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Reith, F. ; Rea, M.A.D. ; Sawley, P. ; Zammit, C.M. ; Nolze, Gert ; Reith, T. ; Rantanen, K. ; Bissett, A.
(Bio)geochemical cycling of gold (Au) has been demonstrated in present-day (semi)-arid, (sub)-tropical and temperate environment. Hereby biofilms on Au-bearing mineral- and Au-particle surfaces drive Au dispersion and reconcentration, thereby (trans)forming the particles. However, it is unknown if biogeochemical cycling of Au occurs in polar environments, where air temperatures can reach −40 °C and soils remain frozen for much of the year. Therefore, placer Au-particles, soils and waters were collected at two placer mining districts in arctic Finland, i.e., the Ivalojoki and Lemmenjoki goldfields. Sites were chosen based on contrasting settings ((glacio)-fluvial vs. glacial-till deposits) and depths (surface to 5m below current surface). Gold particles were studied using a combination of tagged 16S rRNA gene next generation sequencing and electron microscopic/microanalytical techniques. Across all sites a range of Au-particle morphologies were observed, including morphotypes indicative of Au dissolution and aggregation. Elevated Au concentrations indicative of Au mobility were detected in placer particle bearing soils at both districts. Typically Au-particles were coated by polymorphic biofilm layers composed of living and dead cells embedded in extracellular polymeric substances. Intermixed were biominerals, clays and iron-sulfides/oxides and abundant secondary Au morphotypes, i.e., nano-particles, microcrystals, sheet-like Au, branched Au networks and overgrowths and secondary rims. Biofilms communities were composed of Acidobacteria (18.3%), Bacteroidetes (15.1%) and Proteobacteria (47.1%), with β-Proteobacteria (19.5%) being the most abundant proteobacterial group. Functionally, biofilms were composed of taxa contributing to biofilm establishment, exopolymer production and nutrient cycling, abundant taxa capable of Au mobilization, detoxification and biomineralization, among them Cupriavidus metallidurans, Acinetobacter spp. and Pseudomonas spp., were detected. In conclusion, these results demonstrate that placer Au-particle transformation and Au dispersion occur in cold, arctic environments. This corroborates the existence of biogeochemical Au cycling in present-day cold environments.
Eh Hovsepian, P. ; Ehiasarian, A. P. ; Purandare, Y. P. ; Mayr, P. ; Abstoss, K. G. ; Mosquera Feijoo, Maria ; Schulz, Wencke ; Kranzmann, Axel ; Lasanta, M. I. ; Trujillo, J. P.
To increase efficiency, modern steam plants are pushing their operational regime from super-critical (600 °C/300 bar) to ultra-super-critical (740/760 °C/350 bar) stretching existing turbine materials to their limits. The focus is on new generation functional materials and technologies which complement the inherent properties of existing materials.
Current work proposes a novel High Power Impulse Magnetron Sputtering (HIPIMS) Deposition technology, for the first time, for deposition of a ceramic based CrN/NbN coating with a nanoscale multilayer structure (bi-layer thickness Δ = 1.9 nm) with superior adhesion (LC2 = 80 N) to protect low Chromium P92 steel widely used in steam power plants. Thermodynamic calculations predict the equilibrium phases and aggressive gaseous compounds generated by the interaction of steam with the coating. CrN/NbN coated P92 steel samples oxidised at 600 °C in a high pressure (50 bar) 100% steam atmosphere for up to 1000 h reveal the coating's superior oxidation resistance and protective mechanisms, especially against the detrimental effect of Hydrogen. High temperature (650 °C) Tensile Strength, Low Cycle Fatigue and Creep tests confirm that, unlike other state-of-the-art PVD technologies, HIPIMS is not detrimental to the mechanical properties of the substrate material. Water droplet erosion tests confirm no measurable weight loss after 2.4 X 10⁶ impacts.
Kalinka, Gerhard ; Sahin, M. ; Schlögl, S. ; Wang, J. ; Kaynak, B. ; Mühlbacher, I. ; Ziegler, W. ; Kern, W. ; Grützmacher, H.
The present work provides a comparative study on the interface and adhesion properties of surface modified single glass fibers embedded in an acrylate matrix. To facilitate a covalent bonding at the fibermatrix interface, the fibers are functionalized with selected organosilanes that comprise either passive (unsaturated C¼C bonds of methacrylate moieties) or photoactive functionalities (photocleavable bis(acyl)phosphane oxide groups). Immobilization of the functional silanes is carried out by a classic silanization reaction involving a condensation reaction across the surface hydroxyl groups of the inorganic glass fibers. The change of the physico-chemical properties of the fibers due to desizing and subsequent surface modification is monitored by X-ray photoelectron spectroscopy and zeta potential measurements. In addition, scanning electron microscopy is used to follow the changes in surface morphology. After the modification step, the desized and modified single fibers are embedded in a photocurable acrylate resin formulation. By performing single fiber pull-out tests, maximum pull-out force, friction strength and apparent interfacial shear strength are determined as a function of the coupled silanes. The results reveal that the attached organosilanes lead to a significant increase in adhesion strength, whilst the performance of the photo-cleavable organosilane is superior to the passive methacryl-functional derivative.
