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- 6 Materialchemie (7)
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Eingeladener Vortrag
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In this study, bulked adhesives were examined regarding changes in properties for their use in the restoration of stained-glass windows. Two epoxy adhesives commonly used in the restoration of flat glass, Araldite® 2020 and Hxtal NYL-1™, were investigated. The adhesives were mixed with various silica-based micro- and nano-particles as fillers. Different tests were carried out on the adhesives with and without fillers in order to characterise their chemical and mechanical properties. The tests included colorimetry, dynamic-mechanical methods of analysis and tests on bending strength. No property changes could be ascertained in the bulked adhesives that would be negative for the restoration of delicate flat glass.
The maximum magnetisation (saturation magnetisation) obtainable for iron oxide nanoparticles can be increased by doping the nanocrystals with non-magnetic elements such as zinc. Herein, we closely study how only slightly different synthesis approaches towards such doped nanoparticles strongly influence the resulting sub-nano/atomic structure. We compare two co-precipitation approaches, where we only vary the base (NaOH versus NH3), and a thermal decomposition route. These methods are the most commonly applied ones for synthesising doped iron oxide nanoparticles. The measurable magnetisation change upon zinc doping is about the same for all systems. However, the sub-nano structure, which we studied with Mössbauer and X-ray absorption near edge spectroscopy, differs tremendously. We found evidence that a much more complex picture has to be drawn regarding what happens upon Zn doping compared to what textbooks tell us about the mechanism. Our work demonstrates that it is crucial to study the obtained structures very precisely when “playing” with the atomic order in iron oxide nanocrystals.
In dem IGF-Vorhaben IGF-Nr. 17978 N (P 1011) wurden unter gezielter definierter Schrumpfbehinderung Schweißexperimente an hochfesten Feinkornbaustählen durchgeführt, um den Einfluss der Wärmeführung sowie den Einsatz modifizierter Sprühlichtbogenprozesse verbunden mit schmaleren Nahtfugen auf die lokalen Eigenspannungen und die Gesamteigenbeanspruchungen an geschweißten Bauteilen zu analysieren. Diese Kurzdarstellung fasst die wesentlichen Zusammenhänge zu schweißbedingten Beanspruchungen an hochfesten Schweißverbindungen sowie einige der erarbeiteten Erkenntnisse und erreichten Ziele des Forschungsprojektes zusammen.
Observations on the biology of the wasp Baryscapus tineivorus (Hymenoptera: Eulophidae), a parasitoid of tineid moths. Laboratory studies were undertaken to determine the effectiveness of Baryscapus tineivorus, a gregarious parasitoid wasp with high potential to biologically control Tineola bisselliella, the webbing clothes moth and general pest on textiles. It was found that the sex ratio of B. tineivorus is often heavily female-biased (~6 females to one male). Parthenogenetic reproduction occurrs when males develop from unfertilized eggs. Baryscapus tineivorus is oligophagous, parasitising at least another tineid moth, the casemaking clothes moth Tinea pellionella. I investigated how B. tineivorous finds and selects hosts of various larval ages for egg deposition using two different approaches: (1) an acceptance test, for which only one defined larval stage of T. bisselliella or T. pellionella was offered for egg laying; and (2) a choice test, for which different larval stages or different species were offered. In the acceptance tests, B. tineivorus offspring developed within four to seven weeks old webbing clothes moths larvae and within six to seven weeks old casemaking clothes moth larvae. Dual-choice experiments with both tineid host species revealed that B. tineivorus is more attracted to T. bisselliella than to T. pellionella. Because B. tineivorus was reared on T. bisselliella, parasitoid conditioning (learning) could explain the host preference.
Bacterial infections are a global threat to human health1. Especially nosocomial infections with multidrug-resistant Gram-negative bacteria challenge public health systems and endanger successful treatment of patients in many modern medicine applications as e.g. organ transplant. In the last three decades classical approaches failed to find novel chemical scaffolds suitable for the development of antibiotics that reach the market and caused the modern antibiotics crisis1.
Insect microbiomes produce potent antibiotics with low toxicity to eukaryotic cells to defend their hosts against entomopathogenic microorganisms2. In order to exploit insect microbiomes efficiently and to identify novel antibiotics producing bacteria, we implemented an ultra-high throughput Microfluidics/FACS (fluorescence-associated cell sorting) cultivation and screening pipeline. Here we present the technical aspects of our pipeline including downstream processing of identified producer strains and its suitability for antibiotics discovery.
