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Jan 1, 1967

By J. J. Kramer, W. A. Tiller, G. F. Bolling

THE axial orientations of columnar crystals in unidirectionally solidified ingots of zone-refined zinc and tin have been examined using the techniques recently described by us.' Both metals had an initial purity of 99.999+ pct before zone refining and satisfied all qualitative guides for very high purity after zone refining. Fig. 1 presents the orientations of the columnar crystals for tin and zinc, respectively. For tin, there is a preference for grains growing in the [I101 direction, i.e., the dendrite direction.' For zinc, a weak preference for the [0001] direction is seen (a random population in the unit triangle would give equal density on either side of the 60-deg circle centered on [0001]).' There was no apparent evidence for dendritic growth in either metal. These results, and those previously reported,' confirm the recent investigation by Hellawell and Herbert of casting textures observed for zone-refined lead, zinc, and tin.4 The preferred casting orientations for these metals in both the impure and zone-refined states are given in Table I. In the experiments on zone-refined lead,' it was shown that two separate textures existed: a preferred (111) nucleation texture existed at the chill surface and a preferred (111) texture developed during solidification. Either effect is sufficient to produce the result recorded in Table I. Similarly the results recorded for tin and zinc may be attributable to either a preferred nucleation or a preferred growth phenomenon and additional experiments are required to separate these two possible explanations. Hellawell and Herbert' attribute their results to a preferred growth process and account for it on the basis of a "layer-growth" model proposed much earlier by one of the present authors.5 An equally satisfactory growth model would be that based upon anisotropic surface energies. However, both of these growth models would indicate that the preferred growth direction for very pure metals should be normal to the plane of closest packing in the metal. This is consistent for zinc but, contrary to the conclusion of Hellawell and Herbert, it is not consistent for tin since here the (100) is expected to exhibit a greater density of packing than the (110). Although tin is expected to exhibit an anisotropy of thermal conductivity, we would expect the thermal conductivity to be the same in the [1101 as the [l00]

Jan 1, 1963

By W. J. Taylor

SOME eight years ago I became interested to a considerable extent in one of the well-known deposits of sulphury iron ore in New Jersey, and, as a consequence, soon became interested in the subject of the elimination of the sulphur. On investigation I found that no department of pig-iron manufacture had received less attention than that of roasting or calcining ores for the elimination of sulphur, carbonic acid, water, etc. My first devices to eliminate sulphur were naturally in the lime-kiln line, with solid fuel mixed with the ore, in the same way as common lime is burnt with small coal. While this process will succeed tolerably well for carbonates or calcareous ores, even though they contain sulphur as sulphates, I soon found it would not answer for our magnetites, which are very hard and dense, carrying from 2 to 5 per cent. of sulphur as pyrites, and become very sticky as soon as any attempt is made to roast them at a high heat. Some laboratory experiments developed the fact that the nearer the gaseous current surrounding the hot ore approached in composition pure atmospheric air the more rapidly the sulphur was oxidized, while in an atmosphere composed largely of carbonic oxide, carbonic acid, and nitrogen, it seemed almost impossible to reduce the sulphur more than one-half, which was a confirmation of the well-known fact that just one-half of the sulphur in pyrites volatilizes very easily, and that the trouble is mainly to remove the remainder. It was thus apparent that the atmosphere surrounding the ore was of as much importance as the temperature. This led to the trial of a kiln to heat the ore by conduction through the brick. It was divided into ore-chambers, which were surrounded with flues, through which the products of combustion of gaseous fuel passed without coming in contact with the ore. We did not, however, succeed by this arrangement in getting more than a cherry-red heat, which, of course, was too low to accomplish anything. I had at this point become convinced – 1st. That gaseous fuel only would accomplish the work successfully. 2d. That since a high temperature was required to insure a rapid oxidation of the sulphur, and also to make the ore open and porous,

