Measurement of the heat of fusion of tantalum by a microsecond-resolution transient technique

The heat of fusion of tantalum was measured using a microsecond-resolution pulse-heating technique. The technique is based on rapid (about 100-s) resistive self-heating of a specimen by a high-current pulse from a capacitor discharge system and measuring the current through the specimen, voltage across the specimen, and radiance temperature of the specimen as functions of time. Melting of a specimen is manifested by a plateau in the radiance temperature versus time function. The time integral of the power absorbed by the specimen during melting yields the heat of fusion. Measurements gave a value of 34.8 kJ · mot^– for the heat of fusion of tantalum, with a total uncertainty of ±6%. Electrical resistivity of solid and liquid tantalum at its melting temperature was also measured.     

Measurement of the heat of fusion of tungsten by a microsecond-resolution transient technique

A microsecond-resolution pulse-heating technique was used for the measurement of the heat of fusion of tungsten. The method is based on rapid (100 to 125s) resistive self-heating of a specimen by a high-current pulse from a capacitor discharge system and measuring current through the specimen and voltage across the specimen as functions of time. Melting of a specimen is manifested by changes in the slope of the electrical resistance versus time function. The time integral of the power absorbed by a specimen during melting yields the heat of fusion. Measurements gave a value of 48.7 kJ · mol^–1 for the heat of fusion of tungsten with an estimated maximum uncertainty of ±6%. The electrical resistivity of solid and liquid tungsten at its melting temperature was also measured.Paper presented at the Third Workshop on Subsecond Thermophysics, September 17–18, 1992, Graz, Austria.     

A microsecond-resolution transient technique for measuring the heat of fusion of metals: Niobium

A microsecond-resolution pulse-heating technique is described for the measurement of the heat of fusion of refractory metals. The method is based on rapid resistive self-heating of the specimen by a high-current pulse from a capacitor discharge system and measurement of the current through the specimen, the voltage across the specimen, and the radiance temperature of the specimen as a function of time. Melting of the specimen is manifested by a plateau in the temperature versus time function. The time integral of the power absorbed by the specimen during melting yields the heat of fusion. Measurements gave a value of 31.1 kj · mol^–1 for the heat of fusion of niobium, with an estimated maximum uncertainty of ±5%. Electrical resistivity of solid and liquid niobium at its melting temperature was also measured.     

Measurement of the heat of fusion of titanium and a titanium alloy (90Ti-6Al-4V) by a microsecond-resolution transient technique

A microsecond-resolution pulse heating technique was used for the measurement of the heat of fusion of titanium and a titanium alloy (90Ti-6Al-4V). The method is based on rapid (50- to 100-s) resistive self-heating of the specimen by a high-current pulse from a capacitor discharge system and measuring, as functions of time, current through the specimen, voltage across the specimen, and radiance of the specimen. Melting of the specimen is manifested by a plateau in the measured radiance. The time integral of the net power absorbed by the specimen during melting yields the heat of fusion. The values obtained for heat of fusion were 272 J · g^–1 (13.0 kJ · mol^–1) for titanium and 286 J · g^–1 for the alloy 90Ti-6Al-4V, with an estimated maximum uncertainty of ±6% in each value.Paper presented at the Second Workshop on Subsecond Thermophysics, September 20–21, 1990, Torino, Italy.     

A transient (subsecond) technique for measuring heat of fusion of metals

A transient technique is described for measuring the heats of fusion of metals with melting temperatures above 1500 K. The specimen configuration consists of a strip of the metal under study sandwiched between two strips of another metal with a higher melting temperature. The basic method consists of rapidly heating the composite specimen by passing a subsecond-duration electrical current pulse through it and simultaneously measuring the radiance temperature of the containment metal surface, as well as the current through and voltage drop across the specimen. The melting of the metal under study is manifested by a plateau in the temperature versus time function for the containing metal surface. The time integral of the power absorbed by the specimen during melting yields the heat of fusion. Measurements on several tantalum-niobium-tantalum specimens yield a value of 31.5 kJ · mor^–1 for the heat of fusion of niobium, with an estimated maximum inaccuracy of ± 5%.     

