Condensation of Zinc Vapor on Solid Media in Zn(g)-CO-CO2-Ar Mixtures

N.X. FU, T. TAMAGAWA, M. KOBAYASHI, and M. TANAKA The condensation experiments of zinc vapor on the solid media in Zn(g)-CO-CO2-Ar mixtures were conducted in a flow reactor at 800 C to 1000 C under a zinc partial pressure of 0.6 to 7.9 kPa. The condensates were weighed, and the zinc contents and their morphology were analyzed to investigate the effects of various factors on the condensation. It was found that the initial temperature of the media should be as low as possible in liquid condensation for the efficient recovery of zinc. The condensation is enhanced with zinc partial pressure of the gases. The medium made of silica with a smooth surface is favorable for the efficient condensation. In the gases not oxidizing to zinc vapor, metallic zinc can be obtained on the medium with an initial temperature over the range of 120 C to 400 C. For obtaining metallic zinc, it is necessary to raise the temperature of the gases, appropriately limit the zinc partial pressure, or maintain a sufficient CO/CO2 ratio to avoid the oxidation of zinc vapor.

I. INTRODUCTION

CURRENTLY, the quantity of crude steel produced by the electric arc furnace (EAF) approaches 30 million tons each year in Japan, which amounts to about 30 pct of the total output of crude steel. At the same time, over 0.5 million tons of dust from the EAF exhaust gases are generated annually.[1,2] The dust containing about 33 pct iron, 20 pct zinc, and small amounts of other valuable metals is considered a significant resource. About 60 pct of the dust is treated via the processes of the Waelz kiln at 1100 C and the Mitsui furnace and electric distillation both at 1300 C, in which zinc oxide is reduced by coke followed by the evaporation of zinc and the reoxidation of zinc vapor to produce crude zinc oxide or zinc white with low commercial value.[3] These processes are complex and require a large quantity of energy. Additionally, about 30 pct of the dust is disposed of by landfilling after stabilization, and 10 pct is used as raw materials for cement. To save energy and minimize environmental load, a new process to recover iron and metallic zinc with a yield of more than 80 pct directly from the EAF exhaust gases is being developed by the Japan Research and Development Center for Metals (JRCM).[4,5] In this process, the hot exhaust gases from a sealed EAF are first treated by a moving coke bed filter to deposit iron, and second by a condenser to recover metallic zinc on falling ceramic balls with an average diameter of 0.5 mm. Efficient condensation of zinc vapor as metallic zinc is critical to the success of developing the process. The potential for zinc vapor to be oxidized by CO2 on cooling obstructs the acquisition of the metallic zinc. These are influenced by various factors including (1) temperature, flow rate, and
N.X. FU, Visiting Researcher, Metals Recovery Group, T. TAMAGAWA, Technical Staff Member, M. KOBAYASHI, Principal Research Scientist, and M. TANAKA, Group Leader, Metals Recovery Group, are with the Research Institute for Green Technology, National Institute of Advanced Industrial Science and Technology (AIST), Ibaraki 305-8569, Japan. Contact e-mail: mky-tanaka@aist.go.jp Manuscript submitted April 29, 2003.
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composition of the gases, and (2) initial temperature, material, and surface roughness of the condensation media. To furnish the basis for the condenser design and the determination of the optimum operational conditions, it is necessary to investigate the effects of these factors on the condensation process. For this purpose, the condensation experiments were conducted in the present work by inserting the media into Zn(g)-CO-CO2-Ar mixtures in a flow reactor to condense zinc vapor within a short time. The amounts of the condensates were measured, and the zinc contents and their morphology were analyzed.

II. THEORETICAL CONSIDERATIONS OF CONDENSATION A. Condensation Efficiency The equilibrium vapor pressure, p0Zn, of zinc, as a function of temperature,[6] is plotted in Figure 1. To condense a superheated vapor at a temperature of T0 and partial pressure of pi, it has to be cooled to a temperature below its dew point, Td, at which saturation occurs. The condensates will appear in the liquid and solid form at a temperature above and below 419 C, respectively, which is the melting point of zinc. The condensation efficiency of a condenser in recovering liquid zinc from the mixtures of zinc vapor with noncondensing gases depends on the zinc partial pressure and the condenser temperature, which can be understood by the theoretical percentage recovery, R, expressed as follows:[7] R 1 pf (P pi (P pi) pf) P(pi pi (P pf) pf) 100 pct [1]

where P is the total pressure, and pi and pf are zinc partial pressures in the incoming gases and the exhaust gases of the condenser, respectively. This indicates that the condensation efficiency can be favored by reducing the dilution of the zinc vapor or the condenser temperature to decrease the zinc partial pressure at the exit.
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B. Oxidation of Zinc Vapor When the mixtures of zinc vapor, CO, and CO2 are cooled, zinc vapor might be oxidized by the reaction Zn(g) CO2 ZnO CO [2]