Insights into early damage mechanisms during high-temperature gas corrosion provide important aspects for the prediction of the long-term stability of hightemperature materials exposed to a hot and corrosive environment. The current work presents a real time study concerning the combined oxidation and sulfidation of ferritic model alloys in a hot SO2 containing atmosphere using energy dispersive X-ray diffraction. The applied high temperature reactor allows the transmittance of high energetic X-rays in order to collect X-ray diffraction pattern of the sample surface in situ during the reaction with the reactive environment. The results revealed that the first phases crystallizing on iron with 2 wt% chromium and with 9 wt% chromium are oxides. The aging experiments at T = 650° C with 0.5% SO2 and 99.5% Ar were followed in situ and caused an external mixed oxide-sulfide layer on top of iron with 2 wt% chromium. On the higher alloyed material the external scale consists of iron oxides and the inner scale of mixed (Fe,Cr)-oxides and chromium-sulfides. The oxide content continuously increases parallel to an increase of the sulfide amount. Thus, the initially formed (Fe,Cr)-oxides do not have a protective character and support the transport of sulfur through the growing oxide scale.
Comprehensive insights into the early stages of corrosion mechanisms provide fundamental knowledge to further understand and model long time material behaviour. The present work studies the early stages of combined oxidation and sulphidation of ferritic model alloys for time scales up to 250 h at 650 °C to observe the influence of chromium during the corrosion under SO2. Model alloys were used to focus on the reaction of the intended elements: Fe, Cr, S, and O. Pure iron simultaneously forms magnetite and iron sulphide in an early stage of corrosion, covered by a pure oxide layer after 100 h. Iron with 13 wt% Cr shows hematite and mixed Fe-Cr-oxides first, before sulphides nucleate in the inner corrosion zone. With increasing ageing time a magnetite layer is observed below the hematite layer. Quantitative phase fractions of all corrosion products observed were determined from cross section images. Characterization of the Fe13Cr corrosion scale by FIB revealed a highly porous structure in the inner corrosion zone where Cr-rich (Fe, Cr)-sulphides are present, and caused the scale to spall easily.
Morphology and structure of TixOy nanoparticles generated by femtosecond laser ablation in water
(2018)
Donėlienė, J. ; Rudzikas, M. ; Rades, Steffi ; Dörfel, Ilona ; Peplinski, Burkhard ; Sahre, Mario ; Pellegrino, F. ; Maurino, V. ; Ulbikas, J. ; Galdikas, A. ; Hodoroaba, Vasile-Dan
In this work femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated byXRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation.
Kirner, Sabrina V. ; Slachciak, Nadine ; Elert, Anna Maria ; Griepentrog, Michael ; Fischer, Daniel ; Hertwig, Andreas ; Sahre, Mario ; Dörfel, Ilona ; Sturm, Heinz ; Pentzien, Simone ; Koter, Robert ; Spaltmann, Dirk ; Krüger, Jörg ; Bonse, Jörn
Commercial grade-1 titanium samples (Ti, 99.6%) were treated using three alternative methods, (i) femtosecond laser processing, (ii) thermal heat treatment, and (iii) electrochemical anodization, respectively, resulting in the formation of differently conditioned superficial titanium oxide layers. The laser processing (i) was carried out by a Ti:sapphire laser (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz) in a regime of generating laser-induced periodic surface structures (LIPSS). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning setup for the processing of several square-millimeters large surface areas covered homogeneously by these nanostructures. The differently oxidized titanium surfaces were characterized by optical microscopy, micro Raman spectroscopy, variable angle spectroscopic ellipsometry, and instrumented indentation testing. The tribological performance was characterized in the regime of mixed friction by reciprocating sliding tests against a sphere of hardened steel in fully formulated engine oil as lubricant. The specific tribological performance of the differently treated surfaces is discussed with respect to possible physical and chemical mechanisms.
Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C
(2018)
Nofz, Marianne ; Dörfel, Ilona ; Sojref, Regine ; Wollschläger, Nicole ; Mosquera Feijoo, Maria ; Schulz, Wencke ; Kranzmann, Axel
Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far.
Interdiffusion in the Face-Centered Cubic Phase of the Co-Al-W-Ta System Between 1090 and 1240 °C
(2018)
Epishin, A. ; Chyrkin, A. ; Nolze, Gert ; Midtlyng, Jan ; Mayer, H. M. ; Petrushin, N. ; Reimers, W.
Interdiffusion of Al, W, Ta and Co in a Co-base alloy at temperatures between 1090 and 1240 °C has been investigated. The interdiffusion coefficients were found to be close to those reported for these elements in Ni-base alloys. Combining the diffusion simulation software DICTRA with the Ni-base diffusion databases TCNi5 and MobNi3, the interdiffusion profiles of Co, Al W, and Ta were modeled for Co9Al8W2Ta/Co diffusion couples annealed at different temperatures and for different times. The results show that interdiffusion in the Co-Al-W-Ta alloys can be modeled reasonably well using the available commercial databases for thermodynamics and kinetics of Ni-base systems.
A glass of the composition 37BaO·16CaO·47SiO2 wt% produced on an industrial scale is crystallized at 970 °C for times ranging from 15 min to 2 h. The crystallization at the immediate surface as well as the crystal growth into the bulk are analyzed using scanning electron microscopy (SEM) including energy dispersive X-ray spectroscopy (EDXS) and electron backscatter diffraction (EBSD) as well as X-ray diffraction in the Θ–2Θ setup (XRD). The immediate surface shows the oriented nucleation of walstromite as well as the formation of wollastonite and an unknown phase of the composition BaCaSi3O8. All three phases also grow into the bulk where walstromite ultimately dominates the kinetic selection and grows throughout the bulk due to a lack of bulk nucleation. Walstromite shows systematic orientation changes as well as twinning during growth. A critical analysis of the XRD-patterns acquired from various crystallized samples indicates that their evaluation is problematic and that phases detected by XRD in this system should be verified by another method such as EDXS.