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By G. W. P. Rengstorff, H. B. Goodwin

A method is described for purifying iron in batches of 150 Ib or more. Oxygen, carbon, nitrogen, and sulphur are removed from flakes of electrolytic iron by treatment in wet and then dry hydrogen. A special consumable-electrode arc furnace is used to remove hydrogen and to melt the flakes into ingots. A LTHOUGH iron and steel have been made and used for hundreds of years, there are still wide gaps in the knowledge of these metals. One reason for this is that the true properties of the base metal, iron, are not well known, simply because really pure iron has never been readily available for research purposes. Commercial iron, and even the "pure" irons which are readily available, are really complex alloys of iron with oxygen, nitrogen, hydrogen, carbon, sulphur, silicon, and other elements. With such materials, it has not been possible to prepare steels and other iron-base alloys in which all elements are present in exactly controlled amounts. It is an almost impossible task to determine the separate effects of each element or the intereffects of several elements unless alloys can be prepared containing only the desired elements. The ability to make controlled alloys of low impurity content is of far more than academic interest. It will assist in the study of such practical problems as the brittle failure of ship hulls or high pressure gas pipelines, determination of the factors which affect the deep-drawing properties of steels, the improvement of magnetic and electrical properties, the phenomenon of aging, and many others. In 1949, the American Iron and Steel Institute asked Battelle Memorial Institute to prepare high purity iron on a larger scale than had been attempted up to that time. The work was directed toward the preparation of iron as low as possible in carbon, oxygen, nitrogen, hydrogen, and sulphur because these are the contaminating elements of major interest in many research investigations on iron-base alloys. The initial goal was to prepare iron with not more than a few thousandths of one percent of each of these impurities. The purpose was to set up a "bank" of high purity iron on which researchers could draw when a supply was needed and which could be replenished from time to time as the stock became depleted. Of several possible purification methods, heating in hydrogen was selected as the most promising for the removal of both carbon and oxygen from solid iron. Metallic impurities are not removed by hydrogen. Electrolytic iron was chosen as a starting material because it is the most readily available form of iron low in metallic impurities. Decarburization and desulphurization were obtained by annealing in wet hydrogen at relatively low temperatures. The optimum temperature, as found by previous investigators,' is about 1400°F. This treatment also removes nitrogen. Deoxidation is favored by dry hydrogen and higher temperature. There is evidence from previous work that an anneal at 2200°F in dry hydrogen will deoxidize the iron, reduce the nitrogen content, and reduce the sulphur content. These facts suggested the use of a two-stage process: treatment in wet hydrogen followed by treatment in dry hydrogen. To carry out the purification process in a reasonable time, it was necessary that the iron be in thin pieces. Flakes of electrolytic iron were used. Because most research requires that the iron be in massive form, it was nccessary to melt the purified iron to consolidate it into large pieces. For this work, it was decided to prepare ingots weighing at least 15 lb by using a cold hearth arc-melting process in which the iron was melted in an inert atmosphere of argon or helium. This method of melting was selected because the water-cooled copper crucible is not wet by the iron and does not contaminate it as a refractory crucible would. Because the crucible is also the ingot mold, contamination from mold materials was also eliminated. Contamination from electrodes was avoided by making them from purified electrolytic iron. The melting procedure finally developed was an adaptation of the Kellogg electric ingot process.' Two batches of purified iron weighing about 100 Ib each in ingot form were prepared with analyses as shown in Table I. The remainder of this paper describes the procedures in more detail. In general, the process con-

Jan 1, 1956

By L. W. Pommier, F. B. Brien, A. K. Bhasin

The diflerential movement of solid particles through solid-liquid suspensions is very important to many branches of engineering. The flow of suspensions around immersed bodies is mainly of a turbulent nature. Problems are encountered when attempts are made, as is the general practice, to extrapolate the velocity and resistance relationships of Newton, pertaining to Newtonian systems, into non-Newtonian solid-liquid suspensions. The conventional velocity and resistance relationships for turbulent flow in fluids when applied to suspensions, do not take into consideration the two very important variables: suspension particle size and solid volume fraction. A study of the effect of suspension particle size (dgb) on the velocity of falling balls leads to the concept of a critical particle size (dgc) at which the suspensions will be Newtonian. This leads to the classification of static suspensions into two types: suspensions consisting of particle of diameter dgh > dgt, and those with dgh, < dgr. Separate velocity and resistance equations for these two types of suspensions have been proposed, taking into account both the solid particle size and solid volume fraction. The agreement between the velocities predicted from the proposed equations and the measured velocities, confirms their validity. The resistance force offered by suspensions to the movement of immersed bodies has been calculated from the proposed equations, and the effects of suspension particle size and solid volume fraction on the resistance force and velocity have been examined. The movement of immersed bodies in solid-liquid suspensions is of great importance in many areas of engineering such as minerals processing, oil well drilling, suspension flow in pipelines, and hydrometallurgy. A number of mineral dressing processes deal essentially with the movement of solids in suspensions—in particular, classification, thickening, filtration, ore washing, and gravity concentration—thus a study of the fluid characteristics of suspensions is of theoretical and practical interest.&apos; A rigorous analysis of the mechanisms of momentum transport of a solid-liquid system is complex indeed. The rheological properties of the suspensions deviate from those of liquids, varying, for example, with density, solid volume fraction, size and shape of the solid phase of the suspension, and with the density and viscosity of the liquid phase. The flow of suspensions around immersed bodies is mainly of a turbulent nature and hence studies of the turbulent flow characteristics of suspensions are of par- ticular importance. Problems are encountered when attempts are made to extrapolate the velocity and resistance relationships of Newton, pertaining to Newtonian systems, into non-Newtonian solid-liquid suspensions. Due to the numerous variables present in a suspension, certain limitations and assumptions become necessary in order to produce quantitative relationships for predicting their effects. The solid particle size and the solid volume fraction are two of the more important variables. By comparing the measured and calculated Newtonian velocities of falling balls in simple static suspensions, the existing velocity and resistance relationships have been modified to take these variables into account. In order to keep the study less complex, all other variables such as the characteristics of suspending liquid and shape of the particle are maintained constant. Objective The objective of the present investigation is to modify the Newtonian velocity and resistance equations in order to take into account the suspension particle size and solid volume fraction. Theory Liquids are classified on the basis of viscosity, which may be defined as the relationship between applied shear stress and resulting rate of shear.&apos; pure single-phase fluids composed of small light molecules behave as Newtonian liquids, having a single viscosity pa-

