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**On measuring wettability in inﬁltration processing
**

´ 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 inﬁltration rates as a function of applied pressure. Such data are generally interpreted assuming slug-ﬂow. Using the Brooks–Corey correlations we relax this assumption, to indicate possible pitfalls of the slug-ﬂow approach and to show how such data can nonetheless be used to derive meaningful capillary parameters. Ó 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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

Many composite materials are produced by inﬁltration. This process is largely governed by capillarity, which acts to drive or oppose motion of the inﬁltrating ﬂuid into the porous solid preform to be inﬁltrated. 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 Young’s equation [3]: W i ¼ rlv cosðhÞ ¼ rsv À rsl ð1Þ where rlv is the surface tension of the liquid inﬁltrant, h ir its wetting angle on a ﬂat 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 ﬂat and large substrates. Also, wetting in inﬁltration is dynamic, which can inﬂuence h [3–5]. Direct methods are therefore often used to

measure capillary forces in inﬁltration; these come in two classes. The ﬁrst relies on the slug-ﬂow assumption [1,2,4,6,7]. In slug-ﬂow, inﬁltration takes place with a fully saturated inﬁltration front, across which there is a single pressure diﬀerence, 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 quantiﬁed, not with a single pressure diﬀerence but with curves plotting the capillary pressure vs. the fraction of ﬁlled void space (or ‘‘saturation’’), called drainage or imbibition curves, respectively, when the inﬁltrating ﬂuid does not wet, or wets, the solid [1,2,8–13]. 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 ﬁrst method. It rests on Darcy’s law written for fully saturated ﬂow, which states that the rate of ﬂow of a Newtonian and incompressible ﬂuid through a solid at suﬃciently low Reynolds number (typical of inﬁltration processing) is proportional to the local gradient of pressure P within the ﬂuid: vo ¼ À K rP g ð2Þ

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

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

which are well established in soil science. is predicted. DPc is inversely proportional to the average preform pore diameter) [20. and (ii) a ‘‘pore size distribution index’’ k that measures the spread in eﬀective pore diameter within the preform (the greater the spread. intersecting the horizontal axis at p = 1. IL). DPc is the capillary pressure. the governing equation becomes: h i dP d À2 K dV l dV l du g u¼ ð6Þ dV l to be solved with boundary conditions: u ¼ 0 ði:e: x ¼ 0 and t > 0Þ. Champ paign. when the front position is not dynamically tracked. P. this. at x = L. then the position of the inﬁltration front. Pb is inversely proportional to the average pore diameter. [20. We now consider the same experiment. A. the Brooks and Corey correlation reads: k Vl Pb ¼1À ð9Þ Sl ¼ 1ÀVs P and h i ð2þkÞ K ¼ K sat S 2 1 À ð1 À S l Þ k l ð10Þ where x = 0 is the preform entrance. all else being constant. The inﬁltration front position. V l ¼ V l ðDP T Þ ð7Þ Here. which is generally the case in composite processing. Methods vary. DPT. [23. these are known in the form of semiempirical correlations. (3) applies. (6) and integrating once subject to Eq. including in composite material processing [8.9. however. (8) yields: Àðkþ1Þ Z du S l K sat P b ð1 À S l Þ k uðsÞ ds ¼ À2 dS l 0 ð1 À V s Þg k Â S 2 ½1 À ð1 À S l Þ l ð2þkÞ=k ð11Þ This non-linear integro-diﬀerential equation is solved numerically for the function u(Sl) subject to Eq. increases. k tends towards inﬁnity since the preform structure tends towards one of perfectly uniform pores (e. (7) using Mathematica (Wolfram Research Inc.g. after substitution of Eqs. We use hereafter the correlations of Brooks and Corey.34]. of course. Mortensen / Scripta Materialia 56 (2007) 859–862 where the ﬂuid ‘‘superﬁcial velocity’’ vo is the volume of ﬂuid passing through a unit surface cut across the porous medium per unit time. Inﬁltration thus proceeds gradually. but reproducible values that obey expectations are often obtained (e. We deﬁne: x ð5Þ u ¼ pﬃ t and. Michaud. namely the inﬁltration along a single direction (x) of a non-deforming preform driven by a constant pressure. L2 for a ﬁxed inﬁltration time t) vs.38–40].2. (3).. Mass conservation dictates: ovo oV l ¼À ð4Þ ox ot where Vl is the local volume fraction liquid in the preform.g. all curves gradually become straight lines of slope unity. Measurements of capillary pressure drop values conducted in this manner have been published by many authors. for unidirectional inﬁltration driven by a constant pressure the problem can be solved using the Boltzman transformation [8.g.35–37]. (4) and (2) into Eq. and Vl itself varies between 0 and (1 À Vs) as the local pressure in the liquid. which is the ﬁrst pressure at which the liquid penetrates the preform.31]. the liquid saturation Sl depends on P via (i) the ‘‘bubbling pressure’’ Pb. a bundle of straight capillaries) and Eq. Substituting Eqs. as p increases. over a range of pressures described by the drainage–imbibition curve [1. and have been successfully confronted with experimental data [32. deﬁning the inﬁltration front position as TM F ¼ ðufront Þ 2 ð1 À V s Þg 2K sat P b ð12Þ while dimensionless applied pressure is deﬁned as p¼ P Pb ð13Þ This adimensionalization of pressure and inﬁltration velocity is such that inﬁltration under slug-ﬂow will give a straight line of slope 1. The results of this calculation are plotted in Figure 1 in adimensional form. The method.32]. ufront t. When h > (p/2).31]. and Vs is the volume fraction of solid phase in the preform. Solving the problem requires knowledge of the two functions K(Vl) and Vl(P). As is well known. When the total pressure diﬀerential DPT driving the motion of the ﬂuid is kept constant. assumes slug-ﬂow while in many such experiments there is clear evidence that ﬂow is not fully saturated (e. in this case DPc = Pb. DPT then yields a straight line that intersects the abscissa axis at DPT = DPc. an extensive review of the subject is given in Refs. .27]). As seen. Practically.10–13. The permeability K is now a function of Vl. Plotting L2/t (or. In slug-ﬂow continuity dictates that vo be constant everywhere along the inﬁltrated preform. (9) and (10) in Eq. Ksat is the permeability of the fully saturated preform. is: L2 ¼ 2Kt ðDP T À DP c Þ gð1 À V s Þ ð3Þ and u ¼ ufront .6. but assume unsaturated ﬂow. to measure DPc one produces an experimental set-up such that inﬁltration of a homogeneous and non-deforming preform takes place along a single direction parallel to a principal direction (Ox) of K.860 V.33. for both polymer and metal composite systems [4. (3)). the smaller is k). Indeed. 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 ﬂuid (in Pa s). Vl ¼0 ð8Þ 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. is the measured quantity L in slug-ﬂow inﬁltration experiments (Eq.14–30]. counted positive when it opposes inﬁltration.

