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By R. L. Stephenson

The effect of fabrication variables on the creep-rupture properties of TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C), Cb-TZM [columbium-modified TZM (7140-1.5 pct Nb-0.5 pct Ti-0.8 pct Zr-0.05 pct C)], and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C) has been studied at 982º. 1093º, 1204º, and 1315°C for rupture times up to 1000 hr. The creep tests were performed in vacuum creep furnaces, employing cold-trapped oil-diffusion pumps, operating at pressures 2 X 10-7 tory. After-test chemical analyses showed no significant changes in interstitial content. The creep-rupture properties of TZM, fabricated according to current mill practice, were determined in the stress-relieved and in the re crystallized conditions to provide control data. Specimens of TZM, Cb-TZM, and TZC fabricated according to each of two experimental fabrication schedules were then tested. The schedules differed in terms of in-process annealing temperatures and warm -working temperatures. The data make several conclusions evident. Fabrication variables do indeed have a profound effect on the long-time creep-rupture properties of molybdenum alloys. Strengths of these alloys compare very favorably with those of other refractory metal alloys in the temperature range studied. FOR several years we have been engaged in the evaluation of the creep-rupture properties of promising refractory metal alloys. We consider the determination of these properties to 1000 hr at several temperatures necessary for a valid comparison. Such an evaluation indicated that the creep strengths of Mo-0.5 pct Ti and TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C) compare favorably with those of other refractory metal alloys. Tensile and recrystallization data of other investigators1,2 show an effect of fabrication variables. More specifically, those fabrication schedules which produce high strength through work hardening exhibit the least thermal stability. A similar conclusion was reported by perkins3 for Cb-TZM. This would lead one to expect that, in terms of creep, those materials showing higher strength at short times and low temperatures would exhibit lower strength at long times and high temperatures. If these expectations were fact, a substantial improvement could be made in these alloys by optimizing their fabrication schedule in terms of their anticipated service temperature. We therefore undertook a study of the effect of fabrication variables on the long-time creep properties of TZM, Cb-TZM (Mo-1.5 pct Cb-0.5 pct Ti-0.08 pct Zr-0.05pct C) and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C). MATERIALS All materials used were supplied by the Climax Molybdenum Co. of Mich. Our original intention was to test the same heat of each alloy in different conditions. Fabrication difficulties prevented this; however, heats with nearly identical analysis were selected. The compositions of the materials used are listed in Table I. All materials were supplied in the

Jan 1, 1970

H. W. Turner, San Francisco, Cal. (communication to the Secretary*): This excellent paper apparently represents the results of extensive observation and experience among the mines of the Mother-Lode, but I strongly question its relegation of the dioritic intrusions to the period of fissuring and ore-deposition. The dioritic rocks referred to are evidently those areas represented by Ransome in the Mother-Lode folio1 as meta-diorites, and, as he says, are merely basic facies of the great granodiorite batholite of the Sierra Nevada. If followed downward I venture to predict that these meta-diorite areas would be found to connect with the great batholite, and to be in fact mere apophyses of it. I see no reason for supposing that these apophyses were intruded into the Mother-Lode slates at a period later than the intrusion of the granodiorite in general. The period of fissuring was subsequent to this intrusion; the basic granodiorite or quartz-diorite areas of the foot-hill region are themselves fissured extensively; and the fissures were filled with quartz, apparently during the same general period of the formation of the Mother-Lode veins. Prichard and Ransome2 both refer to the deposition of quartz in the same lode at different periods resulting from a reopening of the fissures. Some time since, I saw in the stopes of the

Jan 1, 1904

By A. F. Baker, E. R. Palowitch, A. W. Deurbrouck

As air-pollution regulations become increasingly more stringent, increased significance is being placed on the amount of sulfur present in coals used for steam generation. These regulations are aimed at minimizing the pollution of the atmosphere with noxious gases such as the sulfur oxides that are formed and emitted when coal is burned. Two meet these future requirements, a definite need exists to reduce the sulfur content of some of the coals used for steam generation. Reducing pyritic sulfur involves liberating the pyrite from the coal and then removing it. The specific gravity of pyrite is high (5.0) compared to that of coal (about 1.2, mineral-free), and standard coal-washing devices, such as wet concentrating tables, will efficiently remove pyrite particles larger than about 100 mesh. Particles below this size will be entrained in the table water and will be carried into the clean coal product. Techniques such as froth flotation are of little benefit for pyrite reduction because the flotation characteristics of pyrite are similar to those of coal.

