An experimental investigation of particle size analysis by a modified andreasen pipet

The Andreasen pipet is very commonly used for particle size analysis; however, due to its improper method of vertical sampling, a powder sample with a logarithmic-normal distribution cannot be reproduced by the pipet method. The induced error is rather serious, particularly for the range of smaller particles.Instead of vertical sampling, the present experiment introduces the modification of a stem of tubing extending from the bottom of the vessel to form a sampling slot. Two powder samples are tested and analysis by a micron photo sizer is chosen as the standard for comparison. The results show that powder samples with logarithmic-normal distributions are very well reproduced, and the analysis by the modified pipet is almost as good as that by the photo sizer.     

Design and Characterization of a Fluidized Bed Aerosol Generator: A Source for Dry,Submicrometer Aerosol

A fluidized bed aerosol generator has been designed and built for the purpose of generating a constant output of dry, submicrometer particles with a large number density. The output of the fluidized bed for generating aerosol particles from dry soot powder has been characterized using a differential mobility analyzer and a condensation particle counter. The particle size distribution is bimodal, with a mode in the submicrometer diameter size range and a mode in the supermicrometer diameter size range. The larger diameter mode is fully separated from the smaller mode and can thus be easily removed from the aerosol flow using impaction techniques. The distribution in the submicrometer size range is nearly log-normal, with a count median diameter falling between 0.1 and 0.3 micrometers. A number density of greater than 10⁵ particles cm^-3 of soot particles in the submicrometer range can be produced, constant to within 25% (1 standard deviation) over a 4 h time period. The number density of particles produced in the submicrometer range was found to vary with the ratio of soot to bronze beads in the bed mixture, whether or not a feed system was used, and nitrogen flow rate through the fluidized bed and feed system.     

Preparation of natural microcrystalline graphite with high sphericity and narrow size distribution

Natural microcrystalline graphite with high sphericity and narrow size distribution was prepared by powder engineering methods. The shape of microcrystalline graphite (MCG) particles was modified using a wet agitating method and then the particles were separated into groups with narrow size distribution by means of gravity settling and hydrocyclone combined. Several methods such as scanning electron microscope (SEM), Raman spectroscopy and X-ray diffraction (XRD) were employed to investigate the structure of the sample. The result showed that the present method was effective in classifying the MCG particles into a narrow size range. Galvanostatic cycling was used to investigate the electrochemical performance of the as-prepared MCG as the anode material of lithium ion cells. Compared with raw MCG, the modified MCG shows a large improvement in reversible capacity, though the cycleability is slightly reduced.     

Spherical particles for automotive powder coatings

Clear powder coatings that consist of spherical particles with a narrow particle size distribution were produced via a suspension method that involves the agglomeration and unification of smaller particles. These powder coatings have the advantages of excellent powder flowability and high transfer efficiency. This behavior is attributable to the spherical particle shape and absence of finer particles. This production method has been developed for thinner film build clear coats with improved surface smoothness as compared to powder coatings produced by conventional methods.     

原位生成纳米SiO2及其作为填料对聚氨酯硬质泡沫塑料性能的影响

通过选择适当的乳化剂和水解温度以及控制水对于乳化剂的摩尔比,采用油包水微乳液法在聚醚多元醇中原位合成了纳米SiO2,然后该聚醚多元醇进一步与TDI反应制备出聚氨酯硬质泡沫塑料。TEM照片显示原位合成的SiO2微粒呈球状且分散,粒径分布在50nm-70nm。该聚氨酯硬质泡沫塑料的吸水率,随着SiO2填加量的增加,先升高随后又降低。因为原位生成纳米SiO2的加入,聚氨酯硬质泡沫塑料的拉伸强度得到显著提高,冲击强度缓慢增大,而对于压缩强度则先轻微降低,一直到SiO2的含量为0.9wt%时才开始急剧增大。     

Effect of process conditions on spray dried calcium carbonate powders for thermal spraying

