Absorption and Scattering of Light by Highly Concentrated Two‐phase Flows

The spray cone emerging during an extended metal atomization process (called spray forming) has been investigated in order to quantify the influence of highly concentrated multiphase flows on phase‐Doppler‐anemometry (PDA) measurements. Using this non‐intrusive, optical measurement technique not only the local particle size and velocity distributions of the spray can be obtained but also additional information about the mass flux in the multiphase flow. Since standard phase‐Doppler systems can be easily applied to low concentrated particle systems (spherical particles with smooth surfaces and an optical transparent continuous phase taken for granted) the application of this measurement technique to highly concentrated multiphase flows is more complex. Both the laser light propagating from the PDA device to the probe volume and the scattered one going backward to the PDA receiving system are disturbed by passing the highly concentrated multiphase flow. The resulting significant loss in signal quality especially concerns the measurement of the smaller particles of the spray because of their reduced silhouette (in comparison with the bigger ones). Thus, the detection of the smallest particles becomes partially impossible leading to measurement of a distorted diameter distribution of the entire particle collective. In this study the distortions of the measured distributions dependent on the particle number concentration as well as on the path length of the laser light are discussed.     

Investigation of the Flow Field in the Upper Part of a Cyclone with Laser and Phase Doppler Anemometry

The cyclone is a well known apparatus for separating particles out of a gas stream. With the modern laser diagnostic technologies of laser and phase Doppler anemometry (LDA and PDA), there is the potential to measure the flow and particle field inside the cyclone. The gas phase only measurements used micron‐sized oil seeding droplets, whereas the solid phase, chosen for the PDA particle size measurements, was limestone powder. To assess the possibility of measuring milled limestone particles with PDA, the measured size distribution was compared with those obtained by laser diffraction. The measurements inside the cyclone showed that the flow field in the upper part of the cyclone was different to that commonly thought. Therefore, the vertical height of the cyclone's vortex finder could be shortened without deterioration of the separation efficiency. The particles found in the hold‐up of the cyclone air flow were considerably larger than the average particle size in the feed pipe.     

Assessment of Pulsed Gasoline Fuel Sprays by Means of Qualitative and Quantitative Laser‐based Diagnostic Methods

The combination of qualitative measuring techniques such as imaging, with quantitative drop sizing techniques like Laser Diffraction and Phase Doppler Analyzer (PDA), has been applied for assessing the sprays formed by injectors for gasoline direct injection (DI) engines. Both, the sizing instruments as well as the imaging, are offering temporal resolution in order to investigate the important features of pulsed DI sprays. Using a combination of the spatially integrating Laser Diffraction instrument with strobe illuminated dual view 2D‐imaging, the overall spray properties have been assessed. Having the 2D information of the global spray shape in two perpendicular directions allows one to immediately correlate the concentration and drop size measurement results of the Laser Diffraction instrument with the global spray appearance. Thus, the changes of the spray pattern can be related with the sizing information as the spray propagates away from the injector. For injector design improvements, however, it is required to achieve a higher spatial resolution and especially to measure closer to the injector exit orifice than the Laser Diffraction allows. By using a Phase Doppler Analyzer, the different phases of the injection event, i.e. opening of the injector, main spray and closing phase of the injector, can be distinguished from each other. However, in sprays, where the spray geometry is changing with time, the PDA can suffer due to its high spatial resolution, yielding results that are difficult to interpret.Assisting the PDA with a simultaneous imaging technique of similar spatial resolution creates a very robust experimental approach. By visualizing the plane perpendicular to the PDA probe volume, i.e. the crossing of the PDA laser beams on the spray image itself, a very precise adjustment of the PDA probe volume with respect to the spray rather than the nozzle can be achieved. This becomes critical when getting to the near orifice area at distances closer than 10mm. The synchronized images also bring additional information to the point measurement provided by the PDA. It becomes easier to choose which particular phase of the spray formation the user wants to characterize. Finally, more confidence in the interpretation of PDA data from locations close to the injector tip is reached.     

