Estimation of structural element sizes in sand and compacted blocks of ground calcium carbonate using a void network model

An algorithm has been developed for the calculation of the size of the effective structural or skeletal elements which make up the solid phase of an unconsolidated or consolidated porous block. It is based on a previously presented algorithm, but it has now been validated on unconsolidated samples and tested on consolidated samples. It also includes a virtual reality representation of the structures. First, a network model named Pore-Cor is made to reproduce the percolation behaviour of the experimental sample, by matching its simulated percolation characteristics to an experimental mercury intrusion curve. The algorithm then grows skeletal elements between the cubic pores and cylindrical throats of the void network model until they touch up to four of the adjacent void features. The size distributions of the simulated solid elements are compared with each other and with experimentally determined particle size distributions, using a Mann–Whitney test. The algorithm was shown to simulate skeletal elements with the correct trends in size distribution for two different sand samples, provided the sand packed itself optimally under the applied mercury pressure. It was also applied to two samples of variously compressed calcium carbonate powder, having fine and coarse particle size distributions respectively. The simulation demonstrated that on compressing the powder at the minimum force, the skeletal elements differed from the constituent particle sizes, as expected. The average size of the skeletal elements increased as the compression force was increased on the calcium carbonate powders. The results suggest that the method could be useful as a tool for probing the effect of compaction on aggregation or sintering, and for studying other effects such as cementation in geological samples, where other more direct techniques cannot be applied.     

Measurement of Void Size Correlation in Inhomogeneous Porous Media

In previous works, we have described a void space reconstruction method based on non-wetting fluid intrusion, wetting fluid drainage, and image analysis data. The method has been applied to a wide range of substances, including sandstone, compressed and sintered powders, paper substrates and coatings, soil and fibrous mats. We have also demonstrated in a previous work that the spatial correlation of similarly sized voids within inhomogeneous porous media has a huge effect on permeability. We therefore describe a method of measuring such correlation, suitable for use in our void space reconstructions. The method involves a cubic spline smoothing of a variogram of the void sizes in a binary image of the porous medium. It has been successfully tested on an artificially correlated void network, comprising two sintered glass discs of different void size ranges. Stereological effects, caused by the off-centre sectioning of voids, can interfere with the variogram features. Our method is sh own to be insensitive to artificially generated stereological interference. The method is also applied to sandstone samples.     

Dynamic Ink Oil Absorption in a Pigmented Porous Coating Medium Studied by Near-Infrared Diffuse Reflectance Spectroscopy

The rate of absorption (both long and short timescale) of typical heatset offset printing ink oils, namely mineral and linseed oil, has been studied on model ground calcium carbonate coating pigment tablets containing various amounts of either styrene–acrylic or styrene–butadiene binder. The pore structure characteristics of the tablets were determined using mercury intrusion porosimetry. The movement of the oils both on the surface of and within the porous structure of the pigment/binder tablets was studied under the influence of pressure-less capillary flow with subsequent diffusion through the connected void volume of the tablet. The wetting was analyzed by near-infrared (NIR) diffuse reflectance spectroscopy both as a single probe measurement and by hyperspectral imaging. The results showed that the rate of oil filling the structure was strongly dependent on the binder amount in the structure as well as the binder chemistry (oil- or non-absorbing binder), which supports previous findings. The liquid properties, and especially the viscosity of the liquid (oil), influenced the absorption rate. The gradients in absorbance indicated the presence of latex blocking access to some pores and reducing connectivity.     

Limit Models of Pore Space Structure of Porous Materials for Determination of Limit Pore Size Distributions Based on Mercury Intrusion Data

This paper proposes the application of capillary and chain random models of pore space structure for determination of limit pore diameter distributions of porous materials, based on the mercury intrusion curves. Both distributions determine the range in which the pore diameter distribution of the investigated material occurs and defines the degree of inaccuracy of the method based on the mercury intrusion data caused by the indeterminacy of the sample shape and its pore space architecture. We derived equations describing the quasi-static process of mercury intrusion into the porous layer and porous ball with a random chain pore space structure and analysed the influence of the model parameters on the mercury intrusion curves. It was shown that the distribution of link length in the chain model of the pore space, random location of chain capillaries in the sample and the length distribution of the capillaries do not influence significantly the intrusion process. Therefore, a simple model of the mercury intrusion into the layer is proposed in which chain links of the pore space have random diameters and constant length. This model is used as a basic model of the intrusion process into a sample of any shape and size and with homogeneous and isotropic chain pore space architecture. The thickness of the layer then represents the mean length of chain capillaries in the sample. It was also proved that the capillary and chain models of pore space architecture are limit models of the network model identified in this paper with the pore architecture of the investigated sample. This justifies the application of both models for determination of limit cumulative distributions of pore diameters in porous materials based on the mercury intrusion data.

