Solid electrolytes for electrochromic devices based on reversible metal electrodeposition

Air conditioning and lighting costs can be reduced substantially by changing the optical properties of "intelligent windows." The electrochromic devices studied to date have used copper as an additive. Copper, used here as an electrochromic material, was dissolved in an aqueous animal protein-derived gel electrolyte. This combination constitutes the electrochromic system for reversible electrodeposition. Cyclic voltammetry, chronoamperometric and chromogenic analyses indicated that were obtained good conditions of transparency (initial transmittance of 70%), optical reversibility, small potential window (2.1 V), variation of transmittance in visible light (63.6%) and near infrared (20%) spectral regions. Permanence in the darkened state was achieved by maintaining a lower pulse potential (-0.16 V) than the deposition potential (-1.0 V). Increasing the number of deposition and dissolution cycles favored the transmittance and photoelectrochemical reversibility of the device. The conductivity of the electrolyte (10(-3) S/cm) at several concentrations of CuCl2 was determined by electrochemical impedance spectroscopy. A thermogravimetric analysis confirmed the good thermal stability of the electrolyte, since the mass loss detected up to 100 degrees C corresponded to water evaporation and decomposition of the gel started only at 200 degrees C. Micrographic and small angle X-ray scattering analyses indicated the formation of a persistent deposit of copper particles on the ITO. (C) 2012 Elsevier B.V. All rights reserved.

The Role of Nanometer-Scaled Ligand Patterns in Polyvalent Binding by Large Mannan-Binding Lectin Oligomers

Mannan-binding lectin (MBL) is an important protein of the innate immune system and protects the body against infection through opsonization and activation of the complement system on surfaces with an appropriate presentation of carbohydrate ligands. The quaternary structure of human MBL is built from oligomerization of structural units into polydisperse complexes typically with three to eight structural units, each containing three lectin domains. Insight into the connection between the structure and ligand-binding properties of these oligomers has been lacking. In this article, we present an analysis of the binding to neoglycoprotein-coated surfaces by size-fractionated human MBL oligomers studied with small-angle x-ray scattering and surface plasmon resonance spectroscopy. The MBL oligomers bound to these surfaces mainly in two modes, with dissociation constants in the micro to nanomolar order. The binding kinetics were markedly influenced by both the density of ligands and the number of ligand-binding domains in the oligomers. These findings demonstrated that the MBL-binding kinetics are critically dependent on structural characteristics on the nanometer scale, both with regard to the dimensions of the oligomer, as well as the ligand presentation on surfaces. Therefore, our work suggested that the surface binding of MBL involves recognition of patterns with dimensions on the order of 10-20 nm. The recent understanding that the surfaces of many microbes are organized with structural features on the nanometer scale suggests that these properties of MBL ligand recognition potentially constitute an important part of the pattern-recognition ability of these polyvalent oligomers. The Journal of Immunology, 2012, 188: 1292-1306.

Low-Resolution Molecular Models Reveal the Oligomeric State of the PPAR and the Conformational Organization of Its Domains in Solution

The peroxisome proliferator-activated receptors (PPARs) regulate genes involved in lipid and carbohydrate metabolism, and are targets of drugs approved for human use. Whereas the crystallographic structure of the complex of full length PPAR gamma and RXR alpha is known, structural alterations induced by heterodimer formation and DNA contacts are not well understood. Herein, we report a small-angle X-ray scattering analysis of the oligomeric state of hPPAR gamma alone and in the presence of retinoid X receptor (RXR). The results reveal that, in contrast with other studied nuclear receptors, which predominantly form dimers in solution, hPPAR gamma remains in the monomeric form by itself but forms heterodimers with hRXR alpha. The low-resolution models of hPPAR gamma/RXR alpha complexes predict significant changes in opening angle between heterodimerization partners (LBD) and extended and asymmetric shape of the dimer (LBD-DBD) as compared with X-ray structure of the full-length receptor bound to DNA. These differences between our SAXS models and the high-resolution crystallographic structure might suggest that there are different conformations of functional heterodimer complex in solution. Accordingly, hydrogen/deuterium exchange experiments reveal that the heterodimer binding to DNA promotes more compact and less solvent-accessible conformation of the receptor complex.

