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By Frederic E. Carter

There have been many attempts to prove that platinum was known to the ancients, but since no traces of the metal have been found in the relics of early times, it must be concluded that it was not known to them. As far as records go, it was actually first discovered in the 16th century in a Spanish mine on the Pinto River in South America; from which source it received its name of Platina del Pinto (little silver from the Pinto). It was more or less of a rarity and was a subject of interest to a few chemists only, until the year 1822 when the metal was first discovered in Russia. In 1819 there were noticed in the washings of the gold sands of the southern part of the Ural Mountains, grains of a heavy white substance, but it was not until three years later that this substance was found to contain platinum. While at first the amounts of platinum brought from the Urals were meager, prospecting soon disclosed rich deposits extending over a considerable area, and nuggets from 10 to 20 lb. were by no means rare. This discovery assured to chemists an ample supply of platinum for their crucibles, etc. The ore is now found in various parts of the world but the richest deposits are still found in the Ural Mountains. The platinum of commerce is obtained entirely from alluvial deposits at depths varying from 6 to 40 ft. The sand and gravel of former river beds are subjected to a series of screenings and washings to effect the separation of the ore. Actually, probably all gold-bearing gravel beds of the world contain platinum, and it is more than likely that large quantities of platinum ore have been thrown away with the black sand washings from gold placer deposits. This is especially true of the alluvial deposits of the Pacific Coast in California and Oregon. Platinum ore is usually found in the form of rounded or flattened grains of "sand," and occasionally in irregular lumps of the size of peas. Large nuggets are very rare. The ore has a metallic luster and is distinguished by its steel gray color, but shows light gray streak when rubbed on a hard white surface; it has a high specific gravity, 16 to 19; is infusible in the hottest blast furnaces, and insoluble in any single acid. Platinum ore is a complex body consisting of the metal in combination with varying proportions of the other members of the platinum group; iridium,

By Erwin L. Zodrow

A geological model of the modes of formation of magnetite and its distribution in the Smallwood iron-ore mine, Labrador, Newfoundland, is given, based on observation and geological mapping. This is called the conceptual model. If mathematical expressions plus probabilistic uncertainty are used to represent the conceptual model, then this is termed a mathematical model. The purpose of this paper is to test if there exists a correspondence between the conceptual model and two related mathematical models (called factor analysis). Details of the statistical technique are given. The results of factor analyses in relation to the magnetite formations in the Smallwood mine are discussed. Several practical mine applications are presented. The difficulty of maintaining quality control over ore mined from any deposit naturally depends on geological conditions; these are usually imperfectly known to concerned mining geologists. One geological condition that would greatly facilitate ore predictions is if a relationship between the observed ore particle distribution* and its mode of origin could be demonstrated. Such a casual interrelationship is normally sought through the application of well-defined geochemical principles of primary mineralization in given geological environments. However, the application of conventional tools of geological research, including geochemistry, to areas that have undergone repeated periods of geological deformation and metamorphism subsequent to primary mineralization becomes rather difficult. More important, the interpretation of such research results are nearly impossible on an objective basis. Mineral assemblages may have been reworked and changed due to tectonic influences to the extent that the present-day observable mineralogy and ore-particle distribution can effectively obscure the mode of origin of the ore. Quantitative measurements, based on petrological investigation of mineral assemblages, reflect the sum-total of all geological influences. Which of several influences had the most effect on existing ore particle distribution is difficult to assess, for these influences can neither be measured directly nor quantified by petro-logical logical or geochemical means. The present study is concerned with the magnetite distribution and its modes of origin within the Small- wood mine,' located in the southern extension of the Labrador geosyncline; see Fig. 1. This geosyncline is thought to have undergone at least two periods of geo-tonic tectonic deformation, separated in time, since the fer-rugenous rugenous sediments were deposited." Detailed geological observations and mappings (1 in. to 40 ft) have highlighted subtle, distinctive features of the magnetite distribution in the Smallwood mine: (1) The magnetite is generally concentrated in bands or layers within this ore body; these bands alternate with specularite-rich bands and quartz bands. The banded or layered nature is common in Precambrian iron-ore deposits, and this has been interpreted as a result of changes in depositional environments. (2) The grain size of the magnetite varies; near the contacts between the iron and quartz-carbonate formations, the magnetite occurs as well-crystallized octa-hedra. In areas of intense folding, magnetite is extremely fine grained and concentrated in bands and occurs in association with earthy manganese minerals. (3) Magnetite tends to be more highly concentrated near the geological contacts of the iron and quartz-carbonate formation in the northeast part of this mine, Figs. 2, 3, and 4. (4) Magnetite is also fine grained and tends to higher concentration near and parallel to fold axes; however, in this case, the ore is much softer than given in item 2. (5) Magnetite mineralization decreases along strike and away from the areas of intense folding, i.e., towards the approximate center of the mine, Fig. 3. How can these variations of magnetite be explained on a geological basis? We can postulate a conceptual model that the distribution of magnetite appears to be related to three basic geological influences: (1) geo-tectonics, i.e., concentrations of magnetite near geological contacts of the iron and quartz-carbonate formations, the fine-grained nature of magnetite and its higher concentrations near fold axes, and decrease of magnetite towards the approximate center of the mine; (2) secondary alterations, i.e., variation of grain size of magnetite near the iron and quartz-carbonate contacts, and in areas of intense folding where magnetite occurs together with earthy manganese minerals: (3) original