     

Water Absorption into Construction Materials: Comparison of Neutron Radiography Data with Network Absorption Models

Two different porous building materials have been previously measured and analysed (El-Abd and Milczarek, 2004, IEEE Trans. Nuclear Sci.; El-Abd et al., 2004, J. Phys. D) using neutron radiography to measure the water front position over time. The results from this experimental approach show a similar behaviour to the predictions from idealised model structures, in that there is a cross over point where the fastest rate of absorption at first favours the finer structure material and at later times favours the coarser pore structure material. The computer model, Pore-Cor** is used to generate the idealised structures and the absorption of fluid into porous structures follows a Bosanquet wetting algorithm for fluids undergoing both inertial and viscous dynamical flow (Ridgway and Gane, 2002, Colloids Surfaces A: Physicochem. Eng. Aspects 206, 217–239.). The model structures comprise cubic pores connected by cylindrical throats on a three-dimensional 10× 10× 10 position matrix simulating the void structure of porous media by fitting as closely as possible the modelled mercury intrusion curve to that of the experimentally determined mercury intrusion curve of the actual sample. They show the transition that occurs in the absorption behaviour from the linear t-dependent short timescale inertial regime to the familiar √t Lucas-Washburn viscous regime. The simulated absorption algorithm applied to these model structures also shows a fluid position behaviour that replicates qualitatively, given the limitation of representative sample volume, the cross over seen experimentally. Furthermore, the existence of a preferred wetting path is demonstrated in the experimental as well as the model wetting front behaviour. In the case of the structure containing the broader range of pore sizes, the wetting front is considered to proceed by a network of optimal size combinations (inertial wetting versus viscous drag) and connectivity, leaving some pores behind the wetting front unfilled or only partially filled. ** Pore-Cor is a software program of the Environmental and Fluids Modelling Group, University of Plymouth, Devon, PL4 8AA, U.K.     

Multiscale Structures to Describe Porous Media Part I: Theoretical Background and Invasion by Fluids

A porous medium with a broad pore-size distribution is described on the basis of the Multiscale Percolation System concept. The representative structure is the superposition of several constitutive elementary networks, of which mesh sizes are proportional to the diameter of the class of pores considered. To account for the contribution of each class to the connection of the medium, a recurrent building process, involving rescaling and superposition, is defined. This process leads to an equivalent monoscale network, involving elements representative of the various classes. Mercury intrusion at increasing pressure into a finite-size sample of this equivalent network is modelled. The inverse problem is solved, leading to the identification of the representative multiscale structure of a given material from the experimental intrusion curve.     

Plasticity and ductile fracture of IF steels: experiments and micromechanical modeling

If one aims at the simulation of plasticity and failure of multiphase materials, the choice of an appropriate material law is of major importance. Plasticity models for porous metals contain, in addition to the yield surface and the flow potential, also functions describing the void nucleation, dependent on some macroscopically observable quantities, and the growth of these voids. In this paper, a micromechanically based method to develop a void nucleation function for porous plasticity models is proposed which is valid for all possible microstructures as long as the amount of second phase particles is low (i.e. the particles do not interact with respect to the stress and strain fields), and as long as the particles are large enough (above 0.1 μm) justifying a continuum mechanical approach. The method described consists of two stages: In the first stage, the microstructure is investigated via a finite element model. The FE model implicitly contains the effects of the shape of the precipitates, of the material parameters of both the matrix and the precipitates, of the void nucleation hypothesis (by the assumption of “nucleation limits” for characteristic damage-related quantities), and of the applied stress state. In the second stage, during postprocessing, the volume fraction of precipitates as well as the influences of the particle orientation distribution, size distribution, and size dependence of the damage-related quantities are taken into account. The model is applied to the microstructure of IF (Interstitially Free) steel, a material with a ductile matrix and rigid second phase particles of cubical shape. This microstructure is particularly suited for investigating shape and size effects. The model shows that either the size effect or the shape effect dominate the void nucleation behavior: in the case of particles of roughly the same size, the size distribution will hardly alter the nucleation strain distribution obtained by taking into account only the shape and orientation effects. For particles of very different sizes, the size effect will completely override the rather “sharp” original distribution regarding particle shape and orientation.     

