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Gaosheng Wei1

School of Energy and Power Engineering, Key Laboratory of Condition Monitoring and Control for Power Plant Equipment of Ministry of Education, North China Electric Power University, Beijing 102206, China e-mail: gaoshengw@126.com

Gaseous Conductivity Study on Silica Aerogel and Its Composite Insulation Materials
This paper presents a theoretical and experimental study on gaseous conductivity of silica aerogel and composite insulation materials. First, the insulation material samples (including silica aerogel, xonotlite-type calcium silicate, xonotlite-aerogel composite, and ceramic fiber-aerogel composite) were prepared. Next, the gaseous conductivities of the prepared samples were measured from 0.045 Pa to atmospheric pressure using the transient hot-strip (THS) method. The gaseous conductivity expressions obtained based on the kinetic theory were then compared with the experimental results. It is shown that the gaseous conductivity of both xonotlite-type calcium silicate and silica aerogel decreases significantly with decreasing pressure. The gaseous conductivities of xonotlitetype calcium silicate and silica aerogel reach zero at about 100 Pa and 104 Pa, respectively. The theoretical gaseous conductivity expressions match well with the experimental results of xonotlite-type calcium silicate and silica aerogel but not with the experimental results for the composite insulation materials. This mismatch indicates that the aerogel does not totally fill the original interspace of the xonotlite-type calcium silicate and ceramic fiber in the two kinds of composite insulation materials. [DOI: 10.1115/1.4004170] Keywords: aerogel, thermal conductivity, thermophysical properties, transient hot-strip method, xonotlite-type calcium silicate

Yusong Liu
Energy Department of Beijing Sustainable Development Centre, Beijing 100083, China e-mail: lyscare163@163.com

Xiaoze Du
School of Energy and Power Engineering, Key Laboratory of Condition Monitoring and Control for Power Plant Equipment of Ministry of Education, North China Electric Power University, Beijing 102206, China e-mail: duxz@ncepu.edu.cn

Xinxin Zhang
Department of Thermal Engineering, University of Science and Technology Beijing, Beijing 100083, China e-mail: xxzhang@ustb.edu.cn

Introduction
Silica aerogel is a super insulation material made by sol–gel chemical processing and supercritical drying technologies. It has excellent insulation properties with a thermal conductivity lower than still air at ambient temperature because of its nanostructured SiO2 network and a very high porosity up to 99%. Many arguments have been made in recent years for using aerogels as thermal insulation material [1–5]. The major disadvantage of using monolithic silica aerogel for thermal insulation is that it is brittle and easily broken. Some researchers are trying to composite silica aerogel with other tougher materials [6–8]. Xonotlite-aerogel and ceramic fiber-aerogel composite insulation materials are two typical cases. Xonotlite-type calcium silicate (6CaO  6SiO2  H2O) is a synthesized high porosity insulation material created by hydrothermal processing with quartz powder and limestone as the raw material (with CaO=SiO2 % 1:1). Compared with fire-retardant fiber, xonotlite-type calcium silicate has excellent insulating performance, such as low thermal conductivity, environmentally friendly, high strength, and a wide application temperature range up to 1000  C [9,10]. Better insulation materials with higher strength are expected by compositing an aerogel with xonotlitetype calcium silicate and ceramic fiber [7,8]. The heat transfer mechanisms in porous insulation materials include solid conduction, gaseous conduction, natural convection, and thermal radiation. Natural convection can always be neglected if the pore in the material is small (<4 mm) [11,12]. Compared with solid conduction and thermal radiation, gaseous conduction contributes greatly to the total effective thermal conductivities for aerogel and its composite insulation materials, especially at
1 Current address: School of Energy and Power Engineering, North China Electric Power University, Beijing 102206, China. Contributed by the Heat Transfer Division of ASME for publication in the JOURNAL OF HEAT TRANSFER. Manuscript received August 23, 2010; final manuscript received May 3, 2011; published online February 13, 2012. Assoc. Editor: Pamela M. Norris.

ambient temperature, because of their high porosity [13–15]. This paper engages in a gaseous conductivity study of aerogel and its composite insulation materials, theoretically and experimentally. Samples of aerogel, xonotlite-type calcium silicate, xonotliteaerogel composite, and ceramic fiber-aerogel composite were prepared first. Thermal conductivities of the prepared samples at different pressures were then measured using the transient hotstrip (THS) method. The value of the measured thermal conductivity at a given pressure, minus the measured value at a vacuum condition less than 1 Pa (at this condition, the thermal conductivity is mainly attribute to solid conduction and thermal radiation), is considered as the gaseous contribution to the total thermal conductivity of the material. The expressions derived based on the kinetic theories were used to analyze the gaseous conductivity and were compared with the experimental results.

