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HRVATSKO DRUTVO ZA
MATERIJALE I TRIBOLOGIJU
CROATIAN SOCIETY OF
MATERIALS AND
TRIBOLOGY
I. Lu i a 5
HR - 10000 Zagreb, Croatia
T: +385 1 6168581
F: + 385 1 6157126
hdmt@fsb.hr
MATRIB
2009
INTERNATIONAL CONFERENCE ON
MATERIALS,TRIBOLOGY, RECYCLING
Lipanj / June 24 - 26, 2009
KONA!AN PROGRAM / FINAL PROGRAMME
MATRIB je uvrten u plan stru*nog
usavravanja Razreda inenjera strojarstva,
Hrvatske komore arhitekata i inenjera u
graditeljstvu i vrednuje se s 12 bodova.
28.6.2009 14:06
ZBORNIK RADOVA
PROCEEDINGS
MATRIB 2009
VELA LUKA
OTOK / ISLAND KORULA, HRVATSKA
24-26. lipnja / June 2009.
ORGANIZATORI / ORGANIZED BY:
HRVATSKO DRUTVO ZA MATERIJALE I TRIBOLOGIJU
CROATIAN SOCIETY FOR MATERIALS AND TRIBOLOGY
INSTITUTE OF MATERIALS AND MACHINE MECHANICS
(SLOVAK ACADEMY OF SCIENCES)
DUBLIN INSTITUTE OF TECHNOLOGY
SUORGANIZATORI / CO-ORGANIZERS:
FAKULTET STROJARSTVA I BRODOGRADNJE, ZAGREB
FACULTY OF MECHANICAL ENGINEERING AND NAVAL
ARCHITECTURE
SPONZORI / SPONSORS:
MINISTARSTVO ZNANOSTI OBRAZOVANJA I PORTA
PROPLIN d.o.o. - ZAGREB
IDEF d.o.o. za industrijsku defektoskopiju ZAGREB
ROBERT BOSCH d.o.o. ZAGREB
IZDAVA / PUBLISHER:
UREDNICI / EDITORS:
NAKLADA / ISSUE:
150
TISAK / PRINT:
II
Faculty of Chemical Engineering and Technology, University of Zagreb, Maruliev trg 20,
Zagreb, Croatia
2
Elektroda Zagreb d.d. Ruevje 7, 10290 Zaprei - Zagreb, Croatia
418
1. Introduction
Material thermal property data are important for the engineering solutions of the heat
transfer problems. Measurements of thermal properties of heterogeneous, wet and porous
materials by conventional steady-state methods are subject to large errors. In order to avoid
water migration during the run-time of the thermal tests, transient measurement methods are
preferable [1, 2]. The determination of thermal conductivity is very challenging since it
belongs to a class of inverse problems where an estimated parameter is very sensitive to
measured quantities necessary for its calculation. The hot wire method [1] involves an ideal
line heat source, infinitely long with zero mass, immersed in an infinite sample. As the
parallel wire method is very sensitive to the uncertainty of measuring the radial distance of a
thermocouple from a heater, a resistance technique is employed. Furthermore, by this
method, where the wire acts as both a heater and a resistance thermometer, the influence of
local non-homogeneities of measured materials is minimized. Thermal conductivity is
determined by inverse solution of the differential equation for radial heat conduction. In
order to minimize errors due to an approximation of the used model and effects of the
experimental setup a critical design of an experimental configuration is necessary.
This work describes a developed apparatus and a method to obtain a thermal conductivity of
dry and wet materials. The systematic error due to a electrical conductivity of cement paste is
minimized by the used experimental configuration. The values of the thermal conductivity
for fresh calcium aluminate cement (CAC) pastes are documented to the best of our
knowledge for the first time and compared to the available literature data on portland cement.
Research on thermal properties of CAC is particularly interesting due to rapid heat
generation during hydration and development of significant temperature gradient in material
[3, 4].
2. Hot wire model
When a heat generation is applied to the line heat source, its temperature response is based
on an analytical solution [5] to the heat conduction model given in cylindrical coordinates:
r 2
q
t =t
(1)
E
T ( r , t )t =0 =
4
4at
where is the thermal conductivity of sample (Wm-1K-1), r is the radius of the wire (m) a is
thermal diffusivity of sample (m2s-1), t is time (s), q is rate of heat generation (W/m) and Ei is
the exponential integral computed as:
z 2 z3 z 4
Ei ( z ) = + ln z + z + + .....
