ap-3-11.dvi Acta Polytechnica Vol. 51 No. 3/2011 Fracture Surfaces of Porous Materials T. Ficker Abstract A three-dimensional absolute profile parameter was used to characterize the height irregularities of the fracture surfaces of cement pastes. The dependence of these irregularities on porosity was studied and its non-linear character was proved. Ananalytical form for thedetectednon-linearitywas suggested and then experimentally tested. The surface irregularities manifest scale-invariance properties. Keywords: roughness analysis, fracture surfaces, cement-based materials, confocal microscopy. 1 Introduction The morphology of fracture surfaces have been stud- ied for a long time to reveal the details of fracture processes. However, in the research field of cementi- tiousmaterials therehavebeenonlya restrictednum- ber of studies that deal with surface features of frac- tured specimens. Some of the early surface studies of hydrated cement materials were focused on frac- tal properties [1,2] whereas others [3–5] investigated roughness numbers (RN) or similar surface charac- teristics [6–9]. When dealing with the roughness of the fracture surfaces of porousmaterials like cementitiousmateri- als, an important question arises, namely, what type of relationship is therebetweensurface roughnessand porosity. Recently, Ponson at al [10,11] have pointed to a close relationship between these two quantities. The authors studied the roughness of fracture sur- faces with glass ceramics made of small glass beads sintered in bulk with porosity P that could be var- ied in the interval (0,0.3). They observed that the roughness of the fracture surfaces increases linearly with increasing porosity (see their figure 3.3 in [10]). It would be valuable to know whether such a lin- ear behavior is a general property of all porous ma- terials, or only a specific feature of glass ceramics. For this reasonwe performed a large series of experi- ments with cement pastes. This material was chosen because its porosity can be easily controlled within a broad porosity interval by means of the water-to- cement ratio r = w/c. Correctknowledgeof the func- tional dependence of roughness on porosity may be useful for further surface studies of fractured porous materials. 2 Experimental arrangement Ordinary Portland cement CEM 42,5 I R-sc of do- mestic provenance was used to create 108 specimens of hydrated pasteswith six differentwater-to-cement ratios r (0.3, 0.4, 0.5, 0.6, 0.7, 0.8). The specimens were rotated during hydration to achieve better ho- mogeneity. All specimens were stored for the whole time of hydration at 100 % RH and 20◦C. After 60 days of hydration the specimens were fractured in three-point bending tests and the fracture sur- faceswere immediately used formicroscopic analysis. Other parts of the specimens were used for porosity measurements and for further mechanical tests. Porosity was determined by the common weight- volume method. The wet specimens were weighed and their volume wasmeasured, then they were sub- jected to 105◦C for one week until their weight no longer changed, and the dry specimens wereweighed again. The 3D profile parameter Ha was used to char- acterize the roughness of the fracture surfaces of the hydrated cement pastes. In fact, Ha represents the averaged ‘absolute’ height of the fracture relief z = f(x, y) Ha = 1 L · M ∫ ∫ (LM) |f(x, y)|dxdy (1) where L × M is the area of the vertical projection of the 3D fracture profile f(x, y) into the plane xy. Parameter Ha has great statistical relevancy, since it is a global averaged characteristic covering the en- tire tested surface L × M. The 3D profiles f(x, y) were created using the Olympus Lext 3100 confo- cal microscope. One of these profiles is shown in Figure 1. The profiles are formed by the software that processed a series of optical sections created by the confocal microscope at various heights of the fracture surfaces. Approximately 150 image sections were taken for each measured surface site, starting from the very bottom of the surface depressions (val- leys) and proceeding to the very top of the surface protrusions (peaks). The investigated area L × M = 1280 μm×1280 μm(1024 pixels×1024 pixels) was 21 Acta Polytechnica Vol. 51 No. 3/2011 Fig. 1: 3D confocal relief of fractured cement paste chosen in five different places of each fracture surface (in the center, and in four positions near the cor- ners of the rectangular area), i.e. each plotted point on the graphs of the profile parameters corresponds to an average value composed of 90 measurements (18 samples×5 surface measurements). Each mea- surementwasperformed for threedifferentmagnifica- tions, namely 5×, 20× and 50×, giving 270measure- ments thatwereperformed for the particular r-value. Since each site measurement amounts to about 150 optical sections (digital files), 40500 files had to be processed to create 270 digital maps per one r-value. This resulted in 1620 digital maps for all r-values altogether (6 r-values×270 maps for each r-value). These 1620 digital fracture surfaces were then sub- jected to 3D profile surface analysis. In this way an extensive statistical ensemble was created to provide a sufficiently reliable basis for drawing relevant conclusions. 