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By John W. Cahn, John E. Hilliard

Single crystals of copper and silicon-iron were cold rolled in orientations chosen to produce individually the major components of the poly crystalline deformation texture. The orientation dependence of the recrystallization kinetics was studied relative to the primary recrystallization textures of these specimens. It is not possible to rationalize the poly crystalline re crystallized textures on this basis. The results suggest an important role of the interaction of adjacent crystals during the deformation of aggregates. BRICK and Williamson1 first noted evidence that the recrystallization temperature was different for straight-rolled and cross-rolled copper given comparable reductions. Michalak and Hibbard2 investigated quantitatively the effect of rolling procedure on the kinetics of recrystallization of cold-rolled copper and found that material cold-rolled the same amount by straight-pass, cross-pass, and compression-pass techniques developed different deformation and recrystallization textures, different 1-hr recrystallization temperatures, and different recrystallization kinetics. However, the temperature dependence of the rate of recrystallization was essentially the same for all techniques. Similar results were obtained on iron. Dunn and Koh3 in studying the recrystallization textures of cold-rolled silicon-iron single crystals reported large differences in the annealing temperatures and times required to recrystallize specimens of different orientations cold-rolled the same amount. Liu4 and Liu and Hibbard5 utilized the concept of different recrystallization temperatures for different orientations of cold-rolled crystals to rationalize the difference in recrystallization textures found in various face-centered-cubic metals. Their explanation predicted a significant difference in the recrystallization kinetics of deformed (110) [112] crystals as compared to (358) [352] crystals, and, in fact, Liu4 reported evidence that this difference existed at least qualitatively. Verbraak6 who rolled and recrystallized a series of copper single crystals found that the double (112) [111] rolled orientation is related to recrystallized cube texture formation. The effect of rolling intensity on the relative amount of cube component suggests an important role of recrystallization kinetics. Walter and Hibbard7 while trying to relate the behavior of rolled and recrystallized single crystals of silicon-iron to the behavior of polycrystal-line silicon-iron again noted that differences in recrystallization kinetics were necessary to rationalize their results. The purpose of the present investigation was to obtain quantitative kinetic data on the recrystallization of single crystals of both copper and silicon-iron rolled to initial isolated individual orientations corresponding to those found in the polycrystalline deformation textures. These data might indicate the importance of the deformation orientation, i.e. the range of available nuclei, the deformed matrix orientation into which these nuclei grow, and the orientation dependence of their growth rate during primary recrystallization on this texture. I. COPPER Experimental Procedure—A single crystal of 99.98 pet purity copper, grown by the Bridgman technique, was purchased in the form of a bar 1 1/2

Jan 1, 1962

By Herbert W. Graham

IRON ORE is widely distributed throughout the world. Ores sufficiently high in iron content to be practical for the operations of iron and steel making occur in so many places that it is only by the accident of political subdivisions that any given nation does not have adequate and suitable iron ore. Data prepared by various authorities show that in the Lake Superior region alone there are reserves of 1,200,000,000 tons of iron ore of an iron content and at the level of production cost to which the industry has been accus tomed. At an annual consumption of 80,000,000 tons these reserves will last fifteen years. Taken alone these figures would be alarming, but over a considerable period of years the total reserve tonnage has been more or less steadily increased by improvement and extension of mining and beneficiation methods. The rate of depletion of reserves has been only about one third of the rate of consumption. On this basis the cheap high-grade ores of Lake Superior would last 45 years.

Jan 1, 1947

By Henry Lloyd Smyth

In 1891-92 1 was entrusted with the geological survey of part of the large area lying between the Marquette and Menominee iron-ranges in the Upper Peninsula of Michigan, and extending from the Republic trough on the north, through portions of the valleys of the Michigamme and Fence rivers, to and including the intermediate Felch mountain range on the south. Until a few years back the larger part of this area has been very difficult of access, and much of it is difficult still. The rock-surface is for the most part covered with swamp, forest and glacial deposits of various kinds, and therefore has not invited geological study. For these reasons the district, as a whole, with the exception of the Felch mountain range, remained almost unknown from a geological standpoint until our work in 1892. Our main object was to map the pre-Cambrian rocks, particularly the iron-bearing formations of Algonkian or Huronian age, and to obtain as much information as possible with reference to their sequence and structure, In carrying out this purpose, the use of simple magnetic instruments was found to be of the greatest assistance, and indeed indispensable. In this paper the results of our experience in tracing magnetic rocks by means of the disturbances produced in these instruments, have been brought together in systematic form, with such references to the particular area as are necessary in order to illustrate general principles, with the hope that they will prove useful to other workers in the same region, or in other regions where similar conditions may be encountered. The writer was efficiently aided in the field-work by Messrs. Samuel Sanford and Charlea N. Fairchild for nearly the whole period, and E. B. Mathews and H. F. Phillips for part of it,

