to analyze such material. We study the influence of the synthesis methods and their parameters on the sample's purity, crystallinity, and homogeneity. Moreover, we implement ab initio-based vibrational computations with partially treated anharmonicity in combination with experimental methods to follow temperature-induced structural changes and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder.
X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation.
We thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in materials science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in additively manufactured alloys; 3) Fiber de-bonding in metal and polymer matrix composites.
Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads. Applications of in-situ X-ray refraction radiography on aluminum alloys and composites are also shown.
The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models.
X-ray refraction techniques represent a very promising, yet not so wide-spread, set of X-ray techniques
based on refraction effects. They allow determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with nanometric detectability. While they are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of microstructural features could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
The friction and wear properties of polyetherimide composites under dry oscillating sliding condition at room temperature (RT) as well as at elevated temperature (120 °C) was investigated. The polymer specimens were made to oscillate against steel cylinder as a counterpart. The friction and wear properties of PEI and composites were strongly influenced by the temperature. In case of carbon fiber composite abrasive action of carbon fibers has severely damaged the counterpart and resulted in accelerated wear of the composite at RT. Solid lubricants filled (PTFE, MoS2, graphite) along with glass fiber is beneficial in improving the friction and wear performance of the PEI composite at RT, whereas at elevated temperature wear performance was deteriorated.
A test set-up in intermediate scale was conceived to investigate the structural integrity of materials under fire. The task was to develop a realistic test scenario targeting component-like behaviour. Carbon-fibre-reinforced sandwich specimens (500 X 500 X 20 mm) were used to examine failure mechanisms, times to failure and critical failure loads under compression. Fire tests were performed with fully developed fire applied to one side of the specimen by an oil burner. In a first test series, the applied load was varied, but the fully developed fire remained unchanged. In general, times to failure were short. Decreased load levels resulted in prolonged times to failure and led to a different failure mechanism. Results obtained in the test series were compared with a bench-scale study (150 X 150 X 20 mm) investigating identical material. The comparison clearly revealed the influence of size on the time to failure and the load-bearing capacity.
Structural health monitoring of hydrogen pressure vessels using distributed fiber optic sensing
(2024)
We report on distributed fiber optic sensing-based monitoring of hydrogen composite overwrapped pressure vessels (COPV) to simultaneously increase the operational lifespan and mitigate maintenance costs. Our approach represents, to the best of our knowledge, the first application of distributed fiber optic sensing for COPV Type IV monitoring, where the sensing fibers are attached to the surface, rather than integrated into the composite material. Specifically, we attach an optical fiber of 50 m to the pressure vessel's surface, covering both the cylindrical and dome sections. We note that our fiber optic sensing technique relies on swept wavelength interferometry providing strain information along the entire length of the optical fiber with high spatial resolution even at the millimeter scale. When the vessel is pressurized, the sensing optical fiber shows a linear strain response to pressure at every position along the fiber. After thousands of load cycles, the vessel finally fails with the optical fiber detecting and precisely localizing the damage in the vessel’s blind dome area. Furthermore, we discuss the potential of state-of-the-art signal processing methods and machine learning for advancing predictive maintenance. This could reduce the number of regular inspections, mitigate premature maintenance costs, and simultaneously increase the vessel’s remaining safe service life. We believe that the structural health monitoring of hydrogen pressure vessels with fiber optic sensors can enhance trust in hydrogen technology contributing to the energy transition in the future.
Structural health monitoring of hydrogen pressure vessels using distributed fiber optic sensing
(2024)
We report on distributed fiber optic sensing-based monitoring of hydrogen composite overwrapped pressure vessels (COPV) to simultaneously increase the operational lifespan and mitigate maintenance costs. Our approach represents, to the best of our knowledge, the first application of distributed fiber optic sensing for COPV Type IV monitoring, where the sensing fibers are attached to the surface, rather than integrated into the composite material. Specifically, we attach an optical fiber of 50 m to the pressure vessel's surface, covering both the cylindrical and dome sections. We note that our fiber optic sensing technique relies on swept wavelength interferometry providing strain information along the entire length of the optical fiber with high spatial resolution even at the millimeter scale. When the vessel is pressurized, the sensing optical fiber shows a linear strain response to pressure at every position along the fiber. After thousands of load cycles, the vessel finally fails with the optical fiber detecting and precisely localizing the damage in the vessel’s blind dome area. Furthermore, we discuss the potential of state-of-the-art signal processing methods and machine learning for advancing predictive maintenance. This could reduce the number of regular inspections, mitigate premature maintenance costs, and simultaneously increase the vessel’s remaining safe service life. We believe that the structural health monitoring of hydrogen pressure vessels with fiber optic sensors can enhance trust in hydrogen technology contributing to the energy transition in the future.
The strength of laminates distinctly depends on the transverse strength of the laminas. The transverse failure is dominated by the adhesion between fiber and matrix. Usual strength criteria however do not take into account the adhesive strength explicitly. The determination of the interface strength is performed on the micromechanical scale using single fiber specimens. The fibers are loaded under off-axis loading while the debonding is monitored under a microscope. The stresses acting in the Interface are calculated by finite element analyses. It is found that for off-axial angles up to 35° interfacial debonding is the dominant failure mode while fiber breakage takes place at lower angles. The occurrence of fiber breakage and debonding under off-axis loading shows that the restriction to two potential failure planes - perpendicular or parallel to the fibers - as applied in common failure criteria has to be put in question.
