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- UCST polymers (1)
- UCST-type polymer (1)
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- Ultrasonic Testing (1)
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- Upconversion nanoparticles (1)
- Upconverting nanoparticles (1)
- VM12 SHC (1)
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- Verbundwerkstoffe (1)
- Vereinfachtes Verfahren (1)
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- Volatile organic compounds (1)
- WIG-Blindschweißnaht (1)
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- Wasseraufbereitung (1)
- Wasserstoffpermeation (1)
- Waste heat recovery (1)
- Water/alcohol mixtures (1)
- Wave propagation (1)
- Weld Joint (1)
- Wellenprüfung (1)
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- X-Ray Diffraction (1)
- X-ray Computed Tomography (1)
- X-ray Diffraction (1)
- X-ray computer tomography (1)
- X-ray diffractometry (1)
- X-ray imaging (1)
- X-ray interferometry (1)
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- X-ry Diffraction (1)
- XAS (1)
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- Young´s modulus (1)
- Zahnmedizin (1)
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- Zement (1)
- Zementgebundene Baustoffe (1)
- Zentrifugentechnologie (1)
- Zeolite (1)
- Zersetzungsgasanalyse (1)
- Zerstörungsfreie Prüfung (1)
- Zinc and galvanized samples (1)
- Zirconium (1)
- ZnSe (1)
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- Zünder (1)
- additive manufacturing (1)
- aggregation-induced dual emission (AIDE) (1)
- bioimaging (1)
- burst test (1)
- cocrystal (1)
- creep behaviour (1)
- dangerous goods packagings (1)
- excess isotherms (1)
- excitation power density (1)
- extreme temperature (1)
- gas adsorption (1)
- gas solubility (1)
- high-resolution camera (1)
- hybrid repair (1)
- ionic liquids (1)
- life cycle test (1)
- low energy electrons (1)
- mechanochemistry (1)
- milling (1)
- pH probe (1)
- pH sensing (1)
- polyethylene terephthalate (1)
- porous solids (1)
- position detection (1)
- powder bed fusion of metals utilizing a laser beam (1)
- ssDNA (1)
- stress cracking resistance (1)
- test methods (1)
- µ-XRF (1)
- µCT (1)
- Örtliche Korrosion (1)
- β-cristobalite structure type (1)
Organisationseinheit der BAM
- 6 Materialchemie (196)
- 5 Werkstofftechnik (94)
- 8 Zerstörungsfreie Prüfung (90)
- 6.3 Strukturanalytik (65)
- 8.5 Röntgenbildgebung (60)
- 9 Komponentensicherheit (52)
- 6.6 Physik und chemische Analytik der Polymere (51)
- 1 Analytische Chemie; Referenzmaterialien (43)
- 6.1 Oberflächen- und Dünnschichtanalyse (39)
- 4 Material und Umwelt (36)
- einer der größten zusammenhängenden Gebäudekomplexe in Europa
- Anfang der dreißiger Jahre von Prof. Sagebiel geplant, 1936 Baubeginn, heute zu 70%fertiggestellt
- steht heute wegen großer verkehrs- und baugeschichtlicher Bedeutung unter Denkmalschutz
- in Abfertigungshalle befindliche Fachwerkträger mit selbsttätiger Vorspannung zeigen Anfang des Spannbetonbaus
- ab 1997 Überarbeitung des Nutzungskonzeptes der Räume über den Fachwerkträgern durch Berliner Flughafengesellschaft
- Erfordernis der Abschätzung der Tragfähigkeit der Fachwerkträger
Kiefernholz wird durch Imprägnieren mit einem Vorkondensat aus organischen Disäuren und Glycerin, das kolloidale Kieselsäure enthält, sowie nachfolgende Ofenhärtung in Kieselsäure/Alkydharz/Holz-Verbunde umgewandelt. Diese Nanoverbunde haben eine geringere Porosität als Holz, da Teile der Holzzellen mit Harz und Kieselsäure ausgefüllt sind. Die kugelförmigen, etwa 60 nm großen (SiO1)x-Teilchen liegen in der Polymermatrix mikrophasensepariert vor. Der kolloidale Zustand der eingebrachten Polykieselsäure bleibt erhalten. Durch ihr günstiges Eigenschaftsprofil sind die Verbundmaterialien als modifizierter Holzbaustoff interessant.
Recyclingzuschläge (rezyklierte Gesteinskörnungen, Betonsplitt) werden großtechnisch aus dem Material, das beim Abbruch von Betonbauwerken anfällt, hergestellt. Sie bestehen zu mehr als 90% aus Altbeton. Die Wiederverwendung dieser Materialien zur Herstellung von neuen hochwertigen Beton erfordert umfangreiche Kenntnisse über ihre betontechnologischen und chemisch-physikalischen Eigenschaften. Zwei unterschiedliche Recyclingzuschläge und die damit hergestellten Betone wurden im Vergleich zu einem Referenzbeton mit natürlichen Zuschlägen gleicher Sieblinie untersucht.
Der Filterschlamm (FS) fällt als Reststoff bei der Abwasserbehandlung des Chemiewerkes an. Er liegt als feinteiliges Granulat vor und enthält als Hauptbestandteil amorphe Kieselsäure. Damit eröffnet sich die Möglichkeit, ihn wie einen mineralischen Zusatzstoff bei der Beton- und Mörtelherstellung zu verwenden.
Als Betonzusatzstoff werden fein aufgeteilte Zusätze zum Beton bezeichnet, die durch chemische und/oder physikalische Wirkung die Betoneigenschaften beeinflussen, und die als Stoffraumkomponente zu berücksichtigen sind.
Hochfeste Betone werden durch die Zugabe puzzolanischer Zusatzstoffe (Microsilica, Flugasche) und die Reduzierung des Wasser-Zement-Wertes bei gleichzeitiger Verwendung eines Fließmittels hergestellt. Diese Modifizierungen des Betons beeinflußen die Zusammensetzung und die Mikrostruktur seiner Mörtelmatrix.
Zur Planung und Durchführung umfangreicher Sanierungs- und Umbaumaßnahmen im Pergamon-Museum Berlin bestand die Erfordernis einer Bauzustandsanalyse an antiken Baudenkmälern. Bestandsunterlagen waren unvollständig vorhanden bzw. fehlten. Hieraus ergab sich die Notwendigkeit des kombinierten Einsatzes zerstörungsfreier
Prüftechnik.
Die Regelwerke (RL SIB, ZTV-ING) setzen für die Instandsetzung mit Betoninstandsetzungssystemen vergleichsweise hochwertige Betonuntergründe voraus. Speziell bei älterenWasserbauwerken sind oftmals nur geringerfeste Betonuntergründe vorhanden für die es bis jetzt keine geeigneten und geprüften Instandsetzungssysteme gab. Grundlage für die Entwicklung solcher Systeme sind entsprechende Referenzbetone als Untergrundbeton für die Verbundkörperprüfung.
Ziel der Untersuchungen war es, herauszufinden ob die Druckfestigkeit hochfester Betone zerstörungsfrei mit dem Rückprallhammer PROCEQEQUOSCHMIDT durch Ermittlung des klassischen Rückprallwerts R in Kombination, mit einem aus der Untersuchung von Metallen bekannten neuen Messwert L mit ausreichender Sicherheit beschrieben werden kann.
Im Rahmen von MICROCON, einem europäischen CRAFT-Projekt,
besteht eine wesentliche Zielsetzung in der Optimierung von selbstverdichtendem Beton (SVB) im Hinblick auf Kosten und Leistungsfähigkeit durch den Einsatz von teilweise puzzolanischen Microfillern. Um die Puzzolanität bei der Beurteilung besser bewerten zu können, wird ein Referenzbeton benötigt, der aus weitestgehend inerten Zusatzstoffen besteht. Die Entwicklung eines solchen Referenzbetons fand an der BAM nach der japanischen Methode nach Okamura statt.