Jan 1, 1897

By F. G. Miller

Earlier studies of the mechanism of flotation showed that coal flotation products are contaminated by composite coal and mineral particles. The mineral matter of these particles has the dual effect of increasing the specific gravity and decreasing the coal surface of the particle available for bubble attachment. The present study showed that these particles are more loosely held in the froth column than the high grade coal particles, especially in the coarser sizes. Consequently, it is possible in the laboratory to produce a secondary concentration of the product by sprinkling the froth product with water to wash these loosely held particles from the froth during formation and recovery. To improve coal flotation, Bethlehem Steel Corp.'s research department has been working on a number of related problems based on both physical and chemical factors. The ideal is of course full understanding of the interrelated effects of both sets of factors. However, detailed studies1 of each physical factor have produced immediately usable results in commercial coal flotation and are providing the basis for our current work on the effect of chemical factors. Since these detailed studies provided the basis for the present investigation of froth sprinkling, their key results are highlighted here. For example, for a highly floatable bituminous coal, particle floatability was shown to be directly related to the percentage of coal surface available for bubble attachment and inversely related to particle mass. The data also underscored that in a given size range the addition of mineral matter to a particle makes flotation more difficult both by adding to the mass of the particle and by decreasing the amount of coal surface available for bubble attachment. Size also affects particle floatability in that as the size of particles of a given specific gravity increases, mass increases and the ratio between coal surface area and mass of the particle decreases. Flotation tests showed that any recovery of the coarsest particles in a coal feed is accompanied by progressively higher recovery of finer and finer particles. Consequently, fine high-specific-gravity particles are recovered with the coarse good coal. As a result, when the entire 14 mesh x 0 size range is processed by froth flotation, the good coarse coal is contaminated with high-specific-gravity fines. It is the small quantities of these fines that must be rejected from the froth product if flotation efficiency is to be increased above its present level. These principles and findings, together with work by Professor V. I. Klassen,' led to the froth sprinkling investigation reported in this paper. Working with Russian coals, Klassen had shown that froth sprinkling washes loosely held refuse particles from the froth and compensates for the water lost in the upper froth layers and increases its stability. As a result, the coal particles are retained in the froth and the loss of coarse coal from the froth is prevented. Decreases in ash of 0.1% to 1.5% were reported by Klassen. Working with a 28 mesh x 0 American coal, the author of the present paper found that single-stage flotation coupled with froth sprinkling produced a product comparable to that obtained by the more expensive method of roughing and cleaning.3 The investigation reported in the present paper expanded study of the effect of froth sprinkling to include each of the standard size fractions of a bituminous coal. The main findings are as follows: (1) For those size fractions between 48 mesh and 150 mesh, froth sprinkling produces a marked reduction in both sulfur and ash. In the case of those sizes coarser than 48 mesh, while this reduction is not as significant, the additional benefit of shorter retention time is still a plus for froth sprinkling. Furthermore, when froth sprinkling is coupled with normal fast flotation, the product purity approaches that obtained by starvation reagent feeding, i.e., gradual feeding of flotation reagent to float the recoverable coal from the pulp slowly in several increments. The specific results for these two size groups are: (a) 14 x 48 Mesh. By using froth sprinkling with fast flotation, product sulfur can be reduced to a level

Jan 1, 1970

By Murl R., Schrock

THE use of diamond-drill holes at the Moctezuma Copper Co., Pilares mine, Pilares de Nacozari, Sonora, Mexico, for the ventilation of raises has resulted from experiments that were made in an effort to secure continuous and efficient ventilation in hot and gaseous raises. The method is particularly applicable in long raises and in raises run from development levels where the source of fresh air is distant. In order that the CO, concentration shall not become excessive, 30 cu. ft. per min. per man must be supplied to a heading for breathing purposes:' The quantity of air that will pass through a diamond-drill hole by

