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Se presenta una guía completa del procedimiento experimental para la determinación del valor umbral ΔKth intrínseco y caracterización de curvas FCGR sobre el acero de alta resistencia S960QL empleando probetas de pequeña escala. El análisis se realiza comparando probetas SENB de diferentes geometrías, distinguiendo entre “convencionales” y “miniatura”. Las primeras con espesor (B) de 6 mm y anchura (W) de 19, y las segundas con B = 3 y dos valores distintos de W, 4 y 6 mm. A fin de identificar el valor umbral ΔKth intrínseco, la relación de cargas (R) aplicada en todos los ensayos fue 0,8. La técnica de caída de potencial (DCPD) se utilizó para la monitorización del tamaño de grieta a lo largo de los ensayos.
La evaluación de los resultados experimentales confirma la equiparación de resultados entre las distintas geometrías y configuraciones de ensayo practicadas, así como la viabilidad de emplear probetas de pequeña escala en la determinación del valor umbral ΔKth intrínseco. Esto abre nuevas perspectivas en lo relativo al empleo de probetas de reducidas dimensiones en la caracterización de materiales a fatiga. A su vez, permite ofrecer una serie de recomendaciones para reproducir con éxito ensayos semejantes utilizando probetas de pequeñas dimensiones de acero y otros materiales metálicos.
Für den Anlagenbau werden hochbelastete Komponenten aus Co-Cr-Legierungen hergestellt. Dabei ist die Zerspanung so herausfordernd, dass additive Fertigungsschritte oft wirtschaftlicher sind. Diese bedingen aber vorwiegende heterogene, anisotrope Gefüge und Eigenschaften und bei nachfolgender Fräsbearbeitung unstetige Zerspankräfte und instabile Spanvorgänge. Hierbei können hybride Zerspanprozesse helfen, hohe Belastungen für Werkzeug und Werkstückoberfläche zu minimieren. Diesbezügliche Charakterisierungen erfordern speziell adaptierte Zerspanungsanalysen.
Anhand eines Anwendungsbeispiels, bei dem eine Modifikation der Ausgangslegierung mit 1 % Hf erfolgte, wird die Wechselwirkung zwischen Gefügemorphologie und Fräsprozess dargestellt, der konventionelle mit einem hybriden ultraschallunterstützten Fräsprozess verglichen und die Charakterisierung des Werkzeugverschleißes anhand zweier verschiedener Fräser betrachtet. Analysen auftretender Prozesskräfte mittels Piezo-Mehrkomponenten-Dynamometer, der Werkzeugoszillation mittels Laser-Vibrometer und zusätzliche In-situ-Temperaturmessungen der Werkzeugschneiden mittels Highspeed-Pyrometer bilden den Kern der neuen Zerspanungsprüftechik.
Die vorgestellten Untersuchungsmethoden bilden die Vorgänge bei der Zerspanung additiv gefertigter Werkstoffe detailliert und reproduzierbar ab. Sowohl Legierungsmodifikation als auch hybride Prozessbedingungen lassen gezielte Einflüsse zur deutlichen Verbesserung der Zerspanungssituation zu.
Assessing dissolution of upconverting nanoparticles by TEM, EDXS, potentiometry and fluorometry
(2021)
Inorganic lanthanide-doped upconversion nanoparticles (UCNP) constitute an emerging class of near-infrared (NIR)-excitable luminescent reporters for bioimaging, fluorescence assays, sensors in bioanalysis, and optical thermometry as well as phosphors for photovoltaic and security applications.1 However, the use of UCNPs in bioimaging and cellular studies requires biocompatible particles. One possible cause of UCNP toxicity is the release of potentially harmful fluoride fluoride and lanthanide ions as revealed by dilution studies in aqueous environments, particularly under high dilution conditions.2-5 To address this issue, suitable surface coatings preventing such effects in combination with fast screening methods suited for online in situ analysis are desired.
Here we present a systematic study of differently sized β-NaYF4:Yb,Er nanocrystals stabilized with different surface coatings and different hydrophilic ligands varying in binding strength to the surface atoms in various aqueous environments at different temperatures.
Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS)
(2021)
Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis.
Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS)
(2021)
Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis.
Investigation of the internal impact during a 9 m drop test of an accident-safe waste package
(2021)
The safety assessment of packages for the transport of radioactive material follows the IAEA regulations and guidance. The specified regulatory tests cover severe accidents and demonstrate the package containment system integrity. Special attention must be drawn to the behaviour of the content which could move inside the package due to unpreventable gaps caused by the loading procedure and the structure of the content. A possible internal impact of the content which occurs during the drop tests onto the lid system is investigated. The IAEA regulations SSR-6 and the Guidance SSG-26, revised recently, consider input from Germany and France related to the significance of internal gaps.
In the context of a waste package design assessment, a model was equipped with a representative content to conduct a drop test with an internal impact. The weight and kinetic impact of this content covered all possible real contents. The objective of the test was to maximize the load onto the lid system and to prove the mechanical integrity by complying with the required leak tightness. The test was conducted conservatively at a package temperature lower than -40 °C at the BAM Test Site Technical Safety.
This paper gives an overview of efforts to address internal gaps and their consequences, and the BAM efforts with the implementation of this topic into IAEA regulations and guidance material. The paper then focuses on the conduction of a drop test and investigation of internal component impact.
Steelmaking slags are a by-product of steel production, that are currently used primarily in road construction, earthwork, and hydraulic engineering. In this use, the iron bound in the steelmaking slags (< 30 wt.%) is lost.
Recovery of iron from steelmaking slags is possible by thermochemical reductive treatment. The reductive treatment of liquid steelmaking slags causes iron oxides to be reduced to metallic iron, which separates from the mineral phase due to its higher density. The chemical composition of the mineral phase is thus adapted to that of the Portland cement clinker and the mineral alite, the most important component of Portland cement, is formed. This way, crude iron can be recovered, and at the same time a hydraulic binder can be produced.
This process, however, is uneconomical due to the high temperatures required (~1800 °C). In the current project, the process is to be adapted so that the reduction of liquid steelmaking slag can be carried out at ~1600 °C. The chemical composition is to be modified in such a way that the melting temperature of the slags as well as their viscosity are in a technically suitable range and still a product with good cementitious properties is obtained.