Im Rahmen eines DFG-Forschungsvorhabens (FOR 537) wird ein Teilprojekt an der BAM bearbeitet. Ziel dieser Arbeit ist die quantitative Beschreibung und Bewertung des Korrosionsfortschrittes an Stahlproben mit kleinen Kathodenflächen (Eigenkorrosion) mittels elektrochemischer Messungen. Für die Untersuchungen wurden Betonproben mit eingebetteten Stahlelektroden hergestellt. Dabei wurden gezielt betontechnologische Parameter variiert. Dabei ist der Beton als Elektrolyt zu betrachten. Nach bestimmten Zeitintervallen werden die Betonproben aufgebrochen und die eingebetteten Stahlelektroden durch visuelle Inspektion und anschließende Bestimmung des Masseverlustes bewertet. Zur Charakterisierung des Betons (Elektrolyt) dient das Verfahren der Quecksilberporosimetrie. Mit dem Verfahren lassen sich die Zusammenhänge zwischen den betontechnologischen Parametern und der Porenstruktur aufzeigen und mittels der umfangreichen Variation der Betonparameter die Auswirkung auf den Korrosionsfortschritt nachweisen.
Ultrahochfeste Betone (UHPC) sind durch Druckfestigkeiten > 150 MPa und eine besonders hohe Dauerhaftigkeit gekennzeichnet. Ihre Herstellung gelingt durch die Optimierung der Mischungszusammensetzung, des Mischprozesses und der Nachbehandlung. Maßnahmen dazu bestehen in der Verwendung feinstgemahlener Zemente, puzzolanischer und inerter Feinststoffe, dem Einsatz gezielt ausgewählter grober und feiner Gesteinskörnungen, der Reduktion des Wasser/Bindemittel-Wertes bei Zugabe von Fließmitteln auf Polycarboxylat-Basis sowie einer Wärmebehandlung der Betone.
Das Ziel dabei ist es, eine möglichst hohe Packungsdichte in der Bindemittelmatrix bei Ausbildung einer sehr gleichmäßigen und extrem dichten Gefügestruktur mit einem hohen Anteil an Calciumsilicathydrat-Phasen zu erreichen. Deshalb sind Untersuchungen zur Porosität und Porenstruktur ein wichtiger Bestandteil zur Materialcharakterisierung im Rahmen der Mischungsoptimierung. Die Ergebnisse der Mikrostrukturuntersuchungen werden im Vergleich zu denen an einem hochfesten Beton und einem Normalbeton betrachtet.
Hausmüllverbrennungsasche soll aufgrund ihrer chemisch-mineralogischen Eigenschaften als Gesteinskörnung zur Herstellung von Normalbetonen eingesetzt werden. Durch Bestandteile, wie Chloride, metallisches Aluminium und Altglasfragmente, entstehen aber in kürzester Zeit beträchtliche Betonschäden. Durch zusätzliche mechanische, chemische oder thermische Aufbereitungsschritte können diese betonschädigenden Inhaltsstoffe minimiert werden. Dadurch lässt sich die Qualität der Asche soweit verbessern, dass sie gut zur Betonherstellung verwendbar ist.
Modern municipal solid waste incinerator plants produce bottom ashes, which are used in building industry, especially as base course in road constructions. Because of a highly sophisticated reprocessing technique, the ashes Show a relatively stable composition, comparatively well defined properties and environmentally relevant Parameters below legal Limits. Due to its chemical and mineralogical characteristics, the bottom ash can in principle be used as Aggregate in the production of normal strength concrete. However, if the ash contains concrete damaging components Recycling becomes problematic.
To assess the use of municipal solid waste incinerator bottom ash (MSWI bottom ash) as Aggregate in concrete, different additionally treated ashes were chemical and physical characterised. Furthermore, concrete specimens with bottom ash as aggregates were produced and their Engineering properties were studied.
Holzschutzmittel gegen den biologischen Angriff von Insekten, Pilzen und Bakterien besitzen eine erhebliche volkswirtschaftliche Bedeutung. Zur Vermeidung einer in der DIN EN 252 beschriebenen rein visuellen Beurteilung wurde 1996 durch die BAM auf Grundlage des in der DIN 52186 enthaltenen Biegeversuchs eine alternative Strategie vorgeschlagen. In weiterführenden Untersuchungen soll ergänzend zur Prüfmaschine die Stereo-Fotogrammetrie als optisches 3D-Messverfahren eingesetzt werden. Die Entwicklung eines möglichst objektiven und technisch einfachen Nachweisverfahrens der Schutzwirkung und die vergleichende Bewertung der Aussagekraft beider Normen sind von besonderem Interesse.
Inorganic-organic nanocomposites are synthesised from polyethylene glycol with an average molar mass of 600 g/mol containing colloidal silica (silicic acid) and diphenyl methane diisocyanate as compact and foamed materials according to the European patent EP1414880. Beside the macroscopic properties, the pore structure and the structure of the polymer matrix of the silica/polyurethane nanocomposites with varying silica contents were studied.
Ultra-high performance concrete (UHPC) is characterised by compressive strengths above 150 MPa and an outstanding durability. These properties are achieved by optimisation of the mixture composition, the mixing procedure as well as the curing conditions of the concrete. Heat curing as well as the use of vacuum mixers may contribute to the high strength. The very high brittleness of UHPC can be compensated by the addition of steel or polymer fibres.
UHPC is produced using a very low water/cement ratio of 0.25 or smaller in combination with adding of polycarboxylate ether based superplasticisers. Furthermore, finest cements with contents of 500 kg/m³, defined selections of coarse and fine aggregates with a maximum grain size between 0.5 and 8 mm and fine pozzolanic (silica fume, fly ash) and inert additives (quartz filler) are used. In doing so, the aim is to obtain a very high packing density of the cement paste matrix and the aggregate/paste interface while a very homogeneous microstructure with a high calcium silicate hydrate (CSH) portion is formed.
In the case of optimal mixing and curing conditions, UHPC contains almost no pores and microcracks. Therefore, studies of porosity and pore structure are very important to characterise UHPC materials in connection with the mixture optimisation. Here, the experimental results for UHPC are presented in comparison with those of high-strength concrete (100 MPa) and normal-strength concrete (35 MPa), respectively.
Processed building rubble containing about 90 % of crushed concrete can be used as recycling aggregates. The reuse for the production of new high-grade concrete requires a knowledge of the engineering properties as well as the pore structure of These materials. Two recycling aggregates and the concretes made with them were studied.
Im Hinblick auf eine nachhaltige Entwicklung sollen nach dem KrW/AbfG der Rohstoffeintrag und der Abfallaustrag in den Lebensphasen eines Bauwerks durch weitgehende Verwertung von Sekundärrohstoffen (Reststoffen) möglichst gering gehalten werden. Ein Einsatz von Reststoffen wie Hausmüllverbrennungsaschen (MV-Aschen) im Betonbau kann potenziell einen wesentlichen Beitrag zur nachhaltigen Entwicklung leisten.
Um den Abbau primärer Rohstoffe zu reduzieren, wurden deponierte oder niederwertig eingesetzte industrielle Reststoffe hinsichtlich einer höherwertigen Verwendung im Betonbau untersucht. Zur Bewertung des Einsatzpotentials als Zementbestandteil oder Betonzusatzstoff erfolgte zunächst eine chemisch-mineralogische und betontechnologische Charakterisierung der Materialien. Reststoffe, die die normativen Anforderungen hinsichtlich der Zementzusammensetzung erfüllen, wurden anschließend zu verschiedenen Anteilen als Zementsubstitut in Mörtel eingesetzt. In vergleichenden Untersuchungen erfolgte die Ermittlung der Frisch- und Festmörteleigenschaften.
Kalorimetrische Untersuchungen sollten die Auswirkungen der Reststoffe auf die Zementhydratation zeigen. Ausgewählte Untersuchungsergebnisse an Reststoffen aus der Industrieabwasseraufbereitung, dem Altpapierrecycling, der Biomasseverbrennung und der Metallurgie werden vorgestellt.
Modern CO2-reduced power plants with Oxyfuel-Combustion operate with gas compositions of high CO2 partial pressure and steam (Boiler, Recycling). The corrosion process occurring under such service conditions is different from that under current conditions with air combustion. The effect of temperature, pressure, chromium content on the corrosion reaction of typical power plant steels in CO2 -H2O and CO-H2O-O2 was investigated.
