Characterization of Mechanical Property Distributions on Tablet Surfaces

Powder densification through uniaxial compaction is governed by a number of simultaneous processes taking place on a reduced time as the result of the stress gradients within the packing, as well as the frictional and adhesive forces between the powder and the die walls. As a result of that, a density and stiffness anisotropy is developed across the axial and radial directions. In this study, microindentation has been applied to assess and quantify the variation of the module of elasticity (Emod) throughout the surface of cylindrical tablets. A representative set of deformation behaviors was analyzed by pharmaceutical excipients ranging from soft/plastic behavior (microcrystalline cellulose) over medium (lactose) to hard/brittle behavior (calcium phosphate) for different compaction pressures. The results of the local stiffness distribution over tablet faces depicted a linear and directly proportional tendency between a solid fraction and Emod for the upper and lower faces, as well as remarkable stiffness anisotropy between the axial and radial directions of compaction. The highest extent of the stiffness anisotropy that was found for ductile grades of microcrystalline cellulose (MCC) in comparison with brittle powders has been attributed to the dual phenomena of overall elastic recovery and Poisson’s effect on the relaxation kinetics. As a reinforcement of this analysis, the evolution of the specific surface area elucidated the respective densification mechanism and its implementations toward anisotropy. For ductile excipients, the increase in the contact surface area as well as the reduction and closing of interstitial pores explain the reduction of surface area with increasing compaction pressure. For brittle powders, densification evolves through fragmentation and the subsequent filling of voids

Segregation and mixing of granular material in industrial processes

Within the EU-funded PARDEM network mixing and segregation are studied in silos and heaps, agitated mixers and fluidized beds. A method is presented with which mixing and segregation can be characterized, adapted for quasi-static to dynamic systems and applied at the global system level as well as at the local level. This paper attempts to give an overview of the applicability of this analysis by providing three instances, being chute flow representing flow down a heap, agitated mixing and fluidization, in which the method is applied

The Effect of Water, Nanoparticulate Silica and Dry Water on the Flow Properties of Cohesionless Sand

Cement hydration within particle bed concrete 3D printing processes can be benefited by storing water in the otherwise dry aggregate bulk material. Additional water also has the advantage of acting as a source of passive cooling. However, even small amounts of liquid lead to detrimental effects on bulk properties, such as the flowability. For that reason, this study proposes implementing dry water (DW) in order to store large amounts of water in a bulk material of non-absorbent, coarse sand whilst maintaining its initial bulk properties. DW is essentially created by mixing water and hydrophobic fumed silica in a high shear process, leading to water droplets surrounded by a protective silica shell. Herein, several DW variants, distinguished by their deionised water to hydrophobic silica ratio, were mixed with non-absorbent, coarse sand particles. In addition, mixtures were produced to contain a specific overall water content of up to wH2O = 5% within the bulk material. It was shown that dry water can be used to incorporate large amounts of water into a granular bulk material and simultaneously preserve flow properties. The decisive factor is the proportion of hydrophobic silica for a given water content as the DW capsules may otherwise not endure mechanical stress during mixing. However, even minimal quantities of silica can prevent liquid capillary bridges from forming and, thus, inhibit bulk property degradation