Jan 1, 1881

By J. B. Austin

It is now well established, chiefly through the work of Davenport and Bain,' that the influence of temperature upon the rate of transformation of austenite to ferrite at constant temperature is represented by a curve of the type shown in Fig. 5 on page 295 and the reasons for this general shape have been discussed by them in a qualitative way. Thus, the upper part, or nose, of the curve is the resultant of two factors of which the rate of change with temperature is not the same, and by analogy with other like cases it is almost certain that these factors are: (1) the chemical potential, or driving force, of the transformation, which is zero at the equilibrium temperature and increases rapidly as the temperature falls below this point; and (2) a factor analogous to viscosity, or resistance of the crystal lattice to a change in structure, which also increases as the temperature is lowered. Just below the equilibrium temperature this virtual "viscosity" of the metal is relatively low—that is, the metal offers little resistance to a change in lattice—but the driving force is also small, and the net result is that the reaction proceeds slowly. As the temperature is lowered the magnitude of both factors increases; but at first the driving force increases more rapidly than the resistance and the reaction is observed to proceed more rapidly. At lower temperatures, however, the resistance begins to increase faster than the driving force, and eventually, at the nose of the curve, overbalances it, causing the reaction to proceed more and more slowly thereafter. This concept is somewhat, though not completely, analogous to that employed in certain electrical cases where the precise factors are known and are separately measurable. The current I (in amperes or coulombs per second) flowing through a given wire is proportional to the impressed potential, or driving force E, and is inversely proportional to the resistance R of the wire; that is, I = E/R. Stated in a slightly different way, the time required for one coulomb to pass a given point (1/I) is equal to R/E. If the temperature of the whole circuit is changed, the resultant change in 1/I will depend on the relative rates of change of R and of E,

Jan 1, 1935

By J. B. Austin

It is now well established, chiefly through the work of Davenport and Bain,' that the influence of temperature upon the rate of transformation of austenite to ferrite at constant temperature is represented by a curve of the type shown in Fig. 5 on page 295 and the reasons for this general shape have been discussed by them in a qualitative way. Thus, the upper part, or nose, of the curve is the resultant of two factors of which the rate of change with temperature is not the same, and by analogy with other like cases it is almost certain that these factors are: (1) the chemical potential, or driving force, of the transformation, which is zero at the equilibrium temperature and increases rapidly as the temperature falls below this point; and (2) a factor analogous to viscosity, or resistance of the crystal lattice to a change in structure, which also increases as the temperature is lowered. Just below the equilibrium temperature this virtual "viscosity" of the metal is relatively low—that is, the metal offers little resistance to a change in lattice—but the driving force is also small, and the net result is that the reaction proceeds slowly. As the temperature is lowered the magnitude of both factors increases; but at first the driving force increases more rapidly than the resistance and the reaction is observed to proceed more rapidly. At lower temperatures, however, the resistance begins to increase faster than the driving force, and eventually, at the nose of the curve, overbalances it, causing the reaction to proceed more and more slowly thereafter. This concept is somewhat, though not completely, analogous to that employed in certain electrical cases where the precise factors are known and are separately measurable. The current I (in amperes or coulombs per second) flowing through a given wire is proportional to the impressed potential, or driving force E, and is inversely proportional to the resistance R of the wire; that is, I = E/R. Stated in a slightly different way, the time required for one coulomb to pass a given point (1/I) is equal to R/E. If the temperature of the whole circuit is changed, the resultant change in 1/I will depend on the relative rates of change of R and of E,

Jan 1, 1935

By H. M. Howe

PART I. INTRODUCTORY. § 24. INTRODUCTION.-This paper discusses the chief existing data as to the temperature, in iron-carbon alloys, of Ae.3, the upper limit of the transformation range when in equilibrium, as distinguished from Ac3, the temperature at which the end of the transformation is noted in heating up, and from Ar3, that at which its beginning is noted in cooling down. The former is in fact carried above Ae3 and the latter below Ae3 by lag. I touch incidentally on the influence of manganese on Ae3 (§ 29, p. 1102). The sections, tables, and illustrations, are numbered consecutively with those in the accompanying papers by Howe and Levy on Determination of, the Position of Ae3 in Carbon-Iron Alloys, and by Burgess, Crowe, and Rawdon on Thermal and Microscopical Examination of Professor Howe's Standard Commercial Steels, to which the present paper forms a sequel. § 25. The contradictoriness of our present evidence is shown by grouping it together in Fig. 14. For instance, both Goerens and Meyer (Series 2) and Meuthen (Series 12) used practically stationary temperature, and thus reduced the influence of lag very greatly; yet Ae3 for 0.32 carbon steel according to the former investigators is 894°, but according to Meuthen it is at or below 770°, a discrepancy of 124° or more. In view of our ability to measure these high temperatures within a few degrees, the existence of such a discrepancy is as unwelcome as it seems needless. I attack the thankless task of bringing some order out of this chaos.