Jan 1, 1929

By Clyde E. Williams, V. N. Krivobok, C. H. Herty

THE extreme effect of the depression on the steel industry is well illustrated by the fact that the amount of iron ore shipped from the Lake Superior district was the lowest in 47 years. Something over 3 1/2 million tons of ore was shipped in 1932, compared with over 65 million tons in 1929. It is not surprising then that practically no advancement in iron ore beneficiation has been made. Improved research and development work, however, was continued at the Michigan College of Mines in the survey of the lean iron ores of Michigan with reference to the possibility of their concentration; at the University of Minnesota in its large-scale jigging studies of Lake :Superior ores; and at Battelle Memorial Institute in the development of improved jigging of iron ores. The successful operation of the new Hadsel mill at a gold property in California gave such low grinding costs on a quartz ore as to give much encouragement in the iron ore industry for a cheapening of the cost of grinding lean ores for concentration.

Jan 1, 1933

By C. D. Stahl, S. M. Farouq Ali

This investigation attempts to describe and simulate the alcohol displacement process by means of a cell model, as employed in chemical engineering practice. The proposed model is more simple than previously proposed models. and utilizes parameters chosen on a theoretical basis. The model successfully reproduced the formation of the stabilized bank and the breakthrough of alcohol, the latter depending on one of the model parameters, which may be correlated with the length of the porous medium. Moreover, the effects of the phase behavior of the liquid system involved, as observed in experimental studies, were reproduced. Several variations of the basic model were devised and tested on a digital computer. These included the cases in which: (1) the actual value of fractional flow was used in cell-to-cell computations; (2) the number of cells was varied within the same run; and (3) incomplete rather than complete phase equilibrium was assumed within each cell. The proposed cell model clarifies the basic mechanism of the process. Detailed concentration profiles obtained for each cell, for instance, showed the mechanism of bank formation in relation to the phase behavior characteristics. The results obtained indicated a varying degree of phase equilibrium concommitant with changes in the velocities of the phases in an actual alcohol displacement. This condition was approximated by changing the number of cells during the simulation. Interesting information was obtained on the influence of path length on the efficiency of alcohol displacement, which has been the subject of some controversy. Certain limitations preclude the use of the proposed model as a substitute for experimental studies. The results obtained were, nevertheless, of value in interpreting the experimental results. INTRODUCTION During recent years considerable effort has been directed toward an understanding of alcohol displacement, the process whereby oil and water are recovered from a porous medium by the continuous injection of a solvent. The complex nature of the physical process involved has so far defied a complete mathematical treatment. Other methods of approach, amounting to an overall material balance, have been proposed, yielding useful information on certain aspects of the process.1-3 Taber et al, in particular, defined the displacement mechanism in terms of the phase behavior of the alcohol-oil-brine system invoIved.2 Wachmann reported a mathematical treatment of alcohol displacement subject to certain simplifying assumptions? Donohue proposed the use of a "cell model" for simulating alcohol disPlacement.5 The nature of the assumptions involved limited the utility of the model. The present work attempts to examine the variables involved in the simulation of alcohol displacement and discusses several possible versions of the basic cell model. Under certain conditions the model results are similar to the experimental results. In particular, the spontaneous formation of of the stabilized bank and the effects of the system phase behavior were successfully reproduced. PREVIOUS WORK ON CELL MODELS Cell models and the theoretical plate concept are often used in solving chemical engineering problems in which an explicit mathematical solution may be difficult or impossible to obtain. Examples of such applications occur in distillation, gas-liquid chroma tography,6 reactor technology, absorption, etc. In petroleum engineering, such a model was used by Attra7 to describe non-equilibrium gas drive, and by Higgins and Leigh ton8 to calculate sweep efficiency in water flooding. Aris and Amundsen pointed out the equivalence between the diffusion model and perfectly mixed cells connected in series.9 Deans proposed a three-parameter cell model to simulate two-component

