利用低相干光纤动态光散射法测量浓悬浮液中多分散颗粒粒径分布

本文针对高浓度散射介质,用低相干光纤动态光散射技术测量浓悬浮液中多分散颗粒系的粒径及其粒径分布。利用迭代CONTIN算法对实验数据进行反演运算,得到多分散颗粒系的粒径分布结果。结果表明,浓悬浮液中多分散颗粒系的峰值粒径测量值与给定的两种标准粒径值相吻合,其误差在4%之内,粒径分布曲线中各散射颗粒所反映的散射体光强分布与根据Mie散射计算得到的理论值相吻合。实验结果证明低相干光纤动态光散射实验系统能准确测量浓悬浮液中多分散颗粒粒径及粒径分布。     

电解质对浓悬浮液中胶体颗粒扩散特性的影响

本文利用相位调制光纤低相干动态光散射装置, 研究了不同物质量浓度下电解质 (NaCl及 BaCl₂) 对浓悬浮液中聚苯乙烯胶体颗粒扩散特性的影响. 实验结果表明, 当电解质浓度低于0.01 mol/L 时, 恒温条件下浓悬浮液中聚苯乙烯胶体颗粒扩散系数随电解质离子浓度以及离子化合价的增大而增大, 实验测量得到的扩散系数与Stern模型所得到的扩散系数符合较好. 关键词： 测量 电解质 浓悬浮液 低相干动态光散射     

多模光纤式动态光散射实验研究

介绍了多模光纤在动态光散射中的应用,搭建了基于多模光纤的动态光散射实验系统,并用该系统测量了单分散、多分散以及不同浓度的标准聚苯乙烯乳胶球悬浮液.结果表明,该系统可准确地测量浓度达4.5%的聚苯乙烯乳胶球溶液中悬浮颗粒的粒径分布.     

高散射媒质中的光程可分割动态光散射研究

为研究散射光强度随光子在散射媒质中散射光程的变化,基于单散射理论与扩散波光谱理论,采用了低相干动态光散射装置对不同粒径大小的聚苯乙烯悬浮液进行研究。将测量得到的背散射光光场强度谱的线宽与相应的理论计算结果相比较发现,在短光程区域,考虑容器壁附近拖曳效应的影响后,对于不同粒径的颗粒,光程为约5倍粒子平均自由程的区域可看成为单散射区域;对于光程大于225 m的区域可看成为扩散光波区域。实验结果表明低相干动态光散射法可实现高散射媒质从单散射区域到低次散射再到扩散区域的全光程的可分割的光场强度谱测量。     

浓悬浮液中纳米SiO_2团聚体的渗透率

本文基于悬浮液中渗透性颗粒的短时扩散动力学理论,采用低相干光纤动态光散射方法,测量了相同粒径的纳米SiO_2团聚体在不同体积分数时的扩散系数,利用扩散系数随渗透率的变化关系得到纳米SiO_2团聚体的渗透率.结果表明:恒温条件下,具有一定渗透率的团聚体颗粒扩散得比硬球颗粒快.实验测量得到的团聚体渗透率与采用photoshop CS6对团聚体SEM图像进行处理计算得到的渗透率符合较好.     

基于单模光纤的DLS粒径测量研究

动态光散射技术是一种测量纳米颗粒粒径分布的最有效方法。为了克服高浓度样品溶液中存在的多重散射效应, 本文基于单模光纤搭建了一套DLS实验系统, 传输光纤的输出端与接收光纤的接收端都作了抛光磨平处理。在模拟复杂工业环境下, 分别用低浓度单分散、不同浓度单分散以及高浓度多分散性标准聚苯乙烯乳胶球悬浮液检测了该系统的适用性。实验结果表明, 利用该系统可快速准确的测量体积分数达40%的聚苯乙烯乳胶球悬浮液中的纳米颗粒粒径及其分布。     

