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By W. L. Finlay

Size effects in quenching steel are particularly prominent and well recognized because of the existence of a critical cooling rate separating nuclea-tion and growth transformations, as exemplified by the formation of pearl-ite, from the shear type of transformation characterizing the martensite reaction. The absence of a similar, sharply demarcating cooling rate is characteristic of precipitation hardening systems and size effects in these are correspondingly less prominent. This paper is concerned with a size effect in high-purity, precipitation-hardenable alloys which appears not to have been recognized previously. This effect is believed to result from the thermal fluctuations which inevitably occur in quenching a specimen of finite size into a cooling liquid rather than from the existence of a critical cooling rate. QUENCHING "ANOMALIES" The precipitation hardening literature contains many references to so-called anomalous quenching and aging results. By "anomalous", investigators usually meant that their alloys did not consistently harden on aging after quenching according to some anticipated pnttern: not infrequently virtually no age hardening occurred with compositions known to be precipitation-hardenable. Perhaps the most prominent series of anomalies was reported over a 15-year period by Gayler and coworkers on aluminum-copper.l,2,3,4 Working with silver-rich copper alloy, Cohen5 secured some very interesting Rockwell F hardness changes of from 1-5 Rockwell points between the first peak and valley. Fink and Smith borrowed one of Cohen's specimens and, following his heat treatment and quenching practice to the letter, secured6 very different results in which only one peak was obtained and in which the hardness level at the aging lime of Cohen's first peak was 20 Rockwell F points higher. Fink and Van Horn7 encountered serious deviations in age-hardening high purity aluminum-zinc alloys. They stated that "the discrepancies were larger than might be expected from possible experimental errors in the Brinell readings." Geisler, Barrett and Mehl8 likewise encountered anomalous hardening results in aluminum-silver alloys, securing quite different age-hardening curves from two identical specimens. They stated that "the treatments of these samples had been the same, so that the different behaviors could be attributed only to accidental variations in the quenching practice."

Jan 1, 1950

By Milton E. Wadsworth, John N. Ong, W. Martin Fassell

The temperature and oxygen concentration dependence on the reaction of sphalerite in oxygen at pressures from 6 to 640 mm Hg have been investigated in the temperature range 700° to 870°C. Sphalerite has been found to oxidize linearly over this entire temperature and pressure range. At higher rates, considerable self-heating was observed. The dependence of the oxidation rate on the oxygen concentration may be expressed by: Rate = k' where k' is the specific rate constant and 0 = K1[O2]/(1 + KI[O2]), where K1 is the equilibrium rate constant for the adsorption of oxygen on sphalerite. Values of the activation energy and the enthalpy of adsorption were found to be 60.3 and —59.6 kcal per mol, respectively. Data have been presented that indicate conditions under which either a sulphatizing or an oxidizing roast may be obtained. ROASTING processes have been employed in the metallurgy of a great number of basic metals in use today. Until recently, however, little attempt has been made to deduce the fundamental mechanism by which oxidation takes place. Structural changes upon oxidation have been investigated1 = and thorough work has been performed with regard to the reaction products and the thermodynamics of the oxidation reactions. The objective of this investigation was to determine the rate of oxidation of sphalerite and to apply the absolute reaction rate theory in the theoretilcal interpretation of the experimental results." "O Description of Apparatus The apparatus contains the following features: 1—a furnace with gas system, 2—an autographic weighing system, and 3—a temperature control system. Furnace With Gas System—The furnace was mounted by a yoke on each end and was free to travel up and down on steel guide rods, permitting the introduction and removal of samples from the apparatus with minimum difficulty. The furnace was heated by three sections of Kanthal wire wound externally on a zirconia tube and insulated with Fiber-frax. Pure gases or mixtures of gases were introduced into the lower end of the furnace through two flowmeters, a mixing chamber, and a gas-tight sparger, Fig. 1. The gaseous products of the reaction and the unused gases were prevented from escaping to the atmosphere by maintaining a small negative pressure on the system. This procedure permitted air from the outside to enter through the small an-nulus around the quartz suspension fiber and prevented the escape of the internal gases. Autographic Weighing System—The autographic weighing system consisted of an adapted gold balance, a photoelectric circuit, and a weight recorder, Fig. 2. The sample was suspended from one end of the balance beam by means of a platinum chain outside the furnace and a long thin quartz fiber on the inside of the furnace. On the other end of the balance beam, the necessary weights were added to counterbalance the sample. In addition, a calibrated chain was added to the balance which was linked directly to the weight recording unit. Control was effected by means of a photoelectric circuit." A parallel beam of light from a strong source was directed onto a small front-surfaced aluminum mirror mounted in the middle of the balance beam and then to a front-surfaced mirror mounted on the ceiling of the room. The beam was then reflected onto a front-surfaced right prism at a distance of 9 ft from the balance