Two‐Phase Flow Characterization by Automated Digital Image Analysis. Part 2: Application of PDIA for Sizing Sprays

A series of experiments were conducted in order to assess the robustness and accuracy of a recently developed digital image analysis technique (PDIA). This paper investigates the application of the PDIA technique to the sizing of relatively small fuel droplets of diameters in the range 5 to 30 μm produced by a pressure‐swirl atomizer. The measurement performance of the PDIA system has been assessed in terms of individual object diameters and also number and volume probability density functions of diameter in comparison to phase Doppler anemometry (PDA) data obtained under identical conditions. PDIA measurements revealed good agreement with spray data obtained by PDA at a measurement location 36 diameters downstream from the nozzle orifice with differences in the arithmetic mean diameter, D₁₀ and volume mean diameter, D₃₀ of approximately 5 and 3% respectively. The PDIA technique was shown to detect the presence of very large, predominantly non‐spherical droplets whose diameters were in excess of 100 μm. These droplets, although few in number constitute a significant proportion of the total spray volume and would have otherwise been either erroneously measured or have passed through the probe volume undetected using PDA due to non‐sphericity. Smaller objects may also be measured correctly by both methods although sensitivity to signal‐to‐noise ratio, for both methods can generate spurious and contradictory errors.     

Investigation of nanoscale element distributions at surfaces with grazing incidence X‐ray spectroscopy techniques – an instrumentation study

Grazing incidence X‐ray methods are well‐established in the characterization of nanostructures at interfaces and surfaces. The purpose of the experiments reviewed in this work is the comparative characterization of different instrumentation concepts for grazing incidence X‐ray fluorescence analyses. Fluorescence scans recorded with a total reflection X‐ray fluorescence spectrometer featuring a variable angle of incidence are compared with data obtained with synchrotron radiation. The conclusions to the element distribution profiles, which are drawn from fluorescence scans carried out with the respective instrument, are compared. This way, the suitability of the total reflection X‐ray fluorescence spectrometer to complement synchrotron radiation facilities and the possibility to transfer surface and interface analyses from the synchrotron to the laboratory are assessed. The structures investigated include an Au on Si surfaces in the form of layers and particles, submicrometer‐sized droplets, a liquid film, and ions implanted into a Si wafer. Copyright © 2014 John Wiley & Sons, Ltd.     

Quantitative Measurement of Planar Droplet Sauter Mean Diameter in Sprays using Planar Droplet Sizing

The purpose of this investigation is to assess and improve the accuracy of Sauter Mean Diameter measurements in dense sprays using a Planar Droplet Sizing (PDS) technique, based on the intensity ratio of scattered and fluorescence light. A novel data processing method of the PDS technique is suggested, which was derived from a theoretical light scattering investigation, and reduced possible sizing errors larger than 30% to below 10%. The novel approach for droplet sizing was applied to measure in a spray generated by a pressure swirl atomiser in a liquid‐fuelled burner operated with water at isothermal conditions, in order to avoid the effect of liquid evaporation on the accuracy of PDS technique. The Sauter Mean diameter results from the PDS technique were compared to Phase Doppler Anemometer (PDA) sizing measurements. Good agreement was obtained between the two techniques in dense regions of the spray. Discrepancies remained in dilute spray regions due to systematic statistical uncertainties of the PDS technique and the dynamic range of the intensity of the CCD cameras, which did not allow detection of large single droplets in the dilute spray region.     