Jan 1, 1966

By J. F. Breedis

The morphology and crystallography of marten -site formed during quenclzing were examined by transmission electron microscopy in alloys whose compositions lie between Fe-19 wt pct Cr-11 wt pet Ni and Fe-33 wt pet Ni. Depending upon composition, four types of transformation products were observed in this portion of the Fe-Cr-Ni system. Three of these products are denoted as lath, plate, and surface martensite. The hcp structure found in association with martensite it? certain higlz-clzromium stairzless steels does not influence the transformation crystallogyaphy and cannot he Considered to act as a transitional structure in the transformation from austenite to martensite. DISTINCT changes in the characteristics of mar-tensitic transformations are produced by the partial replacement of nickel by chromium in austenitic iron alloys. Large, discrete martensite plates form in Fe-30 pct Ni, while aggregates of small crystals form in sheets parallel with (111)A austenite planes in stainless steels containing in the vicinity of 18 pct Cr and 8 pct Ni. These transformation structures are termed plate and lath martensite, respectively. In addition, an hcp structure (E) has been observed in certain high-chromium stainless steels in association with martensite. It has been suggested that the E structure acts as an intermediate step in the nucleation of martensitel-' and influences the morphology and crystallography of the final transformation product. However, this structure may be the consequence of the deformation of austenite arising from the shape distortion accompanying the transformation to bcc martensite.' An hcp stacking of atoms is produced in an fcc lattice by the introduction of an intrinsic stacking fault on alternate (111)A planes. At present, the arguments behind each explanation for the E structure are based on circumstantial evidence. This investigation seeks to determine the importance of the hcp structure to the martensitic transformation, and to examine the crystallography and morphology of the structures produced in bulk samples by quenching in alloys whose compositions lie between Fe-19 wt pct Cr-11 wt pct Ni and Fe-33 wt pct Ni. These aspects of the martensitic transformations occurring in these alloys have been studied by electron metallography and selected-area diffraction of foils examined in transmission in the electron microscope. EXPERIMENTAL METHODS The alloys have been prepared from thoroughly mixed powders of pure iron (99.6+ pct, 0.06 max pct C, 0.15 max pct N), chromium (99.9+ pct), and nickel (99.9+ pct). After sintering in an Ar-H2 atmosphere, the mixtures were melted by induction heating in recrystallized alumina boats under purified argon. The ingots were cold-rolled to 0.4-mm sheets (100 pct reduction in thickness) after the removal of at least 1.5 mm from their surfaces by grinding. Three-millimeter discs were punched from the cold-rolled sheet and annealed at 1150°C for approximately 24 hr in evacuated quartz capsules. The average grain size was 40 µ Thin foils for examination in transmission in the electron microscope were prepared from discs quenched to liquid-nitrogen temperature. A depression was first jet-machined into the center of a disc and a thin area (less than approximately 3000A in thickness) was produced at the base of the depression by electropolishing. Electron-microscope studies utilized the RCA EMU-3 and the Philips EM-100B microscopes operating at 100 kv. X-ray examination of the polycrystalline alloys was performed either in a diffractometer or in a

Jan 1, 1964

By R. G. Hudson, L. Yang

In electrochemical separation of metals, it is necessary to control the potential applied between the electrodes so that only the desired electrode reactions can occur. A knowledge of the minimum potential needed for a given electrode reaction to take place continuously is therefore pertinent to the success of the process. In molten chloride systems at high temperatures, activation polarization is believed to be small,1,2 so the minimum potential needed for the electrolytic decomposition of a molten metal chloride MC1n (n = valence of the metal ion) is therefore essentially the equilibrium electrode potential E of the metal-chlorine galvanic cell in the solution. If the decomposition products are pure M and chlorine at a pressure of p atm, E*Eo-rt/nf in [i] Since EO (the standard electrode potential of MCln) is a constant at a given temperature and R (the gas constant), and F (the Faraday's constant) are all constants, the variation of E with the electrolytic bath conditions is largely determined by the effect of the latter on the activity of the metal chloride amcln (standard state = pure MC1,). Measurement of E and study of how amCin varies with temperature and concentration, the nature of the solvent, and that of the coexisting solutes are therefore pertinent in the selection of optimum operating conditions for the electrochemical separation of metals. Because of its low melting point, high decomposition potentials of its components, and the low solubility of heavier metals in it, the LiC1-KC1 eutectic melt is a useful solvent and has been used in the electrodeposition of Mo,3Ce,4 and u5 metals. Senderoff and Brenner3 measured the potentials of Zn/Zn++, Fe/Fe++, Cu/Cu+, Mo/Mo+++, and Ag/Ag+ against an Ag/AgCl (pure) reference electrode at 600°C and a concentration of 4.1 mole pct of each chloride and came to the conclusion that complex ion formation occurred in some of the melts. Laitinen and LiUe gave an electromotive force series at 450°C for a number of {Metal/Metal ions (unit activity)) electrodes in LiC1-KC1 eutectic melt, the {pt/pt++ (unit activity)) electrode being chosen as the reference. Walker and Danly7 studied the ther-modynamic properties of NiC12 in LiC1-KC1 eutectic melt over a wide range of temperatures and concentrations by measuring the electrode potential between a nickel electrode and a chlorine electrode in the melt. Since potential measurements made by using the chlorine reference electrode are of more direct significance both in the study of electrochemical separation and in the evaluation of the thermodynamic properties of the melt, it is therefore decided to measure the electrode potentials of cells of the type {M/MCin (mole fraction = N) in LiC1-KC1 eutectic melt/Cl2 over a range of N values and temperature for a number of metal chlorides. The results should indicate the order by which the various metals plate out on the cathode and how this order is affected by temperature and the concentration of the metal chloride in the solu-

