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- poly(N-isopropyl methacrylamide) (1)
- poly(N-isopropylacrylamide) (1)
- poly(N-vinyl isobutyramide) (1)
- poly(N-vinylcaprolactam) (1)
- poly(O-phospho-L-Serin) (1)
- poly(O-phospho-L-serine) (1)
- poly(amidoamine) (1)
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- reversible addition-fragmentation chain transfer (1)
- reversible shape-memory actuator (1)
- reversible work share (1)
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- rheology (1)
- rhodamine b (1)
- ring closing metathesis (1)
- ring-closing metathesis (1)
- ring-closure (1)
- rising bubble (1)
- rod (1)
- rod-coil; amphiphilic block copolymers; polypeptide; solid state; structure; morphology; kolloids; self assembly; vesicles; switchable aggregates (1)
- roughness (1)
- rp-hplc (1)
- ruthenium carbene (1)
- salt melt (1)
- samples (1)
- scalar product of force and displacement (1)
- scale (1)
- schaltbare Materialien (1)
- schaltbare Polymere (1)
- schizophrenes Verhalten (1)
- schizophrenic behavior (1)
- schmelzbares PAN (1)
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- science communication (1)
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- second harmonic generation (1)
- secondary structure (1)
- sel (1)
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- selbstassemblierende Monolagen (1)
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- separation (1)
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- spacer (1)
- spacer group (1)
- spatial-organization (1)
- speciation (1)
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- spectroscopic ruler (1)
- spektroskopisches Lineal (1)
- spent coffee (1)
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- spezifische Wechselwirkungen (1)
- spherical polyelectrolyte brushes (1)
- spider silk (1)
- spiked and crumble gold nanotriangles (1)
- spiropyran copolymer (1)
- square planar (1)
- squaric acid (1)
- stability (1)
- stannous octoate (1)
- star polymers (1)
- stark eutektisches Lösungsmittel (1)
- state (1)
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- static hyperpolarizability (1)
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- statistische Versuchsplanung (Design of Experiments) (1)
- steigende Blasen (1)
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- stickstoffdotierte Kohlenstoffe (1)
- stilbene (1)
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- stimuli-sensitive (1)
- stokes shift (1)
- strain energy (1)
- strand breakage (1)
- stress relaxation (1)
- stress-relaxation (1)
- structural-characterization (1)
- styrene (1)
- substituted stilbenes (1)
- substrate (1)
- sulfobetain (1)
- sulfoxides (1)
- sulfur host (1)
- sulfur ligands (1)
- supercapacitor (1)
- supercritical carbon dioxide (scCO₂) (1)
- superparamagnetic (1)
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- supported gold (1)
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- surface chemistry (1)
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- surfaces and interfaces (1)
- surfactant (1)
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- sustainability (1)
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- switch (1)
- switchable block copolymer (1)
- switches (1)
- synthetische Biologie (1)
- system-immanent forces (1)
- systemimmanente Kräfte (1)
- sättigbarer Absorber (1)
- tamplat unterstütze Anordnung von weichen Partikeln (1)
- tandem mass spectrometry (1)
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- tannic acid (1)
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- tannins (1)
- temperature (1)
- temperature phase (1)
- temperaturschaltbar (1)
- template (1)
- template assisted alignment of soft particles (1)
- template phase (1)
- tensioactivos (1)
- tetrabromidocuprate(II) (1)
- tetrachlorocuprate(II) salts (1)
- thermal isomerization of azobenzene (1)
- thermal properties (1)
- thermisch angeregte Isomerisierung von Azobenzolen (1)
- thermisch schaltbar (1)
- thermisch schaltbare Polymere (1)
- thermo-responsive polymers (1)
- thermochemistry (1)
- thermometer (1)
- thermoplastic (1)
- thermoplastisch (1)
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- thermosensitive (1)
- thermosensitive polymers (1)
- thiazolium (1)
- thimerosal (1)
- thin film crystallization (1)
- thin films (1)
- thin-films (1)
- thio-dimethylarsinic acid (1)
- thio-glycosides (1)
- thiol-ene (1)
- tight-binding (1)
- time random-walks (1)
- time-dependent density functional theory (1)
- time-resolved luminescence (1)
- tin perovskites (1)
- titania (1)
- to-coil transition (1)
- total work (1)
- trafficking (1)
- trajectory (1)
- trajectory surface hopping (1)
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- uranium (VI) (1)
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- urea (1)
- valerolactone (1)
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- vitro toxicological characterization (1)
- wasser (1)
- water at alumina (1)
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- wetting (1)
- white carbon (1)
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- wood modification (1)
- wrinkled stamps (1)
- wässrige Systeme (1)
- ytterbium (1)
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- Übergangsmetall (1)
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- Überstrukturierte Komposite (1)
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- überkritisches Kohlendioxid (scCO₂) (1)
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- β-Hydroxydihydrochalcone (1)
Institute
- Institut für Chemie (552) (remove)
Im Rahmen einer explorativen Entwicklung wurde in der vorliegenden Studie ein Konzept zur Wissenschaftskommunikation für ein Graduiertenkolleg, in dem an photochemischen Prozessen geforscht wird, erstellt und anschließend evaluiert. Der Grund dafür ist die immer stärker wachsende Forderung nach Wissenschaftskommunikation seitens der Politik. Es wird darüber hinaus gefordert, dass die Kommunikation der eigenen Forschung in Zukunft integrativer Bestandteil des wissenschaftlichen Arbeitens wird. Um junge Wissenschaftler bereits frühzeitig auf diese Aufgabe vorzubereiten, wird Wissenschaftskommunikation auch in Forschungsverbünden realisiert.
Aus diesem Grund wurde in einer Vorstudie untersucht, welche Anforderungen an ein Konzept zur Wissenschaftskommunikation im Rahmen eines Forschungsverbundes gestellt werden, indem die Einstellung der Doktoranden zur Wissenschaftskommunikation sowie ihre Kommunikationsfähigkeiten anhand eines geschlossenen Fragebogens evaluiert wurden. Darüber hinaus wurden aus den Daten Wissenschaftskommunikationstypen abgeleitet. Auf Grundlage der Ergebnisse wurden unterschiedliche Wissenschaftskommunikationsmaßnahmen entwickelt, die sich in der Konzeption, den Rezipienten, sowie der Form der Kommunikation und den Inhalten unterscheiden.
Im Rahmen dieser Entwicklung wurde eine Lerneinheit mit Bezug auf die Inhalte des Graduiertenkollegs, bestehend aus einem Lehr-Lern-Experiment und den dazugehörigen Begleitmaterialien, konzipiert. Anschließend wurde die Lerneinheit in eine der Wissenschaftskommunikationsmaßnahmen integriert. Je nach Anforderung an die Doktoranden, wurden die Maßnahmen durch vorbereitende Workshops ergänzt.
Durch einen halboffenen Pre-Post-Fragebogen wurde der Einfluss der Wissenschaftskommunikationsmaßnahmen und der dazugehörigen Workshops auf die Selbstwirksamkeit der Doktoranden evaluiert, um Rückschlüsse darauf zu ziehen, wie sich die Wahrnehmung der eigenen Kommunikationsfähigkeiten durch die Interventionen verändert. Die Ergebnisse deuten darauf hin, dass die einzelnen Wissenschaftskommunikationsmaßnahmen die verschiedenen Typen in unterschiedlicher Weise beeinflussen. Es ist anzunehmen, dass es abhängig von der eigenen Einschätzung der Kommunikationsfähigkeit unterschiedliche Bedürfnisse der Förderung gibt, die durch dedizierte Wissenschaftskommunikationsmaßnahmen berücksichtigt werden können.
Auf dieser Grundlage werden erste Ansätze für eine allgemeingültige Strategie vorgeschlagen, die die individuellen Fähigkeiten zur Wissenschaftskommunikation in einem naturwissenschaftlichen Forschungsverbund fördert.
