E & P

E X C H A N G E

TWO SEM TECHNIQUES TO INVESTIGATE

RESERVOIR-ROCK WETTABILITY
Michel Robin, SPE, Inst. Franais du Ptrole; Rossana Combes, Marne-la-Valle U.;
and Louis Cuiec, SPE, Inst. Franais du Ptrole

In 1989, Inst. Franais du Ptrole initiated a research program on

the use of cryo scanning electron microscopy (CSEM) in wettability studies. The program led to important results concerning the
role of mineralogy (presence and nature of clays) and pore-size distribution (particularly in the case of carbonates) in the coexistence
of two networks (water wet and oil wet) in so-called mixed-wettability systems.1
The study established that kaolinite found in some clayey sandstone reservoir rocks that is originally preferentially water wet
could, after aging under initial-water-saturation conditions, constitute an oil-wet network, while quartz and illite remain water-wet.
In carbonate rocks, the study led to the deduction that a water-wet
network was made of small pores, while large pores were at the origin of the oil-wet network.
This technique also has been used successfully to study the effect
of wettability and spreading on the distribution of three phases
(water, oil, and gas) within the pore structure and the efficiency of
a gas injection at the pore scale.2 The shortcomings of the technique, however, are that it requires freezing of the rock/fluids and
that it gives a static picture of wetting.
Another research program was launched in 1994 in collaboration with Marne-la-Valle U. to evaluate the potential of environmental SEM (ESEM) to determine the distribution of oil and water
within a porous medium and to observe the dynamics of wetting.

Fig. 1Dry sintered-glass sample.

NOVEMBER 1998

This new method allows investigation of rock samples in the presence of liquids (both oil and brine) without freezing and coating.
Also, fluids can be introduced directly into the observation chamber; consequently, dynamic experiments can be observed (e.g., capillary rise of a wetting fluid in the presence of a nonwetting fluid).
For these observations, the contrast is mainly topographic, presenting a great depth of field (Fig. 1). A slight chemical contrast is
superimposed because of the presence of backscattered electrons.
Chemical contrast is directly related to the variation of the mean
atomic number Z, allowing differentiation between the mineral
(Z=11, light), the brine (Z=7, medium gray), and the oil (Z=5.5,
dark gray).
Experiments first were performed with very simple model
porous media consisting of sintered-glass beads specially treated to
become strongly oil wet. Spontaneous oil imbibition in such cores
saturated with brine was observed on the top of the sample as dark
rings appearing at the edge of the beads (Fig. 2).
Robin et al.3 conducted similar studies on reservoir rocks of
intermediate wettability (spontaneously imbibing either brine or
oil). Their studies showed wettability heterogeneity at the pore
scale, leading to a mixed wettability at a macroscopic scale, and

(SPE 52526)

Fig. 2Oil imbibition in oil-wet sintered glass.

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Fig. 3North Sea sandstone, appearance of oil in a pore filled

by kaolinite.

also demonstrated the influence of composition, size, and distribution of minerals on physicochemical behavior of the sample
toward fluids.
In the mixed-wettability sandstone, oil capillary rise occurred
through kaolinite zones (Fig. 3), while for carbonate, oil capillary
rise occurred through the largest pores (Fig. 4). This was in agreement with the static observation made with CSEM.
Both CSEM and ESEM techniques must be considered as very efficient tools for studying heterogeneous systems. They offer new
perspectives for understanding the influence of surface-properties
distribution on two- and three-phase displacements.

NOVEMBER 1998

Fig. 4Middle East carbonate, appearance of oil in a large pore.

REFERENCES
1. Fassi-Fihri, O., Robin, M., and Rosenberg, E.: Wettability Studies at the
Pore Level: A New Approach by the Use of Cryo-Scanning Electron
Microscopy, SPEFE (March 1995) 11.
2. Vizika, O., Rosenberg, E., and Kalaydjian, F.: Study of Wettability and
Spreading Impact in Three-Phase Gas Injection by Cryo-Scanning Electron Microscopy, J. Petroleum Science & Engineering, (June 1998) 189.
3. Robin, M. et al.: Wettability of Porous Media from Environmental Scanning Electron Microscopy: From Model to Reservoir Rocks, paper SPE
37235 presented at the 1997 SPE International Symposium on Oilfield
Chemistry, Houston, 1821 February.

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