Jan 1, 1971

By J. H. Jackson, P. D. Frost, C. H. Lorig, A. C. Loonam

THIS paper describes (1) the effect of sodium on the tensile ductility of magnesium-lithium base alloys, and (2) the precautions necessary to avoid sodium contamination. Effect of Sodium on Properties The harmful effect of sodium in magnesium-lithium base alloys has been recognized by other investigators.1,2 However, quantitative data on its effect have not hitherto been published. The effect of sodium on the ductility of an 87 pct Mg-9 pct Li-4 pct Zn alloy is shown in fig. 1. The sodium was introduced by adding sodium chloride to the flux, which consisted of 50 pct LiC1-50 pct KC1. Moderately high ductility was obtained at an indicated sodium content of about 0.05 pct. Actually, the value probably was less than 0.05 pct, be-cause analyses of the lithium, which were more accurate than those of the alloy, indicated that the highest ductility was obtained when its sodium content was 0.02 pct or less. In fact, in alloys having somewhat greater strength than this particular composition, the sodium content of the lithium must be under 0.01 pct to avoid embrittlement. The effect of sodium on the ductility of several alloys having fairly low strength levels is shown in fig. 2. These alloys were melted with a flux containing 75 pct LiC1-25 pct LiF, to which various quantities of sodium chloride had been added. Sodium had no significant effect in pure magnesium but markedly decreased the ductility of the magnesium-lithium-zinc alloy, even though the alloy contained only 3 pct Li. As the lithium content of the binary alloys was increased, the ductility of the sodium-free alloys also increased. However, the effect of sodium on ductility became progressively more pronounced. Sodium raised the minimum hot-rolling temperatures, particularly those of the high-strength alloys, but its effect, in this respect, was less critical than its effect on tensile ductility. For optimum cold roll-ability, a low-sodium content was required. No deleterious effect of sodium on the stability of properties at slightly elevated temperatures was found. Control of Sodium in the Alloys Optimum ductility is obtained in the magnesium-lithium base alloys when sodium-free materials are used. Commercial lithium was formerly the chief source of contamination. Now purified lithium is usually available. When lithium of ordinary purity is used, the effects of sodium can be minimized by using a flux consisting of 75 pct LiC1-25 pct LiF. Bubbling nitrogen through the melt also helps remove sodium. The damaging influence of sodium on the ductility of the magnesium-lithium base alloys was observed very early in the alloy development program. The discovery came about as a result of chemical analyses made on the lithium used in the alloys. Ductile alloys had been made from lithium containing about 0.2 pct Na, whereas the lithium used in the brittle alloys contained about 0.9 pct Na. The first magnesium-lithium alloys were melted under commercial fluxes ordinarily used in melting magnesium alloys. These fluxes were unsuited for scavenging the contaminating sodium, and the resulting alloys were not ductile. Next, a flux containing 50 pct KC1-50 pct LiCl was tried. This was somewhat more effective but still was not satisfactory. After a number of different experimental fluxes had been investigated, one containing 75 pct LiC1-25 pct LiF was adopted. This flux made it possible to obtain good ductility in the alloys. The

Jan 1, 1951

By Noel Jarrett, Allen S. Russell, Bernard M. Starner, Stanley C. Jacobs

A process has been developed to refine high-grade commercial aluminum to 99.99 pct purity. This enzploys precipitating titanium, vanadium, and zirconiu~ as borides. The upgraded liquid is partially crystallized under conditions that prevent massive freezing. The resulting crystals are compacted and washed free of adhernig impure liquid aluminum by melting the top crystals while draining off the liquid. Finally, the bottorn portion of the crystal bed is melted and removed as the pure product. Leakage from the crystallizat~on vessel is prevented by a layer of alumina granules that are not wetted by the aluminum. ALUMINUM of 99.99 pct purity is desired in a variety of applications. These include electrolytic capacitors, catalyst carriers, decorative trim for automobiles, aluminum powder, and high-strength alloys. This market was for many years filled by refining commercial-purity aluminum in a three-liquid-layer electrolytic cell of the type originally proposed by Hoopes. To meet the expanding need for lower-cost high-purity aluminum, a refining process based on chemical precipitation and fractional crystallization was developed. The availability of this super-purity metal was announced in November 1961, and three patents1-3 relating to the process were issued in 1965. An alternate process, comprising continuous fractional crystallization of a portion of a liquid-aluminum feed stream under conditions of strong agitation at the surface of the growing crystals, was published by Dewey4 in 1965. Earlier proposals by Larsen 5 and by Regner6 also emphasized the advantage of rapid agitation of the melt in the region of the crystallization zone. johnson 7 more recently proposed extracting purified aluminum from an alloy by mixing crystals of pure aluminum into the molten alloy, allowing them to grow, and removing the pure aluminum as by casting. Aamot's 8 recent patent describes a freeze refining process that involves controlled partial freezing against cooled moving retort walls. The Alcoa process to produce high-purity aluminum is schematically described in Fig. 1. Relatively pure aluminum is treated with boron in a furnace (a) to precipitate high melting point impurities, the supernatant liquid is transferred to a crystallization vessel (b), the liquid is partially crystallized with mechanized "tamping" (c), the remaining impure liquid is tapped out and the crystal bed partially and directionally re-melted to wash the underlying crystals (d), and the balance of the crystals is melted and withdrawn as high-purity aluminum (e). PRINCIPLES OF FRACTIONAL CRYSTALLIZATION Commonly encountered impurity elements form two types of systems with aluminum. Titanium, vanadium, and some other transition elements in periodic groups IV, V, and VI are the high melting point impurities. Initial solidification of aluminum containing small percentages of these elements will produce solid markedly enriched in them at temperatures slightly above the freezing point of high-purity aluminum. Most other elements, such as silicon and iron, produce eutectic type reactions with aluminum. In this case the first solid formed on initial solidification at temperatures slightly below the freezing point for high-purity aluminum is markedly depleted while the remaining liquid is enriched in these elements. The equilibrium change in composition during solidification of aluminum contaminated with silicon, iron, or titanium is illustrated in Fig. 2. Here, for clarity, the temperature scale is expanded beyond the