Jan 1, 1971

By Robert J. Willard

The scanning electron microscope (SEM), became commercially available in 1966. Embodying some unique features not provided by conventional electron microscopes, this new electron-optical instrument offers the scientific community a new way of observing the surfaces of materials. In rock mechanics research, the SEM should prove a useful basic tool in characterizing rock fracture on a very small scale and thus contribute to a better understanding of rock behavior at larger scales. This article presents one example of how the SEM is being applied to such research at the Twin Cities Mining Research Center operated by the U.S. Bureau of Mines in Minneapolis. This research center conducts theoretical and experimental studies on a broad range of mechanisms that induce disintegration by the application of energy to rock.1 Some of these studies are concerned with the relation of microstructure to rock behavior and are carried out mainly with the petrographic microscope. At the same time, however, the center recognizes that this relation must be studied through several orders of magnitude, from lattice-size units of rock-forming minerals to field-size rock units. The SEM fits this scheme by extending the capability of the petrographic microscope into smaller orders of magnitude. However, because its resolution is limited to about 200 A at 10,000x, the SEM is not capable of resolving lattice-size units, and hence a conventional electron microscope with a much greater resolution capability is necessary at this order of magnitude.

Jan 6, 1969

By D. W. Fuerstenau

Measurement of zeta potentials is a useful tool to study the surface chemistry of minerals under flotation conditions. Because there is continued interest in this approach, the apparatus for obtaining zeta potentials of nonconducting solids by the streaming potential method is outlined here. Fig. 1 illustrates the streaming potential apparatus. The streaming potential cell or plug consists of two 24/40 standard ground joints (4) joined with a piece of pyrex tubing 60 mm long and 12 mm in diam (5). The electrodes are made of bright platinum disks 19 mm in diam and 1 mm thick through which 0.5-mm holes have been drilled (6). To the surface of each is welded a piece of 80-mesh platinum gauze. Each electrode is permanently mounted on the ends of the inner parts of the two standard joints by means of a platinum wire (7) which connects it to the tungsten seal at the end of the cell (8). For ease in cleaning and handling the apparatus, the streaming cell is fastened to the 500-ml reservoir flasks (1) by means of two 18/9 ball and socket joints (2). This particular arrangement permits passage of the solution in either direction through the plug of particles. Flow of solution can be stopped by a stopcock (3). One of the reservoir flasks has a large opening to permit insertion of either a thermometer or a pair of electrodes for measuring pH of solutions within the system. In making the experiments, the plug is filled with 48 to 65-mesh particles, but a layer of 28 to 35-mesh particles is placed at each electrode to prevent any of the finer particles from passing through holes in the electrodes.

Aug 1, 1956

By Charles Macdonald

WROUGHT-IRON eye-bars for bridges and roofs, designed upon what is known as the pin connection system, have been successfully manufactured in this country for some years. The most approved methods employed have been the hydraulic upsetting process, and by die-forging under a hammer. In upset eyes the fibre of the iron is necessarily much distorted ; and in bars of considerable size, this disturbance seriously impairs the strength of the connection. Mr. Collingwood, in discussing my paper on "Proportions of the Heads of Eye-bars," read before the American Society of Civil Engineers, Jan. 21st, 1874, submitted sketches of certain bars intended for the anchorage of the East River bridge, which had been exposed to the action of sulphuric acid a sufficient length of time to thoroughly cleanse the surfaces, and expose the condition of the fibre. These sketches are here reproduced for the purpose of illustrating the effect of this methpd of manufacture. In Figs. 1, 2, and 3, it will be observed that the fibres at A, and E, have been folded back upon themselves and otherwise twisted and disturbed, in a manner not calculated to inspire confidence in the integrity of the connection. To compensate for this defect, a large excess of metal is thrown into the eye; but a method of manufacture which involves such a necessity, even although it be the one giving the best results thus far, all things being considered, is far from being perfect.