Effect of Particle Size and Cohesion on Powder Yielding and Flow

The bulk properties of powders depend on material characteristics and size of the primary particles. During storage and transportation processes in the powder processing industry, the material undergoes various modes of deformation and stress conditions, e.g., due to compression or shear. In many applications, it is important to know when powders are yielding, i.e. when they start to flow under shear; in other cases it is necessary to know how much stress is needed to keep them flowing. The measurement of powder yield and flow properties is still a challenge and will be addressed in this study. In the framework of the collaborative project T-MAPPP, a large set of shear experiments using different shear devices, namely the Jenike shear tester, the ELE direct shear tester, the Schulze ring shear tester and the FT4 powder rheometer, have been carried out on eight chemically-identical limestone powders of different particle sizes in a wide range of confining stresses. These experiments serve two goals: i) to test the reproducibility/consistency among different shear devices and testing protocols; ii) to relate the bulk behaviour to microscopic particle properties, focusing on the effect of particle size and thus inter-particle cohesion. The experiments show high repeatability for all shear devices, though some of them show more fluctuations than others. All devices provide consistent results, where the FT4 powder rheometer gives lower yield/steady state stress values, due to a different pre-shearing protocol. As expected, the bulk cohesion decreases with increasing particle size (up to 150 μm), due to the decrease of inter-particle cohesion. The bulk friction, characterized in different ways, is following a similar decreasing trend, whereas the bulk density increases with particle size in this range. Interestingly, for samples with particle sizes larger than 150 μm, the bulk cohesion increases slightly, while the bulk friction increases considerably—presumably due to particle interlocking effects—up to magnitudes comparable to those of the finest powders. Furthermore, removing the fines from the coarse powder samples reduces the bulk cohesion and bulk density, but has a negligible effect on the bulk friction. In addition to providing useful insights into the role of microscopically attractive, van der Waals, gravitational and/or compressive forces for the macroscopic bulk powder flow behaviour, the experimental data provide a robust database of cohesive and frictional fine powders for industrially relevant designs such as silos, as well as for calibration and validation of models and computer simulations

Effect of Particle Size and Cohesion on Powder Yielding and Flow

The bulk properties of powders depend on material characteristics and size of the primary particles. During storage and transportation processes in the powder processing industry, the material undergoes various modes of deformation and stress conditions, e.g., due to compression or shear. In many applications, it is important to know when powders are yielding, i.e. when they start to flow under shear; in other cases it is necessary to know how much stress is needed to keep them flowing. The measurement of powder yield and flow properties is still a challenge and will be addressed in this study. In the framework of the collaborative project T-MAPPP, a large set of shear experiments using different shear devices, namely the Jenike shear tester, the ELE direct shear tester, the Schulze ring shear tester and the FT4 powder rheometer, have been carried out on eight chemically-identical limestone powders of different particle sizes in a wide range of confining stresses. These experiments serve two goals: i) to test the reproducibility/consistency among different shear devices and testing protocols; ii) to relate the bulk behaviour to microscopic particle properties, focusing on the effect of particle size and thus inter-particle cohesion. The experiments show high repeatability for all shear devices, though some of them show more fluctuations than others. All devices provide consistent results, where the FT4 powder rheometer gives lower yield/steady state stress values, due to a different pre-shearing protocol. As expected, the bulk cohesion decreases with increasing particle size (up to 150 μm), due to the decrease of inter-particle cohesion. The bulk friction, characterized in different ways, is following a similar decreasing trend, whereas the bulk density increases with particle size in this range. Interestingly, for samples with particle sizes larger than 150 μm, the bulk cohesion increases slightly, while the bulk friction increases considerably—presumably due to particle interlocking effects—up to magnitudes comparable to those of the finest powders. Furthermore, removing the fines from the coarse powder samples reduces the bulk cohesion and bulk density, but has a negligible effect on the bulk friction. In addition to providing useful insights into the role of microscopically attractive, van der Waals, gravitational and/or compressive forces for the macroscopic bulk powder flow behaviour, the experimental data provide a robust database of cohesive and frictional fine powders for industrially relevant designs such as silos, as well as for calibration and validation of models and computer simulations

Segregation and mixing of granular material in industrial processes

Within the EU-funded PARDEM network mixing and segregation are studied in silos and heaps, agitated mixers and fluidized beds. A method is presented with which mixing and segregation can be characterized, adapted for quasi-static to dynamic systems and applied at the global system level as well as at the local level. This paper attempts to give an overview of the applicability of this analysis by providing three instances, being chute flow representing flow down a heap, agitated mixing and fluidization, in which the method is applied