23rd International Symposium on Transport Phenomena
Auckland, New Zealand
1922 November 2012
Experimental and theoretical studies on the gas thermal conductivity
in nano-porous materials
H. Zhang, Z.Y. Li*, D. Dan, Y.H. Li and W.Q. Tao
Key Laboratory of Thermo-Fluid Science and Engineering, Ministry of Education
School of Energy and Power Engineering, Xian Jiaotong University, Xian 710049, P.R. China
*Corresponding author: lizengy@mail.xjtu.edu.cn
Abstract
The thermal conduction in nano-porous materials (NPM) has
significant nano-scale size effects that make the NPM such as
aerogels have excellent insulation performance. The gas thermal
conductivity in NPM plays an important role on reducing the
effective thermal conductivity of the NPM. In the present work,
the experimental and theoretical studies are conducted to analyse
the effects of temperature, pressure, atmosphere and spatial
structure on the effective thermal conductivity of several typical
NPM. The thermal conductivity test apparatus based on the
transient plane source method is built to measure the effective
thermal conductivity of porous materials at different gas pressure
form 10-3 Pa to 1MPa. It is impossible to obtain gas phase
thermal conductivity in porous medium directly through
experiment method because solid heat conduction and gas heat
conduction are coupled in porous materials due to the randomly
geometric structure. Therefore, an effective method is proposed
to obtain the gas phase heat conduction contribution to the total
effective thermal conductivity by subtracting the effective
thermal conductivity value at ultimate vacuum (less than
0.001Pa) from the effective thermal conductivity at different gas
pressure. The experimental results within the larger pressure
range show that the contribution of gas heat conduction to the
effective thermal conductivity is higher than the gas thermal
conductivity in NPM, and the deviation increases with the
increment of pressure. The results prove that it is inappropriate to
regard the gas thermal conductivity in NPM as its contribution to
the effective thermal conductivity, which is usually adopted to
verify and improve the gas thermal conductivity theory. The
effective thermal conductivity of NPM in argon atmosphere is
less than that in nitrogen atmosphere. At high gas pressure, the
contribution of gas heat conduction could be weakened by
reducing the temperature or increasing the porosity. The
insulation performance of NPM will be deteriorated when a large
number of micron pores are existed in the materials. In addition,
adsorption and desorption hysteresis may happens in nano-pores
when adjusting the gas pressure and the effective thermal
conductivity measurement should be arranged from low pressure
to high pressure.
Nomenclature
c specific heat
d diameter
kB Boltzmann constant
K specific Rossland mean extinction coefficient
Kn Knudsen number
l mean free path
m mass
N number density
n mean refractive index
p pressure
Pr Prandtl number
S specific area
T absolute temperature
Greek symbols
thermal conductivity
accommodation coefficient
heat capacity ratio
viscosity
density
Stefan-Boltzmann constant
sound velocity
porosity
Subscripts
0 contribution
e effective
g gas phase/gas molecules
m mean
p constant pressure
r radiation phase
s solid phase
v constant volume
Introduction
Aerogels are open-cell NPM made by sol-gel process and
supercritical drying technology. Aerogels have high porosity,
high specific area and outstanding thermal insulation
performance for its nano-porous structure and nano-scale solid
skeleton [1]. However, the utilization of aerogels is restricted for
their hydrophilic inner-surface, brittle skeleton and transparency
of thermal radiation. The insulation performance of aerogels can
be improved by hydrophobic processing, adding reinforced fibers
and opacifier [2-4]. The improved composite materials are not
pure aerogels and usually called NPM.
The heat transfer in NPM contains solid phase heat conduction,
gas phase heat conduction and thermal radiation. Heat transfer in
NPM has strong size effect for its nano-scale structure. The pore
size of NPM is about 10nm which is less than the mean free path
of gas (70nm for air) in free space at normal pressure and
temperature. The motion of gas molecules in NPM is suppressed
by solid matrix. Therefore, the gas thermal conductivity in NPM
is lower than that in free space [2]. Because of the random nature
of the NPM structure, regular structures are usually adopted to
analyse the thermophysical property, such as effective thermal
conductivity. Although it is unnecessary to consider all aspects of
the microstructure to obtain the effective thermal conductivity,
the equivalent structure should represent the key features of the
real microstructure [3, 4, 6, 7].