Jan 6, 1966

By J. L. Tokich, A. R. Troiano

INTRODUCTION SINCE 1921, when Hull' discovered that cobalt can exist in the face-centered cubic and hexagonal close-packed modifications, the transitions that occur in cobalt have been extensively studied. It is generally agreed that on heating the hexagonal lattice changes to the cubic structure at temperatures ranging from 400 to 500°C although considerable doubt exists as to the exact temperature. Data concerning the temperature of the transformation on cooling are much less concordant and their interpretation has not been satisfactory. The study is further complicated by the fact that many investigators have reported the existence of a high temperature allotropic change in the range 850 to 1020°C, at which the cubic lattice reverts to the hexagonal modification. The transition on cooling, which has been reported as occurring at various temperatures from approximately 400 to 100°C, is of particular interest. Troiano and Greninger2 have recently suggested and considered the possibility of allotropic transformations occurring in pure metals by a shear-type, diffusionless (martensite) transformation. The case of cobalt was specifically discussed and certain observations of previous investigators evaluated in terms of this type of transformation. Table 1 briefly outlines the methods and results of previous investigators of the transformation temperatures of cobalt. MATERIALS AND METHODS The major portion of this investigation was performed with cobalt sheet containing a total of 0.2 pct impurities with carbon present to the extent of 0.1 pct. After melting in an induction furnace under an atmosphere of hydrogen, the carbon content analyzed 0.03 pct. Some observations were repeated with hydrogen reduced cobalt compresses analyzing 99.9 pct pure. No significant variations in results were observed employing the as-received sheet, the remelted stock, or the cobalt compresses. Filings for X ray diffraction analysis were sealed in evacuated glass ampoules. Pyrex glass tubing was used for temperatures below 600°C and for higher temperatures clear fused quartz was satisfactory. After appropriate heat treatment at various temperatures, the specimen ampoules were furnace cooled, air cooled or quenched by crushing under distilled water. This allowed a range of cooling velocities from less than one degree C per sec to greater than 1,000°C per sec. X ray diffraction patterns were taken with a Debye camera and filtered characteristic cobalt K-alpha radiation. The proportion of the existing phases was roughly approximated by visual examina-

Jan 1, 1948

By J. L. Tokich, A. R. Troiano

Since 1921, when Hull1 discovered that cobalt can exist in the face-centered cubic and hexagonal close-packed modifications, the transitions that occur in cobalt have been extensively studied. It is generally agreed that on heating the hexagonal lattice changes to the cubic structure at ternperatures ranging from 400° to 500°C although considerable doubt exists as to the exact temperature. Data concerning the temperature of the transformation on cooling are much less concordant and their interpretation has not been satisfactory. The study is further complicated by the fact that many investigators have reported the existence of a high temperature allo-tropic change in the range 850 to 1020°C, at which the cubic lattice reverts to the hexagonal modification. The transition on cooling, which has been reported as Occurring at various temperatures from approximately 400 to 100°C, is of particular interest. Troiano and Greninger2 have recently suggested and considered the possibility Of allotropic transformations occurring in pure metals by a shear-type, diffusionless (martensite) transformation. The case of cobalt was specifically discussed and certain observations of previous investigators evaluated in terms Of this type of Of Table 1 briefly outlines the methods and results Of previous investigators Of the transformation temperatures of cobalt. Materials and Methods The major portion of this investigatioll was performed with cobalt sheet containing a total of 0.2 pet impurities with carbon present to the extent of o,I pct. After melting in an induction furnace under an atmosphere of hydrogen, the carbon con. tent analyzed 0.03 pct. Some observations were repeated with hydrogen reduced cobalt compresses analyzing 99.9 pet pure. No significant variations in results were observed employing the as-received sheet, the remelted stock, or the cobalt compresses. Filings for X ray diffraction analysis were sealed in evacuated glass ampoules. Pyrex glass tubing was used for temperatures below (600°C and for higher temperatures clear fused quartz was satisfactory. After appropriate heat treatment at various ternperatures, the specimen ampoules were furnace cooled, air cooled or quenched by crushing under distilled water. This allowed a range of cooling velocities from less than one degree C per set to greater than 1,0oo°C per sec. X ray diffraction patterns were taken with a Debye camera and filtered characteristic cobalt K-alpha radiation. The of of the existing phases was roughly approximated by visual examina-

Jan 1, 1949

By John F. Abel

"The most conservative persons I ever met are college undergraduates." Woodrow Wilson said that in 1905. No one is saying anything like it today. Chaos on the campus was a cliche of the sixties. Since 1905, education has expanded in every direction. Many more people are being educated for much longer periods of time. The school-leaving age has risen from 14 years to 20 years, on an average. Many are in school until after their 25th birthday. On the surface this situation appears all to the good. Our technical society needs a massive yearly infusion of semitrained (or educated, if you prefer) new blood. The efficiency of our economy and our standard of living are tied to high individual productivity which can be achieved only with an educated work force. Our democratic institutions are said to be founded on an educated electorate.

Jan 1, 1970

By S. E. Haszko

SEVERAL new XGa2 intermetallic compounds, Table 1, where X is a rare earth, having the AlB, structure were prepared as part of a continuing study of the magnetic and structural properties of rare-earth alloys.' In this note, the crystallographic results of these compounds are presented. Chart, Eq. 121 for the data in Fig. 1 can be adequately represented by The corresponding standard free-energy change is AF; = -4.576 T log K = -20,900 + 10.20T [5I At low nitrogen concentrations the ratio of mole fraction to weight percentage is a constant so that the mole fraction X of nitrogen is given by X = 0.0392 [%NJ. At low values of X, the activity and the concearation approach each other, hence K, = 0.0392 K,, where K, is expressed in terms of the mole fraction of nitrogen. Hence Eqs. [4]. and [5] become

