High molecular weight polyethylene nanospheres: synthesis physical and mechanical properties

The high molecular weight (MW) polyethylene (PE) particles of particle size varied from macro to micron to nanometer were synthesized by Grignard reagent. The microscopy analysis (scanning electron microscope, SEM; transmission electron microscope, TEM; and atomic force microscope, AFM) shows the spherical shape of PE particles. The effects of particle size, varies from macro to nanometer scale on crystal structure, crystallinity (chic), glass transition temperature (Tg), melting temperature (Tm), surface roughness and mechanical properties were studied. Differential scanning calorimetry (DSC) experiments show that the nanoparticles of PE are highly crystalline (chic approximately equal 72%). The crystal length of PE nanoparticles is found to be approximately 14 A. Although the Gibbs-Thomson equation is explained the depression of melting temperature (DeltaTm) by 5 degrees C, the impervious results of Tg are still not fully understood. The low roughness value (2 A) proves the presence of "atomic-scale-chain" folding at the surface of PE nanoparticles. A novel protocol is developed, and the elastic modulus of individual nanospherical PE particles is computed from 'force-distance' mapping curves of AFM. Hemispherical tungsten (W) tip was fabricated from focused ion beam and used as an indenter to measure the mechanical properties. It is found that the nano sized PE particles have higher elastic modulus (E = 1.2-1.4 GPa) compared to the bulk or macro sized PE (E = 0.6-0.7 GPa). The results corroborate the robustness of our experiments, since, the analogous results for macro sized particles match well with the literature.     

Particle size induced heterogeneity in compacted powders: Effect of large particles

We investigated the effect of particle size distribution on heterogeneity of compacted powders. We used experiments and discrete particle based simulations to compact powders, test the mechanical strength of the compact, and study the microstructure of the compact. A metallic powder which has a wide particle size distribution was used in the experiments. We found that the compaction profile is not reproducible when particles larger than 1/6 of the die diameter are present in the powder sample. The presence of these large particles generate a highly heterogeneous inter-particle contact and bonding forces. The discrete particle simulations showed that for these heterogeneous compacts the tensile strength exhibits high variability, even for one compact if the diametrical compression force is applied along different axes. Based on these results, it is recommend that the largest particle in a powder compact should not exceed one sixth of the die diameter, which is the same as the recommendation of ASTM International D4767 - 11 for compression test of cohesive soils.     

Model filled rubber IV: Dependence of stress-strain relationship on filler particle morphology

The addition of monodisperse size crosslinked polystyrene (PS) particles, synthesized by emulsifier-free emulsion polymerization, to polysulfide matrix enhanced mechanical properties of the cured rubbery composites. The modulus, fracture strength, and elongation at break increased with increasing filler volume fraction up to 30 wt % PS particles. The strength and elongation at break decreased with increasing particle diameter from 0.315 to 1.25 m. The strength at break increased, but the extension decreased, as the particle crosslink density increased from 0 to 5 mol % DVB. Interparticle interactions are dominant and lead to the formation of clusters which form a network structure in PS particle filled composites. Since the number density, as well as the total surface area, of particles increase with decreasing particle diameter, interparticle attractions are enhanced, the tendency for cluster formation increased with decreasing particle size from 1.25 to 0.315 m. As particle crosslink density was reduced, the porosity and surface roughness of particles increased. Then, the dispersion of particles in the matrix was enhanced and particle agglomeration reduced but more polymer matrix was adsorbed on the particles. These particles or clusters act as physical crosslinks, resulting in an increased total effective crosslink density in the filled composites.     