Jan 6, 1913

By W. J. Taylor

Some eight years ago I became interested to a considerable extent in one of the well-known deposits of sulphury iron ore in New Jersey, and, as a consequence, soon became interested in the subject of the elimination of the sulphur. On investigation I found that no department of pig-iron manufacture had received less attention than that of roasting or calcining ores for the elimination of sulphur, carbonic acid, water, etc. My first devices to eliminate sulphur mere naturally in the limekiln line, with solid fuel mixed with the ore, in the same way = common lime is burnt with small coal. While this process will succeed tolerably well for carbonates or calcareous ores, even though they contain sulphur as sulphates, I soon found it would not answer for our magnetites, which are very hard and dense, carrying from 2 to 5 per cent. of sulphur as pyrites, and become very sticky as soon as any attempt is made to roast them at a high heat. Some laboratory experiments developed the fact that the nearer the gaseous current surrounding the hot ore approached in composition pure atmospheric air the more rapidly the sulphur was oxidized, while in an atmosphere composed largely of carbonic oxide, carbonic acid, and nitrogen, it seemed almost impossible to reduce the sulphur more than one-half, which was a confirmation of the well-known Pact that just one-half of the sulphur in pyrites volatilizes very easily, and that the trouble is mainly to remove the remainder. It was thus apparent that the atmosphere surrounding the ore was of as much importance as the temperature..• This led to the trial of a kiln to heat the ore by conduction through the brick. It was divided into ore-chambers, which were surrounded with flues, through which the products of combustion of gaseoua fuel passed without coming in contact with the ore. We did not, however, succeed by this arrangement in getting more than a cherry-red heat, which, of course, was too low to accomplish anything. I had at this point become convinced— 1st. That gaseous fuel only would accomplish the work successfully. 2d. That since a high temperature was required to insure a rapid oxidation of the sulphur, and also to make the ore open and porous,

Jan 1, 1881

By Carl Henrich

Jan 1, 1893

By I. W. Walling, F. B. Plummer

Bastin and others have demonstrated the presence of sulphate-reducing bacteria in oil wells producing salt water. Analyses show that at 125°F. bacteria alone reduce sulphates in East Texas salt water by only 3 per cent in 30 days, forming principally hydrogen sulphide and sodium or calcium hydroxide. The hydrogen sulphide reacts with soluble iron compounds to produce iron sulphide in the absence of oxygen, and ferric hydroxide where oxygen and air are present. Where iron or other metals and iron sulphide are already in the water containing bacteria, I00 per cent reduction of the sulphates is complete in 30 days or less; where magnesium is present, reduction is complete in 15 days. The effects of changes in temperature, of different bactericides, and of concentration of bactericides on sulphate reduction are described in detail and illustrated by tables and curves. The significance of sulphate reduction on corrosive properties of oil-field water is briefly discussed. Chemistry of East Texas Oil-field Water The chemical composition of the water in the East Texas field salt-water disposal pits is shown in Table I. This salt water corrodes pipes, pumps, and steel tanks excessively, principally because of its content of oxygen, hydrogen, sulphide, and carbonic acid. The carbonates in the water when exposed to air tend to give up carbon dioxide and to precipitate calcium carbonate in large quantities. This forms coatings in tanks, settling pits, and ditches, and soon, unless removed by acid treatment, will effectively clog an injection well and reduce the flow of water back into the ground. The iron compounds in the water, most of which are dissolved from tanks and pipes, are in the ferrous form, and when exposed to the air are oxidized from soluble ferrous carbonate to insoluble ferric hydroxide, resulting in the precipitation of a gelatinous precipitate that will clog oil-field sands effectively: 2Fe(HCO3)2 + O + H2O -> 2Fe(OH)3 + 4CO2 The sulphates in strong sulphate-bearing water may be attacked by swarms of sulphate-reducing bacteria and more hydrogen sulphide may be produced. The hydrogen sulphide reacts with soluble minerals in the water to form black sludges. A knowledge of the chemistry of each reaction in oil-field water is important to the oil-field engineer, since means must be devised to prevent the formation of harmful precipitates that clog injection wells and to prevent corrosion of tanks by harmful products of biochemical processes. Methods of Treating Water before Injection into Ground* The open system of handling the waste salt water in the East Texas field consists of aerating and chemically treating the water to precipitate the unstable iron,

