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1
Ziegler, Christoph, André Wolf, Wei Liu, Anne-Kristin Herrmann, Nikolai Gaponik, and Alexander Eychmüller. "Modern Inorganic Aerogels." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2018. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-232333.
Full textAbstract:
Essentially, the term aerogel describes a special geometric structure of matter. It is neither limited to any material nor to any synthesis procedure. Hence, the possible variety of materials and therefore the multitude of their applications are almost unbounded. Here we present a comprehensive picture of the most promising developments in the field during the last decades.
2
Beier, Max Gregor, Christoph Ziegler, Karl Wegner, Albrecht Benad, Frank Simon, Stefan Kaskel, and Alexander Eychmüller. "A fast route to modified tin oxide aerogels using hydroxostannate precursors." Royal Society of Chemistry, 2018. https://tud.qucosa.de/id/qucosa%3A33351.
Full textAbstract:
Nanostructured tin oxide materials with a high specific surface area and porosity are promising for applications such as electrocatalysis, lithium ion batteries or sensors. Here, we present a facile strategy for the synthesis of tin oxide aerogels using inexpensive hexahydroxostannate as tin precursor. This easy and scalable method yields tin oxide aerogels with a high specific surface area and wide pore size distribution. The method can be modified by adding hexahydroxoantimonate to obtain antimony doped tin oxide aerogels that show an electrical conductivity after annealing. A cogelation with other preformed nanoparticles (e.g. Au, Pt) leads to mixed gels. Both modifications do not have a large impact on the porous properties of the obtained aerogels. Tin oxide materials prepared via this route can be tailored to a specific application by versatile modification possibilities.
3
Rengers, Christin. "3D Arrangements of Encapsulated Fluorescent Quantum Dots." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-200303.
Full textAbstract:
Nanomaterials have attracted considerable attention during the past decades due to their unique and fascinating properties. However, this class of materials is not an invention of modern age. People have been using nanomaterials for centuries, although unwittingly. Probably the most famous example for the usage of nanomaterials in ancient times is the Lycurgus Cup, a Roman glass cage cup created in the 4th century which changes the colour of its glass from green to ruby depending on the illumination conditions.
The foundation for the development of the field of nanotechnology was laid by the speech of Feynman “There is plenty of room at the bottom” in 1959, in which he spoke about the principles of miniaturisation as low as to the atomic level. Today, modern nanotechnology made it its business to purposefully develop and synthesise nanomaterials as well as to face their applications in various fields, such as microelectronics, catalysis or biomedicine.
However, the term “nanomaterials” does not solely involve the nanoparticulate units itself, but also their arrangement into two- or three-dimensional structures. Thereby, the maintenance of the nanoscale properties is one of the main challenges. This task was focussed by this work implied the preparation and macroscale arrangement of fluorescent QDs while preserving their optical properties.
The main achievement of this work was the development of a novel aerogel material with non-quenching PL behaviour by using silica coated QDs as nanoparticulate building units. In comparison to other monolithic silica-QD structures or aerogels from pure QDs, a defined and controllable distance between the fluorescent QDs is provided in these structures by the silica shell. The spacing was shown to efficiently disable energy transfers so that no spectral shifts, lifetime shortening or PL QY losses are observed during the colloid to gel transition.
The silica shell, established by a standard reverse microemulsion approach, was found to exhibit a certain porosity, which was proven by gas adsorption measurements. Existing cavities in the micro- and mesoporous range were found to allow small species such as metal ions to pass through the shell and interact with the QD core causing a detectable change of the PL intensity, which makes these materials suitable for future sensing applications.
The gel preparation was based on a metal ion assisted complexation approach, which requires tetrazole functionalisation of the nanoparticulate building units. A major development in this work that permitted this gelation approach for silica-QDs was the development of a novel tetrazole-silane ligand. TMSPAMTz was specifically designed to bind to the silica surface of silica-QDs in aqueous solution and was prepared by a covalent coupling of an alkyl chained silane with a 5-subsituted tetrazole ring. Network formation is subsequently achieved by the interconnection of negatively charged tetrazole rings with metal ions, which allows for a broad spectrum of aerogel materials from different NP species as well as their mixtures as long as tetrazole capping is provided. Considering this diversity and the disabling of energy transfers, straightforward colour tuning was demonstrated herein by mixing differently emitting silica-QD species which gives great prospects for lighting applications. Furthermore, the possibility of plasmon enhanced emission was presented for mixed Au NP/silica-QD gels.
With respect to future sensing applications, thin porous films from silica-QDs gels were prepared, which showed a promising concentration dependant PL quenching for the model analyst hydrogen peroxide. However, the film reproducibility of the applied drop-cast coating method was insufficient. As a suggestion to this, a LbL method was presented, wherein a gel is subsequently grown with the metal ion assisted complexation approach. In addition to the tetrazole ligands on the NP surface, tetrazole-silane ligands were used in this approach to functionalise the glass substrate surface. By this, homogeneous gel films of distinct thickness can be grown while the use of organic polymers can be completely avoided.
Besides the preparation of NP assemblies, standard Cd-based QD materials as well as Au NPs of different sizes and shape, recent progresses in the synthesis of InP-based QDs were presented in this work. A thorough investigation and understanding of the growth influencing parameters allowed for the establishment of preparation routes for In(Zn)P/GaP/ZnS core/shell/shell QDs with emission wavelengths tuneable within a large range from 500 to 650 nm, narrow peak widths of 45 to 70 nm and PL QYs up to 60%. Successful incorporation of these QDs into salt matrices was further demonstrated. The resulting composite materials are very photostable and suitable as colour conversion materials for solid state lighting, as was clearly pointed out by a self-prepared WLED that met the standard commercial LEDs.
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Sayevich, Vladimir, Bin Cai, Albrecht Benad, Danny Haubold, Luisa Sonntag, Nikolai Gaponik, Vladimir Lesnyak, and Alexander Eychmüller. "3D Assembly of All-Inorganic Colloidal Nanocrystals into Gels and Aerogels." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-216698.
Full textAbstract:
We report on an efficient assembly approach to a variety of electrostatically stabilized all-inorganic semiconductor nanocrystals (NCs) via their linking with appropriate ions into multibranched gel networks. These all-inorganic non-ordered 3D assemblies can combine strong interparticle coupling which facilitates charge transport between the NCs with their diverse morphology, composition, size, and functional capping ligands. Moreover, the resulting dry gels (aerogels) are highly porous monolithic structures, which preserve the quantum confinement of their building blocks. The inorganic semiconductor aerogel made of 4.5 nm CdSe colloidal NCs, capped with iodide ions and bridged with Cd2+ ions, exhibited a surface area as high as 146 m2/g.
5
Bigall, Nadja-Carola. "Darstellung von Edelmetallnanopartikeln und deren Überstrukturen." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2009. http://nbn-resolving.de/urn:nbn:de:bsz:14-ds-1235057882909-00350.
Full textAbstract:
Zur Darstellung von Edelmetallnanopartikelüberstrukturen werden zunächst kolloidale Lösungen von Gold, Silber, Platin und Palladium synthetisiert. Dafür wird eine modifizierte Syntheseprozedur für Citrat stabilisierte Goldnanopartikel in wässriger Lösung unter Verwendung gleicher Konzentrationen auf die Systeme Silber, Platin und Palladium übertragen. Die Nanopartikellösungen werden mittels Absorptionsspektroskopie und Elektronenmikroskopie in mittlerer und hoher Auflösung charakterisiert. Die Platinnanopartikel werden verwendet, um mittels Keim vermitteltem Wachstum größere Platinnanopartikel darzustellen. Die resultierenden annähernd sphärischen Partikel haben eine sehr enge Größenverteilung mit einer Standardabweichung von drei bis sieben Prozent. Mit bis zu zwei Schritten des Keim vermittelten Wachstums können Partikel mit einem mittleren Durchmesser im Bereich von 10 bis 100 Nanometern hergestellt werden. Hochauflösende Elektronenmikroskopie zeigt, dass die Oberfläche der Partikel aus Platinkristalliten mit Durchmessern weniger Nanometer besteht, was zu einer Oberflächenrauhigkeit von drei bis zehn Nanometern führt. Mittels eines Kern-Schale-Modells werden Einzelteilchenextinktionsspektren berechnet, welche in sehr guter Übereinstimmung mit den experimentell bestimmten Extinktionsspektren des dispergierten Ensembles sind. Eine über weite Bereiche des sichtbaren Spektralbereichs lineare Abhängigkeit des Extinktionsmaximums vom Partikeldurchmesser wird beobachtet. Dadurch und zusammen mit der Einheitlichkeit der synthetisierten Platinsphären eröffnen sich Anwendungsmöglichkeiten im Bereich der Photonik, der Nanooptik und der oberflächenverstärkten Ramanspektroskopie. Geordnete Überstrukturen der Edelmetallnanopartikel können durch Infiltrieren von Templaten aus Block-Copolymer-Filmen mit wässriger Nanopartikellösung synthetisiert werden. In Abhängigkeit von der Vorbehandlung der Polymerfilme werden entweder zweidimensional periodische Anordnungen mit einer Periodizität von weniger als 30 Nanometern oder Fingerabdruck ähnliche Anordnungen mit einem Rillenabstand im selben Größenbereich hergestellt. Durch Entfernen des Polymers entstehen ein- bzw. zweidimensionale Anordnungen aus Platinnanodrähten bzw. -Nanopartikeln auf einem Siliziumwafer. Diese hochgeordneten Strukturen sind von fundamentalem Interesse für die Entwicklung von nanometerskaligen Schaltkreisen, Sensoren und als Substrate für die oberflächenverstärkte Ramanspektroskopie. Für die Herstellung ungeordneter Überstrukturen werden zwei unterschiedliche Ansätze gewählt: direkte Destabilisierung von Nanopartikellösungen, welche zu Hydrogelen und durch Trocknung zu Aerogelen führt, und Immobilisierung von Nanopartikeln auf einem in die Lösung implantierten Pilzmycel. Aus Gold-, Silber- und Platinnanopartikeln werden monometallische Hydro- und Aerogele synthetisiert. Unterschiedliche Destabilisierungsmittel sowie unterschiedliche Methoden zur Aufkonzentration der Nanopartikellösungen werden getestet. Abhängig von der Methode werden gelartige Überstrukturen mit teilweise komplexen Morphologien aus hierarchischen Anordnungen von Primär-, Sekundär-, Tertiärpartikeln beobachtet. Bimetallische Hydro- und Aerogele können aus Mischungen von Gold- oder Platin- mit Silbernanopartikellösungen hergestellt werden. Hochauflösende TEM-Aufnahmen zeigen ein polykristallines Netzwerk aus 2 bis 10 Nanometer dicken Drähten. Erste BET-Messungen zeigen, dass die Gold-Silber-Netzwerke eine Oberfläche von etwa 48 m2/g besitzen. Diese Systeme aus monometallischen und bimetallischen Nanopartikeln stellen erste Ansätze für hochporöse templatfreie Hydro- und Aerogele dar und besitzen großes Potential für den Einsatz in der heterogenen Gasphasenkatalyse, da fast die gesamte Oberfläche aus Übergangsmetall besteht. Es wird für eine Auswahl an unterschiedlichen Pilzen gezeigt, dass deren Wachstum direkt in den synthetisierten Nanopartikellösungen möglich ist. Ohne weitere Funktionalisierung findet eine Anlagerung von Nanopartikeln auf der Pilzoberfläche statt. Starke Variationen in den Affnitäten verschiedener Pilze zu den unterschiedlichen Metallnanopartikeln werden beobachtet. Auch werden Unterschiede der Nanopartikelaffnität mit Variation der Morphologie innerhalb desselben Hybridsystems beobachtet. Ein Platin-Pilz-Hybrid wird in wässriger Lösung erfolgreich als Katalysator einer Redoxreaktion getestet. Solche Hybridstrukturen besitzen ebenso wie die oben beschriebenen Aerogele großes Potential für den Einsatz in der heterogenen Katalyse, wobei die Verwendung von Pilzmycel als Trägermaterial eine kostengünstige Darstellung größerer Katalysatormengen ermöglichen könnte.
