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By K. Brack, G. H. Schwuttke

Annealing properties of subszerface amorphous lavers produced through high-energy ion implantation in silicon are studied. The buried layers are produced through the implantation of ions (nitrogen), ranging in energy from 1.5 to 2 mev. X-ray interference patterns, transmission electron microscopy, and resistivity profiling are used to study the annealing characteristics of the ion damage. The annealing experiments indicate a low temperature (below 700°C) and a high temperature (above 700°C) region. Significant changes occur in the amorphous layer during the high-temperature anneal. Such changes are corre-lated with the re crystallization of the amorphous silicon and the formation of subsurface (buried) silicon-nitride films. TODAY'S main problems in the field of ion implantation are related to the accurate determination and prediction of 1) the distribution profiles of implanted ions, 2) the lattice sites occupied by the implanted ions, 3) the lattice damage produced through ion implantation, and 4) the annealing characteristics of damage centers in the lattice. This paper reports investigations concerned with the problems listed under 3) and 4). EXPERIMENTAL Our investigations cover the energy range of incident ions from 100 to 300 mev and from 1 to 2.5 mev. The emphasis of this study is on the energy range from 1.5 to 2 mev. The experiments are conducted with single charged nitrogen ions. To implant the ions a van de Graaff generator is used as described by Roosild et al.1 Accordingly, a gas containing the desired ion specie is passed through a thermome-chanical leak into a radio frequency activated source. The positive ions are driven into the van de Graaff with the help of a variable voltage probe. Emerging from the accelerator the ions drift into a magnetic analyzing system and here the desired ion specie is bent 90 deg into the exit port. The ion beam leaving the analyzer is defocused and drifts down a 4-ft long tube to hit the silicon target. At this position the 20 pamp ion beam has a circular cross-section of 2.1 cm. N2 is used as a source gas for nitrogen ions. The implantation target is silicon with zero dislocation density, 2 ohm-cm resistivity, (111) orientation, mechanically-chemically polished, and 1 mm thick. The target is mounted on a water-cooled heat sink and kept at room temperature. A fluence of 1015 to 1016 ions per sq cm is used. RESULTS 1) Silicon Perfection after Bombardment. High-energy ion bombardment of silicon has some striking effects on lattice perfection. Some results were reported in detail previously at the Santa Fe conference2 and are here briefly summarized for the benefit of the experiments described in the following. 1.1) Identification of Surface Films on Silicon. After bombardment all samples are found to be coated with surface films. The films on the silicon surface vary in thickness and color; they can be transparent, slightly brown, or opaque. The films are thicker and darker in the high-intensity area of the beam and they delineate the bombarded surface area of the crystal. The films produce electron diffraction patterns characteristic of carbon and of SiO2. Carbon is predominant. The presence of carbon in these films was confirmed by use of the electron microprobe. Formation of the films occurs independently of the ions used and is attributed to a contaminated vacuum of the high-voltage machine. The carbon is most likely the product of the pump oil which is cracked and polymerized under ion impact. The films stick tenaciously to the silicon surface and burn off in a low-temperature Bunsen flame. 1.2) Mechanical Perfection of the Silicon Surface. The mechanical perfection of the bombarded silicon surface was investigated through optical microscopy, electron microscopy in which the replica technique is used, and optical interferometry. No mechanical damage of the surface was visible after bombardment. However, if a bombarded sample is soaked for several minutes in hydrofluoric acid (HF), gas bubbles may develop in certain spots of the silicon surface. It is also noted that in these areas the surface film starts to peel off. Relatively large patches of film come off if the sample is soaked in HF during ultrasonic agitation. After HF treatment, pits may be present on the silicon surface. The pit dimensions are estimated to be as large as 50 µ. The pits appear in the region of most intense irradiation. 1.3) Lattice Perfection After Bombardment. No lattice damage is found on the silicon surface. Electron transmission micrographs and selected area diffraction patterns of the surface show no difference before and after bombardment. Measured approximately 2 µm down from the surface, the silicon lattice throughout this depth is of good perfection. Well-defined Laue spots and Kikuchi lines are obtained from the surface as well as from the indicated area below the surface. However, some radiation damage is dispersed in this top layer. A sharp boundary line separates this surface layer from a highly damaged layer which extends further downward into the silicon. Typical of this

Jan 1, 1970

By Stephen Taber

JOHN C. BRANNER, Stanford University, Cal. (communication to the Secretary *).-Wideawake teachers of geology are constantly on the lookout for good illustrations of veins, especially where the processes of formation are either clearly shown or suggested. And I long ago found out that one who would learn nature's laws must despise nothing. It thus happened that in 1910, Dr. George J. Peirce of the depart-ment of botany at Stanford University called to my attention a cracked and broken yellow earthenware dish, 8 ½ in. across the top and 2 ½ in. deep, that, to the ordinary observer, seemed to be of no further use, and quite ready for the waste can. The striking thing about this dish was that the thin glaze over much of the outside surface and over the upper margin of the inside surface had been lifted in small scales, varying in. diameter from ½ cm. to 1 cm., and thrust outward and held there by some sort of white fibrous mineral. The process looked very much like one we are familiar with in the Southern States where. we often see in the winter pebbles and soil thrust out from a clay bank or lifted from a clay soil and held there supported by what is popularly known as needle-ice. Upon inquiry I learned the following facts in regard to the history of this particular dish: In the summer of 1910, it had been partly filled with a concentrated salt solution taken from one of the salterns of the Stauffer Chemical Co. at Redwood City, Cal. A qualitative analysis of the original brine showed: Present: iron, magnesium, sodium, potassium, chlorides, sulphates, nitrates (trace), bromides, carbonates, borates (trace), and considerable amounts of organic matter. Absent: calcium, lithium and iodides.

