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Glass-ceramics are noted for their unusual combination of properties and manifold commercialized products for consumer and specialized markets. Evolution of novel glass and ceramic processing routes, a plethora of new compositions, and unique exotic nano- and microstructures over the past 60 years led us to review the Definition of glass-ceramics. Well-established and emerging processing methods, such as co-firing, additive manufacturing, and laser patterning are analyzed concerning the core requirements of processing glass-ceramics and the Performance of the final products. In this communication, we propose a revised, updated definition of glass-ceramics, which reads “Glass-ceramics are inorganic, non-metallic materials prepared by controlled crystallization of glasses via different processing methods. They contain at least one type of functional crystalline phase and a residual glass. The volume fraction crystallized may vary from ppm to almost 100%”.
Die Mikro- und Nanotechnologie gehört zu den Schlüsseltechnologien des 21. Jahrhunderts mit hohen Wachstumsprognosen, wie auch die im Auftrag des BMBF durchgeführte Studie “Nanotechnologie als wirtschaftlicher Wachstumsmarkt” von 2004 ausführlich darstellt. Aus diesem Trend resultiert ein steigender Bedarf an Messsystemen, die Nanostrukturen prozessnah bzw. im Fertigungsprozess charakterisieren können. Virtuelle Messgeräte liefern Erkenntnisse zur Entwicklung neuartiger Messsysteme, Analyse und Optimierung bestehender Verfahren sowie die Bestimmung der Messunsicherheit und modellbasierten Korrektur systematischer Fehler. Der virtuelle Messprozess umfasst neben dem Messmittel auch die Probe und die Wechselwirkungen zwischen beiden. In diesem Beitrag werden virtuelle Messgeräte vorgestellt sowie deren Anwendung diskutiert.
The inhalationof smoke gases is awell-established cause of poisoning and leads to the death of fire victims. Carbonmonoxide(CO) and Hydrogen cyanide (HCN) are two of the main noxious gases,whereby HCN is formed by an incomplete combustion of materials containing nitrogen. These materials may be natural materials, such as wool, silk and feathers or synthetic plastics, such as polyacrylonitrile (PAN), polyamide and polyurethane. These materials are very common in modern household furnishings; therefore, notonlyCObutalsoHCN can be produced during home fires. Up tonowonly a fewstudieshave been carried out on the generation of HCN as the fire proceeds, e. g. by Crewe et al. The data from such analyses are useful for forensic purposes. This enables the possibility to more accurately assess the events at the fire location, the Situation in which the fire victims are found as well as the cause of death. One way to analyze the gas composition of smoke is to perform bench scale fire tests, where various fire scenarios can be simulated on a smaller scale (e. g. using a smoke density chamber). The results from such experiments were compared with the results obtained in an enclosed room fire test.
Laser-induced periodic surface structures (LIPSS) were generated on two types of steel (100Cr6, X30CrMoN15-1) and two types of titanium (Ti, Ti6A14V) surfaces upon irradiation with multiple linear polarized femtosecond laser pulses in air environment (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz, Gaussian beam shape). Teh conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning geometry for the processing of large surface areas covered homogeneously by two different types of LIPSS - either near wavelength or sub-100 nm structures. The tribological performance of the nanostructured surfaces was characterized under reciprocating sliding at 1 Hz against a ball of hardened steel using different lubricants and normal forces. After 1000 cycles the corresponding wear tracks were characterized by optical and scanning electron microscopy. For specific conditions, the wear was strongly reduced and laser-generated nanostructures endured the tribological treatment. Simultaneously, a significant reduction of the friction coefficient was observed in the laser-irradiated LIPSS-covered areas, indicating the benefit of laser surface structuring for tribological applications. The spatially Gaussian shaped beam used for the laser processing was transformed via beam shaping into a top hat distribution at the surface of the samples for optimization. The tribological performance of the laser-induced nanostructures is discussed on the basis of different physical and chemical mechanisms.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences consisting of five Ti:sapphire femtosecond (fs) laser pulse pairs (150 fs, 800 nm) is studied experimentally. A Michelson interferometer is used to generate near-equal-energy double-pulse sequences with a temporal pulse delay from -20 to +20 ps between the cross-polarized individual fs-laser pulses (~0.2 ps resolution). The results of multiple double-pulse irradiation sequences are characterized by means of Scanning Electron and Scanning Force Microscopy. Specifically in the sub-ps delay domain striking differences in the surface morphologies can be observed, indicating the importance of the laser-induced free-electron plasma in the conduction band of the solids for the formation of LIPSS.
