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By H. l. Burghoff, J. S. Porter

This paper presents the results of an investigation of the effect of cold-working and annealing treatments upon the occurrence of preferred orientation in annealed brass wire. The subject has received less consideration than has the same phenomenon in annealed brass sheet or strip, and perhaps very properly so in view of the obvious and undesired results obtained in the forming or drawing of strip having preferred orientation, which results are in contrast with the lack of any spectacular visual evidence in wire. The factors of cold-working and annealing that control preferredness in strip are naturally expected to function similarly in wire. Indeed, one might expect the condition to be commoner in annealed wire, because the severity of the cold-working between anneals in commercial Practice is usually much greater for wire than for strip. For example, a wire that is to be finished in the annealed condition on a diameter of 0.040 in. is commonly subjected to a final reduction of 90 per cent between the last two anneals, the large reduction being accomplished in the successive drafts of a multiple-die machine. Wire for rivets, for instance, on 0.125-in. diameter, although given a slight reduction of about Io per cent after the final anneal, may have been given a prior reduction of 75 to 80 per cent. Barrettl states the fiber axis of annealed 70-30 brass wire to be [111], with some indication of [IOO] as a secondary fiber axis. Croft and Sachs2 have reported briefly on some differences in brass wire with random and with preferred orientations. They showed statistical plots of the twin-band angles with respect to the wire axis or direction of drawing as observed on an axial plane. They also pointed out that the resistance of the wire to corrosion-cracking when externally stressed and exposed to a mercurous nitrate solution decreased as the degree of the preferred orientation increased. Material and PRocedure All the wire for the investigation was processed from one portion as cut for extrusion from a cast billet of the following analysis: 70.13 per cent copper; 0.01 lead; 0.01 iron; 0.02, nickel; 29.83 zinc (by difference). The billet section, 8 in, in diameter, was extruded hot to 3/4-in. diameter, after which it was processed by alternate cold-drawing and annealing treatments as indicated in Fig. I. The earliest anneals in process were at about 1100°F. and the next to the last reductions by drawing were 58 per cent. The diameter of the finally annealed wire was 0.132 in. Semifinal anneals were at 800°F., 950°F. and 1100°F. and reductions of 47.5, 74, 83.5 and 89.5 per cent were employed in drawing to 0.132 in. The final anneals were at 87s°F., 1050°F. and 1250°F. and were

Jan 1, 1944

By Cyril Wells, Robert F. Mehl

THE practical importance of a knowledge of the rates of diffusion of carbon and of alloying elements in steel has often been pointed out 1,13 This importance ties chiefly, though by no means only, in the study of carburizing and in the study of reactions involved in the eutectoid inversion in steel The present paper is one of a series in which the rates of diffusion of carbon and of alloying elements in y-Fe and their mutual effects are measured with precision The present paper reports the results of meas¬urements of diffusion coefficients D of manganese in -y-Fe over wide ranges of temperature, and concentration, and of the effect of carbon and impurities and of grain size upon these diffusion coefficients [$] Data on the rate of diffusion of manganese in y-Fe have been reported by Fry2 and by Paschke and Hauttmann 3 Claussen4 calculated the diffusion coefficient D from Fry's data as 3 X 10-10 sq cm per sec at 960°, which will be shown to be incorrect by many orders of magnitude Paschke and Hauttmann gave a rough value of 9 6 X 10-8 sq cm per sec at 1400° Neither of these workers considered the variation of D with concentration and with temperature, and neither studied the effect of carbon METHOD AND MATERIALS Method -The method employed is identical with that used earlier 5 Owing to the volatility of manganese and the consequent loss of manganese from the outer surfaces of the welded diffusion bars, these surfaces were discarded The diffusion anneals were performed in argon, except one (test 18) in which hydrogen was employed for purposes noted below The temperatures reported are accurate to about 3° and constant within I°C , the diffusion times are reported to the nearest half hour The specimens were furnace-cooled after the diffusion anneal at about 2° per min Layers, usually 0 004 in thick, parallel to the welded interface, were machined from the specimens after the diffusion anneal and analyzed for manganese to 0 01 per cent Mn, the distances of these layers from the interface was measured to ±0 0002 in The concentration-penetration curves obtained were analyzed by both the Grube and the Matano solutions e The D values calculated by these two methods do not differ appreciably 5 The Grube solution was used except in tests in which the effect of concentration upon D was greater than 50 per cent, in such cases the Matano method, which explicitly provides for the variation of D with concentration,1 is the more reliable In general, the number of layers machined from the zones of variable composition were large enough to permit the use of the average layer composition as that of the center of the layer In 3 of the 30 tests, however, this is not justified, and the D values