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Wohlgemuth, Stephanie-Angelika. "Functional nanostructured hydrothermal carbons for sustainable technologies : heteroatom doping and superheated vapor." Phd thesis, Universität Potsdam, 2012. http://opus.kobv.de/ubp/volltexte/2012/6012/.
Full textAbstract:
The underlying motivation for the work carried out for this thesis was the growing need for more sustainable technologies. The aim was to synthesize a “palette” of functional nanomaterials using the established technique of hydrothermal carbonization (HTC). The incredible diversity of HTC was demonstrated together with small but steady advances in how HTC can be manipulated to tailor material properties for specific applications. Two main strategies were used to modify the materials obtained by HTC of glucose, a model precursor representing biomass.
The first approach was the introduction of heteroatoms, or “doping” of the carbon framework. Sulfur was for the first time introduced as a dopant in hydrothermal carbon. The synthesis of sulfur and sulfur/nitrogen doped microspheres was presented whereby it was shown that the binding state of sulfur could be influenced by varying the type of sulfur source. Pyrolysis may additionally be used to tune the heteroatom binding states which move to more stable motifs with increasing pyrolysis temperature. Importantly, the presence of aromatic binding states in the as synthesized hydrothermal carbon allows for higher heteroatom retention levels after pyrolysis and hence more efficient use of dopant sources. In this regard, HTC may be considered as an “intermediate” step in the formation of conductive heteroatom doped carbon. To assess the novel hydrothermal carbons in terms of their potential for electrochemical applications, materials with defined nano-architectures and high surface areas were synthesized via templated, as well as template-free routes. Sulfur and/or nitrogen doped carbon hollow spheres (CHS) were synthesized using a polystyrene hard templating approach and doped carbon aerogels (CA) were synthesized using either the albumin directed or borax-mediated hydrothermal carbonization of glucose. Electrochemical testing showed that S/N dual doped CHS and aerogels derived via the albumin approach exhibited superior catalytic performance compared to solely nitrogen or sulfur doped counterparts in the oxygen reduction reaction (ORR) relevant to fuel cells. Using the borax mediated aerogel formation, nitrogen content and surface area could be tuned and a carbon aerogel was engineered to maximize electrochemical performance. The obtained sample exhibited drastically improved current densities compared to a platinum catalyst (but lower onset potential), as well as excellent long term stability.
In the second approach HTC was carried out at elevated temperatures (550 °C) and pressure (50 bar), corresponding to the superheated vapor regime (htHTC). It was demonstrated that the carbon materials obtained via htHTC are distinct from those obtained via ltHTC and subsequent pyrolysis at 550 °C. No difference in htHTC-derived material properties could be observed between pentoses and hexoses. The material obtained from a polysaccharide exhibited a slightly lower degree of carbonization but was otherwise similar to the monosaccharide derived samples. It was shown that in addition to thermally induced carbonization at 550 °C, the SHV environment exhibits a catalytic effect on the carbonization process. The resulting materials are chemically inert (i.e. they contain a negligible amount of reactive functional groups) and possess low surface area and electronic conductivity which distinguishes them from carbon obtained from pyrolysis. Compared to the materials presented in the previous chapters on chemical modifications of hydrothermal carbon, this makes them ill-suited candidates for electronic applications like lithium ion batteries or electrocatalysts. However, htHTC derived materials could be interesting for applications that require chemical inertness but do not require specific electronic properties. The final section of this thesis therefore revisited the latex hard templating approach to synthesize carbon hollow spheres using htHTC. However, by using htHTC it was possible to carry out template removal in situ because the second heating step at 550 °C was above the polystyrene latex decomposition temperature. Preliminary tests showed that the CHS could be dispersed in an aqueous polystyrene latex without monomer penetrating into the hollow sphere voids. This leaves the stagnant air inside the CHS intact which in turn is promising for their application in heat and sound insulating coatings.
Overall the work carried out in this thesis represents a noteworthy development in demonstrating the great potential of sustainable carbon materials.Das Ziel der vorgelegten Arbeit war es, mit Hilfe der Hydrothermalen Carbonisierung (HTC) eine Palette an verschiedenen Materialien herzustellen, deren physikalische und chemische Eigenschaften auf spezifische Anwendungen zugeschnitten werden können. Die Motivation hierfür stellt die Notwendigkeit, Alternativen zu Materialien zu finden, die auf fossilen Brennstoffen basieren. Dabei stellen vor allem nachhaltige Energien eine der größten Herausforderungen der Zukunft dar. HTC ist ein mildes, nachhaltiges Syntheseverfahren welches prinzipiell die Nutzung von biologischen Rohstoffen (z. B. landwirtschaftlichen Abfallprodukten) für die Herstellung von wertvollen, Kohlenstoff-basierten Materialien erlaubt. Es wurden zwei verschiedene Ansätze verwendet, um hydrothermalen Kohlenstoff zu modifizieren. Zum einen wurde HTC unter „normalen“ Bedingungen ausgeführt, d. h. bei 180 °C und einem Druck von etwa 10 bar. Der Zucker Glukose diente in allen Fällen als Kohlenstoff Vorläufer. Durch Zugabe von stickstoff und /oder schwefelhaltigen Additiven konnte dotierte Hydrothermalkohle hergestellt werden. Dotierte Kohlenstoffe sind bereits für ihre positiven Eigenschaften, wie verbesserte Leitfähigkeit oder erhöhte Stabilität, bekannt. Zusätzlich zu Stickstoff dotierter Hydrothermalkohle, die bereits von anderen Gruppen hergestellt werden konnte, wurde in dieser Arbeit zum ersten Mal Schwefel in Hydrothermalkohle eingebaut. Außerdem wurden verschiedene Ansätze verwendet, um Oberfläche und definierte Morphologie der dotierten Materialien zu erzeugen, welche wichtig für elektrochemische Anwendungen sind. Schwefel- und/oder stickstoffdotierte Kohlenstoff Nanohohlkugeln sowie Kohlenstoff Aerogele konnten hergestellt werden. Mit Hilfe von einem zusätzlichen Pyrolyseschritt (d. h. Erhitzen unter Schutzgas) konnte die Leitfähigkeit der Materialien hergestellt werden, die daraufhin als Nichtmetall-Katalysatoren für Wasserstoff-Brennstoffzellen getestet wurden. Im zweiten Ansatz wurde HTC unter extremen Bedingungen ausgeführt, d. h. bei 550 °C und einem Druck von ca. 50 bar, welches im Wasser Phasendiagram dem Bereich des Heißdampfes entspricht. Es konnte gezeigt werden, dass die so erhaltene Hydrothermalkohle ungewöhnliche Eigenschaften besitzt. So hat die Hochtemperatur-Hydrothermalkohle zwar einen hohen Kohlenstoffgehalt (mehr als 90 Massenprozent), enthält aber auch viele Wasserstoffatome und ist dadurch schlecht leitfähig. Da damit elektrochemische Anwendungen so gut wie ausgeschlossen sind, wurde die Hochtemperatur-Hydrothermalkohle für Anwendungen vorgesehen, welche chemische Stabilität aber keine Leitfähigkeit voraussetzen. So wurden beispielsweise Hochtemperatur-Kohlenstoff-Nanohohlkugeln synthetisiert, die großes Potential als schall- und wärmeisolierende Additive für Beschichtungen darstellen. Insgesamt konnten erfolgreich verschiedenste Materialien mit Hilfe von HTC hergestellt werden. Es ist zu erwarten, dass sie in Zukunft zu nachhaltigen Technologien und damit zu einem weiteren Schritt weg von fossilen Brennstoffen beitragen werden.
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Benkovičová, Monika, Dan Wen, Jan Plutnar, Martina Čížková, Josef Michl, and Alexander Eychmüller. "Mechanism of Surface Alkylation of a Gold Aerogel with Tetra-n-butylstannane-d36." American Chemical Society, 2018. https://tud.qucosa.de/id/qucosa%3A31088.
Full textAbstract:
The formation of self-assembled monolayers on surfaces is often likely to be accompanied by the formation of byproducts, whose identification holds clues to the reaction mechanism but is difficult due to the minute amounts produced. We now report a successful identification of self-assembly byproducts using gold aerogel with a large specific surface area, a procedure likely to be applicable generally. Like a thin gold layer on a flat substrate, the aerogel surface is alkylated with n-butyl-d9 groups upon treatment with a solution of tetra-n-butylstannane-d36 under ambient conditions. The reaction byproducts accumulate in the mother liquor in amounts sufficient for GC-MS analysis. In chloroform solvent, they are butene-d8, butane-d10, octane-d18, and tributylchlorostannane-d27. In hexane, they are the same except that tributylchlorostannane-d27 is replaced with hexabutyldistannane-d54. The results are compatible with an initial homolytic dissociation of a C-Sn bond on the gold surface, followed by known radical processes.
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Cai, Bin, and Alexander Eychmüller. "Promoting Electrocatalysis upon Aerogels." Wiley VCH, 2019. https://tud.qucosa.de/id/qucosa%3A35457.
Full textAbstract:
Electrocatalysis plays a prominent role in renewable energy conversion and storage, enabling a number of sustainable processes for future technologies. There are generally three strategies to improve the efficiency (or activity) of the electrocatalysts: (i) increasing the intrinsic activity of the catalyst itself; (ii) improving the exposure of active sites; and (iii) acceleratingmass transfer during catalysis (both reactants and products). These strategies are not mutually exclusive and can ideally be addressed simultaneously, leading to the largest improvements in activity. Aerogels, as featured by large surface area, high porosity, and self-supportability provide a platform that matches all the aforementioned criteria for the design of efficient electrocatalysts. The field of aerogel synthesis has seen much progress in recent years, mainly thanks to the rapid development of nanotechnology. Employing precursors with different properties enables the resulting aerogel with targeted catalytic properties and improved performances. This report demonstrates the design strategies of aerogel catalysts and reviews their performances for several electrochemical reactions. The common principles that govern electrocatalysis are further discussed for each category of reactions, thus serving as a guide to the development of
future aerogel electrocatalysts.
9
Bigall, Nadja-Carola. "Darstellung von Edelmetallnanopartikeln und deren Überstrukturen." Doctoral thesis, Technische Universität Dresden, 2008. https://tud.qucosa.de/id/qucosa%3A23736.