which is simply computed from Eq. and (ii) the pore size distribution index k. Analyzing results from the present calculations. Graphic validation of the correlation given in Eq. i. for k = 1. as a simple function of Pb and k. it turns out that Pex can be expressed. for various values of k. drainage/imbibition curves can then be used to measure directly the work of immersion Wi. as the degree of pore uniformity decreases. If. such as 2 [8. namely: k þ 0:71 ð14Þ P ex ¼ P b kÀ1 as shown in Figure 3. Therefore.V. i. (14). (3).38–40]. which is measured directly. method described above. as k decreases. DPc. the curve becomes increasingly linear. According to Eq.9. Given the ﬁnite experimental error that comes in such experiments. Also. which increasingly exceeds Pb as k decreases. then taking the intercept of the resulting straight line with the horizontal axis. Ref. if inﬁltration of the porous solid preform by the liquid takes place quasi-statically. as the degree of uniformity of pore size and pore geometry within the preform increases. Pex. slug-ﬂow-based. (1) – provided again that inﬁltration takes place quasi-statically. a suﬃciently wide range of applied pressures is explored that the strictly linear portion of the curve is obtained. Suppose now that a series of experiments be conducted to measure the capillary pressure according to the ﬁrst. the diﬀerence between Pex and Pb is quite signiﬁcant (Fig. over the range of k explored here. Then. Since Rl can be measured directly using the BET technique. showing extensive non-linearity at lower values of P and illustrating the deﬁnition of Pex. experiments of the ﬁrst type. it is still possible to use the data to arrive Figure 2.57 (observed with Saﬃl alumina short ﬁbres). vs. provided the range of pressures explored in experiments of the ﬁrst type is made suﬃciently wide to obtain both (i) a trustworthy value for the lowest (or ‘‘bubbling’’) pressure Pb at which the inﬁltrant ﬁrst penetrates the preform and (ii) the strictly linear. A. Figure 3. Now. For realistic values of k. [25]). Rl. although Pex itself has no direct fundamental signiﬁcance. data are most conveniently plotted as L2 divided by t (i. will yield a pressure. 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.e. deﬁned in Eq. (ufront)2). (14) as: k¼ P ex þ 0:71P b P ex À P b ð15Þ We also note that. Adimensional inﬁltration front kinetic parameter F as a function of P/Pb. Michaud. namely (i) the bubbling pressure Pb. on the other hand. the integral of the drainage curve Z 1 Z 1 k ¼ W i Rl P dS l ¼ P b ð1 À S l ÞÀ1=k dS l ¼ P b ðk À 1Þ 0 0 ð16Þ is the work of immersion Wi. (14). this is a pitfall that will easily be encountered in practice. 1). at the two parameters that describe the drainage curve according to the Brooks and Corey correlation. inserting Eq. that has no physical meaning. k. Adimensional inﬁltration front kinetic parameter F as a function of P/Pb. can also be used to assess Wi as: . 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.g. as illustrated in Figure 2 for a low value of k. Examining Figure 1. as k increases. high-pressure portion of the curves in Figure 1.e. multiplied by the total area of preform/inﬁltrant interface created per unit volume of liquid inﬁltrated into the preform. (16) into Eq. examples of non-linear plots such as those in Figure 1 can be found in many studies (e. much of the data from experiments of this type may lie within the non-linear portion of the curve. Mortensen / Scripta Materialia 56 (2007) 859–862 861 Figure 1. DPT: this is simply a dimensional form of Figure 1.e. conducted over a suﬃciently wide range of pressures to measure both Pb and Pex.