III. EXPERIMENTAL METHOD A. Apparatus The apparatus for the condensation experiments consisted of a silica reactor tube with a 1330-mm length and a 45-mm inner diameter horizontally placed in a furnace, as shown in Figure 2. The furnace was installed with heat elements in three zones, which were separately controlled with a temperature regulator and a thermocouple to give the required temperatures for the generation of zinc vapor, and the heating and cooling of the gas mixtures. An inner silica tube with a 450-mm length and 35-mm diameter was mounted in the left section of the reactor for zinc vaporization, in which argon was introduced as the carrier gas, and a graphite boat charged with analytical-grade zinc ingots was initially placed in the low-temperature side. The mixtures of CO and CO2 were introduced into the reactor through the gap between the reactor and the inner tube to mix with the zinc vapor in the heating zone. Fiber blocks with some small holes were set in the outlet of the inner tube and the passage of CO-CO2 to avoid the backward diffusion of the gas mixtures causing oxidation of the zinc vapor. Another inner silica tube was mounted in the right section of the reactor, in which a silica tube with an outer diameter of 20 mm and a length of 600 mm as a condensation medium was located in the low-temperature side in advance, and counterflow nitrogen was introduced to avoid undesired condensation. In that place, the surface temperature at the front end of the medium was determined as the initial temperature of the medium (ITM), which was changed by its location. To compare the condensation on the media made of different materials, small disks of silica, alumina, and graphite with 10-mm diameter and 1-mm thickness were employed, which were attached to the condensation tube by a graphite holder. To compare the condensation on the media with different surface roughness, an ordinary silica tube and a satin-finish one were also used with the same outer diameter of 20 mm, wall thickness of 1.7 mm, and a length of 600 mm. Additionally, a short silica cap with a 21-mm inner diameter and 30-mm length was also used as a medium sheathing the front end of the condensation tube to favor the more accurate measurement of the weight of the condensates for determining their zinc contents. The surface temperatures of the media in the reactor were measured by an infrared thermometer in independent experiments in nitrogen to approximately simulate those in the condensation experiments.

The occurrence of the oxidation depends on the CO2 content, zinc partial pressure, and temperature of the gases, which can be understood in terms of the diagram of the equilibrium CO/CO2 ratio with the temperature shown in Figure 1.[7,8] Curve A1 (A2) gives the CO/CO2 ratio for Reaction [2] at the zinc partial pressure of 1.0 kPa (10 kPa). At a given temperature, the mixtures at a CO/CO2 ratio below curve A1 (A2) are stable and will not form ZnO, but will tend to deposit ZnO above the curve. Evidently, the CO/CO2 ratio has to be correspondingly raised to avoid oxidation when the zinc partial pressure increases or the temperature decreases. Curve B represents the CO/CO2 ratio for the formation of ZnO from the mixtures in equilibrium with liquid zinc in the condensing temperature range. The CO/CO2 ratio has to be kept above 5 103 to avoid ZnO formation on condensation at 550 C. However, the CO/CO2 ratio of the actual mixtures fed to the condenser is not so high. In this case, if the zinc vapor is condensed nearly at equilibrium conditions, one would find more zinc oxide than metallic zinc. Therefore, it is necessary to quench the mixtures with media at lower temperatures, thus condensing the zinc vapor without allowing time for the formation of zinc oxide. Curve C gives the CO/CO2 ratio of the Boudouard reaction at a CO partial pressure of 50 kPa: CO2 C 2CO [3]

The mixtures with a CO/CO2 ratio above the curve tend to react with solid carbon to reduce their CO2 content, but are stable in the absence of carbon. On the other hand, those with a CO/CO2 ratio below the curve tend to deposit carbon and thus to increase CO2. However, the carbon-deposition reaction is quite slow, so it does not constitute a practical problem.

