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The Kinetics of the Nitrogen Reaction Saturated Iron Alloys* with Carbon

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The Kinetics of the Nitrogen Reaction Saturated Iron Alloys* with Carbon The Kinetics of the Nitrogen Reaction with Carbon Saturated Iron Alloys* By Fumitaka TSUKIHASHI** and Richard J. FR UEHAN * * * Synopsis gen reaction and showed that oxygen and sulfur re- The kinetics of the nitrogen reaction with liquid Fe-C alloys was tarded the rate of the reaction. Later Inouye and investigated by using the isotope exchange technique. The effectof small Choh4) studied the rate of absorption of nitrogen at amounts of S, P, Pb, Sn, Bi and Te in Fe-Csat , alloys on the rate low nitrogen content in liquid Fe and Fe alloys constant of the interfacial nitrogen reaction was studied at l 450°C. using a sampling technique and found that at low The rate constant for Fe-Csat .-S alloys was in agreement with the sulfur and oxygen concentrations the rate of nitrogen previous resultsfor Fe-S alloys. It was also confirmedthat the influenceof absorption was half order with respect to nitrogen carbon in Fe-C-S alloys on the rate of the nitrogen reaction is negligible. The effectof tin on the rate constant is small even when the tin content is pressure. However, at high sulfur and oxygen levels the rate was proportional to the nitrogen pressure. as high as 0.8 wt%. However Pb, Bi and Te have significant effects on the rate constant and the addition of small amounts of these elementsde- Mori and Suzuki7) measured the rate of nitrogen re- creases the rate significantly. Phosphorus also decreasedthe rate constant. moval from liquid iron and found the rate to be According to the adsorption model, the interfacial reaction rate should second order with respect to dissolved nitrogen con- approach zero at high concentrationof surface active elements, but in the tent. Mowers and Pehlke8) investigated the rate of case of Fe-Csat.-P, Fe-Csat.-Pb and Fe-Csat.-Te alloys, there was solution of nitrogen in liquid Fe-Se and Fe-Te alloys evidenceof a residual rate at high concentrationsof P, Pb and Fe. using a modified Sieverts' apparatus at pressure of 1 atm and a temperature of 1 600°C. They demon- Key words: kinetics; nitrogen reaction rate; carbon saturated iron alloy strated selenium and tellurium present in low con- phosphorus; tin; lead; bismuth; tellurium; sulfur. centrations have a marked retarding effect on the rate of solution of nitrogen in liquid Fe alloys, Narita I. Introduction et a1.9)investigated the kinetics of nitrogen desorption In recent years the reaction of nitrogen with iron reaction of liquid iron and steel and found that the and steel has taken on added importance. Dissolved desorption reaction rate is second order. Ban-ya nitrogen can be harmful in several ways. For exam- et a1.12)also studied the rate of removal of nitrogen ple, it can be responsible for porosity or it may react from liquid iron investigating the influence of 0, S, to form nitrides which decrease the formability of the Si, C, Cr and Ni on the rate and they found that the steel. Nitrogen gas is used in many new ladle metal- rate is second order with respect to nitrogen content lurgical processes and subsequently can be absorbed and the surface active elements such as sulfur and into the metal. Once nitrogen is absorbed into the oxygen retard the nitrogen desorption. Amano et metal it is difficult to remove; vacuum degassing, at a1.14>studied the absorption and desorption reaction best, only removes 10 to 20 % of the nitrogen present. of nitrogen by levitation technique. They reported Therefore it is important to control the nitrogen ab- that the reaction is first order when there exists no sorption during all the steelmaking processes. Nitro- gas boundary layer and the reaction is between first gen can also be harmful in the production of cast iron. and second order when there are two boundary In particular, porosity in iron castings resulting from layers. Kadoguchi et al.17) studied the rate of ab- gas evolution can be a major problem. It may be sorption of injected nitrogen in molten iron and found possible to control the reaction of nitrogen with Fe- that the rate controlling steps are the chemical reac- Csat, alloys by the addition of surface active elements tion and the mass transfer in liquid phase. Kawa- which retard the rate. kami et al.18) studied absorption and desorption rates Several researches have been reported on the rate of nitrogen in molten iron by bottom injection. They of the reaction of nitrogen with liquid Fe alloys.l-23) found that nitrogen absorption rate from pure nitro- Pehlke and Elliott1'2) studied the thermodynamics and gen is controlled by the mass transfer in metal phase the kinetics of nitrogen reaction in liquid Fe and and the desorption of nitrogen by Ar-N2 mixture was Fe alloys using a constant pressure