Jan 1, 1960

[59H1-Water Law and Its Significance to the Mining Industry by Wells A Hutchins 59H2-Relation of Land Subsidence to Groundwater Withdrawals in the Upper Gulf Coast Region, Texas by Leonard A Wood and A G Winslow 59F3-Hydraulic Mining of Gilsonite and Its Application to Coal Mining by J H Baker 59H4-Recovery of Phosphates by In Situ Fluid Mining by Sylvain J Pirson 59F5-Coal Cleaning Plant Design for Minimum Operating Labor by Wm M Bertholf and John D Price 59F6-Coke Combustibility A Neglected Characteristic by J D Price 59B7-Union Carbide's Uranium Operation at Maybell, Colorado by K W Lentz and F T Temple 59H8-A Rapid Method for Estimating Alumina in Feldspathic Sands by Hugh H Bein 59H9-Water Laws as Related to Dredging in Idaho by Robert A Lothrop, Richard B Porter, and Robert P Porter 58B19-Separation and Washing of Alumina Process Residue by Morton Handelman 59B11-Feed Preparation and Froth Modification for Fatty Acid Flotation by Carl C Martin and Burt C Mariacher 59B12-Design Requirements for Tailing Disposal in the Southwest by E Vern Given 59B13-Semi-Dome Shaped Buildings for Bulk Storage by Edward E Ives and William L Payne]

Jan 1, 1961

Draftsman and transitman for coal mine work in Middle West. Salary $125 per month. No. 277. Technical graduate wanted for metallurgical work in experimental laboratory of large New England manufacturing concern. A knowledge of metallography of steel is essential. Practical experience is desirable but not required. No. 305. High-class man to install and take charge of a coal mining property. Must be experienced in handling labor and of good sound judgment. Work will require a man to be on the grounds practically all the time. The work is drift mining and is not gaseous. No. 306. Engineer familiar with the acid treatment and melting of cyanide precipitates; also a competent assayer. Applicant must be able to furnish good references. No. 307. Wanted-practical mining man, foreman, or superintendent for work in middle or southern Atlantic States. Salary $200 per month. No. 308.

Jan 5, 1918

(Under this heading will be published notes sent to the Secretary of the Institute by members or other persons.) Mine and mill accountant for Mexico. Knowledge of Spanish desirable. Salary $150 to $200 gold per month with living quarters. No. 60. Master mechanic familiar with mine and cyanide plant machinery for Mexico; $200 gold per month and living quarters. No. 61. Electro-metallurgist for production of ferro-alloys, salary $200 to $400 depending on experience. No. 62. Man familiar with ferro-tungsten products of electric furnaces to draw up specifications for machine tools, to watch these tools in service and revise specifications accordingly. Salary $150 to $200 per month. No. 63. Engineers under 35 years of age for placer mining work in Belgian Congo; $1,500 to $1,700 plus traveling and living expenses, two years' contract. No. 67.

Jan 2, 1916

By Clyde E. Williams

THIS review of the progress made in iron and steel metallurgy during the past year is confined to developments in this country. It attempts to give examples to illustrate progress made rather than to appraise results. As a result of the gradually diminishing supply of rich iron ores and of predictions made as to the probable life of the iron-ore reserves of the Lake Superior District, attention of iron and steel executives was directed to the question of beneficiation of iron ores. Laboratory and plant-scale experimental work was conducted on the wash ores .of Minnesota and an investigation, was, begun on the Old Range low-grade ores.