Achieving Rapid Absorption and Extensive Liquid Uptake Capacity in Porous Structures by Decoupling Capillarity and Permeability: Nanoporous Modified Calcium Carbonate

Porous media with rapid absorption properties are greatly sought after in the fields of super absorbers and catalysts. Natural materials, such as diatomite, or synthetic zeolite feature strongly in industrial reaction processes. Most, or all, of such materials, however, are surface acidic. A novel rapidly absorbing alkaline porous structure, with a high absorption capacity, is presented here. As in the case of diatomite or zeolite, the pigment design incorporates strong capillarity within a highly permeable packed medium. A model is proposed for general use with highly absorbing media that can be proven microscopically to have separate domains of micro- or nano-capillarity embedded within a permeable matrix. The new pigment morphology, based on natural ground calcium carbonate (gcc), exhibits this property using special surface structure modifications. It is contrasted with standard gcc by using consolidated tablet blocks made from a suspension of the pigment and chosen mixtures thereof. The blocks are characterised after drying by mercury porosimetry, and the absorption dynamic of a selected liquid is studied. It is shown that using a self-assembly method of discrete pore structures provides a much faster absorption rate and a liquid capacity for up to 10 times more fluid than a conventional homogeneously distributed pore concept. In such unique discrete network systems, the mercury intrusion curve provides a separable analysis of permeability and capillarity in respect to the inflection point of the cumulative intrusion curve. The discrete decoupled properties each follow the absorption behaviour predicted by previous modelling (Ridgway and Gane, Colloids and Surfaces A: Physicochemical and Engineering Aspects, 206(1–3), 2002). The absorption driving force is shown to be determined by the proportion of fine pores present up to a size equal to a Bosanquet inertially-defined optimum within the timescale of absorption. Combining the wetting force, from the capillarity-controlled fine pore structure, with the experimental flow resistance of the sample, consisting of the assembly of particles, it is possible to predict the trends in absorption dynamic using the pore and throat model Pore-Cor.* Use of this model allows existing materials as well as new synthetic designs to be modelled prior to manufacture. The novel alkaline material is compared with independent absorption data for diatomite and shown to be comparable. *Pore-Cor is a software product name of the Environmental and Fluid Modelling Group, University of Plymouth, Devon PL4 8AA, U.K.     

Statistical Synthesis of Imaging and Porosimetry Data for the Characterization of Microstructure and Transport Properties of Sandstones

The microstructure of a suite of sandstone samples is quantitatively analyzed using a method which combines information from thin section micrographs of the pore space with mercury injection porosimetry in a statistical framework. This method enables the determination of a continuous distribution of pore sizes ranging from few nanometre to several hundred micrometre. The data obtained unify fractal and Euclidean aspects of the void space geometry, yield estimates of the pore-to-throat aspect ratio and challenge the ability of commonly used network models to describe fluid percolation in multiscale porous media. Application of critical path analysis to the prediction of flow permeability and electrical conductivity of sandstone core samples using the new information produces results comparable to those obtained by the classical approach—a fact attributed to the presence of macroscopic heterogeneity at the scale of several millimetres.     

Effect of Wetting on the Dynamics of Drainage in Porous Media

We examine the consequences of the wettability properties on the dynamics of gravity drainage in porous media. The relation between the wetting properties at the pore scale and the macroscale hydrodynamics is studied. Model porous media consisting of hydrophilic and hydrophobic glass beads or sand with well defined wetting properties, are prepared for this study. Gravity drainage experiments with air displacing water (two-phase flow), are performed for different Bond numbers, and using different techniques such as gamma-ray densitometry, magnetic resonance imaging (MRI) and weight measurements. The dynamics of drainage is found to be different for hydrophilic and hydrophobic porous media in the transition zone (funicular regime). Moreover, for hydrophilic (water-wet) porous media, MRI experiments reveal the importance of drainage through the continuous water film, which leads to an increase of the residual quantity of water in the transition zone with time.     