SEPARATION AND BEHAVIOR OF NONSPHERICAL PARTICLES IN SEDIMENTATION/STERIC FIELD-FLOW FRACTIONATION

Sedimentation/steric field-flow fractionation (Sd/StFFF) is an elution separation technique capable of measuring the size distribution of 0.3-100 µm spherical and near-spherical particles with advantages including high resolution, fast analysis, and the ready collection of narrow size fractions. In this study we investigate the applicability of Sd/StFFF to various nonspherical particles including the doublets of spheres, rod-shaped glass fibers, compressed latex discs, and quartz particles (BCR 67 and 70) with complex mixed shapes. Some fractionation, retention, and selectivity features of these particles are defined and measured in relationship to those of spheres (latex beads), which are better understood. While the relative behavior of these two particle types depends on many factors, especially the distance of the particle from the Sd/StFFF channel wall, in most cases the nonspherical particles are eluted before spheres of equal volume and they often display higher selectivity than spherical particles. However, when retention of nonspherical particles is compared with that for spheres whose diameter is equal to the particle length, elongated particles (doublets and rods) eluted after the sphere while flattened particles (discs) eluted earlier than spheres, an observation that might assist in shape discrimination by Sd/StFFF. Thus, when latex microspheres are used for calibration to obtain size distribution curves, the diameter obtained for any given subpopulation will be less than the length of rods but greater than the diameter of discs. For complex particles such as the quartz particles, the diameter of a particle provided by classical sedimentation using spherical calibration is less than the equivalent spherical diameter of the particle in question whereas Sd/StFFF yields a diameter somewhat greater than the particle length. Thus, these two techniques will yield size distribution curves displaced from one another along the diameter axis. The difference in diameters can be eliminated by using a diameter correction factor of 2.7, which brings the distribution curves for quartz obtained by these two techniques into concurrence.     

Effects of mixing ratio and order of admixed particles with two diameters on improvement of compacted packing fraction

To improve particle flowability, a technique is used in which fine particles are admixed with the main particles. However, the effects of coating structure on the improvement in flowability are not yet fully understood. Thus, predicting the improvement resulting from this technique is difficult. In this study, we focused on the effects of the particle diameter distribution of the admixed particles on coating structures and improvement of flowability in terms of the compacted packing fraction in a particle bed. Main particles of size 397 nm with admixed particles of sizes 8 and 104 nm were used. Bimodal particle diameter distributions were adjusted by changing the mixing ratios of the two admixed particles. Furthermore, the main and admixed particles were mixed in various orders. We examined the compacted packing fractions for these different mixing ratios and orders. Scanning electron microscopy images were obtained in order to analyze the coating structures on the main particle surfaces. The results show that the main particle packing fraction was most greatly improved by pre-mixing the two admixed particles. This can be explained by a linked rigid-3-bodies model with leverage based on increasing the apparent diameter of the main particles.     

Effect of particle size on densification of pure magnesium during spark plasma sintering

The effect of particles size ranges (<38 μm, 75–150 μm, 270–550 μm) of atomized magnesium powders on densification mechanisms during spark plasma sintering (SPS) process was investigated. The intrinsic driving force, local pressure and current of Mg powders with different particle sizes were analyzed by theoretical calculation. The results obviously indicate that the densification of pure magnesium can be improved by the reduction of particle size, suggesting the intrinsic driving force, local pressure and current intensity are enhanced significantly by a decrease in the particle size at the same sintering conditions, which can promote shrinkage of pores, formation of the sintering neck and mass transportation in the SPS process. Not only that, rapid densification is also interpreted in term of mechanical movement of particles, Joule heating effect and plastic deformation. However, the mechanical movement of the large particles is higher than that of small particles due to high punch displacement, and plastic deformation, detected by scanning electron microscopy, plays a main role in densification for large particles in the case during the sintering. Joule heating effect is the key factor for densification of small Mg particles, and high densification degree can be obtained by sintering small particles.     

Micronization of dihydroartemisinin by rapid expansion of supercritical solutions

The purpose of this study was to prepare fine particles of antimalarial drug dihydroartemisinin (DHA) by rapid expansion of supercritical solutions (RESS) using carbon dioxide as supercritical fluid. The mechanical grinding by jet mill and additional vibration rod mill also was performed as a comparative method. In the RESS process, drug particles were prepared by varying processing conditions, including extraction condition, pre-expansion condition, nozzle diameter, nozzle temperature, and collecting distance. Particle size and morphology and physicochemical characteristics of the drug particles were investigated. The RESS process could produce the smaller drug particles (about 1-2 microm) when compared to mechanical grinding method (about 7 microm). All RESS processing parameters had an effect on size and morphology of drug particles. The particle size of drug was related to the solubility of drug in supercritical CO(2) at each processing condition. The fine particles of DHA (about 1 microm) with narrow size distribution could be obtained at extraction pressure of 18 MPa and extraction temperature of 32 degrees C, which was closed to the critical temperature of supercritical CO(2) whereas broad size distribution was obtained at extraction temperature of 60 degrees C. Powder X-ray diffraction study indicated that the RESS-processed particles were in crystalline form. The results revealed that RESS process is applicable for micronization of DHA.     