Visualization of mouse spinal cord intramedullary arteries using phase‐ and attenuation‐contrast tomographic imaging

Many spinal cord circulatory disorders present the substantial involvement of small vessel lesions. The central sulcus arteries supply nutrition to a large part of the spinal cord, and, if not detected early, lesions in the spinal cord will cause irreversible damage to the function of this organ. Thus, early detection of these small vessel lesions could potentially facilitate the effective diagnosis and treatment of these diseases. However, the detection of such small vessels is beyond the capability of current imaging techniques. In this study, an imaging method is proposed and the potential of phase‐contrast imaging (PCI)‐ and attenuation‐contrast imaging (ACI)‐based synchrotron radiation for high‐resolution tomography of intramedullary arteries in mouse spinal cord is validated. The three‐dimensional vessel morphology, particularly that of the central sulcus arteries (CSA), detected with these two imaging models was quantitatively analyzed and compared. It was determined that both PCI‐ and ACI‐based synchrotron radiation can be used to visualize the physiological arrangement of the entire intramedullary artery network in the mouse spinal cord in both two dimensions and three dimensions at a high‐resolution scale. Additionally, the two‐dimensional and three‐dimensional vessel morphometric parameter measurements obtained with PCI are similar to the ACI data. Furthermore, PCI allows efficient and direct discrimination of the same branch level of the CSA without contrast agent injection and is expected to provide reliable biological information regarding the intramedullary artery. Compared with ACI, PCI might be a novel imaging method that offers a powerful imaging platform for evaluating pathological changes in small vessels and may also allow better clarification of their role in neurovascular disorders.     

Synthesis and structural characterization of novel flower-like titanium dioxide nanostructures

Titanium dioxide (TiO₂-anatase phase) films, consisting of agglomerated flower-like nanoparticles, have been synthesized using an ultrasonic spray pyrolysis method in conjunction with titanium (IV) oxide acetylacetonate (TiO(acac)₂) and methanol at 550 °C. These films were subsequently thermally treated in air, at 950 °C for 6 h, and the flower-like particles were transformed into smooth surfaces mainly formed by the TiO₂ rutile phase. In this letter, we characterized these structures using scanning electron microscopy, atomic force micrcoscopy, and low-angle X-ray diffraction measurements. It is proposed that these novel flower-like nanostructures, exhibiting a large number of exposed edges, will be important in the development of efficient gas sensor devices.     

Phase Doppler Anemometer for Measurements of Deterministic Spray Unsteadiness

A method and analysis was developed to quantify the amplitude of deterministic spray unsteadiness based on Phase Doppler Anemometry (PDA), which sampled time‐dependent droplet velocity and size measurements, in order to determine the fluctuations of droplet data rate and number density, which are quantities relevant to fluctuations of droplet concentration. The data processing method of the PDA measurements was assessed in a pulsed spray at a frequency of 20 Hz injected in a swirl‐stabilised burner. Comparisons between quantities relevant to droplet concentration fluctuations, measured by PDA and a light scattering technique, quantified the deterministic spray unsteadiness and agreed to within 15%. The developed PDA approach was applied in the swirl‐stabilised burner to measure the amplitude of deterministic spray unsteadiness of an otherwise steady spray, which was caused by the instability of the atomisation process. The intensity of deterministic fluctuations of droplet data rate and number density, occurring at a frequency range around 600 Hz due to the atomisation process, was quantified to 15% of the corresponding mean value and this spray unsteadiness generated fluctuations on the air and droplet velocity fields. The deterministic spray unsteadiness could survive up to the end of the recirculation zone of the air flow at the burner exit and, therefore, could influence flame stability.     

Investigations of Droplet‐Plasma Interaction using Multi‐Dimensional Coupled Model

Recently developed multi‐dimensional coupled fluid‐droplet model is used to investigate the behavior of complex interaction between the liquid precursor droplets and atmospheric pressure plasma (APP). The significance of this droplet‐plasma interaction is not well understood under diverse realm of working conditions in two‐phase flow. In this study, we explain the implication of vaporization of liquid droplets in APP which are subsequently responsible to control major characteristics of surface coating depositions. Coalescence of water droplets is more dominant than Hexamethyldisiloxane (HMDSO) droplets because of its sluggish rate of evaporation. A disparity in the performance of evaporation is identified in two independent mediums, such as gas mixture and discharge plasma using HMDSO precursor. The length of evaporation of droplets is amplified by an increment of gas flow rate indicating with a reduction in the gas temperature and electron mean energy. In particular, the spatio‐temporal density distributions of charged particles show a clear pattern in which the typical nitrogen impurity ions are primarily effective as compared to other helium ionic species along the pulse of droplets in APP. Finally, we contrast the behavior of discharge species in the pure helium and He‐N2 gas mixtures revealing the importance of stepwise and Penning ionization processes. (© 2015 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