The reliance on fossil fuels has resulted in an abnormal increase in the concentration of greenhouse gases, contributing to the global climate crisis. In response, a rapid transition to renewable energy sources has begun, particularly lithium-ion batteries, playing a crucial role in the green energy transformation. However, concerns regarding the availability and geopolitical implications of lithium have prompted the exploration of alternative rechargeable battery systems, such as sodium-ion batteries. Sodium is significantly abundant and more homogeneously distributed in the crust and seawater, making it easier and less expensive to extract than lithium. However, because of the mysterious nature of its components, sodium-ion batteries are not yet sufficiently advanced to take the place of lithium-ion batteries. Specifically, sodium exhibits a more metallic character and a larger ionic radius, resulting in a different ion storage mechanism utilized in lithium-ion batteries. Innovations in synthetic methods, post-treatments, and interface engineering clearly demonstrate the significance of developing high-performance carbonaceous anode materials for sodium-ion batteries. The objective of this dissertation is to present a systematic approach for fabricating efficient, high-performance, and sustainable carbonaceous anode materials for sodium-ion batteries. This will involve a comprehensive investigation of different chemical environments and post-modification techniques as well.
This dissertation focuses on three main objectives. Firstly, it explores the significance of post-synthetic methods in designing interfaces. A conformal carbon nitride coating is deposited through chemical vapor deposition on a carbon electrode as an artificial solid-electrolyte interface layer, resulting in improved electrochemical performance. The interaction between the carbon nitride artificial interface and the carbon electrode enhances initial Coulombic efficiency, rate performance, and total capacity. Secondly, a novel process for preparing sulfur-rich carbon as a high-performing anode material for sodium-ion batteries is presented. The method involves using an oligo-3,4-ethylenedioxythiophene precursor for high sulfur content hard carbon anode to investigate the sulfur heteroatom effect on the electrochemical sodium storage mechanism. By optimizing the condensation temperature, a significant transformation in the materials’ nanostructure is achieved, leading to improved electrochemical performance. The use of in-operando small-angle X-ray scattering provides valuable insights into the interaction between micropores and sodium ions during the electrochemical processes. Lastly, the development of high-capacity hard carbon, derived from 5-hydroxymethyl furfural, is examined. This carbon material exhibits exceptional performance at both low and high current densities. Extensive electrochemical and physicochemical characterizations shed light on the sodium storage mechanism concerning the chemical environment, establishing the material’s stability and potential applications in sodium-ion batteries.
The remarkable antifouling properties of zwitterionic polymers in controlled environments are often counteracted by their delicate mechanical stability. In order to improve the mechanical stabilities of zwitterionic hydrogels, the effect of increased crosslinker densities was thus explored. In a first approach, terpolymers of zwitterionic monomer 3-[N -2(methacryloyloxy)ethyl-N,N-dimethyl]ammonio propane-1-sulfonate (SPE), hydrophobic monomer butyl methacrylate (BMA), and photo-crosslinker 2-(4-benzoylphenoxy)ethyl methacrylate (BPEMA) were synthesized. Thin hydrogel coatings of the copolymers were then produced and photo-crosslinked. Studies of the swollen hydrogel films showed that not only the mechanical stability but also, unexpectedly, the antifouling properties were improved by the presence of hydrophobic BMA units in the terpolymers.
Based on the positive results shown by the amphiphilic terpolymers and in order to further test the impact that hydrophobicity has on both the antifouling properties of zwitterionic hydrogels and on their mechanical stability, a new amphiphilic zwitterionic methacrylic monomer, 3-((2-(methacryloyloxy)hexyl)dimethylammonio)propane-1-sulfonate (M1), was synthesized in good yields in a multistep synthesis. Homopolymers of M1 were obtained by free-radical polymerization. Similarly, terpolymers of M1, zwitterionic monomer SPE, and photo-crosslinker BPEMA were synthesized by free-radical copolymerization and thoroughly characterized, including its solubilities in selected solvents.
Also, a new family of vinyl amide zwitterionic monomomers, namely 3-(dimethyl(2-(N -vinylacetamido)ethyl)ammonio)propane-1-sulfonate (M2), 4-(dimethyl(2-(N-vinylacetamido)ethyl)ammonio)butane-1-sulfonate (M3), and 3-(dimethyl(2-(N-vinylacetamido)ethyl)ammonio)propyl sulfate (M4), together with the new photo-crosslinker 4-benzoyl-N-vinylbenzamide (M5) that is well-suited for copolymerization with vinylamides, are introduced within the scope of the present work. The monomers are synthesized with good yields developing a multistep synthesis. Homopolymers of the new vinyl amide zwitterionic monomers are obtained by free-radical polymerization and thoroughly characterized. From the solubility tests, it is remarkable that the homopolymers produced are fully soluble in water, evidence of their high hydrophilicity. Copolymerization of the vinyl amide zwitterionic monomers, M2, M3, and M4 with the vinyl amide photo-crosslinker M5 proved to require very specific polymerization conditions. Nevertheless, copolymers were successfully obtained by free-radical copolymerization under appropriate conditions.
Moreover, in an attempt to mitigate the intrinsic hydrophobicity introduced in the copolymers by the photo-crosslinkers, and based on the proven affinity of quaternized diallylamines to copolymerize with vinyl amides, a new quaternized diallylamine sulfobetaine photo-crosslinker 3-(diallyl(2-(4-benzoylphenoxy)ethyl)ammonio)propane-1-sulfonate (M6) is synthesized. However, despite a priori promising copolymerization suitability, copolymerization with the vinyl amide zwitterionic monomers could not be achieved.
Global warming, driven primarily by the excessive emission of greenhouse gases such as carbon dioxide into the atmosphere, has led to severe and detrimental environmental impacts. Rising global temperatures have triggered a cascade of adverse effects, including melting glaciers and polar ice caps, more frequent and intense heat waves disrupted weather patterns, and the acidification of oceans. These changes adversely affect ecosystems, biodiversity, and human societies, threatening food security, water availability, and livelihoods. One promising solution to mitigate the harmful effects of global warming is the widespread adoption of solar cells, also known as photovoltaic cells. Solar cells harness sunlight to generate electricity without emitting greenhouse gases or other pollutants. By replacing fossil fuel-based energy sources, solar cells can significantly reduce CO2 emissions, a significant contributor to global warming. This transition to clean, renewable energy can help curb the increasing concentration of greenhouse gases in the atmosphere, thereby slowing down the rate of global temperature rise.
Solar energy’s positive impact extends beyond emission reduction. As solar panels become more efficient and affordable, they empower individuals, communities, and even entire nations to generate electricity and become less dependent on fossil fuels. This decentralized energy generation can enhance resilience in the face of climate-related challenges. Moreover, implementing solar cells creates green jobs and stimulates technological innovation, further promoting sustainable economic growth. As solar technology advances, its integration with energy storage systems and smart grids can ensure a stable and reliable energy supply, reducing the need for backup fossil fuel power plants that exacerbate environmental degradation.
The market-dominant solar cell technology is silicon-based, highly matured technology with a highly systematic production procedure. However, it suffers from several drawbacks, such as: 1) Cost: still relatively high due to high energy consumption due to the need to melt and purify silicon, and the use of silver as an electrode, which hinders their widespread availability, especially in low-income countries. 2) Efficiency: theoretically, it should deliver around 29%; however, the efficiency of most of the commercially available silicon-based solar cells ranges from 18 – 22%. 3) Temperature sensitivity: The efficiency decreases with the increase in the temperature, affecting their output. 4) Resource constraints: silicon as a raw material is unavailable in all countries, creating supply chain challenges.
Perovskite solar cells arose in 2011 and matured very rapidly in the last decade as a highly efficient and versatile solar cell technology. With an efficiency of 26%, high absorption coefficients, solution processability, and tunable band gap, it attracted the attention of the solar cells community. It represented a hope for cheap, efficient, and easily processable next-generation solar cells. However, lead toxicity might be the block stone hindering perovskite solar cells’ market reach. Lead is a heavy and bioavailable element that makes perovskite solar cells environmentally unfriendly technology. As a result, scientists try to replace lead with a more environmentally friendly element. Among several possible alternatives, tin was the most suitable element due to its electronic and atomic structure similarity to lead.