Im Hinblick auf eine nachhaltige Entwicklung sollen nach dem KrW/AbfG der Rohstoffeintrag und der Abfallaustrag in den Lebensphasen eines Bauwerks durch weitgehende Verwertung von Sekundärrohstoffen (Reststoffen) möglichst gering gehalten werden. Ein Einsatz von Reststoffen wie Hausmüllverbrennungsaschen (MV-Aschen) im Betonbau kann potenziell einen wesentlichen Beitrag zur nachhaltigen
Entwicklung leisten.
For the characterization of disperse and porous solids, usually single gas adsorption(GA) is employed. In the case of liquid adsorption (LA), the extraction of information on solids immediately becomes a more sophisticated matter since information on geometric as well energetic parameters of the solids is both superposed by liquid-mixture effects and displayed in excess terms. We have to ask if reliable solid parameters can be also obtained from LA isotherms. The enlarged data bank of gas and liquid adsorption measurements enables us to change systematically solid parameters (e.g., the pore width of MCM-41, the pore entrances of SBA-16, chemical heterogeneity) and to study in this way the influence of solid parameters on LA.
Beim bispektralen Verfahrensprinzip (auch 2-Monochromatoren-Methode genannt) zur Charakterisierung fluoreszierender Reflexionsproben wird das Probenmaterial monochromatisch bestrahlt und für jede dieser anregenden Wellenlängen das emittierte Spektrum monochromatisch gemessen. Dies hat gegenüber einer polychromatischen Anregung (z. B. Normlichtart D65) den Vorteil, dass spektrale Materialfunktionen (Gesamt-, Reflexions- und Lumineszenz-Strahldichtefaktoren sowie das Lumineszenz-Anregungsspektrum) und diverse Farbmaßzahlen (Sicherheits- und Kontrastfarben; Referenzmaterial) für beliebige Anregungsspektren (Normlichtarten) bestimmt werden können.
Untersucht wurde der Einfluss der Applikationsart (konventionelle und gespritzte Herstellung, Wasserlagerung bis zur Prüfung), der Einfluss von Fasern (konventionelle Herstellung, Wasserlagerung bis zur Prüfung) und der Einfluss von Schwindreduzierern (konventionelle Herstellung, Luftlagerung bis zur Prüfung).
Untersucht wird die Entwicklung einer Technologie zur Herstellung hochwertiger Leichtgranulate (Blähgranulate) mit definierten Produkteigenschaften aus heterogenen Bau- und Abbruchabfällen, Anwendung der Granulate als leichte Gesteinskörnung im Beton und die Möglichkeit des rohstofflichen Recyclings mineralischer Bauabfälle
Worldwide, cement and concrete experts are at the cutting-edge to sustainable, green, healthy but nonetheless high-Performance concrete. The current relatively low development of the cement and concrete industry in Africa offers the unique opportunity to start directly on the best achievable and sustainable Level, if only Expertise is sufficiently available. It should not be neglected that concrete is a product with comparably low Transport ranges, which means that an improved concrete market will mainly Support the local economy without exceeding financial Drains to the international market, thus fostering the fight against poverty, which is an urgent Need in most African countries.
- 5.000 bis 10.000 t wasserhaltiger Filterrückstand (FR) entstehen jährlich pro Produzent bei der Neutralisation der Abwässer aus der Silicon- oder Kieselsäureherstellung
- Anfall als fester, feuchter, schollenartiger Filterkuchen
- Verwertung heute: Deponierung, Tagebauverfüllung -> ungenutzte Sekundärrohstoffquelle
- Untersuchung der Einsatzmöglichkeiten der aufbereiteten Filterrückstände zur Eigenschaftsverbesserung
zementgebundener Baustoffe analog der wohlbekannten Anwendung von hochdisperser Kieselsäure und Silicastaub
- Zunehmender Energiebedarf erfordert höhere Übertragungskapazitäten
- Dezentrale ökologische Energiegewinnung, z. B. Offshore, erfordert Übertragung großer Energiemengen in die Ballungszentren (Nord-Süd-Trassen)
- Hohe Auslastung der Netze erfordert Beherrschbarkeit der im Fehlerfall auftretenden Risiken für Menschen, Umwelt und energietechnische Anlagen
- Etwa 90 % der Anlagenausfälle sind verursacht durch Teilentladungen (TE) in Endverschlüssen und Muffen mit modernen polymeren Isoliersystemen
- Etablierte elektrische Verfahren erlauben nur externe Schadensdetektion.
Die Fixierung der Stahlanker im Felsfundament zur Stabilisierung der Schwergewichtsmauer werden mit integrierten faseroptischen Dehnungssensoren überwacht.
In die Glasfaser sind Reflektoren eingebaut; zwei Reflektoren bilden jeweils eine Messstrecke, die Auskunft über die Fixierung geben. Am Ankerkopf wird der Zustand der Messstrecken abgefragt.
- jährlicher Anfall von 5.000 bzw. 10.000 Tonnen
wasserhaltiger Filterrückstände (FR) pro Produzent bei
der Abwasser-Neutralisation aus der Kieselsäure- bzw.
Chlorsilanherstellung (FR1, FR2)
- heute: Deponierung, Tagebauverfüllung
- ungenutzte Sekundärrohstoffquelle
- Untersuchung möglicher Anwendungsbereiche für FR
Leichte Gesteinskörnungen mit Kornrohdichten < 2 g/cm³ werden industriell aus natürlichen Rohstoffen, wie Ton und Schiefer, hergestellt. Dabei fallen hohe Energiekosten an, während außerdem fortwährend die Verfügbarkeit geeigneter Rohstoffe sinkt. Eine Alternative stellen Leichtgranulate, die aus mineralischen Bau- und Abbruchabfällen hergestellt werden, dar.
Im Forschungsprojekt „Aufbaukörnungen“ wurde eine Technologie zur Herstellung hochwertiger leichter Gesteinskörnungen aus Mauerwerkbruch entwickelt. Ziegelhaltige Bau- und Abbruchabfälle fallen in Deutschland mit bis zu 26 Mio. t pro Jahr an und weisen größere Verwertungsdefizite als Betonbruch auf. Der neuen Verwertungsstrategie liegt die Idee des rohstofflichen Recyclings zu Grunde.
Die leichten Gesteinskörnungen werden am Ende eines mehrstufigen Herstellungsprozesses durch thermische oder hydrothermale Erhärtung im Labor- und halbtechnischen Maßstab produziert. Für Herstellungstechnologie und Eigenschaften der Leichtbetone sind neben Kornfestigkeit und Rohdichte die Porosität und Wasseraufnahme der leichten Gesteinskörnungen entscheidende Größen, die wiederum von Kornform, Oberflächenrauigkeit, Sinterschale und Porenstruktur der Körnungen beeinflusst werden.
Ionic Liquids (ILs) are employed in various fields, for example, reaction engineering (reactions with gases, such as hydroformylation (CO, H2), hydrogenation (H2), oxidation (O2)) or separation technology (separations of gases, reactants, and high-volatility reaction products). For the basic engineering of such processes, knowledge of phase equilibria, particularly of mixtures, over a broad (p,T) range is mandatory. This contribution reports on recent experimental results from our laboratory: – for the simultaneous solubility of a binary gas mixture in a pure ionic liquid – for the solubility of a single gas in a binary liquid solvent mixture.
Das Hochtemperatur-Laserprofilometer der BAM4 ermöglicht eine 3D-Formerkennung an keramischen Folien oder anderen flachen Objekten während thermischer Behandlungen wie zum Beispiel bei laufenden Entbinderungs- oder Sinterprozessen. Mit dem Lasertriangulationssensor werden das Höhenprofil, die lateralen und axialen Schwindungen und andere charakteristische Maße der Probe wie die Folienbreite und -dicke, Abstände zwischen spezifischen Merkmalen oder Krümmungen bestimmt. Somit können insbesondere auch Deformationen und Verwerfungen der Objekte sowie Schwindungsinhomogenitäten an strukturierten Objekten erkannt und mit dem Herstellungsprozess verknüpft werden.