Jan 1, 1879

By Charles Macdonald

Wrought-iron eye-bars for bridges and roofs, designed upon what is known as the pin connection system, have been successfully manufactured in this country for some years. The most approved methods employed have been the hydraulic upsetting process, and by die-forging under a hammer. In upset eyes the fibre of the iron is necessarily much distorted ; and in bars of considerable size, this disturbance seriously impairs the strength of the connection. Mr. Collingwood, in discussing my paper on "Proportions of the Heads of Eye-bars," read before the American Society of Civil Engineers, Jan. 21st, 1874, submitted sketches of certain bars intended for the anchorage of the East River bridge, which had been exposed to the action of sulphuric acid a sufficient length of time to thoroughly cleanse the surfaces, and expose the condition of the fibre. These sketches are here reproduced for the purpose of illustrating the effect of this method of manufacture. In Figs. 1, 2, and 3, it will be observed that the fibres at A, and E, have been folded back upon: themselves and otherwise twisted and disturbed, in a manner not calculated to inspire confidence in the integrity of the connection. To compensate for this defect, a large excess of metal is thrown into the eye; but a method of manufacture which involves such a necessity, even although it be the one giving the best results thus far, all things being considered, is far from being perfect.

Jan 1, 1879

By M. J. Stewart, F. Weinberg

PREVIOUS investigations into convective flow in molten metals have examined systems in which the length-to-height ratio of the enclosure is large, usually using long graphite boats.&apos;&apos;2 In normal castings this ratio is generally small and it is not possible to extrapolate the results of previous work to casting configurations. The present investigation was undertaken to examine liquid flow in systems of low length to height ratio. The apparatus used for the experiments is shown in Fig. 1. The molten zone of tin is contained in an aluminum mold of inside dimensions 6.4 by 6.4 by 0.31 cm. A heating block containing a resistance coil is attached to one end of the mold and a cooling block is attached to the other end. These are used to produce a wide range of temperature differences across the mold. The mold is contained in a stainless steel tank which is heated from the outside by resistance heaters to give the required operating temperature during the experiment. Temperature measurements in the molten tin are made with an iron-constantan thermocouple PT equal to 5 atm. The phase diagram derived by us was the same as that found by Krivsky and Schuhmann, except for a similar discrepancy in one boundary line representing the gas composition in equilibrium with SO a. The vapor pressures of the pure components can be neglected at 1700°K, 1 atm and 2500°K, 5 atm. There-fore, in these cases PT is essentially the total pres-sure in the system. This is valid for all the diagrams presented by Krivsky and Schuhmann except for the one at 2500°K and 0.01 atm, where the vapor pressure of silicon is comparable to PT.6 This work was supported in part by the American Iron and Steel Institute. &apos;C. E. Wicks and F. E. Block: Thermodynamic Properties of 65 Elements, U S. Bur Mines, Bull. No. 605, 1963. R. P. Elliott: Constitution of Binary Alloys, 1st supplementary, McGraw-Hill Book Co., New York, 1965. 3W. A. Krivsky and R. Schuhmann, Jr.: Trans. TMS-AIME, 1961, vol. 221, pp. 898-904. 4M. F. Ancey-Moret, M. Olette, and F. D. Richardson: Mem. Sci. Rev. Met., 1964, vol. 61, pp. 169-76. 5J . F. Elliott and M. Gleiser: Thermochemistry for Steelmaking, vol. 1. Addison-Wesley, Reading, Mass. 1960. 6 J.Drowart, G. De Maria, and M. G. Ingraham: J. Chem. Phys., 1958, vol. 29, p. 1015. probe of 0.4 mm diam inserted into the open top of the mold. Radioactive sn113, in the form of a small sphere, was gently lowered into the molten tin at point A in Fig. 1 THERMOCOUPLE> WATER ARGON END HEATER QUENCH ARGON Fig. 1—Apparatus for detecting liquid flow. Point A indicates position the tracer was introduced.

Jan 1, 1970

By John H. Hall

The Frémont test for measuring the energy consumed in breaking a notched bar of steel is not so well known in this country as it deserves to be. The test specimen used in this test is about # by 6 by about 16 in., notched with a hack saw on the lower side to cause the piece to break at a fixed point. A weight of 10 kg. falling 4 m., and provided with a knife or chisel which strikes the specimen, breaks the test piece by impact. The residual force in the falling weight after it has broken the specimen is recorded by a suitable device, and the difference between the total energy and the residual energy of the weight (in kilogrammeters) is the force consumed in breaking the specimen. An experience of several years with the Frémont testing machine has shown its great value in readily detecting brittleness not revealed by tensile testing or slow bending testing. In this paper it is proposed to discuss (1) the supersensitiveness of the test as applied to cast steel and (2) its value in revealing the effect of heat treatment under certain conditions. In testing coupons cut from castings heat treated by quenching and annealing, attention was drawn to the wide variations in the value of the Frémont test of specimens cut from different parts of the coupon. The latter was of the form and dimensions shown in Fig. 1, and Fremont test pieces were cut from two parts of this coupon, marked A and B in that figure. The results of the tests are shown below, tests A and B in each instance being from the same coupon: A. B. A. B. Coupon. Kilogram- Kilogram- Coupon. Kilogram- Kilogram- meters. meters. meters. meters. 1,........ 12.0 12.5 9,........ 27.5 32.5 2,........ 11.0 32.5 10,........17.5 31.0 3,........ 11.5 30.0 11,........ 14.5 31.0 4,........ 20.0 33.0 12,........ 15.0 27.5 5,........ 17.5 33.0 13,........ 19.0 30.0 6,........ 17.5 20.0 14,........ 17.5 25.5 7,........ 17.5 13.0 15,........15.0 30.0 8,........ 10.0 30.0