Theory of Gaseous Conductivity in Porous Media
According to kinetic theory, gas molecules transfer momentum and energy with a solid surface through collisions when a temperature difference exists between them. If a gas molecule does not reach the corresponding energy of the wall temperature through a onetime collision, there will be a temperature jump between the gas molecules and the wall. It means that the temperature of the gas molecules near the wall, Tg , is different than the temperature of the wall, Tw . This is called a “noncomplete temperature accommodation.” The appropriate temperature slip must be adopted at the solid surface in a heat transfer analysis. This temperature slip is given as [16] Tg À Tw ¼ 2 À a 2 c lm @ T a c þ 1 Pr @ y (1)

where a is the accommodation coefficient, c is the ratio of the gas’ specific heat, Pr is the Prandtl number, and lm is the mean free path of the gas molecules. When gas molecules contact a solid surface, some gas molecules achieve heat balance with the solid APRIL 2012, Vol. 134 / 041301-1

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surface before rebounding, and some do not reach the temperature of the solid surface before rebounding. The accommodation coefficient is the quotient of heat accommodation between the gas molecules and the wall, and varies between 0 and 1. For some representative values of the accommodation coefficient between various surfaces and gases, refer to the literature [17]. If gas molecules rebound between two parallel surfaces, the steady net heat flux can be calculated, where the corresponding apparent thermal conductivity is given as
0 kg ðT Þ   kg ¼ 2Àa 2c 1 1þ2 Kn a c þ 1 Pr

and / is the porosity of the media. For conventional porous insulation materials with micron pores, the second part in the denominator of Eq. (7) can be ignored because of their relatively smaller value of specific surface area, and Eq. (4) be used. But pffiffiffi still can 2 for its relative in an aerogel, Sq=/ is comparable to 2ng pdg higher value of S and cannot be simply ignored. Using kinetic theory, and considering the mean free path of Eq. (7), the gaseous conductivity in aerogel was derived by Zeng et al. [22,23] as kg ¼ 60:22 Â 105 pT À0:5 0:25Sq/À1 þ 4:01 Â 109 pT À1 (8)

(2)

0 where kg ðT Þ is the gaseous conductivity related to a temperature at constant pressure, Kn is Knudsen number defined as

Kn ¼ lm =d

(3)

d is the characteristic system size and is the distance between two parallel surfaces. lm is the mean free path of gas molecules in free space and calculated as 1 kB T ¼ pffiffiffi lm ¼ pffiffiffi 2 2p 2ng pdg 2pdg (4)

Both Eqs. (5) and (8) show that the gaseous conductivity in porous media is a function of temperature and pressure for a fixed structure’s material. The gaseous conductivity can be evaluated by measuring the thermal conductivity of porous media at different pressures. The thermal conductivity measured at vacuum condition can be considered the conductivity contribution of solid and thermal radiation. The thermal conductivity measured at a given pressure minus the value at vacuum condition can be a measure of gaseous conductivity contribution.

Experimental Investigation
The Material Preparation. Three samples of silica aerogel with different bulk densities were prepared using a two step method (sol–gel processes and supercritical evaporation technology). First, TEOS=EtOH-based polymeric silica sols were prepared with tetraethoxysilane (TEOS), EtOH absolute alcohol (C2H5OH), and deionized water with hydrochloric acid (HCl) as catalysts. The prepared silica sols were modified by ammonia to a neutral or alkaline condition. After stirring for 3 h, the silica sols were poured into a mould until a gel was formed. An absolute aqueous alcohol solution was then added to the gel for ageing. After ageing, the resulting SiO2 alcogel was taken out and placed into an autoclave. The autoclave was heated to exceed the supercritical point of absolute alcohol (243  C, 6.3 MPa) for supercritical evaporation. Finally, the silica aerogel samples were obtained. Samples with different bulk densities can be obtained by adjusting the molar ratio of the raw material and the technological parameter. For the detailed preparation process and the microstructure features (including the SEM image, pore size distribution, and specific surface area) of the sample refer to the literature [24]. The samples of xonotlite-type calcium silicate were prepared using the conventional hydrothermal process with quartz powder and limestone as the raw material (with CaO=SiO2 % 1:1) [9,10,25,26]. The samples of xonotlite-aerogel and ceramic fiber-aerogel composite insulation materials were prepared using the vacuum dipping technology [7,27]. SiO2 sols were first prepared using the same method mentioned above, then a vacuum chamber containing xonotlite-type calcium silicate or ceramic fiber was vacuumized to 0.5 Pa. The prepared SiO2 sols were placed into the chamber, then the vacuum valve was quickly turned off. The vacuum valve was opened after half an hour, then the floating xonotlite-type calcium silicate or ceramic fiber would suck into the SiO2 sols, and sink down. The vacuum valve was turned off until the gel was formed and then poured into an ethanol solution (water=ethanol = 1=4) for ageing. The composite materials were placed in an autoclave for supercritical drying after replacing the ethanol solution four times at 12 h intervals. The final corresponding samples of xonotlite-aerogel and ceramic fiber-aerogel composite insulation materials were obtained. For the detailed microstructure features (including the SEM image, pore size distribution, and specific surface area) of the prepared samples refer to the literature [28,29]. Thermal Conductivity Measurement. The transient hot-strip method was used to measure the thermal conductivity of aerogel, xonotlite-type calcium silicate, xonotlite-aerogel composite, and Transactions of the ASME

