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Veronique Michauda,* and Andreas Mortensenb

a

Laboratory for Polymer and Composite Technology (LTC), Ecole Polytechnique Federale de Lausanne (EPFL), Station 12, CH-1015 Lausanne, Switzerland b Laboratory for Mechanical Metallurgy, Ecole Polytechnique Federale de Lausanne (EPFL), Station 12, CH-1015 Lausanne, Switzerland

Received 3 January 2007; revised 31 January 2007; accepted 1 February 2007 Available online 26 February 2007

Capillary pressures encountered in composite processing are often evaluated by measuring inltration rates as a function of applied pressure. Such data are generally interpreted assuming slug-ow. Using the BrooksCorey correlations we relax this assumption, to indicate possible pitfalls of the slug-ow approach and to show how such data can nonetheless be used to derive meaningful capillary parameters. 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Inltration; Composites; Capillary phenomena; Wetting; Threshold pressure

Many composite materials are produced by inltration. This process is largely governed by capillarity, which acts to drive or oppose motion of the inltrating uid into the porous solid preform to be inltrated. Quantifying capillary forces, by analysis or measurement, is of obvious importance in understanding the process. In the absence of interfacial reactions (which are important in some systems but complicate the problem immensely), the relevant thermodynamic parameter is the work of immersion Wi [1,2]. According to Youngs equation [3]: W i rlv cosh rsv rsl 1 where rlv is the surface tension of the liquid inltrant, h ir its wetting angle on a at solid substrate, and rsv and rsl are the solid/atmosphere and solid/liquid interfacial energy, respectively. Both rlv and h, and hence Wi, are measurable directly using the sessile drop technique [3]; however, this technique is often not usable for systems of relevance to composite processing. Reinforcement materials are generally not available as at and large substrates. Also, wetting in inltration is dynamic, which can inuence h [35]. Direct methods are therefore often used to

measure capillary forces in inltration; these come in two classes. The rst relies on the slug-ow assumption [1,2,4,6,7]. In slug-ow, inltration takes place with a fully saturated inltration front, across which there is a single pressure dierence, DPc, caused by curved menisci of the liquid surface as with a liquid in a straight capillary tube. The second approach is based on methods that were developed in soil science and reservoir engineering. Here, capillary forces are quantied, not with a single pressure dierence but with curves plotting the capillary pressure vs. the fraction of lled void space (or saturation), called drainage or imbibition curves, respectively, when the inltrating uid does not wet, or wets, the solid [1,2,813]. This approach is more complex and also somewhat more cumbersome experimentally, hence it is more rarely adopted in the study of composite processing. However, it is fundamentally more correct. The point of this note is to examine the former approach in light of theory underlying the second. Consider the rst method. It rests on Darcys law written for fully saturated ow, which states that the rate of ow of a Newtonian and incompressible uid through a solid at suciently low Reynolds number (typical of inltration processing) is proportional to the local gradient of pressure P within the uid: vo K rP g 2

* Corresponding author. Tel.: +41 21 693 49 23; fax: +41 21 693 58 80; e-mail: veronique.michaud@ep.ch

1359-6462/$ - see front matter 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.scriptamat.2007.02.002

860

where the uid supercial velocity vo is the volume of uid passing through a unit surface cut across the porous medium per unit time, K is the permeability of the porous medium (in the most general case a tensor and of units m2) and g is the viscosity of the uid (in Pa s). Practically, to measure DPc one produces an experimental set-up such that inltration of a homogeneous and non-deforming preform takes place along a single direction parallel to a principal direction (Ox) of K. In slug-ow continuity dictates that vo be constant everywhere along the inltrated preform. When the total pressure dierential DPT driving the motion of the uid is kept constant, then the position of the inltration front, at x = L, is: L2 2Kt DP T DP c g1 V s 3