Jan 1, 1914

By E. A. Gulbransen, W. S. Wysong

THE behavior of molybdenum and its surface oxides in oxidizing and reducing gas atmospheres and in high vacua at elevated temperatures is a question of scientific and technical importance The use of molybdenum as a metal or as an important component in alloys in oxidizing atmospheres at elevated temperatures has been limited because of the unprotective nature of its oxide film and the volatility of this oxide at moderate temperatures. This communication will present results of a vacuum microbalance study 1,2 of the following problems. (11) the oxidation kinetics in the temperature range of 250° to 450°C; (2) the reduction with pure hydrogen of thin oxide films formed on molybdenum; (3) the volatility of the thin oxide films, and (4) the vacuum oxidation of molybdenum at high temperatures. Molybdenum is an interesting metal to study for the following reasons: (I) although the oxide-to-metal-volume ratio is greater than one, the metal is not considered protective; (2) the metal oxidizes readily at temperatures of 250°C and higher; (3) the oxides of the metal are reduced at temperatures as low as 500°C by pure hydrogen; (4) the oxide MoO3 melts at 795°C; and (5) the oxides of molybdenum are volatile at moderate temperatures. The following variables are studied in the oxidation kinetics. time, temperature, pressure, surface preparation, surface area, concentration of inert gas in the lattice, cycling procedures in temperature, vacuum effect and high temperature vacuum oxidation The general interpretation of many of these factors has been previously discussed. LITERATURE The oxidation of molybdenum has not been studied critically. Although" many studies have probably been made on the kinetics of the oxidation process, none has been reported in the literature available to us. The crystal structures found in the oxidation of molybdenum have been studied by Hickman and Culbransen 4 Their results showed that MoO2 is the oxide which is stable in contact with the metallic subgtrate throughout the temperature range 300 to 700°C. As the film thickens in the low temperature range, MoO3 becomes predominant on the surface. Above 400°C, Mo03 is no longer observed, Mo02 being the only oxide found. Hagg and Magneli5 have shown from an X ray study that the a-phase, orthorhombic MoO3 is stable up to 1050°C. Two other phases, ß and ß&apos;, with compositions close to Mo02 90 are also obtained The formula for the ß phase is not given but that of the ß&apos; phase is defined as Mo9026. The ß&apos; phase is found to be built upon a monoclinic unit cell. A -?-phase is isolated from a preparation M00275 heated for 17 hrs at 670°C. This phase is

Jan 1, 1947

By d&apos, D. L. Guernsey, J. C. Entremont, John Chipman

The reaction of aluminum with oxygen in liquid iron has been studied at 1740° and 1910°C. Interaction coefficients are very much smaller than those previously published. The equilibrium constant falls within the approximate range of earlier experiments and calculations. It is now well established that the "deoxidation constant" for aluminum in liquid steel at normal steelmaking temperatures is extremely srnall. Thus at 1600 the product [% Al] is of the order of 10- 14. At this temperature, therefore, great experimental difficulties are encountered in any attempt to obtain a direct measure of the constant. If the aluminum content of the metal is high enough to permit accurate analytical determination, that of the oxygen is too low. If the oxygen content is high, the aluminum is below the limits of detection. Our best values of the constant have come, therefore, from indirect calculations or by extrapolation downward from observations at higher temperatures.. For their studies in the range 1695° to 1866°C, Gokcen and chipman&apos; restricted their aluminum concentrations to less than 0.06 pct. Oxygen analyses were made by the vacuum fusion method which appears to be dependable at these low aluminum concentrations. Experimental results, even at the highest temperature employed, are extremely sensitive to small errors in the analysis of either element. The slight change in the equilibrium constant with aluminum and oxygen concentration was utilized in the calculation of interaction coefficients expressing the effect of aluminum on the activity coefficient of oxygen and the reciprocal effect of oxygen on the activity coefficient of aluminum. The range of concentration, however, was so limited that only a rough value for the interaction coefficient could be obtained. This value was much more negative than that found for any other pair of reactants. In view of the very limited range of concentration employed, the reported values have always been regarded as very questionable. A redetermination was the object of the work reported here. EXPERIMENTAL METHOD At high aluminum concentrations, the vacuum fusion method is susceptible to grave error due to absorption of gas by aluminum distilled from the sample. Since it was desirable to extend the study to at least as much as 1 pct Al, another method for analysis was sought. In steels containing more than a few hundredths of a percent aluminum and no other deoxidizing element, it is safe to assume that

Jan 1, 1963

By J. Jolly

THIS short note on the probable character of the organic sulfur compounds in coal can do no more than indicate lines of research. We have no new experimental work to describe, nothing comparable in value with the careful studies of American coals by Powell and Parr1 and Yancey and Frazer.2 A study of the manner in which sulfur compounds exist in British coals (and their behavior on heat treatment) is rendered increasingly necessary by the fact that the British reserves of good coking coals of reasonably low sulfur content are fast being depleted. We believe that it is essentially by a study of the modes of formation, occurrence, and decomposition of the various types of inorganic and organic sulfur compounds in coal that it will be possible, with hope of success, to attack the problem of purifying coals, otherwise eminently suitable for coking, from these objectionable ingredients. Sulfur, so far as is at present known, does not normally occur in the free state in the coal conglomerate, but is chiefly distributed, irregularly, in three forms: 1. As primary constituents of the coal conglomerate, organic in nature and probably associated with those molecular complexes that have resulted from the degradation of the proteins of the plant tissues responsible for the formation of the coal mass. These constituents can be classed as "organic sulfur." 2. As metallic sulfides, e.g., iron pyrites. 3. As metallic sulfates, e.g., calcium sulfate and ferrous sulfate. (The occurrence of these compounds varies with the occurrence and degree of degradation of class 2.)