Constitutive equations for densification of matrix-coated fibre composites during hot isostatic pressing

This work addresses the development of physically based constitutive equations for the consolidation of fibre-matrix-void systems typically arising in the manufacture of matrix-coated fibre metal matrix composite materials. The analyses consider square array packing of the coated fibres under symmetrical in-plane compressive load and take into account the power-law creep of the matrix. Two models have been developed. The first is based on an energy approach in which assumed velocity fields in the deforming matrix are considered and are expressed in terms of an unknown parameter. In this way, the dependence of the deformation rate on volume fraction of voids and fibres is derived through the use of Hill's minimum principle for velocities. The second model makes use of micro-mechanical finite element modelling in which fibre, matrix and void are modelled explicitly. The micro-mechanical finite element model is developed for validation and comparison. Theoretical predictions are examined. The constitutive equation for consolidation derived from Hill's minimum principle shows good agreement with results obtained from micro-mechanical finite element modelling.     

Flow Modeling of Well Test Analysis for Porous–Vuggy Carbonate Reservoirs

Porous–vuggy carbonate reservoirs consist of both matrix and vug systems. This paper represents the first study of flow issues within a porous–vuggy carbonate reservoir that does not introduce a fracture system. The physical properties of matrix and vug systems are quite different in that vugs are dispersed throughout a reservoir. Assuming spherical vugs, symmetrically distributed pressure, centrifugal flow of fluids and considering media that is directly connected with wellbore as the matrix system, we established and solved a model of well testing and rate decline analysis for porous–vuggy carbonate reservoirs, which consists of a dual porosity flow behavior. Standard log–log type curves are drawn up by numerical simulation and the characteristics of type curves are analyzed thoroughly. Numerical simulations showed that concave type curves are dominated by interporosity flow factor, external boundary conditions, and are the typical response of porous–vuggy carbonate reservoirs. Field data interpretation from Tahe oilfield of China were successfully made and some useful reservoir parameters (e.g., permeability and interporosity flow factor) are obtained from well test interpretation.     

Accelerated void growth in porous ductile solids containing two populations of cavities

This paper presents an analytical and numerical study of accelerated void growth in porous ductile solids arising from the presence of two populations of cavities very different in size. It is based on the model problem of some hollow sphere made of porous plastic material and subjected to hydrostatic tension. The central hole plays the role of a typical big cavity of the first population while those dispersed in the matrix stand for the small cavities of the second one. The behavior of the matrix is supposed to obey Gurson's famous “homogenized” model for porous ductile solids (Gurson, A.L., 1977. Continuum theory of ductile rupture by void nucleation and growth: part I — yield criteria and flow rules for porous ductile media. ASME J Engng Materials Technol 99, 2–15). The analytic solution of this model problem shows that the small voids located near the big one grow twice as fast as the latter void. This suggests that in a subsequent step, these small cavities may reach coalescence prior to the big ones, thus creating spherical shells of ruined matter around the cavities of the first population and leading to accelerated growth of the latter cavities; this scenario is in agreement with experimental evidence. Since this subsequent step is not amenable to a complete analytic solution, it is studied numerically. Finally, a simplified model reproducing the two steps of void growth (prior to coalescence of the small voids and after it has started) is developed on the basis of the analytical solution for the first step and some elements of a similar solution for the second one. The results derived from this simplified model are in good quantitative agreement with those obtained through the complete numerical simulations.     

On the modelling conditions of mass transfer in porous media presenting capacitance effects by a dispersion-convection equation for the mobile fluid and a diffusion equation for the stagnant fluid

The modelling of mass transfer in porous media presenting capacitance effects by a dispersion-convection equation for the mobile fluid and a diffusion equation for the stagnant fluid has been shown (Piquemal, 1992) to be erroneous in the general case, because it is assumed that the mean concentration of the flowing fluid equals the point concentration at the boundary of the stagnant fluid. This boundary condition cannot be realized. This paper gives the conditions that allows the use of this kind of model with an acceptable approximation. The problem has been solved in the case of two schematic structures: the first is a cylindrical tube with stagnant pockets in its wall, the second a stratified medium. The characteristic lengths of the mobile and immobile domain must obey a criterion in which the porous medium characteristics and the flow velocity appear.     

