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For centuries, churches, secular buildings and museums have been furnished with valuable works of art. Many works of art are UV- and light-sensitive. It is well known that especially UV radiation causes damage and discoloration in paintings, textiles, plastics, wood and other materials. In particular, the wavelengths between 280 and 410 nm cause color changes, embrittlement or destruction of e.g. plastics over time. Therefore, strongly UV-absorbing glasses are advantageous for architecture and are necessary for the protection of cultural assets. As restorers in all disciplines become more and more aware, the demands placed on buildings and their furnishings in terms of climate are becoming increasingly detailed and precise. The aim in each case is to preserve the valuable artwork.
For some years now, the industry has been offering the protection of cultural objects by installing special UV-protective glasses. Currently, UV protection for church buildings is realized by laminated safety glass equipped with appropriate UV-protective plastic films. Technically, this always means a second pane of glass in front of the windows, which is installed outside the building. This creates climatic gaps that are difficult to control and deterioration due to ageing effects can be expected. At the same time, this protective glazing is not invisible and has a considerable aesthetic influence on the interior and exterior appearance of the building. Meanwhile, the preservation of historical monuments accepts such aesthetic cuts on buildings in order to protect the artwork in the interior from UV light. To this day, however, the long-term durability of UV protection provided by inserted plastic films is still controversial.
To date the only available alternative on the market is a mouth-blown UV protection glass which uses a so-called overlay to provide UV protection. This shows that UV protection can also be achieved by glasses without plastic films thus realizing an exclusive inorganic protection which normally is more stable than a polymeric one. So far there are not enough studies to prove long-term durability.
The aim of this project is to provide existing glazing or new glazing to be created with a highly transparent layer that ensures this UV-protective filter function below 400 nm. The glass coating is to be applied to the glass over a large area and fired into the surface like a classic ceramic enamel paint with the same technics. In addition, it should be long-term durable in its function. It means, that the glass has to be fused at temperatures below 630 °C during the firing process, its chemical durability has to be high, its coefficient of thermal expansion has to be as close as the one of the substrate (usually float glass) and the glass has to absorb the UV-radiation within a thin thickness (thinner as 100 µm).
In this project, the long-term durability of commercial UV-protective glasses is examined. New low melting glasses containing UV-absorbing ions are being developed. Their UV-absorption as a thin layer is analyzed as well as their chemical durability and their thermal properties.
We are grateful to BMWI for the financial support in the frame of the Central Innovation Programme for SMEs (ZIM).
Non-linear optical emitters are promising materials for energy applications and biotechnologies. Solid-state multi-band emitters like lanthanide doped up-conversion nanoparticles (UCNPs) show excellent photostability, are excitable in the near infrared (NIR), and show emission bands from the UV to SWIR spectral regions. The optical properties of these materials strongly depend on the excitation power density, i.e., the number of photons absorbed per time interval. The upconversion (ΦUC) and downshifting quantum efficiencies (ΦDS) of these materials, the excitation power dependent population, and the deactivation dynamics are influenced by nanoparticle architecture, doping concentration, and the microenvironment. We studied the fundamental changes of the luminescence properties of ß-NaYF4 UCNPs doped with Yb3+ and Er3+ depending on size, different surroundings such as aqueous and organic media, and different surface chemistries. We obtained further insights into shelling procedures, FRET optimization, influence of doping concentration, and advantages of different sensitizer ions.
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.
In this work, two novel donor/acceptor (D/A) complexes, namely, diindenoperylene (DIP)/1,3,4,5,7,8-hexafluoro-tetracyanonaphthoquinodimethane (F6TCNNQ) and alpha-sexithiophene (6T)/F6TCNNQ, are studied. The D/A complexes segregate in form of π−π stacked D/A cocrystals and can be observed by X-ray scattering. The different conformational degrees of freedom of the donor molecules, respectively, seem to affect the thin-film crystalline texture and composition of the D/A mixtures significantly. In equimolar mixtures, for DIP/F6TCNNQ, the crystallites are mostly uniaxially oriented and homogeneous, whereas for 6T/F6TCNNQ, a mostly 3D (isotropic) orientation of the crystallites and coexistence of domains of pristine compounds and D/A complex, respectively, are observed. Using optical absorption spectroscopy, we observe for each of the two mixed systems a set of new, strong transitions located in the near-IR range below the gap of the pristine compounds: such transitions are related to charge-transfer (CT) interactions between donor and acceptor. The optical anisotropy of domains of the D/A complexes with associated new electronic states is studied by ellipsometry. We infer that the
CT-related transition dipole moment is perpendicular to the respective π-conjugated planes in the D/A complex.
