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.     

Planar Droplet Sizing for the Characterization of Droplet Clusters in an Industrial Gun‐Type Burner

An important problem in spray combustion deals with the existence of dense regions of droplets, called clusters. To understand their formation mechanism, the droplet dynamics and fuel concentration profile are investigated by means of planar laser techniques in an industrial gun‐type burner. The simultaneous measurement of elastic Mie scattering and Laser Induced Fluorescence (LIF) allows the instantaneous measurement of the Sauter Mean Diameter (SMD), after proper calibration. Using two different CCDs to get the two signals requires a detailed calibration of the CCD response before getting absolute diameters. Pixels are binned 6 by 6 to obtain the final SMD map, this is a compromise between spatial accuracy and noise. Velocity field is measured on both sets of images using standard Particle Image Velocimetry (PIV) algorithms. The comparison of cross‐correlation technique with PDA results shows that the velocity measured on the LIF images are close to the velocity based on D₃₀, whereas the Mie scattering results are similar to D₂₀. On Mie scattering images, regions of high interfacial area forming clusters can be detected. A special tracking scheme is used to characterize their dynamics in terms of velocity and diameters by ensuring that the same volume of fluid is tracked. It is shown that the clusters have a velocity similar to the velocity of droplets with the same diameter as the mean SMD of the cluster. It is also shown that an increase of pressure tends to trigger the appearance of such a group of droplets, due to a smaller diameter of the droplets caused by the increase of pressure discharge. Uncertainties for the different techniques used are discussed.     

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)     

Microfluidic Fabrication of Multi‐Drug‐Loaded Polymeric Microparticles for Topical Glaucoma Therapy

In this paper, the fabrication and characterization of multi‐drug‐loaded microparticles are demonstrated for topical glaucoma therapy. Specifically, latanoprost (“LAT”) and dexamethasone (“DEX”) are loaded in monodisperse microparticles (diameter ≈150 μm) of a biodegradable polymer–poly (lactic‐co‐glycolic) acid (PLGA)—using capillary microfluidics coupled with solvent evaporation. Both individual (LAT in PLGA and DEX in PLGA) and combined (LAT and DEX in PLGA) microparticle formulations are demonstrated. The morphology, size distribution and in vitro release kinetics are studied, and in vitro mucoadhesion of the formulated microparticles is also assessed. In addition, discussion is placed in how precise knowledge of the particle composition enabled by the microfluidic fabrication method and in vitro release rate measurements allow for facile topical formulation design and dose optimization. Such precision‐fabricated, multi‐drug loaded, sustained‐release microparticles are envisioned to serve as a promising platform for topical administration of ocular drugs. This could potentially reduce the frequency of eyedrop‐based drug administration from several times a day to merely once a day (or less), thus greatly facilitating patient compliance and adherence to a strict therapeutic drug regimen.     

A Multi‐Electrode Approach for On‐Line Characterisation of Size and Shape

A multi‐electrode approach is proposed for on‐line characterisation of particle size and shape in dilute particulate suspensions. Based on an electrozone principle, the approach uses four electrodes in a tube rather than two electrodes across an aperture employed in conventional methods. The outer two electrodes are used for current injection, while the inner two electrodes yield voltage measurement. A sensor designed in this way can reduce errors of false counts and oversizing that may occur in conventional methods, thus providing more accurate particle sizing. It is also possible to use the signal slope along with signal peak for particle size and shape characterisation. Both theoretical modelling and experiments were conducted, showing that particle aspect ratio along with particle diameter can be obtained, for example, for cylindrical particles.     

Thermodynamic Parameters of Single‐ or Multi‐Band Superconductors Derived from Self‐Field Critical Currents

Key questions for any superconductor include: what is its maximum dissipation‐free electrical current (its ‘critical current') and can this be used to extract fundamental thermodynamic parameters? Present models focus on depinning of magnetic vortices and implicate materials engineering to maximise pinning performance. But recently we showed that the self‐field critical current for thin films is a universal property, independent of microstructure, controlled only by the penetration depth. Here, using an extended BCS‐like model, we calculate the penetration depth from the temperature dependence of the superconducting energy gap thus allowing us to fit self‐field critical current data. In this way we extract from the T ‐dependent gap a set of key thermodynamic parameters, the ground‐state penetration depth, energy gap and jump in electronic specific heat. Our fits to 79 available data sets, from zinc nanowires to compressed sulphur hydride with critical temperatures of 0.65 to 203 K, respectively, are excellent and the extracted parameters agree well with reported bulk values. Samples include thin films, wires or nanowires of single‐ or multi‐band s ‐wave and d ‐wave superconductors of either type I or type II. For multiband or multiphase samples we accurately recover individual band contributions and phase fractions.     

