Hemispherical Total Emissivity of Niobium, Molybdenum, and Tungsten at High Temperatures Using a Combined Transient and Brief Steady-State Technique

The hemispherical total emissivity of three refractory metals, niobium, molybdenum, and tungsten, was measured with a new method using a combined transient and brief steady-state technique. The technique is based on rapid resistive self-heating of a solid cylindrical specimen in vacuum up to a preset high temperature in a short time (about 200 ms) and then keeping the specimen at that temperature under steady-state conditions for a brief period (about 500ms) before switching off the current through the specimen. Hemispherical total emissivity is determined at the temperature plateau from the data on current through the specimen, the voltage drop across the middle portion of the specimen, and the specimen temperature using the steady-state heat balance equation based on the Stefan–Boltzmann law. Temperature of the specimen is determined from the measured surface radiance temperature and the normal spectral emissivity; the latter is obtained from laser polarimetric measurements. Experimental results on the hemispherical total emissivity of niobium (2000 to 2600 K), molybdenum (2000 to 2700 K), and tungsten (2000 to 3400 K) are reported.     

A dynamic technique for measurements of thermophysical properties at high temperatures

A technique is described for the dynamic measurement of selected thermophysical properties of electrically conducting solids in the range 1500 K to the melting temperature of the specimen. The technique is based on rapid resistive selfheating of the specimen from room temperature to any desired high temperature in less than 1 s by the passage of an electrical current pulse through it and on measuring the pertinent quantities, such as current, voltage, and temperature, with millisecond resolution. The technique was applied to the measurement of heat capacity, electrical resistivity, hemispherical total emissivity, normal spectral emissivity, thermal expansion, temperature and energy of solid-solid phase transformations, melting temperature, and heat of fusion. Two possible options for the extension of the technique to measurements above the melting temperature of the specimen are briefly discussed. These options are: (1) submillisecond heating of the specimen and performance of the measurements with microsecond resolution, and (2) performance of the experiments in a near-zero-gravity environment with millisecond resolution.Paper presented at the Japan-United States Joint Seminar on Thermophysical Properties, October 24–26, 1983, Tokyo, Japan.     

Simultaneous measurements of specific heat and total hemispherical emissivity of chromel and alumel by a transient calorimetric technique

Using a transient calorimetric technique, the specific heat and total hemispherical emissivity of chromel and alumel were measured simultaneously in the temperature range 360–760 K. Two types of specimens for each material were prepared. To obtain reliable experimental values of specific heat and total hemispherical emissivity, an expression for the time history of the temperature of the specimens was developed; this expression is accurate over the whole temperature range. An error analysis is made and the uncertainty (the total error) in the values of specific heat and total hemispherical emissivity is estimated to be 3.1% for the well-designed specimens.

     

Specific heat capacity and emissivity measurements of ribbon-shaped graphite using pulse current heating

A measurement method for specific heat capacity and hemispherical total emissivity of electrically conductive materials with pulse current heating is investigated, in which a ribbon-shaped sample is heated up to 3000K in a subsecond-duration experiment. Specific heat capacity and hemispherical total emissivity of the sample are calculated from the time variations of heat generations and surtace temperature of the sample measured during heating and cooling phases. The true surface temperature of the rihhon-shaped samples is obtained with a radiation thermometer: the directional spectral emissivity of the sample surface is measured using a hemisplicrical mirror centered at the sample surface. Measurements are performed for POCO AXM-5Ql graphite in the temperature range from 1500 to 3000 K.Paper presented at the Twelfth Symposium on Thermophysical Properties. June 19–34, 1994 Boulder, Colorado, U.S.A.     

Evaluation of Hemispherical Total Emissivity for Thermal Radiation Calorimetry

An attempt to derive the hemispherical total emissivity from the normal emission spectrum is proposed for Vycor and fused silica glasses. The normal emission spectrum from a clear surface has been measured at steady state in the temperature range from 400 to 750 K. The sample is heated on one metal-backed face by thermal radiation from a heater. Temperatures inside the sample were monitored by thermocouples at two points near the surfaces. Evaluation of the hemispherical total emissivity from the normal emission spectrum is determined by means of Kramers–Krönig analysis and virtual mode equations. Assuming a linear temperature distribution within the sample, the thermal conductivities of silicate glasses were obtained at elevated temperatures. The results are comparable with those obtained by previous investigators. The effect of radiation heat transfer in a sample is also discussed.     