Tin perovskites were developed to alleviate the challenge of lead toxicity. Theoretically, it shows very high absorption coefficients, an optimum band gap of 1.35 eV for FASnI3, and a very high short circuit current, which nominates it to deliver the highest possible efficiency of a single junction solar cell, which is around 30.1% according to Schockly-Quisser limit. However, tin perovskites’ efficiency still lags below 15% and is irreproducible, especially from lab to lab. This humble performance could be attributed to three reasons: 1) Tin (II) oxidation to tin (IV), which would happen due to oxygen, water, or even by the effect of the solvent, as was discovered recently. 2) fast crystallization dynamics, which occurs due to the lateral exposure of the P-orbitals of the tin atom, which enhances its reactivity and increases the crystallization pace. 3) Energy band misalignment: The energy bands at the interfaces between the perovskite absorber material and the charge selective layers are not aligned, leading to high interfacial charge recombination, which devastates the photovoltaic performance. To solve these issues, we implemented several techniques and approaches that enhanced the efficiency of tin halide perovskites, providing new chemically safe solvents and antisolvents. In addition, we studied the energy band alignment between the charge transport layers and the tin perovskite absorber.
Recent research has shown that the principal source of tin oxidation is the solvent known as dimethylsulfoxide, which also happens to be one of the most effective solvents for processing perovskite. The search for a stable solvent might prove to be the factor that makes all the difference in the stability of tin-based perovskites. We started with a database of over 2,000 solvents and narrowed it down to a series of 12 new solvents that are suitable for processing FASnI3 experimentally. This was accomplished by looking into 1) the solubility of the precursor chemicals FAI and SnI2, 2) the thermal stability of the precursor solution, and 3) the potential to form perovskite. Finally, we show that it is possible to manufacture solar cells using a novel solvent system that outperforms those produced using DMSO. The results of our research give some suggestions that may be used in the search for novel solvents or mixes of solvents that can be used to manufacture stable tin-based perovskites.
Due to the quick crystallization of tin, it is more difficult to deposit tin-based perovskite films from a solution than manufacturing lead-based perovskite films since lead perovskite is more often utilized. The most efficient way to get high efficiencies is to deposit perovskite from dimethyl sulfoxide (DMSO), which slows down the quick construction of the tin-iodine network that is responsible for perovskite synthesis. This is the most successful approach for achieving high efficiencies. Dimethyl sulfoxide, which is used in the processing, is responsible for the oxidation of tin, which is a disadvantage of this method. This research presents a potentially fruitful alternative in which 4-(tert-butyl) pyridine can substitute dimethyl sulfoxide in the process of regulating crystallization without causing tin oxidation to take place. Perovskite films that have been formed from pyridine have been shown to have a much-reduced defect density. This has resulted in increased charge mobility and better photovoltaic performance, making pyridine a desirable alternative for use in the deposition of tin perovskite films.
The precise control of perovskite precursor crystallization inside a thin film is of utmost importance for optimizing the efficiency and manufacturing of solar cells. The deposition process of tin-based perovskite films from a solution presents difficulties due to the quick crystallization of tin compared to the more often employed lead perovskite. The optimal approach for attaining elevated efficiencies entails using dimethyl sulfoxide (DMSO) as a medium for depositing perovskite. This choice of solvent impedes the tin-iodine network’s fast aggregation, which plays a crucial role in the production of perovskite. Nevertheless, this methodology is limited since the utilization of dimethyl sulfoxide leads to the oxidation of tin throughout the processing stage. In this thesis, we present a potentially advantageous alternative approach wherein 4-(tert-butyl) pyridine is proposed as a substitute for dimethyl sulfoxide in regulating crystallization processes while avoiding the undesired consequence of tin oxidation. Films of perovskite formed using pyridine as a solvent have a notably reduced density of defects, resulting in higher mobility of charges and improved performance in solar applications. Consequently, the utilization of pyridine for the deposition of tin perovskite films is considered advantageous.
Tin perovskites are suffering from an apparent energy band misalignment. However, the band diagrams published in the current body of research display contradictions, resulting in a dearth of unanimity. Moreover, comprehensive information about the dynamics connected with charge extraction is lacking. This thesis aims to ascertain the energy band locations of tin perovskites by employing the kelvin probe and Photoelectron yield spectroscopy methods. This thesis aims to construct a precise band diagram for the often-utilized device stack. Moreover, a comprehensive analysis is performed to assess the energy deficits inherent in the current energetic structure of tin halide perovskites. In addition, we investigate the influence of BCP on the improvement of electron extraction in C60/BCP systems, with a specific emphasis on the energy factors involved. Furthermore, transient surface photovoltage was utilized to investigate the charge extraction kinetics of frequently studied charge transport layers, such as NiOx and PEDOT as hole transport layers and C60, ICBA, and PCBM as electron transport layers. The Hall effect, KP, and TRPL approaches accurately ascertain the p-doping concentration in FASnI3. The results consistently demonstrated a value of 1.5 * 1017 cm-3. Our research findings highlight the imperative nature of autonomously constructing the charge extraction layers for tin halide perovskites, apart from those used for lead perovskites.
The crystallization of perovskite precursors relies mainly on the utilization of two solvents. The first one dissolves the perovskite powder to form the precursor solution, usually called the solvent. The second one precipitates the perovskite precursor, forming the wet film, which is a supersaturated solution of perovskite precursor and in the remains of the solvent and the antisolvent. Later, this wet film crystallizes upon annealing into a full perovskite crystallized film. In our research context, we proposed new solvents to dissolve FASnI3, but when we tried to form a film, most of them did not crystallize. This is attributed to the high coordination strength between the metal halide and the solvent molecules, which is unbreakable by the traditionally used antisolvents such as Toluene and Chlorobenzene. To solve this issue, we introduce a high-throughput antisolvent screening in which we screened around 73 selected antisolvents against 15 solvents that can form a 1M FASnI3 solution. We used for the first time in tin perovskites machine learning algorithm to understand and predict the effect of an antisolvent on the crystallization of a precursor solution in a particular solvent. We relied on film darkness as a primary criterion to judge the efficacy of a solvent-antisolvent pair. We found that the relative polarity between solvent and antisolvent is the primary factor that affects the solvent-antisolvent interaction. Based on our findings, we prepared several high-quality tin perovskite films free from DMSO and achieved an efficiency of 9%, which is the highest DMSO tin perovskite device so far.
Im Rahmen dieser Dissertation wurden die erstmaligen Totalsynthesen der Arylnaphthalen-Lignane Alashinol D, Vitexdoin C, Vitrofolal E, Noralashinol C1 und Ternifoliuslignan E vorgestellt. Der Schlüsselschritt der entwickelten Methode, basiert auf einer regioselektiven intramolekularen Photo-Dehydro-Diels-Alder (PDDA)-Reaktion, die mittels UV-Strahlung im Durchflussreaktor durchgeführt wurde. Bei der Synthese der PDDA-Vorläufer (Diarylsuberate) wurde eine Synthesestrategie nach dem Baukastenprinzip verfolgt. Diese ermöglicht die Darstellung asymmetrischer komplexer Systeme aus nur wenigen Grundbausteinen und die Totalsynthese einer Vielzahl an Lignanen. In systematischen Voruntersuchungen konnte zudem die klare Überlegenheit der intra- gegenüber der intermolekularen PDDA-Reaktion aufgezeigt werden. Dabei stellte sich eine Verknüpfung der beiden Arylpropiolester über einen Korksäurebügel, in para-Position, als besonders effizient heraus. Werden asymmetrisch substituierte Diarylsuberate, bei denen einer der endständigen Estersubstituenten durch eine Trimethylsilyl-Gruppe oder ein Wasserstoffatom ersetzt wurde, verwendet, durchlaufen diese Systeme eine regioselektive Cyclisierung und als Hauptprodukt werden Naphthalenophane mit einem Methylester in 3-Position erhalten. Mit Hilfe von umfangreichen Experimenten zur Funktionalisierung der 4-Position, konnte zudem gezeigt werden, dass die Substitution der nucleophilen Cycloallen-Intermediate, während der PDDA-Reaktion, generell durch die Zugabe von N-Halogen-Succinimiden möglich ist. In Anbetracht der geringen Ausbeuten haben diese intermolekularen Abfangreaktionen, jedoch keinen präparativen Nutzen für die Totalsynthesen von Lignanen. Mit dem Ziel die allgemeinen photochemischen Reaktionsbedingungen zu optimieren, wurde erstmalig die triplettsensibilisierte PDDA-Reaktion vorgestellt. Durch die Verwendung von Xanthon als Sensibilisator wurde der Einsatz von effizienteren UVA-Lichtquellen ermöglicht, wodurch die Gefahr einer Photozersetzung durch Überbestrahlung minimiert wurde. Im Vergleich zur direkten Anregung mit UVB-Strahlung, konnten die Ausbeuten mit indirekter Anregung durch einen Photokatalysator signifikant gesteigert werden. Die grundlegenden Erkenntnisse und die entwickelten Synthesestrategien dieser Arbeit, können dazu beitragen zukünftig die Erschließung neuer pharmakologisch interessanter Lignane voranzutreiben.