Full textAbstract:
Zur Darstellung von Edelmetallnanopartikelüberstrukturen werden zunächst kolloidale Lösungen von Gold, Silber, Platin und Palladium synthetisiert. Dafür wird eine modifizierte Syntheseprozedur für Citrat stabilisierte Goldnanopartikel in wässriger Lösung unter Verwendung gleicher Konzentrationen auf die Systeme Silber, Platin und Palladium übertragen. Die Nanopartikellösungen werden mittels Absorptionsspektroskopie und Elektronenmikroskopie in mittlerer und hoher Auflösung charakterisiert. Die Platinnanopartikel werden verwendet, um mittels Keim vermitteltem Wachstum größere Platinnanopartikel darzustellen. Die resultierenden annähernd sphärischen Partikel haben eine sehr enge Größenverteilung mit einer Standardabweichung von drei bis sieben Prozent. Mit bis zu zwei Schritten des Keim vermittelten Wachstums können Partikel mit einem mittleren Durchmesser im Bereich von 10 bis 100 Nanometern hergestellt werden. Hochauflösende Elektronenmikroskopie zeigt, dass die Oberfläche der Partikel aus Platinkristalliten mit Durchmessern weniger Nanometer besteht, was zu einer Oberflächenrauhigkeit von drei bis zehn Nanometern führt. Mittels eines Kern-Schale-Modells werden Einzelteilchenextinktionsspektren berechnet, welche in sehr guter Übereinstimmung mit den experimentell bestimmten Extinktionsspektren des dispergierten Ensembles sind. Eine über weite Bereiche des sichtbaren Spektralbereichs lineare Abhängigkeit des Extinktionsmaximums vom Partikeldurchmesser wird beobachtet. Dadurch und zusammen mit der Einheitlichkeit der synthetisierten Platinsphären eröffnen sich Anwendungsmöglichkeiten im Bereich der Photonik, der Nanooptik und der oberflächenverstärkten Ramanspektroskopie. Geordnete Überstrukturen der Edelmetallnanopartikel können durch Infiltrieren von Templaten aus Block-Copolymer-Filmen mit wässriger Nanopartikellösung synthetisiert werden. In Abhängigkeit von der Vorbehandlung der Polymerfilme werden entweder zweidimensional periodische Anordnungen mit einer Periodizität von weniger als 30 Nanometern oder Fingerabdruck ähnliche Anordnungen mit einem Rillenabstand im selben Größenbereich hergestellt. Durch Entfernen des Polymers entstehen ein- bzw. zweidimensionale Anordnungen aus Platinnanodrähten bzw. -Nanopartikeln auf einem Siliziumwafer. Diese hochgeordneten Strukturen sind von fundamentalem Interesse für die Entwicklung von nanometerskaligen Schaltkreisen, Sensoren und als Substrate für die oberflächenverstärkte Ramanspektroskopie. Für die Herstellung ungeordneter Überstrukturen werden zwei unterschiedliche Ansätze gewählt: direkte Destabilisierung von Nanopartikellösungen, welche zu Hydrogelen und durch Trocknung zu Aerogelen führt, und Immobilisierung von Nanopartikeln auf einem in die Lösung implantierten Pilzmycel. Aus Gold-, Silber- und Platinnanopartikeln werden monometallische Hydro- und Aerogele synthetisiert. Unterschiedliche Destabilisierungsmittel sowie unterschiedliche Methoden zur Aufkonzentration der Nanopartikellösungen werden getestet. Abhängig von der Methode werden gelartige Überstrukturen mit teilweise komplexen Morphologien aus hierarchischen Anordnungen von Primär-, Sekundär-, Tertiärpartikeln beobachtet. Bimetallische Hydro- und Aerogele können aus Mischungen von Gold- oder Platin- mit Silbernanopartikellösungen hergestellt werden. Hochauflösende TEM-Aufnahmen zeigen ein polykristallines Netzwerk aus 2 bis 10 Nanometer dicken Drähten. Erste BET-Messungen zeigen, dass die Gold-Silber-Netzwerke eine Oberfläche von etwa 48 m2/g besitzen. Diese Systeme aus monometallischen und bimetallischen Nanopartikeln stellen erste Ansätze für hochporöse templatfreie Hydro- und Aerogele dar und besitzen großes Potential für den Einsatz in der heterogenen Gasphasenkatalyse, da fast die gesamte Oberfläche aus Übergangsmetall besteht. Es wird für eine Auswahl an unterschiedlichen Pilzen gezeigt, dass deren Wachstum direkt in den synthetisierten Nanopartikellösungen möglich ist. Ohne weitere Funktionalisierung findet eine Anlagerung von Nanopartikeln auf der Pilzoberfläche statt. Starke Variationen in den Affnitäten verschiedener Pilze zu den unterschiedlichen Metallnanopartikeln werden beobachtet. Auch werden Unterschiede der Nanopartikelaffnität mit Variation der Morphologie innerhalb desselben Hybridsystems beobachtet. Ein Platin-Pilz-Hybrid wird in wässriger Lösung erfolgreich als Katalysator einer Redoxreaktion getestet. Solche Hybridstrukturen besitzen ebenso wie die oben beschriebenen Aerogele großes Potential für den Einsatz in der heterogenen Katalyse, wobei die Verwendung von Pilzmycel als Trägermaterial eine kostengünstige Darstellung größerer Katalysatormengen ermöglichen könnte.
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Kornprobst, Tobias [Verfasser], Johann Peter [Akademischer Betreuer] Plank, and Cordt [Akademischer Betreuer] Zollfrank. "Aerogele und Photokatalysatoren als Beispiele für innovative Baumaterialien / Tobias Kornprobst. Gutachter: Johann Peter Plank ; Cordt Zollfrank. Betreuer: Johann Peter Plank." München : Universitätsbibliothek der TU München, 2013. http://d-nb.info/1043317422/34.
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Cai, Bin, Sebastian Henning, Juan Herranz, Thomas J. Schmidt, and Alexander Eychmüller. "Nanostructuring noble metals as unsupported electrocatalysts for polymer electrolyte fuel cells." Wiley-VCH, 2018. https://tud.qucosa.de/id/qucosa%3A31155.
Full textAbstract:
Two major challenges that impede fuel cell technology breakthrough are the insufficient activity of the electrocatalysts for the oxygen reduction reaction and their degradation during operation, caused by the potential-induced corrosion of their carbon-support upon fuel cell operation. Unsupported electrocatalysts derived from tailored noble-metal nanostructures are superior to the conventional carbon-supported Pt nanoparticle catalysts and address these barriers by fine-tuning the surface composition and eliminating the support. Herein, recent efforts and achievements in the design, synthesis and characterization of unsupported electrocatalysts are reviewed, paying special attention to noble-metal aerogels, nano/meso-structured thin films and template-derived metal nanoarchitectures. Their electrocatalytic performances for oxygen reduction are compared and discussed, and examples of successful catalyst transfer to polymer electrolyte fuel cells are highlighted. This report aims to demonstrate the potential and challenges of implementing unsupported catalysts in fuel cells, thereby providing a perspective on the further development of these materials.
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Ji, Shuxin. "ELECTROSTATICALLY ACTIVE AEROGELS FOR AIR FILTRATION AND SYNTHESIS OF SYNDIOTATIC POLYSTYRENE AEROGEL MICROPARTICLES." University of Akron / OhioLINK, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=akron1497454993387357.
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Zera, E., W. Nickel, G. P. Hao, L. Vanzetti, Stefan Kaskel, and G. D. Sorarù. "Nitrogen doped carbide derived carbon aerogels by chlorine etching of a SiCN aerogel." Royal Society of Chemistry, 2016. https://tud.qucosa.de/id/qucosa%3A30313.
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Silicon was selectively removed from a silicon carbonitride (SiCN) aerogel by hot chlorine gas treatment, leading to a N-doped carbon aerogel (N-CDC aerogel). The combined effects of pyrolysis and etching temperature were studied with regard to the change in the composition of the material after etching as well as the microstructure of the produced hierarchically porous material. Upon removal of Si from amorphous SiCN, carbon and nitrogen, which are not bonded together in the starting material, react, creating new C–N bonds. The removal of silicon also gives rise to a high amount of micropores and hence a high specific surface area, which can be beneficial for the functionality of the carbonaceous material produced. The mesoporous structure of the aerogel allows us to complete the etching at low temperature, which was found to be a crucial parameter to maintain a high amount of nitrogen in the material. The combination of a high amount of micropores and the mesopore transport system is beneficial for adsorption processes due to the combination of a high amount of adsorption sites and effective transport properties of the material. The N-CDC aerogels were characterized by nitrogen physisorption, X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG/DTA), and infrared spectroscopy (DRIFT) and they were evaluated as CO2 absorbers and as electrodes for electric double-layer capacitors (EDLCs).
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Zera, E., W. Nickel, G. P. Hao, L. Vanzetti, Stefan Kaskel, and G. D. Sorarù. "Nitrogen doped carbide derived carbon aerogels by chlorine etching of a SiCN aerogel." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-224321.
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Silicon was selectively removed from a silicon carbonitride (SiCN) aerogel by hot chlorine gas treatment, leading to a N-doped carbon aerogel (N-CDC aerogel). The combined effects of pyrolysis and etching temperature were studied with regard to the change in the composition of the material after etching as well as the microstructure of the produced hierarchically porous material. Upon removal of Si from amorphous SiCN, carbon and nitrogen, which are not bonded together in the starting material, react, creating new C–N bonds. The removal of silicon also gives rise to a high amount of micropores and hence a high specific surface area, which can be beneficial for the functionality of the carbonaceous material produced. The mesoporous structure of the aerogel allows us to complete the etching at low temperature, which was found to be a crucial parameter to maintain a high amount of nitrogen in the material. The combination of a high amount of micropores and the mesopore transport system is beneficial for adsorption processes due to the combination of a high amount of adsorption sites and effective transport properties of the material. The N-CDC aerogels were characterized by nitrogen physisorption, X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG/DTA), and infrared spectroscopy (DRIFT) and they were evaluated as CO2 absorbers and as electrodes for electric double-layer capacitors (EDLCs).
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Hendel, Thomas. "Synthese und Charakterisierung von Halbleiter- und Metall-Nanopartikeln und deren Selbstassemblierung in 3-dimensionale Netzwerkstrukturen." Doctoral thesis, Humboldt-Universität zu Berlin, Mathematisch-Naturwissenschaftliche Fakultät, 2016. http://dx.doi.org/10.18452/17571.