Jan 1, 1941

By F. W. Jessen, N. Mungan

The plastic flow characteristics of clay water suspensions were first recognized by Binghaml in 1916 and further studied by Ambrose and Loomis' in 1931-1932. Many physical and chemical properties of clay suspensions are deeply influenced by particle size distribution as well as by the exchange cation. Separation of a number of fractions is particularly helpful in making a detailed study of a suspension. A limited amount of work has been conducted on the effects of particle size on specific properties of mud drilling fluids. A knowledge of particle size distribution is essential for a better understanding of fundamental properties of clay suspensions, particularly viscosity and gel strength. The purpose of this investigation was to study the effect of particle size on the viscosity and gel properties of clay suspensions and to determine any changes in mineral composition accompanying variation in size. EXPERIMENTAL PROCEDURE Numerous methods may be used to fractionate a poly-dispersed clay suspension into nearly mono-dispersed systems. Particles larger than 44 micron (325-mesh) may be obtained by wet screening. For sizes from 44 to 1 micron, the fractionation may be accomplished by sedimentation, elutriation plus microscopy,' or turbidimetry.6 When dealing with systems which contain a major portion of particles below l-mi-cron size, slit ultramicroscopy,7 centrifuge methods of Svedberg,5 eams,9 and McBain,l0 and X-ray methods" may be employed. The Sharples super centrifuge has been proved suitable for the economical separation of suspended particles of submicron range.12,13,14 Three-hundred and forty-five gal of 1 per cent by weight Aquagel suspension was mixed in a high-speed 5-gallon mud mixer and the suspension was allowed to stand in 5-gal glass bottles for 30 days to assure full hydration. All particles larger than 44 microns were removed by wet screening. Five fractions in the range of 44 to 1 micron were obtained by sedimentation. The Sharples super centrifuge method described by Hauser and Reed.13 Norton and Speil,14 Ha user and Lynn,15 and Hauser and Schachman,10 as employed to yield five fractions of submicron size. A super centrifuge operation chart prepared by Fancher, Oliphant, and Houssierre12 was used to determine operating conditions for the desired particle ranges. The clay suspension, after removal of all material above 1-micron size, was centrifuged. During rotation of the bowl, the particles were deposited on a thin plastic liner which fit closely inside the bowl. After passing 5 gal of suspension through the centrifuge, the liner was removed and the particles on the liner were scraped off, remixed and recentrifuged. This was repeated five times. Thus, Fractions H, I, K, and L were obtained. The finest fraction, M, remained in an approximately 0.4 per cent suspension. Water was evaporated under reduced pressure from this suspension to yield the finest particles. Results of the fractionation are included in Table 1. In order to achieve proper orientation and humidity conditions for X-ray diffraction analysis, the following procedure was employed. The dilute suspensions were placed on glass slides and allowed to dry at room temperature. This was repeated several times. Previous to measurement each sample first was placed in a water desiccator for half an hour and then allowed to stand for 15 minutes at room temperature. thus yielding an equilibrium condition of about 52 per cent relative humidity. The relative humidity of the room in which the X-ray diffraction was carried out was maintained at approximately 50 per cent so that there was no change in the spacings during the X-ray examination. Samples

By J. S. Browning

The pegmatites of the Kings Mountain-Lincolnton, N. C., area constitute the largest known domestic reserve of beryl and spodumene. The reserve is estimated to contain 90 million tons of pegmatic material with 1,280,000 tons of recoverable Li2O (lithia) as spodumene.1 The pegmatites also contain 0.4 to 0.5 pct beryl disseminated throughout the orebodies. The pegmatites may contain a potential reserve of 240,000 tons beryl, equivalent to approximately 34,000 tons of BeO. Different flotation methods for separating beryl from feldspar or quartz, or both, have been developed by various investigators.2,3,4,5,6,7 On the other hand, published information is limited on concentration of spodumene-beryl ores. As the response of beryl and spodumene to flotation is essentially the same, a successful separation of the two minerals depends upon use of a selective depressant or a selective collector for one of the minerals.

Jan 7, 1961

By S. D. Michaelson, Eric Sinkinson

Many of the magnesite ores of the western part of the United States contain such large amounts of silica and hydrous silicate minerals that the value of the ores is either low or nominal. Expensive and carefully controlled mining methods are necessary to prevent excessive dilution of the higher grade ores by introduction in mining of small pieces of the hanging walls or footwalls of the deposit. This difficulty is further complicated by the various states of decomposition of the country rock of the deposits in which many of the ores occur. The problem the authors attempted to solve arose from a request to float an impure magnesite containing varying proportions of siliceous gangue with calcium carbonate. The ore is normally enclosed in serpentine masses, somewhat decomposed, and in mining it wall rock is incidentally added, so that variable amounts of siliceous material occur in the samples. The silica, alumina, and iron oxide are so closely associated with the magnesium carbonate in the magnesite that ordinary mechanical separation at coarse mesh sizes is of no avail. It is well known that calcium carbonate can be floated by suitable reagents, therefore it seemed reasonable to suppose that magnesium carbonate minerals would behave in a similar manner, but experimental trial proved that this supposition was unfounded. Therefore the first step in the problem was to find out what differences of behavior there were between magnesium and calcium carbonates under flotation conditions, or when suspended in water. In water at 18" C. magnesium carbonate is slightly more soluble than calcium carbonate; in fact, MgCO3 is soluble to the extent of 0.0106 grams in 100 c.c. of water at 18" C. and CaCO3 to the extent of 0.0013 grams. However, magnesium carbonate in water gradually changes to the basic carbonates of a composition (3MgCO3.Mg(OH)23H2O) or (4MgCO3.Mg(OH)25H2O), depending upon conditions, and calcium carbonate to calcium hydroxide, Ca(OH)2. The relative solubilities of these hydroxides in water are the reverse of the solubilities of magnesium and calcium carbonates. The range in published figures for solubility

