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By Raymond D. Daniels, Frank E. Rizzo, James D. Gerber

ThIS discussion describes a method for the addition of small amounts of oxygen to columbium (niobium) in an accurate and reproducible manner. The method is based on the complete reduction by columbium of a carefully weighed amount of another metal oxide. The equilibrium Pq associated with Cb-CbO mixtures is extremely low, e.g., 10"25 atm at 100O°C, and the pressures over Cb-0 solutions are even lower. The equilibrium Pq associated with a given metal-metal oxide mixture can be easily obtained, with the aid of a Richardson-Jeffes chart.' Although columbium should effectively reduce almost any metal-metal oxide combination, the proper choice of a metal-metal oxide system is complicated by the low rate of oxygen transport in the gas phase at low oxygen pressures and the difficulty in reducing any columbium suboxide formed during the reduction of the oxygen source material. Thermodynamically, oxide formation on columbium will be avoided so long as the oxygen partial pressure over the columbium is below the equilibrium pressure associated with the mixture Cb-CbO. The logical choice of a source for oxygen would appear to be a mixture of Cb-CbO, since oxide formation would be precluded by nucleation difficulty. But calculations using the kinetic theory of gasses indicate that, for a temperature of 900°C, the reaction would proceed too JAMES D. GERBER, formerly Research Assistant, University of Oklahoma, Norman, Okla., is Research Metallurgist, Air Force Weapons Test Laboratory, Kirtland Air Force Base, N. Mex. FRANK E. RIZZO, Junior Member AIME, formerly Assistant Professor of Metallurgy, University of Oklahoma, is Associate Professor of Metallurgy, University of Texas at El Paso, El Paso, Tex. RAYMOND D. DANIELS, Member AIME, Professor of Metallurgical Engineering, University of Oklahoma, is an NSF Fellow, Institute de MBtallurgie Structurale, Universite de euch:tel, Neuchitel, Switzerland. Manuscript submitted October 28, 1968. IMD

Jan 1, 1970

By William E. Harris

Time and experience have demonstrated that by means of the Waelz process zinc, lead, cadmium, arsenic, antimony, bismuth and tin can be volatilized satisfactorily. In this way difficult gold ores are being treated to allow for the recovery of the precious metal. Iron ore containing zinc is being treated to remove the zinc and recover the iron. In Germany, thallium is being recovered in commercial quantities from the zinc oxide fume; indium, germanium and gallium are also concentrated to a degree warranting recovery, even though these rare metals are only recognizable in the ore by means of the spectroscope. The physical, chemical or mineralogical condition of the raw material affects very little the applicability of the process. The name Waelz is derived from the German word Waelzen, meaning a "trundling motion," which very aptly describes the movement of the charge through the slowly rotating kiln. The recovery of zinc and lead by volatilization in a rotary kiln has its origin in a process patented in 1910 by Edward Dedolph, of British Columbia. The Dedolph patent was taken over by the Metallgesell-schaft of Frankfurt-on-Main, Germany, which in cooperation with the Griesheim-Elektron, now a part of a large industrial combine, introduced certain improvements (Ohlmer, Specketer patents), but without bringing the process to a state suitable for large-scale operations. The war temporarily stopped all work on the process, and it was not until after the war that the Krupp Grusonwerk, of Magdeburg-Buckau, Germany, quite independently of the Metallgesellschaft, instituted research work in this field of metallurgy, which in 1923 led to the Waelz process proper. The Krupp Grusonwerk and the Metallgesellschaft A.G. later on collaborated, and by their joint efforts further developed and perfected the Waelz process, which they are marketing together as "Waelz-Gemeinschaft." The process is capable of treating a varied type of material; for instance, oxidized and sulphide zinc ores, calamine (zinc carbonate ore) waste dumps, jig tailings, jig slimes, table concentrate slimes, brass ashes, zinc-bearing iron ores (where the iron sinter is the real objective and the zinc oxide a by-product), electrolytic-zinc leach residues, zinc muffle residues and works sweepings, lead-furnace slags, tin ores and slags, anti-

