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Materials and Structures (2006) 39:8191 DOI 10.

1617/s11527-005-9036-1

A theoretical frame to study stability of fresh concrete


N. Roussel

Received: 4 November 2004 / Accepted: 24 February 2005 C RILEM 2006

Abstract A theoretical frame able to describe the segregation under gravity of a mono-sized granular material in a yield stress suspending uid is presented. Two stability criteria are proposed. The rst one deals with the stability of a single sphere in a yield stress uid while the second one takes into account the mechanical interactions between the particles that could lower the risk of instability. The two criteria are then experimentally validated in the case of polystyrene spheres in a cement paste. Image analysis techniques are used to measure the nal solid fraction in the segregated zone. The comparison of the experimental and theoretical results is followed by an analysis of the possible use of such criteria in a mix proportioning method and a short discussion of the inuence of the change of rheological properties with time on the segregation phenomenon. R sum Un cadre th orique permettant de d crire le e e e e ph nom` ne de s gr gation sous gravit de sph` res e e e e e e ` mono-disperses dans un uide a seuil est pr sent . e e Deux crit` res de stabilit du m lange sont propos s. e e e e Le premier concerne la stabilit dune sph` re unique e e ` dans un uide a seuil alors que le deuxi` me prend e en compte les interactions m caniques entre sph` res e e qui peuvent r duire le risque dinstabilit du m lange. e e e Les deux crit` res sont valid s exp rimentalement dans e e e ` le cas de billes de polystyr` ne m lang es a une e e e p te de ciment. Une technique danalyse dimages a
N. Roussel LCPC, Paris, France

est utilis e pour mesurer la fraction volumique solide e nale atteinte dans les zones s gr g es. Cette vale e e idation exp rimentale est suivie dune courte anale yse de lutilisation possible de tels crit` res dans une e m thode de formulation de b tons et de linuence de e e la thixotropie et du vieillissement sur la stabilit dun e m lange. e

1. Introduction More uid. This is one of the big trends of the last twenty years in the eld of modern concretes. As we do not have any tool to predict the needed workability in terms of the shape of the element to cast, the spacing of steel bars and the chosen casting process, the only way to ensure that the casting will ll a complicated formwork is to use the most uid concretes. This nally leads to the elaboration of Self Compacting Concretes (SCC) [1]. Quickly, however, engineers realized that very high concrete uidity may have two main drawbacks: the pressure on the formwork was almost hydrostatic [2] and the concrete stability was quite difcult to ensure [3]. Concrete is a multiphasic material. The densities of the numerous components entering traditional concrete mix tting vary between 1000 kg/m3 (water) and 3200 kg/m3 (cement). Even lighter material may be used in the case of lightweight concrete. With such a mixture, gravity quickly becomes the enemy of homogeneity. In the eld of cementitious materials,

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heterogeneities induced by gravity are divided in two categories depending on the phase that is migrating: bleeding and segregation. Both are induced by the density difference between the components but bleeding phenomenon is concerned with the water migration whereas segregation is concerned with the movement of the coarser particles. The work presented here focuses on segregation in the case of an homogeneous (i.e. non bleeding) nonNewtonian uid containing solid inclusions. This can be applied to various length scale of observation. For example segregation in mortars would be predicted from paste rheology and the volume fraction, shape and size distribution of the sand particles. This type of multi-scale physical approach was not adapted to traditional concretes, the behaviour of which was dominated by grain to grain contacts. Any attempt to predict a physical phenomena had to take into account all the interactions between the particles, even the smallest [4]. The behavior of modern concretes, without even speaking of SCC, is getting closer to the behavior of a uid suspension. The physical concept of inclusions in a suspending uid becomes adapted to the description of each of the constitutive phase of the concrete and was already used in a paper by Saak and co-workers [5] to study the stability of SCC (the reading of which, by the way, initiate most of the experimental work presented here and should be advised to anybody interested in segregation). Attempts to correlate the rheology of the fresh concrete to its stability can be found in the literature [6,7]. Figures linking either empirical test results or even quantitative measurement of segregation to the slump or the slump ow of a given concrete have often been plotted. Although a correlation may, in certain cases, be obtained, no information about the underlying physics will ever be obtained this way. Segregation is a multiphasic separation phenomenon (the minimum number of phases is two: a suspending uid and some solid inclusions). As such, the only relevant approach is a multiphasic one. The rheological behavior of concrete has no role to play; only the rheological behavior of the suspending uid(s) does matter. When correlations between concrete behavior and its stability are obtained, it is only because concrete behavior is strongly linked to the behavior of its suspending uid(s). Segregation (or stability property) is often associated to static sedimentation. The particles fall towards the bottom of a given sample or of a formwork