Jan 3, 1925

By M. L. Samuels

DURING the period from 1910 to 1920, there was a lively interest in. the subject of grain growth and many papers were published, followed by interesting discussions. Questions dealing with the fundamentals of grain growth-why and how it occurs-were treated in papers by Howe,1 Jeffries,2 Sauveur,3 Chappell,4 Beilby,5 Mathewson -and Phillips,6 McAdam,7 Carpenter and Elam,8 Stead and Carpenter,9 Ruder,10 as well as others. Since that decade, much indeed has been done regarding the practical control of grain size, and it is now possible to order material having a size specified in the American Society for Testing Materials classification. Also, one hears the term "spliced boundaries" used in connection with certain tungsten lamp filaments" wherein it is important to prevent "sagging" between consecutive turns of the helix.12 This practical use of a certain knowledge as to the things that influ-ence or even control grain growth should not be taken as an indication that the subject has been thoroughly explored and that nothing more can be learned from fundamental studies. It is with this thought in mind that a report of some observations and experiments on abnormal grain growth is believed justified. Abnormal grain growth is met with in heat-treating high-carbon steels in the austenitic range,13 in the harden-ing treatments of high-speed steels,14,15 and in the low-temperature annealing of strained low-carbon steels as in sheet and wire material. Entirely aside from these instances of exaggerated grain growth, which some might consider as freakish, it is thought that abnormal growth is simply a case where the growth forces and the forces tending to prevent growth are almost, but not quite, evenly balanced. Information relative to grain-growth characteristics in general may be obtained from a study of abnormal growth conditions, which may be looked upon as vantage points. Reflection will show at once that if growth forces are great in comparison to inertia or resistance to growth, many crystals start to grow and, for that reason, none becomes very large, whereas if inertia is predominant no growth at all takes place. Under conditions in which

Jan 1, 1938

By J. B. Hess, C. S. Barrett

TO reach equilibrium between different phases in cobalt-rich alloys requires prohibitively long annealing cobalt-richalloystimes when temperatures are below about 700°C. The fact that a transformation from face-centered cubic to close-packed hexagonal readily tered takes place at temperatures below this in the cobalt-rich solid solutions is not an indication that thermally activated processes occur at an appreciable rate, for the transformation is well established as martensitic in nature. Wide divergence between heating and cooling experiments and high sensitivity to prior heat treatment make it difficult to judge temperatures of equilibrium between the phases.&apos; One object of the present work was to see if the information object of on the relative stability of phases could be gained by substituting plastic deformation for thermal agitation. Procedures were worked out that led to the determination of a diffusionless type of phase diagram, which represents the temperature of of phase equal stability for phases of the same composition, and the technique was applied to the Co-Ni system. Another object of the work was to see whether or not deformation would generate frequent stacking faults when these were thin lamellae of quentstackingfaultsa phase having higher free energy than the parent phase. The alloys were prepared in 80 to 100 g melts from cobalt (with metallic impurities estimated spectrochemically as follows: Ni, 0.05 pct; Fe, 0.001 pct.; Mg, Si, Cu, Cr, Al, < 0.001 pct) and Mond Car-bony1 nickel (with Fe, 0.05 pct; Si, 0.003 pct; C, 0.61 pct.; Cu, 0.001 pct; Co, Cr not detected, < 0.01 pct). The metals were melted in pure Al2O3 crucibles. An atmosphere of argon, that had been purified by passing over hot magnesium chips, was used for the alloys that, by analysis of the portions of the ingots actually used, were found to contain 15.3, 25.7, and 35.0 pct Ni, and vacuum melting (after degassing) was used for those containing 29.4 and 31.5 pct Ni. After induction melting the alloys were allowed to solidify in the crucible, and slices % in. thick x ½ in. in diam were annealed 12 hr at 1350°C for homogenization. These same specimens were used throughout the series of experiments, with annealing treatments of 4 hr at 900°C in purified hydrogen followed by furnace cooling, alternating with the deformation and X-ray tests discussed below. Results Spontaneous transformation was observed on cooling to room temperature in all alloys containing 29.4 pct Ni or less and by cooling the 31.5 pct alloy to — 195°C but was not observed in the 35 pct alloys after cooling to —195°C. These results are in satisfactory agreement with the cooling experiments of Masimoto.4 From these data it is clear that the temperature of beginning transformation M,,, drops to 20°C with the addition of about 30 pct Ni. The test for spontaneous transformation was metallographic. Specimens were thermally polished by annealing 10 hr in hydrogen at 1350°C, then furnace cooled; if trans- formation had occurred there were relief effects visible on the thermally polished surfaces. These markings were narrow straight lines, usually resolvable at high magnification as clusters of fine lines that resembled slip lines. It was concluded that they resulted from displacements on (111) planes, for the number of directions in individual grains often reached but never exceeded four, and lines could always be found parallel to the thermally etched (111) boundaries of annealing twins. The markings were thus consistent with the idea that the transformation occurs by (111) plane displacements (Shockley partial dislocations moving on (111) planes). This was further confirmed by X-ray tests for stacking disorders. Using an oscillating crystal technique previously employed to detect strain-induced faulting in Cu-Si alloys," streaks indicative of the stacking faults were looked for and found on X-ray films of the spontaneously transformed 25.7 pct Ni alloys, as expected by analogy with Edwards and Lipson&apos;s results on pure cobalt." The streaks were much intensified after rolling at room temperature. Transformation induced by plastic strain was investigated as a function of alloy composition and temperature of deformation. A series of tests was made to determine suitable straining and X-raying techniques. Filing was found inferior to abrasion in converting cubic samples to hexagonal, and abrasion was less effective than peening in producing smooth unspotty Debye rings in the X-ray patterns. Because the diffraction lines were broad, Geiger-counter spectrometer records of filings were less sensitive in revealing small amounts of transformed material than X-ray patterns recorded on films in a small diameter camera. After these exploratory tests the following methods were adopted. Specimens that had been annealed at least 4 hr at 900°C and furnace cooled were mounted in a block of aluminum, brought to temperature, and peened thoroughly with a mullite pestle preheated to the same temperature. The specimens were then quenched to room temperature. In peening, a circular area of % in. diam was given 500 blows. A few control tests showed that an additional 1000 blows did not detectably change the proportions of the phases present. The amount of transformation was judged by X-ray reflection patterns from the peened surface, using the innermost four lines of the cubic and the hexagonal patterns with filtered CoKa radiation,