1 Bisher ist nur die semisynthetische Darstellung von Noralashinol C ausgehend von Hydroxymatairesinol literaturbekannt.
The retention of actinides in different oxidation states (An(X), X = III, IV, VI) by a calcium-silicate-hydrate (C-S-H) phase with a Ca/Si (C/S) ratio of 0.8 was investigated in the presence of gluconate (GLU). The actinides considered were Am(III), Th(IV), Pu(IV), and U(VI). Eu(III) was investigated as chemical analogue for Am(III) and Cm(III). In addition to the ternary systems An(X)/GLU/C-S-H, also binary systems An(X)/C-S-H, GLU/C-S-H, and An(X)/GLU were studied. Complementary analytical techniques were applied to address the different specific aspects of the binary and ternary systems. Time-resolved laser-induced luminescence spectroscopy (TRLFS) was applied in combination with parallel factor analysis (PARAFAC) to identify retained species and to monitor species-selective sorption kinetics. ¹³C and ²⁹Si magic-angle-spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy and X-ray photoelectron spectroscopy (XPS) were applied to determine the bulk structure and the composition of the C-S-H surface, respectively, in the absence and presence of GLU. The interaction of Th(IV) with GLU in different electrolytes was studied by capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS). The influence of GLU on An(X) retention was investigated for a large concentration range up to 10⁻² M. The results showed that GLU had little to no effect on the overall An(X) retention by C-S-H with C/S of 0.8, regardless of the oxidation state of the actinides. For Eu(III), the TRLFS investigations additionally implied the formation of a Eu(III)-bearing precipitate with dissolved constituents of the C-S-H phase, which becomes structurally altered by the presence of GLU. For U(VI) sorption on the C-S-H phase, only a small influence of GLU could be established in the luminescence spectroscopic investigations, and no precipitation of U(VI)-containing secondary phases could be identified.
Despite the popularity of thermoresponsive polymers, much is still unknown about their behavior, how it is triggered, and what factors influence it, hindering the full exploitation of their potential. One particularly puzzling phenomenon is called co-nonsolvency, in which a polymer is soluble in two individual solvents, but counter-intuitively becomes insoluble in mixtures of both. Despite the innumerous potential applications of such systems, including actuators, viscosity regulators and as carrier structures, this field has not yet been extensively studied apart from the classical example of poly(N isopropyl acrylamide) (PNIPAM) in mixtures of water and methanol. Therefore, this thesis focuses on evaluating how changes in the chemical structure of the polymers impact the thermoresponsive, aggregation and co-nonsolvency behaviors of both homopolymers and amphiphilic block copolymers. Within this scope, both the synthesis of the polymers and their characterization in solution is investigated. Homopolymers were synthesized by conventional free radical polymerization, whereas block copolymers were synthesized by consecutive reversible addition fragmentation chain transfer (RAFT) polymerizations. The synthesis of the monomers N isopropyl methacrylamide (NIPMAM) and N vinyl isobutyramide (NVIBAM), as well as a few chain transfer agents is also covered. Through turbidimetry measurements, the thermoresponsive and co-nonsolvency behavior of PNIPMAM and PNVIBAM homopolymers is then compared to the well-known PNIPAM, in aqueous solutions with 9 different organic co-solvents. Additionally, the effects of end-groups, molar mass, and concentration are investigated. Despite the similarity of their chemical structures, the 3 homopolymers show significant differences in transition temperatures and some divergences in their co-nonsolvency behavior. More complex systems are also evaluated, namely amphiphilic di- and triblock copolymers of PNIPAM and PNIPMAM with polystyrene and poly(methyl methacrylate) hydrophobic blocks. Dynamic light scattering is used to evaluate their aggregation behavior in aqueous and mixed aqueous solutions, and how it is affected by the chemical structure of the blocks, the chain architecture, presence of cosolvents and polymer concentration. The results obtained shed light into the thermoresponsive, co-nonsolvency and aggregation behavior of these polymers in solution, providing valuable information for the design of systems with a desired aggregation behavior, and that generate targeted responses to temperature and solvent mixture changes.
The urge of light utilization in fabrication of materials is as encouraging as challenging. Steadily increasing energy consumption in accordance with rapid population growth, is requiring a corresponding solution within the same rate of occurrence speed. Therefore, creating, designing and manufacturing materials that can interact with light and in further be applicable as well as disposable in photo-based applications are very much under attention of researchers. In the era of sustainability for renewable energy systems, semiconductor-based photoactive materials have received great attention not only based on solar and/or hydrocarbon fuels generation from solar energy, but also successful stimulation of photocatalytic reactions such as water splitting, pollutant degradation and organic molecule synthesisThe turning point had been reached for water splitting with an electrochemical cell consisting of TiO2-Pt electrode illuminated by UV light as energy source rather than an external voltage, that successfully pursued water photolysis by Fujishima and Honda in 1972. Ever since, there has been a great deal of interest in research of semiconductors (e.g. metal oxide, metal-free organic, noble-metal complex) exhibiting effective band gap for photochemical reactions. In the case of environmental friendliness, toxicity of metal-based semiconductors brings some restrictions in possible applications. Regarding this, very robust and ‘earth-abundant’ organic semiconductor, graphitic carbon nitride has been synthesized and successfully applied in photoinduced applications as novel photocatalyst. Properties such as suitable band gap, low charge carrier recombination and feasibility for scaling up, pave the way of advance combination with other catalysts to gather higher photoactivity based on compatible heterojunction.
This dissertation aims to demonstrate a series of combinations between organic semiconductor g-CN and polymer materials that are forged through photochemistry, either in synthesis or in application. Fabrication and design processes as well as applications performed in accordance to the scope of thesis will be elucidated in detail. In addition to UV light, more attention is placed on visible light as energy source with a vision of more sustainability and better scalability in creation of novel materials and solar energy based applications.
Lithium-ion capacitors (LICs) are promising energy storage devices by asymmetrically combining anode with a high energy density close to lithium-ion batteries and cathode with a high power density and long-term stability close to supercapacitors. For the further improvement of LICs, the development of electrode materials with hierarchical porosity, nitrogen-rich lithiophilic sites, and good electrical conductivity is essential. Nitrogen-rich all-carbon composite hybrids are suitable for these conditions along with high stability and tunability, resulting in a breakthrough to achieve the high performance of LICs. In this thesis, two different all-carbon composites are suggested to unveil how the pore structure of lithiophilic composites influences the properties of LICs. Firstly, the composite with 0-dimensional zinc-templated carbon (ZTC) and hexaazatriphenylene-hexacarbonitrile (HAT) is examined how the pore structure is connected to Li-ion storage property as LIC electrode. As the pore structure of HAT/ZTC composite is easily tunable depending on the synthetic factor and ratio of each component, the results will allow deeper insights into Li-ion dynamics in different porosity, and low-cost synthesis by optimization of the HAT:ZTC ratio. Secondly, the composite with 1-dimensional nanoporous carbon fiber (ACF) and cost-effective melamine is proposed as a promising all-carbon hybrid for large-scale application. Since ACF has ultra-micropores, the numerical structure-property relationships will be calculated out not only from total pore volume but more specifically from ultra-micropore volume. From these results above, it would be possible to understand how hybrid all-carbon composites interact with lithium ions in nanoscale as well as how structural properties affect the energy storage performance. Based on this understanding derived from the simple materials modeling, it will provide a clue to design the practical hybrid materials for efficient electrodes in LICs.
Fabricating electronic devices from natural, renewable resources has been a common goal in engineering and materials science for many years. In this regard, carbon is of special significance due to its biological compatibility. In the laboratory, carbonized materials and their composites have been proven as promising solutions for a range of future applications in electronics, optoelectronics, or catalytic systems. On the industrial scale, however, their application is inhibited by tedious and expensive preparation processes and a lack of control over the processing and material parameters. Therefore, we are exploring new concepts for the direct utilization of functional carbonized materials in electronic applications. In particular, laser-induced carbonization (carbon laser-patterning (CLaP)) is emerging as a new tool for the precise and selective synthesis of functional carbon-based materials for flexible on-chip applications.