Powder preparation is an important stage in the production of thermal spray coatings with the desired characteristics. An important powder feature is flowability, which can be adjusted through particle morphology, particle size and size distribution. Combined, these features dictate the quality of the coating produced. To increase a powder's flowability, spherical particles within a particular size range are ideal. One way to achieve this is through spray drying. The aim of the present study was to investigate the effect of spray drying process parameters on the physical properties of calcium carbonate powder, with the goal of producing large, spherical particles ranging between 50 and 100 μm in preparation for thermal spray experiments. A key aspect was the use of ethanol to aide in the production of large spheres. A 2³ factorial design of experiments (DoE) was utilised to study the following process parameters: gas flow rate, feed flow rate and solids loading. The resulting powders were characterised in terms of particle size, morphology and production yield. Porous, hollow, spherical particles were produced in a suitable size range for thermal spraying, which was attributed to the rapid evaporation of ethanol. Statistical analysis was utilised to interpret trends between the spray drying parameters and powder characteristics quantitatively.     

矿渣微粉粒度分布对水泥性能的影响

利用灰色关联分析方法,研究了矿渣微粉的粒度分布对矿渣水泥性能的影响。研究结果表明:0~5μm、5~11μm的矿渣微粉颗粒分别对3 d、28 d强度有显著影响;0~23μm的矿渣粉颗粒对3 d,28 d强度起增进作用;水泥强度随23μm的矿渣微粉颗粒含量增大而降低。因此,可以通过优化矿渣微粉的粒度分布来改善水泥性能。     

催化裂化油浆固含量测定及组成分析

采用灰分法、过滤法、离心法测量了某重油催化裂化装置外甩油浆的固体颗粒含量,对几种方法在固含量测定方面的结果差异进行对比分析。实验结果表明,离心法测量的固含量约为2850μg/g,介于灰分法和过滤法之间。离心法结果显示,油浆中重组分与细粉颗粒存在较强的吸附作用,分离中能否准确得到焦粉是造成结果差异的主要原因。离心法耦合后续焙烧能够分离获得油浆中一定量的催化剂细粉颗粒,通过激光粒度仪、元素分析仪、XRD、BET、SEM-EDS等手段对分离得到的固体颗粒以及初始FCC催化剂进行了表征。FCC催化剂粒径集中在32～120μm之间,为规则的球形分布,油浆中的固体颗粒呈不规则的块状分布,粒径在0.4～40μm之间,其中催化剂细粉的粒径在1～30μm之间;催化裂化油浆中的固体颗粒组成主要有催化剂细粉、焦粉和碱金属K、Ca、无机盐和金属元素Sb、Fe等。     

二氧化硅种子在硅溶胶粒径增长中的行为研究

文章描述了粒子在利用单质硅粉制备硅溶胶反应中的一般生长过程,分析表明采用种子生长法制备可控粒径的硅溶胶,其关键是通过反应条件的控制促使种子生长并抑制次生粒子的形成,通过次生粒子的定量计算可反映出体系的粒径分布情况。实验发现当二氧化硅种子浓度为1．5wt％时对硅溶胶粒径增长最为有利。同时利用水溶液中二氧化硅粒子的核／壳模型对种子生长过程的行为做出了合理解释。     

Preparation of Monodisperse and Spherical Zirconia Powders by Heating of Alcohol–Aqueous Salt Solutions

A novel method is demonstrated which yields a spherical ZrO₂ powder of narrow size distribution through heating of a zirconyl chloride solution with an alcohol–water mixture as the solvent. The kind and composition of the solvent mixture greatly influenced the behavior of the precipitation and the morphology of the resulting particles. When 1-propanol or 2-propanol was employed as the alcohol of the solvent mixture, the resulting particles had a spherical shape and a narrow size distribution. The particle size and the particle agglomeration level could be controlled by the amount of hydroxypropyl cellulose (HPC) in the solution. As-prepared amorphous powder was crystallized to a mixture of metastable tetragonal phase and monoclinic phase at about 460°C. The metastable tetragonal phase was converted to the monoclinic phase as the calcination temperature was increased. After calcination, the spherical shape of the zirconia powder was retained, while its particle size was decreased slightly.     

