Abstract

In-die compression analysis is an effective method for the characterization of powder compressibility. However, physically unreasonable apparent solid fractions above one or apparent in-die porosities below zero are often calculated for higher compression stresses. One important reason for this is the neglect of solid compressibility and hence the assumption of a constant solid density. In this work, the solid compressibility of four pharmaceutical powders with different deformation behaviour is characterized using mercury porosimetry. The derived bulk moduli are applied for the calculation of in-die porosities. The change of in-die porosity due to the consideration of solid compressibility is for instance up to 4% for microcrystalline cellulose at a compression stress of 400 MPa and thus cannot be neglected for the calculation of in-die porosities. However, solid compressibility and further uncertainties from, for example the measured solid density and from the displacement sensors, are difficult or only partially accessible. Therefore, a mathematic term for the calculation of physically reasonable in-die porosities is introduced. This term can be used for the extension of common mathematical models, such as the models of Heckel and of Cooper & Eaton. Additionally, an extended in-die compression function is introduced to precisely describe the entire range of in-die porosity curves and to enable the successful differentiation and quantification of the compression behaviour of the investigated pharmaceutical powders.

Highlights

  • Powder compaction is an important production process in diverse industries, such as food, ceramic and pharmaceutical industry

  • The prediction of structural and mechanical properties of tablets based on raw material properties and process parameters is still difficult or rather impossible, the powder compaction process was the object of numerous scientific investigations

  • The hydrostatic pressure is approximated by the overall axial compression stress acting on the powder

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Summary

Introduction

Powder compaction is an important production process in diverse industries, such as food, ceramic and pharmaceutical industry. The main reason for the incomplete predictability is certainly the still limited process understanding due to the complexity of the powder compaction process This complexity can be attributed to various influencing parameters [1,2,3,4,5], such as the deformation behaviour, the particle size and shape and the compression stress on the one hand and to different acting micro-processes [6,7,8,9,10], such as particle rearrangement, elastic and plastic deformation of single particles and particle fragmentation on the other hand. Investigations of the compressibility of single crystals by hydrostatic compression with high pressures up to several GPa show the decrease of specific solid volume with rising hydrostatic pressure according to the Murnaghan equation [46] This equation implies a stress dependency of the bulk modulus.

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