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By E. R. Helderman, C. Y. Ang, C. C. Nealey

Beryllium-base alloys have been successfully p7.-epared by the liquid-phase sintering technique. Depending orz the composition and amount of the intended liquid please, microstructures either single -phase or duplex in feature with randomly oriented grains have been obtained. Qualitative and semi-qualitative determination of distribution of alloying elements md microsegregations in some experi)uzental alloys haue been made by electron-micro-probe analysis in conjunction with microliardness testing and standard metallography. Tensile tests reoealed that some conzpositions possess attractive elastic properties with Young's mot1uli greater than 40 X 10' psi. In powder metallurgy, liquid-phase sintering is a process or phenomenon that has proven to be of practical value. For example, the heavy metals such as tungsten-copper-nickel, high-strength heavy gyro alloys,' heavy-duty electrical contacts,' and tungsten carbide tool materials are all products of liquid-phase sintering. Mechanisms involved in liquid-phase sintering, however, are not completely understood. Questions regarding the exact roles played by rearrangement of particles, liquid/vapor surface energy, solution and precipitation, and so forth, have not been completely answered. Evidence has been cited3 that at least volume shrinkage in the densification process is diffusion-controlled. It is possible that the predominant mechanisms for the complete densification and grain growth in a liquid-phase sintered system depend primarily on the alloy systems involved, in addition to processing conditions. Despite the lack of sound understanding of the mechanisms of the process, liquid-phase sintering has been and is being used to advantage either to synthesize microstructures for their special properties or to prepare alloys which are difficult to form by fusion process. Liquid-phase sintering of beryllium alloys was first attempted by Jones and Williams.4 They first tried infiltrating beryllium with magnesium, and then succeeded in preparing the alloy by sintering Be-Mg powder compact in molten magnesium bath. This investigation resulted in the identification of some Mg-Be intermediate phases. Crossley et a1.5 also used liquid-phase sintering technique in an attempt to produce ductile beryllium alloys for structural applications. The major liquid-phase components investigated by Crossley et al. were aluminum and silver with minor additives of germanium, calcium, lanthanum, cerium, and yttrium. The lack of wetting and the bleeding out of liquid phase were the difficulties encountered during experimentation. According to Hodge,6 the two compositions investigated by Crossley, which showed some promise based on compression tests, involved large amounts (over 35 wt pct) of silver, thus making them too heavy to be of practical interest to the aerospace industry and military users. The present investigation was prompted by the search for light-weight (density less than aluminum) beryllium alloys exhibiting small anisotropy in physical properties for precision inertial navigation instrument applications. In addition to isotropy, good structural properties such as high elastic modulus or desirable combination of mechanical and physical properties are also objectives of this investigation. The technique of liquid-phase sintering was chosen for its versatility in producing either duplex or homogeneous microstructures. This report is concerned with the use of copper and aluminum, with or without silicon addition, as the intended liquid phase, and the resultant micro-structures and some physical properties of the beryllium alloys. Qualitative and semiquantitative electron-microprobe analyses of some of the alloys are presented to illustrate the usefulness of this microanalytical technique for the identification of microconstituents and their distribution. EXPERIMENTAL PROCEDURES The beryllium powder used was -200 mesh Brush Beryllium Co. QMV NP-50 grade. Typical chemical analysis of the powder is shown in Table I. Commercial high-purity copper, aluminum, and silicon powders all screened to —100 mesh were used as additions. Mixed powder compositions were ball-milled in ceramic jars for 1/2 hr to ensure thorough blending. Milled powder was loaded either in 3/4-in.-diam button die or in Metal Powder Association flat tensile specimen die and compacted under top and bottom pressure. No lubricant or organic binder was used. Sintering was carried out in a quartz tube under a vacuum of 50 to 100 µ pressure. Surface hardness and some microhardness readings were taken on sintered specimens. Sintered density was

Jan 1, 1965

By W. M. Ross

AMONG the comparatively few A radical changes in mining equipment in recent years is the introduction and use to an ever greater degree of detachable bits for rock drills. Just how great the possible field for economic application of this innovation is, and to what ex- tent detachable bits are used instead of the conventional type of drill steel, are matters of conjecture. Just as a rough approximation, one might conceive that at least three-quarters of the drilling done in mines today could better be performed by steel with detachable bits, instead of only about one-quarter as at present.