Jan 1, 1962

By Thomas T. Read

THE official title of our topic for today is "Resources of Metals and Other Strategic Minerals," but in accepting the invitation to open this discussion I claimed the privilege of being allowed to talk about problems other than resources for the two reasons that a great deal has already been said about resources and because we can never discuss them with the degree of certainty that an engineer likes. Resources are uncertain for many, reasons. One is that we do not know what is in the earth. It is four thousand miles to its center and although oil wells 1 ½ miles deep are becoming common and engineers are now talking of drilling holes 2 miles deep, even when they do they will have advanced only one two-thousandth part of the total distance. Only a relatively few mines are over a mile deep as yet. We know certainly that it is comparatively expensive to work at such great depth, but it would be a very foolish man who would assert it will be' impossible, one or two hundred years from now, for engineers to obtain from great depths mineral supplies that are now being obtained at or near the surface. As long as- I can remember I have been hearing that our petroleum resources were in imminent danger of speedy exhaustion, and yet the yearly output is now of the same order of magnitude as the total resources were once estimated, with ' the cry of over-production the loudest it has ever been. Tapping progressively deeper and deeper sources of supply, has produced this result. Even in the thin layer that we are now working much-exploration still remains to be done. .

Jan 1, 1929

By F. C. Bond

Since the Third Theory of Comminution was presented eight years ago (I) it has found increasing use in crushing and grinding problems. The practical utility of its wok index equation is quite generally acknowledged (2). However, its theoretical basis has been questioned in at least three technical articles (3) (4) ('). The purpose of this paper is to present experimental proof that it is scientifically correct. Particles under compressive stress are strained and deformed. They absorb strain energy, and when this locally exceeds the breaking strength, a crack tip forms. The surrounding strain energy flows to the crack tip, which rapidly extends and splits the rock, releasing the strain energy as heat. The initial energy flow causes additional crack tips in highly strained areas. If the compression is rapidly applied by impact, crack tips may form before the strain energy has reached equilibrium in the particle, thus decreasing the total work input required for breakage. The energy necessary to break is essentially the energy necessary to produce crack tips, since the energy necessary to extend the cracks to breakage is already present as strain energy in the deformed particles. After breakage nearly all of this energy appears as heat. The crack length cannot be measured directly. However, in particles of regular and similar shape the crack tip length is considered as equal to the crack depth, or crack extension necessary to break, so that the crack length equals the square root of one-half of the surface area. The Third Theory states that the useful work done in crushing and grinding is directly proportional to the total length of the new cracks formed. It can be confirmed by showing that a constant work input produces a constant length of new cracks when reducing the same material to different product sizes. This is done in the present paper on a wide variety of material. The constant work input was supplied by one revolution of the 12" x 12" laboratory ball mill used in making grindability tests by the Allis-Chalmers method (12) (13) The new crack lengths produced per mill revolution were measured from all available grindability test results at 28, 35, 48, 65, and 100 mesh on fifteen different ores, and were found to remain substantially constant for each ore at all mesh sizes. A new technique is used for the measurement of crack lengths. Size distribution plots of the mill feed and product are made by the Third Theory method (9) and the crack lengths are obtained from these plots by the procedure described in the present paper. The energy input required to produce a unit length is of fundamental importance in the size reduction of brittle solids. The crack length Cr is expressed in centimeters per cubic centimeter of solid material. It bears a definite relationship to the external surface area of the crushed or ground solid. A uniform particle shape must be assumed before the surface area and crack length can be evaluated. In this paper it is assumed that the relationship between the surface area and the particle volume of a particle d microns in diameter is the same as that of cube d microns on a side. The external surface areas of particles with a cubical breakage probably agree approximately with this rule, and correction factors can be applied when physical measurements of the surface areas are available for comparison. However, the assumption of equivalent cubes has been found satisfactory for most calculation purposes. Assuming equivalent cubes, one cubic centimeter of particles d microns in diameter will have a crack length Cr of v30.000/d centimeters, and a surface area of 60,000/d square centimeters. The specific crack length is thus equal to the square root of one-half the specific surface area. Where Sa is the surface area in square centimeters per gram and Sg is the specific gravity of the ground solid, then Cr = vSg . Sa/2 = 173.2/ vd (1)