For composite materials, the effective thermal conductivity is
mainly determined by experiment. However, gas thermal
conductivity and solid thermal conductivity could not be
measured directly for gas phase heat conduction and solid phase
conduction is coupled in the porous medium. Many works have
been conducted to obtain the contribution of gas phase heat
conduction, solid phase conduction and thermal radiation [3-5, 8-
10], in which the ambient pressure is lower than 1bar.
In this paper, the transient plane method is adopted to measure
the effective thermal conductivity of the NPM [3]. The hot disk
thermal constant analyser is combined with molecular pump
group, adjustable valves and high pressure source to carry out the
experiments at different gas pressure. The test range of gas
pressure is extended to 1Mpa for thermal conductivity
measurement of porous materials. The gas thermal conductivity
in NPM is mainly influenced by the microstructure of the
material and the environment including temperature, atmosphere
and pressure. This paper presents theoretical and experimental
studies on the influencing factors of gas thermal conductivity in
NPM. Gas thermal conductivity in NPM is calculated by revising
the mean free path of gas molecules. The effective thermal
conductivity of NPM at different temperature, pressure and
atmosphere are experimentally investigated. For a constant
temperature, the amount of gas phase heat conduction
contributed to the effective thermal conductivity at different
pressure is obtained by subtracting the effective thermal
conductivity value at ultimate vacuum (less than 0.001Pa). The
influence of porosity on the contribution of gas conduction is
also studied.
Theoretical analysis
The effective thermal conductivity of NPM can be recognized as
the sum of contributions from several parts: heat conduction
through the gas, g,0, heat conduction through the solid, s,0,
radiation through the skeleton and voids, r,0, and convection of
the gas trapped in the pores, c,0.
e = g ,0 + s ,0 + r ,0 + c ,0 (1) Solid thermal conductivity
Gas convection could be neglected in porous materials when the
pore size is less than 1mm at ambient pressure[9].
Gas thermal conductivity
The gas thermal conductivity between two parallel plates was
presented by Kaganer[4].
2 1 2 material. Hrubesh and Pekala[7] proposed the approximate
g g0 / (1 + 2
= Kn) (2)
+ 1 Pr
where, g0 is the gas thermal conductivity in free space; =cp/cv,
cp and cv are the specific heat at constant pressure and volume
respectively; Kn=lm/lch is the Knudsen number, lm is the mean
free path of gas, lch is the distance between the plates.
The gas thermal conductivity g0 in free space based on the
kinetic theory was derived by Loeb[5].
(9 5)
=
0
cv (3)
g
4 3 por K e , m
where, is the viscosity of gas with formula as
= 0.461N g mg ( 8k BT / mg ) lm
1/ 2
(4)
where, mg is the mass of gas molecules, kB is the Boltzmann
constant, T is the absolute temperature, Ng=p/kBT is the number
density of the gas molecules, p is the gas pressure.
The mean free path of gas molecules in free space is
k BT
lm0 = (5)
2 d g2 p
where, dg is the diameter of the gas molecules.
The motion of gas molecules in porous medium is suppressed by
the porous framework and the mean free path of gas molecules is
different from that in free space. Zeng et al [2] derived the mean
free path of gas molecules in porous medium based on the kinetic
theory.
1
lm = (6)
2 d p / k BT + 0.25S s por 1
2
g
where, por is the apparent density of the porous medium, Ss is the
specific surface area, is the porosity of the porous medium.
In free space, substituting equations (3), (4) and (5) into equation
(2), the thermal conductivity of free gas between two parallel
plates could be obtained.
( 2.25 1.25) 0.461( p / kBT ) (8k BT / mg )
1/ 2
mg cv
2 ( p / k BT ) d g2
g = (7)
2 1 2 k BT
(1 + 2 )
+ 1 Pr 2 d g2 plch
In porous medium, substituting equations (3), (4) and (6) into
equation (2) then the thermal conductivity of gas in porous
materials with certain thickness could be derived.
( 2.25 1.25) 0.461( p / kBT ) (8k BT / mg )
1/ 2
mg cv
0.25S s por 1 + 2 ( p / k BT ) d g2
g = (8)
2 1 2 1 1
1+ 2
+ 1 Pr 2 d g2 p / k BT + 0.25S s por 1 lch
The heat conduction through the tenuous solid structure can be
given by[6]
s ,0 = por0s / ( ) (9)
where, is the density of the solid skeleton, 0 and are the
longitudinal sound velocities of the composite materials and the
solid skeleton, and s is the thermal conductivity of the bulk solid
formulas for the sound velocities of different materials.