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Aus CdTe- und Edelmetallnanopartikeln werden 3-dimensionale Netzwerkstrukturen aufgebaut, welche durch einen überkritischen Trocknungsprozess zu hochporösen, weitverzweigten Halbleiter-Metall-Nanokompositen, sogenannten Aerogelen, umgewandelt werden. Zunächst werden Thiol-stabilisierte CdTe- und Edelmetallnanopartikel im wässrigen Milieu hergestellt und deren Morphologie und optischen Eigenschaften umfangreich mittels UV-Vis-Spektroskopie, Fluoreszenzspektroskopie und -lebensdauermessung, ICP-OES, TEM, STEM-EDX und AFM charakterisiert. Als Metallkomponente kamen Gold-, Palladium- sowie bimetallisch gemischte Gold-Palladium-Nanopartikel zum Einsatz. Die Gelierung der Nanopartikellösungen erfolgt durch Vermischen der Kolloide und anschließender kontrollierter Destabilisierung mithilfe einer Xe-Dampflampe oder der Zugabe von Wasserstoffperoxid. Neben einer mechanistischen Beschreibung der Gelbildungsmethoden wurden die resultierenden Hydrogele und die aus der überkritischen Trocknung erhaltenen Aerogele bezüglich Zusammensetzung, Morphologie und optischen Eigenschaften mithilfe von TEM und REM jeweils gekoppelt mit EDX-Analyse, Stickstoff-Porosimetrie, diffuser Reflexionsspektroskopie, Fluoreszenzspektroskopie und Fluoreszenzlebensdauermessungen untersucht. Weiterhin wird die UV-Vis-Spektroskopie als Methode zur Konzentrationsbestimmung von Gold in Lösungen kolloidaler Gold-Nanopartikel validiert. Dabei wird die Absorption der Kolloide bei einer Wellenlänge von 400 nm als Maß verwendet. Die NP-Lösungen werden anhand der Parameter Partikelgröße, Oberflächenfunktionalität und der Oxidationsstufe des enthaltenen Goldes variiert.3-dimensional network structures are formed combining CdTe and noble metal nanoparticles. A supercritical drying process allows production of highly porous and widely branched semiconductor-metal nanohybrids, so-called aerogels. Primarily, thiol-capped CdTe and noble metal nanoparticles are synthesized in aqueous media and their morphology and optical properties are studied extensively using UV-Vis and fluorescence spectroscopy, time-resolved fluorescence spectroscopy, ICP-OES, TEM, STEM-EDX and AFM. The metal entity involves gold and palladium nanoparticles as well as bimetallic mixed Au/Pd nanoparticles. After mixing of the different colloids gelation is induced by a controlled destabilization process using a Xenon lamp irradiation or the addition of hydrogen peroxide. Gelation techniques are described mechanistically. Resulting hydrogels and aerogels which are obtained by supercritical drying approach are characterized concerning composition, morphology and optical properties using TEM and SEM each coupled with EDX, nitrogen porosimetry, diffuse reflection spectroscopy, fluorescence spectroscopy and time-resolved fluorescence spectroscopy. Moreover, the UV-Vis spectroscopy is validated as a method to determine the gold concentration in gold nanoparticle solutions using the colloids absorbance at 400 nm as a measure. Gold nanoparticle solutions are varied concerning the parameters particle size, surface functionality and oxidation state of contained gold.
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Cai, Bin, Arezoo Dianat, Rene Hübner, Wei Liu, Dan Wen, Albrecht Benad, Luisa Sonntag, Thomas Gemming, Gianaurelio Cuniberti, and Alexander Eychmüller. "Multimetallic Hierarchical Aerogels: Shape-engineering of the Building Blocks for efficient electrocatalysis." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2018. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-236145.
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A new class of multimetallic hierarchical aerogels composed entirely of interconnected Ni‐PdxPty nano‐building‐blocks with in situ engineered morphologies and compositions is demonstrated. The underlying mechanism of the galvanic shape‐engineering is elucidated in terms of nanowelding of intermediate nanoparticles. The hierarchical aerogels integrate two levels of porous structures, leading to improved electrocatalysis performance.
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Ziegler, Christoph. "Syntheses and Assemblies of Noble Metal Nanostructures." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2013. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-101781.
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Shape and size control as well as the control of the assembly of nanostructures are current challenges in nano sciences. Focussing on metal nanostructures all of these aspects have been addressed in the frame of the present work. It was possible to develop a new aqueous seeded growth method that produces gold nanoparticles with adjustable diameters over a large range of sizes. The spherical particles obtained show very low polydispersities and a good long term stability. Furthermore it was possible to reveal the growth mechanism of these particles utilizing electron microscopy and optical investigations coupled with theoretical calculations. It was found that there is a formation of small nucleation sites on the surface of the seeds in the beginning of the growth process. These sites then subsequently grow into "blackberry-like" intermediate particles. A final intraparticle ripening step leads to smooth and uniform spherical gold nanoparticles. By correcting the dielectric function of gold for charging and the free mean path effect and taking into account the particle size distribution it was possible to accurately model the optical properties of the gold sols obtained using Mie theory.
By controlling the concentration of chloride ions it was possible to influence both the ripening of the "blackberry-like" shaped particles and the morphology of gold nanoparticles. An increased concentration of the chloride ions in the standard citrate reduction procedure leads to larger and elongated particles, whereas the complete removal of the chloride ions made it possible to obtain star shaped, decahedral and \"desert-rose\" shaped particle morphologies. Using the layer-by-layer technique gold nanoparticles of different sizes could be immobilized on glass substrates. The surface-enhanced Raman scattering intensity of these mixed films were about 60% higher than compared to a film made of a single particle size. The optical properties were further investigated by comparing experimentally obtained UV/Vis spectra with generalized Mie theory simulations.
Additionally it could be shown that tetrazole and its derivatives are suitable stabilizing agents in the aqueous synthesis of silver nanoparticles. It was found that depending on the tetrazole derivative used the tendencies of the nanoparticles to agglomerate vary significantly. Different agglomeration stages have been investigated by UV/Vis and Raman spectroscopy. The removal of the ligands used and a resulting improvement of the applicability of the silver nanostructures as SERS substrates is still a challenge.
In the last part of this work the focus was changed from the optical properties of noble metal nanoparticles to their catalytic properties. Therefore gold and palladium nanoparticles have been successfully immobilized on highly porous zinc oxide aerogels. It was possible to synthesize sponge-, flake-, and ribbon-like zinc oxide gels with high specific surface areas. The facile approach of generating mixed metal oxide/noble metal aerogels is very promising for the preparation of highly selective and highly active heterogenous catalysts. First catalytic investigations of a sponge-like palladium loaded zinc oxide aerogel toward the semi-hydrogenation of acetylene showed very high selectivities of up to 85%.
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Cai, Bin. "Metallic hierarchical aerogels for electrocatalytic applications." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-229596.
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Progress in nanotechnology has promoted an increasing interest in the rational design of the emerging hierarchical aerogels, which represents a second stage of the NC-based aerogel research. By fine-tuning the surface properties of the backbones, metallic hierarchical aerogels are able to address the growing demands of advanced electrocatalysts. In this dissertation, three types of metallic hierarchical aerogels were designed by introducing different nanostructures (i.e. hollow, porous/dendritic and core-shell) and alloy effects (with noble or transition metals) into the aerogels. Thus, as a proof-of-concept for fuel cells, advanced electrocatalytic performances have been achieved on the resulting metallic hierarchical aerogels towards both anode (oxidation of ethanol) and cathode (reduction of oxygen) reactions.
First, alloyed PdxNi hollow nanospheres with controlled composition and shell thickness were utilized as building blocks for the design of hierarchical aerogels. The combination of transition-metal doping, hollow interior, as well as the 3D aerogel structure make the resulting aerogels promising electrocatalysts for ethanol oxidation with a mass activity up to 5.6-fold higher than that of the Pd/C.
Second, continuously shape-engineering of the building blocks (ranging from hollow shells to dendritic shapes) was achieved by the synthesis of a series of multimetallic Ni-PdxPty hierarchical aerogels. By optimization of the nanoscale morphology and the chemical composition, the Ni-Pd60Pt40 aerogel exhibits remarkable electrocatalytic activity for oxidation of ethanol. Moreover, the particle growth mechanism underlying the galvanic replacement was revealed in terms of nanowelding of the nanoparticulate reaction intermediates based on experimental and theoretical results. Third, a universal approach was demonstrated for core-shell structuring of metallic aerogels by coating of an ultrathin Pt shell on a composition-tunable Pd-based alloyed core. Their activities for oxygen reduction exhibit a volcano-type relationship as a function of the lattice parameter of the core substrate. Largely improved Pt utilization efficiency was accomplished based on the core-shell motifs, as the mass activity reaches 5.25 A mg-1Pt which are 18.7 times higher than those of Pt/C.
Different from the conventional aerogels with nanowire-like backbones, those hierarchical aerogels are generally comprised of at least two levels of architectures, i.e. an interconnected porous structure on the macroscale and a specially designed configuration at local backbones at the nanoscale. This combination “locks in” the inherent properties of the NCs, so that the beneficial genes obtained by nano-engineering are retained in the resulting monolithic hierarchical aerogels. These results expand the exploitation approach of the electrocatalytic properties of aerogels into morphology control of their NBBs and are of great importance for the future development of aerogels for many other electrochemical reactions.
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Schmidt, Thomas Justus, Methap Oezaslan, W. Liu, Maarten Nachtegaal, Anatoly I. Frenkel, B. Rutkowski, Matthias Werheid, et al. "Homogeneity and elemental distribution in self-assembled bimetallic Pd–Pt aerogels prepared by a spontaneous one-step gelation process." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-222784.
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Multi-metallic aerogels have recently emerged as a novel and promising class of unsupported electrocatalyst materials due to their high catalytic activity and improved durability for various electrochemical reactions. Aerogels can be prepared by a spontaneous one-step gelation process, where the chemical co-reduction of metal precursors and the prompt formation of nanochain-containing hydrogels, as a preliminary stage for the preparation of aerogels, take place. However, detailed knowledge about the homogeneity and chemical distribution of these three-dimensional Pd–Pt aerogels at the nano-scale as well as at the macro-scale is still unclear. Therefore, we used a combination of spectroscopic and microscopic techniques to obtain a better insight into the structure and elemental distribution of the various Pd-rich Pd–Pt aerogels prepared by the spontaneous one-step gelation process. Synchrotron-based extended X-ray absorption fine structure (EXAFS) spectroscopy and high-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) in combination with energy-dispersive X-ray spectroscopy (EDX) were employed in this work to uncover the structural architecture and chemical composition of the various Pd-rich Pd–Pt aerogels over a broad length range. The Pd80Pt20, Pd60Pt40 and Pd50Pt50 aerogels showed heterogeneity in the chemical distribution of the Pt and Pd atoms inside the macroscopic nanochain-network. The features of mono-metallic clusters were not detected by EXAFS or STEM-EDX, indicating alloyed nanoparticles. However, the local chemical composition of the Pd–Pt alloys strongly varied along the nanochains and thus within a single aerogel. To determine the electrochemically active surface area (ECSA) of the Pd–Pt aerogels for application in electrocatalysis, we used the electrochemical CO stripping method. Due to their high porosity and extended network structure, the resulting values of the ECSA for the Pd–Pt aerogels were higher than that for a commercially available unsupported Pt black catalyst. We show that the Pd–Pt aerogels possess a high utilization of catalytically active centers for electrocatalytic applications based on the nanostructured bimetallic framework. Knowledge about the homogeneity and chemical distribution of the bimetallic aerogels can help to further optimize their preparation by the spontaneous one-step gelation process and to tune their electrocatalytic reactivity.
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Cai, Bin, Dan Wen, Wei Liu, Anne-Kristin Herrmann, Albrecht Benad, and Alexander Eychmüller. "Function-led Design of Aerogels: Self-assembly of Alloyed PdNi Hollow Nanospheres for Efficient Electrocatalysis." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-208514.
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Amelioration of the building blocks is a plausible approach to graft aerogels with distinguished properties while preserving the aerogel superiority. However, the incorporation of designated properties into metallic aerogels, especially catalytically beneficial morphologies and transition metal doping, still remains a challenge. Here, we report on the first case of an aerogel electrocatalyst composed entirely of alloyed PdNi hollow nanospheres (HNSs) with controllable chemical composition and shell thickness. The synergy of the transition metal doping, combined with the hollow building blocks and the three dimensional network structure make the PdNi HNS aerogels promising electrocatalysts towards ethanol oxidation, among which the Pd83Ni17 HNS aerogel shows a 5.6-fold enhanced mass activity compared to commercial Pd/C. This work expands the exploitation approach of electrocatalytic properties of aerogels into morphology and composition control of its building blocks.