The term „Alternative Solvents“ often refers to ionic liquids (ILs), mainly to distinguish these substances from traditional (i.e., molecular) solvents.
In applications, any „alternative“ is required to perform better than something that is proven and tested.
To bring ILs into practical use, availability and costs are the fundamental points to be addressed.
There are two ways to proceed:
▬ tailoring a molecule, implanting the expected characteristics
advantage: optimization of the targeted performance possible
risks: outcome not always foreseeable, costly and time-intensive (“trial and error“)
▬ to target on mixtures of well-characterized ILs with molecular solvents
advantage: substance characteristics are known, less costly, less time-consuming,
mixture composition another tunable parameter
risks: the same but with less impact
For the basic engineering of technical processes, knowledge of phase equilibria, particularly of
mixtures, over a broad (p,T) range is mandatory.
This contribution reports on recent experimental results from our laboratory:
▬ the solubility of CO2 in a mixture of water and [bmim][CH3SO4]
▬ the solubility of CO2 in a mixture of methanol and [bmim][PF6]
As subcritical crack growth (SCCG) can reduce tensile strength of glasses by many orders of magnitude, the potential for improvement of fatigue behaviour is most intriguing in developing ultra-strong glasses. An essential bottleneck is the basic understanding of the numerous interplaying pressure-, temperature- and water-affected relaxation phenomena at the crack tip and related toughening strategies. Therefore, the present project aims to advance the basic understanding of structural relaxation effects and local properties caused by increased water concentration and tensile stresses at the crack tip as they are a key for structural toughening designs to develop SCCG-free glasses and glass surfaces.
Our first studies give clear evidence that glass structure and dynamics is strongly modified upon hydration of glasses. These changes are highly related to the nature of network formers but are affected as well by the counter ions (network modifier). Results of the 1st project part suggest that structural relaxation below glass transition temperature, i.e. overlapping of short-range (beta) and long-range (alpha) interactions can contribute to SCCG in water-free environments and that structurally dissolved water in the glasses can have decisive impact on this effect.
In the 2nd project stage specific glasses compositions will be investigated to gain an improved understanding on the relation of sub-Tg relaxation and inert SCCG as well as to shed light to the related effects of dissolved water and its speciation. These glasses cover a broader range of different glass topologies and binding partners, whereby the coupling of alpha and beta relaxations is varied systematically by alkali-, alkaline earth ions and water species concentrations. Preparation of hydrous glasses (up to 8 wt% water) will be performed by high pressure syntheses. Structure will be resolved by NMR, Raman and IR spectroscopy while structural relaxation is accessed in the temperature and frequency domain using dynamic mechanical spectroscopy and ultrasonic damping. We will focus on measurements of inert SCCG (region III) conducting experiments in vacuum and dry gas atmospheres using indentation techniques and stressing of glass specimens in DCB geometry.
Experimental data on SCCG will be provided to SPP groups, which deals with fatigue in metallic glasses and vice versa we will test theoretical predictions of ab-initio simulations of partner within SPP 1594 in order to quantify the effect of water on the crack tip. In summa topological factors controlling the subcritical crack growth with respect to water will be identified from which structural toughening designs for highly fatigue resistant-glasses can be derived.
Bioglass® 45S5 is mainly used clinically as powders, granules or pastes instead of sintered compacts. This is due to the inherent problem of crystallization during the sintering, which results in poor mechanical properties and reduced bioactivity. Recently, new bioactive glasses with improved crystallization stability have been developed as promising candidates for manufacturing of sintered powder compacts for bone regeneration, which combine improved sintering behavior with bioactivity. Compared with the well-known Bioglass® 45S5 (SiO2-P2O5-CaO-Na2O) the calcium/alkali oxide ratio was increased, sodium oxide was partially replaced by potassium oxide and up to 3 mol% calcium fluoride were added, in order to stabilize the glass against crystallization. The aim of this study was to investigate the sintering and crystallization behavior of these new bioactive glasses.
Sintering and crystallization were characterized by heating microscopy, XRD, FTIR, SEM, and DTA. The results show that a sintered density of 88-99 % is achieved in contrast to only 57-67% for Bioglass® 45S5. In addition, FTIR and XRD analyses show that Bioglass® 45S5 crystallized during sintering while for the new glasses no crystalline phases are detected. The thermal properties of all glasses were studied by DTA measurements, and the influence of grain size was characterized. These studies showed that full densification can be attained for particle size < 32 µm, whereas coarser particles progressively increase residual porosity. Observed foaming phenomena, are strongly retarded by crystallization of beta-HAp.
Nowadays, the use of bioactive glasses is established for bone regeneration; however glasses are used mostly as powders, granules or in a paste. Sintered scaffolds are not used clinically, because of the in inherent problem of crystallization during the sintering process, resulting in poor mechanical properties and reduced bioactivity. The aim of this study was therefore to design new bioactive glasses, which combine improved processing and sintering with bioactivity.
Compared with the well-known Bioglass® 45S5 (SiO2-P2O5-CaO-Na2O) the calcium/alkalioxide ratio was increased, sodiumoxide was partially replaced by potassiumoxide and up to 8 mol% calciumflorid were added, in order to stabilize the glass against crystallization.
The sintering behavior of the new glasses was characterized by heating microscopy and compared to Bioglass® 45S5. The results showed that the new glasses achieved a sintered density of 88-99 % in contrast to only 57-67% for Bioglass® 45S5. In addition FTIR and XRD analyses showed that Bioglass® 45S5 crystallized during sintering while for the new glasses no crystalline phases were detected. The thermal properties of all glasses were studied by DTA and DSC measures, and the influence of grain size and heating rate were characterized. These studies showed a shift of start and end temperature of sintering process as well as the final density. The structure of sintered specimens during and after sintering was examined using light and electron microscopy (REM).
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.
Optimizing the performance of phase gratings for better visibility in Talbot- Lau interferometry
(2015)
We investigated the efficiency of phase gratings, i.e., the visibility upon variation of different parameters. Rotating around an axis parallel to the grid lines of the phase grating changes the grating’s shape and thereby the initial distribution of phase shifts. This yields high visibilities for shorter propagation distances than derived from box shapes. Tilting the grating in the scattering plane allows continuous tuning of the grating’s height that corresponds to an ideal phase shift for a particular photon energy. This opens the way for tuning the design energy suitable for the material under investigation. Our study included simulations for monochromatic sources with the sampling procedure.
Mg-Y,RE-Zn systems present second phases with high thermal stability, promoting the increase of strength and creep resistance at high temperatures.
Mg and its alloys have a potential application as biomaterials due to their biocompatibility and degradation behaviour. The dominant corrosion mechanism in those alloys is the microgalvanic corrosion through coupling of the more noble second phases with the Mg matrix, and therefore a low concentration of those was sought.
Ultra High Performance Concrete (UHPC) is characterized by high strength and high durability. This is achieved by an optimized grain size distribution, especially within fine grains, and addition of superplasticizer, which allow the reduction of the water/cement ratio in the cement paste and thereby the increase of the density of UHPC. Thermal treatment, i.e. curing at elevated temperature and pressure, contributes to a further increase of compressive strength. The aim of the presented study was to analyze the effect of thermal treatment at 90 ◦C and atmospheric pressure on UHPC samples. Varying factors were the age of the samples when heat treatment started (initial storage time), the duration of heat treatment and the type of heat treatment. It was applied in three ways: 1. treated without any protection, 2. sealed in plastic foil and 3. treated in hot water. Afterwards the samples were analyzed with respect to their mechanical properties and their phase composition. Furthermore, the weight (water absorption) of the samples was observed over 28 days and was correlated with the strength test results. The development of strength depends on the combination of initial storage time and the duration of heat treatment and is also influenced by the type of thermal treatment. The highest compressive strengths have been observed by implementing the hot water treatment. Thereby the weight of the samples increase due to additional absorbed water. This enables an increased hydration of cement clinker inducing a higher strength.