Jan 1, 1939

By Sydney H., Ball

ONE of the important mineral discoveries of the eighteenth century was , that of the Minas Geraes, Brazil; diamond fields. The production of this and of .other diamond discoveries in neighboring states made Brazil the premier producer of diamonds, succeeding India; its 140 years of supremacy finally passed to- South Africa- 60 years ago. Three times have diamonds contributed heavily to Portugal's somewhat checkered financial history; first in the sixteenth and seventeenth- centuries when the diamond trade of India was controlled by its citizens residing in ,Goa, later in the late eighteenth and the first 75 years of the nineteenth century when the Brazilian fields were the world's source of diamonds, and now, when the Angola diamond mines are the principal source of revenue of its colony, Portuguese West Africa. Certain phases in the history of the administration of the Brazilian field are sufficiently curious to warrant description.

Jan 1, 1929

By Allen J. Johnson

With a realization of the rapidly increasing importance of automatic stokers as a medium for domestic heating, the Anthracite Institute Laboratory has conducted extensive investigations, over a period of several years, to determine the various outstanding characteristics of stoker design and performance. The purpose of this paper is to summarize these findings as a guide to current practices. Stokees Investigated One or more models of the underfeed stokers listed below were included in the various phases of this investigation: Beckley Gilkoal Burnwell Iron Fireman Combustioneer Motor Stokor Electric Furnace Man Norristown Super-stoker Erie Heat Generator Whitney Fire Ball (Tests Incomplete.) Fuel Saver Principles of Construction.—The operating principle of the leading makes of underfeed stokers is similar (Fig. 1). A plunger1 or slowly revolving worm2, conveys the buckwheat or rice sizes of anthracite to the center of a specially constructed tuyere pot where air is admitted to the coal through suitable ports of varying design. As the fuel burns, it is slowly forced to the outside circumference of the tuyere by the pressure of the incoming coal; eventually the ash falls over the edge of the pot, either entirely by gravity or aided by mechanical sweepers. In at least one model, the entire firepot revolves. While various special details have been included in the design of a number of stokers, they do not affect the general principles as described above, and therefore have not been included in this discussion.

Jan 1, 1936

By Allen J. Johnson

With a realization of the rapidly increasing importance of automatic stokers as a medium for domestic heating, the Anthracite Institute Laboratory has conducted extensive investigations, over a period of several years, to determine the various outstanding characteristics of stoker design and performance. The purpose of this paper is to summarize these findings as a guide to current practices. Stokees Investigated One or more models of the underfeed stokers listed below were included in the various phases of this investigation: Beckley Gilkoal Burnwell Iron Fireman Combustioneer Motor Stokor Electric Furnace Man Norristown Super-stoker Erie Heat Generator Whitney Fire Ball (Tests Incomplete.) Fuel Saver Principles of Construction.—The operating principle of the leading makes of underfeed stokers is similar (Fig. 1). A plunger1 or slowly revolving worm2, conveys the buckwheat or rice sizes of anthracite to the center of a specially constructed tuyere pot where air is admitted to the coal through suitable ports of varying design. As the fuel burns, it is slowly forced to the outside circumference of the tuyere by the pressure of the incoming coal; eventually the ash falls over the edge of the pot, either entirely by gravity or aided by mechanical sweepers. In at least one model, the entire firepot revolves. While various special details have been included in the design of a number of stokers, they do not affect the general principles as described above, and therefore have not been included in this discussion.