Radiative thermal conductivity
In practical application, the optical thickness of the NPM is
typically very large. The thermal radiation travels only a short
distance and less than the thickness of the NPM. Therefore,
according to the diffusion approximation, the radiative thermal
conductivity of NPM can be described by[9]:
16n 2 T 3
r ,0 = (10)
where, is the Stefan-Boltzmann constant, n is the mean
refractive index, T is the absolute temperature and Ke,m is the
specific Rossland mean extinction coefficient.
Effective thermal conductivity and decomposition
In porous material, the gas thermal conductivity, the solid
thermal conductivity and the radiative thermal conductivity could
not be measured directly through thermal conductivity test
apparatus. Although the thermal conductivity of gas molecules,
solid structure and radiation can be calculated based on the above
theories, the experiment of effective thermal conductivity is the
essential method to evaluate the validity of the theories and the
thermal insulation performance of porous materials.
Many works [3-5, 8-10, 16] have been conducted to decompose
the effective thermal conductivity into its components. The
radiative thermal conductivity, r,0, can be directly calculated
from equation(10) by measuring the specific Rossland mean
extinction coefficient. The solid thermal conductivity, s,0, can be
determined by subtracting the radiative thermal conductivity
from the effective thermal conductivity e at ultimate vacuum.
Then the gas thermal conductivity, g,0, can be obtained by
subtracting r,0 and s,0 from the effective thermal conductivity at
different gas pressure. In the previous works, the gas thermal
conductivity g,0 decomposed from the experiment data at
different gas pressure was compared with the theoretical gas
thermal conductivity g in porous materials to verify and improve
the theory of gas thermal conductivity. However, the definition
of g,0 and g are different. The former is the contribution of gas
heat conduction to the effective thermal conductivity of porous
materials, and the latter is the absolute value of gas thermal
conductivity in porous materials. In porous medium, heat will
transfer through the solid structure and the pores continuously.
Therefore, the heat conduction through solid and gas is coupled
and g,0 is ultimately different with g .
Experimental investigations
The effective thermal conductivity of NPM is determined by the
microstructure with characteristic parameters of porosity and
mean pore diameter and environment conditions including
temperature, pressure and atmosphere. Guarded hot plate, hot
wire/strip and laser flash methods have been adopted to measure
the effective thermal conductivity at different temperature, gas
pressure and atmosphere, however, the gas pressure is not high
than 1bar (normal pressure) [8,17-19]..
In this work, the transient plane method is adopted to measure the
effective thermal conductivity at different gas pressure [3]. In
addition, the test range of gas pressure is extended to 1Mpa in
order to discern the difference between g,0 and g.
Apparatus
The experimental system is established to study the influences of
temperature, pressure and atmosphere on the effective thermal
conductivity of NPM. The experimental apparatus is shown in
Figure 1. The system contains hot disk thermal constant analyser
(type: TPS2500S), tube heating furnace, temperature control
system, pressure gage, molecular pump systems, high pressure
source of inert gas and adjustable valves. The transient plane
source method is similar to hot wire/strip method and the
measurement theory and procedure is discussed in ISO22007-
2:2008(E) standard [20]. The molecular pump systems, high
pressure source of inert gas and adjustable valves are used to
adjust the gas pressure range of 0.001Pa~1MPa. The tube furnace
and its temperature control system could supply enclosed space
and stable, adjustable temperature. The hot disk thermal constant
analyser based on the transient plane source method is used to
measure the effective thermal conductivity of NPM at different
environment.
Validation and procedure
The accuracy of the hot disk thermal constant analyser is
validated by NIST1453 standard sample, an expanded
polystyrene board with thermal conductivity 0.032W/mK at
room temperature and the deviation is within 1.5%.
When carrying out an experiment in the effective thermal
conductivity measurement of NPM at different gas pressure,
special attentions should be paid. The substrate of the NPM
discussed in this paper is silica. Therefore, hydroxyl groups will
be introduced when manufacturing the NPM and plenty of water
vapour in temperature and humidity environment may be
absorbed on the inner surface of the NPM. The thermal insulation
performance will be deteriorated greatly by the absorbed water.
To remove the influence of water, the enclosed tube furnace will
be pumped below 0.001Pa and filled inert gas to normal pressure.