Jan 1, 1938

By S. D. Michaelson, Eric Sinkinson

Many of the magnesite ores of the western part of the United States contain such large amounts of silica and hydrous silicate minerals that the value of the ores is either low or nominal. Expensive and carefully controlled mining methods are necessary to prevent excessive dilution of the higher grade ores by introduction in mining of small pieces of the hanging walls or footwalls of the deposit. This difficulty is further complicated by the various states of decomposition of the country rock of the deposits in which many of the ores occur. The problem the authors attempted to solve arose from a request to float an impure magnesite containing varying proportions of siliceous gangue with calcium carbonate. The ore is normally enclosed in serpentine masses, somewhat decomposed, and in mining it wall rock is incidentally added, so that variable amounts of siliceous material occur in the samples. The silica, alumina, and iron oxide are so closely associated with the magnesium carbonate in the magnesite that ordinary mechanical separation at coarse mesh sizes is of no avail. It is well known that calcium carbonate can be floated by suitable reagents, therefore it seemed reasonable to suppose that magnesium carbonate minerals would behave in a similar manner, but experimental trial proved that this supposition was unfounded. Therefore the first step in the problem was to find out what differences of behavior there were between magnesium and calcium carbonates under flotation conditions, or when suspended in water. In water at 18" C. magnesium carbonate is slightly more soluble than calcium carbonate; in fact, MgCO3 is soluble to the extent of 0.0106 grams in 100 c.c. of water at 18" C. and CaCO3 to the extent of 0.0013 grams. However, magnesium carbonate in water gradually changes to the basic carbonates of a composition (3MgCO3.Mg(OH)23H2O) or (4MgCO3.Mg(OH)25H2O), depending upon conditions, and calcium carbonate to calcium hydroxide, Ca(OH)2. The relative solubilities of these hydroxides in water are the reverse of the solubilities of magnesium and calcium carbonates. The range in published figures for solubility

Jan 1, 1938

By Thomas R. Mager

An in.t!estigation has been made of the equilibrium conditions at 1200°C in the reaction between hydrogen sulfide gas and sulfur dissolved in Fe-Si alloys From this the equilibrium constant, activity coefficient, and activity of sulfur in solution were calculated. A number of studies of the equilibrium of sulfur with iron and iron alloys have given closely agreeing results from which the activity and free energy of the dissolved sulfur may be found. Sherman, El-vander, and chipman1 discussed the significant researches of dilute solutions of sulfur in liquid iron prior to 1950, and the results of this study indicated that the relationship between the ratio of PH2S/PH2 in the environment and the percentage of sulfur in solution is not a linear one. Morris and williams2 studied the equilibrium conditions in the reaction between hydrogen sulfide gas and sulfur dissolved in liquid iron and Fe-Si alloys, and reported that silicon dissolved in iron has a pronounced effect on the equilibrium conditions. They found that the activity of sulfur in iron is increased by the addition of silicon. At a silicon content of 4 pet the activity coefficient of sulfur was about twice that for sulfur dissolved in pure iron. Sherman and chipman3 investigated the chemical behavior of sulfur in liquid iron at 1600°C through the study of the equilibrium: H2 + S = H2S; K = PH2S/PH2 . 1/as [1] From the known equilibrium constant of the reaction between H2, H2S, and S and the experimental data, the activity of sulfur in the melt was determined. They found that the activity coefficient of sulfur defined as fs = as/%s is increased by silicon and decreased by manganese. Morris4 and Turkdogan5 also reported that manganese decreases the activity coefficient of sulfur in liquid iron and iron-base alloys. A recent technique of sulfur analysis developed by Kriege and wolfe6 of the Westinghouse Research Laboratories permits an accurate sulfur analysis of 0.5 * 0.2 ppm in the range of 0.1 to 3 ppm, whereas in the range of 3 to 50 ppm the accuracy is ±1 ppm. This technique of sulfur analysis was utilized in this experiment. Previous unpublished data reported that sulfur analysis by the combustion technique was not accurate below 20 ppm. EXPERIMENTAL PROCEDURE Five 5-lb ingots of high-purity Fe-Si were prepared. Three of these ingots were prepared without the addition of manganese but with a variation of silicon contents from 2 to 4 pet. The remaining two ingots contained 3 pet Si with the addition of manganese. Ingots were made at each of three silicon levels: 2, 3, and 4 pet. No alloys were made with less than 2 pet Si since below approximately 1.8 pet Si the binary alloy exhibits a to ? transformation. The two additional ingots of 3 pet Si-Fe were made at each of two manganese levels: 0.20 and 0.50 pet. To minimize the effects, if any, of impurities on the activity of sulfur on Si-Fe, the best metals available were used for melting. All ingots were vacuum-melted in magnesium oxide crucibles. After obtaining samples for chemical analyses, the ingots were processed. This consisted of hot rolling and subsequently cold rolling the alloys. Each ingot was hot-rolled at 1000°C, reheating between every pass to minimize grain growth. All heating was done in a protective argon atmosphere. The slabs were hot-rolled to strips 50 mils thick. After hot rolling, all the material was pickled to remove the scale formed on the surface of the strip during hot rolling. The material was then cold-rolled to 12-mil strips. Single strips of the material used in this experiment were hydrogen-annealed at 1200°C for 16 hr in an alumina tube. Chemical analyses of strips M-1, M-3, M-4, M-7, and M-8 are given in Table I. Sulfur, silicon, and manganese analyses were made from the millings from the cold-rolled 12-mil strips. The oxygen analyses were made from slugs of the as-cast material. The hydrogen sulfide used in these experiments was supplied from cylinders containing a mixture of argon and 1 pet hydrogen sulfide. The parts per million of hydrogen sulfide were determined from the analysis of the exit gas of the annealing furnace during each anneal. The flow rate of hydrogen was approximately 1 liter per min in all anneals. The

