On-line automatic optical inspection system for coarse particle size distribution

A new online automatic optical inspection system (OAOIS) using digital image processing has been developed to measure the coarse particle size distribution. The OAOIS is composed of particle separation module, image acquisition module, image processing and analysis module and PC/PLC-based electric control module. Experiments were performed with non-uniform particles (1-100 mm). The particle size distribution, number of the particles, and accumulated weight percentages of particles are obtained by using the developed system. The experimental results show that the repeated precision of accumulated weight percentages is around ± 1%. To improve the reliability and accuracy of the OAOIS measuring results, the linear regression equation is applied to mapping the result of OAOIS to that of traditional net sieving system (TNSS). It has been shown that the developed system has a high accuracy and precision for coarse particle sizing distribution.     

图像分析技术在聚合物/粘土纳米复合材料微观结构形态研究中的应用

基于MATLAB图形及影像处理技术，开发了适用于处理聚合物／粘土纳米复合材料（PCN）微观结构形态的应用程序。应用程序包含边界探测和颗粒尺寸分析两个子程序，具有探测孤立颗粒边界和计算颗粒尺寸功能。应用该程度分析了聚丙烯／蒙脱土（PP／MMT）纳米复合材料初级结构的TEM照片，得到蒙脱土片层在PP基体中的微观结构形态和尺寸分布。结果表明：该图像分析技术能够快速有效地确定PCN的TEM照片中粘土片层的形状和尺寸。此外，该图像分析技术还可以用于共混物形态的研究。     

Spatial gradients in particle reinforced polymers characterized by X-ray attenuation and laser confocal microscopy

The goal of this work is to develop techniques for measuring gradients in particle concentration within filled polymers, such as thermosetting polymer encapsulants. A high concentration of filler particles is added to such materials to tailor physical properties such as thermal expansion coefficient. Sedimentation and flow-induced migration of particles can produce concentration gradients that are most severe near boundaries. Therefore, techniques for measuring local particle concentration should be accurate near boundaries. Particle gradients in an alumina-filled epoxy resin are measured with a spatial resolution of 0.2 mm using an X-ray beam attenuation technique, but an artifact reduces accuracy near the specimen's edge. Local particle concentration near an edge can be measured more reliably using microscopy coupled with image analysis. This is illustrated by measuring concentration profiles of glass particles having 40 μm median diameter using images acquired with a confocal laser fluorescence microscope. The mean of the measured profiles of volume fraction agrees to better than 3% with the expected value and the shape of the profiles agrees qualitatively with simple theory for sedimentation of monodisperse particles. Evidence that the microscopic method can be extended to smaller particles is provided by local concentration measurements on an epoxy polymer containing particles having diameters of the order of 1 μm.     

Errors implicit in digital particle characterisation

Factors affecting the accuracy of using digitised images of projected particles in order to determine particle properties such as shape, size and particle perimeter are defined. In particular, the inaccuracies in the representation of particles of known shapes as digitised particles under different resolutions due to loss of information at the particle boundary are quantified. The results are generalised for arbitrary shapes by the use of mathematical proof and implications are considered for relevant particle analysis techniques. An attempt is made to find relationships between resolution and accuracy, and between particle shape and accuracy. Accuracy here is defined as the deviation of the area of the digitised image from the actual area of the real particle. Implications for accuracy of 3D digitised representations of particles are highlighted and its relevance to predictions of 3D particle packing based on the digitised data.     

机制砂颗粒形状的评价方法及其特征研究

为研究机制砂粒形表征方法及特点,采用集料图像测量系统(AIMS)和数字图像处理(DIP)技术测试了5种机制砂的颗粒形态。基于现有研究存在的不足提出了一种改进的粒形测试方法,并研究了不同粒形表征参数之间的关系。结果表明:随着粒径范围从大到小,机制砂的棱角性呈先增大后减小的趋势,而二维形状值无明显变化规律;0.3~0.6 mm的机制砂可以反映整体粒径范围的棱角性;通过单次投影进行图像处理获取的粒形参数有较大的波动范围,无法准确判断机制砂的颗粒形状;纵横比与凹凸度有较强的相关性,粗糙度与纵横比、圆度、凹凸度的相关性较强,而分形维数与其他几种参数都不具有相关性;通过改进的DIP技术得出的粒形评价结论与AIMS得出的评价结论一致,具有一定的可行性和推广价值。     

Application of inline imaging for monitoring crystallization process in a continuous oscillatory baffled crystallizer

In this study, an in situ imaging system has been analysed to characterize the crystal size, the shape and the number of particles during a continuous crystallization process in a Continuous Oscillatory Baffled Crystallizer (COBC). Two image analysis approaches were examined for particle characterization in the suspension containing both small nuclei and larger grown crystals (nonspherical and irregular in shape). The pattern matching approach, in which the particles are approximated to be spherical, did result in an overestimation of the size. Alternatively, a segmentation‐based algorithm resulted in reliable crystal size and shape characteristics. The laser diffraction analysis in comparison to the image analysis overestimated the particle sizes due to the agglomeration of particles upon filtration and drying. The trend in the particle counts during the start of crystallization process, including nucleation, determined by the image analysis probe was comparable with the one measured by FBRM, highlighting the potential of in situ imaging for process monitoring. © 2018 American Institute of Chemical Engineers AIChE J, 64: 2450–2461, 2018     