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Boday, Dylan Joseph. "SILICA AEROGEL-POLYMER NANOCOMPOSITES AND NEW NANOPARTICLE SYNTHESES." Diss., The University of Arizona, 2009. http://hdl.handle.net/10150/194891.
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Aerogels are extremely high surface area, low density materials with applications including thermal and acoustic insulators, radiation detectors and cometary dust particle traps. However, their low density and aggregate structure makes them extremely fragile and practically impossible to machine or handle without breaking. This has led to the development of aerogel composites with enhanced mechanical properties through the addition of polymers or surface modifiers. To date, attempts to strengthen aerogels have come with significant increases in density and processing time. Here I will describe our search for a solution to these problems with our invention using methyl cyanoacrylate chemical vapor deposition (CVD) to strengthen silica, aminated silica and bridged polysilsesquioxane aerogels. This approach led to a strength improvement of the composites within hours and the strongest composite prepared had a 100x strength improvement over the precursor aerogel. We also developed the first approach to control the molecular weight of the polymers that reinforce silica aerogels using surface-initiated atom transfer radical polymerization (SI-ATRP). Although PMMA reinforcement of silica aerogels improved the mechanical properties, further strength improvements were achieved by cross-linking the grafted PMMA. Additionally, we developed the first silica aerogels reinforced with polyaniline nanofibers that were strong and electrically conductive. Reinforcing silica aerogels with polyaniline allowed them to be used as a sensor for the detection of protonating and deprotonating gaseous species. Finally we developed a new approach for the synthesis of silica and bridged polysilsesquioxane spheres using a surfactant free synthesis. This approach allowed for the first in-situ incorporation of base sensitive functionalities during the sol-gel polymerization.
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Cai, Bin, Dan Wen, Wei Liu, Anne-Kristin Herrmann, Albrecht Benad, and Alexander Eychmüller. "Function-led Design of Aerogels: Self-assembly of Alloyed PdNi Hollow Nanospheres for Efficient Electrocatalysis." Technische Universität Dresden, 2015. https://tud.qucosa.de/id/qucosa%3A28672.
Full textAbstract:
Amelioration of the building blocks is a plausible approach to graft aerogels with distinguished properties while preserving the aerogel superiority. However, the incorporation of designated properties into metallic aerogels, especially catalytically beneficial morphologies and transition metal doping, still remains a challenge. Here, we report on the first case of an aerogel electrocatalyst composed entirely of alloyed PdNi hollow nanospheres (HNSs) with controllable chemical composition and shell thickness. The synergy of the transition metal doping, combined with the hollow building blocks and the three dimensional network structure make the PdNi HNS aerogels promising electrocatalysts towards ethanol oxidation, among which the Pd83Ni17 HNS aerogel shows a 5.6-fold enhanced mass activity compared to commercial Pd/C. This work expands the exploitation approach of electrocatalytic properties of aerogels into morphology and composition control of its building blocks.
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Oliveira, Pablo Beluck de. "Produção de aerogel a partir de nanofibras de celulose obtidas de resíduos da indústria moveleira (Pinus elliottii var. elliottii) para sorção de óleos." reponame:Repositório Institucional da UCS, 2017. https://repositorio.ucs.br/handle/11338/3445.
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O petróleo é uma matéria-prima de grande valor econômico. Buscando a substituição de matérias-primas não-renováveis, óleos vegetais vêm sendo usados cada vez mais como matéria-prima para combustíveis e polímeros. Derramamentos durante o manuseio de óleos são graves problemas ambientais. Fibras vegetais são usadas há muito tempo para a sorção de óleos em derramamentos. Resíduos de madeira na forma de serragem já são usados como sorventes de óleos, sendo um recurso barato e disponível. Entretanto, as características hidrofílicas das fibras vegetais reduzem sua capacidade de sorção de óleos. Os aerogéis de celulose tornaram-se um produto de grande interesse nessa área devido à sua alta porosidade (95 a 99%), baixa massa específica (0,004 to 0,15 g.cm-3) e alta área superficial (>60,m².g-1), além da abundância e sustentabilidade da celulose. O objetivo deste trabalho foi desenvolver um aerogel hidrofóbico de nanofibras de celulose a partir de resíduos da indústria moveleira (Pinus elliottii var. elliottii) processados por hidrólise ácida com explosão a vapor para a sorção de petróleo e óleos vegetais. No processo de explosão a vapor a melhor condição experimental foi observada para uma razão volumétrica de ácido acético e ácido nítrico 15:2:1 a 120°C e 30 minutos com rendimento superior a 90% em celulose e a remoção completa da hemicelulose e da lignina. Após a liofilização foi obtido um aerogel com massa específica 0,046 0,0013 g.cm-3 e porosidade 97,08 0,08%. A hidrofobização do aerogel gerou um ângulo de contato de 138,78º 0,78º. O aerogel mostrou capacidade de sorção máxima experimental (CSME) de 19,55 0,10 góleo.gaerogel-1 para petróleo e 13,73 0,62 góleo.gaerogel-1 para o óleo vegetal. A produção de nanofibras de celulose deu-se através de meios físicos (moagem) e a hidrofobização foi efetuada por modificação superficial das fibras com organosilanos (MTMS) por deposição a vapor. Na hidrólise do resíduo da indústria moveleira dois reagentes ácidos (ácido acético e ácido nítrico) foram testados individual e simultaneamente, com variações de temperatura, tempos e quantidade de reagente. A fração sólida rica em celulose obtida foi cominuída em moinho de pedras por 5 horas a 2500 rpm em uma suspensão com 1,5% m/m. O gel obtido foi congelado por 48 horas a -20ºC para posterior liofilização a -40ºC por 50 horas. Os aerogéis obtidos na liofilização foram tratados com o organosilano via deposição em fase vapor por 5 horas a 70ºC. O resíduo da indústria moveleira foi caracterizado quanto ao teor de celulose, hemicelulose, lignina, cinzas, extrativos e umidade. O processo de explosão a vapor foi caracterizado através do rendimento individual dos seus componentes (celulose e hemicelulose). Ensaios de massa específica aparente, ângulo de contato, porosidade, caracterização morfológica por microscopia eletrônica de varredura de emissão de campo, ensaios de sorção de óleos e cinética de sorção em meio homogêneo e heterogêneo de sorção de petróleo e óleo de soja foram realizados para caracterizar o aerogel. Modelos cinéticos de pseudoprimeira, pseudossegunda e pseudoenésima ordem foram ajustados aos dados experimentais em suas formas lineares e não-lineares. A sorção em meio homogêneo de petróleo foi bem ajustada com o modelo linear de pseudoprimeira ordem. A sorção de óleo vegetal foi bem ajustada tanto pelo modelo de pseudoprimeira ordem quanto pelo modelo de pseudossegunda ordem. Os modelos na forma não-linear indicaram um melhor ajuste dos dados experimentais pelo modelo de pseudoenésima ordem (n=0,95) para o petróleo e pelo modelo de pseudoprimeira ordem para o óleo vegetal. Os ajustes cinéticos mostraram que em meio heterogêneo a CSME se mantém constante em relação ao meio homogêneo, mas foi observada uma menor taxa de sorção.Submitted by cmquadros@ucs.br (cmquadros@ucs.br) on 2018-02-01T18:30:09Z No. of bitstreams: 1 Dissertacao Pablo Beluck de Oliveira.pdf: 3113740 bytes, checksum: c1c0b51adf3c34f0f55f7579081223d8 (MD5)
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Ministério do Trabalho e Emprego, MTE.
Petroleum is a feedstock of great economic value. Due to the aim for non-renewable feedstocks substitution, vegetable oils have been used ever more as a feedstock for fuels and polymers. Spills during oil handling are serious environmental problems. Vegetable fibers have been used for a long time now as oil sorbents during spills. Wood residues as sawdust are currently used as oil sorbents, being a cheap and available resource. However, the hydrophilic profile of vegetable fibers reduce their capacity of oil sorption. Cellulose aerogels have become a product of great interest in the oil spill remediation field due to their high porosity (95 to 99%), low specific mass (0,004 to 0,15 g.cm-3) and high surface area (>60,m².g-1), besides cellulose abundance and sustainability. The objective of this work was to develop a hydrophobic aerogel from nanocellulose nanofibers obtained from furniture industry residues (Pinus elliottii var. elliottii) processed via steam explosion acid hydrolysis for petroleum and vegetable oil sorption. In the steam explosion process the best experimental condition was observed for a volumetric acetic acid and nitric acid ratio of 15:2:1 at 120ºC and 30 minutes with a cellulose yield higher than 90% and complete removal of hemicellulose and ligning. After lyophilization an aerogel of specific mass 0,046 0,0013 g.cm-3 and porosity 97,08 0,08% was obtained. Aerogel hydrophobization yielded a contact angle of 138,78º 0,78º. The aerogel exhibited a top experimental sorption capacity (CSME) of 19,55 0,10 goil.gaerogel-1 for petroleum and 13,73 0,62 goil.gaerogel-1 for vegetable oil. Cellulose nanofibers were produced by physical means (grinding) and hydrophobization was accomplished via vapor-phase deposition of organosilane (MTMS). In wood residue hydrolysis two acids were tested (nitric acid and acetic acid) simultaneously and individually, with variations of temperature, time and reagent amount. The solid fraction rich in cellulose was grinded in a rock mill for 5 hours at 2500 rpm in a 1,5% m/m suspension in water. The obtained gel was frozen for 48 hours at -20ºC for lyophilization at -40ºC for 50 hours. The aerogels obtained by lyophilization were treated with organosilane via vapor-phase deposition for 5 hours at 70ºC. The furniture industry residue was characterized as for its amounts of cellulose, hemicellulose, lignin, ashes, extractives and humidity. The process of steam explosion was characterized through the yields of individual components (cellulose and hemicellulose). Procedures like specific mass, contact angle, porosity, morphological characterization by scanning electron microscope with field emission gun, oil absorption tests and absorption kinetic in homogeneous and heterogeneous medium of petroleum and soy oil absorption were performed to characterize the aerogel. Kinetic models of pseudo-first, pseudo-second and pseudo-nth order were fitted to experimental data in their linear and non-linear forms. The absorption in homogeneous medium of petroleum was well fitted by pseudo-first linear kinetic model. Absorption of vegetable oil was well fitted by both pseudo-first and pseudo-second models. Models in non-linear form indicated a better fit for experimental data by the pseudo-nth order model (n=0,95) for petroleum and by pseudo-first order for vegetable oil. Kinetic adjusts showed that in heterogeneous medium CSME is maintained, but sorption rate is smaller.
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Schmidt, Thomas Justus, Methap Oezaslan, W. Liu, Maarten Nachtegaal, Anatoly I. Frenkel, B. Rutkowski, Matthias Werheid, et al. "Homogeneity and elemental distribution in self-assembled bimetallic Pd–Pt aerogels prepared by a spontaneous one-step gelation process." Royal Society of Chemistry, 2016. https://tud.qucosa.de/id/qucosa%3A30258.