Jan 1, 1964

By W. Rostoker, R. F. Domagala, R. P. Elliott

The phase equilibria of the Hg-Th system over the composition range 0-100 pct Th and temperatures up to 1000°C have been studied for a small-volume, closed system. The solubility of Th in liquid Hg is about 5 pct at 300°C and decreases sharply with decreasing temperature. Two intermediate phases occur, Hg3 Th and HgTh. The structures of these are hexagonal (nonideally close-packed) and face-centered cubic, respectively. The HgTh phase decomposes eutectoidally at 400°-500°C. The solubility of Hg in solid thorium seems to be negligible. AFULL-phase diagram for this system would have to be defined on temperature-composition-pressure co-ordinates. This paper describes the pseudo phase diagram of a closed system, that is, where the alloy enclosed in a small volume equilibrates with a vapor pressure of mercury dictated by composition and temperature. Because of the experimental difficulties in studying a system of this nature, many of the phase relations can only be sketched. Alloy Preparation Alloys over the full range of composition were made from triple distilled mercury and one of two grades of thorium. For the bulk of the work, a calcium-reduced metal in sintered pellet form of reported 99+ pct total thorium content was used. Arc-melted specimens of this thorium gave a hardness of 135 VPN. The microstructure showed small primary dendrites of ThO2. A number of alloy compositions were made with a high-purity, iodide-decomposition thorium metal. The are-melted hardness of a button of this material was 35 VPN. Although the microstructure of the arc-melted specimens showed no dendrites of ThO2, there was definite evidence of an unidentified phase enveloping the grain bound-aries. There were no distinguishable differences between the constitution of alloys made with the two grades of thorium metal. Under normal conditions thorium is not wetted by liquid mercury. The film of ThO2 on all thorium metal cannot be penetrated by either liquid or vaporous mercury. It was therefore necessary to comminute thorium in the presence of mercury under such conditions that oxide films could not reform on the newly exposed metal surfaces. This was accomplished by the use of a high-speed, carbide-tipped rotary cutter incorporated in a chamber purged with argon and connected at the bottom to a demountable Vycor bulb containing a weighed amount of mercury. This experimental device is fully described in a separate paper.1 Alloy compositions were calculated by weighing the empty bulb, the bulb containing the mercury, and the bulb containing the mercury and the thorium chips. Many alloys were analyzed chemically for thorium and/or mercury after subsequent homogenization; the agreement between analyzed and calculated compositions was invariably very close. Bulbs containing the requisite amounts of mercury and fine thorium chips were clamped off, removed to a sealing unit, evacuated and sealed. Amalgamation under these conditions proceeded rapidly even at room temperature. To insure homogeneity, the specimens were annealed to 300-400°C. Alloys containing less than 30 pct Th remained pasty after all treatments, indicating an equilibrium condition of liquid plus solid. Alloys with more than 30 pct Th were transformed into a dark powdery product. These latter specimens were annealed for times of up to 1 week to complete interdiffusion. Many of the alloy compositions are pyrophoric. On exposure to air they oxidize with considerable evolution of heat to a mixture of ThO2 and free mercury. It was mandatory that alloy specimens be handled in a "dry box" purged thoroughly with argon. All X-ray diffraction specimens were powdered, screened, and sealed in capillary tubes within the dry box. Experimental Procedures Thermal analysis experiments, useful only in the mercury-rich region of the system, were conducted with the alloys in their original containers. A reentrant thermocouple well formed an integral part of the bulb. These bulbs were heated in a silicone oil bath and cooled in a dry ice-acetone mixture. The rates of heating and cooling were slowed by immersing the specimen bulb in a larger tube containing silicone oil. This provided a suitable thermal lag. In all tests, pure mercury was run as a basic standard. While the invariant reaction at about the melting point of mercury was detected by thermal analysis, the heat effect at the liquidus was not sufficient to produce an inflection in the cooling curve. It was necessary to determine the liquidus temperatures at the mercury-rich end of the system by "breaks" in electrical reslstivity versus temperature curves for individual alloys. The apparatus for this purpose consisted of a pyrex tube about 2 in. diam and 12 in