In structural engineering timber is appreciated due to its low weight, its high aesthetic quality and because it is a renewable resource. The market share of timber structures and wood based hybrid structures will clearly increase over the next few years due to greater environmental awareness and a higher demand for sustainability. However, building with timber is marked by characteristics which lead to significant disadvantages in comparison wifh technical materials. For example, in outdoor areas Chemical and structural approaches offen lead to unsatisfactory and expensive Solutions with respect to durability. An idea is to make natural lumber a high-performance material which can be designed to meet the engineers’ demands conceming strength, stiffness, durability, shape, safety etc. These changes can affect the material itself, new technologies or a new approach to monitoring. Especially hybrids made of common timber products and technical textiles or enhanced timber products are high-capacitive and reach high bearing strengths with low material input and good durability. These hybrids are particularly qualified to use the advantages of wood and minimize the disadvantages. They can be used in different ways for load bearing structures, i.e. bridges. New construction types need monitoring to observe the stress and strains for which they were designed, and the structures’ behaviour as well as to guarantee required safety levels. The aim of successful usage of fibre optic measurement technology in timber elements was the development of a technology for measuring the lengthening in timber elements and wood based hybrid elements by using fibre optic sensors. The scientific and technical challenge was to develop an applicationtechnology for optical glass fibres in timber and densified veneer wood.
In laboratory tests as well as with the erection of a footbridge and during in-situ tests it could be shown that the structurally integrated fibre optic sensor technology used is suitable for short and long term measurement. The developed embedment technology tums out to be practical and fit for good transfer of strain-values from timber to the modified sensor fibres.
Leather is a widely used material for thousands of years and in modern days it is produced on industrial scale. This production produces high amounts of organic waste during the tannery process. These fibers can become a resource and act as a multi-functional bio-filler in flame retardant composites.
This project investigates two leather fibers towards their ability to enhance the flame-retardancy in different composites. These composites use ammonium polyphosphate (APP) or aluminum trihydroxide (ATH) as flame retardants. Different silicon based synergists support polymers with ATH to reduce the load of flame retardant. The different modes of action (charring, gas phase activity, barrier effect) can be quantified of each composite.
The new composites form a stable char layer resulting in an increase in residue, lower peak heat release rates (pHRR) and higher limiting oxygen index (LOI). In addition, the ratings in the UL94-classification increased up to V-0.
Leather is a widely used material for thousands of years and in modern days it is produced on industrial scale. This production produces high amounts of organic waste during the tannery process. These fibers can become a resource and act as a multi-functional bio-filler in flame retardant composites.
This project investigates two leather fibers towards their ability to enhance the flame-retardancy in different composites. These composites use ammonium polyphosphate (APP) or aluminum trihydroxide (ATH) as flame retardants. Different synergists support polymers with ATH.
The new composites form a stable char layer resulting in an increase in residue, lower peak heat release rates (pHRR) and higher limiting oxygen index (LOI). In addition, the ratings in the UL94-classification increased up to V-0.
Two different radical polymerization techniques have been applied to covalently graft vinylformamide (VFA) onto silica particles. Grafting by the polymerization of VFA using an immobilized azo initiator on silica has been found less effective, because monomer conversion is limited in non-aqueous solvents and grafting yields are low in water. Radical copolymerization of VFA with vinyltriethoxysilane (VTS)-functionalized silica particles is suitable to produce poly(vinylformamide) (PVFA) silica hybrid particles in respectable yield. The VFA/VTS-silica ratio determines the degree of grafting. The PVFA-VTS-co-grafted silica particles can be acidically hydrolyzed into poly(vinylamine)-grafted silica particles. Molecular structures of the surface groups and grafted polymer chains have been confirmed by means of solid state 13C{1H} cross-polarization magic-angle spinning (CP MAS) NMR spectroscopy. Zeta potential measurements show the altering of the former silica particles surface charges arising from the introduction of basic groups on the surface.
The pyrolysis of an epoxy resin and the fire behavior of corresponding carbon fiber-reinforced composites, both flame-retarded with either 10-ethyl-9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide or 1,3,5-tris[2-(9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide-10-)ethyl]1, 3,5-triazine-2,4,6(1H,3H,5H)-trione, are investigated. The different fire retardancy mechanisms are discussed, and their influence on the fire properties assessed, in particular for flammability (limiting oxygen index, UL 94) and developing fires (cone calorimeter with different external heat fluxes of 35, 50, and 70 kW m-2). Adding the flame retardants containing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide affects the fire behavior by both condensed phase and gas phase mechanisms. Interactions between the additives and the epoxy resin result in a change in the decomposition pathways and an increased char formation. The release of phosphorous products results in significant flame inhibition. The fire properties achieved are thus interesting with respect to industrial exploration.
Highly soluble 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-(DOPO)-based diamino hardener (2), bearing its amino groups directly on the DOPO framework, is investigated with respect to its use as a reactive flame retardant in thermosets. A mechanism for decomposition of the corresponding phosphorus-modified epoxy resin system based on a diglycidylether of bisphenol A DGEBA and 2 (DGEBA/2) is proposed and compared to the systems using DGEBA and 4,4'-diaminodiphenylsulfon (DGEBA/DDS) and to a similar system based on the structurally comparable non-reactive DOPO-based compound (DGEBA/DDS/1). Additive 1 changed the decomposition characteristics of the epoxy resin only slightly and phosphorus was released. Incorporating 2 induces two-step decomposition and most of the phosphorus remains in the residue. Furthermore, the fire behaviour of neat epoxy resin systems and a representative carbon fibre-reinforced composite based on DGEBA, DDS and 2 (DGEBA/DDS/2) were examined and compared to that of the analogous composite systems based on DGEBA/DDS and DGEBA/DDS/1. Based on different flame retardancy mechanisms both the reactive compound 2 and the additive compound 1 improve flammability (increase in LOI >13% and achieving V-1 behaviour) of the epoxy resin and composites. Under forced flaming only the flame inhibition of the additive compound 1 acts sufficiently. Lastly, the superior key mechanical properties of the epoxy resin and composite based on 2 are sketched.