This procedure should be repeated for three times to remove the
water vapour and gas impurities completely. The experiment is
conducted from low gas pressure to high gas pressure to avoid
the disturbance of the adsorption and desorption hysteresis when
changing the gas pressure. The gas pressure is adjusted by the
molecular pump group, the high pressure gas source and the
valves.
Figure 1. Schematic illustrations of the experimental apparatus
Results and discussion
Influence of gas pressure and temperature
There are three important concepts of gas heat conduction: the
gas thermal conductivities in free space and NPM, the
contribution of gas heat conduction to the effective thermal
conductivity of NPM. These concepts are emphasized again to
avoid the confusion.
Two commercial NPM Super-G and NWX-1000 were measured
at different gas pressure. The test atmosphere is nitrogen. The
Super-G is manufactured by Microtherm and NWX-1000 by
Unithermal. Both materials have apparent density of 240kg/m3.
The effective thermal conductivity of Super-G and NWX-1000
are measured at different gas pressure and temperature.
Figure 2 shows the effective thermal conductivity as a function of
gas pressure for the two NPM. The effective thermal conductivity
keeps constant when the gas pressure is less than 0.01kPa and it
is the overall contributions of solid conduction and thermal
radiation. The effective thermal conductivities of Super-G and
NWX-1000 at 24 after evacuated to high vacuum are as low
as 0.0090W/mK and 0.0120W/mK. When the temperature rises
to 150, the effective thermal conductivities of Super-G and
NWX-1000 at vacuum pressure increase to 0.0103W/mK and
0.0130W/mK. The effective thermal conductivity increases
rapidly when the gas pressure is higher than 0.01kPa. The growth
rate decreases slightly when the pressure is larger than 100kPa.
The effective thermal conductivity varies with gas pressure
because the gas thermal conductivity is sensitive with pressure.
 Figure 2. Effective thermal conductivity of Super-G and NWX-
1000 at different pressure and temperature
The contribution of gas heat conduction is decomposed from the
experiment results and compared with the gas thermal
conductivities in free space and NPM. The comparison results are
shown in Figure3. Both the gas thermal conductivity in free
space and in NPM increases with pressure as the S curve.
In free space, the gas heat conduction could be neglected when
the pressure is less than 0.1Pa, then it increases with gas pressure
and closes to constant when the pressure is higher than 1kPa. In
NPM, however, the gas thermal conductivity could be neglected
when the gas pressure is less than 1kPa, and it still does not reach
the maximum value and less than that in free space at 1Mpa.
The contribution of gas heat conduction to the effective thermal (a) Comparison of Super-G
conductivity decomposed from the experimental results has the
similar variation tendency with the gas thermal conductivity in
NPM. However, the contribution of gas heat conduction is higher
than the gas thermal conductivity when the gas thermal
conductivity could be distinguished. The variation increases with
the increment of pressure, and the gas contribution to the
effective thermal conductivity is even higher than the gas thermal
conductivity in free space. The results prove that its
inappropriate to regard the gas thermal conductivity in NPM with
as its contribution to the effective thermal conductivity of NPM,
because the contribution of gas heat conduction exceeds the gas
thermal conductivity in free space when the gas pressure is
beyond 1bar. Similar phenomenon has been observed in previous
work [21], but without reasonable explanation. The large
deviation between the gas thermal conductivity of NPM and its
contribution is primarily caused by the misunderstanding of the
decomposed contribution of gas heat conduction to the effective (b) Comparison of NWX-1000
thermal conductivity. Figure 3. Comparison of gas thermal conductivity and its
The relationship between the gas thermal conductivity and contribution to effective thermal conductivity
temperature is complicated as shown in equations (7) and (8).
The influence of temperature on the gas thermal conductivity is
not obvious at low pressure. The influence of temperature
becomes distinguished when the gas pressure is higher than
0.02kPa in free space, while the influence of temperature
becomes apparently until the pressure is as high as 400kPa in
NPM. The gas thermal conductivities at 150 in free space and
NPM are 19.3% and 13.3% higher than the values of 24 at
1Mpa. The influence of temperature on the gas heat conduction
contribution has the similar variation with the gas thermal
conductivity in NPM and the variation is more obviously.