Jan 1, 1946

By F. B. Plummer, I. W. Walling

Bastin and others have demonstrated the presence of sulphate-reducing bacteria in oil wells producing salt water. Analyses show that at 125°F. bacteria alone reduce sulphates in East Texas salt water by only 3 per cent in 30 days, forming principally hydrogen sulphide and sodium or calcium hydroxide. The hydrogen sulphide reacts with soluble iron compounds to produce iron sulphide in the absence of oxygen, and ferric hydroxide where oxygen and air are present. Where iron or other metals and iron sulphide are already in the water containing bacteria, I00 per cent reduction of the sulphates is complete in 30 days or less; where magnesium is present, reduction is complete in 15 days. The effects of changes in temperature, of different bactericides, and of concentration of bactericides on sulphate reduction are described in detail and illustrated by tables and curves. The significance of sulphate reduction on corrosive properties of oil-field water is briefly discussed. Chemistry of East Texas Oil-field Water The chemical composition of the water in the East Texas field salt-water disposal pits is shown in Table I. This salt water corrodes pipes, pumps, and steel tanks excessively, principally because of its content of oxygen, hydrogen, sulphide, and carbonic acid. The carbonates in the water when exposed to air tend to give up carbon dioxide and to precipitate calcium carbonate in large quantities. This forms coatings in tanks, settling pits, and ditches, and soon, unless removed by acid treatment, will effectively clog an injection well and reduce the flow of water back into the ground. The iron compounds in the water, most of which are dissolved from tanks and pipes, are in the ferrous form, and when exposed to the air are oxidized from soluble ferrous carbonate to insoluble ferric hydroxide, resulting in the precipitation of a gelatinous precipitate that will clog oil-field sands effectively: 2Fe(HCO3)2 + O + H2O -> 2Fe(OH)3 + 4CO2 The sulphates in strong sulphate-bearing water may be attacked by swarms of sulphate-reducing bacteria and more hydrogen sulphide may be produced. The hydrogen sulphide reacts with soluble minerals in the water to form black sludges. A knowledge of the chemistry of each reaction in oil-field water is important to the oil-field engineer, since means must be devised to prevent the formation of harmful precipitates that clog injection wells and to prevent corrosion of tanks by harmful products of biochemical processes. Methods of Treating Water before Injection into Ground* The open system of handling the waste salt water in the East Texas field consists of aerating and chemically treating the water to precipitate the unstable iron,

Jan 1, 1946

By I. M. Bernstein

The steady-state creep behaviov of zirconium and zivcaloy-2 was examined in the temperature vatlge 520° to 620°C A1 low stresses the creep rates were cimracterized by a linear stress dependence; at highev stresses the stress dependence was much more pronounced. Temnperature-cycling tests yielded values for the aclivation enevgy for creep. Various tlzeories were examined in the ligltt of- the experimental re-sults and it mas concluded that the low-stress creep behavior is the result of the stress-direcled diffusion of vacancies along gain boundaries. It has been observed,"&apos; usually under conditions of high temperature and low stress, that creep deformation can occur for which the steady-state creep rate is linearly dependent on the applied stress. For magnesium and certain magnesium alloys, Harris and ones&apos; and ones&apos; have argued that this type of creep occurs by mass transfer as a result of the stress-induced generation and migration of vacancies, along a gradient defined by the stress direction. Jones&apos; demonstrated that the rate-controlling diffusion path is sensitive to grain size and temperature, and that by suitable control of these variables creep could occur by vacancy diffusion either predominately along grain boundaries or through the lattice. Recently, Jones3 suggested from an examination of limited high-stress data for zircaloy-2, composition in Table I, that significant diffusion creep could occur at low stresses, at least between 375" and 500°C, controlled by grain boundary vacancy diffusion. This process could have an important implication in assessing the role of zirconium alloys as a structural or cladding material in certain classes of nuclear reactors, since it predicts creep deformation far in excess of any estimates based on extrapolating slip creep data from higher stress levels. If the diffusion creep process occurs it should be possible to describe the total steady-state creep rate of zirconium and its alloys as the sum of two terms, Eq. [I]; the first term relates to a slip creep process important at high stresses and which is manifested by a much more pronounced dependence of creep rate on stress4 than diffusion creep and the second to a process controlled by mass transfer,5&apos;6 dominant at low stresses: where A and BI are parameters which can depend on structure, Ql and Q2 are the activation energies for the particular creep process occurring, and n describes the sensitivity of the creep rate on stress. It is the purpose of this paper to present some direct experimental evidence in support of this view. It is recognized that other analytical approaches have been proposed to explain data of this kind and these will also be discussed. 1) EXPERIMENTAL PROCEDURE Flat creep specimens (gage length 1 by 0.25 by 0.02 in. approx) were prepared from cold-rolled, argon-remelted, crystal bar zirconium and cold-rolled commercial-grade zircaloy-2, the analyses of which are given in Table I. The specimens were annealed at a pressure of < 10-5 Torr at temperatures from 625" to 675°C for 2 hr and slow-cooled. This treatment produced stable grains of average size (defined here by the average linear intercept) of for zirconium and -4xin. (-10 p) for zircaloy-2. The specimens were tested in a dead load tensile creep rig. The stress was maintained constant by adjusting the applied load after approximately each 1 pct of strain. The specimen temperature was controlled to better than +1°C. This system had a small thermal lag, so that rapid temperature changes were possible. To minimize corrosion, the specimens were tested in high-purity (99.95 pct) argon, further dried,

