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.     

Discrete element modelling of one-dimensional compression of cemented sand

It has recently been shown that the one-dimensional normal compression of sand can be modelled effectively in three-dimensions using the discrete element method, and that the slope of the compression curve (in log voids ratio–log stress space) is controlled by the size effect on average particle strength. This paper incorporates soil structure by simulating cemented sand, and the effects of inter-particle bonding (including bond strength and strength distributions) on the one-dimensional compression behaviour and evolving particle size distributions are investigated. The results show that bonding reduces particle crushing, and it is both the magnitude and distribution of bond strengths that influence the compression curve of the structured material.     

Influence of drug load on dissolution behavior of tablets containing a poorly water-soluble drug: estimation of the percolation threshold

Drug load plays an important role in the development of solid dosage forms, since it can significantly influence both processability and final product properties. The percolation threshold of the active pharmaceutical ingredient (API) corresponds to a critical concentration, above which an abrupt change in drug product characteristics can occur. The objective of this study was to identify the percolation threshold of a poorly water-soluble drug with regard to the dissolution behavior from immediate release tablets. The influence of the API particle size on the percolation threshold was also studied. Formulations with increasing drug loads were manufactured via roll compaction using constant process parameters and subsequent tableting. Drug dissolution was investigated in biorelevant medium. The percolation threshold was estimated via a model dependent and a model independent method based on the dissolution data. The intragranular concentration of mefenamic acid had a significant effect on granules and tablet characteristics, such as particle size distribution, compactibility and tablet disintegration. Increasing the intragranular drug concentration of the tablets resulted in lower dissolution rates. A percolation threshold of approximately 20% v/v could be determined for both particle sizes of the API above which an abrupt decrease of the dissolution rate occurred. However, the increasing drug load had a more pronounced effect on dissolution rate of tablets containing the micronized API, which can be attributed to the high agglomeration tendency of micronized substances during manufacturing steps, such as roll compaction and tableting. Both methods that were applied for the estimation of percolation threshold provided comparable values.     

Ultrasonic Characterization of Iron Powder Metallurgy Compacts during and after Compaction

Ultrasonic measurements in powder metallurgy (PM) compacts at various stages of production are presented both as a practical means of improving PM production and as a method of providing a fuller understanding of PM materials. Ultrasonic monitoring during powder compaction, a novel process instrumentation technique to follow powder densification, is reviewed. Measurements taken during the compaction of simple PM disk demonstrate that the ultrasonic velocity can be used as a measure of the in situ density. This connection arises due to the acoustic equivalence between powder during compaction and PM compacts after sintering. Ultrasonic monitoring during compaction of a two-level PM part is demonstrated to be fully capable of independently following the density in each level. The results also provide evidence of different regimes of powder flow behaviour during compaction. Ultrasonic velocity mapping of the two-level compact after sintering provides confirmation of the monitoring results. Subsequently, measurements of the ultrasonic velocity in green PM compacts are shown to be consistent with a dependence on the quality of inter-particle bonding. Finally, laser ultrasonic measurements in PM compacts are used to determine the ultrasonic attenuation. Attenuation values in a sintered compact are shown to follow a simple Rayleigh scattering dependence on frequency which yields a powder particle size consistent with the known value.     

The effect of ultrasonic vibration on the compaction characteristics of ibuprofen

An ultrasonic (US) compaction rig has been developed, capable of providing compaction pressure together with high-power ultrasonic vibrations of 20 kHz to a powder or granular material in a die. The rig has been used to investigate the effect of ultrasound on the compaction properties of ibuprofen, a drug with poor compaction properties which produces tablets that are weak and frequently exhibit capping. It was found that coherent ibuprofen tablets could be prepared by ultrasound-assisted compaction at pressures as low as 20-30 MPa. Application of ultrasound before and after compaction was found not to be as effective as ultrasound applied during compaction. The breaking forces of the tablets produced with ultrasound applied during compaction were found to be consistently significantly higher than when compaction was performed conventionally, or with ultrasound applied before or after compaction. Application of ultrasound during compaction made it possible to increase tablet mechanical strength, typically by a factor of 2-5. It was concluded that pressure should be applied together with ultrasound in order to achieve a better acoustical contact, which is required to transmit vibrations from the horn to the material, and also to bond the surfaces of the particles.