Jan 1, 1936

By O. M. TUPPER

REQUIRING a finer ground clay than that obtainable with a dry pan or hammer mill, the Clay Corporation of California installed a five-roller, low- side Raymond impact mill at its Lincoln plant in 1925 and since then has been economically grinding fire clay with a moisture content as high as 15 per cent. This was one of the first, if not the first, of this type of mill to be used in the grinding of clay on the Pacific coast. The pulverizer consists of a die-ring, lying in a horizontal plane, enclosed in a sheet-iron housing. A vertical shaft supports a spider from which five rolls are suspended in such a way as to always have them bearing on the die-ring. The vertical mill shaft is driven by means of beveled gear and pinion from a horizontal shaft which is connected by belt with a 60-hp. motor with suitable pulleys to give a speed of 175 r.p.m. A large fan which has a speed of 1100 r.p.m. and is belt connected to a 40-hp. motor is connected to the mill housing. The discharge end of the fan is in turn connected to a cyclone dust collector.

Jan 1, 1929

By AIME AIME

T HE Mining Methods Committee held its initial meeting* on Tuesday afternoon, with F. W. Bradley in the chair and W. Y. Westervelt as vice- chairman. The first paper to be presented was "A Plea for a U. S. Court of Patent Appeals," for which Kenneth W. Greenawalt ably pleaded. The paper (which was published in full in last month's issue) is so carefully prepared that no synopsis can do it justice. It discusses the opposed views of some patent lawyers and other lawyers and members of the judiciary as, for example, Chief Justice Taft who is quoted as saying in 1921: "I think it is a great deal better to take a first class lawyer and a first-class judge and make him a good patent expert than it is to take a patent expert and try to make him a first-class lawyer and a good judge." Mr. Greenawalt argued the need for specialized scientific and engineering interest and understanding to enable a lawyer or judge to prepare or interpret patent specifications and decide the originality necessary for a valid invention. He proposed the special U. S. Court of Patent Appeals to also counteract the costly confusion and injustice now ruling where a patent may be declared valid in the courts of certain States and invalid by the courts of other States.

Jan 1, 1930

By M. D. Curran

AS applied to coal, the term processing is subject to many interpretations. To some it means preparation of coal for the market by mechanical means such as crushing, sizing, washing, or treating with oil or chemicals to eliminate dust or improve combustion quality. To others it means conversion of the coal to other commodities as in carbonization to produce coke and by- products, or to liquids by application of the hydrogenation process. I prefer to classify the various forms of mechanical treatment under the heading of beneficiation and apply the term processing to those methods of treatment that destroy the coal sub- stance through distillation or hydrogenation.

Jan 1, 1939

By F. W. Aul, R. C. Glenn

EXTRACTION techniques are of particular importance in determining size, shape an: crystal structure of particles smaller than l000Å in steels and other alloys. However, artifacts that can arise during the preparation of extraction replicas may lead to erroneous conclusions. The purpose of this note is to illustrate some of these artifacts and the misinformation that can result from their presence. An alloy of iron with 0.8 pct Cu was investigated in the following conditions: 1) Solution treated 3 days at 925°C in dry hydrogen and quenched in water. Aged in steps to precipitate copper, as follows: heated to 700°C, held 1 day; then furnace cooled to 50O°C, held 3 days; then furnace cooled to room temperature. 2) Solution treated 3 days at 925OC in dry hydrogen and furnace cooled to room temperature. 3) Solution treated 3 days at 925OC or 17 hr at 1100°C in dry hydrogen to dissolve all copper, then quenched in water. A normal parlodion dry-extraction technique was employed after etching the specimens with super picralP or with 2 pct nital. A wet-extraction method

Jan 1, 1962

By C. David Mann

Metal prices continued to improve in 1964, resulting in the opening of new mines and re- activation of old ones. Larger and deeper shafts are being bored. At the AEC's Nevada Test Site, a 72-in. diam shaft is being bored to 3200 ft. In New Mexico a 1650-ft shaft was bored with a 48-in. bit, then reamed to 124 in. to 935 ft, and 102 in. to 1650 ft. Deviation was only 26 in. In California a shaft sinking machine has been developed which combines drilling and mucking equipment into one mobile, integral unit.