Jan 1, 1968

By Dorsey Hager

The possibility of oil and gas production in Alabama his been little considered as yet. Gas and some oil have been found in northwestern Alabama, near Birmingham, in the Pennsylvanian beds, but the oil and gas possibilities in the Cretaceous beds are not generally appreciated. The recent activity of oil companies in that State has attracted much attention, and in this paper the main structural and the general strati-graphic features are described. Four favorable areas are outlined. These contain folds of major interest. There are other favorable areas which have not been mapped-l Commercial pools discovered in this area would have the advantage of being near tidewater. Mobile, Ala., on the Gulf of Mexico, would be the logical site for refineries and shipping facilities. A pipe line could readily be laid to that city from the Hatchitigbee and the Jackson areas. The logical outlet for the Geneva and the Gordon areas would be Panama City, Ha., on the Gulf of Mexico. Topography The whole of the area under consideration lies in the Gulf coastal plain and slopes gently to the southwest and west. The elevations vary from 200 to 400 ft. (60 to 121 m.) above sea level. The streams have sunk their channels into this gently sloping plain, the main drainage flowing south or southwest into the Gulf of Mexico. Between the

Jan 1, 1918

By R. H. Hiltz, N. J. Grant

Solid-solution titanium-cerium alloys, cold-rolled to 0.010 in. thickness, and annealed, were internally oxidized to produce a fine dispersion of CeO2 in the titanium matrix. The oxidized alloys were cut into sheet stress-rupture specimens and tested for rupture life at 426°C, 538°C, and 648°C. There was noted an improvement in strength over that of pure titanium, the internally-oxidized alloys showing curves with a much flatter slope on the log stress—log rupture life plot, characteristic of the stable metal-metal oxide class of alloy. DURING the past 3 to 4-year period, considerable interest has been aroused by the potential offered by alloys based on the ultra fine dispersion of a hard insoluble phase in pure metals or solid-solution alloys for use at high temperatures. The impetus to the development and study of such alloys was provided by Irmann.1,2 through the success of the SAP alloy (pure aluminum containing about 12-14 volume pct of A12O3). Subsequent studies have thrown light on the true potential of this class of alloys in the remarkable stability of the structure after long-time exposure at high stresses and high temperatures.a-5 While success has been demonstrated in the special case of the A1-Al2O3 alloys, and more recently

Jan 1, 1959

By W. C. Ellis, E. S. Greiner

WHEN metallic materials are deformed plastically, the process may be considered as one in which hardening and recovery occur simultaneously. The net hardening is that produced by deformation in the absence of recovery lessened by recovery during and immediately following deformation. Strain hardening takes place through movements of large groups of atoms acting to a degree as an entity. A complex microstress system is developed. Recovery is a diffusive-type process involving single atoms or, at most, only a few atoms in concerted action. This is accompanied by elastic strain relaxation. Recovery is strongly temperature-dependent. The driving energy for the process resides in thermal fluctuations of the atoms augmented by the energy of the stress field producing the deformation, and by that produced by the deformation. At very low temperatures recovery is essentially absent, or very small. At high temperatures in the hot working range, recovery is so rapid that deformation results in no appreciable net hardening. The interplay of strain-hardening and recovery results in differing end structures depending on the temperature and the strain rate of the process. For example, there is a prominent difference in the spacing of the slip markings and in the detail of X-ray diffraction patterns. High temperatures and slow strain rates favor a wide spacing of slip markings and sharp reflections.',' This suggests that change in rate of the recovery concurrent with deformation modifies to a degree the manner of the deformation. Different slip systems may operate. For very slow rates, the mechanism may, as has been suggested, differ from that of "classical slip." In the experimental work that follows the findings will be interpreted from the point of view developed in this section. Recovery and Electrical Conductivity Electrical conductivity is a sensitive indicator of the state of strain in a material3' * and was used in this investigation. The materials studied in wire form were: OFHC copper, a high purity (99.99 pct) and 2s grade aluminum, and grade A nickel. Wire annealed and initially 0.050 in. in diam was drawn through diamond dies in a simple holder maintained at 25", —75°, or — 195°C. Precautions were taken that for each material all conditions of drawing were the same except the temperature. Electrical resistivity was measured for each condition at 20°C. This was done as soon as practical after drawing to minimize possible room temperature recovery. The data for the four materials are plotted in Fig. 1 in terms of the change in resistivity for drawing at the several temperatures. The effect of temperature of drawing on the increase in resistivity is most pronounced for copper. Drawing at 25°C to 80 pct reduction in area increases the resistivity approximately 2 pct; drawing at —195°C to the same reduction increases the resistivity about 6 pct. The increase in resistivity" & in this metal is due to extra scattering of conduction electrons originating in the lack of orderly arrangement of the atoms induced by the deformation process. It has been suggested