Ultrasound application during ibuprofen compaction also resulted in an increase in the apparent density, in relation to the apparent density of conventionally prepared tablets, of up to 14.4%. Ultrasound appears to improve particle rearrangement and provides energy for partial melting of particle asperities and subsequent fusion of particle surfaces, so as to increase interparticulate bonding. Solid bridge formation was thought to result in a reduction of void space, which in turn reduced the rate of water penetration into the compacts and consequently increased disintegration and dissolution times.

It was found that the results of ultrasound-assisted compaction are influenced by formulation and US time. When ibuprofen was mixed with a second material, such as dibasic calcium phosphate dihydrate (DCP) or microcrystalline cellulose (MCC), stronger tablets were prepared by ultrasound-assisted compaction compared to the compacts containing no filler. Positive interactions were considered to have occurred due to ultrasound-induced bonding between the two materials. With an increase in DCP and MCC concentration in ibuprofen formulations, disintegration and drug dissolution rates of the tablets produced with ultrasound significantly increased.

Using temperature-sensitive labels it was found that thermal changes occurred in powdered solids undergoing ultrasound-assisted compaction. Increases in the temperature of tablets were related to US amplitude and US time. With an increase in US amplitude from 5 to 13 µm, the temperature of the DCP tablet surface increased from 40 to 99°C. With an increase in US time from 1 to 5 sec, the temperature of the surface of ibuprofen tablets increased from 43 to 60°C. Increased tablet temperature was thought to be due to ultrasonic energy dissipation turned into heat.

X-ray powder diffraction (XRD) studies of ibuprofen tablets prepared by ultrasound-assisted compaction at 32 MPa revealed that no changes in chemical or/and crystalline structure of the material occurred when ultrasound was applied for up to 5 sec (US amplitude 7 µm). An XRD study of DCP tablets produced by ultrasound-assisted compaction at 32 MPa with ultrasound of different amplitudes (5, 7, 13 µm) applied for 2 sec indicated that no material deterioration occurred in all the tested samples.     

A study of compaction of composite particles by multi-particle finite element method

We study the compaction of composite mixture of soft and hard micro-/nano-size particles using multi-particle finite element method. In this method, each particle is fully discretized into finite element mesh. Local non-uniform contact deformation and non-uniformity stress chains transmitted through the composite are well illustrated. In this work, we focus on the effect of inter-particle friction and volume fraction of hard particles on compaction pressure. Results of closed die compaction of 400 two-dimensional monosize spherical particles of zero and 40% volume fraction hard particles are presented. The results show that compaction pressure increases with inter-particle friction and volume fraction of hard particles. The predicted compaction pressure curves are in good agreement with experimental data and other models.     

Microstructure evolution and densification behavior of TiC/316L composite powders during cold/warm die compaction and solid-state sintering: 3D particulate scale numerical modelling and experimental validation

To identify the microstructure evolution and densification behavior of TiC/316L composites in powder metallurgy (PM) process, 3D particulate scale numerical simulations were conducted to reproduce the cold/warm compaction and solid-state sintering of TiC/316L composite powders with corresponding physical experiments being carried out for model validation. The effects of compaction parameters and sintering temperature on the densification behavior of TiC/316L composite powders were systemically investigated. The particle deformation and morphology, stress/strain and microstructure evolutions, and grain size distribution in the whole process were characterized and compared to further illustrate the densification behavior and the underlying dynamics/mechanisms. The results show that compared with the cold compaction, the warm compaction can not only achieve higher relative density, smaller and more uniform equivalent stress, and weaker spring back effect, but also improve the friction condition among powder particles. The plastic deformation of 316L particles is the main densification mechanism during compaction. In the solid-state sintering of TiC/316L compacts, the densification is mainly indicated by shrinkage and vanishing of large residual pores along with the growth of the sintering necks, accompanied by the particle movement and growth along the boundary regions. Meanwhile, the particle displacement and grain size distribution are more uniform in the warm compacted TiC/316L component. Moreover, the equivalent (von Mises) stress in 316L particles is smaller than that in TiC particles.     

