Measurement of Thermal Diffusivity of Thermal Control Coatings by the Flash Method Using Two-Layer Composite Sample1

The thermal diffusivity of brittle coatings cannot be measured by the flash method directly because of the difficulty of preparing free-standing samples. Adopting the flash method using a two-layer composite sample, it is possible to measure thermal diffusivity if the radiant pulse is well defined and good thermal contact on the interface of the composite sample can be ensured. Using an equilateral trapezoidal pulse of an Nd-glass laser measuring the dimensionless temperature history of the rear face of the sample, we determined the thermal diffusivity of thermal control coatings in the temperature range of 80 to 200°C. The results for different thicknesses of substrate showed that the thermal contact resistance of the interface can be neglected.     

Recent development and applications of an optical method for measurements of thermophysical properties

The experimental determination of thermophysical properties has been greatly improved by the introduction of laser technology. The laser beam is used for sensing and also for heating (or exciting) the specimen. The advantage of using a laser beam is most strongly felt in the measurement of the thermal conductivity or the thermal diffusivity, which are some of the most difficult properties to measure. Interesting features of new techniques for investigating various aspects of thermal conductivity in fluids and solids are reviewed. An optical method, the so-called forced Rayleigh scattering method, or the laser-induced optical-grating method, has been developed and used extensively by the present author's group. The method is a high-speed remote-sensing method which can also quantitatively detect anisotropy, namely, direction dependence of heat conduction in the material. It was used for determination of the thermal diffusivity and its anisotropic behavior for high-temperature materials such as molten salts, liquid crystals, extended polymer samples, and flowing polymer melts under shear. Interesting applications of the method were demonstrated also for thermal diffusivity mapping and microscale measurement.Invited paper presented at the Twelfth symposium on Thermophysical Properties, June 19–24, 1994, Boulder, Colorado, U.S.A.     

Experimental investigation of nonuniform heating and heat loss from a specimen for the measurement of thermal diffusivity by the laser pulse heating method

Nonuniform heating effect and heat loss effect from the specimen in the measurement of thermal diffusivity by the laser pulse heating method have been experimentally investigated using an axially symmetric Gaussian laser beam and a laser beam homogenized with an optical filter. The degree of error is theoretically estimated based on the solution of the two-dimensional heat conduction equation under the boundary condition of heat loss from the surface of the specimen in the axial direction and the initial conditions of axially symmetric nonuniform and uniform heating. A correction factor, which is determined by comparison of the entire experimental and the theoretical history curves, is introduced to correct the values obtained by the conventionalt _1,2 method. The applicability of this modified curve-fitting method has been experimentally tested using materials in the thermal diffusivity range 10⁻³ to 1 cm²·s⁻¹. The experimental error due to the nonuniform heating and heat loss was reduced to approximately 3%.     

Calorimetric and transport properties of Zircalloy 2, Zircalloy 4, and Inconel 625

This paper presents the measurements and the results on thermal and electrical transport properties of three nuclear reactor cladding materials: Zircalloy 2, Zircalloy 4, and Inconel 625. Study of these materials constituted a part of the IAEA coordinated research program aimed at the generation and establishment of a reliable and complete database of the thermal properties of reactor materials. Measured properties include thermal diffusivity, specific heat, and electrical resistivity. Thermal diffusivity was measured by the laser pulse technique. Specific heat and electrical resistivity were measured using a millisecond-resolution direct electrical pulse heating technique. Thermal conductivity was computed from the experimentally determined thermal difusivity and specific heat functions and the room temperature density values. Measurements were performed in the 20 to 1500°C temperature range, depending on the material and property concerned.     

Cu2S相变过程中热扩散系数的精确测量和解析

材料发生相变时, 其结构和物理性能可能会发生剧烈的变化。采用激光闪射法测量热扩散系数时, 激光照射样品可能会伴随有光吸收/发射现象以及温度的显著升高, 导致其测量值偏离真实值。本工作以Cu₂S为研究对象, 发现激光照射样品后, 光吸收/发射的影响很小可以忽略, 但样品温度的升高则会明显影响热扩散系数的测量。通过构建具有不同石墨层厚度的石墨/Cu₂S双层结构, 利用石墨层减弱激光照射时Cu₂S样品的温度增加幅度, 成功使热扩散系数出现显著降低的起始温度接近采用DSC测量材料发生相变的起始温度。本研究进一步建立了石墨/Cu₂S双层结构样品的热流输运模型, 从石墨/Cu₂S双层结构样品的实验测试热扩散系数中解析出了Cu₂S在相变区间的本征热扩散系数。本工作对于理解和精确表征具有相变特征的离子导体热电材料、光敏、热敏材料的热扩散系数具有重要的意义。     