Fig. 1Equilibrium vapor pressures of zinc and CO/CO2 ratios as a function of temperature in Zn(g)-CO-CO2 gases at one atmosphere.
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Fig. 2Apparatus for condensation experiments.

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Table I. Conditions for the Condensation Experiments Series of Experiments A B C D E F G H VZn*, mL/min 34 72 to 195 34 to 110 34 34 8 8, 13, 22 22 FCO mL/min pZn, kPa 2.6 7.9 2.6, 5.3, 7.9 2.6 2.6 0.6 0.6, 1.0, 1.7 1.7 CO/CO2 Ratio 7 9 9 9 9 3.5 3.5 3.5 to 9 T, C 900 to 1000 1000 1000 1000 1000 800 to 900 800 800 ITM, C 150 to 450 225 330 180 to 500 150 to 545 120 to 400 300 300 Medium cap tube tube disks tubes cap cap cap

CO2

800 353 to 1815 800 800 800 800 800 800

*With a flow rate of argon: 500 mL/min; VZn: vaporization rate of zinc; FCO CO2: flow rate of CO CO2; pZn: calculated zinc partial pressure; T: gas temperature; ITM: initial temperature of medium; cap: short silica cap; tube: silica tube; and disks: small disks of silica, alumina, and graphite.

B. Procedure and Conditions Argon, CO-CO2, and nitrogen were introduced into the system at appropriate flow rates during the heating of the reactor. After reaching the required temperatures in the reactor, the boat was pushed to the predetermined place to start the vaporization of zinc, where the temperature was measured by a thermocouple. Passing through the heating zone, Zn(g)-COCO2-Ar gases were further heated to 800 C to 1000 C. After interrupting the flow of nitrogen, the medium was quickly inserted into the gases at high temperature to condense zinc vapor within a given time and then immediately withdrawn to a low-temperature place for rapid cooling followed by the restoration of nitrogen. The boat was also withdrawn to the original position for cooling. After removing the medium from the reactor, the medium was weighed together with the condensates by an electronic balance with a sensitivity of 0.1 or 1 mg depending on the known weight of the medium, which was subtracted from their total weight to obtain that of the condensates. The morphology of the condensates was observed by a microscope, and the zinc contents were determined by an EDTA titration method. The vaporization rate of the zinc measured using the weight-loss method[9] was controlled by changing the temperature and the area of the boat. The experiments of supplying Zn(g)-CO-CO2-Ar gases for the condensation were carried out previously. The partial pressure of the zinc vapor in the supplied gases was calculated by the vaporization rate of the zinc and the flow rates of the CO-CO2-Ar gases. All the conditions for the condensation experiments are summarized in Table I. The calculated zinc partial pressure was used to indicate the actual one, since the zinc vapor was not oxidized in the gases in most cases. In experiment F at 800 C, G, and H, the oxidation of zinc vapor occurred to some extent due to lower temperature or smaller CO/CO2 ratio; thus, the actual zinc partial pressure would be lower than the calculated value. IV. RESULTS AND DISCUSSION A. Effects of Various Factors on the Quantity of the Condensates 1. Initial temperature of medium Experiment A involved the condensation within 5 seconds at 900 C to 1000 C at different ITMs. Figure 3 shows that the amounts of the condensates increase with the lowering
METALLURGICAL AND MATERIALS TRANSACTIONS B

Fig. 3Amounts of condensates as a function of ITM, PZn CO2 7, time: 5 s.

2.6 kPa, CO/

of the ITM from 450 C to 250 C to 300 C, while they gradually decrease thereafter down to about 150 C. It was confirmed that the temperature of the medium quickly increased with time after it reached the high-temperature zone and reached a larger value by employing a higher ITM. In the ITM between 250 C and 450 C, the zinc vapor condensed as a liquid; thus, the decrease in the temperature of the medium by reducing ITM was favorable for obtaining more condensates. In the ITM between 150 C and 250 C, the condensates appeared as a solid. Thus, the condensates decreased by lowering the ITM, probably because some fine solid particles of the condensates formed in a thermal boundary layer around the medium and were partly carried away with the gases. These results indicate that the ITM should be as low as possible under the liquid condensation to obtain more condensates in a given time. 2. Flow rate and zinc partial pressure In experiment B, the condensation was carried out within 10 to 30 seconds at 1000 C by varying the flow rate of the gases from 925 to 2510 mL/min at the same zinc partial pressure. The changes in the amounts of the condensates as a function of time are given in Figure 4, showing that the condensates obtained within the same time generally increase by raising the flow rate corresponding to the enhancement of the mass transfer of the zinc vapor. However, it was found that the percentage of the condensation, defined as the ratio of the amount of the condensate to that of the feed zinc for the same duration, gradually decreased with the flow rate.
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Fig. 4Amounts of condensates for different condensation times with varying flow rates of gases at 1000 C.