Lightweight granules are mineral, spherical and porous particles with bulk density less than 2000 kg m . New types of lightweight granules are made from masonry -3 rubble as an alternative to the commonly used expanded clay and shale. They are produced in a multistage manufacturing process by thermal or hydrothermal treatment. Studies of the microstructure of the new lightweight granules are very important to optimise the engineering properties with regard to different applications from lightweight concrete to planting substrates and wastewater treatment. Here, the results of porosity and pore structure measurements are presented. Characteristic samples with different bulk densities of both thermally and hydrothermally hardened granules have been analysed by means of various methods.
Elastic wave propagation of ultrasound in bituminous road surfaces – simulations and measurements
(2015)
Maintenance costs of road infrastructure are increasing steadily. Adverse environmental impacts on infrastructure get more and more important as well. Therefore, it is important to determine how limited financial resources can be directed with an optimum pay-out. The present study takes first steps towards the usage of low-frequency ultrasound as a tool to evaluate the road condition.
The integration of finite element method (FEM) into the least-squares adjustment presented in is further extended for a joint evaluation of an elastostatic model and displacement field measurement. For linear solids which obey the Hooke's law, the material parameters determination from measurements is being examined.
High resolution in situ monitoring of the initial cement hydration influenced by organic admixtures
(2015)
Numerous admixtures are used in the building practice to customize the properties of the cement paste during application. The influences of admixtures on the course of cement hydration and formation of hydrate phases have to be considered. Polycarboxylate ether (PCE) based polymeric superplasticizers (SPs) are known to retard the setting of the cement paste. The extent of the retardation differs depending on the molecular structure of the SP. Additionally, the presence of a stabilizing agent (SA) in the cement paste has a retarding side effect on the setting. The initial cement hydration processes and the detailed mechanisms of the retardation influenced by PCEs, as well as their interactions with particular SAs, are insufficiently understood. Up to now, only the results of phenomenological studies were taken into account to describe this retardation process. A detailed structure analysis monitoring the change of the phase composition during the hydration was never applied. Both SP and SA affect the adsorption of the sulphate ions on the clinker particles, causing changes in the formation of ettringite during the initial hydration, and are therefore a crucial part of the setting process itself. Here, the initial hydration of cement influenced by the interaction of SP and SA was monitored in situ by synchrotron X-ray diffraction. The high time resolution of the measurements allowed a continuous detection of the hydrates formed. The hydration was followed from the starting point of water addition and for couple of hours afterwards. The hydration of the levitated cement pellets containing starch as SA was initialized by adding aqueous solutions of different commercial SPs. Changes in the ettringite formation were detected in comparison to the reference hydration of pure cement.
Combining CO2 Streams from Different Emitters – A Challenge For Transport And Storage Infrastructure
(2015)
The European Directive 2009/31/EC on the geological storage of CO2 envisages an open access of CO2 streams from different emitters to a nation- or even EUwide CO2 pipeline network if CO2 stream compositions meet “reasonable minimum composition thresholds”. As of today it is not known how such “composition thresholds” may be defined and which impurity levels may be viable in practical application.
To set up recommendations for criteria and respective threshold values for CO2 stream compositions, the project “CLUSTER” will investigate how a dynamic interplay – both in terms of mass fluxes and compositions – of CO2 streams from regionally clustered CO2 sources sharing a transport and storage infrastructure will impact corrosion, e.g., of pipelines and plant components, and geochemical alteration of cap rocks and reservoir rocks. In addition, the behaviour of such a highly dynamic CCS system will be considered for an overall optimization of system design including CO2 stream mixing schemes and facilities or interim CO2 storage.
Oxidation of a Fe-13Cr alloy under water vapor at 600 °C produced a zone of nano-sized precipitation underneath the outside scale formed by iron oxides and Fe‒Cr spinel. The majority of the spinel layer shows a mixed orientation relationship to the ferritic matrix {100}α || {100}sp & <011>α || <001>sp. However, also the discovered precipitated particles are characterized by the same crystallographic orientation relationship to the respective ferritic parent grain. The habit of the precipitates is best described by a lath morphology with their main axis parallel to <100> of ferrite.
Energy dispersive X-ray spectroscopy (EDX) and electron backscatter diffraction (EBSD) in an scanning electron microscope (SEM) have been applied to characterize the oxide layer in the micrometer scale. The clearly smaller precipitates were subsequently investigated by transmission electron microscopy (TEM). Specimens have been prepared by focused ion-beam (FIB) milling at an area previously characterized by EBSD. They cover the ferritic base material, but mainly the precipitation zone and the Fe‒Cr spinel layer. Energy filtered selected area diffraction (SAD) in the conventional (C)TEM and high-angle annular darkfield (HAADF) imaging in the scanning (S)TEM mode were employed in the characterization of the specimens.
Die Entwicklung von Wasserstoffbarrieren aus Glas erfordert die genaue Messung geringster H2-Permeabililtäten. Bisherige Untersuchungen haben gezeigt, dass die VHE-Pulvermethode diesbezüglich eine besonders hohe Empfindlichkeit bietet. Hierbei wird die isotherme Gasabgabe aus sphärischen Partikeln im Rahmen klassischer Diffusionsmodelle gefittet und daraus der Diffusionskoeffizient bestimmt. Für die Untersuchung von Gläsern mit möglichst geringer H2-Permeabilität ist jedoch eine Validierung der Genauigkeit der Methode notwendig. Vor diesem Hintergrund erfolgte die numerische Modellierung der H2-Abgabe mit Hilfe des Programms COMSOL Multiphysics®. Im Poster wird der Einfluss der Korngrößenverteilung der Glaspulverpartikel, der Partikelform sowie der Effekt einer nichthomogenen H2-Startverteilung auf die mittels Pulvermethode ermittelten Diffusionskoeffizienten diskutiert.
Advanced methods for 3D green density characterization like computed tomography and 3D FE sinter modeling can be utilized for increasing the reliability of sintered components. The experimental in situ observation of sin-tering, however, is currently restricted to silhouette methods, i.e. heating microscopy. For complex shaped sam-ples, in situ shape screening during shrinkage would allow better validation of 3D sinter simulation models. Further, by revealing temporary sinter warpage, 3D high-temperature shape screening would allow to locate potential defects of complex sintered components. Against this background, BAM developed a testing device for in situ 3D high-temperature shape screening for ceramic and glass-ceramic tapes up to 1000°C [1-3]. Current work is focused on dropping this restriction in sample shape and temperature. The poster illustrates the current state of this work and possible applications of the method e.g. in detecting sinter warpage of metallized glass-ceramic LTCC tapes.
In the course of miniaturizing modern technology down to the molecular scale, much remain unknown about the materials behavior and the deviations from the bulk that might arises from confinement effects. Here, a combination of nano-sized relaxation spectroscopies (Broadband dielectric spectroscopy (BDS) and Specific heat spectroscopy (SHS); employing AC nanochip calorimetry) were utilized to investigate the glassy dynamics of ultra-thin films of Poly (vinyl methyl ether) (PVME) and of blends PVME / Polystyrene (PS) 50:50 wt-%,, which are miscible in bulk (thicknesses: ca. 8 nm – 160 nm, film thickness was controlled by ellipsometry, film topography by AFM). Both methods are sensitive to different probes; where SHS senses entropy fluctuations while BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement is employed, where ultra-thin films are spin-coated on an ultra-flat highly conductive silicon wafer, sandwiched between a wafer with nanostructured SiO2 nano-spacers with heights between 35 nm and 70 nm. For PVME films, two thickness independent processes were observed and interpreted to be the α-processes of a bulk-like layer and a process due to an absorbed layer to the substrate. This adsorbed layer further undergoes a confinement effect that results in the localization of the segmental dynamics, which results in an Arrhenius-like temperature dependence. A detailed analysis of the dielectric strengths of both processes reveals that the thickness of the adsorbed layer decreases with increasing temperature, while that of the bulk-like layer increases. For the blend system, by measuring the dynamic Tg in dependence of the film thickness, SHS showed that the Tg of the whole film was strongly influenced by a nanometer-thick surface layer at the polymer/air interface due to a self-assembling process. The dynamic Tg obtained from the SHS measurements decreased with decreasing film thickness. On the other hand, BDS measurements showed a completely different behavior. At high temperatures, the temperature dependence of the relaxation times of the films follows that of bulk-like PS/PVME; obeying the VFT-law. With decreasing temperature, the temperature dependence deviates from the VFT to an Arrhenius law; where the apparent activation energy decreases with decreasing film thickness. This is the first example where confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in detail in a comprehensive discussion.
