The Experimental Determination of the Melting Heat for E635 Zirconium Alloy

A procedure is developed for the determination of the melting heat of zirconium alloys which is based on the preparation of an ampoule in the form of a thin oxide film on the surface of a specimen during its rapid heating in air. Owing to its higher melting point, the zirconium oxide film holds the specimen at temperatures exceeding the melting point. The brightness (for the wavelength of 0.65 m) solidus and liquidus temperatures of E635 zirconium alloy are measured, and the respective true temperatures are calculated using the measured values of spectral emissivity. The data obtained on the melting heat and the heat of – transition are presented.     

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.     

Calculation of CO2 laser beam absorptance as a function of temperature for steels by the numerical method

Temperature distributions were measured during the irradiation of a CO₂ laser beam at one end of a rod-shaped specimen and at the centre of a thin plate-shaped specimen. Regarding the measured temperature distributions as one-dimensional and two-dimensional unsteady state heat transfer solutions, CO₂ laser beam absorptances were calculated using a modified finite difference method. Temperature dependence of thermal properties, heat loss due to convection and latent heat during melting of the specimen were taken into account in this numerical calculation. Increasing the specimen temperature from room temperature to melting point, absorptances of STS304 stainless steel and SM45C steel were calculated as 8 40% and 6 41% for the one-dimensional calculation, and as 9.3 41% and 5 41% for the two-dimensional calculation, respectively. These calculated absortances were very close to theoretical values at relatively low temperature, which were calculated from the electrical resistivities of the specimens. Increasing the temperature of the specimens, absorptances increased considerably due to oxidation of the specimens. Regardless of specimen composition and specimen dimension, both absorptances showed nearly the same value of 41% at their melting points, in which the structures of both metals became amorphous phases.     

Sol-gel prepared Ni-alumina composite materials

The microstructure of sol-gel prepared Ni-alumina ceramic-metal composites containing up to 50% Ni has been studied with X-ray diffraction, the scanning electron microscope and the transmission electron microscope. The influence of processing temperature upon the size distribution of Ni was established. It was found that increasing the total amount of Ni increases only the number of micrometre-size Ni inclusions in the alumina, whereas the hot-pressing temperature determines the size distribution of Ni. When temperatures much higher than the melting temperature of Ni are used, a large number of Ni inclusions of the order of 10 nm can be found mainly within alumina grains; only a few are formed in grain boundaries and in triple points. When a temperature close to the melting point is used, there are fewer nanometre-size Ni inclusions and a larger number of Ni inclusions of the order of 100 nm to 1 m. In this case, the large ( 100 nm) and small ( 10 nm) Ni inclusions are found in grain boundaries and triple points.     

Thermophysical Properties of Solid and Liquid 90Ti–6Al–4V in the Temperature Range from 1400 to 2300 K Measured by Millisecond and Microsecond Pulse-Heating Techniques

The heat capacity and electrical resistivity of 90Ti–6Al–4V were measured in the temperature range from 1400 to 2300 K by two pulse-heating systems, operating in the millisecond and microsecond time regimes. The millisecond-resolution technique is based on resistive self-heating of a tube-shaped specimen from room temperature to melting in less than 500 ms. In this technique, the current through the specimen, the voltage drop along a defined portion of the specimen, and the temperature of the specimen are measured every 0.5 ms. The microsecond-resolution technique is based on the same principle as the millisecond-resolution technique except for using a rod-shaped specimen, a faster heating rate (by a factor of 10,000), and faster data recording (every 0.5 s). Due to the rapid heating with the microsecond system, the specimen keeps its shape even in the liquid phase while measurements are made up to approximately 300 K above the melting temperature. A comparison between the results obtained from the two systems with very different heating rates shows significant differences in phase transition and melting behavior. The very high heating rate of the microsecond system shifts the solid–solid phase transition from the (+) to the phase to a higher temperature, and changes the behavior of melting from melting over a temperature range to melting at a constant temperature like an eutectic alloy or a pure metal.     