Jan 1, 1957

By W. M. Gray

The determination of the state of stress existing at a point in any solid body requires the determination of the six components of the stress tensor relative to a convenient set of axes. One general method of doing this in rock is to make strain or deformation measurements associated with local relief of stress in a number of boreholes penetrating a limited volume in the vicinity of the point at which the stress is to be determined. The stress is assumed to be constant throughout this volume. Leeman1 has described a number of the instruments that have been developed for making deformation or strain measurements in boreholes. Panek2 has described the application of statistical methods to the determination of the average components of ground stress from sets of measurements made in boreholes by means of deformation meters of the type developed by the U.S. Bureau of Mines. In this paper attention is given initially to the strain cell developed for use on the flattened ends of boreholes by the Council for Scientific and Industrial Research (CSIR) , South Africa. The equations required for evaluating the average components of ground stress from measurements made by means of the CSIR strain cell are derived. These equations are similar in form to those applying to measurements made by the borehole deformation meter developed by the U.S. Bureau of Mines. The results of an investigation of the properties of the equations are described. These results are important in the practical use of both the instruments mentioned above and any instrument based on similar principles.

Jan 1, 1968

By K. P. Gupta, P. A. Beck, N. S. Rajan

By determining the a phase boundaries in the following ternary systems: V-Fe-Si (at 1175oC), V-Co-Si (at 1175°C), V-Ni-Si (at 1175oC), Cr-Mn-Si (at 1000°C), Cr-Co-Si (at 1175°C), Cr-Ni-Si (at 1175°C), V-Fe-A1 (at 1175°C) and Cr-Co-A1 (at 1175°C), it was found that Si exerts a stabilizing effect on these a phases, while A1 tends to destabilize them. Si atoms in solid solution occupy sites D in the a structure, The co/ao ratio increases with increasing Si-, Mn- or Fe-content. The volume of the unit cell decreases with increasing Si-content. THE stabilization of certain metal silicides (the Nowotny phases) by the addition of relatively small

Jan 1, 1961

By Bruce E. Grant, Thomas Jancic, Lawrence G. Dykers, Frank Buchella

Principal factors influencing equipment selection can be grouped into five basic categories: tonnage requirements, ore and waste; topography and property line considerations; ore control requirements; physical characteristics of ore and waste; and climatic considerations. Loading, transporting and ground preparation equipment are largely determined by tonnage requirements. Large size equipment is appropriate for a production of about six million tpm, medium size for three million tons and small size for one million tons or less.

Jan 12, 1973

By Mark R. Lamb

The treatment of slime is of special interest to those engaged in cyaniding gold- and silver-ores. The usual practice is to make as small a percentage of slime as possible. In many instances the slime is given no treatment, but is impounded in dams in the hope that the future will develop some method of economically treating this product. The filter-press was the first step upward from ordinary decantation, but, on account of heavy labor-charge and high cost, its use has been limited to high-grade material. The slime at the Combination mill at Goldfield averages perhaps $20 per ton, and although the values are quickly dis solved the filter-press installation was not entirely satisfactory, resulting in the erection of the canvas-cell filter, developed by Chas. Butters and his staff. This filter is a great improvement over the filter-press, and the following description of it will be of interest to those engaged in treating slime produced in crushing ores, especially in view of the fact that, by the use of this filter, slime can be treated at a lesser cost and with a higher percentage of gold- or silver-extraction than in the ordinary treatment of sand; and, moreover, the initial outlay for an all-sliming plant is less than that for the ordinary sand- and slime-plant. The economy of construction of the Butters filter-plant is clearly shown in Figs. 1 and 2, which illustrate the 20-frame filter of 40 tons capacity, now being installed by the Nevada Goldfield Reduction Co. In this construction the slime-pump is so connected that it call pump to or from either tank or the filter by changing the valve-settinga—a combination which is necessary in this particular installation, since sufficient fall is not available for filling and discharging the filter by gravity. Ordinarily, a slime-plant comprises: a filter-box with frames