where ng is the number density of gas molecules, dg is the diameter of a gas molecule (for nitrogen dg = 3.798 Â 10À10 m); kB is the Boltzmann constant (kB = 1.38 Â 10À23 J=K), and p is the pressure. For conventional porous insulation material, such as calcium silicate, foam, etc., the Knudsen number in Eq. (3) is close to zero 0 . at atmospheric pressure. Equation (2) is simplified as kg ¼ kg While the mean pore diameter of aerogel is in the range of about 20 nm, it is apparently less than the mean free path of gas molecules (about 70 nm), and Kn > 1. Equation (2) has been adopted to depict the gaseous conductivity in aerogel by many researchers [1,19,20] and can be simplified as kg ¼
0 kg ðT Þ ð1 þ 2fKnÞ

(5)

where, f is a constant, for air f % 2, or Ref. [21] kg ¼
0 kg ðT Þ ½1 þ ðC=pdފ

(6a) (6b)

kB T C ¼ 2f pffiffiffi 2 2pdg

It must be mentioned that Eq. (2) was derived by analyzing the heat transfer problem between two parallel surfaces. Its validity for gas in porous media is questionable, however, especially in aerogel. The pore dimensions of aerogel are in the nanoscales range, and the solid surfaces are silica matrix distributed over the entire space. Accordingly, it is questionable to apply temperature slip conditions directly. In addition, Eq. (4) is the mean free path of gas molecules in free space. The mean free path of gas molecules in nanoporous structures of aerogel is different because the solid matrix in aerogel restricts the gas molecules free movement greatly. Zeng et al. [22] provide a comprehensive investigation of the mean free path of gas molecules in porous media and give the following mean free path expression 1 lm ¼ pffiffiffi 2 2ng pdg þ Sq=/ (7)

where S is the specific surface area of porous media defined as surface area per unit mass (m2=kg), q is the bulk density (kg=m3), 041301-2 / Vol. 134, APRIL 2012

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ceramic fiber-aerogel composite insulation materials with various bulk densities in the pressure range of 0.045 Pa to atmospheric pressure. Figure 1 gives the schematic illustration of the THS method. An electric current is passed through the hot-strip pressed between two equal size slabs of the sample and the temperature of the strip increases. The rate at which the temperature of the strip increases depends on the thermal conductivity of the sample. This is the basis for thermal conductivity measurements using the THS method. For an extensive description of the theory of the THS method, refer to Gustafsson et al. [30]. The result for thermal conductivity is calculated as k ¼ P0 =ð4pÞ=½dT ðtÞ=d lnðtފ, where P0 is the power input to the strip, t is the time, and dT ðtÞ=d lnðtÞ is the slope of temperature versus ln(t) after heating for several seconds. A 2.0 mm (width)  0.1 mm (thickness) nickel–chrome (Ni80Cr20) strip was used as the heat source. The strip was sandwiched between two identical samples, each about 150 mm (length)  100 mm (width)  60 mm (thickness). The PA 36-3 A=AL type stabilized power source supplies 0–3 A=0–36 V direct current output. The variations of temperature were detected using type K 0.1 mm-diameter thermocouples welded on the center of the strip surface. The signals from the thermocouple, together with the voltage signals between two sides of the sample and between two sides of the standard resistance, were all digitized by a YOCOGAWA DL-708E type digital oscilloscope before being processed by a computer. A vacuum system was designed specifically for the THS method as shown in Fig. 2, which can provide any vacuum surrounding for thermal conductivity measurements in the pressure range of 10À3 Pa to atmospheric pressure at ambient temperature. The size of the inner room of the vacuum bell was / 340  400 mm. Three groups, all together 24 electrodes, were set at the bottom of the vacuum bell. It was convenient to connect the inner room to the outer space using a lead. Two 2XZ-4 type direct drive rotary vane vacuum pumps (mechanical vacuum pump), and a molecular pump was used to control the vacuum condition of the system. Here, the measured thermal conductivity value minus the value measured under a pressure less than 1 Pa was considered as the gaseous conductivity of the material at a fixed pressure. This difference was because the contribution of gas on thermal conductivity was reaching zero when the pressure was less than 1 Pa.