Jan 1, 1953

By R. Maddin, W. R. Hibbard

A series of X ray experiments conducted by G. I. Taylor' in 1927 and later substantiated in 1939 by J. A. Collins2 both on axially strained aluminum single crystals, revealed evidence that during single slip crystallite rotation occurs in such a manner that " all parts of the material rotated about the transverse direction in the plane of slip."l The actual method of preparing the specimens for X ray examination is not discussed in detail by Taylor except to say that "this specimen was cut parallel to the plane of slip, as calculated from measurements of marks in the surface of the specimen. It was ground and etched till the effect of the new cuts had disappeared. This was verified by applying the same treatment to an un-distorted specimen. The X ray reflectionsl in this case were perfect ones."' Collins, on the other hand, cut his crystals in a mechanical shaper. These surfaces were polished on No. 1, No. 1/0, No. 2/0 and No. 3/0 papers and on a broadcloth lap using No. 600 alundum as a polishing medium. "Finally, the surface was deeply etched in Tucker's reagent. An unde-formed crystal was prepared in the manner described and X rayed to determine whether or not the machining and polishing operations had produced any strain or distortion in the crystal. The Laue spots all seem to be sharp, free from tails and streaks indicating no detectable strains had been introduced in the crystals." Taylor's X ray technique involved the use of "homogeneous X rays from an iron anti-cathode"; whereas Collins used Ka radiation of copper at 31kv and 20 milliamperes. Glancing angle X ray photograms were taken (1) with the axis of rotation of the spectrometer table in the plane of slip and at right angles to the slip direction, and (2) with the axis of the spectrometer table lying along the slip direction. However, eight minute exposures were used in each case and the angle setting of the spectrometer table was increased by one degree for each exposure. With the discovery of the action of three slip systems3 in the plastic deformation of single crystalline alpha brass where, formerly, only one had

Jan 1, 1950

By Wallace Ralston

The East Texas area includes the northeast 38 counties of the state of Texas. It covers all, and extends beyond, the borders of what is commonly described as the East Texas Basin. It is one of the most important oil and gas-producing areas of the Mid-Continent Province. It includes four important oil fields—Van, East Texas, Cayuga and Long Lake— and the recent extension of Rodessa field into Cass County, Texas, may prove to be of major size. Four commercial gas fields are in this area— Bethany, Waskom, Cayuga and Long Lake. Up to January, 1936, all of the oil has been produced from the Upper Cretaceous formations, and most of that from the basal member, the Woodbine sand. Gas is produced from both the Upper and Lower Cretaceous formations. Development in Fields East Texas Field.—This field continued to dominate the drilling and production situation throughout the United States. There were 4036 wells completed in this field during 1935; that is, 365 more wells than were completed during 1934. Drilling activity was due to close spacing of wells and the addition of 10,000 acres to the field. The field is now drilled to a density of one well to 6½ acres, which is certainly more wells than necessary for economic production of the field. The close spacing of wells is due mostly to the type of proration, which is per well allowable based on a potential test, and does not take acreage into consideration, and also to the numerous small acreage tracts such as town lots and excess strips. The field now has 19,519 producing wells. The allowable production for the field during 1935 was 161,118,659 bbl.; estimated production, including illegal or "hot oil," was 174,200,150. The illegal production of oil gradually decreased throughout the year, until an estimated low was reached of 20,500 bbl. daily during the months of November and December. The price of oil remained at $1.00 per barrel throughout the year. As stated, about 10,000 acres were added to the field during the year, making a total of 128,000 productive acres. There is a possibility that

Jan 1, 1936

Discussion of the paper of GEORGE S. RICE and H. H. CLARK, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin No. 94, October, 1914, pp. 2563 to 2571. NORMAN V. BRETH,* Pittsburgh, Pa.-It was my privilege to visit in the last two months on behalf of the U. S. Bureau of Mines 10 mines where electric shot-firing systems controlled from outside the mine are installed. I will describe briefly what I saw in some of these mines, which are located in Utah, New. Mexico, Oklahoma, Alabama, and Kansas. At a mine in Utah, 230-volt alternating current is used to fire the shots, which is taken from a small transformer in the substation. The shot-iring circuit is independent of all other wires and is tested for grounds every day. There are no lightning arresters on the firing circuit. Porcelain insulators are used inside of the mine, and glass outside. The switches are situated as follows: One in the substation, one in, the shot-firer's cabin, two at each cross entry; where the shot-firing circuit crosses the trolley wire a switch is placed on either side of the entry in series with the shot-firing circuit. The miners are checked in and out of the mine. The coal is undercut and is shot down with permissible explosive, the shots being connected in multiple. There are 75 to 110 shots fired each day. A great many times there are no missed shots. If not more than two or three are missed they are left until next day. The fan is kept running at full speed when the shots are fired. The shot-firing switch is closed only once and the whole mine is shot at once. At another mine in Utah, power wires are used for shot-firing circuits; 500-volt, direct current is used to fire the shots. The only sizes of wire used outside of the power wires are Nos. 8 and 14 B. & S. gauge. The return is connected to the pipe lines and track. Porcelain insulators are. used inside of the mine.