Jan 3, 1917

By H. A. Baumann, A. J. Rostosky

EVER since the first installation of wet-washing methods of coal preparation, the removal of the water added by the washing process has created serious technical and operating problems. The rapid development and widespread adoption of wet washing has necessitated a corresponding development of dewatering methods and equipment. The amount of water retained by coal varies with the size of the coal. The moisture that is largely on the surface of the particles is easily shaken off coarse coal; thus coarse coal can be dried comparatively easily and quickly. Fine coal presents a larger surface area than does coarse coal, so its capacity for retaining moisture is greater. In fine coal, moisture below about 5 per cent is held between the coal particles and its removal is difficult. Draining and drying of the finer sizes is a major problem at many washeries. Two common problems of coal-washing practice that are intimately connected with dewatering and drying are the clarification of washery water and the prevention of stream pollution. The first field has been studied from many angles, including the use of coagulating and settling agents followed by vacuum filters to remove the solids, and the use of sludge tanks with dewatering screens incorporated therein. In many districts, the disposal of sludges into streams has been stopped by law. The lack of space for impounding sludges has created problems of disposal in other districts. Reduction in moisture means a saving in freight costs as well as the elimination of difficulties in unloading and storing. Excess moisture in coal causes it to freeze in localities where severe climatic conditions prevail. Excess water in coals to be used in the production of coke and manufactured gas has a chilling effect on the walls of the oven or retort. Dryness of coal is important in producing good briquettes. CLASSIFICATION OF MOISTURE Moisture in coal can be classified as inherent and surface moisture. Inherent moisture is regarded as a part of the true coal substance, having been present in the original vegetal matter from which coal was

Jan 1, 1943

By O. Hoover, M. Herman, V. V. Damiano

The Jetter and borie' teclznique of determining textures using a spherical specimen has been applied to tlze study of compression-rolled beryllium sheet. Snzall spheres the order of 1 mm in diam cut from the beryllium sheet were autotnatically rotated about tz41o axes using the G.E. single-crystal goniometer. Quantitative pole figures were obtained without tke need to apply absorption corrections. Compression-rolled beryllium exhibited peak intensities ,for (0002) planes of positions tilted 10 deg to the rolling plane and a near random distribution of (1010) planes about the nornal to the rolling plane. TECHNIQUES for determining textures of rolled sheet material are amply described in the literature. The techniques are found to be variations of two basic methods. One due to Decker, Asp, and arker, referred to as the transmission method, utilizes a thin-sheet specimen in which the X-ray beam enters the specimen from one side and the intensity of the beam which emerges from the opposite side is measured. The second method due to chulz,3 referred to as the reflection method, utilizes a thick specimen and the intensity of the beam emerging from the same side is measured. The two rotations of the specimen in the beam are designated a and 8. In order to completely determine the texture of sheet material, it is generally necessary to use a combination of the two methods. The calculations involved in correcting the raw X-ray data for absorption effects and the combining of the data obtained by the two methods are very laborious and time consuming. To avoid the intensity corrections which arise as a result of the changing diffraction volume and path length within the sample other methods have been proposed. The Norton method utilizes a cylindrically shaped specimen cut from the sheet material. Since the rods have rotational symmetry, the absorption correction is constant for rotations about the sheet texture. Jetter and Borie' employed a spherical specimen to analyze the fiber texture of extruded aluminum rods. The spheres were rotated rapidly about the fiber axis to include a large number of grains in the X-ray beam and changes in intensity with respect to tilts of the fiber axis were measured. The absorption correction was constant for all angles and was neglected. The Jetter and Borie' technique finds excellent ap- plication to very fine-grained low-absorbing metals in which the entire sphere volume can contribute to the diffraction volume. In the case of low-absorbing metals, however, serious limitations on specimen thickness occur as demonstrated by Braggs due to de-focussing effects. Peak shifts may occur which negate the assumption that integrated intensities are proportional to peak intensities. These limitations in sphere size to the order of 0.5 to 1 mm for beryllium require that the grain size be sufficiently small to include a large enough statistical sample. The present paper describes the application of spherical specimens less than 1 mm in diam to the quantitative determination of pole figures for compression-rolled beryllium sheet having a grain size the order of 10 p. EXPERIMENTAL 1) Specimen Preparation. Two techniques for spark-machining beryllium spheres were tried. One involved the use of a hollow cylinder as a cutting tool. The tool was fed into the rotating cylindrical specimen as shown in Fig. l(a). The hollow cylinder was carefully aligned such that the axis of the cylinder and the axis of the specimen lay in the same plane and were 90 deg to each other. As the hollow cylinder was fed into the rotating cylindrical specimen, a spherical shape was formed as shown in Fig. 1. Alignment was very critical. Slight misalignment resulted in the formation of a barrel-shaped specimen instead of a sphere. A second technique involved the use of a cutting wheel shaped as shown in Fig. 2 with a groove of the desired radius. A section of the sheet specimen was first turned into a cylinder on the left part of the cutting wheel. It was then shifted to the right and a spherical specimen was turned as shown in Fig. 2. The axis of the cylinder lay in the plane of the sheet. Flats corresponding to the rolling plane of the sheet were used to grip the specimen during the machining operation and these served to identify the rolling plane of the sphere. 2) Rotation of Spec=. The spherical specimen is shown mounted on the G.E. single-crystal goniometer in Fig. 3. The knob A of the goniometer shown in Fig. 3 rotates the specimen about the pedestal axis. These angles have been designated as @ angles. The knob B rotates the specimen about an axis perpendicular to the pedestal axis. These angles have been designated as p angles. A device was made to automatically drive the single-crystal goniometer by means of two flexible shafts connected to the A and B knobs as shown in Fig. 3. The motor system was designed to rotate the knob A, thus rotating the specimen through angles of $I while the B knob remained stationary. After one complete