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Multi-metallic aerogels have recently emerged as a novel and promising class of unsupported electrocatalyst materials due to their high catalytic activity and improved durability for various electrochemical reactions. Aerogels can be prepared by a spontaneous one-step gelation process, where the chemical co-reduction of metal precursors and the prompt formation of nanochain-containing hydrogels, as a preliminary stage for the preparation of aerogels, take place. However, detailed knowledge about the homogeneity and chemical distribution of these three-dimensional Pd–Pt aerogels at the nano-scale as well as at the macro-scale is still unclear. Therefore, we used a combination of spectroscopic and microscopic techniques to obtain a better insight into the structure and elemental distribution of the various Pd-rich Pd–Pt aerogels prepared by the spontaneous one-step gelation process. Synchrotron-based extended X-ray absorption fine structure (EXAFS) spectroscopy and high-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) in combination with energy-dispersive X-ray spectroscopy (EDX) were employed in this work to uncover the structural architecture and chemical composition of the various Pd-rich Pd–Pt aerogels over a broad length range. The Pd80Pt20, Pd60Pt40 and Pd50Pt50 aerogels showed heterogeneity in the chemical distribution of the Pt and Pd atoms inside the macroscopic nanochain-network. The features of mono-metallic clusters were not detected by EXAFS or STEM-EDX, indicating alloyed nanoparticles. However, the local chemical composition of the Pd–Pt alloys strongly varied along the nanochains and thus within a single aerogel. To determine the electrochemically active surface area (ECSA) of the Pd–Pt aerogels for application in electrocatalysis, we used the electrochemical CO stripping method. Due to their high porosity and extended network structure, the resulting values of the ECSA for the Pd–Pt aerogels were higher than that for a commercially available unsupported Pt black catalyst. We show that the Pd–Pt aerogels possess a high utilization of catalytically active centers for electrocatalytic applications based on the nanostructured bimetallic framework. Knowledge about the homogeneity and chemical distribution of the bimetallic aerogels can help to further optimize their preparation by the spontaneous one-step gelation process and to tune their electrocatalytic reactivity.
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Sayevich, Uladzimir. "Synthesis, Surface Design and Assembling of Colloidal Semiconductor Nanocrystals." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-209074.
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The work presented in the thesis is focused on the synthesis of diverse colloidal semiconductor NCs in organic media, their surface design with tiny inorganic and hybrid capping species in solution phase, and subsequent assembling of these NC building units into two-dimensional close-packed thin-films and three-dimensional non-ordered porous superstructures.
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Svingala, Forrest R. "Alkali activated aerogels /." Online version of thesis, 2009. http://hdl.handle.net/1850/10097.
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Liu, Xipeng. "Chemistry in an inorganic-organic hybrid aerogel : chitosan-silica aerogel /." View online version; access limited to Brown University users, 2005. http://gateway.proquest.com/openurl?url_ver=Z39.88-2004&res_dat=xri:pqdiss&rft_val_fmt=info:ofi/fmt:kev:mtx:dissertation&rft_dat=xri:pqdiss:3174640.
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Ozaslan, Mehtap, Wei Liu, Maarten Nachtegaal, Anatoly Frenkel, Bogdan Rutkowski, Matthias Werheid, Anne-Kristin Herrmann, et al. "Homogeneity and Elemental Distribution in Self-Assembled Bimetallic Pd-Pt Aerogels prepared by a spontaneous one-step gelation process." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-210970.
Full textAbstract:
Multi-metallic aerogels have recently emerged as a novel and promising class of unsupported electrocatalyst materials due to their high catalytic activity and improved durability for various electrochemical reactions. Aerogels can be prepared by a spontaneous one-step gelation process, where the chemical co-reduction of metal precursors and the prompt formation of the nanochain-consisting hydrogels, as a preliminary stage for the preparation of aerogels take place. However, detailed knowledge about the homogeneity and chemical distribution of these three-dimensional Pd-Pt aerogels at the nano-scale as well as at the macro-scale is still unclear to date.
Therefore, we used a combination of spectroscopic and microscopic techniques to obtain a better insight into the structure and elemental distribution of the various Pd-rich Pd-Pt aerogels prepared by the spontaneous one-step gelation process. Synchrotron-based extended X-ray absorption fine structure (EXAFS) spectroscopy and high-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) in combination with energy-dispersive X-ray spectroscopy (EDX) were employed in this work to uncover the structural architecture and chemical composition of the various Pd-rich Pd-Pt aerogels over a broad length range. The Pd80Pt20, Pd60Pt40 and Pd50Pt50 aerogels showed heterogeneity in the chemical distribution of the Pt and Pd atoms inside the macroscopic nanochain-network. Features of monometallic clusters were not detected by EXAFS or STEM-EDX, indicating alloyed nanoparticles. However, the local chemical composition of the Pd-Pt alloys strongly varied along the nanochains and thus within a single aerogel. To determine the electrochemically active surface area (ECSA) of the Pd-Pt aerogels for applications in electrocatalysis, we used the electrochemical CO stripping method. Due to high porosity and extended network structure, the resulting values of the ECSA for the Pd-Pt aerogels were higher than that for a commercially available unsupported Pt black catalyst. We show that the Pd-Pt aerogels possess a high utilization of catalytically active centers for electrocatalytic applications based on the nanostructured bimetallic framework.
Knowledge about the homogeneity and chemical distribution of the bimetallic aerogels can help to further optimize their preparation by the spontaneous one-step gelation process and to tune their electrocatalytic reactivity.
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Grogan, Michael D. W. "Aerogel and fibre optics." Thesis, University of Bath, 2010. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.538560.
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Yao, Yimin. "POLYMERIC POROUS AEROGEL MONOLITHS AND AEROGEL PARTICLES SYNTHESIZED FROM OIL-IN-OIL EMULSIONS." University of Akron / OhioLINK, 2020. http://rave.ohiolink.edu/etdc/view?acc_num=akron1590687157263171.
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Kühn, Laura. "Bimetallic aerogels for electrocatalytic applications." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-226469.
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Polymer electrolyte fuel cells (PEFCs) have emerged as a promising renewable emission-free technology to solve the worldwide increasing demand for clean and efficient energy conversion. Despite large efforts in academia and automotive industry, the commercialization of PEFC vehicles still remains a great challenge. Critical issues are high material costs, insufficient catalytic activity as well as longterm durability. Especially due to the sluggish kinetics of the oxygen reduction reaction (ORR), high Pt loadings on the cathode are still necessary which leads to elevated costs.
Alloys of Pt with other less precious metals (Co, Ni, Fe, Cu, etc.) show improved ORR activities compared to pure Pt catalysts. However, state-of-the-art carbon-supported catalysts suffer from severe Pt and carbon corrosion during the standard operation of PEFCs, affecting their reliability and long-term efficiency.
Multimetallic aerogels constitute excellent candidates to overcome these issues. Due to their large open pores and high inner surface areas combined with electrical conductivity, they are ideal for applications in electrocatalysis. In addition, they can be employed without any catalyst support. Therefore, the fabrication of bimetallic Pt-M (M=Ni, Cu, Co, Fe) aerogels for applications in fuel cell catalysis was the focus of this thesis.
Based on a previously published synthesis for Pt–Pd aerogels, a facile one-step procedure at ambient conditions in aqueous solution was developed. Bimetallic aerogels with nanochain diameters of as small as 4 nm and Brunauer-Emmett-Teller (BET) surface areas of up to 60 m2/g could be obtained.
Extensive structure analysis of Pt–Ni and Pt–Cu aerogels by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), scanning transmission electron microscopy coupled with energy-dispersive X-ray spectroscopy (STEM-EDX) and electrochemical techniques showed that both metals were predominantly present in their metallic state and formed homogeneous alloys. However, metal (hydr)oxide byproducts were observed in aerogels with higher contents of non-precious metal (>25 %). Moreover, electronic and geometric structures were similar to those of carbon-supported Pt alloy catalysts.
As a result, ORR activites were comparable, too. A threefold improvement in surface-specific activity over Pt/C catalysts was achieved. The mass-specific activites met or exceeded the U.S. Department of Energy (DOE) target for automotive PEFC applications. Furthermore, a direct correlation between non-precious metal content in the alloy and ORR activity was discovered. Aerogels with nonprecious metal contents >25% turned out to be susceptible to dealloying in acid leaching experiments, but there was no indication for the formation of extended surface structures like Pt-skeletons.
A Pt3Ni aerogel was successfully employed as the cathode catalyst layer in a differential fuel cell (1 cm2), which is a crucial step towards technical application. This was the first time an unsupported metallic aerogel was implemented in a PEFC. Accelerated stress tests that are usually applied to investigate the support stability of fuel cell catalysts revealed the excellent stability of Pt3Ni alloyed aerogels. In summary, the Pt alloy aerogels prepared in the context of this work have proven to be highly active oxygen reduction catalysts with remarkable stability.
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Torres, Rodríguez Jorge Alberto. "Příprava aerogelových povrchových úprav na objemových materiálech." Doctoral thesis, Vysoké učení technické v Brně. CEITEC VUT, 2020. http://www.nusl.cz/ntk/nusl-411059.
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Tato práce se zabývá systematickou studií syntézy a zpracováním pokročilých tepelně stabilních aerogelů pro potenciální vysokoteplotní aplikace. V první části dizertační práce jsou podrobně popsány syntetické implikace pro přípravu aerogelů a jejich aplikace spolu s popisem depozičních metod povlaků vytvořených pomocí sol-gel procesu. Experimentální postup je rozdělen do tří částí. První z nich představuje syntetické protokoly k přípravě ZrO2, YSZ, Ln2Zr2O7 (Ln = La3+, Nd3+, Gd3+, and Dy3+) aerogelů, Ln2Zr2O7 prášků a xerogelů. Dále je popsána depoziční metoda, která byla použita pro přípravu povlaků z aerogelů na kovových substrátech. Poté jsou následně specifikovány techniky, jež byly použity pro charakterizaci. Bylo zjištěno, že množství vody a kyseliny dusičné hraje rozhodující roli v přípravě gelů vhodných pro transformaci na aerogely. Po kalcinaci při 500 °C mají ZrO2 a YSZ aerogely velký povrch, a to až do 114 m2 g-1, avšak při 1000 °C dochází k úplnému zhuštění a ztrácí se tak veškerá jejich porézní struktura. Naopak ve srovnání s ZrO2 and YSZ jsou aerogely Ln2Zr2O7 tepelně stabilnější, protože si zachovávají svou porozitu při vyšší kalcinační teplotě (1000 °C), při které dosahují hodnot > 160 m2 g-1. Experimentálně bylo dále zjištěno, že ve studovaném teplotním rozsahu ZrO2 aerogel tvoří tetragonální komplex monoklinický fázový přechod řízený velikostí krystalitů, zatímco YSZ je tvořena jedinou tetragonální fází. Fázové složení zirkoničitanů vzácných zemin je vysoce závislé na způsobu syntézy; všechny Ln2Zr2O7 materiály jsou pyrochlorické nebo fluoritové krystalické fáze. Přímým odléváním aerogelu na kovový substrát dochází k úplnému rozpraskání povlaku z důvodu smršťování, zatímco máčením kovového substrátu v suspenzi je možné vyrobit homogenní, silné a hrubé povlaky z aerogelu. Tyto povlaky neobsahují fázové změny a zůstávají vysoce porézní i po různých tepelných úpravách.
