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By J. F. Martin, L. M. Melnick, R. Rapp, R. C. Takacs

Recent studies on the determination of hydrogen in steel have shown that the hot-extraction method for removing hydrogen from a solid sample is preferable to its removal from a molten sample by vacuum fusion or by fusion in vacuum with tin. A number of techniques are available, however, for determining the hydrogen so extracted. They include: thermal conductivity, gas chromatography, pressure measurement before and after catalytic oxidation of the hydrogen to water and removal of the water, and pressure measurement before and after diffusion of the hydrogen through a palladium membrane. These techniques have been evaluated on the basis of initial cost, maintenance, speed and accuracy of analysis, and applicable concentration range. The results of this study showed that the palladium-membrane technique is best suited for routine use. FOR some time investigators have been concerned with the origin, form, and effect of hydrogen in steel. In such stdies', the analysis for hydrogen constitutes one of the most important phases. It is quite apparent that the results for hydrogen concentrations in a given steel are dependent on the method of obtaining the sample, storage of the sample until analysis, preparation of the sample, and analysis of the sample, including all the facets inherent in the calibration and operation of an apparatus for gas analysis. There are a number of means available for determining hydrogen. This is a critical study of some of the more common techniques in use today. In most conventional melting and casting methods, hydrogen concentrations of 4 to 6 parts per million (ppm) in steel are quite common. Because of the undesirable effects of hydrogen on steel there has been increased use of techniques such as vacuum melting,' vacuum casting, and ladle-to-ladle stream degassing, which lower the hydrogen content to levels on the order of 1 to 2 ppm. Therefore, the method used for determining hydrogen in steel must be sensitive and precise. In any analytical procedure for gases in metals there are two distinct operations—the extraction of the gas from the metal and the analysis of the extracted gas. To extract the gas from the steel, three methods have been employed: 1) fusion of the sample with graphite at high temperature; 2) fusion with a flux, such as tin, at a lower temperature; and 3) extraction of the hydrogen from the solid sample at a temperature below the melting point of the steel. Fusion with graphite is the least-acceptable method. The blank in this method is higher and more variable than in either of the other two methods. The hydrogen fraction of the total gas composition usually is between 10 and 50 pct; thus, a larger analytical error is possible. The vacuum-tin fusion4 extraction of hydrogen is probably the most rapid method in use today; the extraction time is usually about 10 min. However, with this system a bake-out of the freshly charged tin for 2 hr is necessary and a change of crucible and a charge of fresh tin are required after each day of operation whether one or thirty samples have been analyzed. In addition, frequent checks of blank rates are required since CO and Na are continually being given up by the steel samples dissolved in the tin bath. The composition of the gas in this method lends itself readily to analysis; although the hydroge concentration may fall to as low as 50 pct, more often it is above 90 pct, thus allowing a more precise analysis (because of less interference from other gases). In 1940 ewell' published the hot-extraction method for extracting hydrogen from the solid sample, comparing analysis for hydrogen extracted at 600°C with similar analysis for the gas extracted at 1700°C by fusion with graphite. Good agreement for hydrogen was obtained between these two methods, provided sufficient time was allowed for extraction at the lower temperature. carsone obtained good results in his comparison of this hot-extraction method with vacuum-tin fusion. Subsequent work by Geller and sun7 and Hill and ohnson' has shown that steel samples should be heated to at least 800°C to effect the release not only of the diffusible hydrogen but also of the "residual" hydrogen that may be present as methane. Since the rate of evolution of hydrogene9l0 depends on such factors as sample size and composition, thermal history, and extent of cold work, a fixed extraction time is not possible. Extraction times of 30 min are normal, but 2 hr are not unusual. Induction or resistance heating may be used in the hot-extraction method. With resistance heating the

Jan 1, 1964

By Daryl R. Tweeton, William H. Engelmann, Orin M. Peterson, Jon K. Ahlness, Gregory R. Anderson

The Bureau of Mines measured the geochemical changes as H2SO4 was used for in situ uranium leaching by Rocky Mountain Energy Company near Casper, Wyoming. Cores and ground water were analyzed before leaching. Water samples were taken from observation wells located between injection and production wells as the leach solution was brought up to full strength in several steps. Measurements were made of pH, Eh, temperature, conductivity, total dissolved solids, dissolved oxygen,HC03, U. V, Na, K, Ca, Mg,S04, CI, Mo, Mn, Fe, AI, Si, F, P, As, and Se. The data were gathered to assist in geochemical modeling of leaching and to study the potential environmental effects of acid leaching. Environmental considerations appear favorable. For example, the concentration of Se, a toxic element often found in uranium deposits, stayed below the EPA standard for drinking water.