Jan 4, 1915

By P. Barnes

The tabular statement accompanying this note shows the money cost in each of the three departments of manufacture, of 17 leading items, and also the proportion (expressed in a clecimal fraction) which each of these items bears to the total cost. The statement can hardly be taken for more than an average illustration of the clear showing of ratios and of results which may be made by such an arrangement, for not only will these items vary from month to month in any given works, but the methods themselves of manufacture differ widely in different works. It is obvious that such a statement, however useful it may be, must be submitted with but exceedingly little explanation or discussion, or with none at all, for the reason that to enter at any satisfac-

Jan 1, 1879

By Klaus Detert

Fifteen and 18 pct Ni maraging steel and several binavy and ternary alloys of the iron-rich corner of the Fe-Co-Ni system have been studied. After annealing in the austenite range, these alloys were deformed slightly by cold rolling and subsequently aged. Compavison of experimental measurements at various processing stages indicates that small degrees of deforn~ation (5 to 10 pct reduction in thickness) do not influence hardness and strength or the aging kinetics. Electrical resistivity and ductility are somewhat redu]ced and the coercive force is substantially lower when compared to identical samples which were not deformed. The results are explained in terms of retained austenite which transforms into martensite with the small amount of deformation. RECENTLY there has been increasing interest in maraging steel for applications in electric power generators requiring a high ratio of power to weight.' Fifteen pct Ni maraging steel has been investigated to evaluate its properties and performance for application as high-strength magnetic rotor steel,' and a thorough investigation of the precipitation and transformation processes in this alloy has been conducted in this laboratory.3 The influence of deformation, which preceded the aging treatment, was also studied. It was found that a small deformation in the order of 5 pct has a rather striking effect in reducing the coercive force. Other interesting effects on the properties caused by such deformation have led to the more detailed studies reported herein. EXPERIMENTAL METHOD The methods used to produce the samples from 15 pct Ni maraging steel have been described elsewhere.3 The general procedure of hot forging and cold rolling to sheet has been followed. The composition is included in Table I which also contains the composition of the 18 pct Ni maraging steel grade 250 studied. More data about the material and the processing of the 18 pct Ni maraging steel have been recently reported.4 The experimental alloys of binary and ternary Fe-Ni-Co alloys were made by levitation melting in an argon atmosphere and casting into rod-shaped ingots 7 mm thick weighing 20 g. From these ingots 25-mm-long rods were machined to study the phase transformation by a dilatometer. These rods were then cold-rolled to strips, 2.4 mm thick. Annealing for austenitizing was done in tube furnaces in an argon or helium atmosphere followed by cooling in the water-cooled portion of the tube. Aging was done in a salt bath containing a neutral blend of Alkali nitrates and nitrites. Vickers hardness was measured using a load of 50 kg for 15 sec. Tensile tests were carried out on a hard beam tensile tester at a strain rate of 5 X lo-' per sec using flat samples with a gage length of 37.5 mm and a cross section of 1.25 by 6.25 mm. Estimated sensitivity was 5 K x strain and 0.35 kg per sq mm stress. Magnetic saturation was determined on small cylindrical samples, 2.5 mm in length and diameter, by measuring the force exerted by the gradient of a magnetic field of 1000 oe per cm in a mean field of 11,500 oe. The measured values could be reproduced within *1 pct. Coercive force was measured by a precision-type magnetic field probe in a magnetic coil as described by Foerster.5 The magnetizing field was 1300 oe. The samples were 5 cm long, 1 cm wide, and 2.4 mm thick. he coercive force was measured to within +0.1 oe. Electrical resistivity was measured by using a potentiometer on flat strips with a gage length of 100 mm and a cross section of 2.5 by 0.5 mm. The accuracy of the measurement was 0.1 pct but the reproducibility of the measured specific resistivity among different samples was in the order of 1 pct. The method used to prepare the samples for electron transmission has been reported elsewhere.3 RESULTS Fig. 1 shows the influence of deformation after annealing on the resistivity, hardness, and coercivity. The samples were annealed for 30 min at 1000"C,