Iron-doped SnO2 coatings were deposited in a 50 kHz DC-pulsed magnetron sputtering discharge. The pulses had a duration of 4 µs in selected gas mixtures from pure argon up to
60% of oxygen at a constant total pressure of 0.2 Pa. A single target of SnO2 with Fe inset was used. The mass spectrometry study detected the gas-related ions Ar+, O2+ and O+, where the last one becomes the dominant positive ion at higher oxygen contents. Atomic oxygen ions had a higher energy as it resulted from the collision-caused dissociation on the target surface. The tin-related species were detected as Sn+ and SnO+. SnO2+ species were not detected. The deposition rate decreased by using gas mixtures with oxygen as well as the corresponding amount of Sn-related species in the plasma. The increase of oxygen also increased significantly the sheet resistance of the films. The XPS study showed that the iron concentration decreased by using additional oxygen. But the O/Sn ratio in the coatings was constant, contrary to the increased FeO/Fe ratio in the films. An additional analysis of the coatings by spectroscopic ellipsometry has shown a dependence of the polarizability and the permittivity on the amount of oxygen used during the deposition. In contrast, the study has found no such dependence for the absorption of the layers.
Coatings deposited by magnetron co-sputtering from a single RF magnetron with a ceramic SnO2 target with iron inset in argon plasma were studied. The mass spectra of the process identified Sn+ and SnO+ species as the dominant species sputtered from the target, but no SnO2+ species were detected. The dominant positive ions in argon plasma are Ar+ species. The only detected negative ions were O-. Sputtered neutral tin related species were not detected. Iron related species were also not detected because their concentration is below the detection limit.
The concentration of iron dopant in the tin oxide coatings was controlled by the RF bias applied on the substrate holder while the discharge pressure also has some influence. The iron concentration was in the range from 0.9 at.% up to 19 at.% increasing with the substrate bias while the sheet resistivity decreases. The stoichiometry ratio of O/(Sn + Fe) in the coatings increased from 1.7 up to 2 in dependence on the substrate bias from floating bias (- 5 V) up to - 120 V of RF self-bias, respectively. The tin in the coatings was mainly bonded in Sn4 + state and iron was mainly in Fe2 + state when other tin bonding states were detected only in a small amounts. Iron bonding states in contrary to elemental compositions of the coatings were not influenced by the RF bias applied on the substrate.
The coatings showed high transparency in the visible spectral range. However, an increased metallic behavior could be detected by using a higher RF bias for the deposition. The X-ray diffraction patterns and electron microscopy pictures made on the coatings confirmed the presence of an amorphous phase.
Near-IR femtosecond (fs) (pulse duration = 150 fs, wavelength = 775 nm, repetition
rate 1 kHz) and VUV nanosecond (ns) (pulse duration = 20 ns, wavelength = 157 nm,
repetition rate 1 to 5 Hz) laser pulse ablation of single-crystalline TeO2 (c-TeO2 ) surfaces
was performed in air using the direct focusing technique. A multi-method
characterization using optical microscopy, atomic force microscopy and scanning
electron microscopy revealed the surface morphology of the ablated craters. This allowed
us at each irradiation site to characterize precisely the lateral and vertical dimensions of
the laser-ablated craters for different laser pulse energies and number of laser pulses per
spot. Based on the obtained information, we quantitatively determined the ablation
threshold fluence for the fs laser irradiation when different pulse numbers were applied to
the same spot using two independent extrapolation techniques. We found that in the case
of NIR fs laser pulse irradiation, the ablation threshold significantly depends on the
number of laser pulses applied to the same spot indicating that incubation effects play an
important role in this material. In the case of VUV ns laser pulses, the ablation rate is
significantly higher due to the high photon energy and the predominantly linear
absorption in the material. These results are discussed on the basis of recent models of the
interaction of laser pulses with dielectrics. In the second part of this chapter, we use time-
of-flight mass spectrometry (TOFMS) to analyze the elemental composition of the
ablation products generated upon laser irradiation of c-TeO2 with single fs- (pulse
duration ~200 fs, wavelength 398 nm) and ns-pulses (pulse duration 4 ns, wavelength
355 nm). Due to the three order of magnitude different peak intensities of the ns- and fs
laser pulses, significant differences were observed regarding the laser-induced species in