Successful implementation of an optical polarimetry measurement setup. Due to wall anchoring interactions HAT6 embedded in an untreated alumina membrane exhibits a radial orientation for pore sizes in between 30 nm and 80 nm. Embedded in large membranes, pore size of 180 nm, HAT6 forms the favored hexagonal columnar phase along the pore axis.
By means of an effective medium (EMA) based approach, it is possible to use spectroscopic ellipsometry to determine the mixing ratios between air and material in porous dielectrics and calculate a quantitative value of the porosity for these materials. As this method is model-based, it is very difficult to provide a quantitative measure for the accuracy of porosity values determined by this method. Valuable additional information can often be obtained by combining ellipsometry with other complementary methods. In the present study, the ellipsometry results were validated by Electron Probe Microanalysis (EPMA) with the option of layer analysis (by the socalled “STRATAGem” approach), gravimetry, and electron microscopy. We analysed porous TiO2 thin layers synthesised by means of a template synthesis approach (evaporation induced self assembly).
Ellipsometry measurements on porous samples are difficult to analyse due to the complexity of the models necessary. Often it is difficult to decide if the measured data contains enough information to successfully determine the target quantities (mixing ratio, dielectric function of the matrix material). One method to decrease the complexity of the fit and therefore use the measurement data most efficiently is a multi-sample analysis. In the present case, multi-sample analysis was used for determining the porosity factors of the individual layers while using one common set of dielectric function values for the matrix in all cases.
While the results of the fit analysis in this case can be used to show the feasibility and also the limitations of the multi-method approach, the porosity values themselves show a promising agreement between the independent methods. It can therefore be concluded that determining porosity values with ellipsometry is in accordance to other methods to the level of accuracy provided by the complementary methodologies.
Silicon surface passivation with atomic layer deposited (ALD) thin films has gained more and more interest in the PV community in recent years. With ALD good film quality, accurate thickness control and conformity are reached. Furthermore, ALD is capable of coating difficult substrates such as nanostructured surfaces with the same accuracy as flat surfaces. A variety of materials such as Al2O3, TiO2 and HfO2 demonstrate good surface passivation quality both for front and rear surface of silicon solar cells. In addition of providing good surface passivation, thin films with high refractive index e.g. HfO2, TiO2 and AlN can act simultaneously as antireflection coatings when applied on the front surface of the device. Hence, ALD thin films can reduce both electrical and reflective losses in solar cells.
Thorough investigation of the optical properties of these layers is crucial for several reasons related to their production and use. Optical measurements provide a fast, easy, non-destructive, and in situ capable approach to quality assurance for photovoltaic devices. As the function of the final device is optical, optimisation of the device performance relies strongly on the knowledge of the wide-range dielectric function of the thin layers. In this contribution, we determined the optical constants of ALD generated layers of AlN, Al2O3, TiO2, and HfO2 in a wide spectral range covering the near ultraviolet and the mid-infrared regions by means of spectroscopic ellipsometry. By combining data from a UV-Vis-NIR ellipsometer (Woollam M2000DI) and an FTIR ellipsometer (Sentech Sendira), we can determine the optical constants alongside with the layer thicknesses from one large set of spectroscopic measurements. We consider this a contribution to the metrological treatment of stratified and structured thin films in the optical range by polarisation-sensitive measurement methods.
In recent years, upconversion nanocrystals (UCNC) have shown great promise for biological and medical applications, mainly because of their excitation in the NIR region, which provides minimum fluorescence background and a rather deep penetration into biological samples, as opposed to excitation in the visible or UV region. Moreover, they show a multitude of characteristic narrow emission bands as basis for ratiometric measurements. Commonly, Yb is the sensitizer of choice, because of a comparatively high absorption cross section, simple energy scheme, and rather efficient energy transfer to the activator, mostly Er, Tm or Ho. A main disadvantage of the use of Yb as sensitizer for biological and medical applications is its absorption band at 976 nm and hence the use of an excitation wavelength at which water has a non-negligible absorption. This can lead to significant sample heating, especially at long illumination times or high excitation power densities, and thus, tissue damage or even cell death. A possible solution is the tri-doping of UCNC with Nd as sensitizer, which can be excited efficiently at around 800 nm, where water absorption is at minimum.
The use of Nd as a sensitizer and Yb as a bridge between Nd and the activator Er in NaYF₄ nanocrystals is a relatively new way to overcome the problems of heating of samples in an aqueous environment. Disadvantages can arise from the tri-doping, which can favor non-radiative relaxation due to the more complicated excitation process compared to e.g., simple Yb,Er-doped UCNC, which might lower the upconversion quantum yields in these tri-doped systems. In order to quantify clear advantages, NaYF₄:Yb,Er,Nd nanoparticles were synthesized and spectroscopically studied using an 8 W 804 nm laser diode and a custom-designed Edinburgh instruments FSP980 spectrometer. Wavelength-dependent studies of the emission intensities and the decay kinetics of these tri-doped UCNC at different excitation power densities and excitation pulse widths revealed the clear advantages of preventing water absorption on measurable luminescence signals.
We were able to show the influence of pulse width and excitation power density on the luminescence intensities and decay kinetics lifetimes at different emission wavelengths. Additionally, we can clearly discern power density-dependent and independent peaks in the emission spectra. In summary, we demonstrate that the tri-doping of NaYF₄:Yb,Er,Nd nanoparticles is a very promising approach to render UCNC more efficient and to make them better suitable for biological and medical applications requiring measurements in aqueous environment.
Microbial induced corrosion (MIC) is a crucial problem in many technical plants as well as fuel tanks, leading to considerable damage and huge financial losses. Successful prevention of MIC requires the localization of first signs of corrosion as well as the identification of factors influencing the corrosion process.1 Hence, there is a growing need for sensitive and preferably inexpensive tools that enable the early detection of MIC. Of high importance are methods, which provide spatially and time-resolved information and allow the study of changes on metal surfaces as prerequisites for a more detailed analysis of ongoing corrosion processes at a MIC-affected site.2 In this respect, also the determination of corrosion rates can be of interest for the possible prevention of MIC.
In respect of modern approaches in material sciences and highly increased requirements on materials on safety relevant components, quality management and non-destructive testing reclaims a steadily increased meaning. The destructive meaning of measuring the degree of purity is defined in DIN EN 10247 through metallurgical investigations, especially microsections. For and comparable, but non-destructive testing due ultrasonic testing, the material the SEP 1927 is a well-defined industry standard. A novel and alternative way of reference block construction was focused by this work. The proposed amendments, regarding the manufactoring and machining, are less time and cost consuming. Verified by measurements the presented reference block fits the same acoustical characteristics and the requirements of the guideline.
X-ray powder diffraction (XRD) patterns of the high-temperature (HT) cristobalite form of SiO2 and its isoelectronic AlPO4 analogue are essentially influenced by the dynamic disorder of these crystal structures. The nature of this disorder and of the phase transition between the α- and β-form has been the subject of intensive research during the last four decades [1]. By 1989 it became possible to stabilize the HT-form of cristobalite SiO2 at room temperature in laboratory and engineering ceramic industries by applying solid solution forming techniques [2]. However, for the HT-form of cristobalite AlPO4 nothing similar has been known until 2014 when it was discovered that nanocrystalline and stacking-disordered β-cristobalite AlPO4 is the major component of the fly ash of a large incineration facility operated by the waste water treatment authorities of Frankfurt/M. [3]. Previous comprehensive investigations of this fly ash failed to interpret its complex XRD pattern – presumably mainly due to the lack of a matching experimental digital pattern in the Powder Diffraction Database. The present paper reports on a synthesis route that facilitates the crystallization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 that is free of crystalline impurity phases and long-term stable at ambient. Its room temperature XRD pattern is presented with parameters traced back to certified reference materials.