Pulmonary surfactant contains two extremely hydrophobic proteins, SP-B and SP-C. We present a novel HPLC method for the preparation of these hydrophobic proteins. It is based on size-exclusion chromatography using the apolar stationary-phase butyl silica gel and isocratic elution with acidified chloroform/methanol. Samples for HPLC were prepared from sheep lung lavage fluid by centrifugation and extraction with chloroform/methanol. Amino acid analyses of the two protein fractions revealed sequences that are consistent with SP-B and SP-C, respectively. MALDI-TOF-MS analyses of the SP-B fraction showed one major peak of dimeric SP-B with m/z 17,361, and additional peaks of monomeric and oligomeric forms, which are predominantly even numbered. The SP-C fraction showed a peak at m/z 4200, consistent with the theoretical mass of the dipalmitoylated form of this protein. The biophysical activity of pure sheep SP-B and SP-C was evaluated by measuring the surface tension using axisymmetric drop shape analysis for captive bubbles. We found distinct surface pressure versus surface area isotherms of SP-B and SP-C indicating different biophysical activities for these surfactant proteins. The new preparative HPLC method is able to replace the established, time-consuming low-pressure liquid chromatography method for the isolation of SP-B and SP-C from lipids.
Poly(ether-sulfone)s having an identical backbone were prepared by four different methods. First, silylated bisphenol A (BSBA) was polycondensed with 4,4'-difluorodiphenyl sulfone (DFDPS) and K2CO3 in N-methylpyrrolidone with variation of the temperature. Second, analogous polycondensation were conducted using CsF as catalyst (and no K2CO3). Third, CsF-catalyzed polycondensations BSBA and DFDPS were conducted in bulk up to 290 C. Fourth, free bisphenol was polycondensed with DFDPS or 4,4'-dichlorodiphenyl sulfone and K2CO3 in DMSO with azeotropic removal of water. MALDI-TOF mass spectroscopy revealed that the first method mainly yielded cyclic poly(ether-sulfone)s which were detected up to masses around 13 000 Da. These and other results suggest that these polycondensations take a kinetically kontrolled course at tempeatures 145 C. This interpretation is also valid for the fourth method where high yields of cycles were obtained with DFDPS. With the less reactive 4,4'-dichlorodiphenyl sulfone lower conversions, lower molecular weights and lower fractions of cycles were found. In contrast to KF (resulting from K2CO3) CsF cleaves the poly(ether sulfone) backbone at temperatures > 145 C. Smaller amounts of smaller cycles were found in these CsF-catalyzed polycondensations which were in this case the result of thermodynamically controlled "back-biting degradation".
Various dibutyltin derivatives were polycondensed with aliphatic ,-dicarboxylic acids having chain lengths from 4 (succinic acid) to 22 carbon atoms. White crystalline products were obtained from all experiments, and the structure of the products was independent of the synthetic method. Viscosity measurements revealed low molecular weights (n 1 500 Da) in all cases. Vapor pressure osmometry (VPO) measurements and matrix-assisted laser desorption time-of-flight (MALDI-TOF) mass spectrometry proved that cyclic dimers and trimer were formed from dicarboxylic acids having 6 to 16 carbons, but mainly the monomeric cycle from docosane dioic acid. Heating to 250°C did not change the structure. Therefore, the results indicate that the macrocycles are the result of a thermodynamically controlled ring-closing polycondensation. This means that linear high-molecular weight poly(dibutyltin dicarboxylate)s cannot exist above room temperature.
Various dibutyltin derivatives were polycondensed with aliphatic ,-dicarboxylic acids having chain lengths from 4 (succinic acid) to 22 carbon atoms. White crystalline products were obtained from all experiments, and the structure of the products was independent of the synthetic method. Viscosity measurements revealed low molecular weights (n 1 500 Da) in all cases. Vapor pressure osmometry (VPO) measurements and matrix-assisted laser desorption time-of-flight (MALDI-TOF) mass spectrometry proved that cyclic dimers and trimer were formed from dicarboxylic acids having 6 to 16 carbons, but mainly the monomeric cycle from docosane dioic acid. Heating to 250°C did not change the structure. Therefore, the results indicate that the macrocycles are the result of a thermodynamically controlled ring-closing polycondensation. This means that linear high-molecular weight poly(dibutyltin dicarboxylate)s cannot exist above room temperature.