粉末的爆炸压实工艺

为指导粉末爆炸压实工艺,综述了影响粉末爆炸压实的各种工艺参数,阐述了爆炸装置、装粉套筒、原始粉末、炸药以及其他因素的选择原则,分析了这些工艺因素对粉末爆炸成型质量的影响,提出了粉末爆炸压实中工艺参数优化的复杂性,并展望了爆炸压实工艺在粉末成型中的应用前景.     

Tooling Design and Compaction Analysis on P/M Copper Bushes

The successful production of P/M (powder metallurgy) components depends to a large extent on the tooling used for powder compaction. While designing the tool, the complexities arise from the interaction of the parameters such as powder characteristics, expected green density, the size and geometry of the product, and to whom the properties of the tool materials during compaction should be addressed. Floating type of compaction tooling set (die, punches, and core rod) was designed and fabricated. Pure electrolytic copper powder was compacted in the above-mentioned tool to obtain P/M copper bushes. Compaction pressure-density relationship and their influence on green strength are analyzed.     

Size Ratio Effects on Particle Contact Evolution at Uniaxial Powder Compaction

Cold compaction of composite powders has been analyzed using a discrete element method (DEM). Powder aggregates consisting of up to approximately 10,000 particles and formed by two powder populations with known material strength and size ratios have been compacted both isostatically and uniaxially (die compaction). The particles were assumed constitutively to be perfectly plastic or rigid and as a result, local contacts between the particles were described by a linear force-displacement relation given by previous in-depth analyses of spherical indentation problems. Particular emphasis has been placed on investigating the particle contact evolution at die compaction and to compare the results with previous ones pertinent to the isostatic case. Consequently, the predictive capability of the fundamental assumptions frequently used in theoretical analyses of compaction problems is determined for a uniaxial situation. The main conclusion is that size ratio effects are substantial at die compaction and when such features are present, theoretical predictions overestimates the (average) number of contacts per particle. It was also found that the mechanical behaviors at isostatic and die compaction are very similar even though die compaction values are slightly higher at high values on the relative density of powder materials.     

Tribological behavior of sintered electrolytic iron-zinc stearate added compacts

Powder metallurgy is an effective method to give near net shape to powder particles. In this paper, the influence of powder particle size, lubricant and compaction load on hardness and wear loss has been investigated as it influences the compact. Electrolytic iron powder (250 mesh to 300 mesh and 300 mesh to 350 mesh) with zinc stearate (0 weight % to 2 weight %) was used for preparing the samples. Green samples were prepared by cold compaction process at different loads (400 kN, 450 kN and 500 kN). Pre-sintering was done at 550 °C. Taguchi′s (L₁₈) mixed level model was used to develop the regression equation for hardness and wear loss. The maximum hardness of 79 HRB was achieved with 300 mesh to 350 mesh particle size and 500 kN compaction load. Minimum wear volume loss was observed with samples having composition of 250 mesh to 300 mesh size electrolytic iron powder at 500 kN compaction load and 1 weight % lubricant content.     

Modification of α-lactose monohydrate as a direct compression excipient using roller compaction

Abstract

Roller compaction was used to prepare a direct-compressed lactose excipient using crystalline α-lactose monohydrate. The effect of various roller compaction process parameters (compaction pressure, compaction repetition, and speed ratio) on the characteristics of compacted α-lactose monohydrate was investigated. Results were compared with data obtained using industrial spray-dried lactose and lactose samples with different degrees of crystallinity. XRPD analysis revealed that roller compaction reduced the crystallinity of α-lactose monohydrate, and the resulting material is similar to spray-dried lactose in behavior as a direct compression excipient. Roller compaction introduced desirable characteristics to the raw α-lactose monohydrate by inducing changes in crystallinity and particle morphology. Scanning electron microscopy results indicated that the compaction process converted some of the original torpedo-shaped crystals of α-lactose monohydrate into a more cylindrical shape with rounded edges. Compaction pressure and repetition of compaction have a significant effect on the modification of the crystallinity of the processed, raw α-lactose monohydrate.     