Fundamental understanding of crack healing in glassy crystalline materials is very important for many applications, especially for sealing solid oxide fuel cells (SOFC) since cracks caused by sealing or thermal cycling still remain a substantial bottleneck in developing durable SOFC.
Previous studies on soda lime silicate glass [Sin14] showed that crack healing is driven by viscous flow and that healing progress is proportional to time t and inverse viscosity η. This finding would allow to present healing data of a given glass for different temperatures in a master curve healing progress versus t/η. Such master curves would be a helpful tool in understanding crack healing kinetics.
Against this background, crack healing in non-crystallizing sodium calcium silicate (NCS) and sodium borosilicate glasses (NBS) have been studied. Moreover, to evaluate the influence of micros structure in crystallized glass on crack healing process, glass matrix composites (GMC) where prepared out of NCS and zirconia as inert ceramic filler material mimicking a partially crystalline micro structure. Cracks were generated by Vickers indention and healed isothermally at different temperatures. Crack healing progress was monitored by optical and electron microscopy. Results show that the above mentioned proportionality actually applies for the studied glasses for which such a master curve could be obtained. In comparison to a non-crystallized glass, the effective viscosity of GMC is increased by rigid filler content. This effect substantially retards crack broadening during later healing stages, which often ends up in large pores. On the other hand, local viscous crack healing is still possible in larger glassy regions. This behavior seems to be very interesting for crack healing optimized sealants.
Experimental and phase field studies of age hardening response of a high purity Al‐4Cu‐1Li‐0.25Mn‐alloy (mass %) during isothermal aging are conducted. In the experiments, two hardening phases are identified: the tetragonal θ′ (Al₂Cu) phase and the hexagonal T1 (Al₂CuLi) phase. Both are plate shaped and of nm size. They are analyzed with respect to the development of their size, number density and volume fraction during aging by applying different analysis techniques in TEM in combination with quantitative microstructural analysis. 3D phase‐field simulations of formation and growth of θ′ phase are performed in which the full interfacial, chemical and elastic energy contributions are taken into account. 2D simulations of T1 phase are also investigated using multi‐component diffusion without elasticity. This is a first step toward a complex phase‐field study of T1 phase in the ternary alloy. The comparison between experimental and simulated data shows similar trends. The still unsaturated volume fraction indicates that the precipitates are in the growth stage and that the coarsening/ripening stage has not yet been reached.
The topic of the presentation consists in some basic considerations on the application of fracture mechanics to fatigue live and strengh prediction of metallic componends manufatured by additive manufacturing. These are based on an approach developed at BAM which comprises elements such as the elastic-plastic modelling of the cyclic crack driving force, a physically meaningfull determination of the initial crack size and multipile crack initiation and propagation due to variations of the local geometry and material charactaristics. Spezial emphasis is put to spezific aspects of materials composed by selectiv laser melting such as surface roughness, porosity and gradiants in the microstructure.
Das Ziel des Gesamtvorhabens bestand darin, einen neuartigen kapazitiven Sensortyp zur hochauflösenden Bestimmung von Masse- und Gravitationskraftänderungen zu entwickeln. Bisherige Technologien nutzten dafür Federn oder Biegebalken aus gehärteten metallischen Werkstoffen, deren Alterungsverhalten die Präzision der Kräftemessung begrenzen. Grundprinzip des neuen Sensortyps ist es, eine auf die keramische Feder einwirkenden Änderung der Gewichts- oder Gravitationskraft durch eine Erfassung der Kapazitätsänderung am Sensor zu bestimmen. Dazu muss die durch Stauchung oder Dehnung der Feder entstehende Kapazitätsänderung mit hoher Auflösung reproduzierbar gemessen werden. Neben einem geeigneten Sensordesign waren Lösungen für Messsignalerfassung und -auswertung (Elektronik/Software) und die Systemintegration zu entwickeln.
Die wichtigsten im Rahmen des BAM-Teilvorhabens erzielten Ergebnisse sind:
- Ausgehend von kommerziellen High-end Keramikpulvern wurden durch Optimierung der keramischen Technologie nahezu porenfreie Al2O3, ZrO2 und Si3N4-Werkstoffe hergestellt und bezüglich Gefüge und Phasenbestand sowie mechanischen, thermischen und elektrischen Eigenschaften bewertet. Insbesondere die defektfreie Herstellung von nanostrukturierten Werkstoffen erforderte umfangreiche Variationen der Prozessparameter. Geeignete Werkstoffvarianten wurden für die Federherstellung ausgewählt.