Structure of the haptoglobin-haemoglobin complex

Red cell haemoglobin is the fundamental oxygen-transporting molecule in blood, but also a potentially tissue-damaging compound owing to its highly reactive haem groups. During intravascular haemolysis, such as in malaria and haemoglobinopathies(1), haemoglobin is released into the plasma, where it is captured by the protective acute-phase protein haptoglobin. This leads to formation of the haptoglobin-haemoglobin complex, which represents a virtually irreversible non-covalent protein-protein interaction(2). Here we present the crystal structure of the dimeric porcine haptoglobin-haemoglobin complex determined at 2.9 angstrom resolution. This structure reveals that haptoglobin molecules dimerize through an unexpected beta-strand swap between two complement control protein (CCP) domains, defining a new fusion CCP domain structure. The haptoglobin serine protease domain forms extensive interactions with both the alpha- and beta-subunits of haemoglobin, explaining the tight binding between haptoglobin and haemoglobin. The haemoglobin-interacting region in the alpha beta dimer is highly overlapping with the interface between the two alpha beta dimers that constitute the native haemoglobin tetramer. Several haemoglobin residues prone to oxidative modification after exposure to haem-induced reactive oxygen species are buried in the haptoglobin-haemoglobin interface, thus showing a direct protective role of haptoglobin. The haptoglobin loop previously shown to be essential for binding of haptoglobin-haemoglobin to the macrophage scavenger receptor CD163 (ref. 3) protrudes from the surface of the distal end of the complex, adjacent to the associated haemoglobin alpha-subunit. Small-angle X-ray scattering measurements of human haptoglobin-haemoglobin bound to the ligand-binding fragment of CD163 confirm receptor binding in this area, and show that the rigid dimeric complex can bind two receptors. Such receptor cross-linkage may facilitate scavenging and explain the increased functional affinity of multimeric haptoglobin-haemoglobin for CD163 (ref. 4).

Characterization of Heparin-induced Glyceraldehyde-3-phosphate Dehydrogenase Early Amyloid-like Oligomers and Their Implication in alpha-Synuclein Aggregation

Lewy bodies and Lewy neurites, neuropathological hallmarks of several neurological diseases, are mainly made of filamentous assemblies of alpha-synuclein. However, other macromolecules including Tau, ubiquitin, glyceraldehyde-3-phosphate dehydrogenase, and glycosaminoglycans are routinely found associated with these amyloid deposits. Glyceraldehyde-3-phosphate dehydrogenase is a glycolytic enzyme that can form fibrillar aggregates in the presence of acidic membranes, but its role in Parkinson disease is still unknown. In this work, the ability of heparin to trigger the amyloid aggregation of this protein at physiological conditions of pH and temperature is demonstrated by infrared and fluorescence spectroscopy, dynamic light scattering, small angle x-ray scattering, circular dichroism, and fluorescence microscopy. Aggregation proceeds through the formation of short rod-like oligomers, which elongates in one dimension. Heparan sulfate was also capable of inducing glyceraldehyde-3-phosphate dehydrogenase aggregation, but chondroitin sulfates A, B, and C together with dextran sulfate had a negligible effect. Aided with molecular docking simulations, a putative binding site on the protein is proposed providing a rational explanation for the structural specificity of heparin and heparan sulfate. Finally, it is demonstrated that in vitro the early oligomers present in the glyceraldehyde-3-phosphate dehydrogenase fibrillation pathway promote alpha-synuclein aggregation. Taking into account the toxicity of alpha-synuclein prefibrillar species, the heparin-induced glyceraldehyde-3-phosphate dehydrogenase early oligomers might come in useful as a novel therapeutic strategy in Parkinson disease and other synucleinopathies.