Thermal degradation kinetics and estimation of lifetime of polyethylene particles: Effects of particle size

The thermal stability and degradation behavior of polyethylene (PE) particles having a diameter varies from few nanometers to micrometers were studied by thermogravimetric analysis (TGA). The PE particles of average diameter ～20, ～10, ～1 μm and <500 nm were studied over a range of temperatures from 25 to 600 °C in N₂ atmosphere and heating rates of 5, 10 and 15 °C min^?1. The three single heating-rate techniques such as Friedman, Freeman–Carroll, and second Kissinger; and three multiple heating-rate techniques such as the first Kissinger, Kim–Park and Flynn–Wall were used to work out the kinetic parameters of the degradation reactions, e.g., activation energy (E_a), order of reaction (n) and frequency factor [ln(Z)]. The lifetime of macro, micro and nanosized PE particles were also estimated by a method proposed by Toop. It was found that the activation energy and lifetime of nanosized PE nanoparticles were moderately high compared to the micron sized PE particles. Moreover, the decomposition temperature, order of reaction (n), frequency factor [ln(Z)] do not only depend on heating rates and calculation techniques, but also on particle size of the PE. The results obtained from the kinetic and lifetime studies for nano and micro sized particles were compared with macro sized PE.     

Theoretical calculation of uncertainty region for spherical particles based on a picket fence,quasi-monodisperse particles

In order to confirm the reliability of particle size measurement technique and to prepare standard reference particles for calibrating particle size measurement devices, experimental and theoretical studies have been conducted about the uncertainty region of particle size measurement for the picket fence and quasi mono-disperse particles. The vertical and horizontal uncertainty regions based on Tschebyscheff theory are calculated to the picket fence distribution composed of two kinds of nearly mono-disperse particles. The uncertainty region increases around the intermediate particle diameters between the two kinds of particles.Because the original particle size distribution is nearly mono-disperse, the uncertainty regions around the minimum and maximum particle diameter are small compared to the intermediate particle diameters between the two kinds of particles.The uncertainty region in vertical and horizontal direction changes to decrease with the increase of sample size. For the picket fence distribution composed of two kinds of nearly mono-disperse particles, the sample size about more than 10,000 is necessary to obtain the reliable results in particle size counting process.     

Micronization of Dihydroartemisinin by Rapid Expansion of Supercritical Solutions

The purpose of this study was to prepare fine particles of antimalarial drug dihydroartemisinin (DHA) by rapid expansion of supercritical solutions (RESS) using carbon dioxide as supercritical fluid. The mechanical grinding by jet mill and additional vibration rod mill also was performed as a comparative method. In the RESS process, drug particles were prepared by varying processing conditions, including extraction condition, pre-expansion condition, nozzle diameter, nozzle temperature, and collecting distance. Particle size and morphology and physicochemical characteristics of the drug particles were investigated. The RESS process could produce the smaller drug particles (about 1–2 μm) when compared to mechanical grinding method (about 7 μm). All RESS processing parameters had an effect on size and morphology of drug particles. The particle size of drug was related to the solubility of drug in supercritical CO₂ at each processing condition. The fine particles of DHA (about 1 μm) with narrow size distribution could be obtained at extraction pressure of 18 MPa and extraction temperature of 32°C, which was closed to the critical temperature of supercritical CO₂ whereas broad size distribution was obtained at extraction temperature of 60°C. Powder X-ray diffraction study indicated that the RESS-processed particles were in crystalline form. The results revealed that RESS process is applicable for micronization of DHA.     