Jan 1, 1967

By J. F. Bryson

Instantaneous outbursts of coal in underground workings have occurred frequently in various coal fields in Nova Scotia; British Columbia; Canada; South Staffordshire, England; and the states of Washington, Virginia, West Virginia and eastern Kentucky in the United States. Such outbursts in eastern Kentucky have been called "mountain bumps " because they are more likely to occur under mountain cover than elsewhere, but recently they have become generally known as "coal bumps." The eastern Kentucky coal field has been troubled by these outbursts since 1923. Many men have been injured and killed, and the morale of the workmen in the vicinity of such outbursts has been affected to such an extent that mine production has suffered for a considerable period following each outburst. Such phenonlenal occurrence in any coal field naturally has led to discussion as to the cause and means of prevention. In the eastern Kentucky field, local mine officials, workmen, mining engineers, and many others have offered many ideas as to the cause and many methods of prevention have been suggested, and tried without success. Some of the plans were either practically or economically unsound and in general impossible to follow. To enumerate all the suggestions would require a large volume. One cause mentioned was that they might be due to gas under high pressure, as in Lower Silesian mines, and the remedy reeommcnded was to drain the gas by drilling holes into a suspected area. A hole 30 ft. long was drilled into a 60-ft. pillar to allow the gas to drain off, hut the pillar bumped the next day. Realizing the importance of obtaining the best information available on coal bumps, the writer, with the permission of the Harlan County Coal Operators' Assoeiation, invited Mr. George S. Rire, Chief Mining Engineer of the U.S. Bureau of Mines, who had investigated bumps in several countries, to conduct an investigation of coal bumps in this field. Mr. Rice, by permission of the Director of the G.S. Bureau of Mines, accepted the invitation, and it was the writer's privilege, in company with

Jan 1, 1936

By J. F. Bryson

Instantaneous outbursts of coal in underground workings have occurred frequently in various coal fields in Nova Scotia; British Columbia; Canada; South Staffordshire, England; and the states of Washington, Virginia, West Virginia and eastern Kentucky in the United States. Such outbursts in eastern Kentucky have been called "mountain bumps " because they are more likely to occur under mountain cover than elsewhere, but recently they have become generally known as "coal bumps." The eastern Kentucky coal field has been troubled by these outbursts since 1923. Many men have been injured and killed, and the morale of the workmen in the vicinity of such outbursts has been affected to such an extent that mine production has suffered for a considerable period following each outburst. Such phenonlenal occurrence in any coal field naturally has led to discussion as to the cause and means of prevention. In the eastern Kentucky field, local mine officials, workmen, mining engineers, and many others have offered many ideas as to the cause and many methods of prevention have been suggested, and tried without success. Some of the plans were either practically or economically unsound and in general impossible to follow. To enumerate all the suggestions would require a large volume. One cause mentioned was that they might be due to gas under high pressure, as in Lower Silesian mines, and the remedy reeommcnded was to drain the gas by drilling holes into a suspected area. A hole 30 ft. long was drilled into a 60-ft. pillar to allow the gas to drain off, hut the pillar bumped the next day. Realizing the importance of obtaining the best information available on coal bumps, the writer, with the permission of the Harlan County Coal Operators' Assoeiation, invited Mr. George S. Rire, Chief Mining Engineer of the U.S. Bureau of Mines, who had investigated bumps in several countries, to conduct an investigation of coal bumps in this field. Mr. Rice, by permission of the Director of the G.S. Bureau of Mines, accepted the invitation, and it was the writer's privilege, in company with