Jan 1, 1979

By E. A. Slover

THE usual reverberatory system of smelting cop--1- per concentrate or calcine has for its component parts a furnace and one or two waste heat boilers. These parts are operated on a basis of compromise, since the furnace can send gas to the boilers at too high a temperature and the boilers by plugging, due to dust or slag, can place a definite limit on the amount of fuel the furnace can burn. Over the years the copper concentrate smelting furnace has had few advances in design. The simple rules of design such as the flame should wipe the bath and the speed of the gases should be reasonably low for dust carrying purposes seem to cover the main features. In the construction of the individual furnaces some innovations are always being introduced. Among these are charging so that the work of smelting is a complete bath process, the use of suspended brick arches in place of sprung arches, the use of basic brick, not only in the crucible, but also in roof and sidewalls, the use of various means to feed the charge, the use of magnetite or other heavy material to construct the hearth, water cooling of bridgewall and slag skimming bay, the smelting of raw charge instead of calcine, the use of preheated air, and possibly the use of oxygen-enriched air for combustion. But the general outlines of the furnaces have not changed much except as to size. Furnaces at Hurley As shown on Fig. 1, the furnace at Hurley is 126 ft long between the longitudinal buckstays and 32 ft wide at the skewback plates. The foundation is a concrete retaining wall with piers at intervals that go deeper into the earth. Purposely the wall at the burner end of the furnace is not backed-up as tightly as the other parts of the foundation so that movement due to expansion may take place here rather than into the boiler foundations. Within these foundation retaining walls of concrete, the earth has been removed to allow the placement of the crucible brick base inside of which a silica hearth is laid 4 ft 6 in. in depth. No expansion is left in the brick base and crucible where they are in contact with the hearth. The hearth itself is of quartzite crushed to 1 in. size with fines left in the product. An 8 in. layer is laid and tamped with paving tampers to about 6 in. in thickness. Then a layer of silica flour is spread and vibrated into the hearth. This operation is repeated until a depth of 4 ft 6 in. is occupied by the silica mass onion-skinned in layers of approximately 6 in. Before firing the entire hearth is covered with broken slag to a depth of 4 in. so that a seal may be formed on the hearth. The crucible is completely faced with magnesite chemically bonded brick while the outside, against the foundation, is made of silica brick. The side-walls are carried up with silica brick in which expansion joints are left at intervals. Above the crucible the sidewall is corbelled to form a shelf on which the charge may build up along the side-walls, see Fig. 2. The arch of the furnace is sprung 20 in. silica brick, with the longitudinal centerline horizontal the length of the furnace, and some 9 ft in the center above the bath. Both straight and wedge brick are used in the construction and a thin silica mortar is troweled for joints. After the arch under heat has assumed its permanent shape, a silica slurry is spread over the arch to fill any cracks that have formed, thus giving bearing surface to the brick and preventing dust from entering the body of the arch to act as a future fluxing agent. The uptake of the furnace slopes up to the boiler entrance where a brick pilaster divides the gas stream for the two boilers. Over this flared uptake is a suspended flat arch of firebrick. The pilaster and sidewalls are constructed of firebrick but the bottom of the uptake is lined with silica brick and fettled through holes in the roof with siliceous fettling. Close to the entrance of each boiler is a brick covered slot through which water-cooled dampers may be lowered in event of boiler trouble. These water-cooled dampers are hung permanently in position ready to be lowered when needed. Flexible hoses to follow the dampers as they are lowered are connected at all times and individual chain blocks are used to lower the dampers. A pump supplying water is started before the dampers enter the heat. Charging of the furnace along the sidewalls for some 80 ft from the bridgewall is accomplished by electric vibrating conveyors fed by belt from charge storage bins above the furnace. These conveyors

Jan 1, 1954

W. N. Triplett (Geology of the Silver-Lead-Zinc Deposits of the Avalos-Providencia District of Mexico, P. 583) was born in Tecumseh, Mich., and attended the University of Michigan and Massachusetts Institute of Technology. From 1912 to 1917 he worked for Moctezuma Copper Co., a Phelps Dodge subsidiary at Nacozari, Sonora, Mex. He served in Army as Second Lieutenant Field Artillery from 1917 to 1918 and from 1919 to 1922 returned to Moctezuma Copper Co. From 1922 to 1952 he has been with Compania Minera de Penoles, S. A., a subsidiary of American Metal Co., Monterrey, N. L., Mexico in Unit Dept. as chief geologist and at present is consulting geologist. Mining geology and operation is of particular interest to Mr. Triplett. He presented a previous paper before with M. W. Hayward entitled, "Occurrence of Lead-Zinc Ores in Dolomitic Limestones in Northern Mexico." Besides being an AIME member, he holds membership in Society of Economic Geologists. Fishing, hunting and photography are his favorite hobbies.