- Gemeinsam mit den Projektpartnern wurden Layoutvarianten für Schraubendruckfedern mit rechteckigem Windungsquerschnitt und für die Federeinbindung in das Sensorsystem erarbeitet.
- 4 Federvarianten wurden an der BAM durch Hartbearbeitung von gesinterten Hohlzylindern umgesetzt. Fertigungstoleranzen von < ±10 µm für Windungsbreite, Windungshöhe und Windungsabstand und dünnfilm-kompatible innere Windungsflächen (Ra < 0,2 µm) wurden erreicht. Al2O3- und ZrO2-Federn können rissfrei und mit sehr guter Kantenqualität gefertigt werden, bei Si3N4-Federn konnten Kantenschädigungen nicht vollständig verhindert werden.
- Mit der entwickelten Herstellungstechnologie können sowohl „harte“ als auch sehr „weiche“ Federn produziert werden. Federkonstanten zwischen 0,02 N/mm und 10 N/mm wurden realisiert. Die Reproduzierbarkeit der Federfertigung ist gegeben, innerhalb einer Charge unterschieden sich die Federkonstanten der gefertigten Federn nur um etwa +/- 1%.
- An einem speziell entwickelten Versuchsstand wurden die Federn unter zyklischer Druckbelastung im Temperaturbereich von -20 bis +80 °C untersucht. An den Al2O3- und ZrO2-Federn wurden keine Schädigungen beobachtet, die Federkonstante wird durch die zyklische Langzeitbelastung nicht verändert.
- Die Eignung der keramischen Federn für den Applikationsfall wurde mit zahlreichen Spannungs-Dehnungs-Experimenten, teilweise an speziell aufgebauten Versuchsapparaturen, untersucht. An Al2O3- und Si3N4-Federn wurde – wie erwartet – gefunden, dass die Federkonstante unabhängig von der Belastungsgeschwindigkeit ist und unter konstanter Last auch über lange Zeiträume keine Verformung auftritt. Überraschenderweise zeigten ZrO2 (TZP)-Federn ein zeitabhängiges Verhalten unter Last. Dieses ist besonders stark bei Y-stabilisierten Werkstoffvarianten ausgebildet, wurde aber mit Hochpräzisionsmessungen auch bei Ce-stabilsierten Werkstoffen nachgewiesen. Die Deformation ist reversibel, eine vollständige Relaxation wird erst nach Tagen erreicht. Aufgrund der zeitabhängigen Verformung können ZrO2 (TZP)-Federn, trotz ihrer hervorragenden Festigkeit und Bruchzähigkeit, nicht für die konzipierten Sensorfedern eingesetzt werden.
- Das durch die Fa. Siegert TFT entwickelte Metallisierungs-Schichtsystem, bestehend aus aufgesputterten Ti-, Pt- und Au-Schichten verstärkt durch eine galvanisch aufgebrachte Au-Schicht, wurde an der BAM umfassend bewertet. Die Schichten sind untereinander und mit der Keramik weitgehend defektfrei verbunden, die lokale Schichtdicke schwankt jedoch bedingt durch Abschattungseffekte während der Beschichtungsvorgang. Es wurden Schichtwiderstände zwischen 50 und 90 Ohm und damit die Zielvorgabe des Projektes (< 100 Ohm) erreicht. In statischen und dynamischen Belastungstests wurden keine Veränderungen der Leitungswiderstände festgestellt.
- Zur Erhöhung der Kapazität des Kondensators kann der Raum zwischen den Federwindungen statt mit Luft mit einer Flüssigkeit mit hoher Dielektrizitätskonstante gefüllt werden. Als geeignete Flüssigkeit wurde Propylencarbonat mit einer Dielektrizitätskonstante von 65, einem hohen Siedepunkt und einer geringen Viskosität identifiziert. Um eine noch höhere Dielektrizitätskonstante zwischen den Federwindungen zu erreichen. wurden Suspensionen aus Silikonöl und nanokristallinem Bariumtitanat hergestellt und bezüglich ihrer Langzeitstabiltät charakterisiert.
- Gemäß den Anforderungen des Projektpartners KOMPASS wurden maßgeschneiderte Al2O3-Federn mit einer Federkonstante < 0,1 N/mm hergestellt und für den Aufbau des finalen Demonstrator eingesetzt.