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Laskowski, Jessica Verfasser], Lorenz [Akademischer Betreuer] Ratke, and Jochen M. [Akademischer Betreuer] [Schneider. "Synthese und Eigenschaften von Aerogel-Aerogel-Verbundwerkstoffen / Jessica Laskowski ; Lorenz Ratke, Jochen M. Schneider." Aachen : Universitätsbibliothek der RWTH Aachen, 2016. http://d-nb.info/1126040843/34.
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Laskowski, Jessica [Verfasser], Lorenz Akademischer Betreuer] Ratke, and Jochen M. [Akademischer Betreuer] [Schneider. "Synthese und Eigenschaften von Aerogel-Aerogel-Verbundwerkstoffen / Jessica Laskowski ; Lorenz Ratke, Jochen M. Schneider." Aachen : Universitätsbibliothek der RWTH Aachen, 2016. http://d-nb.info/1126040843/34.
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Zhang, Huan. "Properties and Structures of Sulfonated Syndiotactic Polystyrene Aerogel and Syndiotactic Polystyrene/Silica Hybrid Aerogel." University of Akron / OhioLINK, 2014. http://rave.ohiolink.edu/etdc/view?acc_num=akron1405298489.
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Gu, Zipeng. "Emulsion Templated Polyimide Aerogel Foam and Hybrid Aerogel Foam as Absorbents for Oil Cleanup." University of Akron / OhioLINK, 2018. http://rave.ohiolink.edu/etdc/view?acc_num=akron1525711842824095.
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Johansson, Daniel. "Alternativa isoleringsmaterial : Aerogel inom sjöfarten." Thesis, Linnéuniversitetet, Sjöfartshögskolan (SJÖ), 2019. http://urn.kb.se/resolve?urn=urn:nbn:se:lnu:diva-89566.
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Detta arbete handlar om att med en teoretisk modell kunna beräkna fram de olika mängder värmeförluster som vissa isoleringsmaterial släpper igenom. Syftet med detta arbete är att undersöka om ett specifikt isoleringsmaterial som vanligtvis inte används inom sjöfarten har möjligheten att sänka energin som försvinner igenom isoleringsmaterialen. De metoder som användes är en teoretisk modell som byggdes för att kunna använda de olika isoleringsmaterialens värmekonduktivitet för sedan kunna beräkna de teoretiska värmeförlusterna. Resultatet visar att aerogel skulle vara lämpligt för användning inom sjöfarten tack vara sina egenskaper och isoleringsförmåga som är mycket bättre än mineralull.This work is about using a theoretical model to calculate the various amounts of thermal losses that some insulation materials release. The purpose of this work is to investigate whether a specific insulation material that has not been properly tested in shipping has the potential to lower energy that passes through the insulation materials. The methods used are that a theoretical model was built to use the thermal conductivity of different insulation materials in order to calculate the theoretical heat losses. The result shows that aerogel would be suitable for use in shipping thanks to its properties and insulation ability, which is much better than mineral wool.
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Samvin, Daniel, and Stefan Markovic. "InsuFlex : Framtagning och analys av högpresterande isoleringskoncept i sandwichelement." Thesis, Högskolan i Halmstad, Sektionen för ekonomi och teknik (SET), 2014. http://urn.kb.se/resolve?urn=urn:nbn:se:hh:diva-25546.
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Rapportens huvudsyfte är att ta fram en isoleringskombination av högpresterande material, som ska bidra till ett förbättrat U-värde och reducerad väggtjocklek. Konstruktionen är baserad på en befintlig sandwichvägg från Strängbetong, där författarna ersatt den ursprungliga isoleringen med det utvecklade isolerskiktet för att slutligen studera väggarna med lika villkor. Den framtagna väggens isolerings- förmåga presenteras genom handberäkningar, där det erhålls U-värde och temperaturfördelningar mellan elementens olika skikt vid stationära förhållanden. Det har även utförts värmesimuleringar för att analysera samma fysikaliska faktorer dock baserat på 3D förhållanden. I samarbete med företag har flera högpresterande isoleringsmaterial valts ut att ingå i väggkonstruktionen. Genom fördjupade studier av materialens fysikaliska egenskaper kunde en komplett isoleringskombination utvecklas och fick namnet InsuFlex. InsuFlex applicerades sedan i en sandwichkonstruktion för vidare analyser och värmesimuleringar. De nya väggresultaten visade mycket goda förbättringar av den ursprungliga sandwichväggen, tack vare det utvecklade skiktet av InsuFlex. Genom utförda beräkningar kunde författarna konstatera att isoleringsförmågan förbättrats med 46,5- samt 29 %, samtidigt som tjockleken reducerats med 5,5- samt 16,5 %, i jämförelse med Strängbetongs befintliga produkt. Den nya väggen erbjuder goda förutsättningar att reducera energiförlusterna och komma närmare framtida energikrav. Isoleringsmetoden förväntas även kunna appliceras i flera olika konstruktionselement.The main objective of this report is development of an insulation-layer of high performance materials for a sandwich structure, which will contribute to an improved U-value and reduced wall thickness. The design is based on an existing sandwich wall, where the authors replaced the original insulation with the developed insulation-layer, to study the walls with equal conditions. The insulating ability is presented through calculations and thermal simulation to analyze the thermal aspects of the stationary conditions and 3D conditions. A complete insulation combination was developed through extensive studies of material’s physical properties, and named “InsuFlex”. The insulation-layer was then applied in a sandwich construction for further analysis and thermal simulations. The new design showed improvements in several areas.
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Han, Xiao. "Ambient pressure drying synthesis of aerogels." Thesis, University of Newcastle upon Tyne, 2016. http://hdl.handle.net/10443/3489.
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This PhD thesis reports three novel ambient pressure drying (APD) synthesis methods for producing aerogels and characterisation of the resulting products. Motivated by overcoming the disadvantages of the conventional APD method, a novel approach, which utilises sodium bicarbonate solution instead of the organic low-surface-tension (LST) solvent (e.g. hexane, heptane, etc.) usually employed, has been successfully developed to produce silica aerogels. The novel APD method dramatically reduces costs (~70 times) in comparison with conventional approaches, and it solves the problems associated with generation of hydrochloric acid by trimethylchlorosilane. In order to fabricate nickel nanoparticle/silica (NiNP/SiO2) aerogel composites a new process was developed based on conventional APD with an organic LST solvent. A straightforward approach for dispersing the nickel nanoparticles in a silica aerogel matrix was established. The catalytic activity of the NiNP/SiO2 aerogel composites for the hydration reaction of carbon dioxide in water was then investigated. Finally, to develop the first ambient pressure dried zinc oxide aerogels, zinc-based aerogels were fabricated from zinc nitrate salt precursors by conventional APD with organic LST solvents. The microstructure of the resulting zinc-based aerogels was studied, and the macropores were found to have a flower-like multilayered nanoplate structure. After mild heat treatment, zinc oxide aerogels were generated from the zinc-based aerogels. Depending on the phase composition of the zinc-based aerogels and the different synthesis conditions, general routes for ambient pressure drying synthesis of zinc oxide aerogels are suggested. The morphologic characterisations of synthesised aerogels was performed by transmission electron microscope (TEM), scanning electron microscope (SEM), and scanning transmission electron microscope (STEM). The elemental and structural analysis of prepared aerogel materials was investigated by energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD), respectively. The specific surface area and pore size are analysed by Brunauer–Emmett–Teller (BET) and Barrett-Joyner-Halenda (BJH) methods via nitrogen gas physisorption.
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FOREST, LUC. "Proprietes acoustiques des aerogels de silice." Paris 7, 1998. http://www.theses.fr/1998PA077056.
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Bien que les processus de fabrication des aerogels de silice aient ete developpes depuis maintenant une cinquantaine d'annees, l'etude de leurs proprietes acoustiques ne date que du debut des annees 80. Les tres faibles vitesses du son mesurees et les attenuations relativement importantes, correlees aux tres faibles densites de ces solides, ont permis d'envisager une application des aerogels en tant qu'adaptateur d'impedance aerien et en tant qu'absorbant acoustique. Ces applications necessitent au prealable de mieux connaitre les proprietes acoustiques de ces gels. Alors que seuls des modeles ad hoc concernant la prediction de la vitesse longitudinale ont jusqu'a present ete proposes, nous nous sommes interroges sur la pertinence, dans le cas des aerogels, de la theorie de reference concernant la propagation acoustique dans les milieux poreux a squelette elastique, a savoir la theorie de biot, formulee en 1956 et validee experimentalement en 1980. Nous montrons ici le bon accord de cette theorie, a la fois pour les aerogels et alcogels, sur toute la gamme de porosite. Afin d'etudier plus finement la validite de cette theorie et de mettre en evidence l'influence du fluide saturant sur la propagation acoustique, nous avons effectue un suivi de vitesse pendant la phase de sechage hypercritique, etape conduisant a la transformation d'un alcogel en aerogel. Le fluide saturant les pores passant du stade liquide au stade gazeux tandis que le squelette demeure a peu pres intact, cette experience permet d'effectuer une comparaison entre les vitesses mesurees et les predictions theoriques pour une gamme tres large de densites et de compressibilites du fluide saturant. Enfin, cette experience nous a permis de mettre en evidence dans le cas des gels de silice le caractere non adiabatique de la propagation.
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Athmuri, Kalyan Ram. "Transparent and Crack-Free Silica Aerogels." Thesis, North Dakota State University, 2012. https://hdl.handle.net/10365/26529.
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The process of making silica aerogels has been studied in detail over the past two decades due to its usage in a wide range of low end applications such as thermal insulators, supercapacitors etc., as well as high end applications like particle physics, space explorations. These applications call for control over the properties of aerogels, such as their transparency, density, porosity, pore size, and integrity. However, despite all the past research, controlling properties of aerogels is still not a fully developed science, a lot more research needs to be done.
The literature on silica aerogels does not cover the study of the relation between transparency and cracks in aerogels ? which can be a key factor in making aerogels for many applications. Hence, optimization of the transparency and integrity of the aerogels in order to obtain high transparency and low cracks was attempted in this thesis.
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Tarrés, Farrés Joaquim Agustí. "Endo-β-1,4-glucanasa para la fabricación de micro/nanocelulosa: propiedades y aplicaciones." Doctoral thesis, Universitat de Girona, 2017. http://hdl.handle.net/10803/456211.
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In the recent years, significant interest on the production, characterization and application of cellulose nanofibers has brought out among scientific and technic authorities. This special attention mainly comes from their biodegradability, renewability and versatility, making them able to be used for several applications and fields. This topic outbreak took place about ten years ago, fact that is confirmed by the exponential increase on scientific publications and patents since then.