Jan 1, 1953

By J. H. Palm

Experiments have shown12 that the formula -S = St - (St - Se&apos;)e ne [1] expresses very well the relation between the true stress S and the true form monotonic deformation of plastic metals in single tension and compression (Fig 1). St (asymptotic or final stress), Se&apos; (threshold stress) and ne (characteristic or specific strain) are constants, the significance of which immediately follows from Fig 1. Only at the initial stages of deformation the experimental curve runs below the theoretical curve. This may be due, at least partly, to the uneven stress distribution caused by the anisotropy of the crystals. It is now obvious that a similar formula H = Ht- (Ht- He)e ne&apos; [2] might be valid for the relation between the hardness and the strain. The hardness can be only a function of the strain and must therefore be independent on the hydrostatic tension present in the neck during straining. Hence, if Eq 2 is correct it will also represent the relation between hardness and strain in the middle section of the neck, the strain of which is generally assumed to be almost or fully homogeneous. For aluminum, copper, and several copper alloys it is indeed observed that Eq 2 agrees very well with the experimental Vickers hardness-strain relation from zero strain on up to the strain at fracture. Moreover nc&apos; is, for several metals fairly equal to nc- Hence H = C1 + C2S [3] C1 and C2 are constants during uniform uniaxial tension. Eq 3 was also obtained for copper by Voce.3 According to Hencky&apos;s theory4 the ratio of the Brinell or Vickers hardness and the yieldstress (expressed in kg per mm2) of a non-strainhardening metal is approximately equal to 2.8. If Eq 1, 2 and 3 are correct the ratio Ht/S, must accordingly be the same for all plastic metals and be equal to 2.8. It is now experimentally established that this ratio varies between 2.7 and 3.1 with a mean value of 2.9. Taking into account that Ht and especially St can be obtained only by extrapolation from the range of rather low strains, the agreement with the theory is very satisfactory. References 1. J. H. Palm: Appl. Sci. Res. Al (1948) 198. 2. E. Voce: Jnl. Inst. of Met. (1948) 74, II, 537. 3. E. Voce: Metal Treatment (1948) 15, 53. 4. H. Hencky: Zlsch. f. angew. Math. and Mech. (1923) 3, 241.

Jan 1, 1950

By T. A. Wright

THE-Institute of Metals Division opened on Tuesday afternoon with Wheeler P. Davey as chairman and G. E. Edmunds as vice-chairman. Four papers were on the program, two being of a fundamental character. A paper on "Internal Surface in Minerals and Metals," by R. S. Dean and J. Roster, was presented by the latter; C. H. Gottschalk discussed coercive forces in powders. In answer to a question by the chairman. The author stated that he had not investigated [he temperature coefficient of resistance. A paper on "Recrystallization and Grain Growth in Cold Worked Polycrystalline Metals," by L. W. Eastwood, Arthur E. Bousu, &apos;and C. T. Eddy, was presented by Mr. Eastwood. A. great many quantitative data were given, with little reference to the theory. Theoretical considerations were discussed by Dr. Gottschalk, and C. A. Edwards of the University College of Wales, contributed very interesting comment on the relationship of size and critical strain. Dr. Edwards discussed the necessity of considering strain with time and temperature.