as their density is higher than the density of suspending uid. However, it must not be forgotten that, if the inclusions density is lower than the suspending uid density, the situation may be the opposite. This is true for lightweight concrete and this is the case in the experimental results presented in this paper. The physical phenomena are of course the same no matter in which direction the particles are moving. Moreover, it must not be forgotten that some other reasons than gravity may induce segregation. Indeed, obstacles or conned ows may generate ow conditions in which the suspending uid is not able to carry its particles. In this paper, we will not deal with this type of dynamic segregation. The aim of this paper is to present two criteria for the stability of identical spheres in a yield stress uid. They are not of course directly suitable to the complete prediction of segregation in real concretes but they provide a basic theoretical frame that allowed us to understand many of our experimental data. The paper is divided into three parts. In a rst theoretical part, the two stability criteria are demonstrated. Using these results, several possible segregation cases are isolated and analysed. In a second part, experimental results are presented. Using image analysis, the nal packing fraction of polystyrene spheres in various cement pastes is measured. Finally, in a third part, experimental results and theoretical predictions are analysed and successfully compared. This conrms the validity of the proposed approach. 2. Theoretical analysis of the problem 2.1. Sphere in a yield stress uid: movement criterion and settling velocity The following piece of work is a generalization to yield stress uids of the work done by He and co-workers [8] in the case of the Bingham model. We assume in this study that the behavior of the cement paste may be approximated by a yield stress model of the following general form: = 0 < 0 = 0 = 0 + f( ) (1a) (1b)

where tau 0 is the yield stress, the shear rate and f is a positive continuously increasing function of the shear

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rate with f(0) = 0. In the particular case of a Bingham uid with a plastic viscosity p , f( ) = p In laminar regime, the drag force Fs on a sphere of diameter d with a moving velocity Vs in a Newtonian uid with viscosity writes: Fs = 3 dVs (2)

When studying segregation in concrete, the speed at which the physical phenomena take place is low enough to consider a succession of quasi static states. Thus, at equilibrium, the gravitational and buoyant force combination Fm on a sphere of density s in a uid of density f is equal to the drag force Fs : Fm = d3 (s f )g = Fs 6 (5)

The idea is to substitute in Eq. (2) the apparent viscosity to the Newtonian viscosity to reect the nonNewtonian nature of the uid surrounding the particle. The apparent viscosity a of a general yield stress uid writes if the shear stress overcomes the yield stress: a = 0 + f ( ) = (3)

Introducing Eq. (4) in Eq. (5), kd kVs (s f )g = 0 + f 18 d (6)

The absolute value of the moving velocity of the sphere becomes: Vs = d 1 f k kd |s f |g 0 18 (7)

In order to calculate the apparent viscosity, one needs to determine the shear rate around the particle. On a dimensional point of view, Vs /d is equivalent to a shear rate induced by particle to uid relative movement. It can then be equated to an average shear rate by introducing a constant k: =k Vs d (4)

If there is no segregation, there is no particle to uid relative movement. Vs is then equal to zero and Eq. (6) reduces to: d 0 |s f |g = 18 k (8)

The calculation of the average shear rate constant k is beyond the scope of this paper. However, it can be noted that it depends on the shape of the particles and on the thickness of the unyielded layer around the particle shown on Fig. 1. Ansley and Smith [9] obtained for a Bingham uid k = 24/7 1.09. For practical = purposes, as shown by He and co-workers [8], k may be treated as constant and equal to 1.

Eq. (8) constitutes a stability criterion. An alternative way to write this criterion is to state that, for segregation to occur, the sphere diameter has to be larger than a critical diameter dc for k = 1. Spheres smaller than dc are stable. dc = 180 |s f |g (9)

Fig. 1 Yielded and unyielded regions around a sphere moving in a non-Newtonian uid.