Measurement of size and shape distributions of particles through image analysis

The size and shape of particles can be described using a 2D particle size distribution (PSD) where two characteristic lengths define each particle in the population. The determination of 2D PSDs based on microscopic pictures of particles in suspension is studied. The experimental data are represented as an axis length distribution (ALD) that can be extracted from a series of microscopic pictures by a fully automated image analysis. The problem of finding the underlying bi-dimensional PSD is stated as an optimization problem. For the solution a genetic algorithm is used. The approach is tested on simulated ALDs, as well as on an experimentally measured ALD obtained from carbon fiber particles.     

基于特征相似度匹配PTV法的稀相气固两相流流场的测量

提出一种基于几何特征和归一化转动惯量特征相似度相结合的粒子跟踪测速算法。该方法采用高速摄像机拍摄流化床中气固两相流的稀相颗粒运动图像,经图像处理后,提取特征参数,进而应用面积和周长相似度对颗粒进行初步筛选匹配。然后对经过初步筛选后的颗粒进行归一化转动惯量最佳相似度的匹配,从而准确快速地实现颗粒匹配,进而计算出气固两相流颗粒的流速。实验结果表明,该方法能准确地跟踪稀相颗粒,是一种行之有效的稀相流场速度测量方法。     

Particle Shape and Size Effects on Anisotropic Shrinkage in Tape-Cast Ceramic Layers

The particle shape of a commercial low-temperature cofired ceramic (LTCC) composite powder was determined quantitatively in the as-received and milled state using a new particle image analyzer. All grades of the milled powder with average particle sizes of 3.0, 2.4, and 1.8 μm, respectively, exhibit a considerable stretched particle shape, because 40% of their particles have circularity values below 0.95. On the basis of the fast particle image analyzer, the influence of the raw materials on particle alignment during tape casting was investigated using "design of experiments" (DOE). In the cast LTCC green tapes, the degree of particle orientation was measured and correlated with the information from the particle shape analyses and with other material and process factors from the DOE. The results showed that the degree of particle alignment correlates significantly with the measured particle shape and size; more than 80% of the particles were oriented in the casting direction if their shape factor was below 0.5. The particle orientation causes shrinkage anisotropy. The use of a coarser LTCC powder with an average particle size d ₅₀ of 3.0 μm instead of 1.8 μm increased the sintering anisotropy factor of LTCC tapes and laminates significantly from 1.0% to 1.85% and from 3.6% to 7.6%, respectively. The use of more binder or less solvent led to higher shrinkage anisotropies too. The casting velocity showed only a minor effect on the degree of particle orientation and sintering anisotropy, which is due to the shorter shearing period in which particle rotation can take place.     

基于粒子群优化Hopfield网络匹配的稀相颗粒速度测量

提出了一种基于粒子群算法(PSO)和Hopfield神经网络相结合的粒子跟踪测速算法。该方法采用高速摄影系统拍摄气固两相流的稀相颗粒运动图像,经图像处理后,提取形心参数。将粒子匹配问题转化为优化问题,采用粒子群优化算法与Hopfield神经网络相结合的方法进行优化,求出最优解来实现颗粒的正确匹配,然后计算出颗粒的速度矢量,并与互相关法求出的速度进行对比,实验结果表明,该方法能准确地跟踪稀相颗粒,是一种有效的稀相流场速度测量方法。     

Application of organic nonsolvent in the process of solution-enhanced dispersion by supercritical CO2 to prepare puerarin fine particles

An organic nonsolvent, dichloromethane was employed in the process of solution-enhanced dispersion by supercritical CO₂ (SEDS) to prepare fine particles of puerarin. A 2³ factorial experiment was designed to investigate and identify the relative significance of the processing parameters on the surface morphology, particle size and particle size distribution of the products. The effect of the nonsolvent/solvent ratio was found to be dominant in the results regarding particle size. Increasing the nonsolvent content of the puerarin solution decreased the particle size significantly. After optimization, the resulting puerarin nanoparticles exhibited a good spherical shape, a smooth surface and a narrow particle size distribution, with a mean particle size of 0.19 μm. After SEDS processing, the measurements of high performance liquid chromatography (HPLC), ultraviolet (UV) and mass spectrometry (MS) indicated there was no change in the chemical composition of puerarin particles; Fourier transform infrared (FTIR) spectroscopy measurement found the minor structural changes occurred on a molecular level; X-ray powder diffraction (XRPD) analysis revealed that the physical state of puerarin shifted into an amorphous form; and a significant increase in the dissolution rate of puerarin nanoparticles was observed. The SEDS process combined with the addition of dichloromethane could produce puerarin nanoparticles without contamination.     