Jan 1, 1968

By Peter Beardmore, Michael B. Bever

The effects of the temperature of deformation and the degvee of deformation on the annealing spectrum of a Au-Ag alloy have been determined by vesistance measurements. Specimens were deformed in torsion at 4°, 78K and room temperature up to strains nd/l of about 1.0 and were isochronally annealed. Discrete annealing stages similar to those found for pure metals were observed. Stage A occurred below room temperature; the decrease in reszstance associated with this stage increased as the temperature of deformation was lowered or the strain was increased. Stage B manifested itself as an increase in resistance; this is attributed to the restoration of short-range order promoted by vacancy or vacancy aggregate migration. At temperatures above 48S0K, recrystallization or Stage C occurred. Stages A, B, and C in the annealzng curves of this alloy may be considered to correspond to Stages II, Ill, and V, respectively, in the terminology used to describe the annealing spectrum of pure metals. ThE annealing behavior after deformation below room temperature has been thoroughly investigated on pure metals, in particular gold and copper. The occurrence of several discrete stages in the annealing spectrum of these metals has been established, but the interpretation of some of these stages in terms of specific mechanisms is still controversial.' The annealing of alloys deformed below room temperature has been the subject of only a few investigations. In the investigation reported here, a Au-Ag alloy was annealed after deformation at and below room temperature. This continues a research program on the deformation and annealing behavior of Au-Ag alloys.2-8s EXPERIMENTAL PROCEDURE An alloy rod of composition 82.6 wt pct Au-17.4 pct Ag was reduced to wire, 0.0428 in. diam, by swaging and drawing. After a recrystallization treatment, the grain size was 0.031 mm, as obtained from the average linear intercept.7 The ends of wires about 6 in. long were flattened and sealed into short brass tubes with cold setting cement to form the grips of the torsion specimens. The equipment used for deformation has been described elsewhere.6 The specimens were deformed at room temperature, 78", and 4°K to various strains nd/l, where n is the number of turns, d the diameter of the specimen, and 1 its length between grips. The strain rate ?max was 0.1 min-' at the sur- face of the specimen except where noted otherwise. The specimens were annealed isochronally for 30 min at intervals of approximately 30°K from the temperature of deformation to approximately 800°K, except that after deformation at 4°K the lowest annealing temperature was 78°K. A potentiometric method was used to measure the resistance: all measurements were made at 78°K with the exception of some measurements at 4°K mentioned below. Data obtained with a single specimen yielded a complete annealing curve: in several cases duplicate specimens were used to confirm the reproducibility of the curves. Since the surfaces of the specimens were rough after deformation, their diameters could not be measured accurately. The resistance increments after deformation and annealing are therefore reported as percentages of the resistance of the same specimen measured after completion of the annealing, that is, after full recrystallization. The corresponding resistivity values can be calculated by obtaining the effective diameter of a deformed specimen from the ratio of its resistance after recrystallization to the true resistivity, which was determined with a smooth specimen of known dimensions. This method of calculation was used to obtain data shown in several of the figures. RESULTS AND DISCUSSION The isochronal annealing curves after deformation to various strains at 4", 78K, and room temperature are shown in Figs. 1, 2, and 3, respectively. The resistance increment of the as-deformed specimens as a function of strain is shown in Fig. 4. For the specimens deformed at 4°K. values measured at 78°K are plotted with the exception of those for the as-deformed

Jan 1, 1970

By W. O. Philbrook, R. S. Kaplan

Rates of oxidation were studied for levitation-melted samples of Fe-C, Fe-Si, Fe-C-Si, Fe-C-P, Fe-C-Mn, and Fe-C-S alloys oxidized by mixtures of either 5 or 10 pct O2, in helium at several temperatures in the range 1850o to 2050°C. The concentrations of the oxidized elements decreased linearly with time. Mass transport in the gas phase was found to be the rate-controlling step. Ilowever, a mulliple -film model was necessary to account for the flux of iron and manganese vapor counter to the oxygen flow. THE advent of the basic oxygen and spray-refining processes of steelmaking has generated considerable interest in the kinetics of reactions between oxygen-bearing gases and liquid iron alloys. The object of this research was the determination of the role of mass transport in the gas and metal phases and of surface chemical reactions in the overall oxidation process. Of the reactions for elimination of elements dissolved in liquid iron, the oxidation of carbon has been investigated most extensively. Studies by Fuji and Ura,1 Fuji,' and Gunji et a1.,3 done with pilot-scale basic oxygen furnaces, indicated that mass transport of gaseous oxygen was rate controlling when the metal carbon content was greater than 0.15 to 0.30 pct. When the carbon content was less than this critical amount, diffusion of carbon dissolved in the iron was thought to be rate limiting. L. A. Baker et a1.4,5 levitated samples of iron-carbon alloys and oxidized them in CO-CO2, CO-C02-He, and O2-He atmospheres at 1660°C. These investigators found that the metal carbon concentration decreased linearly with time and their samples exploded when the carbon content fell below about 0.8 pct. They concluded that the rate-limiting step was the transfer of oxidant to the gas-metal interface. A model based on this rate-limiting step predicted decarburization rates within a factor of two of those experimentally observed. The explosion of the samples was attributed to a shift in rate-controlling step from gas-phase mass transport to transport of carbon dissolved in the metal. L. A. Baker and R. G. ward6 and R. Baker7 used freely falling droplets to investigate oxidation kinetics. In both papers, the authors speculated that flame fronts may have been partially responsible for the lack of better agreement between experiment and theory. Swisher and Turkdogan8 oxidized liquid iron having an initial carbon content of 0.97 pct with CO-CO2 and CO-C02-Ar mixtures at 1580°C. They concluded that a surface reaction was the rate controlling step. Iron-silicon alloys have been oxidized by R. Baker7 and Filipov and Martynov.9 R. Baker 7 also studied iron-carbon-silicon alloys falling as liquid droplets through oxygen. He found that the rate of both carbon and silicon oxidation varied inversely with the drop radius. When the initial silicon concentration was greater than 6 pct, the samples cooled during their fall. Manganese oxidation has been studied by R. Baker,7 and by Filipov and Martynov.9 ward10 investigated the loss of manganese from liquid iron under vacuum. He found that mass transport of manganese vapor was rate limiting in argon atmospheres of 0.02 torr to 700 torr pressure. Iron-sulfur alloys were desulfurized with H2-He and H2-Ar mixtures by Peters et al.11 A model based on the transport of H2S from the gas-metal interface into the bulk gas gave fair agreement between the predictions of the model and the experimental results. EXPERIMENTAL TECHNIQUE Essentially, the technique consisted of using helium-oxygen gas mixtures to oxidize levitated samples of liquid binary and ternary iron-base alloys. The fused silica reaction tube is shown in Fig. 1. The coil design is similar to that of L. A. Baker et al.4'5 A Tef-lon-sheathed, ferritic stainless steel lifter (B) and an alumina pedestal (C) were used to support the sample in the coil prior to levitation and for the recovery of the sample. Samples were inserted into