This means that, in a given granular repartition, if we neglect any interactions between particles or any lattice effects [3], some small particles may be stable while larger ones may be segregating. Moreover, the moving speed of these larger particles increases with their diameters. Whereas there exists a complete analytical solution for a sphere moving through a Newtonian uid [10], in the case of a yield stress uid, many solutions (but all approximated) can be found in the literature and compared with Eq. (9). Bethmond and co-workers [11] have shown that a general form of the previous criterion may be written

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as: dc = K0 |s f |g (10)

Let us focus on this aspect. The stress tensor decreases from the surface of the sphere to zero as the distance from the sphere tends to innity. It results that, beyond some critical distance, the yielding criterion is not satised, so that the uid should remain rigid despite sphere motion. This rigid region is bounded by a surface Sc surrounding the sphere beyond which the yielding criterion is not fullled. At the approach of Sc , the velocity tends towards zero so that the amplitude of the shear rate tends towards zero which implies that the shear stress tends towards 0 . When the sphere velocity decreases to zero (incipient motion or stoppage), Sc should approach S but the exact value of Sc stays unknown. The simplest approach [12] consists in assuming that, just when ow starts or stops, the force exerted by the uid corresponds to a shear stress vector at the surface of the object (S = Sc) of amplitude equal to the yield stress and directed tangentially to the sphere surface. The k value is then obtained by integration and is equal to 3 /2 4.71. This value is the lowest that can = be admitted on a theoretical point of view (a lower one would mean that Sc < S, which would be inconsistent). However, using plasticity theory, Hill [13] demonstrated that Sc does not tend towards S when the sphere velocity decreases. Some rigid zones are located at the top and the bottom of the sphere (Cf. Fig. 1) increasing the value of Sc and thus the theoretical value of K. The theoretical expression of Sc obtained in a similar manner by Ansley and Smith [9] leads to a K value equal to 21 /4 = 16.5. It has to be noted here that Saak and co-workers [5] used a relation obtained by [14] with K = 1.5. This relation can not be correct as K is lower than the minimum consistent value (4.71). This relation was however experimentally validated in [14] but it was followed by an erratum. In the present analytical work, the approximation used to obtain a solution lies in the k coefcient used in Eq. (4) that averages the shear rate eld inside Sc. From numerical simulations, Beris [15] obtained K = 20.97 and unyielded zones around the spheres very similar to the ones obtained analytically by Ansley and Smith [9]. This K value was used by Petrou and co-

workers in their very interesting experimental works [16, 17] on aggregate settlement in concrete. There is an even larger discrepancy on the experimental values of K that can be found in the literature. From an average experimental value on several various materials, Jossic and Magnin [18] obtained K = 17.24. But, in general, the existing data give signicantly dispersed values for K (between 11 and 25 [19]). This might be due either to the general uncertainty concerning the experimental determination of the incipient motion or of the yield stress from rheometrical tests. As it seems difcult to nd a denitive answer about the value of K, in the following, the value K = 18 obtained in Eq. (9) will be used. 2.2. Converging spheres in a Bingham uid and prediction of the nal compaction state after segregation What will happen to the particles that are moving if we neglect as a rst approximation the hydrodynamic interactions between particles (It will be demonstrated further in this paper that this assumption is of course not licit in the case of a concentrated suspension of spheres in a yield stress uid)? Let us consider a granular skeleton consisting of identical spheres (i.e. same diameter, same density). We assume in this part that the diameter of the spheres is higher than the critical diameter. Thus spheres start to move in the suspending uid and segregation occur. For identical spheres in a Bingham uid (plastic viscosity p , yield stress 0 ), the moving speed given by Eq. (7) is constant and is equal to Vs = d p d (s f )g 0 18

(11)

This means that, in an innite domain, as all the spheres move at the same speed, the average distance between spheres stay constant and is equal to the initial average distance that only depends on the initial solid fraction. However, during casting, the owing domain is not innite and some moving spheres reach a boundary (free surface, bottom of the formwork according to the sign of (s f ) and stop moving. As soon as some spheres stop moving, the spheres still moving are converging towards the xed ones. One could then expect the packing fraction in this zone to converge to