Jan 1, 1968

By John V. Beall

If you will be patient, we will explain how our plans to research the fishing possibilities of the Buffalo River following the SME Fall Meeting turned out, in general, to be an extension of the main theme of that meeting and, in particular, to confirm an astute observation on research made by Australian T. R. A. Davey in his Award-acceptance address at the Pb-Zn Research Luncheon. Buffalo River State Park is reached via Yellville where we tried without success to find one Odie Tollett who had been recommended as a boat liveryman. However, Mrs. Leon Dodd, in the Park, outfitted us nicely with a 17-foot aluminum canoe. Rain had dominated the recent weather of the Ozarks in northwestern Arkansas. So, under a leaden sky and intermittent showers, we stood on the bank of the turgid Buffalo demonstrating to our spouse, Sylvia, how to cast. Of course, with the water up and the sediment, the outlook for catching fish was bad. Sylvia said, however, "Oh, I get it. Let me try. Umm, like this I got one!" Sylvia reeled in a pretty ten-inch brown trout. "The poor thing, let&apos;s throw him back."

Jan 1, 1970

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

THE tensile and notch tensile ductile-to-brittle transition characteristics of several refractory metals and alloys have been well documented.1-3 Electron-beam melted tantalum and columbium have been shown to retain excellent ductility at very low temperatures. Some indications of brittle behavior (low ductility and cleavage fracture) were observed with columbium tested at -253oC, but no similar effects were noticed with tantalum. Increasing the interstitial oxygen content in these two materials resulted in the detection of indications of brittle behavior at higher temperatures, although good ductility was retained in both bases at -196°C when they contained about 1 at. pet 0. Detailed descriptions of the impact transition behavior of these two materials at various purity levels have not been available. This technical note describes the effect of interstitial oxygen on the impact properties of wrought, fibered tantalum and columbium and compares the transition behavior to the previously determined tensile transition characteristics. Tantalum and columbium impact specimens with three different interstitial oxygen levels indicated in Table I were tested at temperatures ranging from -196o to 300°C. Oxygen additions were made to 1/2-in.-diam bars of electron-beam melted material in a Seiverts Apparatus. The oxygenated bars were then homogenization-annealed to obtain uniform cross-section hardnesses and swaged to

Jan 1, 1964

Carlisle: This is August 1960 and I am sitting across the table from Henry DeWitt Smith. We both took the mining course at Yale the same year; and here we are, over fifty years later, at Nantucket Island where we have spent quite a number of summers together. Now, let&apos;s start the questions with something about the center of your career. Let&apos;s say Tsumeb; not about the mine itself which people know, but some of the details on how you happened to take it over for Newmont. Mr. Smith: I first heard of Tsumeb, a famous German mine, through our own associates O&apos;okiep Copper Co. From 1935 on, the local management at O&apos;okiep, being reasonably close, kept the New York office informed. It served as a listening post for new mine development, as well as being a highly profitable copper mine in the northwest Cape Colony. We had all known of a famous German mine in South West Africa called Tsumeb. But it had a reputation for not welcoming visiting engineers. One engineer who went to this property for the Ministry of Supply in 1943, &apos;44 and &apos;45 was Arthur Storke. He was much impressed with possibilities of profitable operation. This mine had been operated by a German company since 1910. It was finally taken over by the Custodian of Enemy Property for the Union of South Africa.