and u ufront ; Vl 0 8 where Vl(DPT) is the fraction liquid in the preform for P = DPT and ufront is the value of u at the tip of the liquid front advancing into the preform. Solving the problem requires knowledge of the two functions K(Vl) and Vl(P); these are known in the form of semiempirical correlations. We use hereafter the correlations of Brooks and Corey, which are well established in soil science, and have been successfully confronted with experimental data [32,3537], including in composite material processing [8,9,3840]. When h > (p/2), which is generally the case in composite processing, the Brooks and Corey correlation reads: k Vl Pb 1 9 Sl 1Vs P and h i 2k K K sat S 2 1 1 S l k l 10

where x = 0 is the preform entrance, DPc is the capillary pressure, counted positive when it opposes inltration, and Vs is the volume fraction of solid phase in the preform. Plotting L2/t (or, when the front position is not dynamically tracked, L2 for a xed inltration time t) vs. DPT then yields a straight line that intersects the abscissa axis at DPT = DPc. Measurements of capillary pressure drop values conducted in this manner have been published by many authors, for both polymer and metal composite systems [4,6,1430]; an extensive review of the subject is given in Refs. [20,31]. Methods vary, but reproducible values that obey expectations are often obtained (e.g. DPc is inversely proportional to the average preform pore diameter) [20,31]. The method, however, assumes slug-ow while in many such experiments there is clear evidence that ow is not fully saturated (e.g. [23,27]). We now consider the same experiment, namely the inltration along a single direction (x) of a non-deforming preform driven by a constant pressure, DPT, but assume unsaturated ow. Inltration thus proceeds gradually, over a range of pressures described by the drainageimbibition curve [1,2,1013,32]. Mass conservation dictates: ovo oV l 4 ox ot where Vl is the local volume fraction liquid in the preform. The permeability K is now a function of Vl, and Vl itself varies between 0 and (1 Vs) as the local pressure in the liquid, P, increases. As is well known, for unidirectional inltration driven by a constant pressure the problem can be solved using the Boltzman transformation [8,33,34]. We dene: x 5 u p t and, after substitution of Eqs. (4) and (2) into Eq. (3), the governing equation becomes: h i dP d 2 K dV l dV l du g u 6 dV l to be solved with boundary conditions: u 0 i:e: x 0 and t > 0; V l V l DP T 7

Here, the liquid saturation Sl depends on P via (i) the bubbling pressure Pb, which is the rst pressure at which the liquid penetrates the preform, and (ii) a pore size distribution index k that measures the spread in eective pore diameter within the preform (the greater the spread, the smaller is k). Pb is inversely proportional to the average pore diameter, all else being constant. Ksat is the permeability of the fully saturated preform. Substituting Eqs. (9) and (10) in Eq. (6) and integrating once subject to Eq. (8) yields: k1 Z du S l K sat P b 1 S l k us ds 2 dS l 0 1 V s g k S 2 1 1 S l l

2k=k

11

This non-linear integro-dierential equation is solved numerically for the function u(Sl) subject to Eq. (7) using Mathematica (Wolfram Research Inc., Champ paign, IL). The inltration front position, ufront t, is predicted; this, of course, is the measured quantity L in slug-ow inltration experiments (Eq. (3)). The results of this calculation are plotted in Figure 1 in adimensional form, dening the inltration front position as

TM

F ufront

1 V s g 2K sat P b

12

This adimensionalization of pressure and inltration velocity is such that inltration under slug-ow will give a straight line of slope 1, intersecting the horizontal axis at p = 1. Indeed, in this case DPc = Pb, k tends towards innity since the preform structure tends towards one of perfectly uniform pores (e.g. a bundle of straight capillaries) and Eq. (3) applies. As seen, as p increases, all curves gradually become straight lines of slope unity.

861

Figure 1. Adimensional inltration front kinetic parameter F as a function of P/Pb, for various values of k.