Jan 2, 1965

By C. Land, R. Hultgren

Heat contents of four Cr-Ni alloys were determined in a diphenyl ethev calorimeter. Aside from ferromagnetic effects, Kopp's law of additivity of heat capacities is approximately fol-lowed, in disagreement with earlier results of A. W. Foster. In 1934 Foster1 reported heat-capacity measurements of dilute solutions of chromium in nickel, primarily as a study of the effect of alloying on the ferromagnetic Curie temperature. He found that, apart from the Curie temperature effect, the general level of heat capacities was reduced 10 pct by the addition of 1 pct Cr; 20 pct by the addition of 2 pct Cr. His measurements of pure nickel essentially agreed with accepted values. These results indicate that small amounts of dissolved chromium cause an increase in the Debye temperature of nickel, presupposing a change of frequency of interatomic bonding vibrations which is much larger than should be expected. If Foster's results were verified, therefore, they would have important implications for bonding theory. The only other heat-capacity measurements in this system seem to be those of Taylor and Hinton,' who studied anomalies which they attributed to super-lattice formation at 25 at. pct Cr. At temperatures above the anomaly, Taylor and Hinton found heat capacities at this composition were quite normal, approximately obeying Kopp's law of additivity. EXPERIMENTAL WORK In order to verify or disprove the remarkable results of Foster, the heat contents of four dilute solid solutions of chromiunn in nickel were measured in a diphenyl ether calorimeter. This instrument, described elsewhere,, operates on the principle of the Bunsen ice calorimeter, but uses diphenyl ether as the working substance. Diphenyl ether melts at the convenient temperature of 26.S°C and supplies a more sensitive measure of heat than ice. The hot sample, in an atmosphere of argon, is dropped from a furnace at a measured temperature into a chamber which is surrounded by a mixture of solid and liquid diphenyl ether. The heat from the hot specimen melts some of the solid without chang- ing the temperature of the calorimeter. The amount of solid melted, and therefore the number of calories released by the specimen, is measured from the increase of volume of the mixture, which pushes mercury down a graduated capillary tube. The apparatus has been standardized against the known heat content of pure platinum. Heat loss during the dropping of the specimen was estimated by comparing the heat content of an empty platinum capsule with a solid platinum ball of the same radius and degree of polish of the surface. Repeated tests demonstrate the precision of measurement to be closer than *0.3 pct. Smoothed experimental results are listed in Table I. The tabulated values for pure nickel are taken from kelley, several measurements were made which agreed closely with this tabulation. For chromium, however, no similar agreement was found. The values tabulated were taken from a thorough study of chromium with the diphenyl ether calorimeter which will be published elsewhere.= Suitable plots of the data showed the expected ferromagnetic anomalies in the low-chromium alloys, while the 11 pct alloy shows no ferromagnetic anomaly, but a different, small anomaly below 900°K. This is perhaps the same anomaly found in CrNi, which was once attributed to superlattice formation,' but is probably due to some other cause, such as antifer-

Jan 1, 1960

By Kim Beattie

IN spite of the fact that in 1944 Canada experienced a decline in production of all her leading base metals-nickel, zinc, lead, and copper; despite uncured headaches in the coal-mining industry; and cheerfully ignoring a still further drop in gold, the most valuable product of her mines, which had the lowest output of any year since 1931, the Canadian miner retains the traditional optimism of miners everywhere as he looks forward to the postwar period. Some factors should keep the Canadian mining industry from being too optimistic of the coming era of peace, but the fraternity generally holds that its confident attitude towards the future is based on sound reasons. The decline in production in the Canadian mining industry last year can be almost wholly attributed to the serious shortage of labor and the difficulty in obtaining transport and supplies in remote areas. Some falling off occurred in the demand for certain strategic metals, but the diversion of gold miners, especially, without replacements being obtainable, to direct war work or allied pursuits, was certainly the principal cause of the reduced output in 1944. But that is a situation which will right itself at the close of the conflict.