[1] Yuan F. and Huang L., Phys. Rev, B, 2012, 85, 134114. [2] Perrotta J.A., Grubbs D.K., Martin E.S., Dando N.R., McKinstry H.A. and Huang C.-Y., J. Am. Ceram. Soc., 1989, 72, 441. [3] Peplinski B., Adam C., Adamczyk B., Müller R., Michaelis M., Krahl Th. and Emmerling F., Powder Diffraction Journal, 2015, 30, 2, Supp. 1, S31.
In situ investigations using PXRD coupled with Raman spectroscopy permit the evaluation of the formation pathways of milling reactions. The liquid-assisted grinding cocrystallisation of theophylline with benzamide leading to polymorphic compounds was investigated. The dipole moment of the solvent used in the synthesis determines the structure of the polymorphic product. A detailed investigation allows determining the kinetically and thermodynamically favored product. In situ observations of the formation pathway during the grinding process of both polymorphs show that the thermodynamically favored cocrystal is formed in a two-step mechanism with the kinetic cocrystal as intermediate. The evaluation of the mechanochemical formation pathways reveals the importance of in situ investigations for an in depth understanding of mechanochemical synthesis mechanisms. Our study demonstrates that the choice of the solvent in the LAG synthesis is decisive for the controlled formation of a desired polymorphic final product.
The widespread use of antibiotics in livestock farming leads to trace residues in food products and wastewater, potentially entailing antimicrobial resistance in food-borne pathogens. The determination of antibiotics in aqueous environments and foodstuff is thus of major concern.
Analytical assays based on molecularly imprinted polymers (MIPs) have emerged as a valuable tool in this field due to the low production costs, stability, format adaptability and the possibility to imprint and thus their ability to recognize a wide variety of target analytes. With regard to optical sensing technologies, however, MIPs have only been used in considerably few applications, especially in fluorescence sensors. This limitation is basically due to the fact that the incorporation of a fluorescently responding moiety into a polymer matrix is challenging. One way to overcome this limitation is to use tailor-made fluorescent indicator monomers for direct transfer of the binding event into an optical signal. If such a monomer is integrated into a thin MIP-shell on microspheres such core/shell particles can be readily used in advanced multiplexing sensory fiber-optic microarrays.
Here, we propose such a fiber-optic microarray based on fluorescent MIP microspheres for antibiotics. The binding behavior and the selectivity of a microarray using these MIP were examined and compared with a non-imprinted polymer (NIP) control, employing the target molecules and other structurally closely related antibiotics.
Renewable resources become more and more relevant to maintain energy demands for an increasing global population. Biosynthetic fuels like biodiesel might replace conventional petrochemical fuels, such as diesel. However, more research is needed to characterize the interaction between the different fuels and the polymeric material, especially with respect to ageing and degradation.
The poster will present several interaction and degradation phenomena of high density polyethylene (PE-HD) induced by diesel and biodiesel 1-3. Also the possible influence of microbial growth (fungi and bacteria) is considered. The chosen PE-HDs are typical thermoplastic resins for container and storage tank applications. Degradation of PE-HD will be investigated by changes of the mechanical properties – with main emphasis on the Charpy impact strength 2. Furthermore, with alternating sorption and desorption cycles in combination with oven ageing the co-oxidation 3 of PE-HD in contact with biodiesel will be addressed.
Metal reducing bacteria (MRB) are able to utilize various materials such as iron, uranium and manganese as well as many organic compounds as electron acceptors. This process leads to the conversion of Fe(III) containing passive film species to soluble Fe(II) oxides and hydroxides. The reduction process triggers the acceleration of general and local corrosion processes. Electron transfer mechanisms are not yet fully understood. In literature it has been controversially discussed to which extend secreted electron shuttles contribute to the extracellular electron transfer (EET).
To understand the chemical and electrochemical interaction mechanisms of MRB with steel surfaces this project combines a variety of in-situ techniques. The changes in oxide chemistry on Fe/steel surfaces in the presence of biomolecules and MRB are under investigation using a newly designed electrochemical cell for in situ XANES (x-ray absorption near edge structure) spectroscopy. Electrochemical quartz crystal microbalance (eQCM) studies support the spectroscopic investigations to gain information about the kinetics of attachment processes and changes in biofilm viscosity. The biofilm structure and composition as well as cell viability are investigated by complementary ex situ spectroscopic and microscopic analysis.
Combining spectroscopic techniques and eQCM data with electrochemical measurements, biological processes and the resulting degradation of steel surfaces can be observed in a non-destructive manner. Selecting model systems and a defined biological medium allows the determination of individual effects of diverse surface and environmental parameters. The fundamental understanding of bacterial attachment mechanisms and initial steps of biofilm formation will contribute to the development of new antifouling strategies.
The ability to penetrate dielectric materials makes T-rays attractive to reveal discontinuities in polymer and ceramic materials. Changes of travelling time (ToF) and pulse shape due to the interactions of THz pulses with the dielectric material and its inherent discontinuities can be observed. A tomogram of the object under the test can be reconstructed from time of flight diffraction (ToFD) scans if a synthetic focusing aperture (SAFT) algorithm is applied.
Time-resolved studies on the formation of maghemite nanoparticles combining fast-XANES and SAXS
(2016)
Iron oxide nanoparticles find application in different areas like sensing, magnetic storage media, and biomedicine, due to their magnetic properties and environment-friendliness.
In the present contribution, we report on the in situ investigation of an iron oxide nanoparticle synthesis by coupled X-ray absorption near-edge structure (XANES) and small-angle X-ray scattering (SAXS). The combination provides simultaneously information about the size of particles (SAXS) and on the oxidation state and the local structure of the iron atoms (XANES). The co-precipitation synthesis was exemplary studied, using a stabilization agent to decelerate the fast precipitation of the iron oxides. This allows to detect intermediates in situ. The measurements were performed using a custom-made acoustic levitator as sample holder. From the data, a mechanism was derived indicating different phases of particle Formation and oxidation state changes.
In the last years, secondary low-energy electrons (LEE) emerged as important, if not predominant, reductive pathway in ionizing damage of biomolecules. These electrons are created in copious amount as result of inelastic scattering of high energy radiation at water. Until now, all experiments the quantification of the effects of LEEs on the biomolecular damage was either performed in vacuum with LEE sources or with DNA on surfaces in humid atmosphere.
We present a new experimental setup to irradiate biomolecules with electrons under physiological conditions. In combination with monte carlo simulations this setup makes it possible to determine microdosimetric quantities for biomolecules in liquid environment under electron irradiation.
This opens up new possibilities in radiation research to access the LEE damage under well defined physiological condition, for more complex systems, such as DNA-Protein complexes and even living cells.
Invasoren im Kleiderschrank
(2016)
Beton ist als Massenbaustoff vielseitig einsetzbar. Eine der neuesten Entwicklungen ist Ultrahochleistungsbeton (UHPC). Seine besonderen Eigenschaften ermöglichen eine zusätzliche Funktionalisierung der Oberflächen, da annähernd beliebige Mikrostrukturen exakt abgeformt werden können. So lassen sich beispielsweise Fassadenelemente aus UHPC bereits bei ihrer Herstellung im Betonfertigteilwerk mit selbstreinigenden Oberflächen ausrüsten. Eine andere Möglichkeit ist eine Anwendung als Datenspeicher. Wie das Beispiel der Schallplatte aus UHPC zeigt, lassen sich Muster, die hier die Schallinformationen enthalten, exakt von einer Matrize kopieren.
Characterization of statistical EO-PO copolymers containing different end groups by UPLC/ESI-MS
(2016)
Commercial statistical ethylene oxide (EO) and propylene oxide (PO) copolymers of different monomer compositions and different average molar masses were studied by liquid chromatography under critical conditions (LCCC). Theoretical predictions of the existence of a critical adsorption point (CPA) for statistical copolymers with a given chemical and sequence distribution, could be studied and confirmed. An improved way to determine these critical conditions in a copolymer, alongside the inevitable chemical composition distribution (CCD), with the aid of mass spectrometric detection is described. Shift of the critical eluent composition with the monomer composition of the polymers could be observed. Due to the relatively low average molecular weight, broad molecular weight distribution (MWD) and the presumed existence of different end group functionalities as well as sequence distribution, gradient separation only by CCD was not possible. Therefore isocratic separations at the CPA of definite CCD’s were applied. Although the various present distributions partly superimposed the separation process the goal of separation by end group functionality could still be achieved on the basis of the additional dimension of ESI-MS. The existence of HO-H besides the desired AllylO-H end group functionalities could be confirmed and their amount could be estimated.