Jan 1, 1952

By John W. Cahn

Tile avevage value of the mean curvature of surfaces in a specimen can be precisely delermined by sitrlple measurements performed on random sections or on 1 vojectiotzs of these surfaces. For surjaces enclosing particles, the quanlity is sllown to be velated to the probable tlurrrhev ot particles intevcepted by a random platne and, under certain conditions, to the perimeter of their Projected image and to the increuse in surjace area when the particles grow. Many of the velalionsl~ips are valid for any shape or size of the particles. THE recent growth of the field of stereology or quantitative microscopy is largely the result of the discovery of a limited number of rigorously defined geometrical parameters that can be precisely measured on random sections or projections of a structure without assumption about particle shape.' Such parameters have been the volume fraction and surface area and line length in a unit volume. The present paper introduces the average of the mean curvature of surfaces in a volume, and shows that it can be rigorously measured by counting methods alone. AVERAGE CURVATURE ON A PLANE Consider a curve y = v (x) on the xy plane. The curvature Kp in the plane at any point is given by Kp = (dZy/dx2)/[1 + (dy/dx)2]3/2. The average curvature along the curve may be defined as Kp = (1/L) fKpdl |1] where dl = [(dx)' + {dy)2]1/2 is the length of an element of the curve and .(dl = L is the total length of the curve. The integral on the right-hand side of Eq. [l] will be called the total curvature, It is dimensionless and readily evaluated by substituting d = arctan (dy/dx) to give ah which is the change in direction of the tangents to the ends of the curve, Fig. 1. Hence, Kp = (1/L)(?h) [2] It can also be seen that Eq. [2] is applicable in the limit of sharp corners. Even though the curvature is infinite at a corner, f Kpdl remains integrable and equal to the change of angle. The signs of the quantities Kp and dl are arbitrary and, if the areas adjoining the curve are equivalent, there seems to be no compelling reason to fix the signs. For a closed curve, however, it becomes worthwhile to use the signs to distinguish among different types of areas or phases enclosed. For such a closed curve AO = t2r and As a convention, we shall take the direction of the integration along the curve in such a way that the area or phase under consideration (henceforth called a) is kept to the left side of the curve, Fig. 1. Then Kp is positive where the curve is concave and negative where the curve is convex. For a closed curve Ad - +2n if the curve encloses a, and Ad = —2n if the curve is surrounded by a. PLANAR SECTIONS OF THREE-DIMENSIONAL STRUCTURE OF ISOLATED a PARTICLES Consider next a planar section of a microstructure containing particles of a in a matrix. We place no restriction on shape of connectedness of these particles, and begin by considering the curvature of only the boundary between a particles and matrix' Clumps of contiguous a particles are then treated as a single a particle. The two-dimensional section will show in a unit area na simple closed curves enclosing a particles and nh closed curves of holes, in-

Jan 1, 1968

By James F. Howe

EveRy engineer and user of wire rope is desirous of information that will enable him to determine whether the performance of any particular piece of rope is satisfactory, and what conditions can be changed so as to increase the life of a rope. In most cases, it is far from easy to analyze the conditions of service and tell which is the greatest factor in determining the life of wire rope. If we start on a layout for an entirely new rope system, the task of making conditions satisfactory is simplified so far as the engineering details are concerned; but if the plant requiring wire rope is in operation, any change is likely to involve the expenditure of considerable money to replace and change over machinery that must be kept in constant operation, because a large monetary loss will result from a shutdown for even a few days. Often wire rope is kept operating under bad conditions, as the user thinks that it is cheaper and quicker to replace the rope than to make alterations in the hoisting machinery. A typical case is a metal mine operating in what is now almost the center of a large mining city, where it owns a few acres of mineral rights. It was expected that the shaft would go to a depth of 1000 ft. (305 m.), so a moderate-sized rope, about 1 1/4in. (31.7 mm.), was used on a 6-ft. drum with a 7-ft. head-frame sheave and rather short lead from drum to head sheave. This mine has gone deeper each year until it is now 2500 ft. deep and the rope speed has been increased from 1500 ft. per min. to over 3000 ft. The original rope just filled the drum in one layer, now it overwinds three layers. The original ropes were probably 6 X 19 crucible steel and lasted from 12 to 18 mo.; now, the highest grade plow steel is used, yet the average service is only about 6 mo. The cause is not hard to find. If the engineers had known at the outset what would be done with this hoist, the design would have been very different. Conditions at this mine, from a wire-rope standpoint, have gradually become worse and it is difficult to see how rope service on this hoist can be compared with the service of previous years with any fairness to the wire-