Jones. Acta Materialia 50 (2002) 247–257. E.A. Journal of Materials Science 32 (1997) 289–294. Molina. Zweben. New York. A.H.C.A. Manson. [38] H. Geothermics 35 (2006) 198. 3 Colorado State University Hydrology Papers. [14] K. T. Materials Park. Pamies. Mortensen. [24] T.E. Miller.). Kaufmann. Corey. L. Ahn. This work was supported by core funding of the authors’ respective laboratories at EPFL. Volume editor: T. therefore. Bear. Sanchez. [12] R. Pergamon. Louis. Composites Part A-Applied Science and Manufacturing 37 (2006) 92–102. 1979. Society of Petroleum Engineers. New York. A. Verrey. [19] J. the intercept of the resulting straight line with the pressure axis leads to a quantity. Narciso. H. Weber. [33] J. Mortensen. Louis.W. Saravanan. Introduction to Modeling of Transport Phenomena in Porous Media.M. E. SPE Annual Technical Conference. Narciso. G. Molina. E. in: S. to be expected.R. Berg. however. E. J. [16] A. Atkinson. [29] P.-Y. Pex.J. Muscat. Olson. direct measurements of a capillary pressure drop based on inﬁltration kinetics interpreted using the slug-ﬂow assumption can lead to data that have little fundamental meaning. Fluid Transport and Pore Structure. H. ´ [20] J. Wettability of SiC Particulates with Zn and Zn–Al Alloys. J.L. Louis. Li. [6] A. Asthana.C.R.862 V. Michaud.). S.Y. . Rodriguez-Guerrero. Lekakou. Metallurgical Transactions 25A (1994) 2357–2370. A. Rodriguez-Reinoso. Metallurgical Transactions 23A (1992) 2071–2073. Metallurgical Transactions 21B (1990) 475–485. 26–29 September 2004 SPE paper No. Journal of Colloid and Interface Science 122 (1988) 24–34. Garcia-Cordovilla. University of Toronto Press. 1983. J. L. Maxwell. Philip. J. C.C. Bahraini. Wettability at High Temperature. Pinero. Elsevier Science. Narciso. [17] A.V. J. in: Comprehensive Composite Materials. J. Mortensen. Metallurgical Transactions 25A (1994) 2145–2152. p. F. 1999. Amico. Bachmat. chapter 21. E. E.A. Journal of Materials Science 40 (2005) 2487. Hydraulic Properties of Porous Media. Narciso. Dullien. Philip. [13] F. Cornie. K. 1990. [7] Y. particularly at low saturations. 521–554. Yang. M. we expect the basic conclusions of this note to remain valid. Polymer Composites 12 (1991) 146–152. L. R. Clyne (Ed. Dordrecht. Metallurgical Transactions 26A (1995) 1491–1497. [35] R. Pergamon. 1974. [30] J. The Physics of Flow through Porous Media. A. Louis.P. Candan. Louis. R. Greenkorn. Cornie. 89874. [31] C. Louis. Scheidegger. Michaud. Seferis. C. P. Eustathopoulos. H. Scripta Materialia 36 (1997) 363–368. Journal of Materials Science 40 (2005) 2519. Narciso. E.A.M. Michaud.C. [40] M. Cornie. Toronto. Houston. Dhingra (Eds. G. E. C.M. [18] J. [28] D. Kida. Rohatgi. S. Louis. Narciso. [9] T. the diﬀerence between Pex and WiRl is less than 14%. A. other correlations could have been used to link pressure with saturation and relative permeability in the calculations. Edwards. In conclusion. Narciso. Also. Rodriguez. J. H. J. B.N. Bear.L.E. V. Russell. J. Tian. Mortensen. ASM