Particle Characteristics and Analysis Using a Laser-Based Phase Doppler Particle Analyzer (PDPA) and Statistical Method

Particle characterization is an important component in product research and development, manufacturing, and quality control of particulate materials. In this study a laser-based phase Doppler particle analyzer (PDPA) was used to measure particle size and velocity. Two different particles including humid particles and fog particles were tested using the PDPA. Several tests were conducted under different conditions and all data were analyzed using the statistical method and analysis of variance (ANOVA) to see which factor affects particle performance. The humid particle flow rate has a significant effect on both the particle mean diameter and the particle mean velocity with 90% confidence. The type of oil particles has a significant effect on the particle mean velocity with 90% confidence.     

激光粒度法测试结果与库尔特法、沉降法的比较

分别采用马尔文激光粒度仪、库尔特颗粒粒度计数仪、岛津离心粒度分析仪对玻璃微珠、聚苯乙烯微球、钨粉、氧化铝微粉、二氧化硅微粉等6种不同类型的粉末进行了测试,并对几种测试方法所得的结果进行比较。结果表明:激光法测试的结果重复性较好;对于粒径范围窄的球形粉体,几种仪器测得的中位径具有可比性,粒度分布曲线也相似;对于粒径范围较宽的球形粉体和不规则形状粉体,测得的中位径和粒度分布曲线一般没有可比性。     

Theoretical calculation of uncertainty region based on the general size distribution in the preparation of standard reference particles for particle size measurement

In order to confirm the reliability of particle size measurement technique and to prepare standard reference particles for calibrating particle size measurement devices, experimental and theoretical studies have been conducted about the uncertainty region of particle size measurement for the general particle size distribution. A new theoretical equation to calculate fundamental uncertainty region in the case that the maximum and minimum particle sizes are known, is derived based on Tschebyscheff theory. The uncertainty regions calculated based on the proposed method are applied to poly-disperse particles and a picket-fence distribution composed of two kinds of nearly mono-disperse particles.For the poly-disperse particles, the uncertainty region increases with the increase in particle diameter. For the picket-fence distribution composed of two kinds of nearly mono-disperse particles, the uncertainty region increases around the intermediate particle diameters between the two kinds of particles.Numerical simulation of uncertainty region for the picket-fence distribution has also been carried out. The uncertainty region decreases with the increase in sample size or the decrease in geometric standard deviation.     

基于TEM图像的炭黑在聚合物基体中分散性的定量表征

采用熔融共混-母粒稀释技术并辅以高效动态混合器制备了聚丙烯/炭黑薄膜.基于TEM图像定性和定量表征了炭黑在其中的分散与分布.首次将Image J图像分析软件引入分析过程,获取了粒子数目、粒子表面密度、平均粒径及其分布等统计数据.结果表明,粒子平均直径为0.2μm,当量直径服从多峰非正态分布.Origin拟合结果表明,粒...     

湿法超细研磨中白云石机械力化学效应

通过对不同累积研磨时间白云石样品的粒度、浆料中离子浓度和物相分析,研究湿法研磨时白云石的机械力化学效应。结果表明:白云石在湿法超细研磨时,颗粒粒度随着研磨时间的延长而显著地减小;浆料中Mg2+和Ca2+的浓度则先是显著增大后趋于平稳增大,表明白云石超细粉碎过程可以使碳酸镁和碳酸钙在溶液中溶解度有所增大,直至达到溶解和结晶动态平衡;晶体的显微应变和晶粒尺寸都随着研磨时间的延长而先减小后增大,说明在湿法研磨的过程中,由于机械力的作用使得白云石的晶体发生了畸变。     

Particle Characteristics and Analysis Using the Laser-Based Phase Doppler Particle Analyzer (PDPA) and Statistical Method

Particle characterization is an important component in product research and development, manufacturing, and quality control of particulate materials. In this article a laser-based phase Doppler particle analyzer (PDPA) was used to measure particle size and velocity. Two different particles, humid particles and fog particles, were tested using the PDPA. Several tests were conducted under different conditions and all data were analyzed using the statistical method and analysis of variance (ANOVA) to see which factor affects particle performance. The humid particle flow rate has a significant effect on both the particle mean diameter and the particle mean velocity with 90% confidence. The type of oil particle has a significant effect on the particle mean velocity with 90% confidence.     