Jan 1, 1923

By James F. Howe

EveRy engineer and user of wire rope is desirous of information that will enable him to determine whether the performance of any particular piece of rope is satisfactory, and what conditions can be changed so as to increase the life of a rope. In most cases, it is far from easy to analyze the conditions of service and tell which is the greatest factor in determining the life of wire rope. If we start on a layout for an entirely new rope system, the task of making conditions satisfactory is simplified so far as the engineering details are concerned; but if the plant requiring wire rope is in operation, any change is likely to involve the expenditure of considerable money to replace and change over machinery that must be kept in constant operation, because a large monetary loss will result from a shutdown for even a few days. Often wire rope is kept operating under bad conditions, as the user thinks that it is cheaper and quicker to replace the rope than to make alterations in the hoisting machinery. A typical case is a metal mine operating in what is now almost the center of a large mining city, where it owns a few acres of mineral rights. It was expected that the shaft would go to a depth of 1000 ft. (305 m.), so a moderate-sized rope, about 1 1/4in. (31.7 mm.), was used on a 6-ft. drum with a 7-ft. head-frame sheave and rather short lead from drum to head sheave. This mine has gone deeper each year until it is now 2500 ft. deep and the rope speed has been increased from 1500 ft. per min. to over 3000 ft. The original rope just filled the drum in one layer, now it overwinds three layers. The original ropes were probably 6 X 19 crucible steel and lasted from 12 to 18 mo.; now, the highest grade plow steel is used, yet the average service is only about 6 mo. The cause is not hard to find. If the engineers had known at the outset what would be done with this hoist, the design would have been very different. Conditions at this mine, from a wire-rope standpoint, have gradually become worse and it is difficult to see how rope service on this hoist can be compared with the service of previous years with any fairness to the wire-

Jan 1, 1923

By F. R. Hensel

Up to the present time few attempts have been made to produce hard nonmagnetic materials by heat treatment of austenitic steels. The usual result has been to cause them to pass into the martensitic stage, thus destroying to a great extent the typical austenitic properties, since this involves a transition of a portion of the iron from a face-centered to a body-centered type of atomic arrangement. High-strength nonmagnetic materials such as might be provided by properly hardening austenite are required in the electrical industry for different machine parts. In Europe nonmagnetic retainer rings for restraining the end-turns of the rotor windings in turbo-alternators have been developed as a special application of high-strength austenite. In testing1 a 28,000-kva. three-phase Siemens turbo generator running at 3000 r.p.m. at full load current, the losses in the short-circuit test were 450 kw. for the magnetic ring and 286 kw. for the nonmagnetic, and the difference should be attributable to the magnetic ring. The differences in temperatures during the same test are given in Table 1 and these show the advantage of a nonmagnetic over a magnetic retainer ring.

Jan 1, 1931

By Evan Just

DIRECT subsidies for mine production in this country began as an outgrowth of wartime 'price regulation. The price-fixing authorities realized that the volume of production to be required from domestic copper, lead, and zinc mines would invoke costs of production considerably higher than the established ceiling prices. Accordingly, beginning Feb. 1, 1942 the Premium Price Plan was set up, which undertook to pay premiums to mines for production in excess of quota, of 5¢ per lb of copper and 2Y4¢ per lb of zinc or lead. Quotas, except for small mines, were initially established at the average rate of production in 1941, but were later reduced arbitrarily on an individual basis. Subsequently, additional "B" premiums were set for lead and zinc of 2Y40 per lb and a further "C" zinc premium of 2%¢. Additional copper premiums were negotiated on an individual basis, mainly with small mines. Quotas under each of these successive categories were the production obtained at the next lower premium level. In other words, under ceiling prices of 12¢ for copper, 6,14¢ for lead, and 83¢ for zinc, it was possible for high-cost operations to receive prices plus premiums of 17¢ or more for copper, 12¢ for lead, and 16% 0 for zinc on a portion of their production. On the other hand, some of the larger operators received only slight premiums and in at least one instance none at all. The average price plus premium for copper was 12.25¢ in 1942 and rose to 13.65¢ in 1945. That for lead was 6.99¢ in 1942 and 8.73¢ in 1945, and for zinc it was 9.06¢ in 1942 and 11.200 in 1945.