Measurements of Thermal Diffusivity for Thin Slabs by a Converging Thermal Wave Technique

The measurement of thermal diffusivity for thin slabs by a converging thermal wave technique has been studied. Temperature variation at the center of the heat source ring that is produced by a pulsed high-power laser is detected by an infrared detector. A computer program based on the finite difference method is developed to analyze the thermal diffusivity of the slabs. Materials of both high thermal diffusivity (CVD diamond wafer) and low thermal diffusivity (stainless-steel foil) have been used for the measurements. The measurements have been performed by varying the size and the thickness of specimen. The converging thermal wave technique has proved to be a good method to measure the thermal diffusivity of a CVD diamond without breaking the wafer into small specimens. The technique can be applied for a small slab if the diameter of the slab is two times larger than that of the heat source ring. The sensitivity of thickness in measuring the thermal diffusivity is low for ordinary CVD diamond. The use of the converging thermal wave technique for nonhomogeneous, nonuniform, and anisotropic materials has been accomplished by applying the finite difference method.     

Measurement of the Thermal Diffusivity of an Anisotropic Graphite Sheet Using a Laser-Heating AC Calorimetric Method

The thermal diffusivity of a graphite sheet having an extremely high anisotropy has been measured by a laser heating AC calorimetric method in the temperature range from 30 to 350 K. This graphite sheet has characteristics of high thermal diffusivity and high anisotropy, and it is only 100 m thick. Thus, it is difficult to apply the conventional AC technique. Therefore, we propose a simultaneous measurement method for the in-plane and out-of-plane thermal diffusivities, by analyzing the three-dimensional heat conduction process, which contains the effects of anisotropy and thermal wave reflections. This method was verified by checking with thermal diffusivity measurements of isotropic materials such as stainless steel and pure copper and was then applied to the anisotropic thermal diffusivity measurement of the graphite sheet.     

一种进口石墨箔低温热导率的测量

介绍了一套真空环境的热导率测试实验装置,测量了一种进口热解石墨箔在液氮温区到室温范围内的热导率。通过功率修正的方法得到了石墨薄膜热导率与温度的关系,平均误差在5%以内,为工程应用提供了数据支持。     

Thermal Diffusivity Measurements of Candidate Reference Materials by the Laser Flash Method

The National Metrology Institute of Japan (NMIJ) in AIST has investigated the laser flash method in order to establish a thermal diffusivity standard for solid materials above room temperature. A uniform pulse-heating technique, fast infrared thermometry, and a new data analysis method were developed in order to reduce the uncertainty in thermal diffusivity measurements. The homogeneity and stability of candidate reference materials such as isotropic graphite were tested to confirm their qualification as thermal diffusivity reference materials. Since graphite is not transparent to both the heating laser beam and infrared light for thermometry, the laser flash method can be applied to graphite without black coatings. Thermal diffusivity values of these specimens with different thicknesses, were measured with changing heating laser pulse energies. A unique thermal diffusivity value can be determined for homogeneous materials independent of the specimen thickness, by extrapolating to zero heating laser pulse energy on the plot of apparent thermal diffusivity values measured with the laser flash method as a function of heating laser pulse energy.Paper presented at the Fifteenth Symposium on Thermophysical Properties, June 22--27, 2003, Boulder, Colorado, U.S.A.     

Determination of thermal conductivity from specific heat and thermal diffusivity measurements of plasma-sprayed cermets