(2)
2! 3! 4!
419
Furthermore, this paper documents the thermal conductivities of cement pastes obtained
with sample of commercial CAC ISTRA 40 taken from a regular production of Istra Cement
International, Pula, Croatia. The cement has the oxide mass fraction composition listed in
Table 1. Physical properties of used cement are given in Table 2. All mixes were prepared
with deionized water. The main compounds are CA (cement notation: C=CaO, A=Al2O3,
F=Fe2O3, S=SiO2, H=H2O) and ferrite phase (C4AF-C6AF2), with mayenite, C12A7, gehlenite,
C2AS and -C2S as minor compounds. Cement pastes with water to cement mass ratio of 0.3
and 0.4 were prepared.
Table 1. Chemical composition of investigated CAC.
CaO
Al2O3
Fe2O3
FeO
SiO2
TiO2 MgO
SO3
Na2O K2O
Sum
37.10% 38.47% 14.39% 2.90% 4.43% 1.05% 0.90% 0.20% 0.14% 0.17% 99.8%
>90 m,
%
3.76
420
421
MATLABs built-in solver pdepe [7, 8]. The model employed two coupled partial
differential equations of energy conservation: one for the wire and one for the sample [9].
The thermal conductivity was calculated by fitting the experimental results to a theoretical
expression (1) by using literature values for thermal diffusivity [10-12], listed in Table 3, and
eight terms for calculating the exponential integral according to the Eq. (2). This parameter
estimation problem was solved by the Levenberg-Marquardt method of optimization [13,
14]. In order to investigate the sensitivity of thermal conductivity and thermal diffusivity a
simulation analysis was performed by plotting predicted responses by Eq. (1) with 10 %
change in the investigated parameters. The results on parameter sensitivity analysis, shown in
Fig. 2, indicate a low impact of thermal diffusivity and good sensitivity of thermal
conductivity onto the temperature response (T). Therefore, an uncertainty of value on
thermal diffusivity has little impact to estimation of thermal conductivity. Data on thermal
diffusivity of fresh cement pastes are taken from independent transient measurements
conducted in our laboratory [15].
Table 3. Literature data on thermal conductivity and thermal diffusivity at T = 20 C.
Material
/ W m-1 K-1 a 107 / m2s-1
Ottawa sand
0.306 [17]
2.33 [11]
Gelatinous water (Agar)
0.5985 [10]
1.433[10]
0.962 [12]
Glycerol
0.285 [12]
Fresh cement paste w/c = 0.4
2.97 [15]
Fresh cement paste w/c = 0.3
3.30 [15]
4.5
= 0.9
4.0
= 1.0
= 1.1
T / C
3.5
a = 3.3e-7
a = 2.7e-7
3.0
a = 3.0e-7
2.5
2.0
1.5
0
20
40
60
80
100
t/s
422
20) sieve and to be retained on a 600- (US Standard No. 30) sieve. Data on the thermal
conductivity of Ottawa sand in air is readily available from several sources, although no
specific standard exists for this property.
The solid density of the Ottawa sand was measured by submerging a known mass of sand in
water and measuring the volume change of the liquid. The solid density was found to be 2.69
g/cm3, which is very close to the published value of 2.65 g/cm3 [16]. Knowledge of the bulk
density is important because the thermal conductivity can change based on how tightly the
sand particles are packed. Measured bulk density of investigated Ottawa sand of 1.650 g/cm3
is close to the published value of 1.615 g/cm3 [17]. The thermal diffusivity data on Ottawa
sand were not readily found in literature. Hence, the used value in Eq. (1) is taken for sand in
general [15]. The density and thermal conductivity of investigated Ottawa sand are 2.64
g/cm3 and 0.31 Wm-1 K-1, which is close to the published value of 2.6 g/cm3 and 0.3 Wm-1K-1
[15].
Agar is gel-forming polysaccharide, widely used in industry and in scientific applications.
Agar form gels at approximately 35C and once formed does not melt below 85C. Gelation
occurs when a chain of macromolecules forms a network capable of entrapping the
dispersing medium. Such gel has a composition close to a pure liquid but resemble a solid. In
that way heat transfer through agar is by conduction solely, excluding natural convection.