A dynamic technique for measuring normal spectral emissivity of electrically conducting solids at high temperatures with a high-speed spatial scanning pyrometer

A dynamic (subsecond) technique is described for measuring normal spectral emissivity of electrically conducting solids at high temperatures, primarily in the range 1800 K up to near their melting point. The basic method involves resistively heating a tubular specimen from ambient temperature through the temperature range of interest in less than 1 s by passing an electrical current pulse through it, while using a high-speed spatial scanning pyrometer to measure spectral radiance temperatures along a 25-mm length on the specimen. This portion of the specimen includes a small rectangular hole that approximates a blackbody cavity. Measurements of spectral radiance temperature of the specimen surface as well as specimen true temperature enable the determination of the normal spectral emissivity of the surface via Planck's law. The applicability of the technique is demonstrated by measurements performed on molybdenum in the range 1900–2850 K.     

Measurement of thermophysical properties by a pulse-heating method: Thoriated tungsten in the range 1200 to 3600 K

Thoriated tungsten (tungsten, 98%: thorium oxide. 2 % ) is a widely used electrode material for inert-gas arc-welding. Data for the heat capacity, electrical resistivity. and hemispherical total emissivity of this material are reported for the temperature range 1200–3600 K. A subsecond pulse-heating technique was applied to rod specimens: radiance temperature was measured by high-speed pyrometry. Literature values of the temperature dependence of the normal spectral emissivity of tungsten were used to obtain true temperatures, using the melting point of thoriated tungsten as a calibration point. Reported uncertainties for the properties are 4 % for heat capacity, 1.5 % for electrical resistivity, and 7 % for hemispherical total emissivity.Paper presented at the Twelfth Symposium on Thermophysical Properties, June 19–24, 1994, Boulder, Colorado, U.S.A.     

Measurements of specific heat and electrical resistivity of austenitic stainless steel (St. 1.4970) in the range 300–1500 K by pulse calorimetry

A direct heating pulse calorimetric technique has been applied for the measurements of specific heat, electrical resistivity, and hemispherical total emissivity of austenitic stainless steel (St. 1.4970), a candidate for thermal conductivity standard reference material. The specific heat and electrical resistivity were measured in the range 300 to 1500 K, and the hemispherical total emissivity was measured in the range 1300 to 1500 K. The maximum measurement uncertainties were estimated to be 3% for specific heat, 1% for electrical resistivity, and 5% for emissivity.Paper presented at the Second Workshop on Subsecond Thermophysics, September 20–21, 1990, Torino, Italy.     

Normal Spectral Emissivity of Niobium (at 900 nm) by a Pulse-Heating Reflectometric Technique

The normal spectral emissivity of niobium strip specimens was measured using a new pulse-heating reflectometric technique. The hemispherical spectral reflectivity of the surface of a strip tangent to an integrating sphere is determined by a high-speed lock-in technique. At the same time, the radiance temperature of the strip is measured by high-speed pyrometry from approximately 1000K to the melting point. Details of the measurement method and of the related calibration techniques are reported. Results of the normal spectral emissivity of niobium at 900 nm from room temperature to its melting point are presented, discussing differences related to the heating rate and to surface conditions.     

A Transient Method for Total Emissivity Determination

A transient method for determining the hemispherical total emissivity of solids is investigated using an emissometer recently developed at the NPL. The emissivity is calculated from measurement of the sample surface temperature coupled with a knowledge of its bulk thermal properties. This was conducted as part of the current work to validate the new NPL apparatus for high temperature emissivity measurements. A theoretical study shows that when a thermally thick sample is allowed to radiate instantaneously into a cold environment, then the resulting transient surface temperature depends solely on its hemispherical total emissivity and effusivity. This approach is used to obtain a hemispherical total emissivity value for Fecralloy steel, and it is then compared with the normal total emissivity value obtained by integration of normal spectral emissivity measurements in the wavelength range 2 to 9m.     

Thermophysical Properties by a Pulse-Heating Reflectometric Technique: Niobium, 1100 to 2700 K

Pulse-heating experiments were performed on niobium strips, taking the specimens from room temperature to the melting point is less than one second. The normal spectral emissivity of the strips was measured by integrating sphere reflectometry, and, simultaneously, experimental data (radiance temperature, current, voltage drop) for thermophysical properties were collected with sub-millisecond time resolution. The normal spectral emissivity results were used to compute the true temperature of the niobium strips; the heat capacity, electrical resistivity, and hemispherical total emissivity were evaluated in the temperature range 1100 to 2700 K. The results are compared with literature data obtained in pulse-heating experiments. It is concluded that combined measurements of normal spectral emissivity and of thermophysical properties on strip specimens provide results of the same quality as obtained using tubular specimens with a blackbody. The thermophysical property results on niobium also validate the normal spectral emissivity measurements by integrating sphere reflectometry.     