Photoplastic effects in Cd0.2Hg0.8Te

We irradiated Cd_0.2Hg_0.8Te samples at room temperature in the plastic range, with a CO₂ laser beam the wavelength of which (=10 500 nm) is 20% longer than the absorption threshold. We observed a positive photoplastic effect (PPE) of the order _PPE/4 to 5%.     

Tearing of thin polyimide films

Films of BTDA-ODA polyimide up to 58m thick were torn at constant cross-head speed in trousers tests. In common with previous results on polyolefins, the work of tearing was found to increase markedly with specimen thickness. A model for the increase, based on the volume of plastically deformed material adjacent to the crack plane, was found to be only qualitatively valid. The experimental slope of a plot of tearing energy (per unit area) against thickness was 70 MJ m^–3. Optical and scanning electron micrographs of torn films are discussed in regard to the modes of failure.     

A generalized equation for surface tension from the triple point to the critical point

A three-parameter generalized equation is proposed for surface tension from the triple point to the critical point. This equation not only fits the data well but also is good for interpolation between the normal boiling point and the critical point. This equation is also good for extrapolation to the triple point. This equation has been tested using the surface tension of water from the triple point to the critical point. The constants of this equation obtained using orthobaric surface tensions are given for a number of compounds. The isobaric surface tensions determined at a pressure of 1 atm do not differ significantly from the orthobaric surface tensions. Such data also have been used in obtaining equations from the triple to the critical point.Nomenclature T _c Critical temperature, K - T _t Triple point, K - T _m Melting point, K - T _r Reduced temperature, K - X (T _c-T)/T _c - Surface tension, dyne · cm^–1;10^–3N · m^–1 - _m Surface tension at the melting point - _f Surface tension at T _r=0.9 - _t Surface tension at the triple point - Relative deviation 100[ _obsd– _calcd]/ _obsd - Standard deviation [( _obsd– _calcd)²/(No. points—No. parameters)]^0.5     

The Character of Melting for Simple Molecules Deposited on Graphite

The microscopic character of melting for quasi–two dimensional N ₂ adlayers on graphite is examined for surface densities 0.2 1, where the upper limit corresponds to a complete monolayer. A Monte Carlo method, with the multiple histogram procedure, is employed to determine various thermodynamic quantities. Using the calculated specific heats and selected order parameters, determined at various surface densities, the mechanism for melting is shown to be vacancy mediated. The somewhat unusual behavior of the melting temperature versus density is shown to be entirely due to the vacancy concentration and their topology. Because this is determined by the free energy, our analysis should be general. Preliminary results for Xe on graphite supports this claim.     

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%.     

High ductility in poly(methyl methacrylate) induced by absorption and desorption of an acetonitrile aqueous solution

Tension tests were conducted in air at room temperature on PMMA sheet specimens which had been previously soaked in a 40 vol % acetonitrile aqueous solution at 20 °C for 24 h and then dried in air at room temperature for 480 h. In contrast with an untreated specimen which fractured at a stress of 84 MPa and a strain of 9 %, shear yielding clearly took place at 42 MPa and the elongational fracture strain increased to about 148 %. No crazes were observed on the specimen surface and as a result the transparency of the PMMA was thoroughly maintained until fracture. Thus this soaking treatment may change PMMA to a completely ductile polymer without a crazing mechanism. The results of the dynamic viscoelastic measurements at 1 Hz show that the glass transition temperature was lowered to about 80 °C (as compared to about 110 °C), and the relaxation became much sharper with a higher peak value of 20 °C (as compared to a broad curve with a peak at 50 °C). This clear relaxation at room temperature may contribute to shear yielding and large plastic elongation of the treated PMMA.     