Jan 1, 1945

By Frank Harris

THE strength of hard drawn copper wire is a question of considerable importance to both manufacturer and consumer. Unlike steel and alloy wires, in which strength is governed by both chemical and physical considerations, the high conductivity required for copper wire in the electrical industry generally precludes the possibility of obtaining tensile strength through the use of alloys. Consequently, this strength is largely a matter of the physical structure, and all factors known to affect this structure, such as rolling temperature, die contours, lubricants, drawing speeds, etc., are matters of prime importance. The experiments described here have been carried out during the past year at the Baltimore plant of the American Smelting & Refining Co., in connection with a general investigation of some of the questions mentioned above, with the object of studying the physical structure of hard drawn copper, wire and the influence of certain factors on that structure. The work has been of an exploratory nature, rather than comprehensive, but it was thought that the results might prove of sufficient general interest to warrant their publication. The bulk of the hard drawn copper wire used in places where strength is an important factor is manufactured to strict specification, based usually in the United States on that of the American Society for Testing Materials (B-1-23). This specification calls for almost as high a value of tensile strength; consistent with elongation, as it is possible practically to obtain, and only physically perfect material can be relied on to meet such a specification. Obvious defects, such as laminations produced through fins in the original rods or brittleness due to overdrawing, are usually recognized and need only passing reference. Laminations can be detected by twisting and untwisting the wire several times; they will show up on the surface in the form of fins. Fig. 1 shows a very bad example of this defect. The wire may be perfectly smooth before twisting but when such laminations are present they will readily show up under this treatment. This trouble is caused by similar defects in the original rod produced by overfills in rolling. Fig. 2 shows the cross-section of the rod from which the wire in Fig.1 was drawn.

Jan 1, 1928

By F. R. Koeberlin

ABOUT thirty miles south of the port of Coquimbo, Chile, nestling in one of the western outliers of the main Andes range, lies the little mining town of Andacollo, a place whose history and traditions make up one of the most romantic pages in the life story of this southern republic. The beginning of Andacollo is shrouded in the penumbra of the pre-Columbian era, but its first mining activity probably dates from about the years 1440 to 1460. It was in the middle of the fifteenth century that the Inca Tupac-Yupanqui, grandfather of Atahualpa, conquered this part of Chile. His domain extended even as far south as the present site of Santiago, and perhaps farther, but was maintained with increasing difficulty against the fiercely independent and indomitable tribes of Araucanian Indians of the South.

Jan 1, 1938

By Ionel Gardescu

IN connection with some of the experiments carried out by the writer on the behavior of gas and oil in a sand reservoir,1 an interesting phenomenon was observed which may throw some new light on the problem of recovery of oil from a natural reservoir. The experiments are intended to show the effect of the surface area of the occluded gas masses, originally present in a reservoir, on the further evolution of gas from the oil and its consequent effect upon the rate of production of oil. The apparatus used in the experimental work is shown in Fig. 1. It consists primarily of a sand reservoir R and a displacement chamber D, which is used to induce small variations in volume. The reservoir and displacement chamber form a unit, and a lowering of the plunger D is equivalent to increasing the volume occupied by the oil and gas in the reservoir. The reservoir was first filled with dead oil and maintained under pressure until it was ascertained that most of the free gas had gone into solution. The volume of free gas present in the reservoir was computed from the coefficient of compressibility of the fluids by means of the dis-placement chamber D, reading to 0.005 c.c. and a special gage J reading to 0.02 lb. per sq. in. The oil was saturated with gas under pressure in reservoir S by circulating the oil for a long period of time through the gear pump B. Subsequently, the saturated oil was circulated through the sand reservoir following the circuit S6, B, S5, R4, the sand reservoir R, R1, R2, F4, F1, back to reservoir S. In the following experiments the sand reservoir R was filled with gas-saturated oil at a pressure of 415 lb. per sq. in. with no free gas present. This was ascertained by. closing off all the outlet valves, and determining the coefficient of compressibility of the system by means of the dis-placement chamber D.