Jan 1, 1948

By H. D. Outmans

The author applies the theory of hydrodynamic stability to fluid flow in porous media and concludes that the displacement of miscible liquids is stable if the stability coefficient, as defined by Eq. 19.2 or Eq. 27.0, is positive. The conclusion is invalid, however, since it is based on a faulty argument. To demonstrate this, the reader is referred to Eqs. 4.1 through 4.5 of the paper which describe, in differential form, the first-order disturbances c, u, v, w and p. In these same equations, cx, cz, gl, g3 and are functions of the stable concentration c. This concentration c is known and depends on x, z and t (the author assumes cy = 0). It follows that cx, cz, gl, g3 and µ are also functions of x, z and t. With this in mind, we turn to Eqs. 8.1 through 8.5 which were derived from Eqs. 4.1 through 4.5 by substituting Eq. 6.0. The significance of this substitution is that the author thereby limits the solutions of Eqs. 4.1 through 4.5 to equations of the form of Eq. 6.0. Eqs. 8.1 through 8.5 represent an infinite linear system with five unknowns: c, u, v, w and p. The coefficients cx, cz, gl, g3 and µ in this system are known at each point and at each instant; the coefficients containing derivatives of f are unknown. If this infinite linear system in c, u, v, w and p is to have a nontrivial solution, then it is indeed necessary (as the author states) that the determinant of the coefficient matrix of Eqs. 8.1 through 8.5, i.e., ( A 1, be equal to zero. This condition, however, is not sufficient. A non-trivial solution exists if, and only if, the rank of the coefficient matrix of the entire infinite system is smaller than five. In other words. all minors of order five must vanish and only if all the coefficients in Eqs. 8.1 through 8.5 are constant is this equivalent to the condition |A| =0. Constant coefficients means that gl, g3 and µ, for instance, are constant; and, since they depend on c it follows that c must be constant. We conclude that the condition I A I = 0, on which the author bases his calculations, is necessary and sufficient for a nontrivial solution only if the concentration c is constant. In other words, the author does not investigate the stability of a miscible displacement but, rather, only the stability of the flow of a homogeneous liquid. Using the initial condition and the fact that the coefficients are constant, we find

By R. I. Jaffee, C. M. Craighead, G. A. Lenning

THERE has been considerable discussion among A metallurgists and others interested in the development of titanium alloys as to the nature of the fine line markings which appear in the microstruc-tures of unalloyed titanium and a titanium alloys. These markings have been variously called x phase, etching pits, and twins. Figs. 1 to 3 show typical examples of the line markings as they appear, respectively, in high purity iodide titanium, commercial purity titanium rod, and a high purity a alloy containing 0.2 pct N. The commercial purity titanium sample, shown in Fig. 2, contains both line markings and some spheroidal retained-ß phase. The ß phase seen in this micrograph should not be confused with the line marking, since it originates from the iron present as an impurity in the sponge metal. It will be noted that the line markings seem to have a definite orientation pattern with respect to the grains and in titanium noticeably resemble the precipitation occurring in artificially aged high purity Al-Cu alloys. This similarity led to the hypothesis that the line markings observed in titanium and a titanium alloys resulted from precipitation of some unknown phase. With the work of Hägg1 and McQuillan2 as background, there was little reason to suspect hydrogen of being responsible for the line markings. Hagg reported that up to 33 atomic pct H was soluble in a titanium, and McQuillan reported an a solubility of up to 8 atomic pct. Furthermore, McQuillan examined metallographically a 5.1 atomic pct H alloy quenched from 300°C and stated that the structure appeared to be a single-phase a solid solution. Line markings have been observed frequently and were first noted by Jaffee and Campbell3 in 1949. They did not observe them in vacuum-annealed titanium and a Ti-O and Ti-N alloys, but did observe them in Ti-H alloys containing 0.25, 0.5, and 1 atomic pct H. They stated that it was doubtful that the markings were a second phase based on hydrogen, because 1 atomic pct was far from the accepted solid solubility of hydrogen in titanium. Finlay, Resketo, and Vordahl,4 in 1950, concluded that the markings were a true second phase as a result of observations on their etching characteristics. Anderson5 Commenting on these markings in titanium was inclined to associate them with hydrogen, but was loath to call them titanium hydride, because of the reported high solubility of hydrogen. Work at Battelle Memorial Institute for the Navy Bureau of Aeronautics," done concurrently with the work described in this paper, provided information on the experiment converse to that described by Jaffee and Campbell in 1949. This work showed that the amount of line markings in unalloyed titanium could be decreased by vacuum annealing at elevated temperature. It was suggested that this was the result of removal of hydrogen; previously, the data of Jaffee and Campbell9 howed that the markings appeared when hydrogen was added. Recent work at Battelle for the Ordnance Corps, Department of the Army, which is described here, now establishes the identity of the markings as a titanium hydride phase. A sample of high-purity titanium rod 1/4 in. diam, 0.009±0.001 wt pct H (0.43 atomic pct), Fig. 1, was resistance heated in a 0.05 micron vacuum for 41/2 hr at 1500°C. During the early states of heating, the pressure increased to 150 microns, indicating that gases were being evolved. After cooling in vacuum, the iodide titanium rod was analyzed for hydrogen. Vacuum-fusion analysis showed 0.0006 ±0.0003 wt pct H (0.03 atomic pct) to be present.* Metallographic examination of the vacuum-annealed rod showed only a transformed ß structure. There was no evidence of fine line markings, Fig. 4. A section of this vacuum-annealed rod was cold rolled to 0.040 in. thick sheet and annealed for 1 hr