Foam granulation: Binder dispersion and nucleation in mixer-granulators

Traditional wet granulation method involves spraying of liquid binder onto a moving powder bed to granulate the powder particles in the granulator. A new alternative method of wet granulation has been developed where foam delivery of binder is used to granulate the powder particles.This study investigated binder distribution in wet granulation and focused on the nucleation stage, where nuclei are formed during the initial binder distribution. Nucleation experiments were used to study the formation of nuclei by the foam and spray delivery methods in a high shear mixer-granulator. The distribution of foams on a dynamic powder bed were also investigated by filming small portion of foams as they penetrated into moving powder beds under different powder flow conditions in a high shear mixer-granulator.Nucleation experiments in this study show that foam delivery tends to create a narrower nuclei size distribution during the early stage of wet granulation process compared to spray delivery at the same processing conditions, demonstrating the potential of foam granulation in achieving improved binder distribution. For foam delivery, the nuclei formation is influenced by the foam properties and powder flow conditions in the granulator. The experiments show that the narrowest nuclei size distribution is obtained by granulating with high-quality foam and intensive powder mixing conditions. Coarser nuclei are formed when low-quality foam is dispersed in a less intensively agitated powder. The interactions of foam quality and the powder flow pattern are discussed and two distinct wetting and nucleation mechanisms are proposed: (1) under bumping flow, a low-quality foam tends to induce localised wetting and nucleation. The wetting and nucleation is “foam drainage” controlled. (2) Under roping flow, foam will be dispersed by the motion of the agitated powder. The wetting and nucleation is “mechanical dispersion” controlled.     

细粉粉末涂料流动性能的表征研究

为了更好地解决细粉及超细粉末涂料颗粒在加工、气流输送、喷涂等工艺中遇到的问题,本文对影响细粉粉末涂料流动性能的各粒径参数进行了实验研究和回归分析。研究发现:工业上通常应用中粒径(D50)来表征细粉涂料流动性并不够准确。通过对不同特征粒径以及粒径分布跨度等因素的考察,本文提出了一种由代表粒径大小和粒径分布的D10-D50-D90多变量关联模型来表征细粉粉末涂料流动性的方法,使细粉涂料流动性的预测更为可靠和准确,为细粉涂料特别是超细粉末涂料的工业应用提供理论指导。     

Measuring the particle shape mix in a powder with the cascadograph

Particle shape has been recognized as one of the important properties of the particles present in powders, particularly in the fluid-solid reaction system. The currently available technique of Fourier transformation to characterize particle shape is cumbersome and can be used only by a skilled operator. Recently developed, the sieve cascadograph is the first particle chromatograph that characterizes the shape of particles in the 0.1–1.0 mm size range. Working on the principle that the residence time of a particle on a sieve is a function of the particle shape, the cascadograph consists of a stack of sieves of identical size in a shaking device. A small monosized powder sample is placed in the topmost sieve, and shaking commenced. The weight of powder leaving the lowest sieve is measured as a function of time, and is used to produce a signature representative of the particle shape distribution in the powder sample. The sieve cascadograph is theoretically described and the results of preliminary experiments are presented.     

A novel approach to the preparation of powder coating—Manufacture of polyacrylate powder coatings via one step minisuspension polymerization

A novel method for manufacturing powder coating through one step minisuspension polymerization is described. The conventional production of powder coating includes six steps—synthesizing resins, mixing the raw material, extrusion, cooling, pre-crushing and pulverization. Comparatively, the present method can simplify the complicated processes, reduce equipment and save energy. Before polymerization, the TiO₂ particles were treated with a reactive silane coupling agent 3-methacryloxypropyltrimethoxysilane (MPTMS) to obtain enough compatibility with the monomers. The powder coating was directly synthesized through employing one step minisuspension polymerization in the presence of titanium dioxide white particles. The powder coating was characterized using Fourier transform infrared spectra (FT-IR) and thermogravimetric analysis (TGA). The results show that TiO₂ particles and polymer are successfully linked up via MPTMS in the powder particles. The morphology of powder coatings produced via different methods was observed by scanning electron microscope (SEM). The powder coatings obtained from minisuspension polymerization consist of regular spherical morphology particles with narrow particle size distribution. The powder flowability and surface film smoothness were enhanced compared to the pulverization powder coating.     