Resistive Pulse Sensing as a High‐Resolution Nanoparticle Sizing Method: A Comparative Study

One of the main challenges of sizing methods for nanoparticle (NP) suspensions is to distinguish between particles and particle populations with very small size differences. This would be especially important to follow various surface functionalization processes of nanoparticles resulting in small alterations of their size. In this respect, methods involving the detection of single particles, such as resistive pulse sensing (RPS) or nanoparticle tracking analysis, are generally considered superior to ensemble measuring methods such as dynamic light scattering. However, to compare the exact capabilities of these methodologies require systematic investigations in optimized conditions for each method. Here, such a study is presented for a narrow size range of spherical latex nanoparticles (60–200 nm). It is concluded that the RPS methodology based on quartz nanopipets as single nanopore counters, is the only sizing method among those studied capable to fully resolve a ternary mixture of 70, 110, and 140 nm average diameter NPs. The practical usefulness of this size resolution is demonstrated by following the increase in diameter of latex nanoparticles after their surface modification with antibodies.     

miXAFS: a program for X‐ray absorption fine‐structure data analysis

A new program called miXAFS for the analysis of X‐ray absorption fine‐structure (XAFS) data is presented. miXAFS can analyze the XAFS functions simultaneously for all measured X‐ray absorption edges of the constituent elements in a sample under the constraints for the structural parameters over the edges. The program provides a surface plot of the R‐factor as a function of two structural parameters, which is useful to validate the optimized structural parameters. The structural parameters can be obtained from the XAFS data in a few steps using the setting file and batch process. The program, which is coded in MATLAB and freely available, runs on Macintosh and Windows operating systems. It has a graphical user interface and loads experimental data and XAFS functions in a variety of ASCII data formats.     

A twelve‐analyzer detector system for high‐resolution powder diffraction

A dedicated high‐resolution high‐throughput X‐ray powder diffraction beamline has been constructed at the Advanced Photon Source (APS). In order to achieve the goals of both high resolution and high throughput in a powder instrument, a multi‐analyzer detector system is required. The design and performance of the 12‐analyzer detector system installed on the powder diffractometer at the 11‐BM beamline of APS are presented.     

Depth‐resolved micro‐Raman spectroscopy of tri‐layer PFSA membrane for PEM fuel cells: how to obtain reliable inner water contents

Raman depth‐profiling microspectroscopy is currently emerging as a fast and non‐invasive method for the local content measurement of water diffusing across the perfluorosulfonic acid polymer used as electrolyte in low‐temperature fuel cells. However, water depth profiles obtained thereby are affected by the gradual degradation of the Raman signal as the exciting radiation is focused deeper into the sample and, thus, usually exhibit artificial gradients. The appropriate way to rectify raw data, in order to measure reliable inner water contents, is discussed in the case of perfluorosulfonic acid membranes soaked in water. The method is tested on a tri‐layer material composed by stacked ionomers with different chemical composition, ionic exchange capacity and swelling. Comparison of Raman spectra of the different ionomers, obtained under strictly the same hydration and optical conditions, allows critical discussion of previously reported band assignments. It is shown that Raman bands arising from the polymer backbone and from the side chain can be readily discriminated. Reliable water concentration profiles can then be obtained from the ratio between the Raman signal of sorbed water and of the polymer phase. Comparison with depth profiles obtained by using the pure water signal as internal reference shows that quantitative measurement requires the careful choice of the adequate Raman bands for representing the ionomer occupation of the volume probed by the exciting radiation. Different to what usually performed, the ionomer Raman signal to be integrated for compensating optical losses should include both bands arising from the polymer backbone and side chains. Last, obtaining accurate water concentration profiles also needs the knowledge of the so‐called optical factor β, i.e. the ratio between the scattering cross sections of ionomer chemical groups and sorbed water, which has to be measured by independent Raman experiments. Copyright © 2012 John Wiley & Sons, Ltd.     