Jan 1, 1937

By C. H. Brehaut, W. N. Taylor, R. S. Douglas, H. A. Shannon

The name for this new method of mining is derived from a composition of Horizontal, Radial, Diamond, and the drilling is from raises. This method, worked out at Copper Mountain, B.C., is believed to be distinct in many features from other known methods. Geology The ore deposits of copper Mountain are related to the copper Mountain stock, which is an ideal example of the magmatic in in that it grades from a basic gabbro at the border to an almost pure orthoclase-pegmatite core. The "contact" ore bodies lie along the contact of the gabbro and an older complex of volcanies and sediment termed the "Wolfe Creek" formation. These older rocks, collectively referred to as greenstone, had been fractured prior to the intrusion of the stock and were highly metamorphosed during the intrusion. The "outlying" ore bodies are somewhat different in character, though a similar structural pattern prevails. It is believed that a deep-seated magma of which the Copper Mountain stock is a part has given off solutions that caused a partial graniti-zation of some of the volcanies. Mining problems are caused further by the presence of a series of soft barren dikes intersecting a great many of the ore bodies, which are about 30 ft. wide, strike north-south, and dip at a high angle to the east; and are further increased by the presence of four major faults, with a great many minor faults running at acute angles from them. Fault zones average 8 ft. in width, and consist of gouge and breccia. They strike northeast and dip steeply to the northwest. The faults cut through the ore zones and the dikes, and continue on into the gabbro. The general mine structure with two types of Ore bodies, bounded by weak walls and intersected by several series of soft barren dikes and major faults, indicated that a method of mining should be devised that would remove the ore at low cost with the least disturbance of the waste walls and dikes. , Theoretical Estimate of Stoping with the Diamond Drill After consideration of various methods, the most suitable one appeared to be horizontal drilling to break the ore in a manner similar to shrinkage stoping Drilling vertical holes or rings from a bench and breaking to an open slot was eliminated because the weak walls of ore, dike or waste would not permit this type of opening. It was then decided to drill either horizontal radial holes from a raise or parallel holes from a slot cut across the ore body. After discussion, the latter method was believed unsuitable, for the following reasons:

Jan 1, 1946

By Frank Fahrenwald

I. INTRODUCTORY METALLURGICAL research has discovered many an alloy possessing properties not combined in any single metal, and progress still consists chiefly in the investigation and utilization of alloys. In the case of iron, the demands of automobiles, high-speed machines and high-duty engines have led to the production of special iron alloys which will meet any reasonable specifications in that field. In like manner, the bronzes, brasses and other alloys of copper have been brought to remarkable perfection, and for nearly every industrial purpose some alloy has been found more suitable than the pure metal. Less complete success has attended the attempt to find substitutes for gold, platinum, and the other precious metals. Indeed, it is not likely that a material can be produced which will possess all the properties of any one of them; yet it is reasonable to hope that, for any given use, the properties required may, be found in some less expensive material. Thus, in incandescent electric lamps, the wire passing through the thick glass neck of the bulb was, until recently, almost universally made of platinum, for the single reason that no other known material, suitable as a conductor, had the same coefficient of expansion as glass. But a comparatively recent investigation of the iron-nickel series' has shown that alloys of those metals may be produced, the coefficient of expansion of which can be accurately controlled between that of iron or nickel and zero. Thus, in that particular industry, a substitute for platinum has been found. According to statistical reports, not only considerable quantities of gold and iridium, but also more than one-third of the annual supply of platinum, are used (and, in the nature of the case, irrevocably lost) by dentists. Platinum is thus employed in several forms. As a thin foil, it serves various purposes for which its high melting point, pliability, chemical resistance, and other properties-including the ease with which

Jan 1, 1916

By O. Jay Myers

THE war effort has furnished the necessary impetus for better magnesium foundry practice. Four or five years ago, there were but a few formulas in general use for cores and mixtures for magnesium castings. Certain sands, binders, and inhibitors were specified and the proportions of these materials in each mixture were maintained between very narrow limits. As more and more war industries entered the field, much research was carried out and methods and practices were improved. Magnesium founding is still in a state of flux; therefore it is not uncommon to find one foundry spraying inhibitors on its cores, and another foundry using sand mixtures with incorporated protective agents. The basic core or dry-sand mold mixture for magnesium in use today is compounded with sand, core oil or resin binder, cereal, and moisture. Core oil or resin binder are added for baked strength while the cereal binder and moisture are for green strength. The normal mixtures (based on the weight of the sand) contain from 0.5 to 1.5 per cent of both cereal binder and core oil, and the moisture content varies between 1.5 and 5 per cent. The ratio of core oil to cereal binder varies from 60:40 to 40:60, while the correct amount of moisture depends upon the method of coremaking. PROTECTIVE AGENTS In all magnesium practice, protective agents are used in conjunction with the core and molding sands to prevent oxidation of the metal. The use of these inhibitors is not novel, but publications covering this field are not entirely adequate. Beck1 says Magnesium alloys decompose water to form magnesium oxide, hydrogen being liberated in the process (Mg + H20 -+ H21 + MgO). This reaction results in the blackening of the skin and the appearance of areas of porosity on the casting surface, the cavities of which are filled with a grey oxide powder (these are termed `burns'). Although sand cores for magnesium castings are thoroughly dried during the baking cycle, burning will take place on the castings unless the metal is protected properly. This type of burning is more difficult to define than the "water-magnesium" reaction cited by Beck. A possible explanation may lie in the following equation: 2Mg + 02 -s 2MgO Here, the source of the oxygen is not water, but the air in the mold cavity, together with the chemically combined oxygen in the core-binding media. Generally, two methods are used to prevent this reaction from taking place.