Die prinzipielle Funktionsfähigkeit des neuen Sensorkonzeptes auf Basis keramischer Federn wurde mit dem im Projekt aufgebauten Demonstrator nachgewiesen. Die Umsetzung der F+E-ergebnisse in eine industrielle Nutzung zur Herstellung von Gravimetern wird vom Projektpartner KOMPASS angestrebt und ist bereits mit detaillierten Zeitplänen untersetzt.
Ergänzend zu früheren Arbeiten. in denen die Explosionsbereiche für Brenngase aus der homologen Reihe der Alkane und Alkene berechnet worden sind, wurden Ergebnisse der Berechnungen für 1-Propanol, Aceton und Difluormethan vorgestellt. Für die Berechnung ist das Modell erweitert worden. so dass auch die Transporteigenschaften der Gasgemische berücksichtigt werden.
Weiterhin ist eine neue Methode zur Berechnung der Spitze des Explosionsbereichs implementiert worden. Die Ergebnisse zeigen. dass die Berechnung der Explosionsbereiche für Alkohole. Ketone und halogenierte Kohlenwasserstoffe mit ähnlicher Genauigkeit wie für Alkane und Alkene möglich ist.
A novel mixed matrix composite has been prepared using solution-casting method at different volume concentrations of polyvinyl alcohol; PVA (50, 67, 75 and 80 %) and fixed amount of Dimethoxydimethylsilane in air atmosphere. The hydrolyzed dimethyldisilanol acts as in-situ cross linker through a wet-out condensation between the hydroxyl moieties of SiOH and PVAOH. Such process improves the mechanical properties of composite membranes as compared to pristine PVA which has been determined as function of varied membrane components to evaluate the structure/property relationships.
Furthermore, DFT (B3LYP)/6-31G(d) geometry and frequency computations were carried out for the suggested dimeric PVA structures via 1,3-diol linkage followed by condensation and hydrogen bonding interaction. Vibrational interpretations of composite membranes were proposed based on the computed wavenumbers, Cartesian coordinates displacements for the suggested hydrolyzed products involving the dominant PVA/SiOH/SiOC/SiOSi functional groups compared with those given in literatures. FTIR and EDX provide clear evidences for incorporating silicon to 3D network. Meanwhile, the infrared de-convoluted spectral interpretations ensure 17-30% cross-linked SiOC within the network of Composite membranes.
We report on the ferromagnetism of Sn1-xZnxO2 (x < 0.1) hierarchical nanostructures with various morphologies synthesized by a solvothermal route. A room temperature ferromagnetic and paramagnetic response was observed for all compositions, with a maximum in ferromagnetism for x = 0.04. The ferromagnetic behaviour was found to correlate with the presence of zinc on substitutional Sn sites and with a low oxygen vacancy concentration in the samples. The morphology of the nanostructures varied with zinc concentration. The strongest ferromagnetic response was observed in nanostructures with well-formed shapes, having nanoneedles on their surfaces. These nanoneedles consist of (110) and (101) planes, which are understood to be important in stabilizing the ferromagnetic defects. At higher zinc concentration the nanostructures become eroded and agglomerated, a phenomenon accompanied with a strong decrease in their ferromagnetic response. The observed trends are explained in the light of recent computational studies that discuss the relative stability of ferromagnetic defects on various surfaces and the role of oxygen vacancies in degrading ferromagnetism via an increase in free electron concentration.
Der Einsatz von Aluminiumlegierungen als Konstruktionswerkstoff hat in den letzten Jahrzehnten aufgrund seines überlegenen Festigkeits-/ Gewichtsverhältnisses zugenommen. Dabei spielen höherfeste aushärtbare Al-Mg-Si-Legierungen eine wichtige Rolle.
Dieser Beitrag konzentriert sich auf die additive Fertigung von Prinzipbauteilen aus einer Al-Mg-Si-Aluminiumlegierung mittels Wire + Arc Additive Manufacturing. Werkstoffe dieses Legierungssystems weisen eine ausgeprägte Heißrissanfälligkeit auf, weshalb das artgleiche Fügen dieser Materialien, mittels Metallschutzgasschweißen, heutzutage immer noch eine Herausforderung darstellt. Kommerzielle Al-Mg-Si-Schweißdrähte sind am Markt nicht verfügbar.