Evaporation heat transfer in thin biporous media

 This paper deals with the evaporation heat transfer mechanism in thin biporous media that have two characteristic capillary pore radii. The character of the two levels of pore sizes allows the liquid phase to easily occupy the void space of the small pores and vapor phase to occupy the void space of the big pores. Compared with mono-porous media, biporous media increase the number of small evaporating menisci with high heat transfer performance. Evaporation heat transfer in pores of porous media is analyzed in detail. The results indicate that the average heat transfer coefficient increases with the capillary pore size reduction. Under the assumption of the uniform structure of biporous media, a calculation method to predict heat transfer performance for the evaporation in thin biporous media is given. The preliminary results reflect the behavior of observed vaporization heat transfer in thin biporous media well. Received on 22 February 2000     

Modeling of Hysteretic Behavior of Soil–Water Retention Curves Using an Original Pore Network Model

Soil–water retention curve (SRWC), also called soil moisture characteristic, is used for simulation models of soil water storage or soil aggregate stability. The present study addresses the modeling of SRWC with particular attention paid to hysteresis effects of water filling and draining the pores attributed to ink-bottle effects. For that purpose, an idealized pore size distribution previously developed for predicting water sorption isotherms on cementitious materials, and which can consider the double porosity structure of soils, is used. The input data of the model are assessed only from mercury intrusion porosimetry tests (MIP) and from grain size distribution (GSD). The hysteretic behavior of SRWC is reproduced in a satisfactory way. The model can also predict the specific surface area.

     

Verification of the transferability of micromechanical parameters by cell model calculations with visco-plastic materials

Finite element (FE) calculations of a cylindrical cell containing a spherical hole have been performed under large strain conditions for varying triaxiality with three different constitutive models for the matrix material, i.e. rate independent plastic material with isotropic hardening, visco-plastic material under both isothermal and adiabatic conditions, and porous plastic material with a second population of voids nucleating strain controlled. The “mesoscopic” stress-strain and void growth responses of the cell are compared with predictions of the modified Gurson model in order to study the effects of varying triaxiality and strain rate on the critical void volume fraction. The interaction of two different sizes of voids was modelled by changing the strain level for nucleation and the stress triaxiality. The study confirms that the void volume fraction at void coalescence does not depend significantly on the triaxiality if the initial volume fraction of the primary voids is small and if there are no secondary voids. The strain rate does not affect f_c either. The results also indicate that a single internal variable, f, is not sufficient to characterize the fracture processes in materials containing two different size-scales of void nucleating particles.     

Void growth and coalescence in single crystals

Void growth and coalescence in single crystals are investigated using crystal plasticity based 3D finite element calculations. A unit cell involving a single spherical void and fully periodic boundary conditions is deformed under constant macroscopic stress triaxiality. Simulations are performed for different values of the stress triaxiality, for different crystal orientations, and for low and high work-hardening capacity. Under low stress triaxiality, the void shape evolution, void growth, and strain at the onset of coalescence are strongly dependent on the crystal orientation, while under high stress triaxiality, only the void growth rate is affected by the crystal orientation. These effects lead to significant variations in the ductility defined as the strain at the onset of coalescence. An attempt is made to predict the onset of coalescence using two different versions of the Thomason void coalescence criterion, initially developed in the framework of isotropic perfect plasticity. The first version is based on a mean effective yield stress of the matrix and involves a fitting parameter to properly take into account material strain hardening. The second version of the Thomason criterion is based on a local value of the effective yield stress in the ligament between the voids, with no fitting parameter. The first version is accurate to within 20% relative error for most cases, and often more accurate. The second version provides the same level of accuracy except for one crystal orientation. Such a predictive coalescence criterion constitutes an important ingredient towards the development of a full constitutive model for porous single crystals.     

Dynamics of Viscous Entrapped Saturated Zones in Partially Wetted Porous Media

As a typical multiphase fluid flow process, drainage in porous media is of fundamental interest both in nature and in industrial applications. During drainage processes in unsaturated soils and porous media in general, saturated regions, or clusters, in which a liquid phase fully occupies the pore space between solid grains, affect the relative permeability and effective stress of the system. Here, we experimentally study drainage processes in unsaturated granular media as a model porous system. The distribution of saturated clusters is analysed by optical imaging under different drainage conditions, with pore-scale information from Voronoi and Delaunay tessellation used to characterise the topology of saturated cluster distributions. By employing statistical analyses, we describe the observed spatial and temporal evolution of multiphase flow and fluid entrapment in granular media. Results indicate that the distributions of both the crystallised cell size and pore size are positively correlated to the spatial and temporal distribution of saturated cluster sizes. The saturated cluster size is found to follow a lognormal distribution, in which the generalised Bond number (\( Bo^{*} \)) correlates negatively to the scale parameter (μ) and positively to the shape parameter (σ). With further consideration of the total surface energy obtained based on liquid–air interfaces, we were able to include additional grain-scale information in the constitutive modelling of unsaturated soils using both the degree of saturation and generalised Bond number. These findings can be used to connect pore-scale behaviour with overall hydro-mechanical characteristics in granular systems.