Sieverts' appara- controlled by the mass transfer in gas phase. tus. They found that the rate is first order with Fruehan and Martonik19) measured the rate of respect to the nitrogen content and at low sulfur and nitrogen absorption into and desorption from liquid oxygen levels the rate was controlled by mass transfer iron containing sulfur and oxygen by employing a in the liquid phase. They investigated the effect of modified Sieverts' technique with a highly sensitive Al, Cb, Cr, Ni, 0, S and W on the rate of the nitro- pressure transducer. They conclusively demonstrated * Manuscript received on April 16, 1987; accepted in the final form on September 11, 1987. © 1987 ISIJ * * Formerly Carnegie-Mellon University . Now at Department of Metallurgy, Faculty of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo 113. * * * Department of Metallurgical Engineering and Materials Science, Carnegie-Mellon University, Pittsburgh , PA 15213, U.S.A. ( 858 ) Research Article Transactions ISIJ, Vol. 27, 1987 (859) that the rate of nitrogen absorption into iron alloys the effect of S, P, Pb, Bi, Sn and Te on the nitrogen with surface active solute was second order with reaction with liquid Fe-Csat . alloys. The rate was respect to nitrogen concentration or first order with measured by using the isotope exchange technique, respect to nitrogen partial pressure and the rate was since the measured rate is not affected by liquid phase controlled by the dissociation of the nitrogen molecule mass transfer or the evolution of other gases from the on the surface. melt. In the later work, Fruehan and Martonik20~ mea- sured the effect of sulfur on the nitrogen reaction with Fe-Cr and Fe-Cr-Ni alloys. They found that chro- II. Experimental mium increases the rate. At low levels of sulfur con- As described in the papers of Glaws and Frue- tent absorption rate was controlled by liquid phase han,22,23~it is possible to employ both the isotope mass transfer of nitrogen, but at high sulfur levels the exchange and the Sieverts' technique in a single rate was controlled by mass transfer and the chemical apparatus. As Ishii et al.24~have pointed out, since rate on the surface in series. A correction was made CO gas is evolved from Fe-C alloys, the Sieverts' for the influence of liquid phase mass transfer on the technique was not suitable for the measurements in measured rates. These effects are negligible at high the present study. Therefore the isotope exchange sulfur concentrations, but become significant at inter- technique was employed to investigate the kinetics mediate sulfur contents. At low levels of sulfur this of the nitrogen reaction with liquid Fe-C-X solu- method of determining the intrinsic chemical reaction tions, where X is a solute element. The experimental rate constant, becomes very imprecise, since the mass apparatus and technique were previously described in transfer effects become significant. detail.23~ Metal samples weighing approximately 30 To measure the interfacial reaction rate and elimi- g were contained in a crucible which is high density nate the influence of liquid phase mass transfer, Byrne and high purity (99.8 %) alumina with 20 mm I.D., and Belton21 employed the isotope exchange tech- 22 mm O.D, and 33 mm height. Alumina crucible nique in their study of the kinetics of nitrogen reac- was set in the outer safety crucible which was slip cast tion with liquid Fe and Fe-S alloys. This technique lime-stabilized zirconia with approximately 25 mm permits a direct experimental determination of the I.D. and 50 mm height. The crucible was placed in rate of N2 dissociation on the liquid metal surface via a fused silica reaction chamber and carefully induc- measurement of the rate of exchange reaction tively heated to the experimental temperature. The 28N2+30N2 = 229N2 experimental temperature was mainly 1 450°C, and .....................(1) some experiments for Fe-C-S alloys were also con- The experiment is run under the condition of equi- ducted at 1 600°C. The sample temperature was librium between the gas at the interface and liquid monitored by a two-color ratio pyrometer, sighted bulk phase. This permits the measurement of inter- onto the metal surface. The pyrometer was calibrated facial chemical reaction rates that would normally be against the melting temperature of pure iron. Any considered too fast for the conventional kinetic ex- necessary temperature adjustments were made man- perimental technique for inductively stirred melts. ually via the power controls on the R.F. generator. Byrne and Belton21 found the exchange rate to be The desired metal surface temperatures were main- first order with respect to nitrogen partial pressure on tained within +5°C. high purity iron and the rate for Fe-S indicated that During heat up, a N2-H2 gas mixture was passed sulfur closely followed an ideal chemisorption model.
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