Jan 1, 1945

By Torgrim Eftestoel, Leif Olsen, Ove Sandberg

IN the vertical contact Soederberg electrode for aluminum furnaces more or less serious cracks are sometimes formed in the electrode, with harmful effect on furnace operation. The problem of crack formation has been studied on a laboratory scale to obtain a better understanding of this phenomenon. The primary cause of crack formation is the shrinkage of the electrode carbon, which is opposed by the normal thermal expansion of the steel contact studs. The forces thus set up are active in the temperature interval from which the electrode obtains a rigid structure (450" to 500°C) to furnace operational temperature (950°C). A visualization of our reasoning is given in Fig. 1, which shows the different behavior of mild steel and electrode carbon during baking. Research work performed to determine relationships between crack formation and shrinkage will be described. A brief description of the method developed for measurement of shrinkage will be given, as well as a critical analysis of this method. Also, raw material quality and paste composition variables will be related to shrinkage phenomena. Laboratory Test of Crack. Formation To test the tendency toward crack formations of Soederberg electrodes from different pastes, experiments were performed to simulate conditions of actual commercial electrodes, and are described as follows. A cylindrical test electrode is prepared by tamping the electrode paste to be examined in a sheet iron casing, 350 mm diam by 700 mm height. The casing is perforated, with the holes (2 mm diam) 50 mm apart, to facilitate the escape of volatile matter during baking. A cylindrical steel stud of actual service size, 100 mm diam, is welded eccentrically to the bottom steel plate, and protrudes up through the paste. During baking, a crack may thus occur in the weaker part of the test electrode. The electrode is baked by lowering the assembly slowly into an electric furnace, the temperature of which is kept constant at 900°C. After baking of the electrode, the sheet iron casing is removed and the electrode inspected for cracks. The pictures in Fig. 2 are of three different pastes baked according to the present method. Electrode 1 has a large crack; electrode 2, a somewhat smaller one; and electrode 3, only a minor crack. As will be seen from the simplified sieve analysis diagram of Fig. 2, the compositions of the pastes in question are very different. This subject will be discussed later in greater detail. Crack Formation and Shrinkage Relationships It is well known that shrinkage occurs in coke in the higher temperature ranges of coal

Jan 1, 1958

By C. E. Mills

Studies of ground movement and subsidence resulting from mining operations cover a broad field. It is also a very important consideration and one that eventually affects nearly every mining operation of any extent. The damage to surface buildings, removal of mine surface plants and replacements of main hoisting shafts must reach an astounding expenditure were these cost figures available over a period of years. Were the subject one of mathematical formula and dependent only on the angle of draw of the walls or country rocks, the problem would be relatively simple. Consideration must be given to depth and extent of workings; structural conditions of the orebodies and enclosing country rock; physical properties of these same rocks, including schistosity, bedding, jointing, slips, dikes, faults, and other structural weaknesses. The method of mining, extent of openings, supporting pillars, and amount of moisture or water underground are other pertinent factors. With such a large number of variable factors, it is apparent that the subject of subsidence is one that must be based largely on experience and results at other mines where conditions are somewhat comparable. In presenting this paper, it is the intent to describe the progressive results of past ground movements at the United Verde, to bring out physical conditions largely responsible for this movement, but to refrain from theorizing on the ultimate extent of subsidence resulting from future mining operations. Geology and Structure1 The ore deposits of the United Verde are of the massive sulfide, schist-replacement type. A structural anticline formed by the intrusion of diorite between bedding planes of steeply dipping and severely folded greenstones and porphyry localized the deposit of sulfide. The mineralized zone is of great horizontal extent varying from 200,000 to 400,-000 sq. ft., and extends from the surface to the lowest levels at a steep dip of from 50° to 75. The irregular interfingering of the sulfide with

Jan 1, 1934

By José Geraldo Vieira

Companhia Vale do Rio Doce (CVRD), founded in 1942, is located near the town of Itabira, Brazil. Its iron ore deposits include over 500 million metric tons (mt) of high-grade hematite and about 2 billion mt of itabirite (banded rock formed by thin alternate layers of hematite and silica). These deposits are part of the Iron Ore Quadrangle, of which the overall reserves have been estimated at more than 30 billion mt. The magnitude of the project meant difficult early years for the company, including large investments, extensive railroad rehabilitation, and construction of ore port and ore handling facilities. Companhia Vale do Rio Doce was organized as a stock company, and 91% of its shares are presently owned by the Brazilian government. Financing has been accomplished in part through loans from international monetary agencies foreign banks, and foreign industry, as well as Brazilian banks. The company markets mainly abroad. In 1967, it exported 10.6 long tons (It) of ore, principally to West Germany, Japan, Netherlands, Italy, France, United Kingdom, and the United States. The Rio Doce geographic region where CVRD operates is strategically located among the large population centers of Rio de Janeiro, Belo Horizonte, Salvador, and Vitoria (Fig. 1). It covers an area of approximately 81,000 sq km in the states of Minas Gerais and Espirito Santo, and its population in 1968 was about 3.5 million. This region presents excellent prospects for development, with factors favorable for forestry, agriculture, grazing, and exploration for minerals other than iron ore, Electric power (hydroelectric plants) is available, as well as two main systems of transportation: the Rio-Bahia highway and the Vitoria-Minas Railroad. Pioneer activities at Itabira started about 1720 as small gold mining centers. The town is about 80 km northwest of Belo Horizonte and