Jan 1, 1935

By R. Kossowsky

BRIDGMAN has listed five possible transitions in bismuth at 25°C which were observed as volume changes. He was unable however to detect the last three transitions by electrical-resistivity changes. Kennedy and LaMori have verified the pressures at the Bi 1-11 and Bi 11-111 transitions. They suggested however that the 125-kbar transition previously reported by Bundy3 actually corresponds to the 90,000 kg per sq cm transition observed by Bridgman.1 Jura4 reported a well-defined drop in resistivity at 92 kbar obtained by a four-lead method. The Bi 111-IV and Bi IV-V transitions have not been reported in any of the above-mentioned references.&apos;-&apos; Bundy3 observed a small dent in the low-temperature boundary of the Bi Vll region which is consistent with the presence of a 111-IV boundary. Zeitlin and Bray-man5 were the only ones to report small but well-defined drops in resistance of bismuth at 44.0 and 63.8 kbar, corresponding to Bridgman&apos;s 111-IV and IV-V transitions, respectively. High-purity (99.99 pct) 0.020-in.-diam 0.5-in.-long bismuth wire was used to calibrate the Uniram tetra-hedral high-pressure apparatus used in the present work. The bismuth phase changes at 25°C were correlated with changes in electrical resistance as a function of pressure. The output of a sensitive bridge constructed of carbon resistors and kept at a constant temperature of ±°C during the measurements was fed to the Y axis of a MoseleyX-Y recorder and the X axis was used for time scans. Specimens were pressurized using a hydraulic press with maximum capacity of 200,000 lb. Load was applied in increments of 2000 lb and held for about 3 min. The resistance was recorded at the end of this time period. Good contact was established below 20,000 lb. Typical recorder charts are reproduced in Figs. 1 and 2 which show that resistance fluctuations were practically nil during each time scan. Well-defined discontinuities in resistance were observed at 58,000 and 82,000 lb, Fig. 1. Two small but definite "blips" are noticed at 92,000 and 122,000 lb, Fig. 2. At 156,000 lb another drop is observed which

Jan 1, 1967

By Ralph Hultgren, Bernard York, David W. Mitchell

It is a well-known fact that magnesium-alloy castings are apt to be coarse grained if the melt is not superheated several hundred degrees above the melting point before casting. (The casting temperature varies according to the shape of the mold. A typical casting temperature is perhaps 1400°F.) British practice is to heat to 900°C. (1650°°F.) for 15 min., cool rapidly to casting temperature, and cast.1 In Germany superheating is carried out at 850° to 900°C. (1560° to 1650°F.) depending on the amount of scrap used. It is stated that further refinement will be obtained by prolonging the period of superheating or by increasing the superheat temperature to 950°C. (1740°F.).2 In the United States superheating is carried out at i600° to 1700°F. (871° to 927°C.), perhaps even higher in some places. It is stated that superheating effects are found as low as 1500°F. (816°C.), but several hours are required.3 These commercial treatments lead to grain sizes in sand castings that may vary from 4 to 8 grains per sq. mm.§ in heavy sections and from 60 to l00 in 3-in sections to perhaps 380 in thin sections. It is also generally known that the refining effect of superheating is lost if the melt is held for some time at lower temperatures before casting. Aside from these very qualitative statements, there is little to be found in the literature as to the effect of temperature and time of superheat on the final grain size. Because of the uncertainty of these factors, the Office of Production Research and Development of the War Production Board placed a research contract with the University of California, supervised by the War Metallurgy Committee. This research, which was done under the "Restricted" Project NRC-550, is the basis of this paper, which has been released for publication by the O.P.R.D. The material studied was an alloy prepared from carbothermic magnesium. The temperatures required for grain refinement proved to be widely different from those used in practice, as described in the statements in the first paragraph. This difference is attributed to the fact that the magnesium in the specimens was of carbothermic origin instead of the electrolytic magnesium in common use. MATERIALS AND METHODS The magnesium alloy studied was one of the most popular sand-casting alloys, with a nominal composition of 9 per cent aluminum, 2 per cent zinc, and 0.r per cent (minimum) manganese and the balance magnesium. This is designated

Jan 1, 1945

By Ralph Hultgren, Bernard York, David W. Mitchell

It is a well-known fact that magnesium-alloy castings are apt to be coarse grained if the melt is not superheated several hundred degrees above the melting point before casting. (The casting temperature varies according to the shape of the mold. A typical casting temperature is perhaps 1400°F.) British practice is to heat to 900°C. (1650°F.) for 15 min., cool rapidly to casting temperature, and cast.&apos; In Germany superheating is carried out at 850&apos; to 900°C. (1560° to I650°F.) depending on the amount of scrap used. It is stated that further refinement will be obtained by prolonging the period of superheating or by increasing the superheat temperature to 950°C. (I740°F.).2 In the United States superheating is carried out at 1600&apos; to 1700°F. (871&apos; to 927°C.), perhaps even higher in some places. It is stated that superheating effects are found as low as 1500°F. (816°C.), but several hours are required.3 These commercial treatments lead to grain sizes in sand castings that may vary from 4 to 8 grains per sq. mm.! in heavy sections and from 60 to IOO in 1/2-in. sections to perhaps 380 in thin sections. It is also generally known that the refining effect of superheating is lost if the melt is held for some time at lower temperatures before casting. Aside from these very qualitative statements, there is little to be found in the literature as to the effect of temperature and time of superheat on the final grain size. Because of the uncertainty of these factors, the Office of Production Research and Development of the War Production Board placed a research contract with the University of California, supervised by the War Metallurgy Committee. This research, which was done under the "Restricted" Project NRC-550, is the basis of this paper, which has been released for publication by the O.P.R.D. The material studied was an alloy prepared from carbothermic magnesium. The temperatures required for grain refinement proved to be widely different from those used in practice, as described in the statements in the first paragraph. This difference is attributed to the fact that the magnesium in the specimens was of carbothermic origin instead of the electrolytic magnesium in common use. Materials and Methods The magnesium alloy studied was one of the most popular sand-casting alloys, with a nominal composition of 9 Per cent aluminum, 2 per cent zinc, and 0.1 per cent (minimum) manganese and the balance magnesium. This is designated