Hofmeister effects on the colloidal stability of poly(ethylene glycol)-decorated nanoparticles

The colloidal stability of poly(ethylene glycol)-decorated poly(methyl methacrylate), PMMA/Tween-20, particles was investigated by means of phase separation measurements, in the presence of sodium fluoride (NaF), sodium chloride, sodium bromide, sodium nitrate, or sodium thiocyanate (NaSCN) at 1.0 mol L-1. Following Hofmeister's series, the dispersions of PMMA/Tween-20 destabilized faster in the presence of NaF than with NaSCN. After the phase separation, the systems were homogenized and except for the dispersions in NaF, re-dispersed particles took longer to destabilize, indicating that anions adsorbed on the particles, creating a new surface. Except for F- ions, the adsorption of anions on the polar outmost shell was evidenced by means of tensiometry and small-angle X-ray scattering measurements. Fluoride ions induced the dehydration of the polar shell, without affecting the polar shell electron density, and the formation of very large aggregates. A model was proposed to explain the colloidal behavior in the presence of Hofmeister ions.

Crystal structures of Leptospira interrogans FAD-containing ferredoxin-NADP+ reductase and its complex with NADP+

Abstract Background Ferredoxin-NADP(H) reductases (FNRs) are flavoenzymes that catalyze the electron transfer between NADP(H) and the proteins ferredoxin or flavodoxin. A number of structural features distinguish plant and bacterial FNRs, one of which is the mode of the cofactor FAD binding. Leptospira interrogans is a spirochaete parasitic bacterium capable of infecting humans and mammals in general. Leptospira interrogans FNR (LepFNR) displays low sequence identity with plant (34% with Zea mays) and bacterial (31% with Escherichia coli) FNRs. However, LepFNR contains all consensus sequences that define the plastidic class FNRs. Results The crystal structures of the FAD-containing LepFNR and the complex of the enzyme with NADP+, were solved and compared to known FNRs. The comparison reveals significant structural similarities of the enzyme with the plastidic type FNRs and differences with the bacterial enzymes. Our small angle X-ray scattering experiments show that LepFNR is a monomeric enzyme. Moreover, our biochemical data demonstrate that the LepFNR has an enzymatic activity similar to those reported for the plastidic enzymes and that is significantly different from bacterial flavoenzymes, which display lower turnover rates. Conclusion LepFNR is the first plastidic type FNR found in bacteria and, despite of its low sequence similarity with plastidic FNRs still displays high catalytic turnover rates. The typical structural and biochemical characteristics of plant FNRs unveiled for LepFNR support a notion of a putative lateral gene transfer which presumably offers Leptospira interrogans evolutionary advantages. The wealth of structural information about LepFNR provides a molecular basis for advanced drugs developments against leptospirosis.

The influence of both urea and 2,2,2

The influence of external agents on proteins function and structure is essential to elucidate the unfolding pathways and self-assemble properties. The knowledge of the protein amyloid fibril formation process is important due to the fields that this subjected is related, in particular for the neurodegenerative disorders. In the present work we studied the influence of both urea and 2,2,2-Trifluoroethanol (TFE) and temperature on the structure and proteinprotein interactions of Bovine Serum Albumin (BSA), by means of UV-Vis spectroscopy, static fluorescence and small angle X-ray scattering technique. The experiments were performed in samples composed by 10 and 3 mg/ml of BSA at pH 5.8, near the protein pI. First, Thioflavin-T fluorescence measurements indicated that urea, in the absence of TFE, was able to increase the amyloid fibril formation of BSA at 45oC and increasing the urea concentration the rate of amyloid fibril formation also increases. Concerning the presence of TFE, SAXS data suggest that BSA tridimensional structure is not altered by the presence of TFE 5% and 10% v/v in all studied protein concentrations. Interestingly, the presence of TFE on the urea-containing BSA also increases the rate of amyloid fibril formation, as compared to the TFE-free system, indicating that TFE can catalyze the amyloid-fibril formation. The presence of TFE 20% v/v, however, induces the formation of aggregates, but at this time we were not able to infer if such aggregates are amyloidlike or amorphous. Taking together, the results give support to infer that BSA can for fibrils in the presence of urea at 45oC and TFE can act as a stabilizer or as a denaturant agent for BSA.