Jan 1, 1961

By R. S. Sherwin

The extractive metallurgy of primary aluminum from its ores is discussed with special attention to the production of alumina from high grade ores by the Bayer process, including differences between American and European practice and a brief description of some processes for lower grade ores and the electrolytic reduction of the oxide to aluminum. METALLIC aluminum is not found in nature, but the oxides, hydroxides, and especially the silicates are plentiful. The estimated percentage of in in the crust of the earth is about 8 pct while that of iron is about 5 pct. By far the larger portion of this is combined with silica in the form of various clay minerals and igneous silicate rocks. From the point of view of extractive metallurgy of aluminum, these are low grade ores while the better qualities of bauxite are the high grade ores. There have been various definitions of bauxite but perhaps the best definition at the present time is that bauxite is a rock or earth commonly used as an ore of aluminum or its salts in which the aluminum is present predominantly as a hydrate or a mixture of hydrates and hydrous oxides. It contains varying amounts of oxides of silicon, iron, and titanium and traces of compounds of some of the less common elements. The silica is mainly combined with alumina as clay or clay minerals which are hydrous aluminum silicates, although a part of it may be present as quartz sand. On the American continents, the alumina is mainly present as gibbsite, Al2O3 . 3H2O, and the same may be said of the best known deposits of the Dutch East Indies and some of the deposits in India. In France and other countries in Europe as well as in Africa, the alumina is present mainly as boeh-mite, A12O3 . H2O, but in some of these deposits it is mixed with minor amounts of gibbsite. Some other deposits, such as those in the islands of Haiti and Jamaica, evidently contain two or more hydrates or hydrous oxides of alumina in varying proportions. Perhaps the main portion of the alumina may be present as gibbsite and boehmite with the proportion between the two varying rather widely. In the silicate minerals, including clay, the alumina is chemically combined with silica and has not been separated satisfactorily by mechanical or physical ore-dressing methods. Low grade bauxites are mixtures of hydrates, usually gibbsite or boehmite, with clay, iron oxides, etc. In some low grade bauxites, it is possible to separate a portion of the gibbsite or boehmite, which may be present as relatively hard and coarse particles, from soft or finely divided clay minerals by log washing or similar methods. This has been applied to the product of some mines or parts of them, but on other ores it is not applicable. In some cases the gibbsite or boehmite is almost as fine and soft and of nearly the same specific gravity as the clay minerals so that washing and gravity separations are not successful. The iron oxide, the clay minerals, and a part of the titanium minerals are often so finely dispersed in the ore that any of the physical mineral separation methods, including separations by gravity, particle size, flotation, and electrostatic or magnetic separation, have not been commercially SUCCESSFUL except on relatively small lots of ore. For these reasons, the only available methods of separation on the general run of ores have been methods which would be classed as chemical rather than physical or mechanical separations. Aluminum oxide can be reduced by carbon at temperatures above 1800°C to form metallic aluminum and aluminum carbide or nitride. The temperature for rapid reduction of aluminum oxide to metallic aluminum is about the boiling point of aluminum and above the temperatures necessary to reduce iron, silicon, and titanium so that the direct reduction of an aluminum ore with carbon will produce an alloy of aluminum, iron, titanium, silicon, etc., which may be mixed with carbides and nitrides. Also a large amount of the reduced aluminum may be lost as a vapor except in the presence of some alloying agent such as copper or other metals. While it is possible to refine such alloys or mixtures so as to produce commercially pure aluminum, the methods which have been found are too expensive for the present market. One direct reduction method which found limited commercial use in Germany during World War II was the direct reduction of a mixture of clay containing very little

Jan 1, 1951

By R. E. Steiner, A. F. Weinberg, R. J. Van Thyne

Uranium solubility in molten bismuth was determined in the temperature range 350" to 600°C, varying from 0.09 wt pct to near 2 wl pct, respectively. Zirconium and magnesium, simulated fission products, and sodium were found to increase or decrease uranium solubility in bismuth in the temperature range 370° to 420°C, depending upon the addition or temperature. Data were obtained by both chemical analysis of samples obtained by filtration from saturated melts and by measurement of the variation of electrical resistance with temperature. IN a study for the United States Atomic Energy Commission, a Liquid Metal Fuel Reactor Experiment (LMFRE) was proposed in which a solution of uranium dissolved in molten bismuth served as both the fuel solution and the primary coolant. It was proven necessary to add other elements to this solution for certain desirable properties: 1) zirconium acts to prevent reaction of the fuel solution with the graphite core (which would result in the formation of uranium carbide) and also to inhibit mass transfer of iron and chromium from the walls of the reactor tubing to cold spots resulting in blockage; and 2) magnesium acts as a deoxidant and prevents loss of uranium. In addition to these intentional additives, other elements entering the solution are: 1) fission products which are a by-productof reactor operation, 2) sodium (the secondary coolant) through possible small leaks in the heat exchange system, and 3) iron and chromium from the container walls. Each of these elements may affect the solubility of uranium in the fuel solution. Since the concept of this reactor is based upon a liquid solution, the relatively low solubility of uranium in bismuth will dictate the minimum temperature at which the reactor heat exchanger can be operated. The solubility of uranium in liquid bismuth and the effect of some additives on this solubility have pre- viously been investigated1-' (more recent results6" became avaliable after initiation of this investigation). However, some discrepancies between the various results have been noted, and also the cumulative effect of the several additions or impurities was not known. This investigation was commenced to obtain definitive results. MATERIALS Analyses of the materials used are presented in Table I. Although ostensibly of extreme purity (99.999 wt pct), the bismuth was found to contain a significant amount of impurities, probably oxides. Except for determination of the binary system, Bi-U, prior to use all bismuth was hydrogen-refined and