Jan 1, 1936

By Harrison Souder

THE object of this paper is to bring to. the notice of engineers a safety detonating fuse by the use of which misfires in blasting may be eliminated and safety in blasting operations promoted. This new detonator is a French invention and is known as Cordeau detonant or detonating fuse and is sold under the name of Cordeau-Bickford. It consists of a lead tube 5 to 6 mm. in diameter, filled with trinitro-toluene. While applicable to all classes of mining it will appeal especially to those who have to do with deep-hole blasting in open-cut clines or quarries, or any operations where a large number of holes are to be shot at one time. Since the introduction of the deep-hole blasting in the Cornwall iron mines, much trouble has been experienced from misfires and many experiments were made to determine the best and safest method of blasting. Before the introduction of the detonating fuse it was found that to insure the best results, two or more high-power electric exploders, not less than No. 6, with specially insulated conductors, should be placed in each hole; the holes wired in parallel, and for a large number of holes the current to be supplied by a live wire to the bus or lead wires at about the middle of the bench. The voltage in general use is 110 to 220, but as our material is a magnetic iron ore and the holes are generally damp, we found it advisable to reduce this to about 30 volts to prevent short circuits. A No. 7 or No. 8 special insulated detonator was adopted. But with the best of care and attention to the minutest detail, we were not able to eliminate occasional misfires and the consequent ever present danger of accidents.

Jan 10, 1914

Executive SIDNEY .J. JENNINGS, Chairman GEORGE D. BAR HON .I. E. JOHNSON, JR. EDWIN LUDLOW ROBERT M. RAYMOND Membership KARL EILERS, chairman LEWIS W. FRANCIS .1. E. JOHNSON, JR. LOUIS D. HUNTOON ARTHUR. L. WALKER Finance GEORGE D. BARRON. Chairman. CHARLES F. RAND BENJAMIN B. THAYER Library E. GYBBON SPILSBURY1 Chairman ALEX C. HUMIPHREYS3 GEORGE C. STONE .J. H. JANEWAY4 BRADLEY STOUGHTON Papers and Publications BRADLEY STOUGHTON, Chairman

Jan 10, 1918

By E. Stansfield, J. W. Sutherland

It is well known that the ash left when coal is burned is not the same either in chemical composition or in weight as the mineral matter originally present in the coal. This mineral matter has been referred to as "mineral impurity," "ash-forming constituents" and "corrected ash." The authors prefer the simple name used in the title and throughout this paper. The mineral matter in a sample of coal cannot be isolated unchanged and then weighed; but if the relation between the weight of mineral matter in the coal and the weight of ash remaining when the coal is burned can be ascertained, the weight of mineral matter in the sample can be calculated from the determined weight of ash. When the weight of mineral matter in the sample is known, the weight of pure coal can be found by subtraction. This pure coal must be the basis of accurate coal classification. W. F. Wheeler,l,3 W. Brinsmaid,2 S. W. Parr, and many subsequent workers have studied the relation between mineral matter and ash. Wheeler and Parr and others have deduced formulas for calculating this ratio, and used heavy-solution separations for checking the accuracy of their formulas. Brinsmaid hand-picked and analyzed two separate samples (and mixtures of these) and based thereon a graphical method of deducing the ratio. In the Fuel Testing Laboratories of the Scientific and Industrial Research Council of Alberta, a graphical method, based on heavy-solution fractionation of coal samples, has been used with marked success for the past 7¼ years for determining the mineral matter-ash ratio. This method resembles that employed by Brinsmaid in 1907.

Jan 1, 1930

By E. J. Whittenberger, F. N. Rhines

The formation of casting porosity is viewed as a nucleation and growth process with solidification shrinkage and gas precipitation as cooperative driving forces. Experimental evidence evaluating the individual contribution of each force confirms the major premise that microporosity is nucleated by gas precipitation. Additional data disclose the effects of the identity and quantity of gas, the temperature range of freezing, and the freezing rate upon the amount and distribution of porosity in light metal castings. POROSITY, as it commonly occurs in metal castings, has been ascribed to the contraction that accompanies the freezing of the metal, to the evolution of dissolved gases from the liquid during cooling and freezing, and, most frequently, to a combination of the two.'" "Pipe" formation is universally associated with solidification shrinkage; spherical "gas holes" are understood to be retained bubbles of gas; but the origin of microporosity, which usually exhibits an irregular or scalloped outline when viewed in cross-section, remains a subject of continuing debate.", ' The present research constitutes an endeavor to show what parts are played respectively by shrinkage and gas evolution in the initiation and growth of micropores and what factors determine their number, size, shape, and distribution. A preliminary outline of the mechanism of cavity formation in castings will serve to coordinate the experimental findings that will be reported and will at the same time provide a general theory of the origin of casting porosity. Basic to the mechanism of cavity formation that will be proposed are the following established facts: 1—that liquid metals and alloys contract gradually during cooling down to the freezing range, where a relatively large contraction, known as the "solidification shrinkage," takes place (exceptions in bismuth and gallium being noted);' 2—that the capacity of liquid metals and alloys for dissolving gases diminishes with cooling until, in the freezing interval, a large decrease takes place (various exceptions being noted and excluded from present consideration) ;.: and 3—that freezing proceeds counter to the direction of heat flow, the freezing front most commonly being composed of a system of tapering dendrite stalks and side arms which are coarser the lower the freezing rate and which protrude into the liquid for a distance that is greater the longer the freezing temperature interval of the alloy and the smaller the thermal gradient.' The mechanism by which voids are generated