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the maximum random packing fraction of a group of spheres of identical diameters ( max = 0.74). In the case of ne particles, it has been demonstrated that after an initial sedimentation phase, a slow consolidation phenomenon takes place [20]. This is true with cement grouts, with clay suspensions and in general with any very small particles suspension, the permeability of which may reach low values when the solid concentration increases. The consolidation phase is in fact a sedimentation phenomenon slowed down by the difculty of the liquid to be drained out of the skeleton [21]. In the case of small particles with high surface forces involved, the sedimentation may be slowed down but the nal solid fraction will be more or less the maximum random packing of the particles. In the case of coarse particles (sand, gravel), on a theoretical point of view, the same Newtonian uid will always be able to instantaneously cross the skeleton. No consolidation phase should appear and the nal solid fraction after sedimentation should be the maximum random packing of a group of spheres. However, as it will be demonstrated here, when the particles are getting closer to each other, the non Newtonian nature of the suspending uid limits the solid fraction reached after segregation. The following phenomenon has to be kept in mind because it limits the segregation tendency of a given mixture : two converging spheres stop moving towards each other when the driving force (gravitational and buoyant force) becomes smaller than a critical value Fc . In fact, each couple of spheres generates in the separating gap a small squeezing ow. The needed driving force to bring the spheres closer to each other increases as the gap between the sphere decreases. In the case of two identical spheres moving towards each other in a Newtonian uid at a speed Vs , the force acting on one sphere is [22], 3 d2 Vs 4

will converge towards the maximum random packing fraction. This is not the case for a Bingham uid. By substituting the apparent viscosity of a Bingham uid in Eq. (12) and assuming that Eq. (4) still holds, one obtains: F= 3 d2 Vs p 3 d2 Vs (p + 0 ) 3d3 0 = + 4 4 4 (13) At sphere stoppage, Vs tends towards zero and Eq. (13) becomes: Fc = 3 0 d3 4 (14)

In the case of non identical spheres, a coefcient M may be introduced taking into account an eventual radius difference between the two spheres. In this case, d is the diameter of the smallest particle (read [23] for the general formulation of the problem). Fc = M 0 d3 (15)

M = 3 /4 when the spheres are identical. As the driving force Fm is given and known for a type of spheres and a given Bingham uid, it can be compared to Fc , which depends on the packing state. As the spheres are getting closer, Fc increases and, when Fm = Fc , the spheres stop converging. Thus, the packing fraction may be lower than the maximum random packing fraction and segregation may stop before this expected packing state. At stoppage, the gravitational and buoyant force combination Fm is equal to Fc . The shortest gap distance in this particular conguration writes: = 90 2|s f |g (16)

F=

(12)

with the shortest gap distance between the two spheres. This means that, for a given driving gravitational and buoyant force Fm = F, as is decreasing (spheres getting closer to each other), the speed at which the spheres are getting closer is decreasing. Thus, in the case of a Newtonian uid, it may take some time (without even taking into account the permeability of the whole skeleton) but the nal packing fraction

In the general case of non-identical spheres, Eq. (16) becomes: = 6M0 |s f |g (17)

The shortest gap distance between two spheres was linked to the sphere solid fraction by De Larrard [4] in terms of the particle diameter d and the maximum solid

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fraction o . =d
1 3

(18)

Knowing the yield stress of a given cement paste, the lowest value (i.e. the lowest gap distance between the spheres) that can be reached before spheres can not get closer can be calculated using Eq. (17). Using Eq. (18), the solid fraction associated to the obtained value may be calculated. This solid fraction is the one reached after segregation has occurred. It is the nal packing state. What happens if the calculated nal solid fraction is lower than the initial solid fraction? This means that the initial gap distance between the spheres is lower than the one that could be reached after segregation. This state can not of course be reached naturally but it can be reached during a mixing process, the energy of which reduces the value. Such a mix is very stable as, if one sphere moves, then it has to converge towards an other sphere. But, as the force needed is higher than gravity and buoyant forces, this can not happen and there can not be any sphere to sphere relative displacement. This means that the mixed solid fraction fulls the following criterion: 90 +1 2|s f |dg
3

(19)

Using the theory presented above and applied to identical spheres in a cement paste, several cases may be obtained and dealt with: Case 1: the diameter of the spheres is lower than the critical diameter given by Eq. (8) The spheres are stable. They do not have the ability to move as the stress generated by gravity and buoyant forces is not sufcient to overcome the cement paste yield stress. Case 2: the diameter of the spheres is higher than the critical diameter given by Eq. (8). The nal predicted solid fraction in the segregated zone using Eq. (17) and Eq. (18) is lower than the solid fraction initially mixed, which then fulls the inequality (19). The yield stress of the suspending uid is not sufcient to stabilize the spheres. However, they can not move as the gravity and buoyant forces combination is not sufcient to overcome the force needed to bring closer two spheres.

