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The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits.
Glass-ceramics containing Ca2KNa(PO4)2 as the main crystalline phase have a solubility which is 8 times higher than that of alpha-tricalcium phosphate ceramics. When using these compositions in drug delivery systems, especially in bone, it is necessary to create a material with a high open porosity. A Ca2KNa(PO4)2-based glass-ceramic was prepared from a borosilicate glass melt. The processed material includes minor amounts of boron which are low enough for medical application. Tissue response was studied using an animal model. Particles were implanted in rabbit femurs. Bone and soft tissue development occurred at the particle interfaces. In general, most particles were enclosed in the network of trabecular bone. The advantages of using a biomaterial with high porosity (pore size of 1-3 micron), together with rapid biodegradation, bioactivity and biocompatibility, despite traces of boron, were shown. 4 refs.
In vivo test of a high porous rapidly resorbable dicalcium potassium sodium phosphate glass-ceramics
(2002)
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
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.
The formation and properties of laser-induced periodic surface structures (LIPSS) were investigated on carbon fibers under irradiation of fs-laser pulses characterized by a pulse duration τ = 300 fs and a laser wavelength λ = 1025 nm. The LIPSS were fabricated in an air environment at normal incidence with different values of the laser peak fluence and number of pulses per spot. The morphology of the generated structures was characterized by using scanning electron microscopy, atomic force microscopy and Fast-Fourier transform analyses. Moreover, the material structure and the surface chemistry of the carbon fibers before and after laser irradiation was analyzed by micro Raman spectroscopy and X-ray photoelectron spectroscopy. Large areas in the cm2 range of carbon fiber arrangements were successfully processed with homogenously distributed high- and low-spatial frequency LIPSS. Beyond those distinct nanostructures, hybrid structures were realized for the very first time by a superposition of both types of LIPSS in a two-step process. The findings facilitate the fabrication of tailored LIPSS-based surface structures on carbon fibers that could be of particular interest for e.g. fiber reinforced polymers and concretes.
Dynamic stall often occurs under conditions of simultaneous unsteady pitching and surging (e.g., rotorcraft and wind turbines), butmanymodels employ a dimensionless time base that implicitly assumes that surging is superimposed, in a quasi-steady manner, on dynamic pitching. An unsteady wind tunnel was used to examine this assumption, where a technique was developed to quantify the unsteady effects of surging on a pitching NACA 0018 airfoil. The technique involved performing multiple harmonic pitching experiments under nominally steady freestream conditions that bracketed a corresponding 50% surging amplitude (1.25 ⋅ 105 ≤ Re ≤ 3.75 ⋅ 105). By interpolating these data, unsteady-pitching/quasi-steady-surging data sets were constructed and compared with de facto synchronous pitch and surging experiments, thereby isolating the unsteady effects of surging on a pitching airfoil. Both large and small poststall maximum angles of attack (αs + 5° and αs + 15°) were considered at multiple pitch-surge phase differences. During deep dynamic stall (αs 15°), with large-scale separation, surging was seen to have a secondary effect on the unsteady aerodynamics. However, at small poststall maximum angles of attack (αs + 5°), either light or deep dynamic stall behavior was observed depending upon the pitch-surge phase difference. This was attributed to Reynolds number history effects, exemplified by boundary-layer transition, and thus it can be referred to as “transitional” dynamic stall.
A combined theoretical and experimental investigation was carried out with the objective of evaluating theoretical predictions relating to a two-dimensional airfoil subjected to high amplitude harmonic oscillation of the free stream at constant angle of attack. Current theoretical approaches were reviewed and extended for the purposes of quantifying the bound, unsteady vortex sheet strength along the airfoil chord. This resulted in a closed form solution that is valid for arbitrary reduced frequencies and amplitudes. In the experiments, the bound, unsteady vortex strength of a symmetric 18 % thick airfoil at low angles of attack was measured in a dedicated unsteady wind tunnel at maximum reduced frequencies of 0.1 and at velocity oscillations less than or equal to 50 %. With the boundary layer tripped near the leading edge and mid-chord, the phase and amplitude variations of the lift coefficient corresponded reasonably well with the theory. Near the maximum lift coefficient overshoot, the data exhibited an additional high-frequency oscillation. Comparisons of the measured and predicted vortex sheet indicated the existence of a recirculation bubble upstream of the trailing edge which sheds into the wake and modifies the Kutta condition.
Without boundary layer tripping, a mid-chord bubble is present that strengthens during flow deceleration and its shedding produces a dramatically different effect.
Instead of a lift coefficient overshoot, as per the theory, the data exhibit a significant undershoot. This undershoot is also accompanied by high-frequency oscillations that are characterized by the bubble shedding. In summary, the location of bubble and ist subsequent shedding play decisive roles in the resulting temporal aerodynamic loads.
The impact of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on tribological properties was investigated for metal-reinforced ceramic composites (Al2O3-ZrO2-Nb). For this purpose, the metallic niobium (Nb) phase was selectively structured with LIPSS in an air environment with different values of the fs-laser peak fluence by near-infrared fs-laser radiation (λ = 1025 nm, τ = 300 fs, frep = 1 kHz), taking advantage of the different light absorption behavior of ceramic and metal. The tribological performance was evaluated by reciprocating sliding tests in a ball-on-disc configuration using Ringer's solution as lubricant. The surfaces were characterized before and after laser irradiation by optical microscopy, scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, energy dispersive X-ray spectroscopy and by measuring the contact angle with Ringer's solution. The LIPSS formation resulted in an increased wetting of the surface with the lubricant. Moreover, the selectively structured composite surfaces revealed a coefficient of friction significantly reduced by a factor of ~3 when compared to the non-irradiated surface. Furthermore, the formation of a laser-induced oxidation layer was detected with NbO as the most prominent oxidation state. Selectively structured composites with outstanding mechanical properties and enhanced tribological performance are of particular interest for biomedical applications.