基于后向散射的高浓度纳米颗粒粒度分布测量方法研究

传统的动态光散射法通常采集侧向散射进行纳米颗粒粒度分布的测量,由于多次散射的影响,利用侧向散射不能准确测量高浓度样品的颗粒粒度分布。针对该问题,对后向散射测量方法进行了研究,在实验基础上提出了后向散射最佳光程的判断准则。在不同样品浓度下,用侧向散射和后向散射方法对标称粒径分别为110 nm、220 nm的聚苯乙烯乳胶球颗粒进行了测量。实验结果表明,对于高浓度的待测样品,后向散射测量方法通过自适应调整光程,在最优光程处进行测量,能够有效得到高浓度纳米颗粒的粒径及粒度分布,测量结果相对误差为2.72%。     

基于Mie散射理论的颗粒粒度分布转换

使用动态光散射法可以获得颗粒的光强加权平均粒径,以及光强加权颗粒粒度分布。为获得数量或体积加权颗粒粒度分布,提出从光强分布到数量分布转换的直接比值法。该方法首先依据Mie散射理论求解不同粒径颗粒的散射光强,然后将光强分布与对应颗粒的散射光强进行比对,获得颗粒的数量分布,进而得到颗粒的体积分布。使用动态光散射法测量得到聚苯乙烯乳胶球混合样品的光强分布,利用直接比值法将光强分布转换为数量分布和体积分布,并与扫描电子显微镜测量的数量分布进行了对比,实验数据表明采用直接比值法能够获得准确的数量分布。     

拖曳效应对低相干动态光散射测量粒径的影响

低相干动态光散射技术利用低相干干涉计的特性,有效抑制了从浓悬浮液中散射的多次散射光,从而能够检测到的单散射光信号中获取颗粒的动态信息。该技术以单散射理论为解析基础,为避免多重散射的影响,测量区域一般局限于固-液界面附近。分析了固-液界面附近壁的拖曳效应对粒径测量值的影响。利用相位调制低相干动态光散射装置,对体积分数为10%的不同粒径的标准聚苯乙烯溶液进行了检测。通过对结果考虑拖曳效应进行修正,发现不同粒径的粒子在界面附近10～30μm范围内的测量值与给定粒径值标准偏差在5%以内。表明在低相干动态光散射光程可分割测量中,考虑拖曳效应的影响,可以对固-液界面附近的测量结果通过修正并得到准确的颗粒大小信息。     

动态光散射研究纳米级PBA/PMMA核壳颗粒的散射特性

运用动态光散射仪研究PBA(聚丙烯酸丁脂)为核,PMMA(聚甲基丙烯酸甲脂)为壳的核壳双层结构颗粒的角度散射光,并通过测量得到的粒径分布进行理论计算,结果表明:测量结果与理论计算结果总体趋势一致,但在前向散射和后向散射两者相差较大,主要由于动态光散射仪测量粒径分布时反演算法剔除占比例很小的大颗粒造成的.     

Measurement of optical constants for dense media by low-coherence dynamic light scattering

We perform the optical constants measurements for different absorption dense media by low-coherence dynamic light scattering (DLS) technique. The estimated particle size is used to calculate the scattering coefficient of particles suspended in dense media. The path-length resolved intensity distributions of light backscattered from the absorbing dense media are investigated experimentally by virtue of path-length resolved performance in low-coherence DLS measurements. The absorption coefficient can be obtained by applying the measured path-length resolved intensity distributions to the modified Lambert-Beer law. As a result, we proposed a new low-coherence DLS technique in simultaneous measurement of the scattering and absorption coefficients of absorbing dense media.     