The thermal conductivities of three plasma-sprayed cermets have been determined over the temperature range 23–630°C from the measurement of the specific heat, thermal diffusivity, and density. These cermets are mixtures of Al and SiC prepared by plasma spray deposition and are being considered for various applications in magnetic confinement fusion devices. The samples consisted of three compositions: 61 vol% Al/39 vol% SiC, 74vol% Al/26vol% SiC, and 83 vol% Al/17 vol% SiC. The specific heat was determined by differential scanning calorimetry through the Al melt transition up to 720°C, while the thermal diffusivity was determined using the laser flash technique up to 630°C. The linear thermal expansion was measured and used to correct the diffusivity and density values. The thermal diffusivity showed a significant increase after thermal cycling due to a reduction in the intergrain contact resistance, increasing from 0.4 to 0.6 cm²·^–1 at 160°C. However, effective medium theory calculations indicated that the thermal conductivities of both the Al and the SiC were below the ideal defect-free limit even after high-temperature cycling. The specific heat measurements showed suppressed melting points in the plasmasprayed cermets. The 39 vol% SiC began a melt endotherm at 577°C, which peaked in the 640–650°C range depending on the sample thermal history. Chemical and X-ray diffraction analysis indicated the presence of free silicon in the cermet and in the SiC powder, which resulted in a eutectic Al/Si alloy.Paper presented at the Ninth Symposium on Thermophysical Properties, June 24–27, 1985, Boulder, Colorado, U.S.A.     

Thermal Diffusivity Measurement of High-Conductivity Materials by Dynamic Grating Radiometry

A new apparatus based on dynamic grating radiometry (DGR) to measure the thermal diffusivity of high-conductivity materials such as graphite and diamond has been developed. In the DGR method, a sample surface is heated by interference of two pulsed laser beams, and the decay of temperature at a spot on the thermal grating is monitored by an infrared detector. In the ideal case where the grating period is much smaller than the light absorption length, the thermal diffusivity parallel to the surface can be determined from the decay constant and the grating period. This paper describes a procedure to extract the thermal diffusivity parallel to the plane while eliminating the effect of anisotropy and gives results for a preliminary measurement using Zr foil. A quadratic dependence of the time constant on fringe space has been observed in the fringe space change. Data are also presented for a 0.1-mm-thick graphite sheet. The results indicate the capability of DGR to measure anisotropic high-conductivity materials.     

Thermal diffusivity and conductivity of Li2ZrO3 using the modulated electron beam technique

Thermal diffusivity and thermal conductivity of three Li₂ZrO₃ specimens with two different density values, 82.6 and 87% theoretical density, have been measured between 350 and 900°C. The modulated electron beam thermal diffusivity method was used. Heating the specimens above some 850°C but below 900°C results in a reversible increase in both the diffusivity and the conductivity. When heating to higher temperatures generally still higher increases are noticed but measurements become rapidly unstable and irreversible.     

A noncontact method for measuring thermal conductivity and thermal diffusivity of anisotropic materials

A noncontact method for measuring the thermal conductivity and thermal diffusivity of anisotropic materials is proposed. This method is based on the fact that the surface temperature variation with time depends on the thermal properties of the material when its surface is heated locally. The three-dimensional transient heat conduction equation in the material is solved numerically. The dimensionless average surface temperature variations are obtained along each principal axis: that is, thex andy axes. The relation between the dimensionless temperature and the Fourier number is expressed by a polynomial equation and used as a master plot, which is a basic relation to be compared with measured temperature variation. In the experiments, the material surface is heated with a laser beam and the surface temperature profiles are measured by an infrared thermometer. The measured temperature variations with time are compared with the master plots to yield the thermal conductivity λ _x and thermal diffusivityx _v in thex direction and the thermal conductivity ratioE _xy (=λ _y λ _x ) simultaneously. To confirm the applicability and the accuracy of the present method, measurements were performed on multilayered kent-paper, vinyl chloride, and polyethylene resin film, whose thermal properties are known. From numerical simulations, it is found that the present method can measure the thermophysical properties λ _x , α _x andE _xy within errors of ±6, ±22, and ±5%, respectively, when the measuring errors of the peak heat flux, the heating radius, and the surface temperature rise are assumed to be within ±2, ±3%, and ±0.2 K, respectively. This method could be applied to the measurement of thermophysical properties of biological materials.     

Influence of Thermal Strain on Thermal Properties of Composites

The temperature dependence of the thermal expansion characteristics of the AS21 magnesium alloy, AS21–25 vol% Saffil fiber composite and the Mg-10 vol% Saffil fiber composite has been measured in the temperature range from 20 to 380°C. The expansion characteristics were influenced by the residual and thermal strains. The residual strain was removed within the first thermal cycle. The relative elongation of the tensile pre-deformed AS21–25 vol% Saffil fiber composite is lower than that for the sample without deformation and for the composite pre-deformed in compression. The anisotropy of the thermal expansion is demonstrated on the Mg-10 vol% Saffil fiber composite. The coefficient of thermal expansion (CTE) in the transverse direction (TD) (the planes of the short Saffil fibers are laid perpendicular to the axis of the sample) is higher than the CTE in the longitudinal direction (LD) (the planes of the short Saffil fibers are laid parallel to the axis of the sample). The anisotropy and the thermal strain influence the thermal diffusivity for AS21 composites investigated at temperatures between 20 and 380°C.Paper presented at the Seventeenth European Conference on Thermophysical Properties, September 5-8, 2005, Bratislava, Slovak Republic.     