Multilayer carbon nanomembrances (CNMs) could pave the way for a new ultrathin functional conductive coatings with tunable electrical, optical, and chemical properties. Due to their molecular thickness, they can also be regarded as “interfaces without bulk” separating regions of different gaseous, liquid, or solid components and controlling the materials exchange between them, making them optimal materials for membranes applications. Furthermore, their physical and chemical properties depend strongly on their structure, molecular composition, and the surroundings of either sides, thus allowing for tailored properties. Here, nanolayers of Aromatic p-terphenylthiol (TPT) self-assembled into 2D carbon monolayers (thickness - 1.6 nm) were synthesized and further crosslinked by ion bombardment, forming CNMs. Here, though a recently developed multilayer nanosheets routine, stacks of 5, 10, 15 and 20 TPT sheets where transferred on top of each other forming a multilayered CNMs. However, this transfer routine could introduce some intrinsic defects to the sheets, which would alter the molecular composition and / or structure, thus consequently the CNMs properties. Therefore, it is essential to characterize defects in “pure” TPT nanomembranes, before tailoring the molecular compositions, e.g. adding functional groups. For this reason, broadband dielectric spectroscopy (BDS) was utilized to characterize any defects that could be rasied during preparation. Due the structure of pure TPT membranes, no dipole moment should exsist. However, the presence of other elements, e.g. water or sulphur, would result in a dipole moment that could be probed by BDS.
As a main result, for all different stacked-layer numbers, a clear relaxation process is seen, which moves to higher frequencies with increasing the temperature. The temperature dependence of the relaxation rate of this process is independent of film thickness and can be well described by a common VFT function, hence a corporative motion. This relaxation process was assigned to intrinisic defects in the membranes, introduced during preparation, which was further confimed by a detailed anaylsis of the dielectric strength. This is the first BDS measurment on TPT CNMs.
Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle.
Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear
equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle.
Calcium cobaltite is a promising p-type oxide thermoelectric material for high temperature applications due to its high figure of merit between 600 °C and 900 °C in air. The solid-state-reaction is well known for large scale powder synthesis of functional materials. As a high temperature process, the powder synthesis consumes a lot of energy. In different studies, different synthesis conditions were used for the preparation of calcium cobaltite powder. This study showed that a higher energy input (elevated temperatures, longer dwell times, or repeated calcinations) during powder synthesis does not increase but decrease the Seebeck coefficient and the electrical conductivity. The same correlation was determined for the densification. As a higher energy input leads to a larger grain size and therefore to a reduced sinter activity, it can be concluded that the thermoelectric properties are correlated with the sinter activity of the powder. These results can be used to minimize the energy demand for the powder synthesis of Ca₃Co₄ O₉.
Since geothermal wells are a feasible energy source to replace fossil fuel supply, many technologies have been developed to take advantage of geothermal energy. Nevertheless, service conditions in geothermal facilities are due to the chemical composition of hydrothermal fluids and temperatures, in many cases, extreme in terms of corrosion.
Therefore, materials selection based on preliminary material qualification is essential to guarantee a secure and reliable operation of the facilities. The corrosion behavior of different high-alloyed metals including Duplex and austenitic stainless steels as well as a nickel alloy have been evaluated in artificial geothermal fluids simulating the conditions in some locations with geothermal potential in Germany as well as two sites in Indonesia. The suitability of carbon steel 25CrMo4, stainless steels X2CrNiMo17-12-2, X2CrNiMo-22-5, X2CrNiMoCuWN25-7-4 and super austenitic steel X1CrNiMoCu32-28-7 in these geothermal fluids obtained by electrochemical measurements and exposure tests is limited. The nickel alloy NiCr23Mo16Al shows an excellent corrosion resistance against pitting corrosion. Excluding its high cost, it is a very good alternative to be used in the construction of geothermal facilities having highly saline brines. Stainless and Duplex steels exhibit a limited corrosion resistance concerning pitting and crevice corrosion. Beside of the higher alloyed materials, also the lowalloyed steel 25CrMo4 could be employed as a constructional material for the geothermal power plant in stagnant highly acidic non Saline environments, as long as the wall thickness of the material vs. corrosion rate is taken into account.
Derzeit wird der Einsatz metallener Werkstoffe in CCU-/CCS-Anlagen hinsichtlich deren Korrosionsbeständigkeit und eine eventuell daraus resultierende Herausforderung diskutiert. Während des CO₂-Transportes vom Abscheide- zum Injektionsort kann es aufgrund der den CO₂-Strom begleitenden Beimengungen, wie Wasser, O₂, SOₓ , NOₓ , Temperaturschwankungen durchaus zu Kondensationseffekten und daraus resultierenden Schäden kommen.
Es konnte gezeigt werden, dass die sich möglicherweise innerhalb einer CO₂-Rohrleitung bildenden Kondensate infolge von Begleitstoffen wie SO2 und NO2 eine viel korrosivere Wirkung auf Rohrleitungswerkstoffe entfalten, als in reinem CO₂.
In letzter Zeit kommen immer mehr alternative Energiequellen als Ersatz fossiler Brennstoffe zum Einsatz, so auch die Solarthermie. Jedoch sind die Betriebsbedingungen aufgrund der chemischen Zusammensetzung der Wärmeträgermedien und herrschenden Temperaturen extrem hinsichtlich Korrosion. Da die Kraftwerke bei maximaler Lebensdauer ökonomisch vertretbar sein müssen, ist eine Werkstoffauswahl basierend auf Voruntersuchungen notwendig, um einen sicheren und verlässlichen Betrieb dieser Anlagen zu gewährleisten.
Die Werkstoffauswahl hängt von der Betriebstemperatur eines Kraftwerks bzw. der chemischen Zusammensetzung des Wärmeträgermediums ab. In hochkorrosiven Umgebungen werden aufgrund ihrer sehr guten Korrosionsbeständigkeit Nickelbasislegierungen nicht nur für stark korrosiv beanspruchte Bauteile als die Lösung angesehen. Jedoch kann es durchaus beständigkeitsbedingte Einschränkungen für den Einsatz geben, wofür die hier vorgestellten Ergebnisse dienen sollen.
In diesem Beitrag wird die Beständigkeit ausgewählter hochlegierter Werkstoffe (inklusive einer neuentwickelten Legierung in einer Nitrat-Salzschmelze (60 % NaNO3/40 % KNO3) vorgestellt, die mittels elektrochemischer Messungen und Auslagerungsversuchen ermittelt wurde.
Polymers are favorable materials for gas separation membranes. In general, gas transport experiments are performed with films in the range of 100 µm thickness. However, in large-scale processes very thin selective polymer layers in the range of 100 nm to 1 µm are used. Moreover, it was shown that thin films behave different compared to thick films with respect to gas transport properties and physical aging as well. Thus, for fundamental research it is important to realize gas transport experiments with thin films. The Quartz Crystal Microbalance (QCM) is a very sensitive method to detect mass changes in the range of nanograms. Therefore, this method enables sorption experiments with thin films or layers attached to the QCM crystal (100 nm up to 1 µm). Here, we present the experimental set-up for using the QCM technique for characterizing the gas sorption behavior of thin polymer films in a temperature controlled pressurized environment (up to 50 bar) - also quartz crystals and crystal holders were optimized. The study aims for the characterization of long-term behavior and physical aging of high-performance polymers for gas separation membranes - such as polyimides and polymers of intrinsic microporosity (PIMs) and respective nanocomposites. Especially the differences of the behavior of thin films compared to films with thicknesses up to 100 µm as well as nanofiller induced-effects are adressed.