Fig. 2 Picture of the arrangement of THS apparatus in a vacuum system

Uncertainty Analysis in Thermal Conductivity Measurement. The thermal conductivity of the sample is estimated as k ¼ P0 =ð4pÞ=½dT ðtÞ=d lnðtފ in the THS method by estimating the slope of the measured temperature rise versus time evolution in logarithmical scale over a defined time interval. The main sources of thermal conductivity uncertainty are connected to the measurement of temperature, the stability of the power supply, and the satisfaction of the experimental conditions as they are assumed in the theoretical model. Some sources of the nonmeasurement errors may cause differences between the real conditions

and the assumptions of the analytical model. For example, the heating strip has a finite nonzero thickness and a nonzero heat capacity. There are thermal resistances between the strip and the sample, and between the thermocouple and the strip. The sample and the strip have finite dimensions, and heat loss on the sample surface may occur. For a comprehensive discussion of uncertainty assessments of the THS method, refer to the literature [31]. In order to minimize the effect of the power supply on measurement uncertainty, a stabilized, direct current supply was offered through the strip. The heating rate was carefully examined in each test to guarantee the overall temperature rise was in the range of 8–10  C during the heating time interval of 0–500 s. A relative middle time interval of 50–300 s was adopted to determine the thermal conductivity of the measured samples, which can also depress the effects of nonzero heat capacity of the strip and finite dimensions of the samples on thermal conductivity determination. As mentioned in the literature [32,33], the temperature response DT of the strip in the THS method is a sum of two components: DT ¼ A þ Bf ðsÞ, where A is a constant representing thermal contact resistance effect, and the second component, Bf ðsÞ, is not influenced by any thermal contact resistance. In an actual experiment, the transient component B is used to determine thermal conductivity of the material. Therefore, the thermal conductivity determination is not influenced by any thermal contact resistance. According to our previous numerical study [34], the nonzero thickness and the nonzero heat capacity of the heating strip is the main measurement error, especially for materials with relatively low thermal diffusivities. The thermal diffusivities of the materials in this study are all larger than 4.0 Â 10À7 m2=s. By adopting a minimum time tmin of 50 s, the measurement error caused by the nonzero thickness and the nonzero heat capacity of the heating strip can be maintained at less than 2%. The measurement error caused by the heat loss on the sample p surface ffiffiffiffiffiffiffiffiffiffi is governed by the thermal penetration depth: Dp ¼ 2 atmax [32,33]. It represents the minimum distance from any part of the heating area of the sensor to the lateral boundary of the sample, i.e., the available probing depth. By adopting a tmax of 300 s and a relatively large sample dimension, the measurement error can be guaranteed to be less than 1% due to the finite dimensions of the sample in this study. All of the above uncertainties are considered to be independent in this study. By considering uncertainty analysis separately, and using the law of uncertainty propagation, the combined standard uncertainty of the thermal conductivity determination is sure to be less than 3%.

Results and Discussion
Figures 3–5 show comparisons of the experimental gaseous thermal conductivity data measured at ambient temperature with the theoretical heat transfer equation results. In the calculation, the mean pore diameter of the porous media is adopted as the characteristic system size of d in Eq. (5), and d = 20 lm are adopted for xonotlite-type calcium silicate according to measured structural values in the literature [10,35]. For gaseous thermal APRIL 2012, Vol. 134 / 041301-3

Fig. 1 Schematic illustration of transient hot strip setup

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S ¼ ð324:3=q þ 5:03Þ Â 105

(9)

Fig. 3 Pressure dependence of gaseous conductivity in xonotlite-type calcium silicate