We developed an integrated approach for on-the-spot laser-induced synthesis of flexible, carbonized films with specific functionalities. To this end, we design versatile precursor inks made from naturally abundant starting compounds and reactants to cast films which are carbonized with an infrared laser to obtain functional patterns of conductive porous carbon networks. In our studies we obtained deep mechanistic insights into the formation process and the microstructure of laser-patterned carbons (LP-C). We shed light on the kinetic reaction mechanism based on the interplay between the precursor properties and the reaction conditions. Furthermore, we investigated the use of porogens, additives, and reactants to provide a toolbox for the chemical and physical fine-tuning of the electronic and surface properties and the targeted integration of functional sites into the carbon network. Based on this knowledge, we developed prototype resistive chemical and mechanical sensors. In further studies, we show the applicability of LP-C as electrode materials in electrocatalytic and charge-storage applications.
To put our findings into a common perspective, our results are embedded into the context of general carbonization strategies, fundamentals of laser-induced materials processing, and a broad literature review on state-of-the-art laser-carbonization, in the general part.
Hybrid nanomaterials offer the combination of individual properties of different types of nanoparticles. Some strategies for the development of new nanostructures in larger scale rely on the self-assembly of nanoparticles as a bottom-up approach. The use of templates provides ordered assemblies in defined patterns. In a typical soft-template, nanoparticles and other surface-active agents are incorporated into non-miscible liquids. The resulting self-organized dispersions will mediate nanoparticle interactions to control the subsequent self-assembly. Especially interactions between nanoparticles of very different dispersibility and functionality can be directed at a liquid-liquid interface.
In this project, water-in-oil microemulsions were formulated from quasi-ternary mixtures with Aerosol-OT as surfactant. Oleyl-capped superparamagnetic iron oxide and/or silver nanoparticles were incorporated in the continuous organic phase, while polyethyleneimine-stabilized gold nanoparticles were confined in the dispersed water droplets. Each type of nanoparticle can modulate the surfactant film and the inter-droplet interactions in diverse ways, and their combination causes synergistic effects. Interfacial assemblies of nanoparticles resulted after phase-separation. On one hand, from a biphasic Winsor type II system at low surfactant concentration, drop-casting of the upper phase afforded thin films of ordered nanoparticles in filament-like networks. Detailed characterization proved that this templated assembly over a surface is based on the controlled clustering of nanoparticles and the elongation of the microemulsion droplets. This process offers versatility to use different nanoparticle compositions by keeping the surface functionalization, in different solvents and over different surfaces. On the other hand, a magnetic heterocoagulate was formed at higher surfactant concentration, whose phase-transfer from oleic acid to water was possible with another auxiliary surfactant in ethanol-water mixture. When the original components were initially mixed under heating, defined oil-in-water, magnetic-responsive nanostructures were obtained, consisting on water-dispersible nanoparticle domains embedded by a matrix-shell of oil-dispersible nanoparticles.
Herein, two different approaches were demonstrated to form diverse hybrid nanostructures from reverse microemulsions as self-organized dispersions of the same components. This shows that microemulsions are versatile soft-templates not only for the synthesis of nanoparticles, but also for their self-assembly, which suggest new approaches towards the production of new sophisticated nanomaterials in larger scale.
Solar photocatalysis is the one of leading concepts of research in the current paradigm of sustainable chemical industry. For actual practical implementation of sunlight-driven catalytic processes in organic synthesis, a cheap, efficient, versatile and robust heterogeneous catalyst is necessary. Carbon nitrides are a class of organic semiconductors who are known to fulfill these requirements.
First, current state of solar photocatalysis in economy, industry and lab research is overviewed, outlining EU project funding, prospective synthetic and reforming bulk processes, small scale solar organic chemistry, and existing reactor designs and prototypes, concluding feasibility of the approach.
Then, the photocatalytic aerobic cleavage of oximes to corresponding aldehydes and ketones by anionic poly(heptazine imide) carbon nitride is discussed. The reaction provides a feasible method of deprotection and formation of carbonyl compounds from nitrosation products and serves as a convenient model to study chromoselectivity and photophysics of energy transfer in heterogeneous photocatalysis.
Afterwards, the ability of mesoporous graphitic carbon nitride to conduct proton-coupled electron transfer was utilized for the direct oxygenation of 1,3-oxazolidin-2-ones to corresponding 1,3-oxazlidine-2,4-diones. This reaction provides an easier access to a key scaffold of diverse types of drugs and agrochemicals.
Finally, a series of novel carbon nitrides based on poly(triazine imide) and poly(heptazine imide) structure was synthesized from cyanamide and potassium rhodizonate. These catalysts demonstrated a good performance in a set of photocatalytic benchmark reactions, including aerobic oxidation, dual nickel photoredox catalysis, hydrogen peroxide evolution and chromoselective transformation of organosulfur precursors.
Concluding, the scope of carbon nitride utilization for net-oxidative and net-neutral photocatalytic processes was expanded, and a new tunable platform for catalyst synthesis was discovered.
Lanthanide based ceria nanomaterials are important practical materials due to their redox properties that are useful in technology and life sciences. This PhD thesis examined various properties and potential for catalytic and bio-applications of Ln3+-doped ceria nanomaterials. Ce1-xGdxO2-y: Eu3+, gadolinium doped ceria (GDC) (0 ≤ x ≤ 0.4) nanoparticles were synthesized by flame spray pyrolysis (FSP) and studied, followed by 15 % CexZr1-xO2-y: Eu3+|YSZ (0 ≤ x ≤ 1) nanocomposites. Furthermore, Ce1-xYb xO2-y (0.004 ≤ x ≤ 0.22) nanoparticles were synthesized by thermal decomposition and characterized. Finally, CeO2-y: Eu3+ nanoparticles were synthesized by a microemulsion method, biofunctionalized and characterized. The studies undertaken presents a novel approach to structurally elucidate ceria-based nanomaterials by way of Eu3+ and Yb3+ spectroscopy and processing the spectroscopic data with the multi-way decomposition method PARAFAC. Data sets of the three variables: excitation wavelength, emission wavelength and time were used to perform the deconvolution of spectra.
GDC nanoparticles from FSP are nano-sized and of roughly cubic shape and crystal structure (Fm3̅m). Raman data revealed four vibrational modes exhibited by Gd3+ containing samples whereas CeO2-y: Eu3+ displays only two. The room temperature, time-resolved emission spectra recorded at λexcitation = 464 nm show that Gd3+ doping results in significantly altered emission spectra compared to pure ceria. The PARAFAC analysis for the pure ceria samples reveals two species; a high-symmetry species and a low-symmetry species. The GDC samples yield two low-symmetry spectra in the same experiment. High-resolution emission spectra recorded at 4 K after probing the 5D0-7F0 transition revealed additional variation in the low symmetry Eu3+ sites in pure ceria and GDC. The data of the Gd3+-containing samples indicates that the average charge density around the Eu3+ ions in the lattice is inversely related to Gd3+ and oxygen vacancy concentration.
The particle crystallites of the 773 K and 1273 K annealed Yb3+ -ceria nanostructure materials are nano-sized and have a cubic fluorite structure with four Raman vibrational modes. Elemental maps clearly show that cluster formation occurs for 773 K annealed with high Yb3+ ion concentration from 15 mol % in the ceria lattice. These clusters are destroyed with annealing to 1273 K. The emission spectra observed from room temperature and 4 K measurements for the Ce1-xYb xO2-y samples have a manifold that corresponds to the 2F5/2-2F7/2 transition of Yb3+ ions. Some small shifts are observed in the Stark splitting pattern and are induced by the variations of the crystal field influenced by where the Yb3+ ions are located in the crystal lattices in the samples. Upon mixing ceria with high Yb3+ concentrations, the 2F5/2-2F7/2 transition is also observed in the Stark splitting pattern, but the spectra consist of two broad high background dominated peaks. Annealing the nanomaterials at 1273 K for 2 h changes the spectral signature as new peaks emerge. The deconvolution yielded luminescence decay kinetics as well as the accompanying luminescence spectra of three species for each of the low Yb3+ doped ceria samples annealed at 773 K and one species for the 1273 K annealed samples. However, the ceria samples with high Yb3+ concentration annealed at the two temperatures yielded one species with lower decay times as compared to the Yb3+ doped ceria samples after PARAFAC analysis.