Also, as k increases, i.e. as the degree of uniformity of pore size and pore geometry within the preform increases, the curve becomes increasingly linear. Suppose now that a series of experiments be conducted to measure the capillary pressure according to the rst, slug-ow-based, method described above. According to Eq. (3), data are most conveniently plotted as L2 divided by t (i.e. (ufront)2), vs. DPT: this is simply a dimensional form of Figure 1. Examining Figure 1, as the degree of pore uniformity decreases, i.e. as k decreases, much of the data from experiments of this type may lie within the non-linear portion of the curve; examples of non-linear plots such as those in Figure 1 can be found in many studies (e.g. Ref. [25]). Running a straight line through a limited set of data and extrapolating to the horizontal axis will then lead to a measured apparent capillary pressure drop, DPc, that has no physical meaning. Given the nite experimental error that comes in such experiments, this is a pitfall that will easily be encountered in practice. If, on the other hand, a suciently wide range of applied pressures is explored that the strictly linear portion of the curve is obtained, then taking the intercept of the resulting straight line with the horizontal axis, as illustrated in Figure 2 for a low value of k, will yield a pressure, Pex, which increasingly exceeds Pb as k decreases. For realistic values of k, such as 2 [8,9,3840], the dierence between Pex and Pb is quite signicant (Fig. 1). Now, although Pex itself has no direct fundamental signicance, the fact that it increasingly deviates from Pb as k decreases suggests that the deviation between the two may be used to access the pore size distribution index, k. Analyzing results from the present calculations, it turns out that Pex can be expressed, over the range of k explored here, as a simple function of Pb and k, namely: k 0:71 14 P ex P b k1 as shown in Figure 3. Therefore, provided the range of pressures explored in experiments of the rst type is made suciently wide to obtain both (i) a trustworthy value for the lowest (or bubbling) pressure Pb at which the inltrant rst penetrates the preform and (ii) the strictly linear, high-pressure portion of the curves in Figure 1, it is still possible to use the data to arrive

Figure 2. Adimensional inltration front kinetic parameter F as a function of P/Pb, for k = 1.57 (observed with Sal alumina short bres), showing extensive non-linearity at lower values of P and illustrating the denition of Pex.

at the two parameters that describe the drainage curve according to the Brooks and Corey correlation, namely (i) the bubbling pressure Pb, which is measured directly, and (ii) the pore size distribution index k, which is simply computed from Eq. (14) as: k P ex 0:71P b P ex P b 15

We also note that, if inltration of the porous solid preform by the liquid takes place quasi-statically, the integral of the drainage curve Z 1 Z 1 k W i Rl P dS l P b 1 S l 1=k dS l P b k 1 0 0 16 is the work of immersion Wi, multiplied by the total area of preform/inltrant interface created per unit volume of liquid inltrated into the preform, Rl. Since Rl can be measured directly using the BET technique, drainage/imbibition curves can then be used to measure directly the work of immersion Wi, dened in Eq. (1) provided again that inltration takes place quasi-statically. Then, inserting Eq. (16) into Eq. (14), experiments of the rst type, conducted over a suciently wide range of pressures to measure both Pb and Pex, can also be used to assess Wi as:

862

Wi

P ex 0:71P b 1 Rl 1:71

17

From Figure 3 and Eq. (17), we observe that, if k is greater than 5, the dierence between Pex and WiRl is less than 14%, and will therefore generally be within experimental scatter. We nally emphasize that all that precedes is based on the semi-empirical correlations of Brooks and Corey. These are known to be good descriptors of overall drainage curves, but deviations exist, particularly at low saturations. Also, other correlations could have been used to link pressure with saturation and relative permeability in the calculations. Deviations from predictions above are, therefore, to be expected; however, we expect the basic conclusions of this note to remain valid. In conclusion, we show that, if unsaturated ow obtains, direct measurements of a capillary pressure drop based on inltration kinetics interpreted using the slug-ow assumption can lead to data that have little fundamental meaning. We also show, using analysis based on the BrooksCorey correlations, that when pressures explored in experiments of this type include both the lowest pressure for inltration, Pb, and the high-pressure linear portion of the curve giving L2/t vs. P, the intercept of the resulting straight line with the pressure axis leads to a quantity, Pex, that can be used to arrive at the two parameters needed to describe more rigorously wetting for the system at hand. This work was supported by core funding of the authors respective laboratories at EPFL. We also acknowledge interesting discussions with Dr. JoseMiguel Molina and Dr. Ludger Weber.

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