A repeatability analysis was conducted on samples by repeating the measurements 10 times.
The mean values of the thermal conductivities and estimated precision at a 95 % confidence
level are listed in Table 4. Very good agreement was found between the results of the
experimental investigation and sources of available data. This finding validates the accuracy
of the measurement apparatus and provides confidence that further results are accurate. It can
be concluded that the results of the method evaluation on reference materials indicated an
accuracy of 3 % and uncertainty of 0.7 % (for 95 % confidence).
4.3. Effect of cement paste electrical conductivity
The electrical conductivity of cement paste was measured by conductivity meter (Lab 960
Schott instruments) 0.5 h after mixing cement and water. For cement pastes with water to
cement ratio 0.4 and 0.3 the measured electrical conductivities are 1287 Scm-1 and 1098
Scm-1, respectively. The resistance of the cement paste sample in a defined geometry (see
3.3) is calculated by referring to the values of the obtained electrical conductivity. The
deviation of the overall electrical resistance (of the parallel system of sample and Pt
resistance), RII from the Pt resistance is calculated to be less than 0.5 %.
Hence, in the experimental configuration the systematic error due to the electrical
conductivity of cement paste can be assumed to be less than 0.5 %.
4.4. Thermal conductivity of fresh cement pastes
Cement based material is a complex heterogeneous, multiphase and polydisperse system.
Through such a material the heat is transferred by a combination of different modes. They
include conduction through the solid particles, conduction and convection through the
gaseous and liquid phases, evaporation condensation mechanism [2], and radiation at the
particle surfaces. However, this overall process is practically modelled solely by a heat
conduction model considering the conduction parameters as apparent. Therefore, one should
bear in mind that the physical parameters measured in this paper for cement paste and Ottawa
sand are more properly called apparent thermal conductivity [2]. The values of the thermal
423
conductivity for fresh calcium aluminate cement pastes obtained show good agreement with
the literature values for Portland cement (PC) [18], Table 4.
Table 4. Measured and published data on thermal conductivity at T = 20 C.
/ W m-1 K-1
Material
Measured Uncertainty
Reported
Accuracy
Ottawa sand
0.315
0.5 %
0.306 [17]
3%
Gelatinous water (Agar)
0.615
0.7 %
0.5985 [10]
3%
Glycerol
0.290
0.6 %
0.285 [12]
2%
Fresh cement paste w/c =
0.98
0.7 %
(PC)0.97[18]
0.4
Fresh cement paste w/c =
1.06
0.6 %
(PC) 0.99 [18]
0.3
Chi^2/DoF = 3.6e-4
R^2
= 0.99802
P
l
a
Measured (HW)
Analytic Fit
0.9930
0.1760
3.0e-7
0.980
3.8e-5
(fix)
(fix)
(fix)
5e-3
(fix)
1
0
0
20
40
60
80
100
120
t/s
424
The authors acknowledge support from the Croatian Ministry of Science, Education and
Sports under projects no. 125-1252970-2983 Development of Hydration Process Model.
7. Reference
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Int J Heat Mass Transfer, 30 (1987) 1343-1350.
3. Ukrainczyk, N., ipui, J., Dabi, P., Matusinovi, T., Microcalorimetric Study On
Calcium Aluminate Cement Hydration, 13. International conference on Materials,
Processes, Friction and Wear - MATRIB'08 (2008) 382-388.
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P.Barnes), Applied Science, London, (1983) 415-470.
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Press, London (1959).
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Equations, SIAM J Sci Stat Comput, 11 (1990) 1-32.
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18 (1997) 1-22.
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(1998) 379-389.
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Technology, Gaithersburg MD, 20899 (http://webbook.nist.gov).
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Antimony/Potassium Permanganate Pyrotechnic Delay Compositions, Combustion And
Flame, 66 (1986) 67-75.
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Appl. Math. 2, (1944) 164-168.
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SIAM Journal on Applied Mathematics 11 (1963) 431441.
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be published.
16. ASTM Density OTTAWA sand C-190
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Building Materials Database, ID 1023, (http://srdata.nist.gov/insulation/)
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Hydrating Cement Pastes," Materials and Structures, 40 (2007), 1073-1080.
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