原位生成纳米SiO2填料对RPU性能的影响

通过控制水解温度和乳化剂的加入量,采用油包水微乳液法在聚醚多元醇中原位合成了纳米SiO2,聚醚多元醇进一步与TDI反应制备聚氨酯硬质泡沫塑料。TEM照片显示原位合成的SiO2微粒呈球状且分散,粒径范围在50～70nm。该聚氨酯硬质泡沫塑料的吸水率随着SiO2添加量的增加,先升高随后又降低。因为原位生成纳米SiO2的加入,聚氨酯硬质泡沫塑料的拉伸强度得到显著提高,冲击强度缓慢增大,而对于压缩强度则先轻微降低,一直到SiO2质量分数为1.1％时才开始急剧增大。     

A Shock and Expansion Wave-driven Powder Disperser

The paper describes a method for dispersing small (micro- and milligram) quantities of dry powder using a shock and expansion wave technique. The batch-wise operating apparatus aerosolizes any particulate matter with primary particles down to the submicrometer size range. Depending on the initial pressure situation and on the powder mass to be dispersed, the degree of dispersion or the fraction of agglomerates can be adjusted in a wide range. For calibration purposes monodisperse aerosols can also be generated employing monosized powders. The operating characteristics of the device are presented.     

原位生成纳米SiO2及其作为填料对聚氨酯硬质泡沫塑料性能的影响

通过选择适当的乳化剂和水解温度以及控制水对于乳化剂的摩尔比,采用油包水微乳液法在聚醚多元醇中原位合成了纳米SiO2,该聚醚多元醇进一步与TDI反应制备出聚氨酯硬质泡沫塑料.TEM显示原位合成的SiO2微粒呈球状且分散,粒径为50～70nm.随着SiO2填加量的增加,该聚氨酯硬质泡沫塑料的吸水率先升后降.因为原位生成纳米SiO2的加入,聚氨酯硬质泡沫塑料的拉伸强度得到显著提高,冲击强度缓慢增大,而压缩强度则先轻微降低,一直到SiO2的含量为0.9wt%时才开始急剧增大.     

Synthesis of nano-sized gadolinia doped ceria powder by aerosol flame deposition

In this work, aerosol flame deposition method was applied to deposit spherical and dense gadolinia-doped ceria (GDC) particles in the sub-micron range for the electrolyte application in solid oxide fuel cell. The particle size distribution was dependent on processing parameters such as the concentration of the precursor solution, the hydrogen gas flow rate, the oxygen gas flow rate, and flame conditions. GDC electrolyte thin layer was also fabricated from the liquid source materials by AFD method. Microstructure of synthesized powder was characterized using XRD and SEM.     

利用酸性CuCl2蚀刻废液制备微米级Cu2O粉体

以含CuCl2酸性蚀刻废液为原料,葡萄糖为还原剂,采用液相还原法制备分散性好的微米级Cu2O粉. 实验确定最佳制备条件为：反应温度80℃,终点pH值8~9,反应时间1 h,还原剂和铜离子摩尔比为0.8. 所制Cu2O产品纯度为99.34%,Cu回收率可达99.7%. 进一步采用XRD, SEM, LZS, TG等手段对产物进行表征,结果表明产品为高纯Cu2O,粒径为1.8~2.2 mm,空心多面体结构,且常温下抗氧化性好,有可能用于催化剂、涂料、染料等的制备.     

超临界流体技术在粉体粒子制备中的应用

超临界流体技术是制备和控制粉体材料的一种有效手段,利用该技术所获得微粒的平均粒径小,粒子尺寸分布可控。简述了超临界流体技术制备粉体粒子的基本原理、发展历史以及取得的一些研究成果,为超临界流体技术的应用拓展了领域。