Thermophysical Property Measurements on Niobium and Titanium by a Microsecond-Resolution Pulse-Heating Technique Using High-Speed Laser Polarimetry and Radiation Thermometry

A microsecond-resolution technique was used to measure the heat of fusion, specific heat capacity, and electrical resistivity of niobium and titanium in the temperature range of 1600 to 3200 and 1500 to 2200 K, respectively. The method is based on rapid resistive self-heating of a wire-shaped specimen by a current pulse from a capacitor–discharge system. Melting of the specimen occurs in approximately 50 s. Measured quantities are the current through the specimen, the voltage across the specimen, the radiance from the specimen, and its normal spectral emittance, as functions of time. The true temperature of the specimen is computed from the values of the normal spectral emittance and radiance temperature of the specimen at each instant. The latter quantities are measured by means of high-speed laser polarimetry and radiation thermometry, respectively.     

Scanning the Melting Curve of Tungsten by a Submicrosecond Wire-Explosion Experiment

Measurements of temperature and density during a wire-explosion experiment at atmospheric pressure are described. The measurements encompass a parameter range from the solid to near the critical point. The influence of a polytetrafluoroethylene coating of the wire, necessary to prevent surface discharges, on the temperature and density measurements is investigated. The melting curve of tungsten up to 4000 K is detemined.     

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.     

Measurement of the radiance temperature (at 655 nm) of melting graphite near its triple point by a pulse-heating technique

Measurements of the radiance temperature of graphite at 655 nm have been performed in the vicinity of its triple point by means of a rapid pulse-heating technique. The method is based on resistively heating the specimen in a pressurized gas environment from room temperature to its melting point in less than 20 ms by passing an electrical current pulse through it and simultaneously measuring the radiance temperature of the specimen surface every 120 s by means of a high-speed pyrometer. Results of experiments performed on two different grades of POCO graphite (AXM-5Q1 and DFP-1) at gas pressures of 14 and 20 MPa are in good agreement and yield a value of 4330±50 K for the radiance (or brightness) temperature (at 655 nm) of melting graphite near its triple point (triple-point pressure, 10 MPa). An estimate of the true (blackbody) temperature at the triple point is made on the basis of this result and literature data on the normal spectral emittance of graphite.Paper presented at the First Workshop on Subsecond Thermophysics, June 20–21, 1988, Gaithersburg, Maryland, U.S.A.Formerly National Bureau of Standards     

A dynamic technique for thermophysical measurements at high temperatures in a microgravity environment

Millisecond-resolution dynamic techniques for thermophysical measurements, when utilized in the laboratory, are limited to the study of materials in their solid phase because the specimen becomes geometrically unstable during melting and collapses, due (at least in part) to the influence of gravity. Therefore, a millisecond-resolution dynamic technique is being developed for use in a microgravity environment in order to extend accurate measurements of selected thermophysical properties of electrically conducting refractory materials to temperatures above their melting point. The basic method involves heating the specimen resistively from ambient temperature to temperatures above its melting point in about 1 s by passing an electrical current pulse through it, while simultaneously recording the pertinent experimental quantities. A compact pulse-heating system, suitable for microgravity simulations with NASA's KC-135 aircraft, has been constructed and initial experiments have been performed to study the geometrical stability of rapidly melting specimens. Preliminary results show that rod-shaped specimens can be successfully pulseheated into their liquid phase.Paper presented at the First Workshop on Subsecond Thermophysics, June 20–21, 1988, Gaithersburg, Maryland, U.S.A.Formerly National Bureau of Standards     

The effect of impurities on the melting temperature and the heat of fusion of latent heat storage materials

Thermophysical properties of four normal paraffins (tetradecane, hexadecane, octadecane, eicosane) and three fatty acids (lauric acid, palmitic acid, stearic acid) were determined experimentally using a modified differential-thermoanalysis technique. For calibration of the measuring device, literature data in the temperature range from 5 to 70°C of six of these substances of at least 99% purity were used. Melting temperature, heat of fusion, and specific heat of a number of these pure and technically pure organic compounds were measured and compared to determine the effect of impurities and to give values of the application range of the properties required for the construction of thermal storage equipment.     