Clay-containing block copolymer nanocomposites with aligned morphology prepared by extrusion

Clay-containing nanocomposites of polystyrene-b-poly(ethylene-co-butylene)-b-polystyrene (SEBS) copolymers having cylindrical domains were obtained by melt extrusion using a tape die. One type of sample (SEBS-MA) had maleic anhydride attached to the middle block. Two types of organoclays were added, namely Cloisite 20A and Cloisite 30B. Small angle X-ray scattering and transmission electron microscopy (TEM) analyses showed that the addition of 20A clay to SEBS and SEBS-MA resulted in nanocomposites with intercalated and partially exfoliated structures, respectively. The addition of 30B clay to SEBS and SEBS-MA promoted the formation of composites containing relatively large micron-sized and partially exfoliated clay particles, respectively. Our TEM analysis revealed that clay particles embedded in SEBS are preferably in contact with the polystyrene cylindrical domains, while in SEBS-MA they are in contact with the maleated matrix. The extrusion processing promoted alignment of the axes of the polystyrene cylinders along the extrusion direction in all samples, and the basal planes of the clay particles were mostly parallel to the main external surfaces of the extruded tapes. © 2013 Society of Chemical Industry.

Staphylococcus aureus thiaminase II: oligomerization warrants proteolytic protection against serine proteases

Staphylococcus aureus TenA (SaTenA) is a thiaminase type II enzyme that catalyzes the deamination of aminopyrimidine, as well as the cleavage of thiamine into 4-amino-5-hydroxymethyl-2-methylpyrimidine (HMP) and 5-(2-hydroxyethyl)-4-methylthiazole (THZ), within thiamine (vitamin B1) metabolism. Further, by analogy with studies of Bacillus subtilis TenA, SaTenA may act as a regulator controlling the secretion of extracellular proteases such as the subtilisin type of enzymes in bacteria. Thiamine biosynthesis has been identified as a potential drug target of the multi-resistant pathogen S. aureus and therefore all enzymes involved in the S. aureus thiamine pathway are presently being investigated in detail. Here, the structure of SaTenA, determined by molecular replacement and refined at 2.7 A ° resolution to an R factor of 21.6% with one homotetramer in the asymmetric unit in the orthorhombic space group P212121, is presented. The tetrameric state of wild-type (WT) SaTenA was postulated to be the functional biological unit and was confirmed by small-angle X-ray scattering (SAXS) experiments in solution. To obtain insights into structural and functional features of the oligomeric SaTenA, comparative kinetic investigations as well as experiments analyzing the structural stability of the WT SaTenA tetramer versus a monomeric SaTenA mutant were performed.

Properties of a new poly-ether-glycol copolymer.

Triblock copolymers are made of monomer segments, being the central part usually hydrophobic and the outer parts hydrophilic. By varying sizes, molecular weights and monomer types of the segments one obtains different final molecules, with different physico-chemical properties, which are directly related to the performance of the final product. Looking for new products to be used, among other possibilities, in biological applications, a new polymer (Figure 1) was synthesized by the Dow Chemical and studied by Size Exclusion Chromatography, Fourier Transformed Infrared Spectrometry, Small-angle X-ray Scattering (SAXS) and its cloud point was determined by measuring light transmittance. The studies showed low molecular polydispersivety, but different polarities in the macromolecules fractions. Due to the low solubility of Diol in water, a mixture of water/butyl diglycol was used as solvent. An extensive analysis by SAXS was performed for concentrations from 50 wt% to 80 wt% of Diol in solution. Small concentrations showed very low signal to noise ratio, making it impossible to be analysed. The scattering intensity including the form factor of polydisperse non-homogeneous spheres, and the structure factor of interacting hard spheres was fitted to the curves. As the polymer concentration is high, the fitting of form factors of direct and reverse micelles were compared. The results for direct micelles were better up to 80 wt%, whereas at 90 wt% and 95 wt% the curves were better fitted by reverse micelles. It might seem odd that direct micelles are present up to such high concentrations, but it might have been caused by the presence of butyl diglycol, which increases the solubility of Diol in water. The inner and outer radius of the micelles, electron density distribution, and interaction radius of the micelles were obtained. The polydispersivety increases with Diol concentration. Besides, the interaction radius increases with solvent concentration, even when reversed micelles are present. In the last case, accompanied by an increase of inner radius (water content), as there are fewer Diol molecules to involve the water nuclei, which become larger, further apart, and in less number.

