Uncertainty of Thermal Diffusivity Measurements by Laser Flash Method

The laser-pulse method is a well-established nonsteady-state measurement technique for measuring the thermal diffusivity, a, of solid homogeneous isotropic opaque materials. BNM-LNE has developed its own bench based on the principle of this method in which the thermal diffusivity is identified according to the “partial time moments method.” Uncertainties of thermal diffusivity by means of this method have been calculated according to the ISO/BIPM “Guide to the Expression of Uncertainty in Measurement.” Results are presented for several cases (Armco iron, Pyroceram 9606) in the temperature range from 20 to 800°C. The relative expanded (k = 2) uncertainty of the thermal diffusivity determination is estimated to be from ±3 to ±5%, depending on the material and the temperature. Paper presented at the Fifteenth Symposium on Thermophysical Properties, June 22–27, 2003, Boulder, Colorado, U.S.A.     

基于激光闪光法的立式热扩散率测量装置研究

介绍了基于激光闪光法的立式热扩散率测量装置,利用脉冲激光对样品进行均匀加热,使样品内部产生一维热流,并通过红外探测器测量样品温升信号,采用立式真空加热炉控制测量温度环境,实现室温至1600℃的热扩散率测量。用该装置测量厚度为1. 1 mm,直径为10 mm的不锈钢样品,测量结果与PTB参考数据的偏差小于1%。     

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.     

Evaluation of the Effective Sample Temperature in Thermal Diffusivity Measurements Using the Laser Flash Method

In the measurement of thermal diffusivity by the laser flash method, a temperature rise occurs in the sample as a pulsed laser hits on the sample surface. Due to the temperature dependence of thermal diffusivity of the sample, the thermal diffusivity corresponds to a temperature that is larger by T _eff than the temperature before laser irradiation is applied. This effective temperature rise, T _eff, has been investigated by using a numerical simulation. The results indicate that the effective temperature rise is almost equal to a maximum temperature rise, T _M, of the back surface of the sample in cases where both linear and nonlinear temperature variations of thermal diffusivity are considered.     

Thermal Diffusivity Measurements on Insulation Materials with the Laser Flash Method

An iterative approach is adopted to determine the thermal diffusivity of the xonotlite-type calcium silicate insulation material with very low thermal conductivity. The measurements were performed with a conventional laser flash apparatus by rear-face detection of the temperature response of the three-layered sample, where the insulating material is sandwiched between two iron slices. In the evaluation of the thermal conductivity, the theoretical curve is fitted to the complete temperature–time curve, instead of just using the t _1/2 point. The theoretical model is based on the thermal quadrupole method. The nonlinear parameter estimation technique is used to estimate simultaneously the thermal diffusivity, heat transfer coefficient, and absorbed energy. Based on experimental results, the optimal thickness range of the insulation material in the sample is indicated as 1.6 to 1.9 mm. The effects of the uncertainties of the thicknesses, contact resistance, and thermophysical properties of the three layers on the measurement uncertainty are estimated, giving an overall uncertainty in the thermal conductivity of approximately 7.5%.Paper presented at the Seventh Asian Thermophysical Properties Conference, August 23–28, 2004, Hefei and Huangshan, Anhui, P. R. China.     

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

A working group for standardization has organized to establish the Japanese Industrial Standard (JIS) for thermal diffusivity measurements of metals in the temperature range of 300–1700 K by the laser flash method. As candidate reference materials with high purity, high-temperature stability, and easy-to-get on a commercial basis, tantalum, niobium, and molybdenum have been selected. Thermal diffusivity values of the specimens, cut out of these materials, have been measured independently by members of the working group. Comparisons of results have been performed for different high-temperature stabilities, repeatabilities, and manufacturers, as well as by different members. Comparisons show that the measured values agree within 10% for different specimens by different institutions, and no systematic differences have been observed for materials from different manufacturers. The measured results for molybdenum specimens agree well with the recommended values of thermophysical properties of matter from the TPRC data series, and the high-temperature stability is found to be the best. The results for tantalum and niobium, however, show significant differences with those of the TPRC data series in the high-temperature range, and some further study on the stability of these materials is needed for recommending these values. As a result, molybdenum can be recommended as a reference material for practical use of the laser flash method. Paper presented at the Fifteenth Symposium on Thermophysical Properties, June 22–27, 2003, Boulder, Colorado, U.S.A.     

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.     

激光闪光法测量固体材料热扩散率的研究进展

基于瞬态原理的激光闪光法因其具有所用试样小、测试周期短等优点,在测量固体材料的热扩散率方面发挥了重要作用,应用较为广泛。根据近些年来在激光闪光法可测材料种类、关键技术问题以及优化和改进3个方面的研究进展,介绍了其应用情况,并分析总结了其研究重点、难点以及研究价值,最后讨论了激光闪光法存在的挑战和前景,为未来激光闪光法在更多领域的应用提供参考。     

Evaluation of the Heat Leakage in the Thermal Diffusivity Measurement of Molten Metals by a Laser Flash Method

Evaluation of the radiative and conductive heat loss from a molten metal sample to the cell has been made in order to obtain accurate thermal diffusivities of molten metals at high temperature with a laser flash method. The results suggest that thermal diffusivity values of molten nickel can be determined in the temperature range from 1728 to 1928 K with an uncertainty of ±3% in comparison with case considering only the effect of radiative heat loss. The usefulness of a cell for a laser flash method has been confirmed by applying simulated results to evaluate the heat leakage in the thermal diffusivity measurement of molten metals.     