Jan 1, 1969

By A Allen, J. A. Garcia

The large increase in the wages of mine workers makes it imperative that all factors tending to limit production per miner be eliminated, if possible. The trolley and storage-battery locomotive, mining machine, hoisting engine, mining system, etc., have increased the possible output per man. But this output is still limited by the capacity of the hoisting engine and cable and by the size of the mine car. The superiority of skip hoisting in metal mining is shown by its almost universal adoption. By varying the size of skip and the rope speed, any desired tonnage can be secured and, since frequently only one kind of material is handled and breakage is unimportant, the loading of the skips can be easily and cheaply effected from bins into which the cars are dumped. The cars may then be designed to fit the conditions in the mine instead of being a compromise between hoisting and mining conditions, very likely suiting neither. In coal mines, the usual practice has been to hoist the car to the surface, either on platform or self-dumping cages. Of late years the number of skip-hoisting plants in coal mines has been rapidly increasing, but there is more or less inertia to overcome in establishing so radical a change in practice; also the earlier skip operations were not uniformly successful. As a result, it became evident that metal-mining practice would require radical modification before skip hoisting could be successfully used in coal mining. Objections to Skip Hoisting Breakage Except where coal is used for coking, or for other purposes whcre breakage is unimportant, breakage of the coal is vitally important all the way from the face to the railroad car. The average selling price is seriously reduced when the percentage of screenings is increased. Following metal-mining practice exactly, the coal would be dumped into a deep pocket, cut off into a skip load by a measuring hopper or other means, dumped into a deep, narrow skip, and dropped into a bin at the top, all of which would contribute to excessive breakage.

Jan 1, 1922

By Howard C. Pyle, John E Sherborne

Core analysis is a recent development in the field of petroleum technology. The earliest work on this subject was done in connection with evaluating and planning secondary oil recovery by water-flooding. Present-day analysis of sands of flush fields requires new and independent interpretations of the data provided by cored material. Particular attention is being paid to the development of rapid, routine methods for measuring physical characteristics of sandstone, such as permeability, porosity and grain size, as well as the sand's fluid content. Permeability may be defined as the fluid-passing capacity of a rock. For a sandstone to be permeable it must be possible to pass a measurable quantity of fluid through the material in a finite period of time. The common unit of permeability is the darcy, which may be defined as the rate of viscous flow, in milliliters per second, of a fluid of one centipoise viscosity through a porous medium having a cross section of one square centimeter, under a pressure gradient of one atmosphere (76.0 cm. Hg) per centimeter.' For convenience the subunit millidarcy, or one-thousandth darcy, is often used. Porosity is defined as the fluid-containing capacity of a rock and is usually expressed as a percentage ratio of the total pore volume to the rock or bulk volume. Since measurement of only the effective or communicating pore volume is often made, porosities are distinguished as total or effective.2,3 Net effective porosity is defined as the net pore volume available for oil and gas. Oil and water content of sand is measured and expressed either as the percentage saturation of the total pores or of the bulk rock. The oil content may also be expressed as the percentage saturation of the net effective pores. In connection with water-flooding, methods of core analysis were developed to furnish data that could be used in determining the quantity of recoverable oil14-6 and the probable rates at which various sands or divisions of a sand open to the wells would take water or produce oil. In flush fields, the analytical data are used to predict the productivity of a cored interval. They indicate the presence of oil, gas and water and may