颗粒接触摩擦系数空间变异性对颗粒流双轴数值试验的影响

提出了考虑颗粒摩擦系数空间变异性的砂土双轴剪切响应分析方法。采用随机场模型表征颗粒摩擦系数空间变异性,通过Karhunen-Loève展开方法离散接触摩擦系数随机场,编写了基于颗粒流程序PFC2D和MATLAB的随机模拟耦合分析程序。研究了摩擦系数空间变异性对密砂试样的双轴剪切响应影响规律。结果表明:1） 提出方法可有效地考虑颗粒间接触摩擦系数变异性对土体材料双轴压缩宏观力学行为影响;2） 密砂试样在剪切过程中的应力-应变关系曲线、体积-应变关系曲线的变化规律与颗粒间接触摩擦系数不确定性密切相关,在初始加载阶段随机模拟的偏应力曲线、体积应变曲线基本重合,继续加载后曲线开始发散;3） 垂直相关距离对峰值偏应力均值与标准差影响明显大于水平相关距离。颗粒接触摩擦系数的均值对峰值偏应力的影响大于摩擦系数空间分布的影响。摩擦系数的空间分布会影响剪切带的形成位置。     

不同放电能量下铜粉的电磁压实特性与烧结体性能研究

目的 研究放电能量对铜粉电磁压实特性与烧结体性能的影响,提升铜材料的制备效率与质量.方法 通过电磁粉末压实技术在不同放电能量下制备铜压坯,研究压坯的相对致密度与微观形貌随放电能量的变化趋势.随后对其进行真空烧结,对烧结体的拉伸性能与断口形貌进行测试,评估放电能量对烧结体性能的影响.结果 随着放电能量的增加,铜压坯的相对...     

Distinct simulation of earth pressure against a rigid retaining wall considering inter-particle rolling resistance in sandy backfill

The focus of this paper is to analyze earth pressure against a rigid retaining wall under various wall movement modes with a contact model considering inter-particle rolling resistance implemented into the distinct element method (DEM). Firstly, a contact model considering rolling resistance in particles was generally explained and implemented into the DEM. The parameters of the contact model are determined from DEM simulation of biaxial tests on a sandy specimen. Then, the influence of inter-particle rolling resistance in the backfill is discussed by comparing the active and passive earth pressure against a rigid wall subjected to a translational displacement with and without inter-particle rolling resistance in the material. Third, the DEM model considering the rolling resistance is used to investigate active and passive earth pressures while the rigid wall moves in a more general manner such as rotation or translation. The influence of rolling resistance on the earth pressures is examined from the microscopic particle scale (e.g., shear strain field) as well as the macroscopic scale (e.g., the magnitude and action point of resultant earth pressures). Finally, the effect of the initial density and the particle size of the backfill are discussed. The results show that when rolling resistance in the particles is taken into account in the DEM simulation, the simulation results are more appropriate and are in line with practical situation. Hence, particles rolling resistance should be taken into account to get more realistic results in DEM analyses.     

Use of Tablet Tensile Strength Adjusted for Surface Area and Mean Interparticulate Distance to Evaluate Dominating Bonding Mechanisms

In this study, tablet tensile strength has been adjusted for tablet surface area and the average distance between particles in compacts of different materials. The aim of the study was to evaluate the feasibility of using this concept to assess the dominating interparticulate bonding mechanisms. Adjustment of the tensile strength for both tablet surface area and mean pore radius gave similar bonding strength values for materials bonding mainly by weak distance forces (crystalline lactose, sucrose, and microcrystalline cellulose) almost independently of compaction pressure. However, particle size and other factors may still affect the compensated strength values. The bond strength was much higher and more varied for materials bonding also with solid bridges (potassium chloride, sodium chloride, and possibly also sodium bicarbonate and amorphous lactose). For these materials, particle size and compaction pressure had a substantial effect on the bond strength. It is probably the formation of continuous bridges between adjacent particles that is important in these materials rather than the surface properties and the average distance between particles positioned at some distance from each other. Hence, adjusting the tensile strength of compacts does not necessarily reflect all the dominating factors responsible for interparticulate bonding. Nonetheless, adjustment for tablet surface area and mean pore radius allowed discrimination between different dominating interparticulate bonding mechanisms in these compacted materials.     