High-temperature creep response of a commercial grade siliconized silicon carbide

Creep studies conducted in four-point flexure of a commercial siliconized silicon carbide (Si-SiC, designated as Norton NT230) have been carried out at temperatures of 1300, 1370, and 1410°C in air under selected stress levels. The Si-SiC material investigated contained 90% -SiC, 8% discontinuous free Si, and 2% porosity. In general, the Si-SiC material exhibited very low creep rates (2 to 10×10^–10 s^–1) at temperatures 1370°C under applied stress levels of up to 300 MPa. At 1410°C, the melting point of Si, the Si-SiC material still showed relative low creep rates (0.8 to 3 × 10^–9 s^–1) at stresses below a threshold value of 190 MPa. At stresses >190 MPa the Si-SiC material exhibited high creep rates plus a high stress exponent (n=17) as a result of slow crack growth assisted process that initiated within Si-rich regions. The Si-SiC material, tested at temperature 1370°C and below the threshold of 190 MPa at 1410°C, exhibited a stress exponent of one, suggestive of diffusional creep processes. Scanning electron microscopy observations showed very limited creep cavitation at free Si pockets, suggesting the discontinuous Si phase played no or little role in controlling the creep response of the Si-SiC material when it was tested in the creep-controlled regime.     

Vapor pressure measurements of para-hydrogen adsorbed on exfoliated graphite

Monolayer isotherms were measured for 15, 18, and 20 K for para-hydrogen adsorbed on exfoliated graphite foam, and for the second, third, and fourth layers in the temperature interval of 8 to 20 K, using the standard volumetric method. From the data, the isosteric heat of adsorption, molar entropies and internal energies were obtained as a function of coverage. The values for coverages above the third layer were compared to those at the p-H₂ bulk triple point, showing that, within our experimental uncertainty, the results are closer to the values of bulk solid para-hydrogen. Critical temperatures for the second and third layers and the triple point temperature for the second layer, were determined, yielding values of T_c2 = (10.0±0.1) K, T_c3 = (11.0±0.5) K and T_t2 = (6.5±0.1) K respectively. Features occurring along the monolayer coverages are compared to transitions which occur in the para-hydrogen phase diagrams adsorbed on graphite, obtained from heat capacity measurements by other authors. From the isotherms, compressibilities were calculated as a function of coverage for several temperatures. Whenever possible the obtained results were compared to existing data in the literature.     

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.     

Microsecond Laser Polarimetry for Emissivity Measurements on Liquid Metals at High Temperatures—Application to Niobium

Prior to now, all existing pulse heating systems capable of investigations on liquid samples could measure the radiance temperature only during the experiment. To determine the true temperature, it was necessary to assume that the emissivity is constant over the entire temperature range, with a value equal to that at the melting point. This assumption can cause large uncertainties in temperature measurements, especially at elevated temperatures. To avoid these uncertainties, a microsecond-division of amplitude photopolarimeter (s-DOAP) was added to our experiment. The s-DOAP detects changes in the polarization state of a laser beam (=684.5nm) reflected by the sample surface during the pulse-heating experiments. This change in the polarization state is used to determine the index of refraction n and the extinction coefficient, k. This leads to the reflectivity R of the sample, and by means of Kirchhoff's law for opaque materials, the normal spectral emissivity is obtained. The application of simultaneous laser polarimetry and spectral radiometry leads to the true temperature and is demonstrated on liquid niobium.     

Two-dimensional pressure-temperature phase diagram and latent heats of neon adsorbed on exfoliated graphite

A two-dimensional pressure-temperature phase diagram was constructed for neon adsorbed on exfoliated graphite using the heat capacity data obtained in our laboratory for this system. The two-dimensional pressures at the triple and critical points were found to be _t=64×10^–6 N/m and _c=128×10^–6 N/m, respectively. From Clapeyron's equation and assuming an ideal behavior for the two-dimensional gas phase, the latent heat of sublimation was calculated as a function of temperature. The latent heat of vaporization was also calculated at the triple point and consequently the latent heat of fusion was found. The following values were obtained at the triple point:l _s/k=86 K,l _v/k=24 K, andl _f/k=62 K.     