Jan 1, 1931

By E. P. Pfleider, W. G. Pariseau

Even as the rational selection of excavation equipment requires a matching of machine performance capabilities to rock response characteristics, the functional features of transportation systems must be matched to the characteristics of the materials handled in order to secure optimum, trouble-free operation. In particular, ore passes and chutes must be designed for flow in order to insure controlled draw whenever a chute is opened. The alternative to quantitative design is, of course, the well known ad hoc procedure of freeing plugged ore passes, cleaning up spillage from flooded chutes, etc., after installation of the system. Since the voluminous empirical work sporadically undertaken through the years evidently had not led to reliable design methodology, it seemed worthwhile to attempt a rational and complete description of the movement of material through ore passes. The concepts of de- formable body mechanics applicable to gravity-induced flows of granular media or "soils" were involved. Accordingly, the mathematical theory of soil plasticity was adopted as a working hypothesis, and a two-dimensional laboratory model of an ore pass constructed in order to investigate the appropriateness of the theory. The general experimental strategy consisted of formulating the movement of material in ore passes as a boundary value problem in soil plasticity, determining the required boundary values of stress and velocity experimentally, and then using these data for the initiation of a theoretical solution for stress and velocity throughout the moving mass of material. A comparison between the theoretical and experimental constituted the test of the original hypothesis.

Jan 6, 1968

R. V. NorHis, Wilkes-Barre, Pa. (communication to the Secretary*) : The electric-haulage plant of the Short Mountain Colliery of the Lykens Valley Coal Co., mentioned by Messrs. Stoek and Harris as the earliest underground electric plant in the United States (and, I believe, the second in the world), was started July 23, 1887. The plant, designed by W. M. Schlessinger, consists of two motor-cars, each weighing about 5 tons and equipped with a 32-h.p. Union Electric Go. motor. The original general construction of the motor-cars is shown by Mr. Stoek; but they were rebuilt, the same year, with some important improvements in design; and, except for strengthening the frames and replacing the original pig-iron weights by a casting, they have not been greatly changed since that time. The generating-plant consists of two Union Electric Co. dynamos of 65-h.p. each, driven by an old 18- by 48-in. plain slide-valve engine; the ordinary voltage is 450 and the amperage varies from 40 to 200; the average indicated h.p. of the engine is about 75, with a steam-consumption of about 75 lb. per i.h.p. per hour; and as the cost of steam at this colliery is 8.11 cents per 1,000 lb.,the steam-cost per day is about $4.56.

Jan 1, 1904

THE John Fritz Medal Board of Award, at its regu¬lar annual meeting Oct. 19, awarded its gold medal to Herbert Clark Hoover. Thus ended a process of selection begun a few years ago. The award was tentatively made a year ago by the Board, which is composed of sixteen recent past-presidents of the four national societies of Civil, Mining and Metallurgical, Mechanical, and Electrical Engineers, having together a membership of nearly 60,000. The sixteen members of the Board are: American Society of Civil Engineers : C. E. Grunsky, Robert Ridgway, George S. Davison and John F. Stevens ; American Institute of Mining and Metallurgical Engineers: William Kelly, J. V. W. Reynders, Samuel A. Taylor and E. DeGolyer; American Society of Mechanical Engineers: Fred R. Low, D. S. Jacobus, Dexter S. Kimball and Charles M. Schwab; American Institute of Electrical Engineers: Farley Osgood, M. I. Pupin, C. C. Chesney and Bancroft Gherardi.