In dieser Arbeit wird die Anwendbarkeit eines neuartigen Al-Mg-Si-Schweißdrahtes mit zusätzlichen kornfeinenden Elementen für die additive Fertigung mittels MSG-Verfahren gezeigt. Dazu wird der Zusammenhang von verwendeten Prozessparametern und der resultierenden Bauteilqualität untersucht, wobei die Größe und Verteilung von Poren sowie die Kornmorphologie analysiert werden. Darüber hinaus wird der Einfluss einer T6 Wärmenachbehandlung auf die mechanischen Eigenschaften des Werkstoffes untersucht und ein Vergleich zum entsprechenden Referenzmaterial (Knetlegierung) gezogen.
Classic non-destructive fatigue crack detection methods reveal the state of the fatigue damage evolution at the moment of application, generally not under operational conditions. The here introduced crack luminescence method realizes a clear visibility of the occurred and growing crack in loaded components during operation. Different established experiments show that due to the sensitive coating a crack Formation can be detected even in early stage under the premise the crack reached the surface. The coating consists of two layers with different properties and functions. The bottom layer emits light as fluorescence under UV radiation. The top layer covers the fluorescing one and prevents the emitting of light in case of no damage at the surface. In case of surface crack occurrence, the luminescent light is clearly noticeable by visual observations and also by standard camera equipment which makes automated crack detection possible as well. It is expected that crack luminescence can increase structural safety as well as reduce costs and time for inspections and preventive maintenance.
Biodiesel is viewed as a major source of energy. In areas such as the European Un-ion, where 80 % of the oil-based fuel is imported, there is also the desire to reduce dependence on external oil supplies.
Materials compatibility is a major concern whenever the fuel composition is changed. The question arises of whether polymeric materials are resistant to heating oil with 20 % biodiesel (B20) in comparison to pure heating oil.
The polarity of biodiesel increases its solvency and facilitates permeation and extrac-tion. Solvation, swelling and/or extraction lead to changes in the physical properties. Extraction alters the fuel chemistry. These chemical changes could also accelerate the degradation (hydrolysis and oxidation) of the polymeric material with the loss of additives and stabilizers.
Exposure tests to determine the resistance of polymers frequently used for compo-nents in middle distillate facilities, such as ACM, FKM, HNBR, PA, PE, POM, PUR and PVC in heating oil and a blend of heating oil and 20 % biodiesel (B20) were al-ready performed.
The objective of this research was to determine the resistance of these polymers in 8-year aged heating oil blend B10 and 1-year aged blend B20 at 40 °C.
Mass, tensile strength, breaking elongation and Shore hardness A (D) of the test specimens were determined before and after exposure for 84 (42) days in the test fuels under static conditions.
There is not determined a threshold for the reduction in tensile properties and Shore hardness in the international standards. Therefore, a threshold of 15 % was deter-mined for the evaluation of the compatibility.
A significant reduction in Shore hardness was determined after exposure of ACM and PUR test specimens in 1-year aged B20.
The tensile strength of PUR test specimens in 1-year aged B20 was reduced by more than 50 %, and the breaking elongation by more than 30 %.
A decrease in breaking elongation was measured for POM test specimens after ex-posure to 1-year aged B20 by 25 % (limited resistance).
8-year aged B10 had a stronger effect than 1-year aged B20 on the polymers. ACM test specimens were softened by B10 resulting in a drop of Shore hardness by over 20 %. B10 reduced tensile strength and breaking elongation of PUR test specimens by over 50 %. In contrast, the breaking elongation of POM was increased by over 270 %.
It can be concluded that the polymers HNBR, FKM, PA6, PE and PVC are resistant in 1-year aged B20 whereas ACM and POM are limited resistant. PUR is not re-sistant.
HNBR, FKM, PA6, PE and PVC are resistant in 8-year aged B10, whereas PUR and POM are not resistant, and ACM just limited resistant.
Radioaktive Stoffe in besonderer Form (SFRM) sind nicht dispergierbare feste radioaktive Stoffe oder dichte Kapseln, die radioaktive Stoffe enthalten /1/. SFRM sind eine Kategorie innerhalb der verkehrsrechtlichen Vorschriften. Für die Beförderung zu Anwendern in der Industrie, Medizin und Forschung werden umschlossene radioaktive Stoffe (Strahler) gemäß ihrem aktivitätsabhängigen Gefahrenpotenzial verpackt. Strahler mit einer hohen Aktivität (> A2) erfordern entsprechend der verkehrsrechtlichen Vorschriften eine Beförderung in Typ B (U) Versandstücken, die als unfallsicher gelten. Alternativ besteht bis zu einer Aktivität < A1 die Möglichkeit der Beförderung in nicht unfallsicheren Typ A Versandstücken, wenn die Strahler nachweislich unfallsicher ausgelegt sind und eine Zulassung als SFRM vorliegt.