Comparative Test of Methods to Determine Particle Size and Particle Size Distribution in the Submicron Range

Among the most important characteristic properties of disperse systems such as latices, pigments, ceramic materials or drug formulations are the particle size and the particle size distribution. To measure these quantities, several methods and measuring instruments based on different physical principles are available. These include turbidimetry, dynamic and static light scattering, electron microscopy with image analysis, ultra- and disc centrifugation, light diffraction and the electrical sensing zone method. All these measuring techniques are doubtless necessary because of the large product variety and the broad particle size range. However, some problems arise if different techniques are used and the results are compared uncritically without considering to the application range and the resolution of the methods. An extensive comparative test was therefore carried out using seven latices in the submicron range with defined monomodal, bimodal and hexamodal particle size distributions. The most important methods of determining average particle size values and particle size distributions were tested and compared. Of the methods to determine only average particle sizes, turbidimetry is the most efficient, followed by dynamic light scattering with cumulants evaluation. Static light scattering only yields accurate results for small particles with narrow particle size distributions. Of the methods to determine particle size distributions, ultracentrifugation and, somewhat less, disc centrifugation and electron microscopy with image analysis are the most efficient. Dynamic light scattering only yields reliable results in the case of small particles with narrow distribution curves. Light diffraction and the electrical sensing zone method are less suitable for the submicron range.     

Sizing Polydisperse Dispersions by Focused Beam Reflectance and Small Angle Static Light Scattering

In this work, two different methods for particle characterization, namely focused beam reflectance and small angle static light scattering, are quantitatively compared. The results are presented in the form of moment ratios of the particle size distribution, i.e., the number weighted diameter, D_1/0, and the volume weighted diameter, D_4/3, for a broad range of particle size distributions ranging from 20 to 400 μm. Various aqueous dispersions including narrow, broad, and bimodal particle size distributions of spherical shaped ceramic beads were used in the comparison. It was found that the moment ratios obtained by focused beam reflectance measurements and small angle static light scattering correlate well, in the case of spherical particles. Furthermore, it was found that the D_1/0 values obtained by focused beam reflectance measurements are more sensitive to the presence of a small fraction of fine particles in a bimodal distribution than those obtained by small angle static light scattering.     

双峰分布颗粒体系的多角度动态光散射数据反演

采用多角度动态光散射和加权正则化反演方法,对4组模拟的双峰分布颗粒体系(100/600 nm,200/600 nm,300/600 nm和350/600 nm)分别选取1、3、6和10个散射角进行测量.粒度反演结果表明,采用加权正则化方法反演双峰颗粒体系的多角度动态光散射测量数据,可获得峰值位置比小于2∶1且含有大粒径(＞350 nm)颗粒的双峰颗粒粒度分布.采用标准聚苯乙烯乳胶颗粒进行实测的结果验证了这一结论.得到含大粒径颗粒的双峰粒度分布反演结果的原因在于,多角度动态光散射能提供更多的大粒径颗粒的粒度信息,加权正则化反演方法能减少测量数据中的噪声,因而多角度动态光散射测量数据的加权反演能实现峰值位置比小于2∶1且含有大粒径颗粒的双峰颗粒体系的测量.     

A V-curve criterion for the parameter optimization of the Tikhonov regularization inversion algorithm for particle sizing

The regularization parameter plays an important role in applying the Tikhonov regularization method to recover the particle size distribution from dynamic light scattering experiments. The so-called V-curve, which is a plot of the product of the residual norm and the norm of the recovered distribution versus all valid regularization parameters, can be used to estimate the result of inversion. Numerical simulation demonstrated that the resultant V-curve can be applied to optimize the regularization parameter. The regularization parameter is optimized corresponding to the minimum value of the V-curve. Simulation and experimental results show that stable distributions can be retrieved using the Tikhonov regularization with optimum parameter for unimodal particle size distributions.     