Three new aromatic polyazomethines have been synthesized by solution polycondensation reactions of terephthalic dialdehyde with fluorine containing aromatic diamines. The polymers were obtained in high yields. The investigation of these polymers by means of matrix-assisted laser desorption ionizationtime-of-flightmass spectrometry (MALDITOFMS) proved the initial members of the four theoretical possible series of the corresponding oligomers with 210 repeating units per molecule.
The role of 1,1-diphenylethylene (DPE) in radical emulsion polymerization of methyl methacrylate is investigated. The presence of DPE causes a strong decrease in both the rate of polymerization and the molecular weight. According to the results of structure analysis by means of MALDI-TOF mass spectrometry, UVvis spectroscopy, and 1HNMR spectroscopy, DPE is incorporated in the copolymer chain exclusively as a reactive recombinant ?,p-dimer, underlining the peculiar role of DPE in radical polymerizations.
Hydrolytic condensation of different methacrylate groups containing alkoxy silanes yielded resins which showed interesting properties as a matrix for dental composites. For this purpose, resins of low viscosity are desired resulting in composites with a high amount of inorganic fillers. Our investigations demonstrated that the viscosity of the obtained polycondensates was predominantly influenced by the kind of organic spacer between the methacrylate group and the silicon atom. In addition, the viscosity also significantly changed in dependence of the kind of structure units built. NMR spectroscopic investigations as well as size exclusion chromatography (SEC) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry showed that the formed structures depended both on the kind of catalyst used for hydrolysis/condensation and the bulkiness of the organic substituent at the silicon atom.
Structuring of dielectric and metallic materials with ultrashort laser pulses between 20 fs and 3 ps
(1997)
Laser-micromachining of barium aluminum borosilicate glass, fused silica and stainless steel has been extended down to a pulse duration of 20 fs generated by a Ti:sapphire laser system at a wavelength of 0.8 micrometer. A systematic study shows that, below 100 fs, an enhanced precision and a substantial decrease of the ablation threshold fluence in comparison to pulse laser processing with pulses in the picosecond and nanosecond range could be achieved. The physical mechanism and the technical relevance of this novel microtechnology is discussed.
A femtosecond pulse laser in the visible spectral region shows promise as a potentially new powerful corneal sculpting tool. It combines the clinical and technical advantages of visible wavelengths with the high ablation quality observed with nanosecond-pulse excimer lasers at 193 nm. A femtosecond and a nanosecond dye laser with pulse durations of 300 fs and 7 ns, and centre wavelengths at 615 nm and 600 nm, respectively, both focused to an area of the order of 105 cm2, have been applied to human corneal ablation. Nanosecond laser pulses caused substantial tissue disruption within a 30100 m range from the excision edge at all fluences above the ablation threshold of F th60 J cm2 (I th9 GW cm2). Completely different excisions are produced by the femtosecond-pulse laser: high quality ablations of the Bowman membrane and the stroma tissue characterised by damage zones of less than 0.5 m were observed at all fluences above ablation threshold of F th1 J cm2 or I th3 TW cm2 (3×1012 W cm2). The transparent cornea material can be forced to absorb ultrashort pulses of extremely high intensity. The fs laser generates its own absorption by a multiphoton absorption process.
Numerous polycondensations of isosorbide and suberoyl chloride or other aliphatic dicarboxylic acid dichlorides were performed with pyridine as a catalyst and HCl acceptor. The reaction conditions were varied to optimize both the molecular weight and the fraction of cyclic oligo- and polyesters. Furthermore, we attempted to obtain the cyclic monomer by catalyzed back-biting degradation of the molten cyclic polyesters above 220 °C in vacuo. The polyesters were characterized by viscosity and size exclusion chromatographic measurements as well as matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. In selected cases, mixtures of linear and cyclic polyesters were treated with a hot solution of partially methylated ß-cyclodextrin in methanol. This treatment allowed for a selective extraction of the linear chains up to approximately 5000 Da.