Die Bundesanstalt für Materialforschung und –prüfung (BAM) ist gemäß GGVSEB §8 (2) /2/ in Deutschland die zuständige Behörde für die Prüfung und Zulassung radioaktiver Stoffe in besonderer Form.
The image designed by Natalia Cano Murillo and colleagues shows the cross section of a ternary composite (boehmite/polycarbonate/epoxy, 80μm x 80μm). The surface was measured by AFM kelvin probe microscopy, yielding the surface potential which is shown as 3D‐surface and contour lines. The sample was further subjected to AFM force spectroscopy with a lateral resolution of 1μm², yielding the local Young's modulus, projected in false colors on the 3D surface. The ternary system, containing boehmite nanoparticles, shows a broad distribution of modulus, desirable for optimized macroscopic mechanical properties, such as high stiffness as well as toughness.
Fracture mechanics is a key to fatigue assessment in AM metal components. Short fatigue cracks are initiated at defects and pronounced surface roughness intrinsic to AM. The subsequent crack-propagation is strongly influenced by microstructural interactions and the build-up of crack-closure. The aim of the present study is to give an insight into short-crack propagation in AM-metals. Fatigue crack propagation resistance curves were determined experimentally for AISI 316L manufactured by Laser Powder Bed Fusion (L-PBF) which was heat treated at three different temperatures. Differences in the build-up of the fatigue-crack propagation threshold in between the L-PBF specimens and compared to wrought material are due to the residual stress states, a pronounced roughness of the crack-faces in the L-PBF specimens and phase transformation in the vicinity of the crack-tip, resulting in increased crack-closure. This, together with crack-branching found along the crack path, enhances the resistance to the propagation of fatigue cracks.
The effect of two types of scanning strategies on the grain structure and build-up of Residual Stress (RS) has been investigated in an as-built IN718 alloy produced by Laser Powder Bed Fusion (LPBF). The RS state has been investigated by X-ray diffraction techniques. The microstructural characterization was performed principally by Electron Backscatter Diffraction (EBSD), where the application of a post-measurement refinement technique enables small misorientations (< 2°) to be resolved. Kernel average misorientation (KAM) distributions indicate that preferably oriented columnar grains contain higher levels of misorientation, when compared to elongated grains with lower texture. The KAM distributions combined with X-ray diffraction stress maps infer that the increased misorientation is induced via plastic deformation driven by the thermal stresses, acting to self-relieve stress. The possibility of obtaining lower RS states in the build direction as a consequence of the influence of the microstructure should be considered when envisaging scanning strategies aimed at the mitigation of RS.
Thermography is one on the most promising techniques for in-situ monitoring of metal additive manufacturing processes. Especially in laser powder bed fusion processes, the high process dynamics and the strong focus of the laser beam cause a very complex thermal history within the produced specimens, such as multiple heating cycles within single layer expositions. This complicates data interpretation, e.g., in terms of cooling rates. A quantity that is easily calculated is the time a specific area of the specimen is at a temperature above a chosen threshold value (TOT). Here, we discuss variations occurring in time-over-threshold-maps during manufacturing of an almost defect free cuboid specimen.
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.
L-Lactide was polymerized with tin(II)acetate, tin(II)2-ethyl hexanoate, diphenyltin dichloride and dibutyltin bis(pentafluorophenoxide) at 130 °C in bulk. When an alcohol was added as initiator, linear chains free of cycles were formed having a degree of polymerization (DP) according to the lactide/initiator (LA/In) ratio.
Analogous polymerizations in the absence of an initiator yielded high molar mass cyclic polylactides.
Quite similar results were obtained when ε-caprolactone was polymerized with or without initiator.