Jan 1, 1945

By Alvin Kaufrnan

This chapter will deal with the policy issues relating to mineral land disposal. The first portion of the chapter will discuss in general terms the legal systems utilized in disposing of mineral rights and the major problems encountered; the second section will comprise an analysis of the policy alternatives with emphasis on the pricing aspects. In this section, we are not attempting to provide a legal text, but simply to outline very briefly and sketchily the details of the systems. More detailed information can be obtained by contacting the appropriate governmental agency for specific information. Mining laws throughout the world are based on two major legal groupings: English Common Law and the Civil Law. These basic systems are often modified by Islamic Law and by negotiated -mixtures of these. Under English Common Law, which is embraced by the United States, Canada, and many of the members of the British Commonwealth of Nations, individuals can hold property and can extract minerals from it. The owner can dispose of minerals as he sees fit, either through contract, deed, or whatever other system is appropriate. CIVIL LAW Under Civil Law (also known as Regalian Law), mineral ownership is normally placed in the state, regardless of who owns the surface. This legal system applies in most European countries and their former colonies. It is derived from Roman law. The mineral deposits, thus, are worked under concessions. Most countries use a negotiated concession system and sometimes a combination of negotiation and competitive leasing. The negotiated system has advantages as well as disadvantages for both government and industry. In a system where the government administratively determines who is to get what, the concessions are normally large. Frequently they range up to several millions of acres and involve a considerable investment on the part of the concessionaire. There is no duplication of effort on the part of producers to obtain information, since a single concessionaire controls a given area. Consequently, less money is spent in toto because several prospective operators are not required to seek the same information. The system also has the advantage to the industry of permitting the concessionaire to select and retain the best producting area. Thus, major developmental expenditures are made on the production unit only, with a resulting reduction in the risk factor. The large initial size of the concession also minimizes the possibility of expending a large bonus payment for a barren property. The major governmental advantage of a concession is its flexibility in accomplishing other national objectives. For example, a lease could be negotiated at less than fair market value, but requiring substantial de-

Jan 1, 1976

By K. P. Gupta

In ternary systems containing silicon and transition elements, silicon was found to stabilize the a phase.1 At 1000°C a broad a-phase region was found in the Cr-Mn-Si system,1 which extends very close to the Mn-Si binary line (within about 3 at. pct Cr). Later investigation showed that, if chromium was replaced by small amounts (3 to 5 at. pct) of v,1 Ti, Nb, Ta, Mo, or w,1 the a phase or the R phase was again stabilized. Whether stabilization of complex crystal structures is possible by small additions of iron, cobalt, or nickel to Mn-Si is not known. Investigation of the Co-Mn-Si system4 shows the presence of several ternary phases, but at cobalt concentrations higher than 10 at. pct. In the present work the ternary systems Fe-Mn-Si and Co-Mn-Si were investigated at low iron and cobalt concentrations (< 7 at. pct Fe or Co) in search of phases of complex crystal structure. Experimental Procedure. The alloys were pre-pared by induction melting Co (99.8 pct), Si (99.9 pct), electrolytic Fe (99.88 pct), and Mn (99.9 pct) in recrystallized alumina crucibles under an inert atmosphere of argon gas. The alloy specimens were wrapped in molybdenum foil, sealed in argon-filled (at 1/2 atm) silica capsules and annealed for 72 hr at 1000" 1°C, and water-quenched. The use of argon-filled capsules was found to reduce the losses during annealing and the molybdenum foil prevented reaction of the manganese with silica. The total weight loss due to annealing and melting was found to be less than 1 pct for each alloy. The alloys were not analyzed chemically. A part of each annealed specimen was polished and examined metal-lographically using etching solutions, a) 0.1 to 0.5 pct oxalic acid solution in water, or b) 0.5 pct HNOs in methyl alcohol. Even though the etching solutions were quite dilute, the specimens were heavily etched and stained if the etching time exceeded more than 5 sec. Etching times found suitable were usually 1 to 3 sec. For X-ray diffraction work, a part of each annealed specimen was powdered by crushing after the exposed surface was ground off. X-ray diffraction patterns were taken with powder specimens using a 20-cm-diam asymmetrical focusing camera and Fe K radiation. These powder patterns were found quite satisfactory for the purpose of phase identification. However, X-ray diffraction patterns of single-phase alloy powder specimens were also taken using a Siemens diffractometer and filtered Cr-Ka radiation for greater resolution of the diffraction lines. Results and Discussion. In the Fe-Mn-Si system a new ternary phase was found at 1000°C between the p manganese and the MnsSi phase regions. The approximate phase relationships in this region of the 1000°C isothermal section are shown in Fig. 1. The new ternary phase, designated as the K phase, was found to occupy a narrow region about 1 at. pct in width and extending from Fee.oMn74.5Silg.5 to Fe.Mn.Silg.. At the high-iron content region, the K phase was found in equilibrium with the p manganese and the MnsSi phases but, at the low-iron content end of the K-phase region, the phases in equilibrium with the K phase were the p manganese phase, the MnsSi phase, and another new phase, designated in Fig. 1 as the v phase. The v

Jan 1, 1964