Jan 1, 1959

By Paul R. Bluekamp

The Mather Mine property is composed of a 5.2 sq km (2 sq mile) area within the Cities of Ishpeming and Negaunee which are located in the Upper Peninsula of Michigan. Production in this mine started in 1943; it ran continuously until its closing in 1979, having produced slightly over 55 million tons of iron ore. This mine was a joint venture between several steel companies and The Cleveland- Cliffs Iron Company (CCI), with CCI being the fee holder and operator. For the first 17 years of operation, the ore was shipped in its natural state directly from the mine to the steel mill. By 1960, iron ore pellets were on the market and they proved so superior to the natural soft Mather ore that the latter became difficult to sell except for the coarser portions. It was decided to develop a pelletizing process for the Mather ore, and this was accomplished by 1965 when the first Mather pellets were produced. From this date, all but the coarse fraction of the Mather ore was shipped as pellets. The geological setting is that of a large east-west trending synclinorium which plunges to the west. The lowest member of this trough-like structure is, for the most part, a quartzite-like graywacke, the upper 20 m of which grades into a softer, fine grained slate. Lying conformably on this graywacke footwall member is an iron- formation member which is over 1,300 m in thickness. This iron-formation is cow posed of thin alternate bands of iron oxides and chert and is intruded by a number of diorite sills - some up to 122 rn (400 ft) in thickness. The north limb of this synclinorium dips at approximately 45' and bottoms out at about 1,000 m from surface in the central part of the mine. There are two sets of faults, many of which are intruded by diorite dikes, which trend east-west and southeast-northwest. Displacements are varied, reaching a maximum displacement of 243 m (800 ft). The ore is found lying directly on the slatey footwall and its position is largely controlled by the faults and dikes, with the bulk of the ore being on the upper side of these structures. The ore is composed of soft earthy hematite and martite with vertical thicknesses up to 122 m (400 ft) although the average thickness would be closer to 46 m (150 ft). The ore averaged 60% iron and 7% silica on a dried analysis. The Mather Mine is located on the north limb of the syncline and was worked from two shafts, the deepest of which. was 1,09 7 m. These two shafts are about 2 km apart and serviced a total of 8 working levels between them during the life of the mine. The level spacing was about 61 m (200 ft). The main haulageways were driven parallel to the ore/footwall contact in the hard cow petent graywacke wherever possible. On the lower levels, deeper into the footwall, naked development was common. This material graded into roof bolting ground towards the upper stratigraphic portion. As drifting progressed further into the upper stratigraphic portion of the footwall, progressively stronger steel sets had to be used. From the main haulageway, cross-cuts were turned into the orebody on 61 m (200 ft) centers and extended as far as needed to recover the ore available to that particular cross-cut. The main haulageways and cross-cuts were driven 3 m (10 ft) high, 3 m (10 ft) wide at the top and 4.6 m (15 ft) wide at the bottom. This configuration would accomodate a set composed of a 2.7 m (9 ft) cap on top of two 2.7 m (9 ft) legs angled out at 18'. A sill plate was used under each leg to prevent its sinking into the ore below. The type of steel used was dependent on the expected weight to be experienced. Sets were placed on 1.63 m (5 ft 4 in.) centers; however, in extremely heavy areas, it was sometimes necessary to install sets on 0.8 m (2 ft 8 in.) centers. On the top two levels (5th and 6th), the ore was considerably hard-er and was mined by sub-level stoping and long hole drilling. Very light steel sets were used in the main haulageways and cross-cuts and timber was used in the production drifts. Some con- crete production drifts were installed on 6th level, but proved to be uneconomical. However, as mining reached greater depths, the ore became softer and more massive, reaching its maximum vertical heights on 11th and 12th levels. On levels 7 through 10, yielding steel sets were used extensively in the slusher drifts. While they were satisfactory on 7th and 8th levels, their success diminished with depth and they were

Jan 1, 1981

By F. Twyman, D. M. Smith

THOSE chemists (they are still greatly in the minority) who use the spectroscope, use it very often, and find it almost indispensable. As a means of detecting minute quantities of the metals it is unrivalled. A metal can be readily distinguished in the presence of any other element, compound, or mixture without the necessity of separation. The qualitative analysis of the metallic constituents of a substance, which the spectroscope gives so easily, is a sure basis for planning a chemical analysis. As the determination of each element proceeds the purity of precipitates may be checked as often as desired. If, possessing these advantages, the spectroscope has been neglected in general chemistry, it is not surprising that it was neglected in metallurgical chemistry; for many of the impurities which are of industrial interest, even when they are present in a metal or alloy in small quantities, are not then always easily detected by the examination of their visible spectrum. The history of the development of the art has been given in Bureau of Standards Scientific Paper No. 444.

Jan 1, 1928

By C. R. Whitney, G. N. Maniar, D. R. Muzyka

Previous results have shown that Pyromet 860, an Fe-Ni-base heat-resistant alloy, is stable at temperatures as high as 1500°F for aging times as long as 100 hr. This Paper describes the results of long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Times as long as 37,660 hr were employed. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffraction, and microprobe techniques. phase, containing cobalt, nickel, and molybdenum, was detected after extended exposures from 1200" to 1400°F and careful study was performed to describe the kinetics of its formation in this alloy. µ phase formation apparently has little effect on the elevated-tem-perature properties of Pyromet 860. For times as long as 500 hr at 1300°F and below, with µ phase present, m significant effects on ambient temperature properties were noted. For longer times at 1300°F and after 1400°F exposure, the effects of u phase on ambient temperature tensile strength properties are not clear due to y' effects and grain boundary reactions. Electron-vacancy, N,, numbers were calculated using different methods described in literature and correlated with the present findings. In the selection of alloys for use in gas turbine applications, structural stability ranks as a primary criterion. High-temperature strength and cost are also of major concern. With these factors in mind, Pyromet 860 alloy, an Fe-Ni-base superalloy was designed. This alloy combines the cost advantages of Fe-Ni-base alloys such as A-286, 901, and V-57 with improved strength and structural stability'1,2 and no tendency to form the embrittling cellular 77 phase. A previous study3 reported on the stability of Pyro-met 860 at temperatures from 1375" to 157 5°F and times up to 100 hr. That study showed that the y' precipitates increased in size and separation and decreased in number with an increase in time or aging temperature. No deleterious phases were found to occur. In the present work, samples from four production heats were subjected to long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Various heat treatments were used on the starting samples and tests were run up to 37,660 hr. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffrac- tion, and microprobe techniques. Electron vacancy numbers, Nv , calculations were made by TRW.4 Experimental results are correlated with the Nv data used to predict occurrence of intermetallic phases such as a phase. EXPERIMENTAL PROCEDURE Mechanical Tests. Material for the present study came from four production size heats of Pyromet 860 alloy, weighing from about 3000 to about 10,000 lb. All of these heats were made by vacuum induction melting plus consumable electrode vacuum remelting. The nominal analysis for this alloy is compared with the actual analysis of the four heats in Table I. Sections of these heats were forged to 9/16-in. round bar,3/4-in. square bar, 3-in. round bar, 4-in. square bar, and a gas turbine blade forging about 16 in, long, about 6 in. wide, and weighing about 20 lb. In general, all forging of this alloy is done from a 2050°F furnace temperature. Longitudinal test blanks were cut from the centers of the smaller bars, from mid-radius positions for the 3- and 4-in. bars, and from the air foil of the gas turbine blade and heat-treated according to the procedures outlined in Table 11. Heat treatment A is the "standard treatment" recommended for this alloy for best all-around strength and ductility. Heat treatment B is a modification of treatment A for improved tensile strength at moderate temperatures. The treatment coded C was designed for treating large sections according to a procedure previously described.' Heat treatment D was developed to yield optimum stress relaxation characteristics at 1050°F for a steam turbine bolting application. After heat treatment, the test blanks were machined either to plain bar creep specimens with a gage diameter of 0.252 in., to combination smooth-notched stress-rupture bars with a plain bar diameter of 0.178 in. and a concentration factor of Kt 3.8' at the notched section, or to notch-only specimens. All specimens conformed to ASTM requirements. Metallography. Most of the creep-rupture tests were continued to failure. A few bars were fractured as smooth or notch tensiles after creep-rupture exposures. After fracturing, ordinary metallographic sections were made primarily in gage areas adjacent to fractures to represent a "high-stress" region and through specimen threads to represent a "low-stress" region. All metallographic sections were made in a longitudinal direction with respect to the test specimen axes. For optical microscopy, the samples were etched in glyceregia (15 ml HC1, 5 ml HNO,, 10 ml glycerol). For XRD analysis, the phases were extracted electrolytically in two media: 20 pct &Po4 in H20 for selective extraction of y' and 10 pct HC1 in methanol for carbides and other phases.