Effect of particle size ratio and contribution of particle size fractions on micromechanics of uniaxially compressed binary sphere mixtures

This paper is an extension of the recent work of Wi?cek (Granul Matter 18:42, 2016), wherein geometrical parameters of binary granular mixtures with various particle size ratio and contribution of the particle size fractions were investigated. In this study, a micromechanics of binary mixtures with various ratio of the diameter of small and large spheres and contribution of small particles was analyzed using discrete element simulations of confined uniaxial compression. The study addressed contact normal orientation distributions, global and partial contact force distributions and pressure distribution in packings of frictional spheres. Additionally, the effect of particle size ratio and contribution of particle size fractions on energy dissipation in granular mixtures was investigated. The particle size ratio in binary packings was chosen to prevent small particles from percolating through bedding. The bimodality of mixtures was found to have a strong effect on distribution of contact normal orientation and distribution of normal contact forces in binary mixtures. Stress transfer in binary packing was also determined by both, particle size ratio and volume fraction of small particles. Dissipation of energy was higher in mixtures with higher particle size ratios and decreased with increasing contribution of small spheres in system.     

Verbesserung des Verschleißverhaltens von Al-Werkstoffen

Improvement of Wear Resistance of Al-materials Wear behaviour of ductile materials can be improved by embedding suitable hard particles of appropriate size. With the Al materials tested here, embedding was achieved by extrusion of the powder mixtures. Wear resistance of the materials thus produced was determined using pin-disc and Klüber testers, commercially available fine grinding discs being used as abrasive partners. Thus, the effect of various parameters on wear behaviour and mechanical strength could be investigated. The mechanical properties are generally deteriorated by embedding hard particles, the amount of embedded material being of primary importance, but there is also a profound influence of the matrix-particle interface strength and, to a lesser degree, of particle size and shape. With regard to the wear resistance, the hard particles result in the desired improvement which is the more pronounced the higher the particle content and hardness. Even at low interface strength the particles are not torn of the matrix during wear stress. At lower matrix hardness (plain Al, Al alloys) better wear resistance is observed, as the abraded particles are more effectively rembedded and thus protect the matrix from wear. If suitable materials are used, excellent wear resistance combined with only insignificantly lowered mechanical strength is obtained.     

Synthesis of crosslinked poly(styrene-<Emphasis Type="Italic">co</Emphasis>-divinylbenzene-<Emphasis Type="Italic">co</Emphasis>-sulfopropyl methacrylate) nanoparticles by emulsion polymerization: Tuning the particle size and surface charge density

We have synthesized highly charged, crosslinked poly (styrene-co-divinylbenzene-co-sulfopropyl methacrylate) copolymer colloidal particles using emulsion polymerization. The effects of concentration of the emulsifier and the initiator on the particle size and the charge density of the colloidal particles are studied. Colloidal particle size is highly dependent upon the concentration of the emulsifier and the initiator. The colloidal particle diameter decreases with increasing concentration of the emulsifier and increases with increasing concentration of the initiator in the polymerization mixture. Number of particles, surface charge density and charges per particle are also functions of both the emulsifier and the initiator concentration. The surface charge density and the number of charges per sphere increase with increasing particle diameter. These copolymer colloid particles self assemble readily and diffract visible light. Polymer hydrogel imbibed with these colloids shows the light diffraction.     

钛酸钡陶瓷电容机械性能的尺寸效应

以粉体粒径为0．3pm～0．7pm的BaTiO3粉体为原料．采用传统陶瓷工艺,研究了微粉尺寸对钛酸钡陶瓷机械性能的影响,从粉体形貌、晶粒形貌、相结构、微观结构、应力变化及最终的机械性能改变等方面分析了纯BaTiO3陶瓷的晶粒尺寸效应。实验中发现,晶粒较小时,陶瓷断裂所需要破坏的晶粒多,由于晶界所占比例大,陶瓷断裂走过的路程长．强内应力为陶瓷结构稳定提供支撑,因此机械强度提高。