Fig. 5Amounts of condensates with the condensation time under different partial pressures of zinc at 1000 C.

This is probably due to the increase in the temperature of the medium with the flow rate, because more latent heat was released during the condensation, and the coefficient of convective heat transfer between the surface of the medium and the gases could become larger. These facts imply that the feed rate of the medium should be raised with the flow rate in the practical operation of the condenser to maintain high condensation efficiency. In experiment C, the condensation within 10 to 30 seconds was performed at 1000 C by varying the zinc partial pressure from 2.6 to 7.9 kPa at the same flow rate of the CO-CO2-Ar gases. The amounts of the condensates with time, presented in Figure 5, indicate that there were always more condensates at a higher zinc partial pressure than at a lower one for the same time. This is consistent with the fact that the supersaturation of zinc vapor increases with its partial pressure at a given temperature to give a larger driving force for the condensation.[10] 3. Materials and surface roughness of the media The condensation on the disks of silica, alumina, and graphite was compared in experiment D. The amounts of the condensates within 5 seconds with the ITM over the range 180 C to 500 C are shown in Figure 6. The data seem to scatter because the time taken for inserting the disks into the gases at high temperature was not identical for the different runs due to the limitation of the operating conditions. However, it can be seen that the condensates on the silica disks are generally about 0.2 to 1.5 mg more than those on the alumina ones, while those on the graphite ones are much less. It was observed that the condensates mostly formed as liquid droplets, and those on the silica disks were much plumper and denser than those on the alumina ones, as shown in Figure 7. When the ITM was about 180 C, additionally, it was found that the condensates appeared as solid particles in the lower left section of the silica disk and as liquid droplets in the rest, while those formed on the alumina disk were all fine liquid droplets (Figures 8(a) and (b)). These findings show that the temperatures of the silica disks would be somewhat lower than those of the alumina ones during the condensation. This was probably caused by a difference in the heat conduction between the silica disks and alumina ones due to their different physical parameters such as the thermal conductivity, specific heat, and density (Table II[11,12,13]). As a result, more condensates were obtained on the silica
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Fig. 6Amounts of condensates on different media by varying their initial temperatures.

Fig. 7Droplets of condensates on silica disk (upper half) and on alumina disk (lower half), initial temperature of medium: 340 C.

disks than on the alumina. Relative to the silica and alumina disks, the temperatures of the graphite disks would become much higher in the gases at high temperature due to smaller specific heat and density of graphite (Table II), which made the condensation very difficult.
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Fig. 9Amounts of condensates on silica media with different surface conditions as a function of ITM and condensation time.

B. Effects of Several Factors on the Quality of the Condensates 1. Gas temperature and ITM In experiment F, the condensation was conducted at 800 C to 900 C within 5 seconds at the zinc partial pressure of 0.6 kPa and the CO/CO2 ratio of 3.5. The ITM was varied from 120 C to 400 C to change the cooling rate of the gases. The zinc contents of the condensates are presented in Figure 10 and compared with those of the condensates obtained in experiment A shown in Figure 11. Those of almost all the condensates were approximately 100 pct in the two experiments at 900 C to 1000 C, at which the feed gases were not oxidizing to the zinc vapor. This shows that the medium with the ITM ranging up to at least 400 C caused a sufficient cooling rate of the gases to avoid the oxidation of the zinc vapor during the condensation on it; thus, metallic zinc was obtained. In experiment F at 800 C, the gases were oxidizing to zinc vapor by CO2[1519] due to the lower temperature and smaller CO/CO2 ratio. Although the zinc contents of some condensates approached 100 pct, those of others were obviously lower than this limit, indicating that they contained small amounts of zinc oxide. Since the possibility of the oxidation of zinc vapor on the medium is excluded due to its cooling role on the gases, zinc oxide in the condensates probably results from the partial deposition of that formed in the gases because of the oxidation of zinc vapor on the existing solid fine particles, which probably dropped from the fiber blocks in the outlet of the vaporization tube. 2. Partial pressure of zinc vapor In experiment G, the condensation was conducted at 800 C within 5 seconds by varying the zinc partial pressure from 0.6 to 1.7 kPa at a CO/CO2 ratio of 3.5. The zinc contents of the condensates are compared in Figure 12 at the ITM of 300 C. Those are more than 95 pct at 0.6 kPa, but less than 90 pct at 1.0 and 1.7 kPa, showing a tendency that the zinc contents of the condensates decrease with the partial pressure of zinc. The gases were oxidizing to the zinc vapor under these conditions, which is the reason for the existence
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Fig. 8(a) Solid particles with a few droplets of condensates on silica disk and (b) droplets of condensates on alumina disk. Initial temperature of medium: 180 C.