Case 3: the diameter of the spheres is higher than the critical diameter given by Eq. (8). The nal predicted solid fraction in the segregated zone using Eq. (17) and Eq. (18) is higher than the solid fraction initially mixed, which then does not full the inequality (19). The yield stress of the suspending uid is not sufcient to stabilize the spheres. They will move and a segregated zone will appear. The nal sphere volume fraction reached in this zone is the one predicted by Eq. (17) and Eq. (18) but is not equal to the maximum packing fraction of a group of spheres (except in the case of a purely Newtonian suspending uid). Finally, it should be kept in mind that, according to the two above criteria, segregation tendency in a given mixture depends on the yield stress of the suspending Bingham uid but not on its plastic viscosity. This afrmation is conrmed by Petrou and co-workers experimental results [16,17]. The plastic viscosity has of course an inuence on the separation velocity if the particle is not stable but does not affect whether or not the particle is stable. One could object that, if the plastic viscosity is high enough, then, even if the particle is not stable, the separation velocity will be so low that the displacement of the particles before setting will be negligible. To have an idea of the order of magnitude of the plastic viscosity that would be needed to prevent a sand (Dmax 4 mm, density 2700 kg/m3 ) from settling in a cement paste (density 1900 kg/m3 ), let us do the following calculation: We assume that segregation is negligible if the sand particles displacement before setting is less than 1 mm and that setting occurs after 4 hours. The settling velocity of the 4 mm sand particle should then be lower than 7.108 m/s. The viscosity needed to reach this velocity may be calculated using Eq. (11) for a yield stress equal to zero and is higher than 9000 Pa.s, which is at least 9000 times higher than a standard cement paste. Of course, one could try to nd an equilibrium between yield stress and plastic viscosity, to get a quasi-stable mixture but, most of the time, the chosen yield stress will have to be very close to the critical yield stress that fully prevents a sphere from moving under its own weight.

3. Experimental results In this part, experimental results are presented. They consist in the observation of the segregation of different

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87 Fig. 2 The vane test. Two different geometrics were used to cover the studied yield stress range. FL 10 geometry: height = 60 mm: radius = 20mm FL 100 geometry: height = 16 mm: radius: 11 mm

volume fractions of polystyrene aggregates in cement pastes displaying various yield stresses. The cement paste yield stress was measured using a Vane test procedure. After setting, each sample was cut in two halves and numerical pictures of the segregation state were taken. These images were analyzed and the nal solid fraction after segregation was calculated in each sample and compared to the solid fraction that was initially mixed.

3.1. Materials, preparation and rheological measurements 3.1.1. Materials The prepared suspending uids were cement pastes. Class A HTS cement was used. The superplasticizer (Chrysouid OPTIMA 100) amount was varied between 0.7 and 1% of the cement weight and the water to cement weight ratio W/C was varied between 0.26 and 0.30. The studied inclusions were polystyrene spheres (POLYSBETO c , BS Technologies S.A.). Their average diameter was 3.0 mm. The dispersion around this average value was about 0.5 mm and their random packing fraction was measured and equal to 0.70 0.01, which is higher than 0.63 for identical spheres. This results might come from the small size deviation of the polystyrene spheres used here.