Measurement of the heat capacity of molybdenum (Standard Reference Material) in the range 1500–2800 K

Measurement of the heat capacity of molybdenum (Standard Reference Material 781 of the National Bureau of Standards) in the temperature range 1500–2800 K by a subsecond-duration, pulse-heating technique is described. The results of the measurements on three specimens are in agreement within 0.6%. The heat capacity of molybdenum in the temperature range 1500–2800 K based on the present results is expressed by the following function (standard deviation =0.5%): C _p =–3.0429+4.7215×10^–2 T–2.3139×10^–5 T ²+4.7090× 10^–9 T ³ where T is in K and C _p is in J · mol^–1 · K^–1. The inaccuracy of the reported results is estimated to be not more than 3%.     

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.     

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.     

Heat capacity and electrical resistivity of liquid niobium near its melting temperature

A microsecond-resolution capacitor discharge technique is used to heat niobium specimens rapidly to temperatures several hundred degrees above the melting point. From the measurements of current, voltage, and temperature as a function of time, the heat capacity and electrical resistivity of liquid niobium in the range 2850 to 3200 K were determined. Maximum uncertainties in the results are estimated to be ±5% for heat capacity and ±3% for electrical resistivity.     

Critical evaluation of the thermodynamic properties of molybdenum

The thermodynamic properties and the pressure-temperature phase diagram of pure Mo have been evaluated from experimental information using thermodynamic models for the Gibbs energy of the individual phases. A set of parameters describing the Gibbs energy of the various phases as a function of temperature and pressure is presented. The agreement between experimental data and calculated values is satisfactory.     

Variationally consistent computational homogenization of transient heat flow

A framework for variationally consistent homogenization, combined with a generalized macro‐homogeneity condition, is exploited for the analysis of non‐linear transient heat conduction. Within this framework the classical approach of (model‐based) first‐order homogenization for stationary problems is extended to transient problems. Homogenization is then carried out in the spatial domain on representative volume elements (RVE), which are (in practice) introduced in quadrature points in standard fashion. Along with the classical averages, a higher order conservation quantity is obtained. An iterative FE²‐algorithm is devised for the case of non‐linear diffusion and storage coefficients, and it is applied to transient heat conduction in a strongly heterogeneous particle composite. Parametric studies are carried out, in particular with respect to the influence of the ‘internal length’ associated with the second‐order conservation quantity. Copyright © 2009 John Wiley & Sons, Ltd.     

Heat Sealing measurement by an innovative technique

To obtain a proper heat seal is an important requirement in packaging, since seal failure is a more frequent cause of product deterioration than the package itself. Different kinds of seal, such as peelable or non‐peelable, can be obtained by changing the conditions under which a material is sealed. Therefore, identifying these conditions is very important. A new technique, the m ethod for m easuring t emperature of m elting s urface (MTMS), was used to predict the strongest peelable seal on various packaging commercial films. The temperature of the seal interface was measured using a thermocouple. The time–temperature profile, which was obtained by means of a thermocouple, was electronically processed so as to obtain the derivatives of the profile. The inflection point, also called the fusion point, was located on these profiles. This inflection point is associated with the physical change of the state of the material being sealed. The inflection point analysis was done using two different methods: (a) the MTMS method, based on the second derivative of temperature data with time; (b) ‘Table Curve’ software, based on non‐linear regression. This technique was successfully used to evaluate widely used packaging films such as LDPE, HDPE, LLDPE and CPP. The inflection point for these films was identified and the seal strength was verified using a universal testing machine. This method appears to be applicable to design the strongest peelable heat seals for many packaging materials. It also seems to have promise as a method of process measurement and validation for heat seal processes. Copyright © 2006 John Wiley & Sons, Ltd.     

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.     

Measurement of the transient heat transfer to liquid helium from a thin metal film

A method to measure transient heat transfer to liquid helium from a thin metal film heater under the condition of pulsed heating during τ ≤ 400 ns is proposed. The experimental equipment used for the measurements is described. The method is based on the comparison of heat pulses transfered from the heater into a monocrystal substrate which is surrounded either by vacuum or by liquid helium. The method can also be used to investigate the heat flux density transmitted into liquid helium over a wide region of thermal loads. Experimental results showing the heat flux density radiated from a Cu heater into liquid helium at 3.8 K as a function of the electric power fed into the heater by pulses of 200–400 ns duration are demonstrated.