International. Water Resources Research 5 (1969) 1070– 1077. Oxford. Garcia-Cordovilla. [15] S. Kluwer Academic Publishers. Drevet. These are known to be good descriptors of overall drainage curves. Composites Part A-Applied Science and Manufacturing 32 (2001) 981–996. Acta Materialia 54 (2006) 1821. [25] E. Marcel Dekker. that when pressures explored in experiments of this type include both the lowest pressure for inﬁltration. V. Academic Press.F.A. D. A. Mortensen. Sanchez. A. [8] V. J.C. Metallurgical Transactions 26A (1995) 983–990. J. in: vol. R. [32] J. C. [21] J. Horne. Kistler.G. [11] A. Bahraini. TX. We ﬁnally emphasize that all that precedes is based on the semi-empirical correlations of Brooks and Corey.A. Martins. New York. Zograﬁ. 2000.T. Pinero.K. [22] S. GarciaCordovilla. Narciso. Narciso. Dopler. Scripta Materialia 53 (2005) 1483. JoseMiguel Molina and Dr. Y. E. 2004. [3] N. Flow Phenomena in Porous Media. if unsaturated ﬂow obtains. if k is greater than 5. and the high-pressure linear portion of the curve giving L2/t vs. J. Marcel Dekker. [39] M. American Elsevier.A.G. Dynamics of Fluids in Porous Media. Alonso. R. [27] R. Composites Science And Technology 61 (2001) 1945–1959. Narciso. Weber. F. Zeitschrift fur Metallkunde 83 ¨ (1992) 887–892. E. OH. Arpon. A. Acta Materialia 47 (1999) 4461–4479. [26] S. J. G. Mortensen. New York. [34] J. Modaressi. Drew. that can be used to arrive at the two parameters needed to describe more rigorously wetting for the system at hand. Metallurgical Transactions 21A (1990) 2257–2263. Jonas. We also ´ acknowledge interesting discussions with Dr. Garcıa-Cordovilla.A. Soil Science 83 (1956) 345–357. Melt inﬁltration of metal matrix composites. We also show. we show that. Metallurgical and Materials Transactions B-Process Metallurgy And Materials Processing Science 31 (2000) 225–234.R. Oh. we observe that. A. pp. [37] K. (17). Fletcher. A. Louis. Nicholas. M.L.W. Hydrodynamics of Wetting. Jones. Porous Media. Kelly and C. J.A. Li. Volume 3: Metal Matrix Composites. Current Opinion in Solid State and Materials Science 9 (2005) 196. 21–25. Brooks. Current Opinion In Solid State & Materials Science 9 (2005) 202–210. 27. E. Deviations from predictions above are. [1] V.R. Metallurgical Transactions 20A (1989) 527–532. Materials Science and Engineering A A173 (1993) 233–237. Michaud.B.J. Russell. K. Series editors A. [10] J.E. [4] J. Rodriguez-Reinoso. 1988. Wong. Mortensen / Scripta Materialia 56 (2007) 859–862 Wi ¼ P ex þ 0:71P b 1 Rl 1:71 ð17Þ From Figure 3 and Eq. but deviations exist. Mortensen.K. Russell.R. K. Chong. P. Fishman.V. Ludger Weber. and will therefore generally be within experimental scatter. 1993. Garcia-Cordovilla. C. Atkinson. [5] S. Cast Reinforced Metal Composites. [36] K. J. pp. A. 1972. Michaud. Compton. [23] T. Amsterdam. [2] A. using analysis based on the Brooks–Corey correlations. 1964. Pb. Molina.

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