Jan 1, 1953

By W. F. Guenther

The usual hand-operated drilling outfit consists of a 4-in. post-hole auger with 3/4,-in. pipe for drill stem, in 4-ft lengths, with a turning handle fitted to a top pipe T. The auxiliary tools are: a chisel-bit drill made from 3/4 or 7/8-in. tool steel welded to a 4-ft length of 3/4-in, pipe, so that the regular pipe string can be used; also a churn or "mule foot" made from 3-in. pipe, slotted on one side, belled to a 4-in. tempered cutting edge on the bottom, all welded to a 3/4-in. coupling by a yoke. Other tools required are pipe wrenches and cleanout tools made from old auto springs (Fig I). A 4 1/2 or 5-in. collar welded to a plate is often used to protect the mouth of the drill hole. In general the auger is used in the typical clay overburden and brown phosphate matrix, which is relatively soft. The churn or "mule foot1' is used in hard pan, lump phosphate or cherty ground. The drill is used for breaking flint, often found loose in the overburden. The drill with the chisel bit is used for trimming sides of the hole, sounding for lime bottom and breaking through hard lumps. Holes have been drilled to a depth of 80 ft, but the limit of efficient operation is about 50 ft. In deep holes it is necessary to unscrew the string in 20-ft lengths, to

Jan 1, 1948

By W. F. Guenther

The usual hand-operated drilling outfit consists of a 4-in. post-hole auger with 3/4,-in. pipe for drill stem, in 4-ft lengths, with a turning handle fitted to a top pipe T. The auxiliary tools are: a chisel-bit drill made from 3/4 or 7/8-in. tool steel welded to a 4-ft length of 3/4-in, pipe, so that the regular pipe string can be used; also a churn or "mule foot" made from 3-in. pipe, slotted on one side, belled to a 4-in. tempered cutting edge on the bottom, all welded to a 3/4-in. coupling by a yoke. Other tools required are pipe wrenches and cleanout tools made from old auto springs (Fig I). A 4 1/2 or 5-in. collar welded to a plate is often used to protect the mouth of the drill hole. In general the auger is used in the typical clay overburden and brown phosphate matrix, which is relatively soft. The churn or "mule foot1' is used in hard pan, lump phosphate or cherty ground. The drill is used for breaking flint, often found loose in the overburden. The drill with the chisel bit is used for trimming sides of the hole, sounding for lime bottom and breaking through hard lumps. Holes have been drilled to a depth of 80 ft, but the limit of efficient operation is about 50 ft. In deep holes it is necessary to unscrew the string in 20-ft lengths, to

Jan 1, 1948

By FREDERICK J. ALCOCK

THE high prices which lead and zinc have commanded during recent months have given a great impetus to search for workable deposits of these metals, and there has accordingly risen a demand for information about deposits which have been worked in the past and which might possibly be opened up anew under these more favorable conditions. Production of zinc and lead in Canada has been on the increase during the last few years. In 1924, 175,- 485,499 lb. of lead with a computed value of $14,221,- 345 were mined. Of this, 96 per cent. was produced in British Columbia, 3 per cent. in Ontario, while Quebec and the Mayo district of the Yukon accounted for the remaining one per cent. During the same year the production of zinc amounted to 98,909,077 lb.. valued at $6,274,791. Of this 96,000,069 lb. were produced in British Columbia and the remaining 2,909,008 in Quebec. The large producer of zinc and also of lead is the Sullivan Mine at Kimberley, B. C. In comparison with the Sullivan, the deposits which are known to occur in eastern Canada are relatively small. Two, however, the Kingdoll lead mine at Galetta, Ontario, and the Tetreault zinc property at Notre Dame des Anges, Quebec, are steady producers. The object of this paper is to describe briefly these and other deposits of eastern Canada, to show their relation to geological events and to point out what are the chances of any of those which are idle at present developing into active producers or what are the possibilities of new deposits being discovered.