Jan 1, 1932

By F. H. Buttner, E. R. Funk, H. Udin

Gold wires, 5 mil in diam, are found to creep viscously up to approximately 5.5x106 dynes per sq cm around 1300°K. Beyond this point, an additional slip mechanism appears. The average coefficient in the viscous range at these temperatures is 18.9 ± 7x10 12 poises. This observation and other visual observations made during the experiments agree with Herring's predictions. EARLY creep studies by Chalmers on single crystals of tin produced some of the first experimental evidence to suggest that metals deform viscously under very light stresses. That is to say, over a small initial stress range up to 150 g per sq mm, the single crystals of tin elongated at a rate proportional to the stress. The proportionality constant between strain rate and stress is by definition the coefficient of viscosity. Chalmers named this range of proportionality the microcreep range. One of the first theoretical attempts to explain the microcreep phenomenon was given by Kauzman,' who applied Eyring'sQ eneral statistical mechanical theory of shear rates to creep data then available. From the rate theory, he deduced the general hyperbolic sine law for shear rate on the assumption that the distortion of the reaction path due to stress is negligible and that the system is an infinite continuum. In order to fit the available data to the equation, it was necessary to assume that creep occurs by shear of rather large blocks of material, rather than by an atomistic shear process as in diffusion. The size of the shear units was shown to increase with increasing temperatures and lower stress, or lower strain rates. In applying the hyperbolic sine law equation to the microcreep data of tin, it was shown by Kauzman that the unit shear blocks became quite small, which suggested to him that microcreep might be a self-diffusion process. Making this an assumption, Kauz- man reworked the rate theory and arrived at an equation where the shear rate is proportional to the stress. In the form of viscosity coefficient, the equation is: o- _ \LkT V = 2qAlA where u is the stress; S, the shear rate; X, the distance in shear direction moved by flow units relative to one another in the unit process; L, the distance between layers of units of flow; T, the absolute temperature; k, Boltzmann's constant; qAL, a constant proportional to the size of flow units; and kT A, the diffusion coefficient = ------kTe-Q/RT = K X2 h Kauzman applied the expression to molten lead with a fair degree of success, the calculated viscosity being low by a factor of four. For solid lead the result is 5000 times too high. Taking q = 1, and X = dA = L = 21 = nearest neighbor distance, Udin, Shaler and Wulff8 found the equation low by a factor of lo7 for solid copper. On the basis of the discrepancy in lead, Kauzman indicated that microcreep is probably not a simple diffusion process of molecular shear units, but one involving preferential diffusion paths, or even that diffusion in solids does not involve shear at all. Cottrell and Jaswon4 treat the microcreep phenomenon on the basis of slow moving dislocations and apply it to Chalmers' data on tin with fair success. Nabarro Suggested a microcreep model in which mass movement in the direction of pull is effected by the diffusion of holes. The tension on the crystal effectively creates a greater hole concentration at regions near the crystal surfaces perpendicular to

Jan 1, 1953

By Chas. A. Ashburner

The occurrence of oil- and gas-springs in the State of New York has been a fact of historical record since 1627, when the existence of the Cuba oil-spring was first recorded. The utilization of natural gas at Fredonia in 1821 attracted the attention of the public to the possibility of obtaining an illuminating gas by digging and drilling into the rocks. No active search was made, however, for oil or gas by the drilling of wells until after the discovery of commercial oil in Pennsylvania in 1859. In 1862 a well was drilled at Bradford, McKean County, Pennsylvania, but a few miles south of the New York state line, to the depth of 200 feet, in search of the oil-sand which had been found at Titusville, Oil City, and at other points in Western Pennsylvania. Immediately subsequent to this, other wells were drilled in search