Jan 1, 1970

By J. Paces, E. Miller, K. L. Komarek

The resistivity was determined as a function of temperature over the composition range from pure cadmium to 40 at. pct Cd. Melts with cadmium contents less than 85 at. pct had negative temperature coefficients of resistinity. On cooling below a transition temperature close to the liquidus temperature, the slope of the resistivity-temperature curve changed sharply. The activation energy calculated from the slope was 0.07 ev above the transition temperature and 0.14 ev below. The resistivity vs composition curve shows two maxima corresponding in composition approximately to CdSb and Cd3Sb2. THE relationship between the structure of a liquid and that of the crystal formed on solidification is at present not well-under stood. Various experimental determinations of the properties of liquids indicate that deviations from random atomic arrangements in liquids occur and that the properties of a solid and of its melt are closely related. Thermody-namic activities of liquids usually show negative deviations in systems where compound formation occurs in the solid,' and X-ray data indicate that close-packed solids and their melts frequently have nearly the same coordination number. Electrical resistivities and viscosities of liquids frequently exhibit maxima at compositions corresponding to compounds in the solid state. It should be of interest to study systems which have both stable and metastable compounds in the solid, and to determine if the short-range order in the liquid is affected by the existence of the metastable solid phase. The Cd-Sb system exhibits such a metastable phase. The phase diagram is shown in Fig. 1.3 The stable system has one intermetallic compound, CdSb, crystallizing in the orthorhombic crystal structure, with a melting point of 456°C. The metastable system also has one compound, Cd3Sb2, melting at 420°C and crystallizing in the monoclinic structure. Metastable alloys transform to the stable crystal structure in the temperature range from 250o to 350°C. Several distinct indications of very strong short-range order in the liquid phase have been reported in this system, with a close relation between the ordering in the liquid and the existence of both the stable and metastable solid phases. Scheil and Baach4 have observed distinctly different vapor pressures for liquid Cd-Sb alloys depending on whether the liquid solidified to the metastable- or stable-phase configuration. They observed an unusually sharp increase of the activity in a limited temperature interval immediately above the liquidus temperature of stable alloys, followed by a sudden decrease in slope to what they considered normal values. On cooling, the activity data reproduced the values in the normal range but then deviated from the values obtained on heating. They also observed that specimens of the stable phase upon melting and resolidifying always crystallized in the stable crystal structure as long as the melt was not heated to more than 485° to 525°C; otherwise solidification to the metastable phase occurred. However, in a later investigation, these results were not reproduced (13). The resistivity of liquid Cd-Sb alloys has been investigated by Matuyama 5, Oleari and Fioram, 8 and Belaschenko (141, but only above 500°C, the temperature region where Scheil and Baach observed no vapor-pressure anomalies. The data of Matuyama and of Oleari and Fiorani are reproduced in Fig. 5 and show a maximum in resistivity at 50 at. pct Cd. The data of Oleari and Fiorani, however, show the maximum as being rounded, and their values in general are slightly higher than those of Matuyama.

Jan 1, 1964

By Thomas H. Clagett

ThE Pocahontas coal field comprises the area in Tazewell County, Va. and Mcrcer and McDowell counties, W. Va., in which Nos. 3 and 4, Pocahontas seams of bituminous coal are mined. It is a mountainous region with ridges rising 300 to 1000 ft. (91 to 305 111.) above the very narrow valleys and, except for some poorly kept farms along the tops of the ridges and the area occupied by the mining and coking plants and villages, is wooded throughout. First shipments were made from Pocahontas in 1883. There are now about 100 mines, 95 per cent. of which are drift mines. At the end of 1920, approximately 298,000,000 gross tons of coal had been produced and 35,000 acres of coal mined. No. 3 seam is from 4 to 10 ft. (1.2 to 3 m.) thick, but the change is gradual and the thickness fairly uniform in any particular locality. It has a streak of bone, about 2 in. (5 cm.) thick, to which the coal adheres on both sides. In parts of the field this bone is replaced by hard slate, usually from 2 to 4 in. thick. The seam has a slate or fireclay bottom and a draw-slate top. No. 4 seam is from 65 to 80 ft. (19.8 to 24 m.) above No. 3 seam, and of minable section only in the western part of the field. It is from 3 to 8 ft. thick and has two streaks of bone, cach from 1 to 2 in. thick. It has a fireclay or slate bottom and is overlaid by from 4 to 24 in. of a laminated coal and slate, locally termed "black rash," which is separated from the coal seam by about 3 in. of slate. This "black rash" averages about 2.5 per cent. ash, but contains some clean coal. The coal in both seams is quite soft. Cleavage sufficieiltly well defined to exert an influence on the mining is rare. Overlying strata arc slates, shales, and sandstones, the sandstones predominating, extending from 30 to 1000 ft. above No. 3 seam. The strata directly above the draw slate of No. 3 seam, or "black rash" of No. 4 seam, and up to the first sandstone are usually slates or shales, about 10 ft. thick over the.