Isochoric pvT measurements of SF6 in the density range 100 to 1200 kg · m−3

The pvT properties of SF₆ were determined by an isochoric method. The pressure p and the temperature T were measured in the pressure range 1.5 MPa p 9.0 MPa and in the temperature range 293 K T 340 K. The results are compared with data in the literature. The adsorption of SF₆ on glass and iron surfaces and its influence on the pvT measurements are also briefly discussed.Paper presented at the Tenth Symposium on Thermophysical Properties, June 20–23, 1988, Gaithersburg, Maryland, U.S.A.     

The significance of many-body interactions in physical adsorption

The significance of many-body interactions in the physical adsorption of rare gas atoms on solid surfaces has been investigated. A simple model of the system was considered in which the atoms of the solid and the adsorbed atom were represented by interacting isotropic point dipoles. The fullN-body interaction energy between the adsorbed atom and the solid was calculated exactly to lowest order in the expansion parameter [₀(₀/)²]/4d ³ (, and ₀, ₀ are the solid atom's and adsorbed atom's characteristic frequency and polarizability,d is the distance from the surface of the adsorbed atom, and is the number of atoms per unit volume in the solid). The interaction was then evaluated for the adsorption of various rare gas atoms on rare gas solids. It was found that the fullN-body interaction deviated at most by only2 1/2% from the interaction obtained by considering only two-body interactions. In addition, it was found that a finite expansion in two-, three-, ... body expressions may lead to erroneous results for the interaction energy since extensive cancellations occur between successive terms of the series.     

Picosecond laser heating and melting of graphite

Ultrashort laser pulses impinging onto solid, strongly absorbing surface deposit their energy within an absorption depth from the surface. This localized energy deposition may result in rapid and very efficient heating of the surface to temperatures far exceeding the melting or boiling point. Temperature evolution at the surface of samples and their electronic structure may be studied with nonperturbing, time-resolved optical diagnostic techniques. Picosecond laser pulses provide the fastest means for heating matter at high temperature, since the characteristic energy transfer times from photoexcited electrons to the lattice occur in this time scale. Surface evaporation is not affecting the observations in this time scale, simply because there is no time for the surface atoms to escape. As an illustration, measurements on graphite are presented here. The complex index of refraction of highly oriented pyrolytic graphite (HOPG) during picosecond laser irradiation has been measured at 1.06 m via time-resolved ellipsometry at angles of incidence up to 80. In particular, a value of the complex index of refraction for the liquid phase has been derived.Paper presented at the First Workshop on Subsecond Thermophysics, June 20–21, 1988, Gaithersburg, Maryland, U.S.A.     

Susceptibility and Pressure Study of 3He nano-Clusters

Simultaneous measurements of pressure and magnetic susceptibility have been made in ³ He nano-clusters embedded in a ⁴ He matrix, following phase separation of the mixture. Susceptibility measurements extend from 0.5 mK to 10 mK for three different samples, which either undergo partial melting upon further cooling, or separate with liquid already present. The magnetic behavior of the clusters indicates solid fractions of 77, 54, and 19%, respectively, for pressures of 3.36 MPa, 3.06 MPa, and 2.88 MPa. The susceptibility of the 3.36 MPa sample follows a Curie law to the lowest temperature. For 3.06 MPa, we observe a kink in at 1.1 mK, which is approximately the ordering temperature T_N of the pure bulk ³ He if it existed at this pressure. However is almost constant down to 0.6 mK, with no drop at 1.1 mK, and no frequency shift, within our resolution of 10 Hz. Thus if there is magnetic ordering at 1.1 mK it is quite different than for bulk ³ He, not the U2D2 phase. For 2.88 MPa, follows a Curie-Weiss law with a positive Weiss =140 K, indicative of a ferromagnetic tendency, similar to that seen in 2D films.