Colloidal Analysis of Particles Extracted from Microalloyed Steels

Different colloidal particle characterization methods are examined for their suitability to determine the particle size distribution of particles extracted from steels. Microalloyed steels are dissolved to extract niobium and titanium carbonitride particles that are important for the mechanical properties of these steels. Such particles have sizes ranging from several nanometers to hundreds of nanometers depending on the precipitation stage during the thermomechanically controlled rolling process. The size distribution of the particles is analyzed by dynamic light scattering (DLS), analytical ultracentrifugation (AUC), and hollow fiber flow field-flow fractionation (HF5) and compared to data obtained for reference particles as well as data from electron microscopy, the standard sizing technique used in metallurgy today. AUC and HF5 provide high-quality size distributions, average over large particle numbers that enables statistical analysis, and yield useful insights for alloy design; however, DLS fails due to a lack of resolution. Important aspects in the conversion and comparison of size distributions obtained for broadly distributed particle systems with different measurement principles and the role of surfactants used in sample preparation are discussed.     

Appearance of an artifact peak in the particle size distribution measured by DLS at low concentrations

The dynamic light scattering (DLS) method allows the determination of the particle size distribution of suspensions. At high dilutions, an artifact peak appears in the size distribution, which does not correspond to actual particles, but is caused by crossing the scattering volume boundaries by individual particles. The parameters of this peak are analyzed, the causes of its appearance and its effect on determined particle sizes are studied.     

Laser induced incandescence measurements of soot volume fraction and effective particle size in a laminar co-annular non-premixed methane/air flame at pressures between 0.5–4.0 MPa

An auto-compensating laser-induced incandescence (AC-LII) technique was applied for the first time to measure soot volume fraction (SVF) and effective primary particle diameter (dp_eff) in a high pressure methane/air non-premixed flame. The measured dp_eff profiles had annular structures and radial symmetry, and the particle size increased with increasing pressure. LII-determined SVFs were lower than those measured by a line of sight attenuation (LOSA) technique. The LOSA measured soot volume fractions were corrected for light scattering using the Rayleigh–Debye–Gans polydisperse fractal aggregate (RDG-PFA) theory, the dp_eff data, and assumptions regarding the soot aggregate size distribution. The correction dramatically improved agreement between data obtained using these two measurement techniques. Qualitatively, soot volume distributions obtained using LII had more annular shapes than those obtained using LOSA. Nonetheless, it has been demonstrated that the AC-LII technique is very well suited for application in media where attenuation of the excitation laser pulse energy can exceed 45%. This paper also underlines the importance of correcting LOSA SVF measurements for light scattering in high pressure flames. PACS 07-60.-j; 47.70.Pq; 65.80.+n; 78.67.-n     

Fractal Character of Dynamic Light Scattering of Particles

Dynamic light scattering signals from particles, exhibit fractal characteristics. This feature can be used to determine the particle size. The use of the fractal dimension, as a quantitative method to analyze the properties of dynamic light scattering signals from submicron particles, is presented. The analysis is performed directly on the time‐resolved scattered intensity, and the Box Dimensions of light scattering signals of particles with diameters 100, 200, 500 and 1000 nm. The experimental results show that the fractal dimensions of light scattering signals correlate well with particle size. In the submicron size range, the smaller the particles, the larger their fractal dimensions. Compared with the PCS technique, only several hundreds of samples are required in the fractal method. Therefore, the data processing is easily accomplished. However, this method only provides the mean particle size, but not the particle size distribution.     

Application of the Model of Spheroidal Scatterers for Determination of Particles Sizes of Aqueous Suspensions by the Laser-Polarimetry and Dynamic-Light-Scattering Methods

Results of measurements of particle sizes of a dispersed medium by the methods of laser polarimetry and dynamic light scattering are presented for water suspensions of ZnO, CuO, TiO₂, and BaTiO₃ with particles of irregular shape. When using the laser-polarimetry method, the particle-size distributions within the framework of the spheroidal-scatterer model are reconstructed. The same model was used to correct data obtained by the method of dynamic light scattering. The data obtained are compared with results obtained by electron microscopy. It is shown that, at values of the size parameter of 2–5, correction of the results of measurements obtained by the dynamic-light-scattering method makes it possible to reduce the error in determining the average particle size by this method to no more than 11%.