the plasma plume. Positive singly, doubly and triply charged Te ions (Te+, Te2+, Te3+) in
the form of many different isotopes were observed in case of both irradiations. In the case
of the ns-laser ablation, the TeO+ formation was negligible compared to the fs case and
there was no Te trimer (Te3+) formation observed. It was found that the amplitude of Te
ion signals strongly depends on the applied laser pulse energy. Singly charged oxygen
ions (O+) are always present as a byproduct in both kinds of laser ablation.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of silicon wafer surfaces by linearly polarized Ti:sapphire femtosecond laser pulses (pulse duration 130 fs, central wavelength 800 nm) is studied experimentally and theoretically. In the experiments, so-called low-spatial frequency LIPSS (LSFL) were found with periods smaller than the laser wavelength and an orientation perpendicular to the polarization. The experimental results are analyzed by means of a new theoretical approach, which combines the widely accepted LIPSS theory of Sipe et al. with a Drude model, in order to account for transient (intra-pulse) changes of the optical properties of the irradiated materials. It is found that the LSFL formation is caused by the excitation of surface plasmon polaritons, SPPs, once the initially semiconducting material turns to a metallic state upon formation of a dense free-electron-plasma in the material and the subsequent interference between its electrical field with that of the incident laser beam resulting in a spatially modulated energy deposition at the surface. Moreover, the influence of the laser-excited carrier density and the role of the feedback upon the multi-pulse irradiation and its relation to the excitation of SPP in a grating-like surface structure is discussed.
Prerequisite for the rational design of functional organic materials with tailor-made electronic properties is the knowledge of the structure–property relationship for the specific class of molecules under consideration. This encouraged us to systematically study the influence of the molecular structure and substitution pattern of aromatically substituted 1,3,4-oxadiazoles on the electronic properties and packing motifs of these molecules and on the interplay of these factors. For this purpose, seven diphenyl-oxadiazoles equipped with methyl substituents in the ortho- and meta-position(s) were synthesized and characterized. Absorption and fluorescence spectra in solution served here as tools to monitor substitution-induced changes in the electronic properties of the individual molecules whereas X-ray and optical measurements in the solid state provided information on the interplay of electronic and packing effects. In solution, the spectral position of the absorption maximum, the size of Stokes shift, and the fluorescence quantum yield are considerably affected by ortho-substitution in three or four ortho-positions. This results in blue shifted absorption bands, increased Stokes shifts, and reduced fluorescence quantum yields whereas the spectral position and vibrational structure of the emission bands remain more or less unaffected. In the crystalline state, however, the spectral position and shape of the emission bands display a strong dependence on the molecular structure and/or packing motifs that seem to control the amount of dye–dye-interactions. These observations reveal the limited value of commonly reported absorption and fluorescence measurements in solution for a straightforward comparison of spectroscopic results with single X-ray crystallography. This underlines the importance of solid state spectroscopic studies for a better understanding of the interplay of electronic effects and molecular order.
MgF2 and TiO2 single layers and layer stacks were produced by a spin-coating sol-gel process. The final temperature treatment was carried out at 100 °C. The layers were deposited onto silicon and fused silica substrates and were analysed by means of atomic force microscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, ellipsometry, and UV-vis transmission spectroscopy. MgF2 and TiO2 single layers have morphological and optical properties comparable with physical vapour deposited layers. By using spectroscopic mapping ellipsometry, a good inter- and intra-sample homogeneity was confirmed. Multiple deposition steps result in a linear increase of layer thickness. Various films were deposited with thicknesses between 25 nm and 350 nm.
It was shown that the low temperature sol-gel process results in films of optical quality. Anti-reflective and high reflective layer stacks consisting of MgF2 and TiO2 were designed and can be produced now by a sol-gel process, whereas the MgF2 layers in the layer stacks contains also traces of MgF2-2xOx.