Jan 11, 1963

By Charles L. Mantell, Kurt Straler

The hydrogen reduction of Cr2O3 to chromium metal was found to be feasible at very low water-vapor concentrations, corresponding to dew points of -38° to -24°C, over a temperature range of 1130" to 1490°C. Hydrogen reduction under these conditions was predicted by the calculated equilibrium curves which also indicated that CrzOs is reduced directly to chromium without forming the intermediate oxide, CrO. This reduction path was confirmed by X-ray diffraction analysis. The percent reduction of Cr2O3 at each reaction temperature was constant with time, suggesting an inhibiting effect of water vapor. A small increase in the residual water-vapor concentration of a single temperature, 1490°C, strongly retarded the rate of reduction This effect was expressed by an empim&apos;cal equation which indicated a direct relationship between "distance from equilibrium" and the rate of reduction. me effect of temperature over the range of 1130" to 1490°C was expressed in an Arvhenius plot of log rate vs reciprocal absolute temperature. From this curve the apparent enthalpy of activation was found to be 29,600 cal. Based on the hypothesis that the rate of reductiun is contvolled at the oxide-metal interface, an over-all rate equation consistent with the experimental data and the thery of absolute reaction rates was formulated. A simplification of this expression to an Arrhenius equation was justified by the overriding effect of temperature on the rate of reaction for the minimum water-vapor concentration range. MOST of the metals in Subgroup V1 of the periodic table can be prepared commercially by direct reduction of their oxides by hydrogen or carbon monoxide, at temperatures considerably below the melting points of both the metals and their oxides. Chromium is an exception, being generally reduced from its ore, Cr2O3 . FeO, by silicon in an electric arc furnace which operates above the melting point of the Fe-Cr alloy or above the melting point of chro- mium if a chromium oxide be the starting material. In reduction of chromium oxide by hydrogen, either reduction does not occur at all or the rate of reduction is extremely slow. Theoretical considerations based on the high, exothermic, free energy of formation of Cr2O3 compared to the oxides of the other Subgroup VI metals, molybdenum, tungsten, and uranium, would also suggest a slow rate of reaction and a high activation energy. Interest in the direct gaseous reduction of fine-powdered ores in fluidized beds was considered justification for examination of this reaction. In order to develop a basis for a continuing study of the commercial feasibility of the direct gaseous reduction of chromite, a study of the kinetics of the reduction of Cr2O3 with hydrogen was undertaken. To the authors&apos; knowledge no accurate kinetic data for this reaction have been obtained. Neither has an activation energy been determined nor has an attempt been made to establish a mechanism of reaction. LITERATURE Maier10 compared the data of I. Y. Granaat,6 H. von Wartenburg and S. Aoyama, and G. Grube and M. Flad7 with that derived from calorimetric and ther-modynamic properties for the equilibria for the reduction of Cr2O3 with hydrogen. These results, plotted as the log of the equilibrium constant vs absolute temperature for the reduction of Cr2O3 and the intermediate oxide, CrO, to chromium, show agreement between the differently derived data. In both cases the equilibrium constants were extremely low. Maier showed that, over a temperature range of 1000° to 2000°K, Cr2O3 is more readily reducible than CrO. Granat assumed that CrO was preferentially formed from Cr2o3 above 1100°C. Grube and Flad&apos;s analysis of their reaction products in the 895" to 1000°C range indicated the coexistence of only Cr2O3 and chromium. The hydrogen reduction of the other Subgroup VI metals, molybdenum, tungsten, and uranium, shows that reduction of the higher oxide proceeds through all of the intermediate oxides before being reduced to the metal. Since evidence pointed to an anomaly in the reduction behavior of Cr2O3, the authors investigated the reduction path of Cr2Os.to chromium. This was done theoretically with more recently available free-energy data and experimentally by X-ray diffraction analysis. This work reinforces Maier&apos;s conclusion.