As shown in equations (3) and (4), the gas thermal conductivity
is proportional to the number density of gas molecules and the
mean free path. The number density of gas molecules increases
linearly with pressure while the variations of the mean free path
in free pace and NPM are different. The gas thermal conductivity Figure 4. Mean free path of nitrogen molecules
has different performance in free pace and in NPM due to the Influence of atmosphere
influences of mean free path and number density of gas
molecules. The means free paths in free space and NPM are The effective thermal conductivities of NWX-1000 in nitrogen
shown in Figure4. The mean free path in free space decreases and argon atmosphere are measured at 24 and different
linearly with the increases of pressure. However, the mean free pressure. The effective thermal conductivity and the contribution
path in NPM remains constant when the pressure is less than of gas heat conduction decomposed from the effective thermal
100kPa, then the mean free path decreases and closes to the value conductivity are shown in Figure5. The effective thermal
in free space gradually when the pressure is higher than 100kPa. conductivities between nitrogen molecules and argon molecules
Such difference is caused by the suppressed motion of gas in NWX-1000 are also compared. The experimental results show
molecules in NPM, which make the apparent difference of gas that the effective thermal conductivities in nitrogen and argon
thermal conductivity in NPM and in free space. atmosphere are all 0.0120W/mK when the pressure is less than
0.01kPa, which implies that the gas heat conduction could be
neglected here. Then the effective thermal conductivity increases
rapidly with the increment of pressure. It is higher in nitrogen
atmosphere and the difference becomes larger and higher with
the increase of pressure. Therefore, the contribution of gas
conduction in argon is smaller than that in nitrogen because the (b) Comparison at 150
thermal conductivity of argon molecules is smaller than that of Figure 6. Influence of porosity
nitrogen molecules, especially at high pressure.
Influence of adsorption and desorption hysteresis
As shown in Figure 7, there exists an obvious gap in the effective
thermal conductivity when increasing the pressure and when
decreasing the pressure. It is due to desorption of gas molecules
on the inner surface is incomplete. Figure 8 shows the adsorption
and desorption isotherms of nitrogen at 77K. The test is
conducted with ASAP 2020 and the adsorption and desorption
hysteresis is apparent at high relative pressure. Therefore, when
conducting the effective thermal conductivity experiments of
NPM, the adsorption and desorption hysteresis should be avoided
by adjusting the pressure from low to high.

Figure 5. Influence of atmosphere on effective thermal

conductivity
Influence of porosity
The effective thermal conductivities of NPM with porosity range
of 71.8%~89.8% are experimentally investigated in nitrogen
atmosphere at 24 and 150. Figure 6 shows the decomposed
contribution of gas heat conduction. The variation tendency of
gas heat conduction contribution is similar to that mentioned
above. In general, the higher porosity, the higher the contribution
of gas heat conduction. The difference at 150 is more obvious
than that at 24. However, the sample 4# is different from other Figure 7. Influence of adsorption and desorption hysteresis
samples, which may be caused by the quantity of micron pores
existing in the materials. The supposition could be proved by the
study of the relationship between pore size and the gas pressure
[8,21].

Figure 8. Adsorption and desorption isotherm

Conclusions

(a) Comparison at 24 The thermal conductivity measurement apparatus based on the

transient plane source method is established. The effective
thermal conductivity of NPM at different gas pressure could be
measured accurately and the pressure range is extended from
0.001Pa~100kPa to 0.001Pa~1Mpa.
The effective thermal conductivity and decomposed contribution
of gas heat conduction of NPM are obtained. The experimental
results within the larger pressure range shows that the
contribution of gas heat conduction to the effective thermal
conductivity is higher than the gas thermal conductivity in NPM
from existing theoretical models. It is not reasonable to regard
the gas thermal conductivity in nano-porous materials as its
contribution to the effective thermal conductivity of NPM
because the contribution of gas heat conduction exceeds the gas
thermal conductivity in free space when the pressure is beyond
1bar.
The influences of temperature, atmosphere and porosity on the
gas thermal conductivity are not apparent at low gas pressure,
while at high gas pressure, the contribution of gas heat
conduction could be reduced by reducing the temperature or
increasing the porosity.
The insulation performance of NPM is also influenced by the
microstructure. The existence of micron pores will enhance the
gas heat conduction. In addition, adsorption and desorption
hysteresis may happens in nanostructure when adjusting the gas
pressure, which can be avoided by adjusting the pressure from
low to high. Therefore, how to adjust the gas pressure should be
clarified when conducting the experiments at different gas
pressure.
Acknowledgement
This work is supported by the National Natural Science
Foundation of China (51136004) and the National Basic
Research Program of China (2010CB227102)
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