Jan 1, 1926

By L. W. Pommier, F. B. Brien

In order to determine the ability of cyclones with heavy liquids to preconcentrate ores, a study of the variables which govern the behavior of the solids in the apparatus has been made. To assess the test results, the cyclone products have been examined by sink and float analysis at various specific gravities and the results examined by the Tromp type curves. This analysis has allowed the development of the SG50 unit — specific gravity of the particles, 50% of which goes to overflow and 50% to underflow — rather than the d50 (size) unit used in classification. The results of tests using the closed circuit laboratory cyclone assembly with dry feed samples show the validity of the equation: Results indicate that 83% of the feed may be rejected containing 0.1% Sn. Recoveries in excess of 80% are obtained at a grade of 1.7% Sn from feed samples assaying 0.4% Sn. As water-wetted particles may comprise the plant feed, separate tests were performed to examine the effect of water in the feed material. Results indicate that the entrained water divides into two fractions, one of which is defined as free water and is rejected to the cyclone overflow, the other fraction forms an adhering envelope of water on the ore particles, altering their effective size and density. The presence of the envelope of water on the particles increases the ease with which the heavy liquid can be recovered but decreases the concentration efficiency. It is proposed that the detrimental effect of water in the cyclone may be minimized by using a higher feed pressure cx by the use of surfactants. A higher feed pressure, by increasing shearing forces, would reduce the thickness of the water envelope on the particles. The surfactants, by adsorbing on the particles and producing hydrophobic surfaces, would displace the water envelope and allow the heavy liquids to wet the modified surfaces. In both cases a larger proportion of the entrained water would report to the cyclone overflow as free water, thus minimizing the detrimental effect of water on the concentration efficiency. Additional testing is required on the behavior of water in the system; to determine the optimum particle size for the preconcentration step; to determine final particle size for optimum liberation and subsequent treatment of the products in present plants and to determine the efficiency with which the heavy liquids may be recovered from the products. For many years tin mining in Bolivia has been very important to the economy of the country. In recent years the tin content of the ore reserves has been steadily declining. An improvement in concentration efficiency is highly desirable in order to increase productivity from the present low-grade mine ores and to allow retreatment of the many millions of tons of tailings from past operations, some of which equal the present ores in tin content. A number of investigators have been or at present are working on various phases or approaches to the problem. Gravity concentration is used in Boliva today as it has been in the past to recover tin minerals from the mine ores. An objective of the work reported in this paper was to examine the possibility of treating present low-grade ores and sink-float tailings products, at a relatively coarse grind, in order to produce a higher grade feed material to the present gravity concentration plants. The possibility of using heavy liquids in cyclones to treat large tonnages with a minimum of outlay presented itself and is of particular interest since heavy liquids are now available with physical properties which lend themselves to simple recovery methods. Tests were carried out using a closed circuit laboratory cyclone assembly. It was desirable to determine the value of using the SG50 concept and Tromp curves for analyzing the cyclone concentration test results. The effects of entrained water on the behavior of ore particles in the cyclone were examined. THEORY AND TECHNICAL CONSIDERATIONS Three types of heavy liquids are available: aqueous solutions of very soluble salts, salts or mixtures of

Jan 1, 1964

By George F. Comstock

IT has been reported recently1 that the hardenability and toughness of forging steels may be improved appreciably by the use of complex deoxidizers containing titanium, aluminum, and vanadium. In the light of these results, an investigation of similar deoxidizers containing various hardening and grain-refining elements was proposed. These deoxidizers included three manganese-silicon-aluminum-titanium al- [ ] loys with and without boron and calcium, three titanium-aluminum ferroalloys with vanadium, molybdenum and zirconium, respectively, an aluminum-zirconium ferro-alloy, and plain ferroboron. Their approximate compositions are given in Table I, and the results obtained so far in the investigation of their effects on steel are presented in the later parts of this paper. METHOD OF USING DEOXIDIZERS The deoxidizers listed in Table I were used in three series of 0.40 per cent carbon steels, which were melted in a small basic-lined induction furnace and cast in the form of I7-lb. ingots about 2.75 in. square. The basic charge for each heat was 10 lb. Armco iron and 6 lb. of clean low-carbon sheet-steel scrap. When melted, this charge was deoxidized with 15 grams of ferrosilicon, then about 500 grams of pig iron was added to give the desired carbon content. After the pig iron was dissolved, nickel [ ] shot and high-carbon ferrochromium were added if required, and additions of 80 per cent high-carbon ferromanganese and 50 per cent ferrosilicon were made to provide the proper amounts of those elements. Aluminum was added to every heat 2 min. after the silicon, for grain-size control and preliminary deoxidation. One minute later the special deoxidizer was added to the clean bare surface of the molten steel, and 2 min. afterward the steel was poured into the ingot mold, using a hot-top and pipe-preventing compound after pouring to decrease the depth of the shrinkage cavity. The special deoxidizers were used mostly in the form of about ½ to ¾ -in. lumps,