Jan 1, 1939

By Howard C. Pyle, John E. Sherborne

Core analysis is a recent development in the field of petroleum technology. The earliest work on this subject was done in connection with evaluating and planning secondary oil recovery by water-flooding. Present-day analysis of sands of flush fields requires new and independent interpretations of the data provided by cored material. Particular attention is being paid to the development of rapid, routine methods for measuring physical characteristics of sandstone, such as permeability, porosity and grain size, as well as the sand's fluid content. Permeability may be defined as the fluid-passing capacity of a rock. For a sandstone to be permeable it must be possible to pass a measurable quantity of fluid through the material in a finite period of time. The common unit of permeability is the darcy, which may be defined as the rate of viscous flow, in milliliters per second, of a fluid of one centipoise viscosity through a porous medium having a cross section of one square centimeter, under a pressure gradient of one atmosphere (76.0 cm. Hg) per centimeter.' For convenience the subunit millidarcy, or one-thousandth darcy, is often used. Porosity is defined as the fluid-containing capacity of a rock and is usually expressed as a percentage ratio of the total pore volume to the rock or bulk volume. Since measurement of only the effective or communicating pore volume is often made, porosities are distinguished as total or effective.2,3 Net effective porosity is defined as the net pore volume available for oil and gas. Oil and water content of sand is measured and expressed either as the percentage saturation of the total pores or of the bulk rock. The oil content may also be expressed as the percentage saturation of the net effective pores. In connection with water-flooding, methods of core analysis were developed to furnish data that could be used in determining the quantity of recoverable oil14-6 and the probable rates at which various sands or divisions of a sand open to the wells would take water or produce oil. In flush fields, the analytical data are used to predict the productivity of a cored interval. They indicate the presence of oil, gas and water and may

Jan 1, 1939

By Carl F. Lutz, Robert F. Mehl

A layer of brass was formed on 0 brass using a vapor-solid reaction technique. The variation in composition with distance within the phase layer and across the a -ß interface was determined by an electron probe. The diffusivities were calculated as a function of concentration; the diffusion coefficient in brass was found to change by a factor of twenty-five over a compositional range of 8 at. pct. An explanation is proposed to account for the large change in the diffusivity, based on possible stresses in the diffusion zone; it is suggested that the concentration dependence of the thermodynamic factor might decrease the activation energy with increasing zinc content. ALTHOUGH the body of data on diffusion coefficients (D- values) in terminal solid solutions and in isomorphous systems is quite large, there is but little quantitative information for intermediate alloy phases. This paper recounts measurements of D-values for the ? phase in the Cu-Zn system. The experimental method employed consists in the forming of alloy layers and determining and analyzing the concentration-distance (c-x) curve. The experimental method employed could have been applied to several systems; the Cu-Zn system was chosen because the D-values in the a and ß phases are well known, and can thus be used for purposes of comparison. The rates of growth, of intermediate alloy layers are known for a number of systems. In nearly all cases the thickness varies parabolically with time, as to be expected if the rate of growth is controlled by the D-values. In a few cases, nonparabolic behavior has been noted.1 Nonparabolic growth may be the result of a) a variation of the composition at the phase interface with time, b) interface-controlled kinetics, c) short diffusion times coupled with long vacancy lifetimes (in vacancy diffusion),2 and d) crystal reorientation during diffusion in anisotropic systems.3 In the Al-Ni system4 and in the Al-u5 system parabolic growth kinetics are slowly approached after an initial transient period. In general those phases stable at a given temperature in a system A-B appear as separate phase layers when A and B are put in contact and given a diffusion he at-treatment. In most cases the compositions at the interface of adjacent phase layers are those read from the phase diagrams for the termini of the respective phases. This discontinuity in concentration is taken as independent of time, and the growth of one phase at the expense of another is assumed to be independent of interface kinetics, i.e., the rate of interface movement is controlled by volume diffusion in the phases concerned. wagner6 has given many solutions for multi-phase diffusion processes, assuming that the chemical diffusion coefficient, D, is independent of concentration, as have others. Jost7 has pointed out that the familiar Boltzmann-Matano solution is as valid for a (c-x) curve exhibiting concentration discontinuities at phase boundaries as for the usual single-phase case. Heumann and associates8,9 have applied this solution to the multi-phase case, but lacking concentration data within the several layers were forced to assume linear concentration gradients, thus calculating only average D-values. The purposes of the present study were: 1) to determine the dependence of D on concentration, 2) to calculate the intrinsic diffusion coefficients D?Cu and D?Zn, 3) to establish the time-law for the movement of the interface, 4) to determine the concentration limits at the ß-? interface, and, 5) to attempt to clarify the mechanism of diffusion. EXPERIMENTAL PROCEDURE The ? phase is exceedingly brittle; conventional solid couples and conventional sectioning methods were thus inapplicable. Vapor-solid couples were accordingly employed. Unfortunately the equilibrium vapor pressures of Zn for the ? phase are unknown; to escape this awkwardness, samples were enclosed in a capsule containing powder of an alloy of known composition, sufficiently large in quantity as to be effectively an infinite source, maintaining the concentration of Zn at the sample surface constant with time. The sources of Zn-vapor which can be employed in reaction with Cu, or a brass, or ß brass, to form a layer of ? brass satisfactorily wide in concentration range, are alloys of the phases ?, or ? + E or ? + d (depending on the temperature).