Untersuchung der Ordnung und Diffusion von Polymerdispersionen bei ihrer Verfilmung

Im Rahmen dieser Arbeit wurde die, für industrielle Applikationen sehr wichtige, Trocknung und Verfilmung von Latexdispersionen untersucht. Unter der Verfilmung wird in diesem Zusammenhang allgemein der Übergang einer Polymerdispersion in einen transparenten, mechanisch stabilen Polymerfilm während ihrer Trocknung verstanden. Für die Untersuchungen wurden schwerpunktmäßig Streumethoden verwendet. Die Untersuchungen haben gezeigt, daß die Streuung eine besonders geeignete Methode zur Untersuchung der Verfilmung ist, die in Abhängigkeit des beobachteten Streuvektorbereichs, der verwendeten Strahlung, der Probenpräparation und des resultierenden Kontrasts eine Vielzahl unterschiedlicher Informationen über die Verfilmung in ihren verschiedenen Phasen liefert. Von besonderem Interesse war es, den prinzipiellen Verlauf der Verfilmung bei den heterogen trocknenden Reinacrylatlatices zu untersuchen. Dazu wurde mit Hilfe der Röntgenultrakleinwinkelstreuung gezielt der Zustand der Partikel in den einzelnen Phasen der heterogen trocknenden Proben beobachtet. Mit Hilfe der Neutronenkleinwinkelstreuung konnte das Verhalten des Emulgators während der Verfilmung und dessen Verteilung im resultierenden Film genauer untersucht werden. Die Röntgenkleinwinkelstreuung erlaubte eine eingehende Untersuchung der Kristallisation des Emulgators im trockenen Film. Geeignete Kontrastierung durch gezielte Deuterierung ermöglichte die Untersuchung des Comonomereinflusses auf die Interdiffusion von Latexpartikeln mit Neutronenkleinwinkelstreuung. Aus den Meßergebnissen wurde ein Modell zur heterogenen Trocknung von Latexdispersionen entwickelt, das den Ablauf der Verfilmung in einem konsistenten Bild zusammenfaßt.

Bruchmechanismen an Polymergrenzflächen

In der vorliegenden Arbeit wurden Untersuchungen zur Aufklärung des Versagens thermisch verschweißter Polymergrenzflächen (hier: Polymethylmethacrylat) durchgeführt. Solch ein Wissen kommt in der Praxis bei sogenannten Sollbruchstellen zum Einsatz. Dabei muss die Grenzschicht bis zu einer bestimmten Belastungsintensität stabil bleiben bei höherer Belastung jedoch brechen. Zudem ist eine stabile Risspropagation entlang der Grenzschicht wichtig.Neben der Bruchstabilitätsbestimmung mit Hilfe des Double Cantilever Beam Tests wurden die beim Versagen der Grenzschicht entstandenen Defekte untersucht. Die Analyse der Bruchfläche erfolgte mit Mikroskopie und Höhenprofilometrie. Defekte im Volumen wurden durch Scanning-Ultra Small Angle X-ray Scattering und Scanning Microfokus-Small Angle X-ray Scattering untersucht.Im Modellsystem können Sollbruchstellen bis zu einer Belastungsintensität von maximal 280J/m² durch die Verschweißungsdauer eingestellt werden. Die Untersuchung der Bruchflächen lieferte ein kombiniertes Modell aus Ausheil- und Interdiffusionsprozess. Ferner folgt aus den Streuuntersuchungen, dass beim Modellsystem keine hochgeordneten Defektstrukturen vorliegen. Die entstandenen Strukturen folgen einem Modell diffuser Defektgrenzflächen. Über die gemessene Diffusivität kann zudem auf die Energiedissipation im Bereich um das Rissende geschlossen werden. Sie ist im unmittelbaren Rissbereich am Höchsten und nimmt mit Entfernung davon ab. Dabei haben die Defektbereiche eine Größe bis zu 650µm. Die Richtung der von außen angelegten Belastung spielt bei der räumlichen Orientierung der Defekte keine Rolle.