Jan 1, 1942

By T. P. Chen, F. W. Bowdish

Studies made with a captive bubble apparatus on the sulfidization and collection by amyl xanthate of true chrysocolla specimens have defined the ranges of pH value and sulfide concentration which permit contact between the bubble and the mineral surface. Titanium compounds were the most effective of the materials found to activate the sulfidization of chrysocolla. With titanium activation, the contact angles and the ranges of pH value and sulfide wncentration giving bubble contact were all increased. Chrysocolla ores were concentrated by flotation. Chrysocolla ores occur at many localities in grade and quantity sufficient to make mining and millin feasible, but no satisfactory method of concentratio has been found. Although chrysocolla may be leached with acid, only those ores without acid-consuming gangue may be leached economically. Because of its potential importance, a study of the conditions nece sary for flotation of chrysocolla has been carried ou The literature contains a few references to flotation of chrysocolla. Two methods were developed by the U. S. Bureau of Mines.1,2 The first consisted of a fatty acid soap and a high xanthate as collectors of chrysocolla from a synthetic ore, while the second involved the use of hydrogen sulfide and xanthate. Ludt and DeWitt3 demonstrated the difference in adsorptive powers of chrysocolla and quartz for bas triphenyl methane dyes and suggested the use of butyl, hexyl or octyl-substituted malachite green as collector. Jackel4 emphasized the effects of combin tions of reagents such as Aerofloat 31, pine oil, and Reagents 404 and 425 with sodium sulfide and zinc hydrosulfite as conditioning agents. Although he reported recoveries of 89% from a synthetic ore and 98% from a natural ore containing azurite, malachite, chalcopyrite and chrysocolla, careful application of Jackel's method to chrysocolla from Tyrone, N.M., failed to give a high recovery. MATERIALS AND TECHNIQUE Samples from Inspiration, Ariz., and Tyrone and Magdalena, N. M., were used for experimentation and verified as true chrysocolla by leaching tests, specific gravity tests and X-ray diffraction. Chrysocolla does not dissolve at pH 4, although malachite and azurite do. Chrysocolla is about half as dense as the copper carbonates. X-ray diffraction analyses by the powder camera method confirmed the samples as true chrysocolla. A captive bubble apparatus, which cast an enlarged image of the air bubble and the mineral surface upon a screen, was used to check on the character of the surfaces. The specimens were prepared by grinding a flat surface on a glass plate using fine abrasive; then they were washed and kept in distilled water until they were to be treated with reagents. Before each reagent treatment, the specimen was carefully checked for cleanliness in the captive bubble apparatus. It was assumed that the surface was clean if, after fine grinding and washing of the specimen, the bubble would not stick. Specimens were handled with glass forceps, and precautions were taken to avoid contamination of the mineral surfaces. Contact angle measurements were carefully made several times on each treated specimen to obtain reliable average values. EFFECT OF pH VALUE AND SODIUM SULFIDE CONCENTRATION In each experiment, a specimen with a freshly ground surface was immersed for 10 min in a solution of sodium sulfide, washed and immersed for 15 min in a solution containing 30 mg per 1 of potassium amyl xanthate. The specimen was then washed again in distilled water and tested for contact angle in the captive bubble apparatus while submerged in distilled water. In this series of experiments, the pH of the sulfidizing solution was varied from 3 to 7, and the concentration of sodium sulfide, containing 60% Na2S, was varied from 50 to 650 mg per 1. Many combinations of pH value and sulfide concentration resulted in no contact between the bubble and the surface, but over a limited range of conditions, contact angles varying from 24ºto 52ºwere obtained. The data in Fig. 1 show sulfidization conditions that lead to bubble contact and those that do not. The region of contact is surprisingly small, which may indicate why flotation of chrysocolla involving sulfidization has proven so difficult in practice. Several features of the system are illustrated in Fig. 1. In the region between pH values of 4 and 6 with sodium sulfide concentrations below about 350

Jan 1, 1963

By C. R. Boyd

WITHOUT attempting to do more than give a preliminary or skeleton report upon the geology and minerals of Southwestern Virginia at this time, I am led to hope that the great commercial importance of the sixty miles of cross-section here crudely treated of