Jan 1, 1970

By R. A. Grange, H. M. Stewart

Man.; steel parts may crack if quenched directly into a bath near room temperature, but not if quenched at a temperature just above the range where martensite forms and then allowed to cool slowly to room temperature. This latter procedure, which is the basis for such modern hardening techniques as "martempering" and "isothermal quenching," may entail some sacrifice in depth of hardening but very little, if any, in intensity of hardening. In planning such treatments, it is necessary to know the upper limit of the martensite range, and often desirable to know the proportion of martensite that would form on cooling to any lower temperature; furthermore, the tendency of a particular steel to crack when quenched is unquestionably associated with the temperature range of martensite formation, and consequently knowledge of this range aids in selecting the optimum composition for a given application. Certain puzzling phenomena associated with the properties of quenched and tempered steel may be at least partly clarified as the manner in which martensite forms is more fully understood. Information on the temperature range of martensite formation, particularly with respect to how much martensite results from quenching to a given temperature, is lacking for most commercial types of carbon and low-alloy steel. These considerations led us to study martensite formation in 14 carbon and low-alloy steels. The resultant data may be directly used in the following ways: (I) for selecting the lowest quenching temperature at which no martensite will form; (2) for selecting the highest quenching temperature at which virtually all marten . site will form, thereby avoiding quenching to an unnecessarily lower temperature with attendant danger of cracking; and (3) in producing a mixture of tempered martensite and bainite, which in high-carbon steels has been found to possess somewhat better ductility than tempered martensite, yet does not require the full transformation time necessary for a completely bainitic (austempered) structure. PART I. OBSERVATIONS OF MARTENSITE FORMATION IN FOURTEEN CARBON AND LOW-ALLOY STEELS Transformation of austenite to pearlite or bainite can be conveniently studied by observing the change that occurs over a period of time at constant temperature; such studies are the basis of the isothermal transformation diagram (S-curve). This isothermal technique is not applicable to martensite formation, which occurs within a time interval too small to measure, at least by any ordinary means. For all practical purposes, therefore, martensite may be regarded as forming only during cooling and not during a period of time at constant temperature. As austenite is cooled below

Jan 1, 1947

By H. M. Stewart, R. A. Grange

Man.; steel parts may crack if quenched directly into a bath near room temperature, but not if quenched at a temperature just above the range where martensite forms and then allowed to cool slowly to room temperature. This latter procedure, which is the basis for such modern hardening techniques as "martempering" and "isothermal quenching," may entail some sacrifice in depth of hardening but very little, if any, in intensity of hardening. In planning such treatments, it is necessary to know the upper limit of the martensite range, and often desirable to know the proportion of martensite that would form on cooling to any lower temperature; furthermore, the tendency of a particular steel to crack when quenched is unquestionably associated with the temperature range of martensite formation, and consequently knowledge of this range aids in selecting the optimum composition for a given application. Certain puzzling phenomena associated with the properties of quenched and tempered steel may be at least partly clarified as the manner in which martensite forms is more fully understood. Information on the temperature range of martensite formation, particularly with respect to how much martensite results from quenching to a given temperature, is lacking for most commercial types of carbon and low-alloy steel. These considerations led us to study martensite formation in 14 carbon and low-alloy steels. The resultant data may be directly used in the following ways: (I) for selecting the lowest quenching temperature at which no martensite will form; (2) for selecting the highest quenching temperature at which virtually all marten . site will form, thereby avoiding quenching to an unnecessarily lower temperature with attendant danger of cracking; and (3) in producing a mixture of tempered martensite and bainite, which in high-carbon steels has been found to possess somewhat better ductility than tempered martensite, yet does not require the full transformation time necessary for a completely bainitic (austempered) structure. PART I. OBSERVATIONS OF MARTENSITE FORMATION IN FOURTEEN CARBON AND LOW-ALLOY STEELS Transformation of austenite to pearlite or bainite can be conveniently studied by observing the change that occurs over a period of time at constant temperature; such studies are the basis of the isothermal transformation diagram (S-curve). This isothermal technique is not applicable to martensite formation, which occurs within a time interval too small to measure, at least by any ordinary means. For all practical purposes, therefore, martensite may be regarded as forming only during cooling and not during a period of time at constant temperature. As austenite is cooled below