Optical inline analysis and monitoring of particle size and shape distributions for multiple applications: Scientific and industrial relevance

Particles occur in almost all processes in chemical and life sciences. The particle size and shape influence the process performance and product quality, and in turn they are influenced by the flow behavior of the particles during production. Monitoring and controlling such characteristics in multiphase systems to obtain sufficient qualities will greatly facilitate the achievement of reproducible and defined distributions. So far, obtaining this information inline has been challenging, because existing instruments lack measurement precision, being unable to process overlapping signals from different particle phases in highly concentrated multiphase systems. However, recent advances in photo-optics made it possible to monitor such features (particle size distribution (PSD), aspect ratio and particle concentration) with advanced image analysis (IA) in real-time. New analysis workflows as well as single feature extractions from the images using multiple image analysis algorithms allowed the precise real-time measurements of size, shape and concentration of particle collectives even separated from each other in three phase systems. The performances, advantages and drawbacks with other non-photo-optical methods for assessing the particle size distribution are compared and discussed.     

Microparticle characterization using digital holography

Digital holography is an effective 3D imaging technique, with the potential to be used for particle size measurements. A digital hologram can provide reconstructions of volume samples focused at different depths, overcoming the focusing problems encountered by other imaging based techniques. Several particle analysis methods discussed in the literature consider spherical particles only. With the object sphericity assumption in place, analysis of the holographic data can be significantly simplified. However, there are applications, such as particle analysis and crystallization monitoring, where non-spherical particles are often encountered. This paper discusses the processing of digital holograms for particle size and shape measurement for both spherical and arbitrarily shaped particles. An automated algorithm for identification of particles from recorded hologram and subsequent size and shape measurement is described. Experimental results using holograms of spherical and non-spherical particles demonstrate the performance of the proposed measuring algorithm.     

室内大气颗粒物分形结构分析

颗粒物的分形结构能表示颗粒物本身的性质特征,大气颗粒物对人体的危害与其分形结构有关。这里通过制作室内大气悬浮颗粒采集器,采集室内大气颗粒,然后通过数字显微技术和图像处理技术,分析颗粒投影图像的轮廓曲线分形维数值、圆度数值。结果表明：轮廓曲线分形维数值具有近似正态分布特征,圆度值和分形维数值间具有相关关系。通过测算分形维数值和圆度值可以近似判断室内空气的性质,对实现室内大气质量实时监测和计算机处理具有一定意义。     

高压静电抗溶剂法制备聚乳酸微球

以无水乙醇为非溶剂,采用高压静电抗溶剂法制备聚乳酸微球。通过24全因子试验设计对微球粒径和粒径分布的影响因素进行了显著性分析。并考察最显著因素对微球表面形貌的影响规律。结果表明,推进速度是影响微球粒径的最显著因素,最优条件下微球表面光滑、球形度好,粒径分布窄。浓度为3%,相对分子质量为5万～10万的聚乳酸制备的微球,球形度较好。经过高压静电处理后,傅里叶红外光谱测定表明聚乳酸无明显结构摄动;X射线粉末衍射分析表明聚乳酸晶体结构未发生明显变化。     

Rubber-modified epoxies: Interfacial tension and morphology

The interfacial tension between carbomethoxy-terminated butadiene–acrylonitrile copolymers and an epoxy resin as a function of temperature and copolymer composition is investigated. Using a digital image processing technique, the shape of a pendant drop of the epoxy in the copolymer is determined. Analysis of the drop shape is performed by profile discrimination and subsequent robust shape analysis. The data are used to examine the relationship between interfacial tension and particle size of the dispersed copolymer-rich phase in rubber-modified epoxy resins, that are immiscible in the uncured state.     

多喷嘴对置式气化炉内颗粒挥发分火焰可视化研究

基于实验室规模多喷嘴对置式水煤浆气化炉及其可视化装置,研究了气化炉喷嘴平面非射流区颗粒挥发分燃烧过程。结合图像处理技术,在气化条件下对粒径小于300 μm颗粒挥发分火焰尾迹形态及变化过程进行分析。研究结果表明,颗粒挥发分火焰非典型包络型火焰,而是形成挥发分火焰尾迹。颗粒挥发分尾迹形态受颗粒脱挥发分所处阶段和颗粒相对于气流的运动状态的影响,随时间不断变化。颗粒挥发分最大火焰尺寸随颗粒粒径增加而增加。气流床气化还原性气氛条件下颗粒挥发分燃烧时间较颗粒在富氧气氛中燃烧时间显著增加。     

Temperature-dependent properties of silver-poly(methylmethacrylate) nanocomposites synthesized by in-situ technique

Ag/PMMA nanocomposites were successfully synthesized by in-situ technique. Transmission electron microscopy (TEM) images show that the particles are spherical in shape and their sizes are dependent on temperature. The smallest particle achieved high stability as indicated from Zeta sizer analysis. The red shift of surface plasmon resonance (SPR) indicated the increases of particle sizes. X-ray diffraction (XRD) patterns exhibit a two-phase (crystalline and amorphous) structure of Ag/PMMA nanocomposites. The complexation of Ag/PMMA nanocomposites was confirmed using Raman spectroscopy. Fourier transform infrared spectroscopy spectra confirmed that the bonding was dominantly influenced by the PMMA and DMF solution. Finally, thermogravimetric analysis (TGA) results indicate that the total weight loss increases as the temperature increases.