Jan 1, 1953

By John P. Ashby

Mine production blasting is a process of destruction of rock masses in order that ore may be extracted. Many open pit operations are faced with the apparently conflicting requirements of providing large quantities of fragmented rock for the processing plant and of minimizing the damage inflicted upon the surrounding pit slopes. A reasonable compromise between these two conflicting demands may often be found by means of simple engineering of production blasts. Many operations tend to rely too heavily upon traditional wall control techniques to alleviate a problem already created by the production blasts. Various production trends including use of larger blastholes and patterns have tended to aggravate the situation. These practices only serve to emphasize the need for engineered improvements. Central to blasting engineering is the process of systematic trial and evaluation. Changes to the blasting system should be made singly, starting with the simplest. This paper discusses simple changes involving drill pattern control, effective use of blastholes and explosives, adequate delaying including use of down-the-hole sequential techniques, effective utilization of free faces, and avoidance of "choked" situations. By directing explosive effort where it is needed, such changes generally result in a significant improvement of slope conditions and of production blasting cost and performance.

Jan 1, 1983

By Orville R. Lyons

THE Russellton preparation plant of Republic Steel Corp., located north of Pittsburgh, Pa., prepares 395x0-in. Thick-Freeport coal by means of a 13-ft 6-in. diam Chance cone and 16 No. 7 Deister tables. The plant feed ranges between 370 and 410 tons per hr, of which approximately 31 pct is 1/4xO-in. size, and the plant reject ranges between 14 and 16 pct of the feed.

Jan 6, 1953

By W. A. Backofen, A. T. English

The kinetics of re crystallization were determined metallographically for a 3-1/4 pcl Si-Fe rapidly compressed at temperatures of 710° to 911°C, and held for various times at the working temperature. As in re crystallization following cold wwk, the time for re crystallization was reduced by increased temperature and strain. Nucleation occurred chiefly at grain edges, although other pre-existing interfaces, notably inclusions, also served as nucleation sites. The importance of intragranular nucleation to grain refinement in hot working is pointed out, together with some possible techniques by which nucleation might be induced within the grains. The observed isothermal growth rates are quite accurately described by the equation G = 4 x 10-'/t (cm per sec), independent of temperature and strain at all but the shortest times. Changes in G during recrystalliza-tion can exceed two orders of magnitude. It is argued that release of stored energy associated with lattice defects cannot adequately explain the time dependence. A suggested alternative involves processes of solute segregation and desegregation in the unrecrystallized matrix and at the moving boundary, respectively. EFFORTS to improve hot-working practice are hampered by an incomplete understanding of the fundamental metallurgy involved. Research directed at establishing the required basic foundation falls into two categories, the first concerned with measurement of mechanical properties under the conditions of high temperature and strain rate which characterize such processing, the second focused on structure and its relation to the deformation conditions. Rossard,' Rossard and Blain,2 and Hardwick and Tegart have conducted many high-speed, high-temperature torsion tests on various metals. One of their objectives was interpretation of stress-strain curves in terms of the structures of specimens rapidly quenched following interruption of twisting. They showed that appreciable hardening occurred in the early part of the test, and that this hardening reflected the concurrent development of an increasingly dense substructure within the grains. The detailed nature of this substructure was observed to depend on the ease of polygonization which, at least in fcc metals, varies with the stacking-fault energy.= By holding specimens after interruption but before quenching, the nucleation and growth of new grains could also be studied. Some success has been realized in relating the microstructure of hot-rolled steel to its temperature:strain rate:strain history with such testing.' The same general observations have been made by others investigating rolling4f5 and drop-hammer forging.~-~ Incident to these experiments, some efforts were made to determine the kinetics of re-crystallization as well as the velocity of the migrating boundaries. The results have been largely qualitative, owing to difficulties of interpreting hardness measurements5 and microstructures. The work described here was undertaken to obtain more quantitative information from tests on a material having suitable metallographic properties, and, in this way, to provide further insight into the fundamentals of this practically most important kind of deformation processing. I) MATERIALS AND EXPERIMENTAL TECHNIQUES Materials. Electrolytic etching of a Si-Fe alloy reveals dislocations and substructure in unrecrystallized grains.8'9 This unique characteristic makes possible a precise determination of the extent of recrystallization. For that reason, it was the material selected for all experiments in the present work. The two particular alloys that were used are identified in Table I. A major difference between "A" and "B" is the number of inclusions, as noted in the table. Most of the experiments were made with material "A". It was received as hot-rolled plate 1 in. thick, sawed to 2-in. widths, hot-forged at 1200°C to 5/8-in. rounds, and finally annealed in a mechanical vacuum at 1000°C for 24 hr. The result was substructure-free grains of mean diameter 0.05 cm.*