The formation of laser-induced periodic surface structures (LIPSS) in different materials (metals, semiconductors, and dielectrics) upon irradiation with linearly polarized fs-laser pulses (τ~30–150 fs, λ~800 nm) in air environment is studied experimentally and theoretically. In metals, predominantly low-spatial-frequency-LIPSS with periods close to the laser wavelength λ are observed perpendicular to the polarization. Under specific irradiation conditions, high-spatial-frequency-LIPSS with sub-100-nm spatial periods (~λ/10) can be generated. For semiconductors, the impact of transient changes of the optical properties to the LIPSS periods is analyzed theoretically and experimentally. In dielectrics, the importance of transient excitation stages in the LIPSS formation is demonstrated experimentally using (multiple) double-fs-laser-pulse irradiation sequences. A characteristic decrease of the LIPSS periods is observed for double-pulse delays of less than 2 ps.
The formation of laser-induced periodic surface structures (LIPSS) on two different silica polymorphs (single-crystalline synthetic quartz and commercial fused silica glass) upon irradiation in air with multiple linearly polarized single- and double-fs-laser pulse sequences (τ = 150 fs pulse duration, λ = 800nm center wavelength, temporal pulse separation Δt < 40 ps) is studied experimentally and theoretically. Two distinct types of fs-LIPSS [so-called low-spatial-frequency LIPSS (LSFL) and high-spatial-frequency LIPSS (HSFL)] with different spatial periods and orientations were identified. Their appearance was characterized with respect to the experimental parameters peak laser fluence and number of laser pulses per spot. Additionally, the 'dynamics' of the LIPSS formation was addressed in complementary double-fs-pulse experiments with varying delays, revealing a characteristic change of the LSFL periods. The experimental results are interpreted on the basis of a Sipe-Drude model considering the carrier dependence of the optical properties of fs-laser excited silica. This new approach provides an explanation of the LSFL orientation parallel to the laser beam polarisation in silica—as opposed to the behaviour of most other materials.
The formation of laser-induced periodic surface structures upon irradiation of titanium, silicon, and fused silica with multiple irradiation sequences consisting of parallel polarized Ti:sapphire femtosecond laser pulse pairs (pulse duration 50–150 fs, central wavelength ~800 nm) is studied experimentally. The temporal delay between the individual near-equal energy fs-laser pulses was varied between 0 and 5 ps with a temporal resolution of better than 0.2 ps. The surface morphology of the irradiated surface areas is characterized by means of scanning electron microscopy (SEM). In all materials a decrease of the rippled surface area is observed for increasing delays. The characteristic delay decay scale is quantified and related to material dependent excitation and energy relaxation processes.
Femtosecond diffraction dynamics of laser-induced periodic surface structures on fused silica
(2013)
The formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration, 800?nm center wavelength) is studied experimentally using a transillumination femtosecond time-resolved (0.1 ps-1 ns) pump-probe diffraction approach. This allows to reveal the generation dynamics of near-wavelength-sized LIPSS showing a transient diffraction at specific spatial frequencies even before a corresponding permanent surface relief was observed. The results confirm that the ultrafast energy deposition to the materials surface plays a key role and triggers subsequent physical mechanisms such as carrier scattering into self-trapped excitons.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences of parallel polarized Ti:sapphire femtosecond laser pulse pairs (160 fs pulse duration, 800 nm central wavelength) was studied experimentally. For that purpose, a Michelson interferometer was used to generate near-equal-energy double-pulse sequences allowing the temporal pulse delay between the parallel-polarized individual fs-laser pulses to be varied between 0 and 40 ps with ~0.2 ps temporal resolution. The surface morphologies of the irradiated surface areas were characterized by means of scanning electron and scanning force microscopy. In the sub-ps delay range a strong decrease of the LIPSS periods and the ablation crater depths with the double-pulse delay was observed indicating the importance of the laser-induced free-electron plasma in the conduction band of the solids for the formation of LIPSS.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica and silicon with multiple (NDPS) irradiation sequences consisting of linearly polarized femtosecond laser pulse pairs (pulse duration ~150 fs, central wavelength ~800 nm) is studied experimentally. Nearly equal-energy double-pulse sequences are generated allowing the temporal pulse delay Δt between the cross-polarized individual fs-laser pulses to be varied from -40 ps to +40 ps with a resolution of ~0.2 ps. The surface morphologies of the irradiated surface areas are characterized by means of scanning electron and scanning force microscopy. Particularly for dielectrics in the sub-ps delay range striking differences in the orientation and spatial characteristics of the LIPSS can be observed. For fused silica, a significant decrease of the LIPSS spatial periods from ~790 nm towards ~550 nm is demonstrated for delay changes of less than ~2 ps. In contrast, for silicon under similar irradiation conditions, the LIPSS periods remain constant (~760 nm) for delays up to 40 ps. The results prove the impact of laser-induced electrons in the conduction band of the solid and associated transient changes of the optical properties on fs-LIPSS formation.