Jan 1, 1962

By B. M. Larsen, T. E. Brower

A perspective is presented of the steel plant sulphur distribution and elimination problem from coal to liquid steel ready for teeming, giving distributions of sulphur over a range of coke sulphur content, and some methods of sulphur control, in the blast furnace, external desulphuriza-tion between blast furnace and open hearth, distribution between fuel, slag, and metal, and methods and limitations of control of sulphur in the open hearth furnace. AS a part of the 1951 AIME symposium on sulphur in steelmaking, it was thought that a discussion of the distribution of sulphur throughout the whole series of operations, from coal and ore to finished steel ingots, might have some value in giving a perspective on the whole problem. The following discussion is an attempt to present such an overall picture. The order is that of the actual plant operations, beginning with a very brief consideration of the coking process. Sulphur in Coal and Coke Since by far the largest source of sulphur entering the steelmaking cycle is in the coal used to make coke for the blast furnace, it would seem reasonable to eliminate some of it, either from the coal, or the coke, or during the coking process. This has appeared impracticable up to the present, at least, for two main reasons: the low activity of the organic sulphur in either coal or coke, and because of price limitations involved in treating a low cost material such as coke. A variable portion, usually M or less, of the sulphur is present in coal in the form of pyrites or similar compounds, and a large part of this sulphur may be removed in the coal washery. Most of the sulphur, however, is normally present as "organic" sulphur, intimately associated with the coal structure. Its distribution prevents any separation by mechanical means. Its low activity makes improbable ' any rapid chemical removal, although hydrogen will remove sulphur from both coal and coke. Thus, prolonged recirculation of coke oven gas in the coking process would tend to leave a smaller percentage of the total sulphur in the coke residue. Table I shows a typical distribution of sulphur from coal into products in the coking process. As the sulphur in the coal increases, the sulphur in the coke tends to increase in about the same proportion. Sulphur in the Blast Furnace The best picture of the situation in the blast furnace is provided by a sulphur balance of raw materials entering, and of products leaving, the furnace. The difficulties in accurate weighing and sampling of the variable solid materials entering this process, and the number of hours required for the raw materials to descend through the furnace under variable operating conditions, make it difficult to obtain an accurate balance. However, balances made over periods of weeks or months tend to average out some of these uncertainties. Table I1 presents three typical sulphur balances similar to a number that the writers have calculated. In most of these the slag volume calculated from the sulphur balance is, in some instances more, and in other instances less, than the value corresponding to the best input and output balances of the other slag constituents (lime, silica, alumina, etc.). Probably the greatest source of error in these calculations is the sulphur content of the slag. Despite some possible inaccuracies the balances of Table II show rather definitely the following points: 1—That 87 to 95 pct of the total sulphur input is in the coke and 95 to 97 pct of the total sulphur output is in the slag. Also, that if any sulphur leaves the furnace with the gas it is relatively small, amounting to a possible 1 pct or less. 2—At the lower sulphur coke level of 0.86 pct the total amount of sulphur charged is 15 Ib of sulphur per ton iron increasing to 26 lb per ton at the higher sulphur, intimately associated with the coal struc-rare burdens containing sulphur-rich ores will the total sulphur burden fail to be nearly proportional to the content in the coke used. 3—The 7 to 9 pct of the total sulphur input from the limestone of furnaces B and C is due to the relatively high sulphur content of the stone, 0.226 and 0.265 pct, respectively. In the case of furnace A, the sulphur content of the limestone was only 0.06 pct which resulted in only 3 pct of the total sulphur input coming from this source. It is rather interesting to compare the sulphur balances of a typical ferromanganese furnace with

Jan 1, 1952

By John Chipman, Eric R. Jette, O. B. Ellis

IN the study of the chemical reactions occurring in the open-hearth furnace, it is frequently assumed that a condition of equilibrium between slag and metal is attained. In order to test this assumption it is necessary to have dependable operating data as well as an exact knowledge of the equilibrium state. Considerable progress has already been made in the study of slag-metal equilibria, notably in the earlier work of Herty1 and of Oberhoffer and Schenck2 and in the more recent researches of Krings and Schackmann3 and of Koerber and Oelsen.4 None of these investigators, however, have employed basic slags comparable to those encountered in basic open-hearth practice, so that up to the present time our only information regarding the equilibria of these slags is based upon observations drawn from steelmaking practice in which there is little assurance that actual equilibrium was attained. The original plan of this investigation was to secure simultaneous slag and metal samples at intervals during the making of an open-hearth heat, recording the heat history in detail and obtaining complete analyses of slag and metal, then to bring these slag samples into equilibrium with liquid iron in the laboratory induction furnace and thus to determine directly whether or not the observed relationships in the open hearth represent conditions approaching equilibrium. This plan was only partly successful. While slags were obtained from the open hearth under satisfactorily recorded conditions and these were remelted in the laboratory under equilibrium conditions, changes in slag composition, which accompanied the remelting operation, were so great that the final slag from the induction furnace bore little resemblance to its open-hearth parent and the direct comparison was therefore abandoned. The results, however, lie within a range of slag composition that is of interest in the making of low-carbon steel. As far as we are aware, they represent the first published laboratory study of equilibria involving slags that contain all the constituents of basic open-hearth slag. EXPERIMENTAL HEATS The first set of measurements on slagmetal equilibrium was made in the Research Laboratories of the American Rolling Mill Co. at Middletown, Ohio. This will be known as series A. The second set was made in the Metallurgical Research Laboratories at Massachusetts Institute of Technology, and will be referred to as series B. Series A.-The induction furnace used has been described.5 Approximately I kg. of a special ingot iron containing less than