Jan 1, 1964

By F. Rosenblum

An on-stream particle size analyzer (PSA) based on the sedimentation principle has been developed to the commercial prototype stage and tested at a concentrator. The current instrument gives a direct reading of the weight % finer than any two sizes, although the capability exists for providing a complete size distribution through the sieve and sub-sieve range. The readings obtained at intervals of about 10 minutes are derived from 0.5-L samples of slurry cut from the monitored stream. The accuracy of the PSA meets the requirements of process control.

Jan 1, 1984

By Carleton C. Long, George F. Weaton

Two years ago the general features of the St. Joseph Lead Company's zine-smelting process were described.' At that time the discussion was limited to a description of the production of high-purity electrothermic zinc oxide. The present paper will describe the commercial production of electrothermic zinc metal. Since a fairly complete description of the plant of the Josephtowlz smelter was given in the earlier paper, the brief recapitulation given here will be limited to mention of additional equip-ment recently installed and a bare outline of the preparatory process. The raw material is zinc sulphide concentrate received from the company's mines in St. Lawrence County, New York. An average dry-weight analysis of this material is: Zn, 58.28 per cent; Pb, 0.56; insoluble, 1.6; SiO², 1.12; Fe, 6.4; CaO, 0.47; MgO, 0.27; S, 31.9; Cd, 0.1; Cu, 0.06; Mn, 0.24. Moisture content is usually about 3 per cent. Three 21-ft. 6-in. diameter, 12-hearth Nichols-Herreshoff furnaces roast the coacentrate to a calcine of average conlposition (first 10 months of 1938): Zn, 67.69 per cent; Pb, 0.06; insoluble, 1.75; SiO², 1.26; Fe, 7.24; CaO, 0.47; MgO, 0.36; S, 1.88; Cd, 0.1; Cu, 0.07'; Mn, 0.27. The sulphur dioxide gas, after passing through a waste-heat boiler, proceeds through a recently redesigned low-resistance gas-purification assembly to the contact sulphuric acid plant, of which the capacity is 200 tons of concentrates per day. The calcine is mixed with a portion of returned furnace residues and sintered on 42-in, by 44-ft. Dwight-Lloyd sintering machines, gas-fired. Wind-box gases pass through air coolers before filtering in a 1440-bag Dracco unit, and thence to stack. The Dracco fume is mixed with Cottrell dust, from roaster gas cleaning, and sent to the leach plant, where it is roasted (SO² to acid plant) and leached with sulphuric acid to recover, as end products, lead sulphate, zinc sulphate and cadmium.

Jan 1, 1943

By George F. Weaton, Carleton C. Long

Two years ago the general features of the St. Joseph Lead Company's zine-smelting process were described.' At that time the discussion was limited to a description of the production of high-purity electrothermic zinc oxide. The present paper will describe the commercial production of electrothermic zinc metal. Since a fairly complete description of the plant of the Josephtowlz smelter was given in the earlier paper, the brief recapitulation given here will be limited to mention of additional equip-ment recently installed and a bare outline of the preparatory process. The raw material is zinc sulphide concentrate received from the company's mines in St. Lawrence County, New York. An average dry-weight analysis of this material is: Zn, 58.28 per cent; Pb, 0.56; insoluble, 1.6; SiO², 1.12; Fe, 6.4; CaO, 0.47; MgO, 0.27; S, 31.9; Cd, 0.1; Cu, 0.06; Mn, 0.24. Moisture content is usually about 3 per cent. Three 21-ft. 6-in. diameter, 12-hearth Nichols-Herreshoff furnaces roast the coacentrate to a calcine of average conlposition (first 10 months of 1938): Zn, 67.69 per cent; Pb, 0.06; insoluble, 1.75; SiO², 1.26; Fe, 7.24; CaO, 0.47; MgO, 0.36; S, 1.88; Cd, 0.1; Cu, 0.07'; Mn, 0.27. The sulphur dioxide gas, after passing through a waste-heat boiler, proceeds through a recently redesigned low-resistance gas-purification assembly to the contact sulphuric acid plant, of which the capacity is 200 tons of concentrates per day. The calcine is mixed with a portion of returned furnace residues and sintered on 42-in, by 44-ft. Dwight-Lloyd sintering machines, gas-fired. Wind-box gases pass through air coolers before filtering in a 1440-bag Dracco unit, and thence to stack. The Dracco fume is mixed with Cottrell dust, from roaster gas cleaning, and sent to the leach plant, where it is roasted (SO² to acid plant) and leached with sulphuric acid to recover, as end products, lead sulphate, zinc sulphate and cadmium.