The formation of laser-induced periodic surface structures (LIPSS) on titanium upon irradiation with linearly polarized femtosecond (fs) laser pulses (τ = 30 fs, λ = 790 nm) in an air environment is studied experimentally and theoretically. In the experiments, the dependence on the laser fluence and the number of laser pulses per irradiation spot has been analyzed. For a moderate number of laser pulses (N < 1000) and at fluences between ~0.09 and ~0.35 J/cm², predominantly low-spatial-frequency-LIPSS with periods between 400 nm and 800 nm are observed perpendicular to the polarization. In a narrow fluence range between 0.05 and 0.09 J/cm², high-spatial-frequency-LIPSS with sub-100-nm spatial periods (~λ/10) can be generated with an orientation parallel to the polarization (N = 50). These experimental results are complemented by calculations based on a theoretical LIPSS model and compared to the present literature.
In this paper, safety-related experiments with ultra-short laser pulses (down to 30 fs) on various components
(goggles, curtains) for laser protection are presented. The damage and failure behaviour of
protective devices has been investigated dependent on practical conditions such as pulse duration, laser
.uence, pulse number, and repetition rate.
The e.ects of laser-irradiation on materials can be roughly divided into transient ones like laserinduced
transmission (LIT) or short-lived colour centres and permanent damages like the stable colour
centres and ablation. The former e.ects are particularly important for transparent devices like laser
goggles.
To obtain a complete overview on laser safety issues and the prevention of failure there are two
important .elds of investigation:
1. the e.ects of laser radiation on human eyes and skin, and
2. on the possible protection materials.
Both .elds have been addressed during the recently .nished German project SAFEST (safety aspects
in femtosecond technology). The amount of safety data available in the ultrashort pulse region has
been increased remarkably. This allows for a re-evaluation of known laser protection materials for this
region of pulse durations and for the evaluation of new designs that promise high protection levels
while being light-weight and convenient to use.
We report measurements of the optical breakdown threshold and ablation depth in dielectrics with different band gaps for laser pulse durations ranging from 5 ps to 5 fs at a carrier wavelength of 780 nm. For tau <100 fs, the dominant channel for free electron generation is found to be either impact or multiphoton ionization (MPI) depending on the size of the band gap. The observed MPI rates are substantially lower than those predicted by the Keldysh theory. We demonstrate that sub-10-fs laser pulses open up the way to reversible nonperturbative nonlinear optics (at intensities greater than 1014 W/cm2 slightly below damage threshold) and to nanometer-precision laser ablation (slightly above threshold) in dielectric materials.
Results of a round-robin experiment in multiple-pulse LIDT measurement with ultrashort pulses
(2004)
The formation of near-wavelength laser-induced periodic surface structures (LIPSS) on silicon upon irradiation with sequences of Ti:sapphire femtosecond laser pulse pairs (pulse duration 150 fs, central wavelength 800 nm) is studied theoretically. For this purpose, the nonlinear generation of conduction band electrons in silicon and their relaxation is numerically calculated using a two-temperature model approach including intrapulse changes of optical properties, transport, diffusion and recombination effects. Following the idea that surface plasmon polaritons (SPP) can be excited when the material turns from semiconducting to metallic state, the 'SPP active area' is calculated as function of fluence and double-pulse delay up to several picoseconds and compared to the experimentally observed rippled surface areas. Evidence is presented that multi-photon absorption explains the large increase of the rippled area for temporally overlapping pulses. For longer double-pulse delays, relevant relaxation processes are identified. The results demonstrate that femtosecond LIPSS on silicon are caused by the excitation of SPP and can be controlled by temporal pulse shaping.