Fig. 4 Pressure dependence of gaseous conductivity in silica aerogel

It is shown (Fig. 3) that the theoretical gaseous thermal conductivity from Eq. (5) matches well with experimental data of xonotlitetype calcium silicate when pressure is less than 104 Pa. The gaseous conductivity decreases significantly with a drop in pressure and reaches zero at about 100 Pa for various bulk densities of xonotlite-type calcium silicate. Equation (5) does not match well with experimental data of xonotlite-type calcium silicate at atmospheric pressure, which indicates that one cannot simply use the experimental measured data at atmospheric pressure minus the experimental thermal conductivity data at vacuum condition to represent the gaseous conductivity contribution to the total thermal conductivity of the material. It is because the coupled process of gas and solid, as well as radiation, may enlarge the total thermal conductivity at atmospheric pressure. Therefore, if the total heat transfer process is analyzed, Eq. (5) still can be used to depict the gaseous thermal conductivity in the xonotlite-type calcium silicate as mentioned in our previous work [13,39]. Figure 4 indicates a great error when using Eq. (5) (with d = 18 nm, which is the mean pore diameter of silica aerogel samples) to depict the gaseous conductivity of aerogel. As mentioned above, Eq. (4) is the mean free path of gas molecules in free space, which is different from the mean free path of gas molecules in nanoporous structures of aerogel. It is because the solid matrix in aerogel greatly restricts the gas molecules free movement. The results show that Eq. (8) derived by Zeng et al. [22,23] is a perfect depiction of gaseous thermal conductivity in aerogel. The gaseous conductivity of aerogel decreases greatly with the drop of pressure and reaches zero at about 104 Pa, which decreases dramatically faster than gaseous conductivity in xonotlite-type calcium silicate for the nanoporous structure features of aerogel. Figure 5 depicts the pressure dependence of gaseous conductivity in the composite insulation materials, where the experimental gaseous conductivity data includes both xonotlite-aerogel and ceramic fiber-aerogel composite insulation materials. It is shown that both Eqs. (5) and (8) do not match well with the experimental results. Generally, the gaseous conductivity of composite insulation materials should have the same trend as aerogel with a variation of pressure if xonotlite-type calcium silicate and ceramic fiber are filled fully with aerogel. Here, it does not meet this variation because the aerogel does not fill xonotlite-type calcium silicate and ceramic fiber materials entirely, and some micro level pores still exist in the composite insulation materials. All of the experimental data show that the gaseous conductivity decreases distinctly with the drop of pressure for xonotlite-type calcium, aerogel, and the composite insulation materials. This indicates that gaseous conductivity still contributes significantly to the total thermal conductivity of these kinds of insulation materials.

Concluding Remarks
Gaseous conductivity is one of the main contributors to the thermal conductivity of silica aerogel and its composite insulation materials, well known for their high porosity (>90%) and opencell structures, especially at ambient temperature. Many studies have researched materials preparation, thermal conductivity analysis, and measurement for these kinds of insulation materials during the past decade. However, the gaseous conductivity in these insulation materials is rarely discussed comprehensively. In this study, the gaseous conductivities confined in silica aerogel and its composite insulation materials are measured at different pressures with the THS method. Expressions derived based on the kinetic theory are used to analyze gaseous conductivity and compare the outcomes to experimental results. It is shown that both the gaseous conductivity of xonotlite-type calcium silicate and silica aerogel decreases significantly with the drop of pressure. The theoretical gaseous conductivity expressions match well with the experimental results of xonotlite-type calcium silicate and silica aerogel, respectively, but do not match with the experimental Transactions of the ASME

Fig. 5 Pressure dependence of gaseous conductivity in the composite insulation materials

conductivity estimation using Eq. (8), considering that a dependence relationship exists between the specific surface area and the bulk density of aerogel, the following relation is adopted [15] to estimate the specific surface area of aerogel according to the measured and simulated results in this study and in literature [36–38] 041301-4 / Vol. 134, APRIL 2012

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results for the composite insulation materials. This indicates that the aerogel does not completely fill the composite insulation material samples prepared using the vacuum dipping technology, and some microlevel pores still exist. The uncertainty analysis shows that the measurement error of the thermal conductivity determination is less than 3%.

Acknowledgment
The authors wish to express their appreciation to Dr. Hailong Yang for his help with the materials preparation. This research was financially supported by the National Natural Science Foundation of China (No. 50806021), the Fundamental Research Funds for the Central Universities (No. 10MG22) and the National Basic Research Program of China (2009CB219804).

Nomenclature
dg ¼ kB ¼ Kn ¼ K¼ lm ¼ ng ¼ P¼ Pr ¼ p¼ S¼ T¼ t¼ q¼ a¼ d¼ c¼ f¼ /¼ diameter of a gas molecule, m Boltzmann constant, J=K Knudsen number thermal conductivity, W=(m K) mean free path, m number density of gas molecules power, W Prandtl number pressure, Pa specific surface area, m2=kg temperature, K time, s density, kg=m3 accommodation coefficient characteristic system size, m ratio of gas constant porosity

Subscripts
g ¼ gas w ¼ wall

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Journal of Heat Transfer

APRIL 2012, Vol. 134 / 041301-5

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