New Generation of Phase-Doppler Instruments for particle velocity,size and concentration measurements

Phase-Doppler anemometry (PDA) is applied for particle size, velocity and concentration measurements in two-phase or multi-phase flows of ever increasing complexity. For accurate measurements the experimenter must be provided with software and hardware which permit an optimal layout of the PDA optics for a given application, reliable detection of signals over a wide particle diameter range, accurate determination of particle concentration and precise discrimination between particles of different composition. Recent work at LSTM, Erlangen, has been directed to developing a complete PDA package for the above purposes. Progress in this direction is summarized in this paper.     

Application of X‐ray fluorescence to turbulent mixing

Combined measurements of X‐ray absorption and fluorescence have been performed in jets of pure and diluted argon gas to demonstrate the feasibility of using X‐ray fluorescence to study turbulent mixing. Measurements show a strong correspondence between the absorption and fluorescence measurements for high argon concentration. For lower argon concentration, fluorescence provides a much more robust measurement than absorption. The measurements agree well with the accepted behavior of turbulent jets.     

Measuring partial fluorescence yield using filtered detectors

Typically, X‐ray absorption near‐edge structure measurements aim to probe the linear attenuation coefficient. These measurements are often carried out using partial fluorescence yield techniques that rely on detectors having photon energy discrimination improving the sensitivity and the signal‐to‐background ratio of the measured spectra. However, measuring the partial fluorescence yield in the soft X‐ray regime with reasonable efficiency requires solid‐state detectors, which have limitations due to the inherent dead‐time while measuring. Alternatively, many of the available detectors that are not energy dispersive do not suffer from photon count rate limitations. A filter placed in front of one of these detectors will make the energy‐dependent efficiency non‐linear, thereby changing the responsivity of the detector. It is shown that using an array of filtered X‐ray detectors is a viable method for measuring soft X‐ray partial fluorescence yield spectra without dead‐time. The feasibility of this technique is further demonstrated using α‐Fe₂O₃ as an example and it is shown that this detector technology could vastly improve the photon collection efficiency at synchrotrons and that these detectors will allow experiments to be completed with a much lower photon flux reducing X‐ray‐induced damage.     

Nanoresolution interface studies in thin films by synchrotron x‐ray diffraction and by using x‐ray waveguide structure

In the last years we performed several measurements with synchrotron radiation of several facilities to reveal interesting interface phenomena on the nanoscale. We used both x‐ray diffraction [1] , [2] (XRD) and spectrometry techniques. In this paper, we briefly summarize the results obtained from diffraction measurements, which lead us to our recent grazing incidence x‐ray fluorescence analysis (GIXRF) and extended x‐ray absorption fine structure (EXAFS) experiments. We show how a combination of experimental methods of GIXRF analysis and EXAFS spectroscopy in fluorescence detection with x‐ray standing waves (XSW) technique was applied for the depth profiling of a‐Si/Co/a‐Si layers with nanometer resolution to monitor the growth of CoSi intermetallic phase. The investigated layers were placed into the waveguide structure formed by two Ta films to increase sensitivity and accuracy of the measurements. Copyright © 2009 John Wiley & Sons, Ltd.     