Through the calcination of the nanocomposites at two high temperatures, the evolution of the emission patterns from specific Eu3+ lattice sites to indicate structural changes for the nanocomposites was followed. The spectroscopy results effectively complemented the data obtained from the conventional techniques. Annealing the samples at 773 K, resulted in amorphous, unordered domains whereas the TLS of the 1273 K nanocomposites reveal two distinct sites, with most red shifted Eu3+ species coming from pure Eu3+ doped ZrO2 on the YSZ support.
Finally, for Eu3+ doped ceria, successful transfer from hydrophobic to water phase and subsequent biocompatibility was achieved using ssDNA. PARAFAC analysis for the Eu3+ in nanoparticles dispersed in toluene and water revealed one Eu3+ species, with slightly differing surface properties for the nanoparticles as far as the luminescence kinetics and solvent environments were concerned. Several functionalized nanoparticles conjugated onto origami triangles after hybridization were visualized by atomic force microscopy (AFM). Putting all into consideration, Eu3+ and Yb3+ spectroscopy was used to monitor the structural changes and determining the feasibility of the nanoparticle transfer into water. PARAFAC proves to be a powerful tool to analyze lanthanide spectra in crystalline solid materials and in solutions, which are characterized by numerous Stark transitions and where measurements usually yield a superposition of different emission contributions to any given spectrum.
Soft-template strategy enables the fabrication of composite nanomaterials with desired functionalities and structures. In this thesis, soft templates, including poly(ionic liquid) nanovesicles (PIL NVs), self-assembled polystyrene-b-poly(2-vinylpyridine) (PS-b-P2VP) particles, and glycopeptide (GP) biomolecules have been applied for the synthesis of versatile composite particles of PILs/Cu, molybdenum disulfide/carbon (MoS2/C), and GP-carbon nanotubes-metal (GP-CNTs-metal) composites, respectively. Subsequently, their possible applications as efficient catalysts in two representative reactions, i.e. CO2 electroreduction (CO2ER) and reduction of 4-nitrophenol (4-NP), have been studied, respectively.
In the first work, PIL NVs with a tunable particle size of 50 to 120 nm and a shell thickness of 15 to 60 nm have been prepared via one-step free radical polymerization. By increasing monomer concentration for polymerization, their nanoscopic morphology can evolve from hollow NVs to dense spheres, and finally to directional worms, in which a multi-lamellar packing of PIL chains occurred in all samples. The obtained PIL NVs with varied shell thickness have been in situ functionalized with ultra-small Cu nanoparticles (Cu NPs, 1-3 nm) and subsequently employed as the electrocatalysts for CO2ER. The hollow PILs/Cu composite catalysts exhibit a 2.5-fold enhancement in selectivity towards C1 products compared to the pristine Cu NPs. This enhancement is primarily attributed to the strong electronic interactions between the Cu NPs and the surface functionalities of PIL NVs. This study casts new aspects on using nanostructured PILs as novel electrocatalyst supports in efficient CO2 conversion.
In the second work, a novel approach towards fast degradation of 4-NP has been developed using porous MoS2/C particles as catalysts, which integrate the intrinsically catalytic property of MoS2 with its photothermal conversion capability. Various MoS2/C composite particles have been prepared using assembled PS-b-P2VP block copolymer particles as sacrificed soft templates. Intriguingly, the MoS2/C particles exhibit tailored morphologies including pomegranate-like, hollow, and open porous structures. Subsequently, the photothermal conversion performance of these featured particles has been compared under near infrared (NIR) light irradiation. When employing the open porous MoS2/C particles as the catalyst for the reduction of 4-NP, the reaction rate constant has increased by 1.5-fold under light illumination. This catalytic enhancement mainly results from the open porous architecture and photothermal conversion performance of the MoS2 particles. This proposed strategy offers new opportunities for efficient photothermal-assisted catalysis.
In the third work, a facile and green approach towards the fabrication of GP-CNTs-metal composites has been proposed, which utilizes a versatile GP biomolecule both as a stabilizer for CNTs in water and as a reducing agent for noble metal ions. The abundant hydrogen bonds in GP molecules bestow the formed GP-CNTs with excellent plasticity, enabling the availability of polymorphic CNTs species ranging from dispersion to viscous paste, gel, and even dough by increasing their concentration. The GP molecules can reduce metal precursors at room temperature without additional reducing agents, enabling the in situ immobilization of metal NPs (e.g. Au, Ag, and Pd) on the CNTs surface. The combination of excellent catalytic property of Pd NPs with photothermal conversion capability of CNTs makes the GP-CNTs-Pd composite a promising catalyst for the efficient degradation of 4-NP. The obtained composite displays a 1.6-fold increase in conversion under NIR light illumination in the reduction of 4-NP, mainly owing to the strong light-to-heat conversion effect of CNTs. Overall, the proposed method opens a new avenue for the synthesis of CNTs composite as a sustainable and versatile catalyst platform.
The results presented in the current thesis demonstrate the significance of using soft templates for the synthesis of versatile composites with tailored nanostructure and functionalities. The investigation of these composite nanomaterials in the catalytic reactions reveals their potential in the development of desired catalysts for emerging catalytic processes, e.g. photothermal-assisted catalysis and electrocatalysis.
In dieser Dissertation konnten erfolgreich mechanisch stabile Hydrogele über eine freie radikalische Polymerisation (FRP) in Wasser synthetisiert werden. Dabei diente vor allem das Sulfobetain SPE als Monomer. Dieses wurde mit dem über eine nukleophile Substitution erster bzw. zweiter Ordnung hergestellten Vernetzer TMBEMPA/Br umgesetzt.
Die entstandenen Netzwerke wurden im Gleichgewichtsquellzustand im Wesentlichen mittels Niederfeld-Kernresonanzspektroskopie, Röntgenkleinwinkelstreuung (SAXS), Rasterelektronenmikroskopie mit Tieftemperaturtechnik (Kryo-REM), dynamisch-mechanische Analyse (DMA), Rheologie, thermogravimetrische Analyse (TGA) und dynamische Differenzkalorimetrie (DSC) analysiert.
Das hierarchisch aufgebaute Netzwerk wurde anschließend für die matrixgesteuerten Mineralisation von Calciumphosphat und –carbonat genutzt. Über das alternierende Eintauchverfahren (engl. „alternate soaking method“) und der Variation von Mineralisationsparametern, wie pH-Wert, Konzentration c und Temperatur T konnten dann verschiedene Modifikationen des Calciumphosphats generiert werden. Das entstandene Hybridmaterial wurde qualitativ mittels Röntgenpulverdiffraktometrie (XRD), abgeschwächte Totalreflexion–fouriertransformierte Infrarot Spektroskopie (ATR-FTIR), Raman-Spektroskopie, Rasterelektronenmikroskopie (REM) mit energiedispersiver Röntgenspektroskopie (EDXS) und optischer Mikroskopie (OM) als auch quantitative mittels Gravimetrie und TGA analysiert.
Für die potentielle Verwendung in der Medizintechnik, z.B. als Implantatmaterial, ist die grundlegende Einschätzung der Wechselwirkung zwischen Hydrogel bzw. Hybridmaterial und verschiedener Zelltypen unerlässlich. Dazu wurden verschiedene Zelltypen, wie Einzeller, Bakterien und adulte Stammzellen verwendet. Die Wechselwirkung mit Peptidsequenzen von Phagen komplettiert das biologische Unterkapitel.
Hydrogele sind mannigfaltig einsetzbar. Diese Arbeit fasst daher weitere Projektperspektiven, auch außerhalb des biomedizinischem Anwendungsspektrums, auf. So konnten erste Ansätze zur serienmäßige bzw. maßgeschneiderte Produktion über das „Inkjet“ Verfahren erreicht werden. Um dies ermöglichen zu können wurden erfolgreich weitere Synthesestrategien, wie die Photopolymerisation und die redoxinitiierte Polymerisation, ausgenutzt. Auch die Eignung als Filtermaterial oder Superabsorber wurde analysiert.