Jan 1, 1923

By Thomas H. Clagett

ThE Pocahontas coal field comprises the area in Tazewell County, Va. and Mcrcer and McDowell counties, W. Va., in which Nos. 3 and 4, Pocahontas seams of bituminous coal are mined. It is a mountainous region with ridges rising 300 to 1000 ft. (91 to 305 111.) above the very narrow valleys and, except for some poorly kept farms along the tops of the ridges and the area occupied by the mining and coking plants and villages, is wooded throughout. First shipments were made from Pocahontas in 1883. There are now about 100 mines, 95 per cent. of which are drift mines. At the end of 1920, approximately 298,000,000 gross tons of coal had been produced and 35,000 acres of coal mined. No. 3 seam is from 4 to 10 ft. (1.2 to 3 m.) thick, but the change is gradual and the thickness fairly uniform in any particular locality. It has a streak of bone, about 2 in. (5 cm.) thick, to which the coal adheres on both sides. In parts of the field this bone is replaced by hard slate, usually from 2 to 4 in. thick. The seam has a slate or fireclay bottom and a draw-slate top. No. 4 seam is from 65 to 80 ft. (19.8 to 24 m.) above No. 3 seam, and of minable section only in the western part of the field. It is from 3 to 8 ft. thick and has two streaks of bone, cach from 1 to 2 in. thick. It has a fireclay or slate bottom and is overlaid by from 4 to 24 in. of a laminated coal and slate, locally termed "black rash," which is separated from the coal seam by about 3 in. of slate. This "black rash" averages about 2.5 per cent. ash, but contains some clean coal. The coal in both seams is quite soft. Cleavage sufficieiltly well defined to exert an influence on the mining is rare. Overlying strata arc slates, shales, and sandstones, the sandstones predominating, extending from 30 to 1000 ft. above No. 3 seam. The strata directly above the draw slate of No. 3 seam, or "black rash" of No. 4 seam, and up to the first sandstone are usually slates or shales, about 10 ft. thick over the.

Jan 1, 1923

By B. J. Harlan

THE trying times experienced by the steel industry during the past four years have emphasized the necessity of producing pig iron at the lowest possible cost. The trend in both design and operation of blast furnaces has been toward this end rather than securing maximum production from a unit or group of units. In the following discussion the trend in design of stacks and auxiliary equipment will be taken up before operation is considered. Although few furnaces have been constructed in the past few years, the trend is definitely toward larger furnaces with a hearth diameter of 24 or 25 ft. Such a furnace is very flexible, being able to produce efficiently any desired daily tonnage between 500 and 1000 or more. The detail of the design of furnace stacks, with the exception of the top, has changed little in recent years.

Jan 1, 1934

For the year ending February, 1920 PRESIDENT HORACE V. WINCHELL.. . MINNEAPOLIS, MINN. PAST PRESIDENTS PHILIP N. MOORE ST. Louis, Mo. SIDNEY J. JENNINGS NEW YORK, N. Y. FIRST VICE-PRESIDENT A. R. LEDOUX NEW YORK, N. Y. TREASURER GEORGE D. BARRON NEW YORK, N. Y SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y VICE-PRESIDENTS CHARLES W. GOODALE,1 . . . . District 5 BUTTE, MONT. MARK L. REQUA,1 District 6 SAN FRANCISCO, CAL. HENRY S. DRINKER, District 2 So. BETHLEHEM, PA. ROBERT M. RAYMOND,2 . . . . District 0 NEW YORK, N. Y. EDWIN LUDLOW,3 District 2 LANSFORD, PA. A. R. LEDOUX,3 District.0 NEW YORK, N. Y.

Jan 11, 1919

By Jay N. Fairbanks, Richard G. Robinson

This paper discusses a computer program and related formulas for fire fighting responses by coal mine personnel. The computer will interpret the mine air analysis, print reports, and provide relevant graphs allowing quick and accurate responses to coal mine fires.