Jan 1, 1928

By A. H. Geisler, F. Keller

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947

By F. Keller, A. H. Geisler

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947

By J. Kent Smith

THE object of this investigation was to ascertain the effect of varying percentages of beryllium upon pure copper and the properties of the resultant alloys in their softest condition, the effect of heat hardening on them, and the extents to which these properties could be augmented by different combinations of heat hardening and cold rolling. The data compiled in this paper represent partial results of continuing work done by the writer during the years 1930 and 1931, which was a continuation of the unpublished ground work incepted in the laboratory of the Beryllium Corporation of America by H. B. Pulsifer in the year 1926. A short bibliography on beryllium alloys is appended to this paper. It has, of course, long been known that copper subjected to cold work is hardened and strengthened to a considerable extent, furthermore it had been qualitatively noted in previous experiments that copper-beryllium alloys seemed to take on hardness and strength as the result of cold work at a greater rate even than does plain copper. It was decided therefore to endeavor quantitatively to determine such rate of increase, as also the relative increases by combinations of cold working and heat hardening. The results are summarized in Tables 3, 4 and 5. A preliminary series of experiments had indicated that by an exposure to the heat of 575° F. for 2 1/2 hr. age-hardening of a 2.50 per cent beryllium-copper alloy took place. Slab ingots of nine different beryllium-copper alloys were prepared under identical conditions by means of the addition of a previously prepared 12.5 per cent beryllium-copper alloy to well melted and deoxidized pure copper. The ingots were then reduced by hot rolling to 12 gage (about 0.080 in.). These strips were heated to 1450° F. and quenched in cold water, and thus brought to their softest condition. (See Table 1.) Strips were next "precipitation-hardened" by reheating to a definite temperature. Similar strips to those itemized in Table 1 (which had been quenched from 1450° F.) were reheated for varying periods of time at 575° F. The hardness figures show that a metastable condition, of which the range of stability is dependent entirely upon time at the given temperature, begins to be noted in copper samples containing as little as 0.85 per cent beryllium. It is extremely noticeable in samples containing

Jan 1, 1932

By Harry M. Mikami, A. Gene Sidler

Chemistry of the evolution of materials in contact with copper converter tuyeres is delineated by means of analyses of periodic punch rod samples taken during a converter cycle. Lining samples from known peripheral and end locations from three converters were investigated chemically and petrographically. One set of eight specimens representative of all lining parts was removed for study before completion of the campaign. Purely surface removal by slag action is minor. Slag filling of interconnecting cracks extending to the hot face results in a "stoping'' action which shapes the hot face contour and is a significant factor. Major wear mechanism is believed to be copper metal slabbbing caused by metal first penetrating joins and invading fractures or impregnating brick structure laterally from the joints. Importance of lining design and joint fit are emphasized. New laboratory tests are indicated. In the copper converter, molten matte, which is essentially a solution of iron and copper sulfides, is blown with air to produce blister copper. During the first stage of the process the FeS component is oxidized to SOz and FeO, the latter combining with a siliceous flux to form a predominantly ferrous silicate slag. Successive increments of matte and flux are charged, blown, and skimmed of slag until sufficient CuzS ("white metal") has accumulated. This white metal is then blown to copper metal in the final or blister-forming stage by the oxidation of sulfur to SOz and the reduction of combined copper to metal. The reactions of both stages are exothermic so provide the required heat. Temperature is controlled by cold scrap copper, flue dusts, smelter reverts, and so forth. Considerable vari- ation in practices occur depending on the type of converter, grades of the matte and flu, and other factors. Lathe and Hodnett's' survey of world converter practices gives much information on these variations and their effects on the refractories. Principles of converting chemistry are presented by Newton and wilson,' Ruddle,' and schuhmann. Most copper converting occurs within the temperature range 2100" to 2370°F although individual smelters report1 ranges from as low as 1700" to 2240°F to a high of 2200" to 2400°F. Temperature intervals reported from beginning to end of blow varied from 45" to 540°F. Average temperature range was 2030" to 2260°F and the average interval 250°F During the matte-blowing stage varying amounts of magnetite (FeO.Fe,O,) are formed in the slag as suspended crystals and also the liquid portion of the slag will contain, in addition to ferrous silicate, some Fe20s which adds to the potential magnetite formation if the temperature falls. This is a component of the so-called "dissolved magnetite" often referred to in the literature. Although the slag may contain minor amounts of CaO, A1209, MgO, and alkalies, the principal components are Fe0-Fez03-SiO,. The phase equilibria relationships of this system have been elucidated by Muan~ and Schuhmann, et a1.' These data and estimates of converting atmospheres by schuhmann4 are useful tools in studying slag behavior. It would appear that in many cases reported magnetite contents of slags are apparently higher than actually is present at operating temperature. This is probably because much of it is formed during slag solidification. The quaternary systems which have Mg-0,1,0,' and addition to iron oxides and silica are also of interest in considering the reactions of the slags with basic refractories. The formation of magnetite has an important interrelationship throughout the pyrometallurgy of copper (Mossman,' Gronningsater and Drummond," Ruddle,' Elwood and Henderson") but its presence in the converter particularly relates to operating efficiency and lining life in certain instances. Archi-

Jan 1, 1963