Complex emulsions are dispersions of kinetically stabilized multiphasic emulsion droplets comprised of two or more immiscible liquids that provide a novel material platform for the generation of active and dynamic soft materials. In recent years, the intrinsic reconfigurable morphological behavior of complex emulsions, which can be attributed to the unique force equilibrium between the interfacial tensions acting at the various interfaces, has become of fundamental and applied interest. As such, particularly biphasic Janus droplets have been investigated as structural templates for the generation of anisotropic precision objects, dynamic optical elements or as transducers and signal amplifiers in chemo- and bio-sensing applications. In the present thesis, switchable internal morphological responses of complex droplets triggered by stimuli-induced alterations of the balance of interfacial tensions have been explored as a universal building block for the design of multiresponsive, active, and adaptive liquid colloidal systems. A series of underlying principles and mechanisms that influence the equilibrium of interfacial tensions have been uncovered, which allowed the targeted design of emulsion bodies that can alter their shape, bind and roll on surfaces, or change their geometrical shape in response to chemical stimuli. Consequently, combinations of the unique triggerable behavior of Janus droplets with designer surfactants, such as a stimuli-responsive photosurfactant (AzoTAB) resulted for instance in shape-changing soft colloids that exhibited a jellyfish inspired buoyant motion behavior, holding great promise for the design of biological inspired active material architectures and transformable soft robotics.
In situ observations of spherical Janus emulsion droplets using a customized side-view microscopic imaging setup with accompanying pendant dropt measurements disclosed the sensitivity regime of the unique chemical-morphological coupling inside complex emulsions and enabled the recording of calibration curves for the extraction of critical parameters of surfactant effectiveness. The deduced new "responsive drop" method permitted a convenient and cost-efficient quantification and comparison of the critical micelle concentrations (CMCs) and effectiveness of various cationic, anionic, and nonionic surfactants. Moreover, the method allowed insightful characterization of stimuli-responsive surfactants and monitoring of the impact of inorganic salts on the CMC and surfactant effectiveness of ionic and nonionic surfactants. Droplet functionalization with synthetic crown ether surfactants yielded a synthetically minimal material platform capable of autonomous and reversible adaptation to its chemical environment through different supramolecular host-guest recognition events. Addition of metal or ammonium salts resulted in the uptake of the resulting hydrophobic complexes to the hydrocarbon hemisphere, whereas addition of hydrophilic ammonium compounds such as amino acids or polypeptides resulted in supramolecular assemblies at the hydrocarbon-water interface of the droplets. The multiresponsive material platform enabled interfacial complexation and
thus triggered responses of the droplets to a variety of chemical triggers including metal ions, ammonium compounds, amino acids, antibodies, carbohydrates as well as amino-functionalized solid surfaces.
In the final chapter, the first documented optical logic gates and combinatorial logic circuits based on complex emulsions are presented. More specifically, the unique reconfigurable and multiresponsive properties of complex emulsions were exploited to realize droplet-based logic gates of varying complexity using different stimuli-responsive surfactants in combination with diverse readout methods. In summary, different designs for multiresponsive, active, and adaptive liquid colloidal systems were presented and investigated, enabling the design of novel transformative chemo-intelligent soft material platforms.
Im Rahmen dieser Arbeit wurden Energie induzierte Nanopartikel-Substrat Interaktionen untersucht. Dazu wurden Goldnanopartikelanordnungen (AuNPA) auf verschiedenen Silizium-basierten Substraten hergestellt und der Einfluss eines Energieeintrages, genauer gesagt einer thermischen Behandlung oder des Metall-assistierten chemischen Ätzens (MaCE) getestet. Die Nanopartikelanordnungen, welche für die thermische Behandlung eingesetzt wurden, wurden nass-chemisch in Toluol synthetisiert, mit Thiol-terminiertem Polystyrol funktionalisiert und mittels Schleuderbeschichtung auf verschiedenen Substraten (drei Gläser und ein Siliziumwafer) in quasi-hexagonalen Mustern angeordnet. Diese AuNP-Anordnungen wurden mit Temperaturen zwischen 475 °C – 792 °C über verschiedene Zeiträume thermisch behandelt. Generell sanken die Nanopartikel in die Substrate ein, und es wurde festgestellt, dass mit Erhöhung der Glasübergangstemperatur der Substrate die Einsinktiefe der Nanopartikel abnahm. Die AuNPA auf Siliziumwafern wurden auf Temperaturen von 700 °C – 900 °C erhitzt. Die Goldnanopartikel sanken dabei bis zu 2,5 nm in das Si-Substrat ein. Ein Sintern der Nanopartikel fand ab einer Temperatur über 660 °C statt. Welcher Sintermechanismus der dominante ist konnte abschließend nicht eindeutig geklärt werden.
Für die Untersuchung des Einflusses des zweiten Energieeintrages mittels MaCE wurden AuNPA sowie Goldkern-Silberschale-Anordnungen auf Siliziumsubstraten genutzt. Die AuNPA wurden mit Hilfe von Poly-N-Isopropylacrylamid Mikrogelen und Natriumcitrat-stabilisierten Goldnanopartikeln (Na-AuNP) bzw. Tetrachloridogoldsäure (TCG) präpariert. Es ergaben sich Nanopartikelanordnungen mit hemisphärischen Partikeln (aus Na-AuNP) und zum anderen Nanopartikelanordnungen mit sphärischen Partikeln (aus TCG). Durch eine anschließende Silberwachstumsreaktion konnten dann die dazugehörigen Goldkern-Silberschale Nanopartikelanordnungen erhalten werden. Beim MaCE konnten signifikante Unterschiede im Verhalten dieser vier Nanopartikelanordnungen festgestellt werden, z.B. mussten bei den hemisphärischen Partikelanordnungen höhere Wasserstoffperoxidkonzentrationen (0,70 M – 0,91 M) als bei den sphärischen Partikelanordnungen (0,08 M – 0,32 M) für das Ätzen eingesetzt werden, um ein Einsinken der Nanopartikel in das Substrat zu erreichen.
Technologically important, environmentally friendly InP quantum dots (QDs) typically used as green and red emitters in display devices can achieve exceptional photoluminescence quantum yields (PL QYs) of near-unity (95-100%) when the-state-of-the-art core/shell heterostructure of the ZnSe inner/ZnS outer shell is elaborately applied. Nevertheless, it has only led to a few industrial applications as QD liquid crystal display (QD–LCD) which is applied to blue backlight units, even though QDs has a lot of possibilities that able to realize industrially feasible applications, such as QD light-emitting diodes (QD‒LEDs) and luminescence solar concentrator (LSC), due to their functionalizable characteristics.
Before introducing the main research, the theoretical basis and fundamentals of QDs are described in detail on the basis of the quantum mechanics and experimental synthetic results, where a concept of QD and colloidal QD, a type-I core/shell structure, a transition metal doped semiconductor QDs, the surface chemistry of QD, and their applications (LSC, QD‒LEDs, and EHD jet printing) are sequentially elucidated for better understanding. This doctoral thesis mainly focused on the connectivity between QD materials and QD devices, based on the synthesis of InP QDs that are composed of inorganic core (core/shell heterostructure) and organic shell (surface ligands on the QD surface). In particular, as for the former one (core/shell heterostructure), the ZnCuInS mid-shell as an intermediate layer is newly introduced between a Cu-doped InP core and a ZnS shell for LSC devices. As for the latter one (surface ligands), the ligand effect by 1-octanethiol and chloride ion are investigated for the device stability in QD‒LEDs and the printability of electro-hydrodynamic (EHD) jet printing system, in which this research explores the behavior of surface ligands, based on proton transfer mechanism on the QD surface.
Chapter 3 demonstrates the synthesis of strain-engineered highly emissive Cu:InP/Zn–Cu–In–S (ZCIS)/ZnS core/shell/shell heterostructure QDs via a one-pot approach. When this unconventional combination of a ZCIS/ZnS double shelling scheme is introduced to a series of Cu:InP cores with different sizes, the resulting Cu:InP/ZCIS/ZnS QDs with a tunable near-IR PL range of 694–850 nm yield the highest-ever PL QYs of 71.5–82.4%. These outcomes strongly point to the efficacy of the ZCIS interlayer, which makes the core/shell interfacial strain effectively alleviated, toward high emissivity. The presence of such an intermediate ZCIS layer is further examined by comparative size, structural, and compositional analyses. The end of this chapter briefly introduces the research related to the LSC devices, fabricated from Cu:InP/ZCIS/ZnS QDs, currently in progress.