3.1.3. Rheological measurements The yield stress of the cement paste was measured using a HAAKE ViscoTester R VT550 with a Vane tool similar to the one shown in Fig. 2. The yield stress of the various cement pastes was measured using the Vane procedure described by NGuyen and Boger [26]. The rotation speed was equal to 0.4 min1 . It can be noted that two different Vane test geometries were used to measure the yield stresses of the tested mixtures. Indeed, as the yield stresses of the studied mixtures varied from 0.1 Pa to several hundreds Pa, it was necessary to change the geometry of the rotating tool in order to measure an acceptable torque with a sufcient precision in the entire studied range of yield stresses. 3.2. Image analysis method The freeware ImageJ c [27] was used in this work. Each sample was carefully cut in two halves and numerical pictures of the cut section were taken. Because of the obvious colour difference between cement paste and polystyrene spheres, no further treatment of the obtained grey levels pictures was needed (Fig. 3(a)). When segregation occurred, a zoom on the converging zone was done (Figure 3(b)) in order to get rid of any edge effects. A threshold treatment was then applied on the picture (Fig. 3(c)). A granular analysis was carried out by the software (Fig. 3(d)) and the volume fraction

3.1.2. Preparation procedure The superplasticiser was introduced in the water and the obtained solution was mixed at 260 rpm for 60 s (mixer: Rayneri Turbotest). The cement was then added. The obtained suspension was mixed at 700 rpm for 15 min and then at 260 rpm for 15 min. This (long) mixing aims at giving the superplasticizer enough time to play its full role in the mixture and to limit any further irreversible evolution of the rheological behavior [24, 25]. One small sample was then used to measure the yield stress (see next section). The rest of the prepared cement pastes was carefully mixed by hand with the polystyrene spheres and poured in a cylindrical mould. It has to be noted that it seemed not technically possible in our experiments to incorporate a volume fraction of polystyrene spheres higher than 0.45.

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of the spheres in the studied zone was then calculated. In this paper, only the average volume fraction in the converging zone is studied and a simplied procedure could be used. If the initial sphere volume fraction is noted f0 , the height of the mould is h0 and the height of the converging zone is noted h1 (see Fig. 3(a)), the nal average volume fraction in the converging zone should be f0 h0 /h1 . Both methods give about the same results. This fact is important as it means that the sphere volume fraction is not far from being homogeneous in the converging zone. However, it should not be forgotten that this may not be the case for larger scale testing. The initial (mixed) and nal volume fractions of the tested samples are plotted on Fig. 4 in terms of the yield stress of the suspending cement paste. The squares represent the theoretical initial state of he sample and is in fact the spheres volume fraction initially mixed in the sample whereas the crosses represent the measured spheres volume fraction in the converging zones. If no segregation occurred, the plotted sphere and square representing a given mix can not be dissociated.

Fig. 3 (Continued) Fig. 3 Image analysis of the sample (a) Numerical picture of the segregated sample and studied zone. (b) Zoom on the converging zone. (c) Numerical picture after a threshold treatment. (d) Numerical picture after analysis. The total surface of the sample of the surface of the inclusions is calculated. (Continued)

4. Results analysis and discussion Depending on the yield stress of the cement paste, some of the prepared mixtures were stable while some others

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Fig. 4 Initial and nal packing state in terms of cement paste yield stress. The predicted sample nal solid fraction in the converging zone is plotted in dashed lines.

were not. In the particular case of the mixture with the cement paste displaying a 4.0 Pa yield stress, it was observed that most of the spheres were stable whereas the largest ones did move. This is a meaningful illustration of the critical diameter dened in Eq. (9). In this case, this critical diameter was equal to 3.5 mm, which is about the size of the largest spheres. For the studied spheres (average diameter = 3.0 mm), the predicted critical yield stress obtained with K = 18 in Eq. (10), under which the spheres are not stable, is 3.8 Pa. This limit is plotted as a straight line in Fig. 4. This theoretical boundary between stability and instability is in agreement with the obtained experimental results. For all the samples prepared with cement pastes with a yield stress lower than this value, the nal packing state was higher than the initial one. Moreover, from these experimental results, the K value in Eq. 10 can also be recomputed in the two cases below and above the critical yield stress. It is comprised between 17 and 29. This is in agreement with K = 18 obtained in the theoretical approach presented in this paper but it is not sufcient to conclude on the exact