Jan 1, 1962

By Strathmore R. B. Cooke, Thomas E. Ban

MUCH experimental work has been performed on the mechanism of agglomeration and pelletizing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiöld and Ilmoni1 much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the microstructures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was. added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.2 Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl methacrylate monomer.3 The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45°C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.4 Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wüstite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1952

By R. F. Mehl, C. S. Barrett, A. H. Geisler

THE mechanism by which the super-saturated solid solution of 20 per cent silver in aluminum decomposes has been reported in two previous publications. 1,2 The analysis of streaks in Laue photograms showed that thin platelike particles (the so-called Guinier-Preston aggregates) form upon {111} matrix planes in the early state of decomposition.1 The size of these particles is larger, the higher the temperature at which they form in accordance with nucleation theory;3 at all temperatures they increase in size with aging.2 When they have grown thick enough to afford three-dimensional diffraction, powder X-ray photograms show that the structure is not that of the equilibrium precipitate y but that of a transition lattice ?'. Since this is also platelike in shape and also lies upon the {111} matrix planes with the {110} direction in the matrix parallel to the {11.0} direction in ?', it seems likely that the original platelet particles are merely ?' in an early stage of formation, and thus finely dispersed. The atomic spacing and pattern on the {00.0} plane in ?' are identical with those on the {111} matrix plane to which it lies parallel, and since comparable directions in the two planes are parallel, the lattices are thus coherent at the interface; an analogous coherence has been found in aluminum-copper alloys.3 The structures ?' and y are both close-packed hexagonal and are oriented alike; they differ only in interatomic distances. Consequently, ? ' is regarded as y strained from its ordinary dimensions by the lattice coherency between it and the matrix.2 The lattice movements that transform the matrix to the equilibrium precipitate appear to be very simple.2 The mechanism of precipitation in this system is simpler and is more precisely known than that in any other system,2,4 hence the system should be a profitable one for the difficult task of correlating property changes with structural alterations. The present report provides additional studies on powder X-ray diffraction from alloys of 10 per cent, 20 per cent and 30 per cent Ag, and presents the correlation of crystallographic changes with changes in microstructure, Brinell hardness and electrical resistivity of the three alloys. PREPARATION OF SAMPLES AND EXPERIMENTAL PROCEDURE The preparation of the 20.2 per cent Ag alloy has been described.2 Alloys containing 9.9 and 29.7 per cent Ag were prepared from 99.97 per cent Al and 99.99+ per cent Ag using a similar procedure. Rolled

Jan 1, 1943

By Daniel R. Hull

IN 1026 Genders' reviewed the existing theories of this subject and stated his views in support of the gas-pressure theory. Again, in 1937, the subject was thoroughly reviewed by N. B. Vaughan,3 and by Phillips and Brick,2 so that no resume is called for here. The purpose of this paper is to describe certain observations made in the course of mill work, and to point out that they mostly tend to confirm the gas theory of Genders. VAPOR SEGREGATION There is, however, one type of inverse segregation that can be accounted for by considering the volatility of one of the constituents of an alloy. The most familiar case is ordinary brass, which is subject to a zinc enrichment of a few tenths of a per cent at the surface of a chill casting. This has been noted in 70-30 brass by Genders, and a typical example of it is given in Table I, which represents a [ ] cylindrical billet 7 in. in diameter by 5; in. long. After lathe-turning 1/32 in. from the surface, the remaining distance to the center was sampled at six equally spaced intervals. The lead, which is essentially the same throughout, will be mentioned later. Consider a brass-mill mold, either round or rectangular in cross section, standing several feet high. It may require a minute or two for pouring. Before it is full, the metal in the lower end has partly solidified and contracted somewhat away from the mold. The initial shell of solidification follows not far behind the top of the column, even if the central portion is liquid for a long way down. There is, then, a space between metal and mold that is filled with zinc vapor. The vapor has no exit, because the liquid at the top of the rising column is not only in contact with the mold but keeps up a fresh supply of zinc vapor, which has, perhaps, already begun to condense in the lower portion. The cycle is short. Within a minute or two after the mold is full the bar has cooled enough to condense all the zinc. Some of it may condense on the mold; it might be expected that most of it would condense there, but the mold at that time is well coated with a velvety carbon residue from the oil dressing, overlain by fluffy zinc oxide that commenced covering the inside of the mold as soon as pouring began. The clean skin of the freshly cast brass offers a preferred surface for condensation. Reabsorption is quick and inevitable. A simple experiment indicates that a surprisingly large quantity of zinc vapor is trapped in the space between mold and