Worldwide, abandoned coal mines release substantial amounts of methane, which is largely of biogenic origin. The aim of this study was to understand the microbial processes involved in mine-gas formation. Therefore, coal and timber samples and anaerobic enrichments from two abandoned coal mines in Germany were subjected to DGGE analyses and quantitative PCR. The primers used were specific for Bacteria, Archaea, Fungi, and the key functional genes for sulfate reduction (dsrA) and methanogenesis (mcrA). A broad spectrum of facultative anaerobic bacteria and acetogens belonging to all five groups (α-ε) of the Proteobacteria, as well as the Bacteroidetes, Tenericutes, Actinobacteria, Chlorobi and Chloroflexi were detected. Archaea were represented by acetoclastic Methanosarcinales and Crenarchaeota with an unknown metabolism. Fungi formed thick biofilms particularly on timber, and were identified as typical wood degraders belonging to the Ascomycetes and Basidiomycetes. The community analysis as well as the environmental conditions and the metabolites detected in a previous study are consistent with the following scenario of methane release: Weathering of coal and timber is initiated by wood-degrading Fungi and Bacteria under a suboxic atmosphere. In the lower, oxygen-depleted layers Fungi and Bacteria perform incomplete oxidation and release reduced substrates which can be channeled into methanogenesis. Acetate appeared to be the main precursor of the biogenic methane in the investigated coal mines.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences consisting of laser pulse pairs (50 fs single-pulse duration) of two different wavelengths (400 and 800 nm) is studied experimentally. Parallel polarized double-pulse sequences with a variable delay Δt between -10 and +10 ps and between the individual fs-laser pulses were used to investigate the LIPSS periods versus Δt. These two-color experiments reveal the importance of the ultrafast energy deposition to the silica surface by the first laser pulse for LIPSS formation. The second laser pulse subsequently reinforces the previously seeded spatial LIPSS frequencies.
Scrap tyres are widely reused in the form of granules as infill materials or component of sub-base layers in construction of sporting grounds such as synthetic turf areas and athletic track surfaces. The recycled rubber may contain organic and inorganic pollutants due to the presence of vulcanisation catalysts, stabilisers and other additives which can be released into soil and groundwater in the case of outdoor sports facilities. In order to evaluate the amount of potentially mobile pollutants, leaching tests can be employed. This study aimed particularly at the investigation of the feasibility of column tests using complete synthetic surface flooring or turf system assemblies. The release of zinc and polycyclic aromatic hydrocarbons (PAH) leached from components of sports surfaces containing recycled rubber granules was considered. Additionally, batch tests on coated and uncoated styrene butadiene rubber (SBR) granules aged by artificial weathering were performed to indicate its possible influence on the leaching behaviour of zinc and PAH. The chosen approach of column tests simulating typical complete synthetic sports surface installations has been proven to be feasible and robust. The time-dependent leaching behaviour and interactions between single components can be evaluated by column tests. Zinc was the most relevant contaminant in the eluates and its leachability was enhanced after accelerated ageing by artificial weathering. Leachable PAH were found in relatively low but well detectable amounts which increase by ageing as well.
Für die vom Bundesumweltministerium vorgesehene Mantelverordnung sind validierte Unter-suchungsmethoden erforderlich. Dazu gehört auch die Herstellung von wässrigen Eluaten, z.B. zur Beurteilung der Mobilität von Schadstoffen und der Ableitung von Grenzwerten.
Ziel des Vorhabens war es, auf der Grundlage geeigneter Testmaterialien (mit prioritären organischen Schadstoffen kontaminierte Böden und Bodenmaterialien) Ringversuche zur Validierung des Schüttelverfahrens nach E DIN 19527 und des Säulenverfahrens für die Übereinstimmungs-untersuchung nach DIN 19528 durchzuführen. Auf der Grundlage der Untersuchungsergebnisse sollten beide Normen bezüglich der Vorgehensweise präzisiert werden und es sollten die während des Ringversuchs ermittelten Verfahrenskenndatenn zur Validierung der Normen herangezogen werden. Darüber hinaus sollten Säulen- und Schüttelverfahren als Übereinstimmungstest vergleichend bewertet werden.