Jan 1, 1888

By E. D. Gardner

Introduction Oil shale deposits have been exploited in various countries throughout the world, but generally with government aid. The oil-shale industry of Scotland perhaps is the oldest and best-known; the largest was conducted in Manchuria by the Japanese during World war 11 as a source of liquid fuels for military uses. In general, foreign oil-shale deposits that have been exploited are much lower grade than those in the western United States. Considerable interest began to be shown in western oil shales in 1916; the peak of activities was in 1923. The catlin operation, near Elko, Nevada, perhaps was the nearest approach in this country to an oil-shale enterprise on a commercial scale. Over 100 companies were formed, ostensibly for exploiting the oil shale; a large number of them, however, proved to be stock promotions only, which gave the embryo industry a black eye. The Bureau of Mines operated an experi-mental oil-shale retort plant near Rifle, Colorado, from September 1926 to June 1927 and again from April 1928 to July 1929, after which the plant was dismantled. By this time the East Texas oil fields had come ill and the country lost interest in substitute liquid fuels. During World War II the Nation again became concerned about the magnitude of its petroleum reserves. Congress (April 1944) directed the Bureau of Mines to build and operate demonstration plants to produce synthetic liquid fuels from coal, oil shales, and agricultural and other products; a five-year Program was authorized. *' a part of this program the Bureau of Mines has built, at Anvil Points near Rifle, Colorado, a retort plant and develOped an experimental mine to supply the plant with oil shale. An important part of the mining work at Rifle is to devise methods and select practices for mining the oil shale on a commercial scale at the lowest practicable cost. The product to be mined has a relatively low value, a fact that must be kept in in mind. The combined aim of those in charge of the mining and those in charge of retorting is to demonstrate that the shale oil can be produced at a cost per barrel corresponding to the current quotation for crude petroleum —or at least very close to it. Plans call for an uninterrupted flow of broken oil shale from the lace in the mine, through crushers, through the retorts and thence to the disposal dump. The disposal of the spent shale in the Ride area should present no unusual problem. Mining research has consisted so far of Paper studies of the general phases of the probleml determination of the widest Span that the roof Stone will stand safely unsupported, and drilling problems. underground development has not proceeded far

Jan 1, 1949

By Martin Rubenstein

CdS crystals have been grown from a number of metallic solvents such as bismuth, tin, lead, and cadmium. Etching studies have shown that plastic deformation occurs if the crystals are not removed from the solvent prior to the solidification of the solvent, on cooling. The deformed crystals show a umique exciton fluorescence as a function of edge dislocation density. If one grows the CdS in the eutectic alloy of the above four metals (commonly called Wood's metal) the crystals can be removed from the solvent with hot water and no plastic deformation occurs. In this paper, the liquidus solubility measurements of CdS, as a function of temperature, are presented. The data were obtained using a high -temperature filtration technique. CADMIUM-SULFIDE crystals have been grown from a number of metallic solvents1 such as cadmium, bismuth, tin, and lead. Liquidus solubilities of CdS in cadmium,2 bismuth,3 and tin4 have already been measured. Crystals of CdS, in all four metals, have been grown by solution growth: 1) by cooling a saturated solution and 2) by a solution transport method.1'"1 CdS crystals grown in these four solvents have a few characteristics in common: 1) 1.8°K photolumines-cent emission consisted mainly of the radiative recombination of the bound exciton commonly known as I,, 2) slip lines which could easily be seen by the naked eye, and 3) edge dislocation densities in the order of l05 per cu cm.1 It was decided that these slip lines and the high edge dislocation densities were caused by a plastic deformation of the CdS crystals. It was felt that this plastic deformation did not occur during the growth of the crystals nor during the cooling of the solution, but did occur when the solvent which was in contact with the crystals froze. If these assumptions were valid, the slip lines and the high number of dislocations could be reduced or eliminated by removing the crystals from the solvent before the solvent froze. Since crystals of CdS had already been grown separately in such solvents as bismuth, lead, tin, and cadmium, it was felt that crystals could be grown in a eutectic mixture of these four metals. In this work a eutectic (or near eutectic) mixture of bismuth, lead, tin and cadmium in the proportion 50, 26.5, 13.5, and 10 wt pct, respectively, was used to grow CdS crystals. Such a mixture has a melting point of about 70°C and is close in composition to the alloy commonly known as Wood's metals. If the crystals could be grown from this mixture of solvents, and if hot water (>75°C) could be used to separate the crystals of CdS from the metallic solvent, it was hoped that CdS crystals could be grown with little or no plastic deformation which had been ob- served when crystals were grown from these solvents uncombined. CdS crystals were grown from this low melting eutectic mixture of bismuth, lead, tin, and cadmium using the solvent transport method. CdS powder and the appropriate amount of metals were sealed in a quartz tube under a pressure of about 5 X 10-6 torr. This ampule was then placed in a vertical position in a furnace. The temperature was raised to about 900°C. The furnace was designed so that the top of the liquid column within the ampule was between 10° to 40°C higher than the bottom of the liquid column. These temperatures were measured on the outside of the quartz ampule. The ampule was maintained at temperature for 7 to 14 days (depending on the temperature at which transport was taking place) and then the furnace temperature was lowered until the temperature was about 125°C. The ampule was then removed from the furnace, placed in water maintained at about 90°C, and opened in this 90°C environment. The crystals could then be removed from this two-phase liquid (Wood's metal and water) by mechanically picking them out. Alternatively, the crystals could be quantitatively removed by adding an excess of mercury to the mixture of metals, crystals, and hot water. The hot solution of metals and the hot water could be evacuated using a small diameter tube connected to a vacuum. Small amounts of mercury and water could be removed by heating the crystals in vacuum. Crystals prepared using this technique showed no evidence of slip. However, some of these crystals did show edge dislocation densities as high as l04 per cu cm. Some few selected crystals showed no dislocations. Single crystals of CdS were grown as large as 5 by 5 by 0.5 mm. The ampules for the growth of these crystals were 13 mm O.D., 11 mm I.D., 150 mm! LIQUIDUS SOLUBILITY MEASUREMENTS The CdS starting materials was G.E. 118-8-2 powder which was fired in H2S at 1000°C, and then a vapor transport technique5 was applied to produce a "sound" mass of CdS. The Wood's metal was prepared by weighing out bismuth, lead, tin, and cadmium in the proportions of 50, 26.5, 13.5, and 10 wt pct, respectively. The bismuth, cadmium, and lead were from the American Smelting and Refining Co. (ASARCO) and all had purities of 99.999+ pct. The tin was 99.9999 pct spectroscopic grade from the Vulcan Materials Co. The appropriate mixture was placed in a quartz tube, evacuated to a pressure of 5 X 10-6 torr, melted to a liquid, cooled to room temperature under this same vacuum. This ingot was then placed in another quartz tube, evacuated to 5 x l0-6 torr, and sealed off under vacuum. The ampule was then horizontally placed in a furnace. The temperature was raised to 600°C, and over a period of several hours the ampule was vigorously shaken several times. The ampule was then removed from the furnace, and the metallic liquid was