激光脉冲法研究半透明PI/SiO_2薄膜的热扩散率

激光脉冲法在应用于测量对实验探测波段红外线半透明的材料热扩散率时遇到了困难。文中提出了新的解决办法:即通过对理论探测曲线进行分析,并通过在实际探测曲线上的升温幅度和特征点计算得到了热扩散率,成功地解决了这一难题。在-73℃~290℃的范围内获得了对激光和红外线都是半透明的聚酰亚胺(PI)薄膜的热扩散率,并研究了室温下PI/SiO2复合材料的热扩散率随SiO2含量的变化规律。     

Depth-Resolved Surface Thermophysical Property Measurement by Laser-Produced Plasmas

A new laser-based method for real-time in situ measurement of thermophysical properties of materials has been developed. It entails production by a high-power laser pulse of a plasma plume from the surface of a condensed-phase specimen and simultaneous measurement of a material's response to the excitation. The specimen may be a solid or in a molten state at high temperatures. It has been shown that the thermal diffusivity can be determined, for instance, from the mass loss due to laser excitation. In one implementation the mass loss is determined from the impulse imparted on the surface by the ablated matter which is measured by an impulse transducer. In this paper, we present a new spectroscopic method for measurement of the mass loss, facilitating in situ non-contact measurement of the thermal diffusivity for the first time. An implementation of this method is described, whereby the thermal diffusivity of a complex layered surface is determined as a function of depth with resolutions as small as 13 nm.     

Study on a Thermal-diffusivity Standard for Laser Flash Method Measurements

The National Metrology Institute of Japan (NMIJ) of AIST has been studying the laser flash method in order to establish an SI traceable thermal- diffusivity standard. Key technologies have been developed to reduce the uncertainty in laser flash measurements. In the present study, an uncertainty evaluation has been carried out on the laser flash measurement method in order to determine the thermal diffusivity value of IG-110, a grade of isotropic high-density graphite, as a candidate reference material. The thermal diffusivity measured by the laser flash method is derived from a specimen thickness and a heat diffusion time. And a laser flash measurement is carried out at a given temperature. The measurement system is composed of three sections corresponding to each measured quantity: length, time, and temperature. Therefore, we checked and calibrated our measurement system, and estimated the uncertainty of measurement results for the case of a grade of isotropic graphite.Paper presented at the Seventeenth European Conference on Thermophysical Properties, September 5–8, 2005, Bratislava, Slovak Republic.     

Thermal expansion of siliconated pyrolytic carbon

The lattice and bulk thermal expansions perpendicular to the layer plane of siliconated pyrolytic carbon, PC(Si), produced by pyrolyzing a mixture of propane gas and silicon tetrachloride vapour at the deposition temperatures of 1440 to 2025° C, have been measured over the temperature ranges 20 to 550° C and 20 to 960° C, respectively. The expansion behaviours of PC(Si) are related to the density and the degree of preferred orientation of crystallites, as is the case for pyrolytic carbon without silicon PC. At a deposition temperature of about 1700° C, the bulk thermal expansion coefficient of PC(Si) is about three times as large as that of PC.     

Measurement of thermal diffusivity by the flash method for a two-layer composite sample in the case of triangular pulse

A method for measuring thermal diffusivity in one of the layers of a two-layer composite sample has been described. The heat transfer problem of a two-layer sample associated with pulse thermal diffusivity measurements has been analyzed for two cases: exponential and square-wave pulses. According to our measurements, a triangular heat-pulse function approximates reasonably well the output of the Nd-glass laser. In this paper, an expression is derived for the temperature transient at the rear face of two-layer sample being subjected to a triangular heat-pulse input on the front face. The analytical solution of the problem forms the basis of our method of data reduction. This solution has been programmed for computer processing of the data. The method described here has been successfully tested by limited measurements on copper and iron.Paper presented at the Ninth Symposium on Thermophysical Properties, June 24–27, 1985, Boulder, Colorado, U.S.A.