Particle‐in‐cell/Monte Carlo simulation of electron and ion currents to cylindrical Langmuir probe

Electron and ion currents to a cylindrical Langmuir (electrostatic) probe were calculated using the particle‐in‐cell/Monte Carlo (PIC/MC) self‐consistent simulation for a neutral gas in the pressure range 2–3,000 Pa. The simulation enables us to calculate the probe currents even at high neutral gas pressures when the collisions of collected charged particles with neutral gas particles near the probe are important. The main aim of this paper is the calculation of probe currents at such high gas pressures and the comparison of the results with experimentally measured probe currents. Simulations were performed for two cases: (a) probes with varying radii in a non‐thermal plasma with high electron temperature at low neutral gas pressure of 2 Pa (in order to verify the correctness of our simulations), and (b) probe with the radius of 10 μm in the afterglow plasma with low electron temperature and a higher neutral gas pressure (up to 3,000 Pa). The electron probe currents obtained in case (a) show good agreement with those predicted by the orbital motion limited current (OMLC) theory for probes with radii up to 100 μm for the given plasma conditions. At larger probe radii and/or at higher probe voltages, the OMLC theory incorrectly predicts too high an electron probe current for the plasma parameters studied. Additionally, a formula describing the spatial dependence of the electron density in the presheath in the collisionless case is derived. The simulation at higher neutral gas pressures, i.e. case (b), shows a decrease of the electron probe current with increasing gas pressure and the creation of a large presheath around the probe. The simulated electron probe currents are compared with those of measurements by other authors, and the differences are discussed.     

Calibration method at the N K‐edge using interstitial nitrogen gas in solid‐state nitrogen‐containing inorganic compounds

The standard method of soft X‐ray beamline calibration at the N K‐edge uses the ν = 0 peak transition of gas‐phase N₂. Interstitial N₂ gas trapped or formed within widely available solid‐state ammonium‐ and amine‐containing salts can be used for this purpose, bypassing gas‐phase measurements. Evidence from non‐nitrogen‐containing compounds (KH₂PO₄) and from He‐purged ammonium salts suggest that production of N₂ gas is through beam‐induced decomposition. Compounds with nitrate or nitrite as anions produce coincident features and are not suitable for this calibration method.     

X‐ray absorption and x‐ray fluorescence for the characterization of titanium oxide‐modified HPLC silicas

Titanium oxide grafted on to the surfaces of chromatographic silica was investigated by x‐ray fluorescence (XRF) and x‐ray absorption (XAS) spectroscopy and the latter used before and after the extensive use of this material as a support for reversed‐phase high‐performance liquid chromatography (RP‐HPLC). XRF indicated the formation of a complete 2:1 monolayer whereas XAS suggested the presence of more than one titanium oxide structure. These structures show some slight modification after immobilization of PMOS and use in HPLC. Copyright © 2005 John Wiley & Sons, Ltd.     

X‐ray absorption measurements on an ultrasonic spray aerosol

Spray deposition of thin films and coatings is a widely used manufacturing process owing to its low cost, versatility and simple implementation. The objective of the presented experiments was to investigate whether X‐ray absorption measurements on solutes carried by aerosols are possible, and what count rates can be achieved depending on solution flow through and the resulting mass density in the interrogation volume. The investigated prototypical spray aerosol was InCl₃ dissolved in water or ethanol dispersed via an ultrasonic nebulizer. InCl₃ spray is essential for the ion layer gas reaction process used for the deposition of In₂S₃ buffer layers for highly efficient chalcopyrite solar cells. The discussed experiments demonstrate that measurements are possible, but that the achievement of good signal‐to‐noise ratios requires extended sampling times and concentrated solutions.     

Novel high‐temperature reactors for in situ studies of three‐way catalysts using turbo‐XAS

Two novel high‐temperature reactors for in situ X‐ray absorption spectroscopy (XAS) measurements in fluorescence are presented, each of them being optimized for a particular purpose. The powerful combination of these reactors with the turbo‐XAS technique used in a dispersive‐XAS beamline permits the study of commercial three‐way catalysts under realistic gas composition and temporal conditions.