Jan 1, 1941

By F. B. Foley

IT is with an unusual degree of personal satisfaction that I find myself in a position to pay tribute to the memory of Henry Marion Howe. One could not have spent any length of time in the presence of Dr. Howe without profiting intellectually. I do not hesitate to say that my years of association with him were the most stimulating of all my years of metallurgical study. He always impressed one with his own eager search for knowledge. Never dependent on the written word alone he sought information from anyone whose opinion he valued. His ability to piece together bits of apparently conflicting data from various sources so as to build up a logical hypothesis was unique. A small slight man with the intellect of genius he would have gone to the top in any endeavor he undertook and it was fortunate for metallurgy that its study attracted him as it did. Howe was a modest man. I like to recall an incident which left a lasting impression with me. The lab- oratory in his home, "Green Peace," was in the basement and access was by way of stairs leading down from his secretary's room. In using these stairs my attention was attracted many times to an ordinary cardboard shoe box which reposed on the shelf above the landing. It was crudely labeled on its side in black ink "Vanity Box." My curiosity was aroused to the point that I finally asked his secretary what it was. With some amusement she took the box from its shelf on the stairway, opened it and showed me its contents—numerous letters, from the foremost men of science of every civilized country throughout the world, commending his "Metallography of Steel and Cast Iron." I recall that in reply to one who thought there was not enough of Howe's own researches in his book he wrote, "Primarily I am a writer, secondarily an investigator." Howe wrote to make his readers think. No one ever strove harder than he to be right but above all, whether his viewpoint proved ultimately to be right or wrong, he was always content if by his stand, he provoked a reader to take the next step along the path to greater knowledge. I doubt that he was ever afraid to be wrong for he was always secure in the thought that his effort was guided by a sincere search for the truth. One continually searching for truth is entitled to occasional excursions up the wrong alley. A glance backward to the metallurgical confusion of some thirty to forty years ago, or need one go back so far, provides convincing proof of what a host of companions one may have in a common acceptance of ideas which the future will prove to be wholly untenable. Well over a hundred years have passed since investigators have interested themselves in the effect of increasing the temperature of iron and steel on their mechanical properties. We are told by Charles Walrandl in "Industrial Annals" for June 11, 1822, that bend tests, conducted in a Russian steel works of Prince Demidoff, on steel bars "highly heated" and bent during cooling became brittle when bent at an iris blue color. He concluded, "That when steel is heated to a temperature between 473°F and 662°F the mettle was more brittle between these limits than at a much lower or at a much higher temperature." It was a curious bit of information recognized as true to this day and still not explained satisfactorily. In 1878 Charles Houston in Annales de Mines associated this brittleness with an increase in tensile strength at 572°F. When this relatively low temperature is exceeded it is recognized that steel becomes weaker as temperature is increased up to the melting point, where no strength of practical importance remains. It is easy to believe, in fact it goes without saying, that this weakening as the temperature of a metal is increased is the result of the motion of the atoms making up the metal, a motion which itself is evidence of the temperature increase. However, if we are considering iron or steel we find that this decrease in strength is not a steady one, for, besides the increase in strength just referred to, one comes to a temperature, the critical temperature, where results of tests indicate the metal to be extremely weak and then as temperature increases to become sensibly stronger again. This apparent anomaly was made the subject of the first Howe Memorial Lecture, delivered by Albert Sauveur in 1924. It may be of interest to review these findings of Sauveur. He used two methods of investigation. One involved the twisting of bars. The bars were heated in an

Jan 1, 1951

By Wm. Reuben Webster

THE greatly enlarged demand for small sizes of seamless copper tube which has recently occurred, due particularly to the rapid growth of the electric household-refrigerator industry, has emphasized the superiority of phosphorized to tough pitch copper for the purpose of producing this commodity. In the manufacture of this material exceedingly heavy reductions by cold drawing are employed, customary practice involving as much as 90 per cent. reduction of cross-sectional area in four runs without intermediate annealing. Although this superiority has long been recognized by tube makers, no quantitative expression of it has heretofore been published. It is believed that the data herewith presented will serve this purpose. Recent investigators are not in agreement as to the relative mechanical properties of copper containing small amounts of oxygen as compared with copper containing sufficient oxygen to produce that condition known as tough pitch. Hanson, Marryat and Ford' found that "oxygen has a relatively small effect on the properties of copper." Johnson,2 on the contrary, states "it cannot be denied that it (tough pitch copper) is inferior, to deoxidized copper where severe mechanical manipulation is concerned." These authorities in the reports of their investigations, as might be expected from their conclusions, do not present data of a character requisite to a conclusive determination of the question.

