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Organisationseinheit der BAM
- 6 Materialchemie (392) (entfernen)
Eingeladener Vortrag
- nein (164)
Modeling of silicon surface topographies induced by single nanosecond laser pulse induced melt-flows
(2019)
Irradiation with a single nanosecond laser pulse in the melting regime can result in a characteristic change in the surface morphology of crystalline silicon. This has been verified experimentally in a variety of situations, where dimple-shaped surface topographies are produced. In this work, the dimple height, depth, and width are modeled following and extending in a more rigorous manner the approach of Wood and Giles [Phys. Rev. B 23, 2923–2942 (1981)] and that of Schwarz-Selinger and coworkers [Phys. Rev. B 64, 155323 (2001)], upon varying the laser irradiation parameters such as peak energy density, pulse duration, and wavelength. This is achieved with numerical simulations of one-dimensional heat flow as input to the analytical fluid-flow equations.
We report on the ferromagnetism of Sn1-xZnxO2 (x < 0.1) hierarchical nanostructures with various morphologies synthesized by a solvothermal route. A room temperature ferromagnetic and paramagnetic response was observed for all compositions, with a maximum in ferromagnetism for x = 0.04. The ferromagnetic behaviour was found to correlate with the presence of zinc on substitutional Sn sites and with a low oxygen vacancy concentration in the samples. The morphology of the nanostructures varied with zinc concentration. The strongest ferromagnetic response was observed in nanostructures with well-formed shapes, having nanoneedles on their surfaces. These nanoneedles consist of (110) and (101) planes, which are understood to be important in stabilizing the ferromagnetic defects. At higher zinc concentration the nanostructures become eroded and agglomerated, a phenomenon accompanied with a strong decrease in their ferromagnetic response. The observed trends are explained in the light of recent computational studies that discuss the relative stability of ferromagnetic defects on various surfaces and the role of oxygen vacancies in degrading ferromagnetism via an increase in free electron concentration.
The exploration of metal phosphonates has gained great interest during the last decades, because of their structural diversity. They are promising candidates for a variety of applications ranging from adsorbance to electrocatalysis. The knowledge of the Crystal structure is significant for assigning a coordination polymer for a specific function. We investigated the influence of the fluorination degree of the organic linker on the Crystal packing, the interlayer distance, and the hydrophobicity of the resulting compounds. With fluorinated and nonfluorinated benzylphosphonic acids as starting materials in mechanochemical synthesis, four novel cadmium benzylphosphonates were obtained. Their structures were solved from powder X-ray diffraction.
Metal phosphonates are metal-organic compounds consisting of a metal core and a phosphonate ligand. Depending on the nature of the ligand, metal phosphonates appear in different structures covering the range from molecular compounds to three-dimensional networks. Due to their structural diversity, the chemistry of metal phosphonates has gained great interest during the last decades. Metal phosphonates can be used for various applications as gas storage and separation, magnetism, and energy conversion. Especially transition metal phosphonates are promising candidates as electrocatalysts. Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. By milling the reactants, various organic, inorganic, and metal-organic compounds can be obtained in high yields. Here, we present the synthesis of different new metal phosphonates obtained by grinding of metal acetates with respective phosphonic acids. By varying the ratio of the reactants, we are able to determine the composition of the final products. The addition of small amounts of liquid to the grinding process tends to increase the product’s crystallinity. The crystal structures of the new compounds were determined from powder X-ray data.
Cadmium benzylphosphonate Cd(O3PBn)·H2O and its fluorinated derivates Cd(O3PBn-3F)·H2O, Cd(O3PBn-4F)·H2O, and Cd(O3PBn-F5)·H2O were synthesized mechanochemically. The Crystal structures of the compounds were determined based on powder X-ray diffraction (PXRD) data. The influence of the ligand substitution on the crystal structure of the metal phosphonate was determined. The hydrophobicity as a function of degree of fluorination was investigated using dynamic vapor sorption.
Ca-, Sr-, and Ba-Based coordination polymers (CPs) were prepared mechanochemically by milling metal-hydroxide samples with anthranilic acid (oABAH). {[Ca(oABA)2(H2O)3]}n consists of one-dimensional polymeric chains that are further connected by a hydrogen-bonding network. {[Sr(oABA)2(H2O)2]·H2O}n is a one-dimensional CP in which water molecules bridge Sr2+ ions and increase the dimensionality by building an extended network. {[Ba(oABA)2(H2O)]}n crystallizes as a two-dimensional CP comprising one bridging water molecule. The cation radii influence the inorganic connectivity and dimensionality of the resulting crystal structures. The crystal structures were refined from powder X-ray diffraction data using the Rietveld method. The local coordination environments were studied via extended X-ray absorption fine structure (EXAFS) measurements. The compounds were further characterized using comprehensive analytical methods such as elemental analysis, thermal analysis, MAS NMR, imaging, and dynamic vapor sorption (DVS) measurements. Compounds 1, 2, and 3 exhibit small surface areas which decrease further after thermal annealing experiments. All compounds exhibit a phase transformation upon heating, which is only reversible in 3.