Using the T‐Matrix Method for Light Scattering Computations by Non‐axisymmetric Particles: Superellipsoids and Realistically Shaped Particles

Light scattering by non‐axisymmetric particles is commonly needed in particle characterization and other fields. After much work devoted to volume discretization methods to compute scattering by such particles, there is renewed interest in the T‐matrix method. We extended the null‐field method with discrete sources for T‐matrix computation and implemented the superellipsoid shape using an implicit equation. Additionally, a triangular surface patch model of a realistically shaped particle can be used for scattering computations. In this paper some exemplary results of scattering by non‐axisymmetric particles are presented.     

Particle‐in‐cell simulation of an optimized high‐efficiency multistage plasma thruster

Electric propulsion attracts increasing attention in contemporary space missions as an interesting alternative to chemical propulsion because of the high efficiency it offers. The High‐Efficiency Multistage Plasma thruster, a class of cusped field thruster, is able to operate at different anode voltages and operation points and thereby generate different levels of thrust in a stable and efficient way. Since experiments of such thrusters are inherently expensive, multi‐objective design optimization (MDO) is of great interest. Several optimized thruster designs have resulted from a MDO model based on a zero‐dimensional (0D) power balance model. However, the MDO solutions do not warrant self‐consistency due to their dependency on estimation from empirical modelling based on former experimental studies. In this study, one of the optimized thruster designs is investigated by means of particle‐in‐cell (PIC) analysis to examine the predicted performance characteristics with self‐consistent simulations. The 0D power balance model is used to develop additional diagnostics for the PIC simulations to improve the physics analysis. Using input parameters for the 0D power balance model from the PIC simulations allows further improvement for the design optimization.     

A novel multi‐detection technique for three‐dimensional reciprocal‐space mapping in grazing‐incidence X‐ray diffraction

A new scattering technique in grazing‐incidence X‐ray diffraction geometry is described which enables three‐dimensional mapping of reciprocal space by a single rocking scan of the sample. This is achieved by using a two‐dimensional detector. The new set‐up is discussed in terms of angular resolution and dynamic range of scattered intensity. As an example the diffuse scattering from a strained multilayer of self‐assembled (In,Ga)As quantum dots grown on GaAs substrate is presented.     

Characterization of Nano‐Particles Using Laser‐Induced Incandescence

Laser‐induced incandescence (LII) is introduced as a valuable tool for the characterization of nanoparticles. This optical measurement technique is based on the heating of the particles by a short laser pulse and the subsequent detection of the thermal radiation. It has been applied successfully for the investigation of soot in different fields of application, which is described here in the form of an overview with a focus on work done at the LTT‐Erlangen during the last 10 years. In laboratory flames the soot primary particle size, volume concentration, and relative aggregate size have been determined in combination with the number density of primary particles. Furthermore, the primary particle sizes of carbon blacks have been measured in situ and online under laboratory conditions and also in production reactors. Measurements with different types of commercially available carbon black powders, which were dispersed in a measurement chamber yielded a good correlation between LII results and the specified product properties. Particle diameters determined by LII in a furnace black reactor correlate very well with the CTAB‐absorption number, which is a measure for the specific surface area. It turned out that the LII method is not affected by variations of the aggregate structure of the investigated carbon blacks. The LII signal also contains information on the primary particle size distribution, which can be reconstructed by the evaluation of the signal decay time at, at least, two different time intervals. Additionally, soot mass concentrations have been determined inside diesel engines and online measurements were performed in the exhaust gas of such engines for various engine conditions simultaneously providing information about primary particle size, soot volume, and number concentration. The LII results exhibit good correlation with traditional measurement techniques, e.g., filter smoke number measurements. In addition to the soot measurements, primarily tests with other nanoparticles like TiO₂ or metal particles are encouraging regarding the applicability of the technique for the characterization of such different types of nanoparticles.     