Measurement of Total Hemispherical Emissivity Using a Calorimetric Technique

An apparatus has been designed to measure, using a calorimetric technique, the total hemispherical emissivity of opaque solid materials from –20 to 200°C. The originality of the technique is the use of two samples and thermal guard rings in order to ensure one-dimensional heat flow in each sample and to reduce heat-loss corrections. Two temperatures are measured in each sample at two distances from the surface, and the surface temperature of each sample is linearly extrapolated. The mean total hemispherical emissivity of the two samples is calculated using a model that considers the main surfaces radiating in the chamber. Unwanted heat losses are evaluated and corrected. The facility design, model of calculation, evaluation of corrections, and uncertainty assessment are described. The measurement technique was validated by comparison to results from a study using another technique. The expanded uncertainty (k = 2) of the total hemispherical emissivity is between ±0.005 and ±0.03. Paper presented at the the Seventeenth European Conference on Thermophysical Properties, September 5–8, 2005, Bratislava, Slovak Republic.     

Radiance temperatures (in the wavelength range 519–906 nm) of tungsten at its melting point by a pulse-heating technique

Radiance temperatures (at six wavelengths in the range 519–906 nm) of tungsten at its melting point were measured by a pulse-heating technique. The method is based on rapid resistive self-heating of the specimen from room temperature to its melting point in less than 1 s; and on simultaneously measuring the specimen radiance temperatures every 0.5 ms with a high-speed six-wavelength pyrometer. Melting was manifested by a plateau in the radiance temperature versus time function for each wavelength. The melting-point radiance temperatures for a given specimen were determined by averaging the measured temperatures along the plateau at each wavelength. The melting-point radiance temperatures for tungsten were determined by averaging the results at each wavelength for 10 specimens (standard deviation in the range 0.5–1.1 K, depending on the wavelength) as follows: 3319 K at 519 nm, 3236 K at 615 nm, 3207 K at 652 nm, 3157 K at 707 nm, 3078 K at 808 nm, and 2995 K at 906 nm. Based on estimates of the random and systematic errors arising from pyrometry and specimen conditions, the total uncertainty in the reported values is about ±7 K at 653 nm and ± 8 K at the other wavelengths.Paper presented at the Third Workshop on Subsecond Thermophysics, September 17–18, 1992, Graz, Austria.     

Efficiency and behavior of textured high emissivity metallic coatings at high temperature

Three metallic coatings with textured surfaces, made of rhenium, tungsten and molybdenum, were studied in the frame of the Solar Probe Plus mission (NASA) as candidate materials. The role of these coatings is to dissipate a maximum of energy from a hot instrument facing the Sun, by the mean of their high total hemispherical emissivity. The total hemispherical emissivity of the three coatings was measured in the temperature range 1100–1900 K, as well as over time in order to study their high temperature stability. Various emissivity levels were obtained depending on the surface texture. The highest total hemispherical emissivity was obtained on a rhenium coating, with an emissivity of 0.8 in the temperature range 1300–1700 K. However, this rhenium coating with a fine, sharp surface texture, presented an instability at high temperature, which might limit its optimal operating temperature to about 1500 K. As for the tungsten coating, the total hemispherical emissivity was increased by a factor 2 due to the enhanced surface texturation and its great stability over the whole temperature range was shown.     

A Multiwavelength Reflectometric Technique for Normal Spectral Emissivity Measurements by a Pulse-Heating Method

A new technique has been developed for the direct measurement of the normal spectral emissivity at several wavelengths in pulse-heating conditions, adding some novel features to previous versions of this type of apparatus. Pulse-heating experiments were performed on niobium strip specimens, taking the specimen from room temperature to the melting point using rapid resistive self-heating. The normal spectral emissivity was measured at three wavelengths by a multi-wavelength reflectometric technique. At the same time, the radiance temperature was measured at the same wavelengths by a high-speed pyrometer from approximately 1100 K to the melting point. Details of the method, the measurement apparatus, and the calibration technique are described. Preliminary results for the normal spectral emissivity of niobium at 633, 750, and 900 nm over a wide temperature range are presented.     