Table II. Physical Constants of the Different Materials (200 C to 600 C) Thermal Conductivity W/(m C) 1.32 to 1.98 4.67 to 6.92 93.44 to 154.01 Specific Heat kJ/(kg C) 0.86 to 1.13 1.05 to 1.17 0.79 Density g/cm3 3.94 3.88 1.56

Materials Silica Alumina Graphite

The comparisons between the condensation on the silica media with smooth and rough surfaces were made in experiment E. The changes in the amounts of the condensates with IMT and condensation time are shown in Figure 9. On the smooth medium, there were about 1 to 4 mg more condensates than on the rough one depending on the IMT and the condensation time, except for the results with a high IMT of 545 C or a short time of 1 second. In the case of liquid condensation, moreover, the droplets on the smooth medium mostly were even in size and dense in distribution, while those on the rough one were uneven and relatively dispersed. These may be attributed to the fact that the temperature of the rough medium would be higher than that of the smooth one during the condensation, since more radiation energy is probably absorbed by the former than by the latter due to less absorptivity of the smooth surface.[14]
METALLURGICAL AND MATERIALS TRANSACTIONS B

Fig. 10Zinc contents of condensates with varying initial temperatures of medium, PZn 0.6 kPa, CO/CO2 3.5.

Fig. 13Zinc contents of condensates as a function of CO/CO2 ratio in the gases at 800 C.

Fig. 11Zinc contents of condensates with varying initial temperatures of medium, PZn 2.6 kPa, CO/CO2 7.

3. CO/CO2 ratio The condensation was carried out at 800 C within 5 seconds with varying CO/CO2 ratio from 3.5 to 9 in experiment H. Figure 13 shows that the zinc contents of the condensates increased with the rise in the CO/CO2 ratio. They were lower than 90 pct at lower CO/CO2 ratios up to 5, but tended to be 100 pct thereafter. These results demonstrate that the condensates obtained at lower CO/CO2 ratios contained partial zinc oxide formed in the gases, and there was a trend to obtain metallic zinc by raising the CO/CO2 ratio up to 9. This is attributed to the fact that the oxidation potential of the zinc vapor increases with the lowering of CO/CO2 ratio or raising CO2 content in the gases.[7,9] Therefore, the CO/CO2 ratio has to be maintained above a limit under the given conditions; otherwise, the oxidation of zinc vapor would occur to reduce the zinc content of the condensates. This limit would be higher for the gases at lower temperature or higher zinc partial pressure, as shown in Figure 1. V. CONCLUSIONS The condensates increased by lowering the ITM on the liquid condensation, and decreased by further reducing that on the solid condensation due to partial losses of the solid particles with the outlet gases. The ITM should be as low as possible for efficient condensation in the liquid form. Although the condensates increased with the flow rate of the gases due to the enhancment of the mass transfer, the percentage of the condensation simultaneously decreased. This suggests that the feed rate of the medium should be raised with the flow rate to gain condensation efficiency in the practical operation on the condenser. The condensates increased with the zinc partial pressure because of the increased supersaturation of the zinc vapor at a given temperature. The materials of the media affect the amounts of the condensates due to their different heat conductivities, which are related to their thermal conductivity, specific heat, and density. Silica appears to be preferable to alumina as a medium for efficient condensation. In addition, it was confirmed that the medium with a smooth surface is more favorable to the condensation than one with a rough surface because of their different absorption properties of radiation energy. The medium with the ITM over a broad range from 120 C to at least 400 C could cause a sufficient cooling rate of the
METALLURGICAL AND MATERIALS TRANSACTIONS B