Jan 1, 1964

By R. M. Hudson, P. E. Perry

Weight-gain data obtained by nitriding low-carbon sheet steel in an amrnonia CNH,) atmosphere indicated that the process obeyed a parabolic rate law. The calculated actization energy for nitriding in the range 964" to 1268°F agreed reasonably well with published data. At 1358"F, rate data indicated that the activation energy decreased. Weight-gain data obtained by uszng mixtures of NH3 -Nz at 1268°F containzng jrom 10 to 100 zol pct NH3 also obeyed a parabolic rate law. The rate of &apos;nitriding increased with an increase in the NH3 content of the gas Mixture. It is well-known that steel heated in gas mixtures containing ammonia (NH3) takes up much larger quantities of nitrogen than steel heated in nitrogen, both gases having a total pressure of 1 atm;&apos; this phenomenon can presumably be attributed to the catalytic decomposition of NH3 on the steel surface to furnish nascent (monatomic) nitrogen. This process was studied bv Brunauer. Jefferson, Emmett, and Hend-ricks at furnace temperatures of 752" and 831°F2 using mixtures of NH3 in Hz. Englehardt and wagner3 reported that, at a furnace temperature of 914°F and under their experimental conditions, both nitriding and denitriding were controlled by the rate of gas-metal reactions at a steel surface rather than by the rate of diffusion of nitrogen in iron. The present study was undertaken to obtain information on the kinetics of nitriding low-carbon steel strip at higher temperatures so that practical rates for short-time strip-annealing treatments could be estimated. Variables studied included time: temperature, and NH, content in the annealing atmosphere. Mechanical and chemical characteristics of steel nitrided in this manner will not be considered in the present article. MATERIALS AND EXPERIMENTAL WORK The samples used were from a commercial low-carbon steel, 0.0244 cm thick, in the cold-reduced condition. The chemical composition of this steel is given in Table I. Panels were cut to 5.1 by 17.8 cm, degreased in toluene, and weighed just before treatment. Four specimens were nitrided under each of the experimental conditions. A study was made of the nitriding rate of steel in a 100 vol pct ammonia atmosphere, 740 mm pressure, at five specific temperatures within the range 964" to 1358°F. The nitriding rates of steel in ammonia-nitrogen gas mixtures containing 10, 18, 26, 50, and 100 vol pct ammonia, 740 mm total pressure, at 1268°F were also determined. All atmospheres used were dried by successively passing them through drying towers packed with soda lime and with Linde Molecular sieve Type 4A. Quoted gas compositions refer to those entering the furnace. Specimens were held in the constant-temperature zone of a vertical annealing tube furnace for times of 14, 3, 5, 10, or 15 min. Gas flow rates were maintained at 3.8 cu ft per hr, which was nineteen volume changes per hour for the system used. The rate of flow was selected to provide a high level of free NH3 for cracking on the steel surface where the ammonia gas is most effectively used as a nitriding agent. The vertical annealing tube furnace consisted of a Hevi-Duty tube furnace with a 2 1/2-in.-ID mullite ceramic high-temperature tube. The constant-temperature zone (controlled within 10°F) was about 10 in. long. After each specimen was degreased, a hole was punched in one end, for attaching the specimen by hook to a chain so that it could be lowered into or raised from the high-temperature portion of the tube by means of a power-driven winch. A stainless-steel access port with O-ring seals was connected by suitable glass-to-metal seals to the cool upper portion of the furnace tube. After the weighed specimen was placed in the access port, the furnace tube was evacuated to approximately 10"3 torr, and then the system was flushed thoroughly with the atmosphere under study. When the gas flow rate and constant-temperature zone of the furnace were established, the specimen was lowered into the constant-temperature zone. The atmosphere flowed from the top to the bottom of the vertical furnace tube and was then vented. For all these runs, during the first 3 min of the time the specimen was in the constant-temperature zone of the furnace the specimen was heating up to the tempera-

Jan 1, 1970

By T. V. Philip, R. E. Lenhart

C. G. Dunn(General Electric Research Laboratory)— It is well recognized that understanding of the formation of the cube-on-edge texture in annealed commercial cold-rolled Si-Fe strip is important industrially as well as scientifically. I would like to make a few remarks on this subject, discuss some points in the present paper, and list two remaining problems that appear to be particularly outstanding. Attention should be drawn to the paper by P. K. Koh,23 which also considers the kinetics of secondary recrystallization in 3 pet Si-Fe, produced commercially by the Allegheny Ludlum Steel Corp. Koh covered a much larger temperature range than do either the present authors or P. N. Richards, whose work is mentioned in a footnote. Koh found an induction period (of short duration) even for isothermal anneals at 1260oC (2300°F). Koh and Dunn24 also found a change in texture during the 1260oC anneal for the same material. On the other hand, the material in coil D, according to Philip and Lenhart, underwent no sec-condary recrystallization, only continuous grain growth. The grade classifications of the four coils studied would suggest, however, that all four materials had developed the cube-on-edge or (110) [001] texture, but to varying degrees. Since no data on this are given and since watt loss depends