Jan 1, 1970

By GERALD H. HUTTON

SINCE the inception of dredge mining, the attention of engineers and operators has been directed primarily toward mechanical improvements and refinements calculated to, reduce operating costs and to increase recoveries. The result has been to develop an efficient excavating and value-saving machine, which, in some instances, has an actual capacity of 15,000 cu yd. per day. Steel hulls and superstructures minimize the risk of destruction by fire and lengthen the life of the plant. Dredges now restore, to some extent, agricultural possibilities to mined ground. Large buckets, with correspondingly heavy parts, are able to handle heavy wash and massive boulders. Mechanical weaknesses have been strengthened. The use of manganese steel in bucket lines and tumblers permits the application too the bank of a digging force that can be withstood only by solid material, such as rock, cement or frozen ground. Various alloys of steel have been applied to certain duties and experiments in their heat treatment are still progressing. Haulage by tractor or truck is in common use. Discarded and worn steel parts are repaired or rebuilt by the use of the oxy-acetylene flame and the arc-welding machine. Gold and platinum saving is more efficient, although still subject to improvement. Dredging for tin ore is in successful operation. Crews are now highly specialized and experience has developed improved methods of work; particularly in the manipulation of dredges to build levees of tailings and to leave open waterways where desired. To sum up by the distribution of overhead expense over several units, ground under favorable conditions can now be dredge-mined for 5)2 c. per cu: yd., in spite of the increase in cost of supplies, power, and labor during, the past few years. Improvements in prospecting methods, however, have not kept pace with mechanical developments. Standard practices of ; testing ground today produce only wide approximations of values; although they obtain information concerning the character of the deposit and bedrock. It is interesting to note that few important changes in the methods of ten years ago are .to be recorded; the latest comparisons between pros¬pecting results and mined recoveries-have been at such variance as to cause confusion to the operator, and, in a degree, the sacrifice of the confidence of the capitalist. On this account, and because the growing scarcity of dredging ground. demands closer calculations on the part of the engineer, this appeal for collaboration and

Jan 1, 1921