3 Results and discussion Figure 2presents threedependences of Ha(P) formed within threemagnifications: 5×, 20×and50×. Their graphs do notmanifest linear behavior. All the three graphs show very similar shapes, which are well de- scribed by non-linear functions (curves in Figure 2) that can be expressed as follows Ha(P)= Ho (Po − P)β + ho (2) This is in fact a power-law function pointing to fractal-like properties. Relation (2) contains fourpos- itive fitting parameters Ho, Po, β, and ho, the mean- ings ofwhich canbe explained on the basis of asymp- totic patterns. Firstly, Po must always be greater than variable P , otherwise function (2) would be a decreasing function, and this would contradict the experimental data in Figure 2. This means that Po is the limiting value of porosity P when the water- to-cement ratio r goes to infinity Po = lim r→∞ P =1 (3) Assuming Po = 1 and P → 0 (material with ‘zero porosity’), the limiting roughness of the correspond- ing fracture surfaces reads lim P → 0 Po = 1 Ha(P)= Ho + ho (4) 22 Acta Polytechnica Vol. 51 No. 3/2011 Fig. 2: The dependence Ha(P) between the roughness of the fracture surfaces and the porosity of the cement paste Fig. 3: Normalized scale-invariant data Ha/M ax(Ha) in dependence on porosity P From (4) it follows that the sum Ho + ho represents the height irregularityat ‘zero porosity’. Since differ- entmagnifications provide different resolutions, ‘zero porosity’ will be determined differently for different magnifications, and thus the sum Ho + ho will also vary with magnification. The asymptotic form of Ha(P) when the material contains a very small but non-zero porosity value, e.g. 0 < P < 0.30 can also be useful for further consideration. In this case, the Taylor expansion of (2) may be utilized Ha(P) ≈ Ho P β o ( 1+ β P Po ) + ho = aP + b (5) a = βHo P 1+β 0 , b = Ho P β o + ho. (6) It is obvious from(5) that at sufficiently small porosi- ties the roughness of the fracture surfaces can be ap- proximated by a linear function Ha(P) ≈ aP + b, which is in agreement with the observation of Pon- son [10],whose experimentswith glass ceramics (P < 0.3) indicated such behavior (figure 3.3 in Ref [10]). Our data in Figure 2 does not contain a suffi- cient number of experimental points in the region of small porosities (P < 0.35), within which linear behavior can be observed. However, the clearly non- linear behavior of function Ha(P) at higher porosi- ties is a real fact illustrated by all the graphs in Figure 2. The interval P ∈ (0.35,0.50) is char- acterized by an abrupt non-linear increase, and at P > 0.50 rapid growth unmistakably continues fur- ther. With our specimens, these three intervals of porosities P < 0.35, P ∈ (0.35,0.50) and P > 0.50 correspond to the following water-to-cement ratios: r1 < 0.4, r2 ∈ (0.4,0.6) and r3 > 0.6, respec- tively. It is well known that at sufficiently small water-to-cement ratio values (r1 < 0.4), gel poros- ity dominates over capillary porosity in hydrated ce- ment pastes. Within the specimens mixed with in- termediate r-values r2 ∈ (0.4,0.6), capillary porosity starts to assume a governing role, and at still higher r-values r3 > 0.6 the porosity of the specimens is prevalently formed by capillary porosity. The over- all non-linear surface irregularity (2) of cementitious materials seems to be a result of the interplay be- tween gel and capillary porosities. As soon as the onset of capillary porosity appears, the height irreg- ularities of the fracture surfaces increase their values abruptly, as can be seen with all the graphs in Fi- gure 2 and still more straightforwardly with the two graphs in Figure 3, where the boundary between the 23 Acta Polytechnica Vol. 51 No. 3/2011 gel and the capillary porosities can be recognized at P ≈ 0.3. This effect can be characterized as a cross- over to larger scale porosities. It is interesting to note that the shapes of the graphs of functions Ha(P) shown inFigure 2 aremu- tually very similar, regardless of the magnifications that are used. In this connection, the question of their scale invariance arises. Thismeans that the de- pendence Ha(P) can be described by the same func- tional type (2), but with the fitting parameters Ho, Po, β, ho adapted to the results of the particular magnification. However, when these three functions are normalized by using the highest measured val- ues M ax(Ha), a unified function results (Figure 3A). Using the pattern of the unified function, the linear behavior of surface roughness at small porosities can be illustrated straightforwardly— see Figure 3B. The graph of the unified function shown in Fi- gure 3A represents the results of all three magnifica- tions used here— 5×, 20× and 50× — and it simul- taneously manifests the scale invariant properties of the height irregularities of the fracture surfaces. 4 Conclusion The experiments have proved a close relationship be- tween the roughness (height irregularities) of fracture surfacesandtheporosityofmaterials. The functional relationof these twoquantities is generallynon-linear and may be described by a power law function (2). When normalizing this function, it becomes indepen- dentof themagnification that is used. Thenon-linear behavior of Ha(P) with cement pastes is the result of the influence of gel and capillary porosities. The region of small gel porosities is characterized by a moderate (almost linear) increase in surface rough- ness Ha(P), whereas the region of capillary porosity is a domain with an abrupt increase in this quantity. The presentedproperties of the surface roughness of fracturedcementpastesmayalsobeuseful formor- phological and structural studies of other porousma- terials. Acknowledgement This work was supported by the Ministry of the Czech Republic under Contract no. ME09046 (Kon- takt). References [1] Lange, D. A., Jennings, H. M., Shah, S. P.: A fractal approach to understanding cement paste microstructure, Ceram. Trans. 16 (1992) 347–363. [2] Issa, M. A., Hammad, A. M.: Fractal charac- terization of fracture surfaces in mortar, Cem. Concr. Res. 23 (1993) 7–12. [3] Lange, D. A., Jennings, H. M., Shah, S. P.: Analysis of surface-roughness using confocal microscopy, J. 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M.: Roughness of fracture surfaces and compressive strength of hydrated cement pastes,Cem. Conr. Res. 40 (2010) 947–955. [10] Ponson, L.: Crack propagation in disordered Materials; How to decipher fracture surfaces, Annales de Physique 32 (2007) 1–120. [11] Ponson, L., Auradou, H., Pessel, M., Laza- rus, V., Hulin, J. P.: Failure mechanisms and surface roughness statistics of fractured Fontainebleau sandstone, Phys. Rev. E 76 (2007) 036108/1–036108/7. Prof. RNDr. Tomáš Ficker, DrSc. Phone: +420 541 147 661 E-mail: ficker.t@fce.vutbr.cz Department of Physics Faculty of Civil Engineering Brno University of Technology Veveř́ı 95, 662 37 Brno, Czech Republic 24