Several transesterification experiments were conducted at 130 °C, either with polylactide or poly(ε-caprolactone) indicating that several transesterification mechanisms are operating under conditions that do not include formation of cycles by back-biting. Furthermore, reversible polycondensations (revPOCs) with low or moderate conversions were found that did not involve any kind of cyclization. Therefore, These results demonstrate the existence of revPOCs, which do neither obey the theory of irreversible polycondensation as defined by Flory nor the hypothesis of revPOCs as defined by Jacobson and Stockmayer. A new concept encompassing any kind of revPOCs is formulated in the form of a “polycondensation triangle”.
This presentation deals with the influence of the counterface materials on the sliding behaviour of some polymer materials in hydrogen. Polyimide (PI), polyetheretherketone (PEEK) and Polytetrafluoroethylene (PTFE) materials were investigated against hardened 52100 martensitic bearing steel and 304 austenitic stainless steel with similar roughness (Ra = 0.2 μm). Results indicate that the friction and wear of PI and PEEK materials depend on the counterface material. This effect wasn’t observed for PTFE composites.
While the tribological performance of polyimide is better against 52100 in hydrogen, improved sliding behaviour of PEEK materials is observed with 304 counterface, particularly at higher sliding speed. Surface analyses of the transfer film reveal that the influence of the counterface is primarily related to the chemical nature of the steel for PI and to the thermal conductivity of the disc for PEEK materials.
The crack propagation rate of environmental stress cracking was studied on high-density polyethylene compact tension specimens under static loading. Selected environmental liquids are distilled water, 2 wt% aqueous Arkopal N100 solution, and two model liquid mixtures, one based on solvents and one on detergents, representing stress cracking test liquids for commercial crop protection products. The different surface tensions and solubilities, which affect the energetic facilitation of void nucleation and craze development, are studied. Crack growth in surface-active media is strongly accelerated as the solvents induce plasticization, followed by strong blunting significantly retarding both crack initiation and crack propagation. The crack propagation rate for static load as a function of the stress intensity factor within all environments is found to follow the Paris–Erdogan law. Scanning electron micrographs of the fracture surface highlight more pronounced structures with both extensive degrees of plasticization and reduced crack propagation rate, addressing the distinct creep behavior of fibrils. Additionally, the limitations of linear elastic fracture mechanisms for visco-elastic polymers exposed to environmental liquids are discussed.
Colours, nano and surface
(2022)
The basic ideas of colours and pigments are presented. The correlation between nanomaterials and colours are explained. Different methods are presented for investigating nanoparticles and their surface. At the end a case study is presented explaining the importance of coating for the properties of nanoparticles.
Thin polymer films are of vital importance due to their low production costs and wide range of applications in sensors, electronics, and coatings. Their geometry is ideal for the study of confinement effects, specifically one-dimensional confinement, on the thermodynamic properties and segmental dynamics of polymers. For this investigation, films of PC are prepared on both glass and silica substrates to measure the dielectric and calorimetric behavior as a function of film thickness. The methodology consists of broadband dielectric spectroscopy (BDS), ellipsometry, and atomic force microscopy (AFM). Using ellipsometry, the glass transition shows an increase with decreasing film thickness. Compared to a previous investigation of PC where dilatometry was used, an increase in PC was seen, but now only at thicknesses below 20 nm. Therefore, the critical thickness of PC, where the bulk-like layer no longer percolates through the film, is dependent on the method probing the glass transition. The dielectric behavior shows a deviation from bulk behavior with decreasing film thickness, although still showing a Vogel-Fulcher-Tammann (VFT) temperature dependence for all films. The influence of the adsorbed layer on the molecular mobility was also addressed.
In this paper, we demonstrate the value of 1H NMR relaxometry for studying the hydration of clinker-reduced, more climate-friendly cementitious binders. The results were obtained on typical CEM I cements and sister samples containing two different reactive agricultural ashes as well as non-reactive biochars as supplementary cementitious materials. The findings prove that time-resolved NMR measurements provide valuable additional information when combined with classical heat flow calorimetry.
We introduce a novel adaptive Gaussian Process Regression (GPR) methodology for efficient construction of surrogate models for Bayesian inverse problems with expensive forward model evaluations. An adaptive design strategy focuses on optimizing both the positioning and simulation accuracy of training data in order to reduce the computational cost of simulating training data without compromising the fidelity of the posterior distributions of parameters. The method interleaves a goal-oriented active learning algorithm selecting evaluation points and tolerances based on the expected impact on the Kullback-Leibler divergence of surrogated and true posterior with a Markov Chain Monte Carlo sampling of the posterior. The performance benefit of the adaptive approach is demonstrated for two simple test problems.