value of this parameter. However, K = 18 seems like a safe and reasonable value. When segregation occurred, the nal volume fraction in the converging zone is of course higher than the initial one. But, as predicted by the theory proposed here, it is lower than the maximum packing fraction of a group of spheres (0.74). Apart from the value obtained with the cement pastes with the lowest yield stress (0.71 for 0.1 Pa), it is also lower than the random packing fraction measured for theses spheres (0.70). Moreover, it increases when the yield stress of the cement pastes (i.e. the suspending uid) decreases. Finally, the agreement between the nal predicted state and the measured one is good. It can be noted that the nal packing fraction in the converging zone does not depend on the initial volume fraction but just on the yield stress of the cement paste. It has however to be noted that the model predicts that the packing fraction tends towards the maximum packing fraction (0.74) when the yield stress tends towards zero. On a practical point of view, this could be reached but probably only by applying a strong vibration to the samples. As already suggested in the paper by Saak and coworkers [5], such stability criteria may be a basis for a mix design method. The rst criterion (Eq. (9)) allows the choice of the rheological behaviour of the suspending uid (cement paste or mortar) for a given granular materials (sand or gravel) whereas the second (Eq. (19)) allows the choice of the amount of granular materials. Of course, work is still needed to take into account the dispersion of the granular sizes, the non spherical shape of most granular materials and the possible overlap between particle species distribution. The gures given in the analysis below are certainly not correct but the underlying physics should stay the same. As a rst step, the use of the rst criterion (Eq. (9)) leads to the following yield stresses: a cement paste (density 1900 kg/m3 ) should display a yield stress of the order of magnitude of 2 Pa to prevent a sand (Dmax 4 mm; density 2700 kg/m3 ) from settling. Similarly, a mortar (density 2200 kg/m3 ) should display a yield stress of the order of magnitude of 10 Pa to prevent a gravel (Dmax 20 mm; density 2700 kg/m3 ) from settling. The second way to ensure stability of the mix is based on the second criterion. It consists in introducing enough granular materials in the mix for the mixed solid fraction to fulll the inequality (19) knowing that each particle on its own is unstable. The interactions between the particles should stabilize the mixture. In the case

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of a cement paste displaying a 2 Pa yield stress and the above sand, applying Eq. (19), one nds that, by introducing 900 kg/m3 , a stable mortar should be obtained. Similarly, in the case of a mortar displaying a 10 Pa yield stress and the above gravel, one nds that, by introducing 700 kg/m3 of gravel, a stable concrete should be obtained. In the approach proposed here, the strong evolution in time of the behaviour of cement pastes [28, 29] has not been taken into account. To study the consequences of this evolution on the segregation phenomenon, we have to separate two aspects: the thixotropic behaviour and the aging phenomenon. Thixotropy is by denition a reversible phenomenon. If a cement paste is left at rest, its occulation will increase. This occulation is however reversible by mixing the sample strongly enough. This is not the case with aging phenomenon, which affects in an irreversible way the rheological behaviour. In the case of a thixotropic material, a simplied way to describe what happens is the following: the yield stress is very low while the material is owing (low occulation of the suspension) but, as soon as the material stops (i.e. end of casting), the yield stress strongly increases (fast increase of the occulation state) and then keeps on increasing with time. This means that the 10 Pa yield stress needed to prevent the gravel from settling in the above example is the yield stress just after the end of casting. The fact that the yield stress keeps on increasing gives a further security against segregation. In the case of an aging material, an irreversible evolution of the rheological behaviour occurs. The yield stress may either increase (inuence of the hydration process for example) or decrease (delayed action of the superplasticizer for example), which can create strong instabilities in the material. The only way to take this risk into account in the above calculation is to carefully study the evolution in time of the rheological behaviour and introduce in the two above criteria the minimum value reached by the yield stress before setting.

demonstrated in the last part of this paper, this theoretical frame may be applied to study the stability of sand in a cement paste or gravels in a mortar. Two stability criteria have been written. The rst one deals with the stability of a single sphere in a yield stress uid while the second one takes into account the mechanical interactions between the particles that could lower the risk of instability. The two criteria have been experimentally validated in the case of polystyrene spheres in a cement paste. Image analysis techniques have been used to measure the nal solid fraction in the segregated zone. The comparison of the experimental and theoretical results was followed by an analysis of the possible use of such criteria in a mix tting method and a discussion of the inuence of the evolution of the rheological behaviour in time on the segregation phenomenon.
Acknowledgements The author would like to thank P. Coussot (LMSGC, France) for the always useful and pleasant scientic discussions.

References
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