Use of Tablet Tensile Strength Adjusted for Surface Area and Mean Interparticulate Distance to Evaluate Dominating Bonding Mechanisms

In this study, tablet tensile strength has been adjusted for tablet surface area and the average distance between particles in compacts of different materials. The aim of the study was to evaluate the feasibility of using this concept to assess the dominating interparticulate bonding mechanisms. Adjustment of the tensile strength for both tablet surface area and mean pore radius gave similar bonding strength values for materials bonding mainly by weak distance forces (crystalline lactose, sucrose, and microcrystalline cellulose) almost independently of compaction pressure. However, particle size and other factors may still affect the compensated strength values. The bond strength was much higher and more varied for materials bonding also with solid bridges (potassium chloride, sodium chloride, and possibly also sodium bicarbonate and amorphous lactose). For these materials, particle size and compaction pressure had a substantial effect on the bond strength. It is probably the formation of continuous bridges between adjacent particles that is important in these materials rather than the surface properties and the average distance between particles positioned at some distance from each other. Hence, adjusting the tensile strength of compacts does not necessarily reflect all the dominating factors responsible for interparticulate bonding. Nonetheless, adjustment for tablet surface area and mean pore radius allowed discrimination between different dominating interparticulate bonding mechanisms in these compacted materials.     

A DEM-based analysis of the influence of aggregate structure on suspension shear yield stress

This study theoretically examined the effect of aggregate structure on the suspension shear yield stress. The aggregation process of colloidal particles was simulated using the discrete element model (DEM) combined with the well-known DLVO theory. The predicted aggregate structural characteristics, namely the coordination number and inter-particle forces were then used in a modified version of the Flatt and Bowen mechanistic model [6] to calculate the corresponding suspension yield stress. The effect of key parameters such as solid volume fraction, suspension pH and ionic strength on the aggregate structure and hence the yield stress of the suspension was investigated.The results showed that the yield stress increased significantly under conditions that were favourable for formation of complex net-like aggregate structures, such as high solid volume fractions, pH values near the iso-electric point, and high ionic strengths. In such cases, the mean coordination number reached a maximum value which was considered to be dependent on the particle size and size distribution. The suspension yield stress exhibited a power law dependency on the solid volume fraction. The interconnected network structure developed at high solid volume fractions was found to be the major contributing factor to the observed high suspension yield stress. As the particle–particle repulsion became significant, a decrease in both the number of bonds and the mechanical bonding strength of the aggregate structure was observed. That was considered to be responsible for the reduction in the suspension yield stress. The suspension yield stress became independent of the suspension ionic strength when the ionic strength exceeded the critical coagulation concentration. Satisfactory agreements were obtained between simulation results and the published experimental data.     

颗粒尺寸对颗粒增强型金属基复合材料动态特性的影响

利用有限元模型分析了颗粒增强型金属基复合材料 ( PMMCs ) Al/SiC的颗粒尺寸对复合材料在不同应变率下的动态特性的影响。采用有限元三维立方体单胞模型嵌入单个和多个球形增强颗粒,颗粒直径分别为16 μ m和7.5 μ m,多颗粒模型内部颗粒随机分布。基体材料假设为弹塑性,应变强化及应变率强化均符合指数规律。模拟结果表明:颗粒尺寸、颗粒体积含量及应变率对金属基复合材料的动态特性的影响是相互耦合的。颗粒体积含量一定时,颗粒尺寸越小,复合材料流动应力越高;颗粒含量越高,材料流动应力越高;应变率越高,材料流动应力越高。      

Is the adjustment of the impeller speed a reliable attempt to influence granule size in continuous dry granulation?

As the field of continuous manufacturing of solid pharmaceutics is developing, the interest in implementing continuous granulation methods is growing. Process analytical technology tools should be integrated to ensure the monitoring of the product quality and therefore enforce control strategies.Three single materials which are often used in dry granulation and additionally two formulations, one containing ibuprofen and the other acetaminophen were processed at various process parameters. They all differed in their compaction and fracture behavior. A statistical analysis of the influence of process parameters was executed, to work out which parameters could be used for a granule size control approach in continuous dry granulation. Thereby, the specific compaction force and the impeller speed were found to be significant factors in each design of experiment. However, the impeller speed was evaluated as the only suitable parameter to control granule size, as an impact on granule density is unlikely. Nevertheless, some restrictions such as an upper impeller speed limitation to avoid excessive fines and a lower speed limitation to impede a downturn of the throughput, have to be considered. Furthermore, a decreasing median granule size was observed at higher throughputs for plastically deforming materials and formulations.