Synthese von flüssigkristallinen Polysiloxanen und Charakterisierung der smektischen Phasen

Gegenstand dieser Arbeit ist die Untersuchung der smektischen Phasen von Polysiloxanen mit flüssigkristallinen Seitengruppen (LC-Polysiloxane). Der erste Teil der vorliegenden Arbeit befasste sich mit der Herstellung verschiedener flüssigkristalliner ferroelektrischer Polysiloxane. Die Polymere wurden in Bezug auf das verwendete Polymerrückgrat (Homo- und Copolysiloxan) sowie durch den zusätzlichen Einbau von vernetzbaren Seitengruppen variiert. Im zweiten Teil der Arbeit wurden die Eigenschaften der smektischen Phasen der hergestellten Substanzen näher untersucht. Ein erster Untersuchungsgegenstand war das Dehnungsverhalten von freistehenden flüssigkristallinen Elastomerfilmen (LCE). Bei der Verwendung eines Polymers, in dem nur ein Teil des Polysiloxanrückgrats mit Seitengruppen substituiert ist, wird die uniaxiale Dehnung des Films parallel zu den smektischen Schichten durch eine gleichmäßige Kontraktion in der Filmebene und parallel zur Schichtnormalen ausgeglichen, was auf einen außergewöhnlich niedrigen smektischen Schichtkompressionsmodul zurückzuführen ist. Im Gegensatz dazu ist dieser Modul bei den Homopolymersystemen so groß, dass praktisch senkrecht zu den smektischen Schichten keine Kontraktion stattfindet. Ein zweiter Untersuchungsgegenstand der Netzwerkbildung bestand in der Bestimmung der dynamisch-mechanischen Eigenschaften der LC-Polysiloxane mittels eines Oszillationsrheometers. Hier erfolgten die Messungen von Speicher- und Verlustmodul in Abhängigkeit vom Polymerrückgrat und von der Vernetzung. Die unvernetzten Systeme zeigten in den smektischen Phasen (oberhalb Tg) noch – im wesentlichen – Festkörpereigenschaften (physikalische Vernetzung) mit einem dominierenden Speichermodul beim LC-Homopolysiloxan. Beim LC-Copolysiloxan haben beide Module eine gleiche Größenordnung. Am Phasenübergang in die isotrope Phase wurden beide Module absolut kleiner, der Verlustmodul aber relativ größer. In der isotropen Phase verhalten sich die LC-Polymere damit überwiegend wie viskose Schmelzen. Außerdem korrelierten die mittels DSC bestimmten Phasenübergangstemperaturen mit einer Änderung der dynamisch-mechanischen Eigenschaften. Nach der Vernetzung dominierte der Speichermodul sowohl beim LC-Homo- als auch beim LC-Copolysiloxan bis in die isotrope Phase, und es war aufgrund der Bildung einer festen Netzwerkstruktur keine Abhängigkeit der Module von Phasenübergängen mehr erkennbar. Als dritter Untersuchungsgegenstand wurde der Phasenübergang zwischen den beiden smektischen Phasen (SmC* nach SmA*) der flüssigkristallinen Polysiloxane näher behandelt. Als wichtigstes Ergebnis ist festzuhalten, dass die verdünnten LC-Polysiloxane an diesem Übergang fast keine Schichtdickenänderung aufweisen. Dazu wurde jeweils die röntgenographisch ermittelte Schichtdicke mit der aus den optischen Tiltwinkeln theoretisch berechneten Schichtdicke verglichen. Dadurch konnte gezeigt werden, dass sich die Phasenübergänge nach dem de Vries-Modell verhalten. Damit konnte zum ersten Mal an Polymersystemen ein de Vries-Verhalten nachgewiesen werden. Im Gegensatz dazu zeigte das Homopolysiloxan mit dem Dreiringmesogen beim Übergang von SmC* nach SmA* einen ausgeprägten Sprung in der Schichtdicke. Wie auch durch DSC-Messungen nachweisbar, lag ein Phasenübergang 1. Ordnung vor. Bei den LC-Copolysiloxanen liegt dagegen ein Phasenübergang 2. Ordnung vor. Schließlich wurde die Schichtdicke unter dem Einfluss der Vernetzung untersucht. Beim LC-Copolysiloxan mit dem Dreiringmesogen und einem Anteil an vernetzbaren Gruppen von 15 % wurde eine Stabilisierung der smektischen Phasen erreicht. Zum einen war die Änderung der Schichtdicke am SmC*-SmA*-Phasenübergang geringer im Vergleich zum unvernetzten System und zum anderen war noch 50 °C über der ursprünglichen Klärtemperatur eine smektische Schichtstruktur röntgenographisch nachzuweisen. Insgesamt ist es mit den verschiedenen Untersuchungsmethoden gelungen, einen systematischen Unterschied zwischen smektischen Homo- und Copolysiloxanen aufzuzeigen, der seinen Ursprung – aller Wahrscheinlichkeit nach – in der Mikrophasenseparation von Mesogenen und Polysiloxanketten findet.