Jan 1, 1943

Texture Transition in Ordered CuAu, by E. A. Starke, Jr., J. C. Ogle, and C. J. Sparks, Jr., Trans. TMS-AIME, 1969, vol. 245, pp. 169-70. pole figures should have had two parts not one. On the Estimation of Oxygen Absorption by Continuous Molten Metal Streams, by J. Szekely, Trans. TMS-AIME, 1969, vol. 245, pp. 341-44.

Jan 1, 1970

By A. Steiner, K. L. Komarek

Activities of aluminum in solid Ni-A1 alloys have been determined between 20 and 60 at. pet Al and 1200" and 1400°K by an isopiestic method in which nickel specimens, heated in a temperature gradient, are equilibrated with aluminum vabor in a closed all-alumina system. The activity of aluminum shows a strong negative deviation from Raoult's law at low concentrations but increases by three orders of magnitude within the ß(NiAl) phase. The partial molar enthalpy and entropy of mixing are negative. Using Wagner and Schottky's theory of ordered compounds, a degree of disorder of 4 x 10 -4 for NiAl and 1.25 X 10-2 for FeAl has been calculated THE Ni-A1 system has been studied by a great number of investigators, and the results, as far as the phase diagram is concerned, have been compiled by Hansen.1 The phase boundaries from 0 to 50 at. pet Ni are well-established. At higher nickel contents the boundaries are still in dispute and an additional phase, A12Ni3, has been reported.' The phase diagram is dominated by a very stable high-melting compound, NiA1, with a relatively wide range of homogeneity. Heats of formation of solid alloys have been determined calorimetrically by Oelsen and Middel3 from 20 to 95 at. pet Ni and by Kubaschewski4 from 25 to 80 at. pet Ni. According to the most recent compilation5 no other thermodynamic investigations have been reported for the Ni-A1 system. Due to the corrosive nature and the low vapor pressure of aluminum, a method has been employed for determining activities of aluminum which was previously developed for the Fe-A1 system.= Nickel specimens, heated in a closed evacuated alumina system in a temperature gradient, were equilibrated with aluminum vapor from a source within the system kept at constant temperature. After complete equilibration the specimens were analyzed and activities calculated from the known vapor pressure of aluminum. APPARATUS AND EXPERIMENTAL PROCEDURE Materials. The nickel specimens were made from wafers of electrolytic nickel (International Nickel Corp.) of 99.99 pet purity which were rolled to a 0.001-in.-thick foil by Driver-Harris Co. and to a 0.005-in.-thick sheet in our laboratory. The aluminum (Aluminum Corp. of America) had a purity of 99.99+ pct. The alumina tubes and crucibles were made of impervious recrystallized alumina with an alumina content of 99.7 pet (Triangle RR, Mor-ganite Inc.). Experimental Procedure. Annular specimens were punched from the sheet, the punching burrs removed, and the specimens degreased in carbon tetrachloride and acetone and weighed on a micro-balance to within an accuracy of ±0.01 mg. The specimens were positioned with alumina spacers along an alumina tube, and the positions measured. Aluminum metal was machined into cylindrical shape, and placed into an alumina crucible. The tube with the specimens was then inserted into a hole drilled into the aluminum metal. An alumina tube with its closed end at the top was slipped over the specimens so that its lower end fitted snugly into the alumina crucible. The assembled reaction tube was inserted into a mullite tube with a water-cooled brass head which had an opening for a quartz thermocouple protection tube and a metal-to-glass connection to a conventional vacuum system. A Pt-Pt 10 pet Rh thermocouple could be raised and lowered in the quartz tube which was placed along the outside of the alumina reaction tube. The mullite tube was heated by two separately controlled resistance-tube furnaces so that in the experimental temperature range an over-all temperature gradient of approximately 150o to 250°C could be imposed on the reaction tube. The position of the mullite tube was adjusted so that the surface of the aluminum metal was always at the temperature minimum. The reaction tube was thoroughly evacuated before and during slowly heating the assembly up to the melting point of aluminum. A pressure of less than 2 µ (Hg) was maintained during an experiment. Once the aluminum had melted, it isolated the contents of the alumina tube from the surroundings. Several times during an experiment the temperature gradient was carefully measured. An experiment lasted from 3 to 6 weeks and it was terminated by air cooling the evacuated mullite tube. For further details of the experimental procedure the paper on the Fe-A1 system6 should be consulted.

Jan 1, 1964