In a nutshell, the present thesis aims to demonstrate that enzymatically hydrolyzed cellulose nanofibers can be successfully produced and used in several sectors. Their versatility, availability, low cost and low environmental impact justify the ongoing research in this fieldEn els darrers anys, entre la comunitat científica i tecnològica s’ha despertat un gran interès en la producció, caracterització i utilització de nanofibres de cel·lulosa. Aquesta especial atenció es deu, principalment, al seu caràcter biodegradable, el seu origen renovable i la versatilitat que presenten, fent-les aptes per ser utilitzades en multitud d’aplicacions. L’esclat d’aquesta temàtica de recerca va tenir lloc aproximadament deu anys enrere, doncs només cal observar el creixement exponencial de publicacions científiques i patents des d’aleshores. De manera general, la present tesi pretén demostrar que les nanofibres de cel·lulosa obtingudes mitjançant un pretractament d’hidròlisi enzimàtica poden ser produïdes de forma efectiva, de manera que pugin ser aplicades en una gran varietat de camps científics i tecnològics. La seva gran versatilitat, disponibilitat, baix cost i baix impacte mediambiental, justifiquen que en el futur es continuï amb la seva investigació sobre noves aplicacions
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Paetkau, Mark Jeffrey. "Helium mixtures in 87% porous aerogel." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1998. http://www.collectionscanada.ca/obj/s4/f2/dsk3/ftp04/nq29088.pdf.
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Cohen, Ellann. "Thermal properties of advanced aerogel insulation." Thesis, Massachusetts Institute of Technology, 2011. http://hdl.handle.net/1721.1/67795.
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Thesis (S.M.)--Massachusetts Institute of Technology, Dept. of Mechanical Engineering, 2011.Cataloged from PDF version of thesis.
Includes bibliographical references (p. 74-76).
Buildings consume too much energy. For example, 16.6% of all the energy used in the United States goes towards just the heating and cooling of buildings. Many governments, organizations, and companies are setting very ambitious goals to reduce their energy use over the next few years. Because the time periods for these goals are much less than the average lifetime of a building, existing buildings will need to be retrofitted. There are two different types of retrofitting: shallow and deep. Shallow retrofits involve the quickest and least expensive improvements often including reducing infiltration around windows, under doors, etc and blowing more insulation into the attic. Deep retrofits are those that involve costly renovation and typically include adding insulation to the walls and replacing windows. A new, easily installable, inexpensive, and thin insulation would move insulating the walls from the deep retrofit category to the shallow retrofit category and thus would revolutionize the process of retrofitting homes to make them more energy efficient. This thesis provides an overview of a concept for a new, easily installable, inexpensive, thin aerogel-based insulation and goes into detail on how the thermal properties of the aerogel were measured and validated. The transient hot-wire method for measuring the thermal conductivity of very low thermal conductivity silica aerogel (1 0mW/m K at 1 atm) along with a correction for end effects was validated with the NIST (National Institute of Standards and Technology) Standard Reference Material 1459, fumed silica board to within 1 mW/mK. Despite the translucence of the aerogel at certain wavelengths, radiation is not an issue through the aerogel during the hot-wire test but may be an issue in actual use as an insulation. The monolithic aerogel thermal conductivity drops significantly with slightly reduced pressure (3.2 mW/m K at 0.1atm). For the final composite insulation, the new silica aerogel formula is a great choice and it is recommended to reduce the pressure around the aerogel to 1 / 1 0 th. In the future, a prototype of an insulation panel combining a 3-D truss structure, monolithic or granular silica aerogel, and reduced pressure will be constructed and tested.
by Ellann Cohen.
S.M.
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Abbas, Ibrahim, and Alexander Thurann. "Implementering av Aerogel-matta vid köldbryggor." Thesis, Tekniska Högskolan, Jönköping University, JTH, Byggnadsteknik och belysningsvetenskap, 2020. http://urn.kb.se/resolve?urn=urn:nbn:se:hj:diva-50259.
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Coman, Marius. "The Hall A Aerogel Čerenkov detector." FIU Digital Commons, 2000. http://digitalcommons.fiu.edu/etd/2413.
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The efficiency of the Aerogel Čerenkov detector for detecting particles having velocities greater than the speed of light in the aerogel media and the yield for rejecting particles having subthreshold velocities - smaller than the speed of light in the interaction media - was studied and is presented. The efficiency/inefficiency determination of the Aerogel Čerenkov detector consists of calculating the probabilities that a particle having a velocity above/below threshold generates a photoelectron in the aerogel block. The efficiency is determined using the normalised pulse height distribution of the photoelectrons. The Aerogel Čerenkov detector will play a key role in particle identification (PID) processes in Hall A at Jefferson Lab, allowing the separation of pseudoscalar mesons from pions which is required for many experiments to tag the flavor of the mesons and to identify the final states of interest for various experiments performed at Jefferson Lab.
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Carl, Michael. "Particle identification with aerogel Ĉerenkov detectors." FIU Digital Commons, 2003. http://digitalcommons.fiu.edu/etd/2046.
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Two detectors for charged particle identification have been built and tested. First, a test setup for a diffusion box threshold detector, using a 5 cm thick aerogel radiator has been designed and tested at the KEK PS facility in Japan. Using white Millipore paper as a diffuse reflector inside a diffusion box, the Ĉerenkov light gets scattered randomly until it hits one of the photomultipliers. On average up to 20 photoelectrons detected for pions at 1.2 GeV/c have been observed. Second, collection of Ĉerenkov light with an acrylic wavelength shifting plate was investigated. The test setup consisted of a plate, 30 cm long, 10 cm wide, and 1 cm thick placed behind a 5 cm deep stack of aerogel tiles. On the long ends the wavelength shifter was read out by two 5-inch photomultipliers. The response of the system to pions and protons at 1.2 GeV/c momentum was measured at the KEK PS facility in Japan. On average 6 photoelectrons radiated in the aerogel could be detected.
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Cao, Shengli. "Preparation, characterization and applications of monolithic titania-silica aerogels /." View abstract or full-text, 2007. http://library.ust.hk/cgi/db/thesis.pl?EVNG%202007%20CAO.
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Wang, Liang. "Aerogels based on biodegradable polymers and clay." Doctoral thesis, Universitat Politècnica de Catalunya, 2015. http://hdl.handle.net/10803/336971.
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Foam-like aerogels based on biodegradable polymers and sodium montmorillonite (Na+-MMT) clay were prepared through an environmentally friendly freeze-drying process. Both synthesized and bio-based polymers were utilized in this thesis, including polyvinyl alcohol (PVOH), carboxylmethylcellulose (CMC), xanthan gum, agar, Arabic gum and starch. The morphologies of aerogels were characterized using scanning electron microscopy. The mechanical properties investigation included compression and impact tests. Porosities and solid densities were measured using a helium pycnometer while the pore size distribution was determined by automated mercury porosimeters.
Most of polymer-clay aerogels exhibited porous and layered structures that were formed via ice templating. However, high viscosity of the precursor solution may break the layered architecture by retarding the formation of ice crystals (e.g. 2.5 wt% agar aqueous solution). The structures as well as the properties of aerogels were mainly influenced by polymer/clay proportion. Polymer molecules play a role of glue linking the clay nanoparticles, improving the structural integrity and hence the mechanical performance of the aerogels. On the other hand, clay platelets serve as a physical barrier that increases the heat endurance.
Recycled cellulose fibers (RCF) that were isolated from waste paper pulp were also used to prepare bio-based aerogels. Adding another biopolymer CMC into RCF aerogels, the resultant RCF-CMC composite aerogels showed different microstructures and enhanced mechanical properties.
Physical blending and chemical crosslinking were used to tailor the mechanical properties of xanthan gum/clay aerogels and starch/clay aerogels, respectively. Blending agar with xanthan gum in aqueous solution, the resultant aerogels displayed a significant improvement in mechanical properties compared with those containing a single biopolymer. Moreover, they exhibited tunable microstructures and mechanical properties by changing agar/xanthan gum ratio in the aerogels. As to starch/clay aerogels, the incorporation of glutaraldehyde enhanced the structural integrity and mechanical properties of the aerogels through crosslinking reaction between glutaraldehyde and starch molecules, which was proved by Fourier-Transform infrared (FT-IR) spectroscopy analysis.
The evaluation of the flammability of aerogels was conducted with a cone colorimeter while the thermal stability was obtained from the results of thermogravimetric analysis. In regard to PVOH-clay aerogel, different types of flame retardant fillers, such as aluminum trihydroxide (ALH), ammonium polyphosphate (APP), silica gel and potassium carbonate, were adopted to modify their flame retardant properties. The results showed that ALH addition enhanced the flame retardancy as well as mechanical properties. For RCF-CMC aerogels, APP and clay played a synergetic effect on the flame retardancy and thermal stability.En esta Tesis se han preparado diversos aerogeles usando polímeros biodegradables como matriz y arcilla como refuerzo, a través de un proceso de fabricación amigable con el medio ambiente. Los polímeros empleados han sido tanto de origen natural (goma árabiga, agar-agar, goma xantana, almidón) o sintéticos como la carboximetilcelulosa (CMC) o el alcohol polivinílico. Los compuestos formados se han caracterizado a través de diferentes técnicas con el objeto de relacionar las morfologías generadas con las propiedades térmicas y mecánicas resultantes. La gran mayoría de los aerogeles polímero/arcilla exhiben una estructura porosa y laminar que se forma a raíz de la liofilización. Sin embargo, se ha apreciado que altas viscosidades en la solución precursora puede romper la arquitectura laminar al retardar el crecimiento de los cristales de hielo (ej. Solución acuosa de 2.5 % peso de agar). La estructura y las propiedades de los aerogeles están asimismo y en general influenciados por la relación polímero/arcilla. En estos sistemas, las moléculas de polímero actúan a manera de pegamento uniendo las partículas de arcilla, incrementando de esa manera notablemente la capacidad mecánica de los aerogeles. Por otro lado la arcilla actúa entre otras formas, como barrera térmica incrementando la resistencia térmica y al fuego de las espumas formadas. Dentro de este trabajo se han empleado fibras de celulosa recicladas de residuos de papel en un intento de preparar bio-aerogeles a partir de material de desecho. La unión de estas fibras con CMC permitió obtener aerogeles con propiedades mejoradas y la posibilidad de emplear estos residuos en un segundo uso. Además del mezclado físico, en algunos casos se ha realizado una reacción de entrecruzamiento para ajustar las propiedades finales, como en el caso de los aerogeles goma xantana/arcilla o almidón/arcilla. La mezcla de agar con goma xantana en solución acuosa resultó en un notable aumento de propiedades con respecto a las composiciones que contenían un único polímero, debido al cambio morfológico inducido, pasando de una estructura laminar a una de tipo panal de abeja (honeycomb). De esta forma y a través de la relación entre estos dos polímeros naturales ha sido posible balancear y definir las propiedades finales deseadas para el aerogel. En los sistemas almidón/arcilla el entrecruzamiento se ha conseguido a través de un agente externo como el glutaraldehido. Atendiendo a su posible uso final, unas de las propiedades más relevantes en los aerogeles que se ha estudiado ha sido la estabilidad térmica y la resistencia al fuego. En este sentido, se han preparado sistemas basados en Polivinilalcohol/arcilla modificados con diferentes retardantes de llama. De los diversos aditivos probados la combinación con hidróxido de aluminio ha mostrado un efecto sinérgico incrementando tanto de la resistencia a fuego como las propiedades mecánicas. En los sistemas basados en celulosa la presencia de polifosfato de amonio y arcilla ha demostrado así mismo un efecto potenciador de la estabilidad térmica y en el retardo de llama.
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Tan, Hong Wee. "Neon in porous glass samples and aerogels." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1998. http://www.collectionscanada.ca/obj/s4/f2/dsk2/tape15/PQDD_0027/MQ34425.pdf.
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