Jan 1, 1941

By O. B. Ellis, Eric R. Jette, John Chipman

In the study of the chemical reactions orcurring in the open-hearth furnace, it is frequently assumed that a condition of equilibrium between slag and metal is attained. In order to test this assumption it is necessary to have dependable operating data as well as an exact knowledge of the equilibrium state. Considerable progress has already been made in the study of slag-metal equilibria, notably in the earlier work of Hertyl and of Oberhoffer and Schenck2 and in the more recent researches of Krings and Schack-mann3 and of Koerber and Oelsen.4 None of these investigators, however, have employed basic slags comparable to those encountered in basic open-hearth practice, so that up to the present time our only information regarding the equilibria of these slags is based upon observations drawn from steelmaking practice in which there is little assurance that actual equilibrium was attained. The original plan of this investigation was to secure simultaneous slag and metal samples at intervals during the making of an open-hearth heat, recording the heat history in detail and obtaining complete allalyses of slag and metal, then to bring these slag samples into equilibrium with liquid iron in the laboratory induction furnace and thus to determine directly whether or not the observed relationships in the open hearth represent conditions approaching equilibrium. This plan was only partly successful. While slags were obtained from the open hearth under satisfactorily recorded conditions and these were re-melted in the laboratory under equilibrium conditions, changes in slag composition, which accompanied the remelting operation, were so great that the final slag from the induction furnace bore little resemblance to its open-hearth parent and the direct comparison was therefore abnndoned. The results, however, lie within a range of slag composition that is of interest in the making of low-carbon steel. As far as we are aware, they represent the first published laboratory study of equilibria involving slags that contain all the con stituents of basic open-hearth slag. Experimental Heats The first set of measurements on slag-metal equilibrium was made in the Research Laboratories of the American Rolling Mill Co, at Middletown, Ohio. This will be known as series A. The second set was made in the Metallurgical Rescarch Laboratories at Massachusetts Institute of Techology, and will be referred to as series B. Series A.—The induction furnace used has been described. Approximately I kg. of a special ingot iron containing less than

Jan 1, 1941

By John Chipman, Eric R. Jette, O. B. Ellis

In the study of the chemical reactions orcurring in the open-hearth furnace, it is frequently assumed that a condition of equilibrium between slag and metal is attained. In order to test this assumption it is necessary to have dependable operating data as well as an exact knowledge of the equilibrium state. Considerable progress has already been made in the study of slag-metal equilibria, notably in the earlier work of Hertyl and of Oberhoffer and Schenck2 and in the more recent researches of Krings and Schack-mann3 and of Koerber and Oelsen.4 None of these investigators, however, have employed basic slags comparable to those encountered in basic open-hearth practice, so that up to the present time our only information regarding the equilibria of these slags is based upon observations drawn from steelmaking practice in which there is little assurance that actual equilibrium was attained. The original plan of this investigation was to secure simultaneous slag and metal samples at intervals during the making of an open-hearth heat, recording the heat history in detail and obtaining complete allalyses of slag and metal, then to bring these slag samples into equilibrium with liquid iron in the laboratory induction furnace and thus to determine directly whether or not the observed relationships in the open hearth represent conditions approaching equilibrium. This plan was only partly successful. While slags were obtained from the open hearth under satisfactorily recorded conditions and these were re-melted in the laboratory under equilibrium conditions, changes in slag composition, which accompanied the remelting operation, were so great that the final slag from the induction furnace bore little resemblance to its open-hearth parent and the direct comparison was therefore abnndoned. The results, however, lie within a range of slag composition that is of interest in the making of low-carbon steel. As far as we are aware, they represent the first published laboratory study of equilibria involving slags that contain all the con stituents of basic open-hearth slag. Experimental Heats The first set of measurements on slag-metal equilibrium was made in the Research Laboratories of the American Rolling Mill Co, at Middletown, Ohio. This will be known as series A. The second set was made in the Metallurgical Rescarch Laboratories at Massachusetts Institute of Techology, and will be referred to as series B. Series A.—The induction furnace used has been described. Approximately I kg. of a special ingot iron containing less than

Jan 1, 1941

By Alexander Coucoulas

FABRICATION of thin-film circuits deposited on glass substrates requires the formation of permanent electrical contacts. Since thin films are in the order of a few thousand angstroms thick and are deposited on nonconductive surfaces such as glass, new methods of lead attachment are being pursued in the microelectronics industry. Ultrasonic welding is being considered in thin-film technology since joining can be accomplished between a wide variety of dissimilar materials.l,' Ultrasonic welding is accomplished by a transducer-coupling-tip system which converts high-frequency electrical energy into mechanical vibrations and delivers it into the weld region. During the process the tip oscillates in a direction parallel to the surface of the weldments, inducing shear stresses in the work pieces which are clamped between the tip and anvil. Though the basic bonding mechanism is not clearly understood, it has been described as closely akin to friction welding. In the course of an investigation concerned with ultrasonic we!ding of aluminum wires to tantalum thin films (1400A) deposited on glass, low weld strengths were related to glass failure. Upon investigating this condition, an improved method of bonding was developed where the aluminum was held at a temperature where a minimum amount of strain hardening occurred during the introduction of ultrasonic energy. Experimental Procedure. Aluminum wires (0.015 in,) were bonded to tantalum thin films with an optimized set of welding parameters (power, time, clamping force) employing a commercial 100-w 60-kc ultrasonic welder. Forty-five degree shear-peel tests, where the lead is pulled at a 45-deg angle with respect to the substrate at 0.2 in. per min, produced a large variation from zero to the strength of the wire, Table I. Inspection of the weld region generally revealed: glass cracking before and after testing; the removal of glass nuggets from the substrate by the lead during testing, Table I; thin-film penetration. In an effort to improve the shear-peel strength, the aluminum between the tip and substrate was heated above ambient temperature through an argon gas media prior to and during welding with the same parameters employed above. With the addition of heat: wire deformation was increased; shear-peel tests all failed at the weld-wire junction, leaving the bonded portion undisturbed; no evidence of glass cracking or film penetration prior to or after testing was observed. In order to prevent failure at the weld-wire junction due to excessive wire deformation, 0.035-in. aluminum wires were welded to tantalum thin films with an optimized set of welding and heating parameters. As