Radiance temperatures at 1500 nm of niobium and molybdenum at their melting points by a pulse-heating technique

Radiance temperatures at 1500 nm of niobium and molybdenum at their melting points were measured by a pulse-heating technique. The method is based on rapid resistive self-heating of the strip-shaped specimen from room temperature to its melting point in less than I s and measuring the specimen radiance temperature every 0.5 ms with a high-speed infrared pyrometer. Melting of the specimen was manifested by a plateau in the radiance temperature-versus-time function. The melting-point radiance temperature for a given specimen was determined by averaging the measured values along the plateau. A total of 12 to 13 experiments was performed for each metal under investigation. The melting point radiance temperatures for each metal were determined by averaging the results of the individual specimens. The results for radiance temperatures at 1500 nm are as follows: 1983 K for niobium and 2050 K for molybdenum. Based on the estimates of the uncertainties arising from the use of pyrometry and specimen conditions, the combined uncertainty (two standard-deviation level) in the reported values is ± 8 K.Paper presented at the Fourth International Workshop on Subsecond Thermophysics, June 27–29, 1995, Köln, Germany.     

Radiance temperatures (in the wavelength range 525 to 906 nm) of vanadium at its melting point by a pulse-heating technique

The radiance temperatures (at six wavelengths in the range 525 to 906 nm) of vanadium at its melting point were measured by a pulse-heating technique. The method is based on rapid resistive self-heating of the specimen from room temperature to its melting point in less than 1 s and on simultaneously measuring the specimen radiance temperatures every 0.5 ms with a high-speed six-wavelength pyrometer. Melting was manifested by a plateau in the radiance temperature-vs-time function for each wavelength. The melting-point radiance temperatures for a given specimen were determined by averaging the measured temperatures along the plateau at each wavelength. The melting-point radiance temperatures for vanadium as determined by averaging the results at each wavelength for 16 specimens (standard deviation in the range 0.3 to 0.4 K. depending on the wavelength) are 2030 K at 525 nm, 1998 K at 622 nm, 1988 K at 652 nm, 1968 K at 714 nm, 1935 K at 809 nm, and 1900 K at 906 nm. Based on estimates of the random and systematic errors that arise from pyrometry and specimen conditions, the resultant uncertainty (2 SD level) in the reported values is about ±7 K at each wavelength.     

Development of a Millisecond Pulse-Heating Apparatus

A millisecond pulse-heating apparatus is presently under development at the Harbin Institute of Technology (HIT). The design is based on systems previously developed both at NIST (U.S.A.) [1, 2] and IMGC (Italy) [3] for the measurement of several thermophysical properties with millisecond time resolution. The apparatus uses rapid resistive self-heating of a strip-shaped specimen from room temperature to a pre-chosen maximum temperature. Power is furnished by a subsecond-duration electrical current pulse through the specimen. Simultaneous measurements are carried out for several quantities. The maximum current is up to 2000 A. Experiments are performed on strip-shaped specimens with the following typical dimensions: 80 mm in length, 10 mm in width, and 1 mm in thickness. The specimen is contained in a large vacuum chamber (bigger than 300 mm in both diameter and height) whose inner wall is coated with a nonreflecting paint. A special designed high-speed pyrometer will be used to measure the temperature of the specimen through one of two quartz windows of the chamber. The heat capacity, the electrical resistivity, the total hemispherical emissivity, and normal spectral emissivity of the specimen are measured by using this apparatus for various materials.     

Thermophysical Properties of Solid Phase Hafnium at High Temperatures

The thermophysical properties of several hafnium samples with a content of zirconium below 1% were experimentally studied over a wide temperature range. The specific heat capacity and specific electrical resistivity were measured from 300 to 2340 K, the hemispherical total emissivity from 1000 to 2130 K, while the thermal diffusivity was measured in the range from 300 to 1470 K. The thermal conductivity and Lorentz number were computed from measured properties for the range from 300 to 1470 K. The specific heat capacity, specific electrical resistivity, and hemispherical total emissivity were measured by subsecond pulse calorimetry, and the thermal diffusivity using the laser flash method. Samples in the form of a thin rod or wire, and in the form of a thin disk were used in the first and second methods, respectively. For data reduction and computation of relevant parameters, recent literature values of the linear thermal expansion were used. The results are compared with literature data and discussed.