Jan 1, 1962

By D. Kunstelj, M. Stubicar, A. Tonejc, A. Bonefacic

A. Bonefafcic, D. Kunsfeli, M. Stubicar, and A. Tonejc The present communication is concerned with the variation of the texture in aluminum wires with die angle and temperature, at constant speed of extrusion. Experiments were carried out concurrently on refined samples, with a stated purity of 99.997 pct pure A1 and commercial samples of 99.5 pct Al. Ingots of refined aluminum samples were machined to 30-mm-diam by 150-mm-long billets. These billets were transformed to 5-mm-diam wires by drawing. The final form, suitable for examination, was obtained by extrusion through conical-face dies with a 1-mm hole diam and extrusion ratio 5:l in diam. The initial form of the commercial aluminum samples was drawn wire 5 mm in diam. These samples showed a poorly defined texture with (111) as a major and (001) as a minor component. A similar defined texture appeared in the refined aluminum samples after drawing to 5 mm diam. Conical-face dies with different angles (defined by the axis and the generating line of the cone) were used in our experiments. The values of the angles were 27, 35, 45, 57, 63, and 90 deg. The extrusion container was fitted with a heating element and controller permitting temperatures up to 600°C to be maintained within i5"C. Extrusion was performed at 250°, 300°, 350°, 400°, and 500°C at constant speed (approximately 1 mm per sec) and constant die reduction. The extrusion product was a wire 1 mm in diam and approximately 20 cm long. In order to remove the surface layer with the "conical" texture and to reduce the absorption by the X-ray examination of the samples, the extruded wire was etched to 0.22 mm in diam. Experiments were performed in the middle sections of the 20-cm-long wires. In addition to the die of l-mm hole diam, dies with a 1.5-, 0.7-, 0.6-, 0.5-, and 0.4-mm hole diam and 63-deg die angle were constructed. In our experiments we did not find in these ranges any important difference concerning the texture of the extruded wires and we continued our work solely on the 1.0-mm die. The diffracted X-rays (Cu K radiation) were recorded photographically. Diffracted intensities were measured on the (111) reflection with a microphotometer. The relative amounts of texture components were determined from the areas under the diffracted maxima. We found the texture of extruded aluminum wires to be strongly influenced not only by the temperature of extrusion and the purity of the sample but also by the form of the die. It is generally admitted that cold-drawn aluminum wires have mainly a (111) texture with a small amount of (001) component, Table I of Ref. 1. In our experiments with wires extruded in conditions represented by Fig. 1, in some cases a single (001) texture was obtained. If these wires were drawn repeatedly at room temperature, X-ray measurements revealed a duplex (001)-(111) fiber texture. Further drawings increased the (111) and decreased the (001) texture component. In Fig. 1 the percentage of material oriented with (001) parallel to the extrusion direction is represented as a function of the temperature and the die angle (a), for commercial and refined aluminum samples, respectively. From these diagrams we may draw the following conclusions. The slope of the die (a) influenced more strongly the texture at the lower rather than the higher temperatures. Again, a stronger influence was found in the case of the commercial in comparison with refined aluminum samples. In the case of the commercial aluminum samples the amount of material with (001) texture increases with increasing wire temperature in an approximately linear manner. This effect is less pronounced in the pure aluminum samples, with the exception of the die with a = 45 deg. In this case the (001) texture decreases with increasing temperature, as shown in Fig. 1. Component (001) is more pronounced in higher-purity aluminum samples. Our experiments led to the conclusion that both (001) and (111) components are essentially stable in extruded aluminum wires. As we obtained a single (001) texture starting with a sample of drawn wire in which the (001) component was very weak, our experiments revealed that the (001) component is not a remnant of the initial texture; this is in disagreement with the findings of Vandermeer and McHargue.1 We gratefully acknowledge discussions with Professor M. Paic. 1 R. A. Vandermeer and C. J. McHargue: Trans. 7MS-AME, 1964, vol. 230, p. 667.

Jan 1, 1969

By H. M. Morse

During the year of 1940, wildcat wells were drilled in 32 counties of Mississippi; 85 wells in all. These were scattered over the state from the most northern county to the southern counties and from the Mississippi River on the west to the Alabama line on the east. Yazoo County, with 19, received the largest number. The average depth of all the wells was 5333 ft. The shallowest well completed as a dry hole was in Yalobusha County, aban-doned at 1392 ft. in the Selma. The deepest well drilled was in Scott County, abandoned at 10,365 ft. in the Lower Cretaceous Paluxy. G. C. Grasty drilled the Kentucky Lumber Company No. I well, sec. 7, T. 10 S., R. 10 E., Itawamba County, to a depth of 3530 ft. and bottomed his hole in the Ordivician. Tinsley Oil Field.—In the Tinsley oil field 104 wells were completed as producers during 1940. Five producing sands have been logged with a total average thickness of I57 ft. of oil sand. One of these sands is in the Selma, three in the Eutaw, and one in the Tuscaloosa. Vaughan-Pickens Field.—The Vaughan-

Jan 1, 1941

By H. M. Morse

During the year of 1940, wildcat wells were drilled in 32 counties of Mississippi; 85 wells in all. These were scattered over the state from the most northern county to the southern counties and from the Mississippi River on the west to the Alabama line on the east. Yazoo County, with 19, received the largest number. The average depth of all the wells was 5333 ft. The shallowest well completed as a dry hole was in Yalobusha County, aban-doned at 1392 ft. in the Selma. The deepest well drilled was in Scott County, abandoned at 10,365 ft. in the Lower Cretaceous Paluxy. G. C. Grasty drilled the Kentucky Lumber Company No. I well, sec. 7, T. 10 S., R. 10 E., Itawamba County, to a depth of 3530 ft. and bottomed his hole in the Ordivician. Tinsley Oil Field.—In the Tinsley oil field 104 wells were completed as producers during 1940. Five producing sands have been logged with a total average thickness of I57 ft. of oil sand. One of these sands is in the Selma, three in the Eutaw, and one in the Tuscaloosa. Vaughan-Pickens Field.—The Vaughan-

Jan 1, 1941