Jan 1, 1967

By F. W. Clark

At the present time, when lixiviation versus amalgamation is being so thoroughly discussed by practical men, and published information is so meagre, the following tests, made by students in the mining laboratory of the Massachusetts Institute of Technology, may be of interest to others. The ore experimented upon was obtained from the Sombrerete mines near Zacatecas, Mexico. A careful analysis of the dried sample resulted as follows : Per cent. SiO2,............62.79 S.............13.86 Al2O3............4.39 Fe,............11.26 Zn,............1.57 CaO.............2.91 MgO,........... 0.06 Cu,.............0.12 Pb,.............0.40 Sb and As,..........trace CO2,............2.35 Ag,.............0.16 99.87

Jan 1, 1886

By Ö. Valla, A. Muan, K. Grjotheim

The solid miscibility gap between CaO and "FeO" in the system CaO-"FeO" in contact with metallic iron gradually closes as MnO is added as a third component. On the liquidus surface of the system CaO-"FeO"-MnO, this situation gives rise to a boundary curve which originates in the bounding system CaO-''FeO", proceeds a short distance into the composition triangle of the ternary system, and then vanishes. A new approach has been used to follow the course of this boundary curve. It is shown that the curve vanishes at a much lower temperature and at much lower MnO contents than has been inferred previously. The oxides CaO, "FeO", and MnO together with SiO2 are the major components of the slag phase formed in the basic oxygen process. Hence, the system CaO-"Fe0"-MnO is of considerable technological interest. In addition, the system is theoretically interesting. The three oxides above all have sodium chloride structure. The size differences among the cations are such that in the bounding "binary"* systems CaO-MnO and "FeO"-MnO complete solid-solution series are formed,1,2 whereas in the system CaO-"FeO" there is only limited mutual solubility in the solid state,3 see Fig. 1. Hence, a solid miscibility gap exists in a part of the "ternary"* system Ca0-"Fe0"-Mn0, and a liquidus boundary curve originates at the peritectic point, point a in the insert in Fig. 1, in the system CaO-"FeO", extends a certain distance into the ternary system, and then vanishes. Very little quantitative information on the system Ca0-"Fe0"-Mn0 is available in previous literature. Fischer and Feischer4 sketched isothermal sections at 1600° and 1700°C, and estimated that the vanishing boundary curve extends to approximately 1650°C and a composition of 42 wt pct MnO. The work to be described in the following was aimed at locating experimentally the "vanishing" liquidus boundary curve, determining its end point, and deriving representative isothermal sections below and above the temperature of the end point of this curve. EXPERIMENTAL METHODS The phase relations were determined by the well-known quenching method. (For a description of this method as applied to oxide systems, see the original paper of Shepherd, Rankin, and wright.5) Prereacted oxide mixtures of desired compositions were contained in iron crucibles and heated in a vertical tube furnace in an atmosphere of purified nitrogen. After equilibrium was judged to have been attained, the samples were quenched to room temperature, the phases present were identified by microscopic and X-ray examination, and total iron oxide contents were determined by chemical analysis. "Fisher Certified" reagents (MnCO3, CaCO3, Fe2O3, and Fe) served as starting materials. The calcium carbonate and ferric oxide were heated in air at 400° and 800°C, respectively, for 24 hr prior to use. Manganese oxide was prepared by decomposing the carbonate in a graphite crucible in hydrogen atmosphere at 1000°C. The product was ground under acetone to -100 mesh. The iron powder was used directly without any preparation. Dicalcium ferrite was used as a starting material for some mixtures. It was made by mixing some of the above prepared CaCO3 and Fe2O3 in proportions corresponding to the formula 2CaO. Fe2O3. This mixture was then fired in air for

