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ABSTRACT: A capacitive sensor-based apparatus is used to study the ice-water phase change in consolidated
porous media subject to freezing and thawing. This technique relies on the dielectric properties of water, ice,
air, and mineral substrate in the radio-frequency range. A semi-empirical method based on the Lichtenecker
model and on comparison between drying and freezing tests, provides an accurate estimation of the temperature-
dependent liquid water amount in frozen porous materials. This is then analyzed through thermoporometry
concepts to characterize pore size distribution and specific surface area. The results obtained are roughly in the
same order range than those obtained from gravimetric sorption/desorption isotherms.
1 INTRODUCTION
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any liquid water variation inside the porous network
of the material results in resonant frequency variation.
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3.2 Dielectric constants of unsaturated cement
pastes
The changes in the dielectric constant w,a with respect
to temperature were first determined at liquid satura-
tion degree Sw held constant. Samples with different
liquid saturation degrees Sw were prepared by con-
serving initially dried specimens in an oven at 70 C
during 6 months, within atmospheres at various con-
trolled humidity rh = 12%, 33%, 44%, 85%, and 100%
by using salt solutions (Raoof 1998). This procedure
provided samples with liquid water saturation degrees
Sw = 0.12, 0.17, 0.18, 0.49 and 1 respectively. The
sample dielectric constant w,a was then determined
from 20 C to 5 C for Sw = 100%, and from 20 C
to 40 C for Sw = 0.12, 0.17, 0.18, 0.49. It must be
again stressed out that these temperature ranges were
allowed since primary freezing occurs only at 5 C for
saturated cement pastes, and no freezing is observed Figure 3. Evolution of the apparent dielectric constant and
for unsaturated cement pastes with Sw < 0.5 before its derivation with temperature at a fixed saturation ratio for
45 C. Whatever the porous material tested here, the cement paste P5-1d.
relation between the dielectric constant w,a and the
temperature was found to be linear (see figure 3A for
cement paste P5-1d), so that the corresponding slope
a(Sw ) is a function of liquid saturation only. Further-
more, as reported in figure 3B, a(Sw ) curve was found
to be a line. We finally write:
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4 POROUS NETWORK CHARACTERIZATION
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3 Table 1. Comparison between surface area
values from capacitive sensor based apparatus
Capacitive device
Sorption device (CS), MIP and sorption/desorption test (SD) in
2.5
m2 /g.
2 Paste MIP CS SD
dVi /drp [mm3/A/g]
0.5
Sw Sw, min , with Sw,min the volumic proportion
of unfreezable water. Thus, for cylindrical assumed
pores, using (14):
0
0 20 40 60 80 100 120 140 160 180 200
Pore radius [A]
5 CONCLUSION
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radii distribution and specific surface area are found dielectric constant in porous media by the capacitive
to be consistent with those obtained on similar sam- method. Comptes- Rendus Mecanique 332, 639645.
ples from sorption/desorption isotherms by means of Jehng, J., D. Sprague, and W. Halperin (1996). Pore struc-
a homemade apparatus. ture of hydrating cement paste by magnetic resonance
relaxation analysing and freezing. Magnetic Resonance
Imaging 14(7/8), 785791.
Kaufmann, J. (1999). Experimental identification of damage
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