Jan 1, 1947

G. Sherburne Rogers (written discussion*).—Mr. Kennedy's discussion1 of Mr. Matteson's paper takes the form of a criticism of my own comments2 on this paper. Mr. Kennedy is a respected authority on matters pertaining to the salt-dome oil fields, and his characterization of my "elaborate figures" as "worthless" is sufficiently candid and comprehensive to warrant a brief reply. My 'voluminous figures" consisted simply of a rough estimate of the minimum quantity of salt in the Humble dome, and a, calculation of the volume of sea water and of the volume of saturated brine which this salt would represent. Mr. Kennedy apparently interprets my remarks as opposing the idea that so,large a volume of salt could have been deposited from sea water, for he cites the area and thickness of European salt beds; but nothing was further from my intention. Given an arm of the sea, an arid climate, and evaporation under a hot sun, it is easy to conceive the formation of almost any thickness of bedded salt. I cited the figures in connection with Harris' theory of the origin of salt domes, according to which the plugs were formed by the deposition of salt from ascending brine solutions, owing to the drop in temperature as they neared the surface. I pointed out the well known fact that the solubility of salt is only slightly affected by temperature, and that a drop of 80" C. would cause the deposition of less than one-tenth of the salt in solution; hence that more than ten times the volume of salt actually forming the plug must have been involved. If ten times the salt actually in sight be computed in terms of brine and multiplied by 50 or 60 to take into account all of the known salt domes, the resulting figure is so enormous that I am not at all so sure as Mr. Kennedy seems to be that the porous stratified rocks of eastern Texas and western Louisiana could contain or furnish so great a volume of migratory brine. Mr. Kennedy, however, does not dwell on drop in temperature as the cause of the precipitation, but contents himself with ascribing the whole process to lateral secretion. As I understand it, this implies that the connate waters and brines contained in the rocks migrated to the Gulf Coast region, and there deposited their salt at various loci of crystallization. Just what started the crystallization or what force caused the

Jan 1, 1918

By R. S. Busk

A PREVIOUS paper1 has summarized the effect of A all metallic elements on the lattice parameters of magnesium. The present paper deals with the effect of temperature on the lattice parameters and the way in which that effect is modified by alloyed elements. The experimental techniques for sample preparation, exposure to the X-ray beam, measurement of line diameters, and calculation of the parameters were the same as reported in the previous paper. The temperature of the specimen was raised by surrounding the mounted compact with a conical Glas-Col,* the base of which was sealed with Saran film. In this way the temperature of the specimen could be raised to 200 °C, which was the maximum desired in the present study. Control of temperature was effected by maintaining a constant, desired voltage to the resistance coils of the Glas-Col through a Variac. Temperature was measured by an iron constantan thermocouple embedded in the body of the specimerl so that the thermocouple bead was within 1/16 in. of the surface exposed to the X-ray beam. Variation of temperature during an exposure was less than + 1/4 oF. A series of eight alloys, consisting of pure Mg, Mg+Ag, Mg+Al, and Mg+Sn were studied. All percentage values are in atomic percent. The results are given in Table I. The density values given in Table I were calculated from the lattice parameters, using an equation due to Foote and Jette:"

Jan 1, 1953

By V. Damiano, M. Herman

CELLULAR substructure observed in metal crystals grown from the melt. has been studied extensively'-' and is attributed to the existence of a constitutionally supercooled zone in the liquid ahead of the solidifying interface. The mathematical description of this process has been given in terms of the concentration of solute in the liquid phase, the rate of solidification, and the temperature gradien.t in the liquid as the only variables.5 This technical note presents some evidence of 1) the effect of crystal orientation on some aspects of cellular growth, and 2:) the degeneracy of these cells into dislocation arrays. The zinc single crystals used in these studies were alloyed with cadmium sufficient to produce the constitutional supercooled cellular substructure. Crystals containing 0.05 pct Cd exhibited substructure formation for a growth rate of 10 cm per hr and a temperature gradient of 15°C per cm in accord with the theory. The growing liquid-solid interface was examined after we liquid had been decanted away in a fashion similar to that described by Rutter and Chamers.' The cellular substructure was also observed after polishing and etching the surface directly behind the decanted interface with a solution of HNO, and water. Fig. 1 is a photomicrograph of a typical polished and etched surface revealing substructure, the cleavage plane, and twins. The crystal has been grown with its basal plane parallel to the direction of growth and the plane of the micrograph is per-

Jan 1, 1960

By Richard E. Gray, William S. McCann, Robert C. Speck, Robert W. Bruhyn

Subsidence of the ground surface is the inevitable result of high recovery longwall and room and pillar coal mining operations. Up to now, U.S. research into this phenomenon has been concerned primarily with documenting the magnitude and extent of ground movements and prediction of the attendant ground strains through traditional ap¬proaches that have been developed in Europe and the United Kingdom. Preoccupation with ground strain prediction has, unfortunately, diverted attention from the more meaningful objective of predicting the severity of damage to structures at ground surface and the prob¬able cost to repair such damage. An attempt has been made to rectify this situation by reviewing in detail one hundred thirty four cases of subsidence damage to dwellings above active mines in western Pennsylvania, identifying the types of damage and the circumstances under which damage took place. The data reveal that damage to dwellings virtually always includes basements in addition to the readily apparent effects to the superstructure. In 90 percent of the subsidence cases, more than half the repair cost is associated with damage to subgrade components. A damage classi¬fication system has been devised that relates observed damage to severity and repair cost in a uniform manner for conditions in the Northern Appalachian Coal Field. Damage severity has been examined in the context of depth to the mine, the character of the near¬ surface overburden materials, mining type and other parameters.

Jan 1, 1983