Jan 1, 1969

By C. A. Bruch, W. E. McHugh, R. W. Hockenbury

Commercially pure molybdenum specimens were irradiated in the Materials Testing Reactor for an estimated exposure of 1.9 to 5.9x10 20 thermal nvt. Prior to irradiation, the material was ductile in the tension test; whereas after irradiation, it was brittle. The results of tension tests conducted at various temperatures revealed that the transition temperature for this material had been increased from —30' to +70°C as a result of the radiation exposure. From metallographic studies, it is concluded that the embrittlement is due to submicroscopic changes which raise the flow stress-temperature curve of the material. PRIOR to ten years ago, the bombardment of metals with high speed heavy particles such as protons, deuterons, a particles, and neutrons was primarily of academic interest. These particles existed in extremely small numbers in a few laboratories and only under very special conditions. With the introduction of the nuclear power reactors, these particles are now available in enormous quantities and it has become important from a practical standpoint to learn how well metals withstand severe reactor radiations. The principal radiations of concern in reactors are neutrons and y rays, since the heavier charged particles exist only in limited regions of reactors. Seitz,' in a theoretical approach, has shown that all of these high energy particles, except y rays, have enough energy to knock atoms from lattice sites and that these knocked-on atoms have enough energy to cause additional displacements of neighboring atoms. The result of this process would be a lattice containing many imperfections in the form of interstitial atoms and vacancies. Hence, it would be expected that the properties of metals can be changed by reactor radiations, and such has been found to be the case. Only a limited amount of data have been published in the open literature,2,3 and these data have been for relatively low integrated-neutron-flux exposures. In general, one effect of reactor radiations on the mechanical properties of metals has been to increase strength and decrease ductility. It is now possible to irradiate specimens in the Materials Testing reactor at much higher fluxes and to higher integrated exposures than previously possible.' The data which are being presented here describe the effects of a relatively high exposure on some mechanical properties of molybdenum. Experimental Procedures Material: The molybdenum used in this investigation was obtained from the Climax Molybdenum Co. The two heats from which the material originated were melted under a vacuum of 5 to 30 microns and cast in 7 in. diam water-cooled copper molds. One ingot contained 0.061 pct C and the other 0.066 pct. Both ingots were hot worked by extrusion and rolling into % in. diam rods, after which they were annealed and straightened. The rods were subsequently heated to 1100°C in a hydrogen atmosphere and swaged to ½ in. diam rods at the Research Laboratory of the General Electric Co. The resulting material had an average hardness of 264 VPN, or 99.2 Rb, and had an average of 5000 grains per sq ml in the transverse section, Test Specimens: Substandard-size tensile specimens were prepared according to the specifications shown in Fig. 1. These specimens were used also for hardness measurements. The metallographic specimens were small disks which were polished, etched, and photographed at X1000 prior to irradiation. The field studied was

Jan 1, 1956

By C. F. Floe, M. Cohen, M. B. Bever, V. G. Paranjpe

NITROGEN is becoming recognized as one of the important elements in ferrous physical metallurgy. Several investigations indicate that nitrogen plays a significant part in such phenomena as strain aging and temper brittleness. Nitrogen is known to be a powerful austenite stabilizer and may be a useful alloying element in stainless steels. The hard-enability of steels has been found to be increased by nitrogen. The nitriding and carbonitriding pro- cesses are examples of successful industrial application of nitrogen in ferrous materials. For a complete understanding of the various roles played by nitrogen in ferrous metallurgy a knowledge of the phase relations in the binary iron-nitrogen system is essential. The literature contains a variety of iron-nitrogen phase diagrams. Those suggested by Fry, Sawyer,² Epstein and his coworkers,³,4 Lehrer,5 Eisenhut and Kaupp, and Hägg7,8 differ significantly from one another. Moreover, the most recent of these investigations dates back about twenty years. A re-determination of the entire diagram, therefore, appeared desirable. In addition to the published phase diagrams, investigations have been carried out on portions of the iron-nitrogen system. Bramley and Haywood determined the composition and temperature of the iron-iron nitride eutectoid. The maximum solubility of nitrogen in a iron was investigated by Portevin and Seferian10 and by Diikstra. 11 Several investigators have determined the crystal structure of the various iron-nitrogen phases. In fact, Eisenhut and Kaupp6 and Hägg7 based their entire phase diagrams on the results of such studies. Epstein' and Emmett12 reported lattice-parameter measurements on the E (hexagonal close-packed) phase. Osawa and Iwaisumi13 also studied the change in lattice parameters of the a, ? and E phases with nitrogen content. Brill" and Hägg7 showed that the y' phase has an ordered structure, and Hendricks and Kostingsl5 suggested a structural relation between the E and phases. In a recent investigation Jackl6 arefully studied the super-lattice reflections from the y' and phases. Experimental Procedure A large variety of experimental methods has been used by previous investigators in studying the iron-nitrogen system. These methods include thermal analysis, microscopic examination, X ray diffraction, magnetic measurements, dilatometric analysis and anelastic experiments. Thermal analysis is of low accuracy in determining changes in the solid state. This accuracy is further decreased for iron-nitrogen alloys since composition changes will occur during heating or cooling unless extreme care is taken to use a proper atmosphere. Metallographic methods are of small value . because homogeneous iron-nitrogen alloys of sufficient size can be produced only with great difficulty. The dilatometric method is open to the same objections as thermal analysis in that changes in composition may occur during heating and cooling. Lattice parameter measurements by X ray diffraction can be used satisfactorily for determining phase boundaries if cooling is fast enough to prevent structural changes. In view of the limitations of the various other techniques two methods only were adopted in this investigation, (1) X ray diffraction measurements, and (2) a controlled nitrogenizing method. The second method is an innovation for investigating the iron-nitrogen system, and will be described at length. Materials: All iron-nitrogen alloys were prepared from carbonyl iron powder of the analysis shown in table I. The average particle size was about 20

Jan 1, 1951