Chapter 4 mainly deals with ligand effect in 1-octanethiol passivation of InP/ZnSe/ZnS QDs in terms of incomplete surface passivation during synthesis. This chapter demonstrates the lack of anionic carboxylate ligands on the surface of InP/ZnSe/ZnS quantum dots (QDs), where zinc carboxylate ligands can be converted to carboxylic acid or carboxylate ligands via proton transfer by 1-octanethiol. The as-synthesized QDs initially have an under-coordinated vacancy surface, which is passivated by solvent ligands such as ethanol and acetone. Upon exposure of 1-octanethiol to the QD surface, 1-octanthiol effectively induces the surface binding of anionic carboxylate ligands (derived from zinc carboxylate ligands) by proton transfer, which consequently exchanges ethanol and acetone ligands that bound on the incomplete QD surface. The systematic chemical analyses, such as thermogravimetric analysis‒mass spectrometry and proton nuclear magnetic resonance spectroscopy, directly show the interplay of surface ligands, and it associates with QD light-emitting diodes (QD‒LEDs).
Chapter 5 shows the relation between material stability of QDs and device stability of QD‒LEDs through the investigation of surface chemistry and shell thickness. In typical III–V colloidal InP quantum dots (QDs), an inorganic ZnS outermost shell is used to provide stability when overcoated onto the InP core. However, this work presents a faster photo-degradation of InP/ZnSe/ZnS QDs with a thicker ZnS shell than that with a thin ZnS shell when 1-octanethiol was applied as a sulfur source to form ZnS outmost shell. Herein, 1-octanethiol induces the form of weakly-bound carboxylate ligand via proton transfer on the QD surface, resulting in a faster degradation at UV light even though a thicker ZnS shell was formed onto InP/ZnSe QDs. Detailed insight into surface chemistry was obtained from proton nuclear magnetic resonance spectroscopy and thermogravimetric analysis–mass spectrometry. However, the lifetimes of the electroluminescence devices fabricated from InP/ZnSe/ZnS QDs with a thick or a thin ZnS shell show surprisingly the opposite result to the material stability of QDs, where the QD light-emitting diodes (QD‒LEDs) with a thick ZnS shelled QDs maintained its luminance more stable than that with a thin ZnS shelled QDs. This study elucidates the degradation mechanism of the QDs and the QD light-emitting diodes based on the results and discuss why the material stability of QDs is different from the lifetime of QD‒LEDs.
Chapter 6 suggests a method how to improve a printability of EHD jet printing when QD materials are applied to QD ink formulation, where this work introduces the application of GaP mid-shelled InP QDs as a role of surface charge in EHD jet printing technique. In general, GaP intermediate shell has been introduced in III–V colloidal InP quantum dots (QDs) to enhance their thermal stability and quantum efficiency in the case of type-I core/shell/shell heterostructure InP/GaP/ZnSeS QDs. Herein, these highly luminescent InP/GaP/ZnSeS QDs were synthesized and applied to EHD jet printing, by which this study demonstrates that unreacted Ga and Cl ions on the QD surface induce the operating voltage of cone jet and cone jet formation to be reduced and stabilized, respectively. This result indicates GaP intermediate shell not only improves PL QY and thermal stability of InP QDs but also adjusts the critical flow rate required for cone-jet formation. In other words, surface charges of quantum dots can have a significant role in forming cone apex in the EHD capillary nozzle. For an industrially convenient validation of surface charges on the QD surface, Zeta potential analyses of QD solutions as a simple method were performed, as well as inductively coupled plasma optical emission spectrometry (ICP-OES) for a composition of elements.
Beyond the generation of highly emissive InP QDs with narrow FWHM, these studies talk about the connection between QD material and QD devices not only to make it a vital jumping-off point for industrially feasible applications but also to reveal from chemical and physical standpoints the origin that obstructs the improvement of device performance experimentally and theoretically.
Facing the environmental crisis, new technologies are needed to sustain our society. In this context, this thesis aims to describe the properties and applications of carbon-based sustainable materials. In particular, it reports the synthesis and characterization of a wide set of porous carbonaceous materials with high nitrogen content obtained from nucleobases. These materials are used as cathodes for Li-ion capacitors, and a major focus is put on the cathode preparation, highlighting the oxidation resistance of nucleobase-derived materials. Furthermore, their catalytic properties for acid/base and redox reactions are described, pointing to the role of nitrogen speciation on their surfaces. Finally, these materials are used as supports for highly dispersed nickel loading, activating the materials for carbon dioxide electroreduction.
The present thesis focuses on the synthesis of nanostructured iron-based compounds by using β-FeOOH nanospindles and poly(ionic liquid)s (PILs) vesicles as hard and soft templates, respectively, to suppress the shuttle effect of lithium polysulfides (LiPSs) in Li-S batteries. Three types of composites with different nanostructures (mesoporous nanospindle, yolk-shell nanospindle, and nanocapsule) have been synthesized and applied as sulfur host material for Li-S batteries. Their interactions with LiPSs and effects on the electrochemical performance of Li-S batteries have been systematically studied.
In the first part of the thesis, carbon-coated mesoporous Fe3O4 (C@M-Fe3O4) nanospindles have been synthesized to suppress the shuttle effect of LiPSs. First, β-FeOOH nanospindles have been synthesized via the hydrolysis of iron (III) chloride in aqueous solution and after silica coating and subsequent calcination, mesoporous Fe2O3 (M-Fe2O3) have been obtained inside the confined silica layer through pyrolysis of β-FeOOH. After the removal of the silica layer, electron tomography (ET) has been applied to rebuild the 3D structure of the M-Fe2O3 nanospindles. After coating a thin layer of polydopamine (PDA) as carbon source, the PDA-coated M-Fe2O3 particles have been calcinated to synthesize C@M-Fe3O4 nanospindles. With the chemisorption of Fe3O4 and confinement of mesoporous structure to anchor LiPSs, the composite C@M-Fe3O4/S electrode delivers a remaining capacity of 507.7 mAh g-1 at 1 C after 600 cycles.
In the second part of the thesis, a series of iron-based compounds (Fe3O4, FeS2, and FeS) with the same yolk-shell nanospindle morphology have been synthesized, which allows for the direct comparison of the effects of compositions on the electrochemical performance of Li-S batteries. The Fe3O4-carbon yolk-shell nanospindles have been synthesized by using the β-FeOOH nanospindles as hard template. Afterwards, Fe3O4-carbon yolk-shell nanospindles have been used as precursors to obtain iron sulfides (FeS and FeS2)-carbon yolk-shell nanospindles through sulfidation at different temperatures. Using the three types of yolk-shell nanospindles as sulfur host, the effects of compositions on interactions with LiPSs and electrochemical performance in Li-S batteries have been systematically investigated and compared. Benefiting from the chemisorption and catalytic effect of FeS2 particles and the physical confinement of the carbon shell, the FeS2-C/S electrode exhibits the best electrochemical performance with an initial specific discharge capacity of 877.6 mAh g-1 at 0.5 C and a retention ratio of 86.7% after 350 cycles.
In the third part, PILs vesicles have been used as soft template to synthesize carbon nanocapsules embedded with iron nitride particles to immobilize and catalyze LiPSs in Li-S batteries. First, 3-n-decyl-1-vinylimidazolium bromide has been used as monomer to synthesize PILs nanovesicles by free radical polymerization. Assisted by PDA coating route and ion exchange, PIL nanovesicles have been successfully applied as soft template in morphology-maintaining carbonization to prepare carbon nanocapsules embedded with iron nitride nanoparticles (FexN@C). The well-dispersed iron nitride nanoparticles effectively catalyze the conversion of LiPSs to Li2S, owing to their high electrical conductivity and strong chemical binding to LiPSs. The constructed FexN@C/S cathode demonstrates a high initial discharge capacity of 1085.0 mAh g-1 at 0.5 C with a remaining value of 930.0 mAh g-1 after 200 cycles.
The results in the present thesis demonstrate the facile synthetic routes of nanostructured iron-based compounds with controllable morphologies and compositions using soft and hard colloidal templates, which can be applied as sulfur host to suppress the shuttle behavior of LiPSs. The synthesis approaches developed in this thesis are also applicable to fabricating other transition metal-based compounds with porous nanostructures for other applications.