Jan 1, 1983

By T. Kilner, A. Plumtree

DURING an investigation of electro-deposited silver structures, samples were prepared for metallographic examination by cold mounting in plastic, grinding on successive grades of emery paper down to 3/0, and chemically polishing by swabbing using the chromic acid solution described by Gilpin and Worzala.1 Attempts to etch these samples using the standard solutions described for silver (e.g., 5 pet KCN-5 pet Na2S2O8, H2O2-NH4OH, and various potassium dichro-mate solutions) all failed to give good results due to staining of the samples and to rapid etching. The staining was caused by the chromic acid polishing solution being trapped in small fissures between the sample and the mounting plastic, and also in small fissures in the sample itself. To overcome these difficulties, an etchant was developed which prevented staining at the same time as it slowly etched the sample. This resulted in a very clean, crisply etched surface as shown in Figs. 1 and 2. This etch consisted of 10 ml of orthophosphoric acid, 10 ml of distilled water, and 2 drops of the polishing solution noted above,' which is made by mixing 100 ml of saturated CrO3 solution, 45 ml of 10 pet HC1 solution, and 800 ml of distilled water. The etching procedure involved taking the final polished sample, either immersing or swabbing in the etchant for a period of 1 to 2 min, rinsing as quickly as possible in distilled water, alcohol, and ethyl ether in that order, and then immediately drying. This etch is easily controlled due to its slow rate of etching, and produces samples with clean, sharp surfaces. Pits due to overetching produced varying contrast effects when viewed under polarized light, and are therefore obviously useful for revealing many structural details within the sample. Another effect of overetching was to produce a height varia-

Jan 1, 1968

By N. V. Melnikov, L. N. Marchenko

The latest theoretical and experimental study of physical processes initiated by explosions in solid media have made it possible to obtain a deeper insight into the mechanism of the energy transfer to ambient rock from char es of explosives interspersed with various air gaps. As shown in (17, high explosive action causes excessive fragmentation of medium in the vicinity of the charge, while expansion of the process into the massif is negligible. A theoretical outline of a more rational application of explosion energy was given with a view of obtaining more uniform fragmentation of rock convenient for loading and transportation. The proposed idea proven by experimental study consisted of the possibility of explosion control based on redistribution of explosion energy. Practical realization of the above idea was proposed (1) involving charges with air gaps for rock fragmentation. Since the Rolla Symposium on Mining Research (USA, 1961) (2), borehole charges with air gaps have become common practice. This method of rock blasting is applied in open cast and underground mines working the hardest and viscous, hard, medium hard and soft rocks (ore, quartzites, granites, 1 imes tones, sandstones, coals, etc.) as well as at enterprises for extraction of building materials and raw chemical minerals of any strength. Application of charges with air gaps results in an increase of the degree and uniformity of fragmentation (up to 94 percent of the blasted rock mass consists of fragments not exceeding 400 mm), the average fragment size decreases by 1.5-2 times and the amount of lumps is reduced by 2-10 times (in some cases there are no lumps at all ). Besides, the amount of operation for filling boreholes with tamping material is reduced, the specific consumption of explosives

Jan 1, 1971

By E. A. Elevatorski

Wollastonite, named after William H. Wollaston, an English chemist, is a calcium metasilicate, CaSiO3. It has a short history as an industrial mineral. The earliest production of wollastonite is reported to be from a deposit near Code Siding, located north of Randsburg, Calif. At this locality small tonnages of wollastonite were quarried during 1933-34 and 1938-41, and processed into mineral wool. This operation was largely experimental and virtually no United States production was again reported until the 1950s when a large deposit near Willsboro, N.Y., was developed by the Cabot Corp. A processing plant was placed on-stream in 1953, with nearly continuous production to date, and it is currently operated by Interpace Corp. Since 1958, wollastonite deposits in the Little and Big Maria Mountains of Riverside County, and in the Panamint Range of Inyo County, both in California, have operated intermittently for production of both ornamental and commercial wollastonite. During 1973, the United States was the major producing country, furnishing about 75% of the world's output. Recent production also has come from Finland, Mexico, and Kenya. Small amounts have been shipped intermittently from India, USSR, New Zealand, Republic of the Sudan, Republic of South Africa, and South-West Africa. The principal use of wollastonite is in the manufacture of ceramics, especially wall and floor tiles. Other uses are for paints, fillers, adhesives, reinforcing agents, plastics, fluxes, and glazes. Mineralogy Pure wollastonite, CaSiO3, has the composi¬tion of 48.3 % CaO and 51.7 % SiO,. However, it is seldom found in the pure state due to the ease with which it takes into solution the metasilicates of manganese, magnesium, iron, and strontium. Predominantly, wollastonite occurs as a contact metamorphic deposit forming between limestones and igneous rocks. Commonly associated minerals are garnet, diopside, epidote, calcite, and quartz. It has a specific gravity of 2.8 to 3.0, and hardness of 4.5 to 5 on Mobs' scale. When pure, it has a brilliant white color, but with impurities it may be grayish or brownish. Luster is vitreous to pearly. Melting point of wollastonite is about 1540° C. Wollastonite occurs in coarse-bladed masses, rarely showing good crystal form. It is usually acicular or fibrous, even in the smallest of particles. The most unique property of crushed and ground wollastonite is its cleavage. Fragments of crushed wollastonite tend to be needle-shaped, imparting a high strength, and this property is the basis for many of its uses. The fiber lengths are commonly in the ratio of 7 or 8 to 1, length to diameter. Some crystals of wollastonite fluoresce under short-wave or longwave ultraviolet light, or both; colors ranging from yellow-orange to pink-orange. Specimens may also show phosphorescence. The brightness of wollastonite is a property of considerable importance to the paint industry. Material, 99% pure, with a size of -325 mesh, has a General Electric reflectance rating of 92 to 96%. Chemically, wollastonite is inert and this property makes it useful as a filler and reinforcing agent. There are two polymorphs of calcium silicates: wollastonite, a low temperature form, and pseudowollastonite, a high temperature form. Inversion of wollastonite to pseudowollastonite occurs at about 1120° C, resulting in an increase in the coefficient of expansion and a color change. Pure white wollastonite, on inversion, may change to a cream tint, or various shades of red or brown. The color change is thought to be due to the presence of iron and strontium.

Jan 1, 1975