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Hierarchical Imaging of the Dynamics During Pulsed Laser Ablation in Liquids

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Hierarchical Imaging of the Dynamics During Pulsed Laser Ablation in Liquids Hierarchical imaging of the dynamics during pulsed laser ablation in liquids Zur Erlangung des akademischen Grades Doktor der Naturwissenschaften (Dr. rer. nat.) von der KIT-Fakultät für Physik des Karlsruher Institut für Technologie (KIT) genehmigte Dissertation von M. Sc. Stefan Reich optical imaging transmission contrast scattering contrast Tag der mündlichen Prüfung: 24. Mai 2019 Referent: Prof. Dr. Tilo Baumbach Korreferent: PD Dr. habil. Anton Plech KIT – Universität des Landes Baden-Württemberg und nationales Forschungszentrum in der Helmholtz-Gemeinschaft www.kit.edu This document is licensed under a Creative Commons Attribution-ShareAlike 4.0 International License (CC BY-SA 4.0): https://creativecommons.org/licenses/by-sa/4.0/deed.en ”Some people - some companies and some decision makers in particularly - have known exactly what priceless values they are sacrificing to continue making unimaginable amounts of money. And I think many of you who are here today belong to this group of people.” Greta Thunberg, World Economic Forum 2019 Cover image: Images of optical imaging and X-ray multi-contrast imaging of the first cavitation bubble rebound of an ablation on a free zinc wire with a diameter of 1 mm. The ablation was performed in pure water with a laser of 7 ns pulse duration, a wavelength of 1064 nm and a pulse energy of 11 mJ. The multi- contrast imaging was performed on an imaging beamline of the synchrotron at KIT with a compound array refracting lens as optical element. In optical imaging a predominantly opaque mushroom-like re- bound is visible. The X-ray imaging proves that the rebound consists of a vapor cavity containing many microbubbles. i Abstract With Pulsed Laser Ablation in Liquids (PLAL) it is possible to produce nanoparticles (NPs) that are directly dispersed in liquid and no residual surfactants or reactants do contaminate theseNPs. After laser excitation of the target, a millimeter-sized cavitation bubble is formed in which theNPs are confined. Using a series of complementary measurement techniques and in situ hierarchical imaging, this work examines the fundamental processes during PLAL. The laser-matter interaction is investigated by optical imaging of the cavitation bubble and the ignited plasma in combination with absorption spectroscopy. A direct correlation between these three parameters is identified which allows indirect conclusions to be drawn about the ablation process. The incubation effect occurring on pristine targets and the presence of a plasma threshold fluence indicate that efficient ablation requires either pre-irradiated targets or fluences above the threshold. An ablation with low flu- ences on pristine targets leads to strong loss mechanisms, which results in a strongly reduced energy localization and thus a low ablation rate. It is found that the energy dose required for stable and effi- cient ablation depends on material parameters such as the Young’s modulus and the enthalpy required for material heating and evaporation. As soon as the plasma threshold fluence is exceeded, the material parameters have a minor influence. For nanosecond laser ablation above the threshold, most of the pulse energy is absorbed by the plasma. Below the threshold, the loss mechanisms dominate, which leads to a strongly reduced ablation efficiency. For the in situ detection ofNPs during the lifetime of the cavitation bubble X-ray methods are used. The NP size distribution is examined with high temporal resolution by Small-angle X-ray Scattering (SAXS), while Wide-angle X-ray Scattering (WAXS) measures the crystalline domain size. The early appearance of largeNPs with large crystal domain sizes confirms the recent models of the ablation process. The multimodalNP size distribution is caused directly by film lift-off and Rayleigh instabilities on the liquid metal surface. Furthermore, the temporal distribution of theNPs confirms thatNPs are located at or even in front of the cavitation bubble boundary, as well as the almost homogeneous filling of the bubble withNPs. Two different mechanisms of emergence of largeNPs are also identified. SphericalNPs are produced directly from the molten target, while the agglomeration of smallNPs occurs mainly during bubble collapse. A multiplexing of the SAXS measurements to directly obtain a 2D image of theNP distribution is per- formed by Hartmann mask-like multi-contrast imaging. For this purpose, a broad X-ray beam is divided into a 2D array of beamlets by a custom Hartmann mask respectively the newly developed Compound Array Refractive Lenses (CARLs). The transmission and scattering contrast of this Single-Exposure Multi-Contrast Imaging (SEMCI) technique is used for