The novel synthesis route has been developed for hierarchically structured; nanorods and nanosheets of Sb4O5Cl2 from a single precursor, with dimension range between 57–90 nm. X-ray powder diffraction analysis confirmed the monoclinic crystal symmetry in P21/c(14)with structure type Sb4O5Cl2 for both forms; the nanorods and nanosheets. Rietveld refinements and crystallite size investigations of the powder patterns revealed significant enhancement in intensity with subtle variation in the lattice parameters and crystallite size decrease in case of nanosheets in comparison to the nanorods assembly. Through scanning electron microscopy, a composition commensurate to Sb4O5Cl2 at% with averaged dimensions; dia.∼90 nm, l ∼ 2 μm for nanorods and dia.∼50–150 nm for nanosheets got corroborated. Owing to the quantum confinement a band gap widening was observed while moving from bulk to nano regime, i.e. 3.25, 3.31 and 3.34 eV, for bulk, nanosheets, and nanorods, respectively. In the case of nanosheets, the highest value of dielectric constant was observed, i.e. 87, as compared to nanorods and the bulk, i.e. 40 and 35.5, respectively. The nanosheets also showed the highest value of dielectric and tangent loss with an increase in frequency due to the least crystallite size of these nanonetworks. Nanosheets depicted the higher AC conductivity at low frequency due to the alignment of the charges but its value decreases at the higher frequency due to lack of time for charge reorientation. The hopping phenomenon was observed in all three cases with the most prominent one in bulk case at higher frequencies.
CsCoO2, featuring a two-dimensional layered architecture of edge- and vertex-linked CoO4tetrahedra, is subjected to a temperature-driven reversible second-order phase transformation at 100 K, which corresponds to a structuralrelaxation with concurrent tilting and breathing modes of edge-sharing CoO4tetrahedra. In the present investigation, it was found that pressure induces a phase transition, which encompasses a dramatic change in the connectivity ofthe tetrahedra. At 923 K and 2 GPa, beta-CsCoO2 undergoes a first-order phasetransition to a new quenchable high-pressure polymorph,alpha-CsCoO2. It is built up of a three-dimensional cristobalite-type network of vertex-sharing CoO4 tetrahedra. According to a Rietveld refinement of high-resolution powderdiffraction data, the new high-pressure polymorph gamma-CsCoO2 crystallizes in the tetragonal space groupI41/amd:2 (Z= 4) with the lattice constants a= 5.8711 (1) and c= 8.3214 (2) A, corresponding to a shrinkage in volume by 5.7% compared with the ambient-temperature and atmospheric pressure-CsCoO2polymorph.The pressure-induced transition (beta>gamma) is reversible;-CsCoO2 stays metastable under ambient conditions, but transforms back to the-CsCoO2structure upon heating to 573 K. The transformation pathway revealed isremarkable in that it is topotactic, as is demonstrated through a clean displacive transformation track between the two phases that employs the symmetry oftheir common subgroupPb21a(alternative setting of space group No. 29 that matches the conventional-phase cell).
The number of publications reporting the amount of microplastic (MP) all over the world increased rapidly. Methods used so far are very time consuming and not able to provide information on total contents. As harmonised sampling, sample preparation and analysis strategies are missing different studies can hardly be compared and quantitative data, including identification and mass contents of the polymers found, are missing. This leads to a lack of comprehensive understanding of MP occurrence, source and entry pathways into the environment.
We developed a method, Thermal Extraction/Desorption-Gaschromatography-Massspectrometry, as a fast screening method for MP analysis. Solid residues of water samples are heated up to 600 C under a N2 atmosphere without any sample preparation. The collected decomposition gases are separated in a gas chromatography system and detected in a mass spectrometer. Mass contents of the identified polymers can be calculated.
In this presentation we will show first results from the influent of the wastewater treatment plant Kaiserslautern (Germany) and its combined sewage system as possibly entry pathway. In order to determine the relevance of wastewater split streams analysis of grey water will be conducted. Samples are fractionally filtered by a sieve cascade with mesh sizes of 500, 100, 50 µm.