Jan 1, 1877

By A. S. Venkatadri, H. B. Bell

The equilibrium sulfur distribution between molten iron and Ca0-Mg0-Al203 slags containing iron oxide was investigated at 1550°C. The results were used to derive the iron oxide activities at low iron oxide concentrations in the slag by combining the sulfide capacity data obtained from gas-slag work with the free energies of both the sulfur solution in iron and the iron oxide formation in slag. The derived ferrous oxide activities were compared with values based on Tem-kin's kin's and Flood's ionic models. One difficulty in using these models is that the nature of the aluminate ion in slag is uncertain. Nevertheless, such indirect methods, in particular, those described in the present paper, are of value because of the difficulty of measuring small amounts of oxygen in liquid iron in equilibrium with slag. It is shown that these methods confirm the consistency of thermodynamics data on liquid iron and slags. It is well established that decreasing the iron oxide activity in the slag increases the desulfurization of molten iron at constant slag basicity. This effect is most pronounced at the very low iron oxide activities, characteristic of blast furnace slags. Yet a precise quantitative determination of the significance of low iron oxide contents in slag in blast furnace desulfuri-zation is not possible for the following reasons: a) difficulty of separation of iron "shots" from the slag, and b) errors in chemical analysis of small amounts of iron oxide in slags. In view of these obstacles, one must resort to indirect methods of calculating iron oxide activities. EXPERIMENTAL TECHNIQUE The apparatus for providing the sulfur equilibrium data has been described previously1 and was similar to that used by ell' in connection with the study of slag-metal manganese equilibrium. The procedure consisted of: a) melting about 50 g of Armco iron in a magnesia crucible in a platinum furnace, b) adding a mixture of about 15 g of lime-alumina slag and varying amounts of Fe2O3 and CaS, and c) maintaining the temperature at 1550°C for more than an hour in an atmosphere of argon to enable the sulfur equilibrium to be attained. Several melts were made using lime-alumina slags with basic composition 55, 50, and 45 pct lime. During the experiment the temperature was controlled manually using a Pt/10 pet Rh-Pt thermocouple. After the experiment, the Power was shut off and the flow rate of argon was increased to freeze the melt as quickly as possible. The analysis of sulfur in the metal was carried out by the oxygen combustion method3 using uniform drillings from the top and bottom of the metal button. After crushing and grinding and removal of any iron particles with the aid of a hand magnet, the slag was analyzed for sulfur by the CO2 combustion method.4 The E.D.T.A. method was employed for the analysis of lime5,6 and magnesia,= the ceric sulfate method7 for the analysis of slag iron oxide, and the perchloric acid dehydration method5 for the analysis of silica. The remaining amount was taken to be Al2O3 precipitation with ammonium hydroxide in several preliminary melts had confirmed the propriety of using this simple procedure. RESULTS The activity of iron oxide in binary, ternary, and more complex slags has been the object of numerous investigations, and the two experimental methods for its determination are: 1) Equilibrating the metal with the slag in question and measuring the oxygen content of the metal. The ferrous oxide activity is then given by aFeO L%OJSat where [%0]sat is the oxygen content of the metal in equilibrium with pure iron oxide slag. This method was used by Chipman et al.8,9 2) Equilibrating the slag in iron crucibles with known partial pressures of H2/H2O or CO/CO2 mix-tures.10-12 This method is limited to temperatures between 1265" and 1500°C. The very low oxygen content of the melts in this investigation made it impossible to derive the ferrous oxide activity by the first of these methods. Therefore, the iron oxide activities were computed by means of: Sulfide capacity data from the gas-slag work" Temkin's concept14 Flood's approach15 a FeO from Sulfide Capacity. The method of calculating the aFeO involves the sulfide capacity of the slag (c,), the sulfur distribution coefficient (Ls), the free energy of dissolution of sulfur in iron, and the free energy of formation of iron oxide in the slag. Bell and Kalyanram13 have investigated the sulfur absorption characteristics of lime-alumina slags containing magnesia by the Carter-Macfarlane method16 (based on comparing the sulfide capacity of the slag in question with that of a standard slag of unit lime activity) and have derived lime activity values. The relation between sulfide capacity and their lime activity a'CaO is given by: Cs= 3—: Xa'CaO at 1500°C

Jan 1, 1970

E. L. BLOSSOM, New. York, N. Y.-That this paper deals with a real problem is illustrated by a statement made to the speaker a few months ago by the manager of a silver-lead property: "Our ore contains 60 per cent. silica on which the smelters are penalizing us heavily, and they are not able to take all our stuff even then. We have simply got to find some method other than smelting for getting the silver and lead out of our ores. We have had experts down here and have investigated flotation, leaching and volatilization, of which processes the latter is by far the most promising. We are continuing investigation." I was somewhat concerned in certain chloride volatilization experiments which we carried on in Denver in 1903, working on a carload of ore from Butte. Now being connected with the Cottrell process, by which method the fumes will undoubtedly he recovered if they solve the volatilization problem, I have looked into the matter again, and believe it can be developed into a commercial process. On a laboratory scale, working With silver-lead ores, experimenters have obtained a volatilization of over 90 per cent. of the total values in 30 to 60 min, on quantities of 1 to 5 lb., using a roasting dish and a muffle. That looks very good, and would be entirely commercial. On attempting to duplicate these results in a reverberatory furnace, they found that it is more likely to take 8 hr. firing to yield 75 per cent. extraction, which is not commercial at all, as it requires too much time, labor, and fuel, and the whole process is too slow. Of course it can be done, because we have done it in the laboratory.

Jan 1, 1918

IT is difficult to judge how much influence the success attained during its first year, 186465, by the School of Mines at Columbia had on developments in education for the mineral industry elsewhere in the immediately subsequent years. The facts are as follows: 1. The Massachusetts Institute of Technology began giving instruction in February 1865, with a mining course included in its curriculum. 2. Early in 1865 the faculty of the Department of Science, Literature and the Arts of the University of Michigan requested permission from the Regents to establish "a course of study to be called the School of Mines . . . Also that the degree of Mining Engineering be conferred on students who should complete the course of study prescribed in the same." A resolution authorizing this was adopted by the Regents on March 28, 1865. 3. Samuel Hooper endowed a Sturgis-Hooper professorship of geology at Harvard in 1865 with the intention of making it a nucleus of a new School of Practical Mining and Geology. 4. Yale appointed Alfred P. Rockwell professor of mining in 1865. 5. Lafayette College appointed Henry S. Osborn professor of mining and metallurgy in 1865. 6. Washington College (as Washington and Lee was then known), rising out of the ashes of Civil War destruction, made a fresh start in 1865, with General Lee as its president, and offered a mining course in the first catalogue thereafter published. 7. Lehigh University, founded in 1866, had a mining curriculum from its beginning. 8. Rensselaer Polytechnic began offering a curriculum in mining and metallurgical engineering in 1867. It would be natural to suppose that these events were a reaction to the success of the school at Columbia, and possibly they

Jan 1, 1941