Synthesis and characterization of metal-chalcogenide MQ 2-Nanoparticles (M = Mo, W, Zr; Q = S, O)

Here, we present the adaptation and optimization of (i) the solvothermal and (ii) the metal-organic chemical vapor deposition (MOCVD) approach as simple methods for the high-yield synthesis of MQ2 (M=Mo, W, Zr; Q = O, S) nanoparticles. Extensive characterization was carried out using X-ray diffraction (XRD), scanning and transmission electron micros¬copy (SEM/TEM) combined with energy dispersive X-ray analysis (EDXA), Raman spectroscopy, thermal analyses (DTA/TG), small angle X-ray scattering (SAXS) and BET measurements. After a general introduction to the state of the art, a simple route to nanostructured MoS2 based on the decomposition of the cluster-based precursor (NH4)2Mo3S13∙xH2O under solvothermal conditions (toluene, 653 K) is presented. Solvothermal decomposition results in nanostructured material that is distinct from the material obtained by decomposition of the same precursor in sealed quartz tubes at the same temperature. When carried out in the presence of the surfactant cetyltrimethyl¬ammonium bromide (CTAB), the decomposition product exhibits highly disordered MoS2 lamellae with high surface areas. The synthesis of WS2 onion-like nanoparticles by means of a single-step MOCVD process is discussed. Furthermore, the results of the successful transfer of the two-step MO¬CVD based synthesis of MoQ2 nanoparticles (Q = S, Se), comprising the formation of amorphous precursor particles and followed by the formation of fullerene-like particles in a subsequent annealing step to the W-S system, are presented. Based on a study of the temperature dependence of the reactions a set of conditions for the formation of onion-like structures in a one-step reaction could be derived. The MOCVD approach allows a selective synthesis of open and filled fullerene-like chalcogenide nanoparticles. An in situ heating stage transmission electron microscopy (TEM) study was employed to comparatively investigate the growth mechanism of MoS2 and WS2 nanoparticles obtained from MOCVD upon annealing. Round, mainly amorphous particles in the pristine sample trans¬form to hollow onion-like particles upon annealing. A significant difference between both compounds could be demonstrated in their crystallization conduct. Finally, the results of the in situ hea¬ting experiments are compared to those obtained from an ex situ annealing process under Ar. Eventually, a low temperature synthesis of monodisperse ZrO2 nanoparticles with diameters of ~ 8 nm is introduced. Whereas the solvent could be omitted, the synthesis in an autoclave is crucial for gaining nano-sized (n) ZrO2 by thermal decomposition of Zr(C2O4)2. The n-ZrO2 particles exhibits high specific surface areas (up to 385 m2/g) which make them promising candidates as catalysts and catalyst supports. Co-existence of m- and t-ZrO2 nano-particles of 6-9 nm in diameter, i.e. above the critical particle size of 6 nm, demonstrates that the particle size is not the only factor for stabilization of the t-ZrO2 modification at room temperature. In conclusion, synthesis within an autoclave (with and without solvent) and the MOCVD process could be successfully adapted to the synthesis of MoS2, WS2 and ZrO2 nanoparticles. A comparative in situ heating stage TEM study elucidated the growth mechanism of MoS2 and WS2 fullerene-like particles. As the general processes are similar, a transfer of this synthesis approach to other layered transition metal chalcogenide systems is to be expected. Application of the obtained nanomaterials as lubricants (MoS2, WS2) or as dental filling materials (ZrO2) is currently under investigation.