Es wurden vier geeignete Ringversuchsmaterialien hergestellt und an insgesamt 18 Ringversuchsteilnehmer ausgegeben. Die Auswertung der Ringversuche erfolgte auf der Grundlage klassischer Statistik nach DIN ISO 5725 mit Hilfe der AuswertesoftwareProLab 2011 (quo data).
Auf der Grundlage der Validierungsringversuche wurden die Verfahrenskenndaten für die Norm DIN 19527 ermittelt. Die statistische Auswertung der eingereichten Datensätze war aufgrund der großen Streubreite der Daten schwierig. Die vorgeschriebenen statistischen Methoden zur Datenauswertung adressieren die Behandlung nicht gleichverteilter Datensätze nur ungenügend. Das muss bei der Bewertung der Ergebnisse und deren Zuverlässigkeit berücksichtigt werden.
Generell kann festgestellt werden, dass keine signifikanten Unterschiede zwischen den Ergebnissen der Schüttel- und Säulenelution beobachtet werden. Dabei werden beim Schüttelverfahren tendenziell etwas geringere Gesamtmittelwerte erzielt als beim Säulenverfahren, die berechneten Vergleichsvariationskoeffizienten sind für das Schüttelverfahren meist etwas niedriger. Dennoch erweisen sich beide Elutionsverfahren bei den eingesetzten Ringversuchsmaterialien als gut vergleichbar.
Extensive research is being conducted on magnesium (Mg) alloys for bone implant manufacturing, due to their biocompatibility, biodegradability and mechanical properties. Gadolinium (Gd) is among the most promising alloying elements for property control in Mg alloy implants; however, its toxicity is contro- versial. Investigating Gd behavior during implant corrosion is thus of utmost importance. In this study, we analyzed the degradation byproducts at the implant site of biodegradable Mg-5Gd and Mg-10Gd implants after 12 weeks healing time, using a combination of different imaging techniques: histology, energy-dispersive x-ray spectroscopy (EDX), x-ray microcomputed tomography (μCT) and neutron μCT. The main finding has been that, at the healing time in exam, the corrosion appears to have involved only the Mg component, which has been substituted by calcium and phosphorus, while the Gd remains localized at the implant site. This was observed in 2D by means of EDX maps and extended to 3D with a novel application of neutron tomography. X-ray fluorescence analysis of the main excretory organs also did not reveal any measurable accumulation of Gd, further reinforcing the conclusion that very limited or no removal at all of Gd-alloy happened during degradation.
The current state in the field of laser-induced periodic surface structures (LIPSS, ripples) is reviewed. Their formation mechanisms are analyzed in ultrafast experiments (time-resolved diffraction and polarization controlled double-pulse experiments) and technological applications are demonstrated.
Polycyclic aromatic hydrocarbons (PAH) are severe environmental pollutants that are analyzed frequently. The risk assessment of PAH impact to groundwater can be performed using leaching tests. Therby a liquidsolid separation step including centrifugation may be required, which in turn might lead to loss of analytes due to sorption on the equipment. Thus we determined the PAH recoveries from various container materials (polyethylene (PE), polypropylene (PP), polytetraflourethylene (PTFE), stainless steel (ES), and perflouroalkoxy (PFA)) and compared them to selected PAH properties. We found the best recoveries for PFA (68%) and PTFE (65%) containers. We found good negative correlations (-0.93 and better) between PAH recovery and log partition coefficient organic carbonwater (log KOC) for PFA, PTFE, and ES containers.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of silicon by multiple (N = 100) linearly polarized Ti:sapphire femtosecond laser pulses (duration τ = 30 fs, center wavelength λ0 ~ 790 nm) is studied experimentally in air and water environment. The LIPSS surface morphologies are characterized by scanning electron microscopy and their spatial periods are quantified by two-dimensional Fourier analyses. It is demonstrated that the irradiation environment significantly influences the periodicity of the LIPSS. In air, so-called low-spatial frequency LIPSS (LSFL) were found with periods somewhat smaller than the laser wavelength (ΛLSFL ~ 0.7 × λ0) and an orientation perpendicular to the laser polarization. In contrast, for laser processing in water a reduced ablation threshold and LIPSS with approximately five times smaller periods ΛLIPSS ~ 0.15 × λ0 were observed in the same direction as in air. The results are discussed within the frame of recent LIPSS theories and complemented by a thin film based surface plasmon polariton model, which successfully describes the tremendously reduced LIPSS periods in water.