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。     

Nonlinear Effects in Laser Flash Thermal Diffusivity Measurements

The numerical solution of the nonlinear heat conduction equation is used to analyze nonlinear effects in the laser flash method, when the thermophysical parameters of the sample depend on the temperature. A parameter estimation technique is proposed to determine the temperature dependence of the thermal diffusivity from a response curve. Computer generated data, as well as real experimental data, were used to demonstrate the reliability of the technique.     

The Effect of the Surrounding Medium and Its Pressure on Data Obtained in Thermal Diffusivity Measurements Using the Flash Method

This work describes experimental measurements made with a high temperature–high pressure flash thermal diffusivity instrument, using nitrogen, argon, and helium as environment. Data was generated using pressures from vacuum to 30 bar in the temperature range of ambient to 1000°C. NIST SRM 8425 (Poco AXM 5Q, fine grain graphite) was used for the tests. A total of 2.970 data points were obtained, showing a clear and prominent shift in the data, depending on the pressure and the thermal properties of the surrounding gas. Preliminary conclusions drawn from the work indicate the influence of heat conduction, convection, and diffusion through the environmental gas, on the thermal diffusivity results.     

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.     

Thermal Diffusivity Measurements of Liquid Silicate Melts

The effect of structure on the thermal diffusivities/conductivities for liquid silicates have been summarized based on recent experimental work carried out by the Royal Institute of Technology, Stockholm and the Tokyo Institute of Technology using the laser-flash and the hot-wire methods, respectively. In the former case, the effective thermal diffusivity was measured by a three-layer method. The relationship proposed by Mills that the thermal conductivity of silicates increases with a decrease in the ratio of NBO/T (number of non-bridging oxygens per tetrahedrally coordinated atom) has been well supported by the effective thermal diffusivity data for the liquid CaO-Al₂O₃-SiO₂ slags. However, it has been shown that for the slags having a higher CaO/Al₂O₃ ratio, the effective thermal diffusivity is roughly constant independent of the ratios of NBO/T. It has been concluded that when the silicate network is largely broken down, the phonon mean free path is not affected by the structure. It has been found by the hot-wire method that the magnitudes of thermal resistivity are in the hierarchy Li₂O-SiO₂2O-SiO₂2O-SiO₂ despite their similar values of NBO/T. It has been concluded that the ionicity of non-bridging oxygen ions is also a factor controlling the thermal conductivity of silicates as well as the number of broken bridges in the silicate network. The effective thermal diffusivity was measured for the CaO-Al₂O₃-SiO₂-FeO system to elucidate the radiation contribution to the effective thermal diffusivity. It has been found that the effective thermal diffusivity increases with an increase in FeO content. It can be considered that the strong absorption and emission within the liquid slag films caused by the Fe²⁺ ions enhances the photon heat transfer.     

Multidimensional Flash Diffusivity Measurements of Orthotropic Materials

A generalization of the radial flash technique is presented whereby the thermal diffusivity of an orthotropic solid is measured in directions parallel and perpendicular to the flash source. The theoretical formulation is based on a Green's function approach which assumes a general orthotropic solid with three mutually orthogonal thermal diffusivities (or conductivities). Using this approach, a solution to this problem is presented which can be used to develop solutions for arbitrary pulse waveforms and incident geometries. Analytical and numerical results are presented for two-dimensional and three-dimensional cases of finite and semiinfinite solids. Characteristic equations which describe the ratio of the temperatures at two points along a principal axis are given. The equations show excellent agreement with numerical predictions as well as experimental results. A parameter estimation approach is given which improves on the accuracy of the radial flash technique in the determination of thermal diffusivity from experimental data.     

Effect of the Response Delay of the Measuring System on Thermal Diffusivity Measurement Using the Flash Method1

This work investigates the effect of the response delay of a measuring system on a thermal diffusivity measurement. A model of an m th-order delay in the measuring system is introduced, and a general expression for the output of the system with temperature response as input is derived. The effect on the temperature response caused by such a system is discussed. As a practical example, a third-order measuring system is considered. The measured temperature responses of stainless steel foils are compared with those calculated with the model of a third-order delay system. Good agreement between the two results is shown.     

New Apparatus for Thermal Diffusivity and Specific Heat Measurements at Very High Temperature

The thermal characterization of a material under its conditions of use (temperature, pressure, etc.) is an essential step to check its adequacy with regard to a specific application and to predict its behavior. For needs of material characterization, Commissariat à l’Energie Atomique (CEA) has developed with Laboratoire National de Métrologie et d’Essais (LNE) a new apparatus to study thermophysical properties of solid materials in the range from 300 to 3300 K. This setup allows measurements of either the thermal diffusivity by the laser flash method or the specific heat by drop calorimetry. First, thermal diffusivity measurements have been performed on Armco iron and POCO AXM-5Q1 graphite. The measured values are in agreement with results obtained by other laboratories with a relative deviation of less than 6%.Paper presented at the Seventeenth European Conference on Thermophysical Properties, September 5–8, 2005, Bratislava, Slovak Republic.     

Evaluation of the Thermal Diffusivity of Thin Specimens from Laser Flash Data

Thermal-diffusivity data obtained by a pulse technique are substantially in error if the sample thickness becomes too small. In this case the inevitable spike caused by the trigger pulse for the laser and the thermogram of the specimen are interacting, and a superposition of both signals is recorded, whose evaluation with standard algorithms systematically underestimates the thermal diffusivity of materials. Therefore, this incorrect calculation corresponding to the spike-thermogram overlay was investigated for general tendencies, and a calculation method transferring the experimental data obtained for small thicknesses into representative thermal diffusivity values for the investigated material will be introduced.