数字显微全息重建图像的景深扩展研究

显微物镜的景深问题限制数字显微全息在大纵深视场中的应用. 本文充分利用数值重建的特点, 采取低频和高频系数子图上的最大亮度梯度的局部方差作为聚焦判据, 在小波分解域内对显微全息重建图像的景深扩展问题进行了研究. 对倾斜的连续物体碳纤维进行三维重建, 分析了重建距离与直径测量误差的关系. 以超声波雾化器生成的微液滴颗粒场为例, 对离散颗粒场的重建图像进行了景深扩展. 利用基于广义洛伦兹-米散射理论的模型分别模拟1-15 μm 的非透明与透明离散颗粒的显微全息图, 分析了该方法重建的颗粒场的纵深定位误差与夫琅禾费系数的关系, 对比了非透明与透明颗粒纵深定位误差的异同点. 实验和模拟结果显示出该方法对于连续物体和离散颗粒场的显微全息重建图像的景深扩展能力, 且能由此准确重建物体信息.     

自动调焦系统中一种调焦的判别方法

准确有效的调焦评价函数是采用数字图像处理技术实现自动调焦的关键环节,而调焦评价函数的好坏又直接影响着调焦系统的结构精度和运算的复杂程度。分析了灰度标准差比较法和灰度对比度比较法的优缺点,提出了经改进的灰度比较法作为调焦评价函数,该方法具有响应速度快、计算量小、信噪比高、可靠性好等特点。实验与分析结果表明,该方法对具有复杂细节和纹理特征的图像能得到较好的处理结果,而对于背景高亮度的图像则不能判断其是否聚焦。     

A robust method for high‐precision quantification of the complex three‐dimensional vasculatures acquired by X‐ray microtomography

The quantification of micro‐vasculatures is important for the analysis of angiogenesis on which the detection of tumor growth or hepatic fibrosis depends. Synchrotron‐based X‐ray computed micro‐tomography (SR‐µCT) allows rapid acquisition of micro‐vasculature images at micrometer‐scale spatial resolution. Through skeletonization, the statistical features of the micro‐vasculature can be extracted from the skeleton of the micro‐vasculatures. Thinning is a widely used algorithm to produce the vascular skeleton in medical research. Existing three‐dimensional thinning methods normally emphasize the preservation of topological structure rather than geometrical features in generating the skeleton of a volumetric object. This results in three problems and limits the accuracy of the quantitative results related to the geometrical structure of the vasculature. The problems include the excessively shortened length of elongated objects, eliminated branches of blood vessel tree structure, and numerous noisy spurious branches. The inaccuracy of the skeleton directly introduces errors in the quantitative analysis, especially on the parameters concerning the vascular length and the counts of vessel segments and branching points. In this paper, a robust method using a consolidated end‐point constraint for thinning, which generates geometry‐preserving skeletons in addition to maintaining the topology of the vasculature, is presented. The improved skeleton can be used to produce more accurate quantitative results. Experimental results from high‐resolution SR‐µCT images show that the end‐point constraint produced by the proposed method can significantly improve the accuracy of the skeleton obtained using the existing ITK three‐dimensional thinning filter. The produced skeleton has laid the groundwork for accurate quantification of the angiogenesis. This is critical for the early detection of tumors and assessing anti‐angiogenesis treatments.     

Nondestructive elemental depth profiling of Japanese lacquerware ‘Tamamushi‐nuri’ by confocal 3D‐XRF analysis in comparison with micro GE‐XRF

We have applied recently two XRF (micro x‐ray fluorescence) methods [micro‐Grazing Exit XRF (GE‐XRF) and confocal 3D‐XRF] to Japanese lacquerware ‘Tamamushi‐nuri.’ A laboratory grazing‐exit XRF (GE‐XRF) instrument was developed in combination with a micro‐XRF setup. A micro x‐ray beam was produced by a single capillary and a pinhole aperture. Elemental x‐ray images (2D images) obtained at different analyzing depths by micro GE‐XRF have been reported. However, it was difficult to directly obtain depth‐selective x‐ray spectra and 2D images. A 3D XRF instrument using two independent polycapillary x‐ray lenses and two x‐ray sources (Cr and Mo targets) was also applied to the same sample. 2D XRF images of a Japanese lacquerware showed specific distributions of elements at the different depths, indicating that ‘Tamamushi‐nuri’ lacquerware has a layered structure. The merits and disadvantages of both the micro GE‐XRF and confocal micro XRF methods are discussed. Copyright © 2009 John Wiley & Sons, Ltd.