Jan 1, 1927

WITHOUT in any way detracting from the credit due those engineer-miners of copper who operate with power shovels, it may be said that compared with block-caving underground their work is simplicity itself. True enough, ingenuity and foresight of high order are required to lay out an open-cut operation to the best advantage; good organization and intelligent care and use of machinery are required to achieve minimum costs. But really successful undercut block-caving demands all this; and, in addition, it requires a conception and application of unseen natural forces that reflect a type of genius that is rare. Assuming that preparatory work has gained access to the orebody, mining of whatever kind consists essentially of three operations: 1. Breaking the ore "in place," as Nature left it, into pieces small enough for convenient handling. 2. Loading these pieces into some kind of a vehicle on wheels. 3. Transporting the broken ore to some central plant on the surface where the process of extracting the valuable metals can be commenced. In shovel mining, dynamite and steam or electric power are used-with remarkable efficiency, be it said-to accomplish each of these three processes. In underground-caving methods the old force of gravity is called upon to accomplish, in large part, processes 1 and 2. To do this with success is an artistic achievement of a sort. Put it another way. The earlier methods of underground mining constituted a translation of surface procedure to an underground theater. The ore was blasted and dug out in small quantities; in its place were put props, usually of timber, to prevent the caving of the rock above; and men toiled with

Jan 1, 1933

By I. R. Kramer, H. Shen, S. E. Podlaseck

The tensile and creep properties of aluminum in vacuum have been investigated. It was found that the general effect of a vacuum environment was to reduce the rate of work hardening. Results obtained from creep tests showed that lowering the test pressure from 2 x 10-4 to 10-7 torr produced a decrease in the activation energy as much as 500 cal per mole. An attempt is made to explain these effects in terms of how the surface-stress field of a specimen may be affected by a vacuum environment during plastic deformation. In a previous paper,' the results were reported of some of our early work on the effect of vacuum environment on the stress-strain curve of aluminum single crystals. This effort has been extended to the studies of the tensile and creep properties in vacuum as a function of various metallurgical parameters. Some of the recent surface-effect studies2'3 have revealed that a region of high dislocation density, the so-called "debris" layer, is formed near the surface of the specimen as a result of plastic deformation. This layer acts as a surface barrier to oppose dislocation movement. The strength of this barrier depends on the surface condition such as oxidation or surface removal. Experimental results obtained from surface-removal work2, 3 indicate that such a surface barrier, which may be characterized by a stress field, affects the applied stress and the rate of work hardening. In the case of aluminum, this stress field was found to be directly proportional to the strain and the strain rate; however, the slope of this curve is independent of orientation of the crystal and may be altered by using different surface treatment. Since the escape of dislocations may be retarded by the presence of an oxide on the surface of a specimen, it is expected that a change in the rate of oxidation in vacuum will affect the process of dislocation accumulation in the debris layer. Consequently, it also affects the plastic behavior of a metal. This paper reports the changes in some of the creep and tensile properties of aluminum in vacuum and discussions of the observed effects in terms of the concept of the "debris" layer. EXPERIMENTAL PROCEDURE Tensile Tests. A sketch of the tensile apparatus is given in Fig. 1. This apparatus was contained in a bell jar (14 in. diam by 24 in. high) connected to a 10-in. vacuum system. The load was applied to the specimen by means of a gear train which was driven by a magnetic clutch located outside the vacuum chamber. The specimen, held by a pair of square shoulder grips, was attached to the load cell at the top and the drive gear at the bottom. A displacement transducer was placed between the two grips as shown in the figure to measure the elongation. Signals of elongation and load were amplified and recorded on an X-Y recorder. The system was capable of detecting loads as small as 0.025 lb and displacements of 0.0002 in. Shoulder-grip specimens of aluminum single crystals, having a nominal square cross section of 1/8 by 1/8 in. and a 3-1/2-in, gage length, were grown by the Bridgeman techniques. The original purity was 99.997 pet. The orientations of the crystals investigated are shown in Fig. 4(a). The crystals were annealed at 600°C for 2-1/2 hr, electropolished, and placed in the vacuum test chamber without any delay. All the crystals were deformed at a strain rate of 4 x 10-5 sec-1 at 24o ± 3°C. A study was made to find whether a chemically passive surface film would give the same effect as a vacuum environment. Specimens of aluminum 1100 (0.187 in. diam with a grain size of 0.1 mm)

Jan 1, 1965

By A. W. Doepke

CLIMAX is situated in the heart of the high Rockies at Fremont Pass on the Continental Divide. This setting naturally throws some of the romantic aura of the old mining camps around the town. In its early days it was much like them, even to its air of impermanence. Its founders had faith in the future-as did every adventurer who started a hole in the ground and called it a mine. In those days, however, all available money was expended on the mine, and those who labored on the job had to he content with rugged living arrangements. The visitor at Climax today. however, sees a townsite carefully laid out to enhance the natural' beauty of the surroundings. There are 250 houses and 43 apartments which have been carefully designed by an architect, and missing is the long line of houses of the same type. Every house is of a different design, all being modern in every respect, with haths, running water, electricity, and .sewage disposal. They vary in size from three to six rooms and rent for $5 per room per month. A complete, well-designed water-treatment plant supplies water for domestic purposes.

Jan 1, 1946