the hierarchical imaging of the ablation process. The in situ quenching capabilities of goldNPs with inorganic electrolytes and macromolecular ligands are investigated. It is found that the quenching mechanisms of the two additives are different. Electrolytes act in situ in the cavitation bubble, while ligands do not. By changing the scattering sensitivity fromNPs iii Abstract to the micrometer range, the nature of the first bubble rebound of an ablation on a free wire target is clar- ified. This detached rebound consists of micrometer-sized bubbles and contains no significant amounts ofNPs anymore. The X-ray efficiency of the SEMCI is improved by replacing the commonly used Hartmann masks with lens arrays. These CARLs are produced by embossing 2D arrays with 100 × 100 concave lenses in polymer films. The pitches are around 50 µm and the apex radii of the parabolic lenses are around 8 µm. The positioning accuracy of the beamlets is less than 1 µm. By stacking up to six lens array foils, focal lengths between 60 cm and 125 cm are achieved at X-ray energies of 9 keV. The maximum visibility is about 0.5. Beside theNP detection by the scattering contrast, the wavefront distortion of samples or X-ray optics can be analyzed with a resolution of 0.2 µrad. iv Kurzfassung Mittels gepulster Laserablation in Flüssigkeiten (Pulsed Laser Ablation in Liquids, PLAL) ist es möglich, Nanopartikel (NP) herzustellen, die direkt in der Flüssigkeit dispergiert und nicht durch verblie-bene Ten- side oder Reaktanden verunreinigt sind. Nach der Laseranregung des Targets bildet sich eine millime- tergroße Kavitationsblase, in der dieNP verteilt und größtenteils gefangen sind. In dieser Arbeit werden die fundamentalen Prozesse während PLAL mit einer Reihe von komplementären Messtechniken und hierarchischer in situ Bildgebung untersucht. Die Laser-Materie-Wechselwirkung wird durch optische Abbildung der Kavitationsblase und des gezündeten Plasmas in Kombination mit Absorptionsspektroskopie untersucht. Es wird eine direkte Korrelation zwischen diesen drei Parametern gezeigt, die es erlaubt, indirekte Rückschlüsse auf den Ab- lationsprozess zu ziehen. Der Inkubationseffekt, der bei unversehrten Targets auftritt, und das Vorhan- densein einer Plasma-Schwellfluenz zeigen, dass für eine effiziente Ablation entweder vorbestrahlte Targets oder Fluenzen oberhalb der Schwelle erforderlich sind. Eine Ablation mit geringen Fluenzen auf unversehrten Targets führt zu starken Verlustmechanismen, was in einer stark reduzierte Energielokali- sation und damit niedrigen Ablationsrate resultiert. Es wird gezeigt, dass die für eine stabile und ef- fiziente Ablation erforderliche Energiedosis von Materialparametern wie dem Elastizitätsmodul und der für die Materialerwärmung und -verdampfung erforderlichen Enthalpie abhängt. Sobald die Plasma- Schwellfluenz überschritten wird, haben die Materialparameter jedoch nur noch einen geringen Einfluss. Bei der Nanosekunden-Laserablation oberhalb der Schwellfluenz wird der größte Teil der Pulsenergie vom Plasma absorbiert. Unterhalb der Schwellfluenz dominieren die Verlustmechanismen, was zu einer stark reduzierten Ablationseffizienz führt. Für den in situ Nachweis vonNP während der Lebensdauer der Kavitationsblase werden Rönt- genstreumethoden verwendet. DieNP-Größenverteilung wird mit hoher zeitlicher Auflösung mittels Röntgen-Kleinwinkelstreuung (Small-angle X-ray Scattering, SAXS) untersucht, während Röntgen- Weitwinkelstreuung (Wide-angle X-ray Scattering, WAXS) zur Messung der kristallinen Domänen- größe verwendet wird. Das frühe Auftreten von großenNP mit großen Kristalldomänengrößen bestätigt die jüngsten Modelle des Ablationsprozesses. Die multimodaleNP-Größenverteilung wird direkt durch Filmabhebung und Rayleigh-Instabilitäten auf der flüssigen Metalloberfläche hervorgerufen. Darüber hinaus bestätigt die zeitliche Verteilung derNP, dass sichNP an oder sogar vor der Kavitationsblasen- grenze befinden, sowie die nahezu homogene Füllung der Blase mitNP. Zwei verschiedene Mechanis- men der Entstehung von großenNP werden ebenfalls identifiziert. SphärischeNP entstehen direkt aus der Schmelze, während die Agglomeration von kleinenNP hauptsächlich während des Blasenkollapses stattfindet. Ein Multiplexing der SAXS-Messungen, um direkt ein 2D-Bild derNP-Verteilung zu erhalten, erfolgt durch Hartmann-Blenden artiger Multikontrast-Bildgebung. Zu diesem Zweck wird ein breiter Röntgen- strahl durch eine maßgeschneiderte Hartmann-Blende beziehungsweise die neu entwickelten gestapelten v Kurzfassung Röntgenlinsenarrays (Compound Array Refractive Lenses, CARLs) in ein 2D-Array von Teilstrahlen aufgeteilt. Für die hierarchische Abbildung des Ablationsprozesses werden die Kontraste Transmission und Streuung dieser Einzelbild Multikontrast-Bildgebung (Single-Exposure Multi-Contrast Imaging, SEMCI) verwendet. Die in situ Größenreduktion vonNP aus
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