Fig. 12Zinc contents of condensates with varying partial pressures of zinc, CO/CO2 3.5, ITM 300 C.

of zinc oxide in the condensates, as previously mentioned. Thus, the decrease in the zinc content of the condensates with the partial pressure of zinc may be attributed to the fact that the oxidation extent of the zinc vapor increases with the partial pressure of zinc when the temperature and CO/CO2 ratio are given.[16,17]
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gases to prevent the oxidation of zinc vapor during the condensation on it. When the feed gases were oxidizing to zinc vapor, zinc oxide arose on some fine particles in the gas stream and deposited with the condensates on the medium. To obtain metallic zinc, it is essential to avoid the oxidation of zinc vapor in the gases. The zinc contents of the condensates increased by raising the temperature of the gases, lowering the partial pressure of zinc vapor, or increasing the CO/CO2 ratio to reduce the oxidation tendency of the zinc vapor. It is suggested that we have a combined control of these parameters according to the actual conditions for obtaining metallic zinc.

ACKNOWLEDGMENTS The authors are grateful to the New Energy and Industrial Technology Development Organization (NEDO) for the financial support for this work. We carried out the present work as participants on the project Technology for Energy-Saving Recovery of Metallic Dust organized by JRCM.

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3. M. Shima and S. Kawakita: J. Min. Mater. Processing Inst. Jpn., 1991, vol. 107, pp. 85-94. 4. S. Sato: J. Min. Mater. Processing Inst. Jpn., 1999, vol. 115, pp. 484-85. 5. M. Yasui and H. Sasamoto: Proc. 21st Int. ATS Steelmaking Conf., Paris, France, Dec., 2000, ATS (The French Steel Technical Association), pp. 214-15. 6. O. Kubaschewski: Metallurgical Thermochemistry, Pergamon Press, Ltd., London, 1956, p. 330. 7. C.H. Mathewson: Zinc: The Metal. Its Alloys and Compounds, Reinhold Publishing Co., New York, NY, 1959, pp. 79-95. 8. T. Rosenqvist: Principles of Extractive Metallurgy, McGraw-Hill Book Co., New York, NY, 1974, p. 307. 9. T. Tamagawa, M. Kobayashi, and N.X. Fu: Proc. TMS Annual Meeting, New Orleans, LA, Feb. 1115, 2001; EPD Congress 2001, P.R. Taylor, ed., TMS, Warrendale, PA, pp. 195-201. 10. J.P. Hirth: in Vapor Deposition, Carroll F. Powell, ed., John Wiley & Sons, New York, NY, 1966, pp. 126-33. 11. International Critical Tables of Numerical Data Physics, Chemistry and Technology, E.W. Washburn, ed., McGraw-Hill Book Co., New York, NY, 1928, vols. II, III, and V. 12. Handbook of Heat Transfer, W.M. Rohsenow and J.P. Hartnett, eds., McGraw-Hill Book Co., New York, NY, 1973, pp. 2-71. 13. Max Jakob: Heat Transfer, John Wiley & Sons, New York, NY, 1949, pp. 95-98 and 278-83. 14. Hoyt C. Hottel: Radiative Transfer, McGraw-Hill Book Co., New York, NY, 1967, pp. 140-45. 15. P.M.J. Gray and S.E. Woods: Proc. 9th Commonwealth Mining and Metallurgical Congr., M.J. Jones, ed., Institute of Mining and Metallurgy, London, 1970, vol. 3, pp. 872-75. 16. F. Noguchi and T. Nakamura: J. Min. Mater. Processing Inst. Jpn., 1995, vol. 111, pp. 181-85. 17. J.A. Clarke and D.J. Fray: Trans. Inst. Min. Metall., Sect. C, 1982, vol. 91, pp. C26-C31. 18. L.A. Lewis and A.N. Cameron: Metall. Mater. Trans. B, 1995, vol. 26B, pp. 911-18. 19. J.M. Osborne, W.J. Rankin, D.J. McCarthy, and D.R. Swinbourne: Metall. Mater. Trans. B, 2001, vol. 32B, pp. 37-45.

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