Jan 1, 1908

By Herbert R. Hanley

THE One Hundred and Twenty-sixth meeting-of the Institute, held in San Francisco, Sept. 25 to 29, 1922, was a success in every way. Character-istically, San Francisco presented climate suited, to the occasion, while the Committees on Arrangements left nothing undone that would contribute to the interest and entertainment of the members and their wives. There was a registration of over 230, and all sections, save three, were represented. In the technical meetings, under the leadership of Albert Burch in the mining session and C. W. Merrill in the milling session, the greatest interest was manifested in ore-hunting geology and modern ore-dressing methods. The general geologic phase developed numerous discussions and had for its aim the study and correlation of known data and the application-of these to the finding of commercial orebodies. The geologic features of the Comstock and their significance to the development of the present orebodies were discussed. This brought out matters of much technical interest as well as those of romantic nature in the history of the early life of that camp. The profitable application of modern milling methods to ores, non-commercial a short time ago, was discussed with much interest. The recent work on the Comstock ores occupied a conspicuous part in these discussions. Basic principles delineated by mathematical study of mechanical devices for the milling of ore came in for a prominent part in the program as well as the physical-chemical side of the processes devised for the winning of precious metals as a profit.

Jan 11, 1922

By Stuart S. Forbes

Changes and additions made to the Canadian Copper Refiners Ltd. electrolytic refinery between 1949 and 1955 are reviewed. The effect of high current density on current efficiency and section work is discussed. OPERATING and physical changes which have been made to the electrolytic tank house of Canadian Copper Refiners Ltd. suggest a review of present conditions. Previous papers1 a have described the general arrangement. Since then, expansion, closer anode spacing, and higher current densities have increased annual cathode capacity from 112,000 to 182,000 tons. A recent extension to the tank house, begun in the spring of 1954 and completed in August 1955, was undertaken to handle the monthly production of about 3,000 tons of anodes from Gasp6 Copper Mines. The anticipation of these additional receipts and large stocks of unrefined copper caused by the increase in custom smelting at Noranda made it necessary to increase production without immediately available additional cell capacity. Accordingly, from December 1954 through March 1955, the tank house was operated successfully at a current density of 24.0 amp per sq ft. Again, as of September 1955, one of the two tank house circuits is being operated at this high density. Although other refineries may operate at current densities higher than 24 amp per sq ft, none is doing so with anodes which contain silver and gold content as high as those being refined at Canadian Copper Refiners Ltd. General Arrangement The original building consisted of two parallel bays, each 660 ft long and 60 ft wide, with a 24 ft pump bay extending along the west side of the building. A previous expansion, completed in 1939, was to the west of the original building and consisted of two 60 ft parallel bays 240 ft long. The length of these two bays was extended in 1954 to 540 ft, adding one stripper and 12 commercial sections to No. 2 electrical circuit. Space is still available for an additional six commercial sections and one stripper section. Construction on these seven sections started in September 1955, and will be completed early in 1956. The tank house capacity will then be 206,000 tons of cathodes per year. In the two tank houses there is a total of 900 cells distributed as follows—commercial, 468; stripper, 36; total, 504 in the No. 1 tank house (No. 1 circuit): commercial, 360; stripper, 36; total, 396 in the No. 2 tank house (No. 2 circuit). Section arrangement consists of nine cells to a tier and two tiers or 18 cells to a section. Anodes, weighing 620 lb each, are cast with a Baltimore groove and are refined by the multiple system. Solution enters each cell through a bottom inlet at one end and overflows at the top of the opposite end. Rate of solution flow through the cells is controlled by valves at each section to 4.5 gpm. Electrical power to the tank house is now provided by nine 675 kw motor generator sets. Each set consists of a 135-12 v 5000 amp dc generator, driven by a 980 hp 2300 v synchronous motor. When No. 1 circuit is operated at 22,000 amp, five sets, at 4400 amp each, are connected in parallel. As the maximum allowable current on No. 2 electrical circuit has recently been set at 18,000 amp, only four sets are connected in parallel on No. 2 circuit. A tenth set, now being installed, will be reserved as a spare, for use in either circuit as required. Recent Changes In 1949, the annual capacity of the tank house was increased from 112,000 to 132,000 tons by closing the

Jan 1, 1957

As one surveys the extensive taconite operations on the Mesabi Range, he may find it difficult to believe that only 15 years ago, the iron ore mining industry here was staring at its own imminent demise. Due to the high demands for iron ore during World War II the postwar period of 1946-1950, and the subsequent "police action" in Korea, there was rapid consumption of the Mesabi's already depleted ores, and some economists were giving the Range only 20-25 years of life. In the 13-year period 1941-1953, more than 850 million tons of iron ore were shipped to steel mills, an amount almost equal to the total production during the preceding 30 years. Proven ore reserves dropped from 1.1 billion tons in 1940 to 8.3 million tons in 1954, the largest decrease being recorded in the famed direct shipping ores.

Jan 9, 1968

By G. L. Oldright

NEARLY all of the present schemes for treating complex (i. e. lead¬silver-zinc-copper) ores are based on the idea that lead holds, and will hold for some time, the strongest economic place from the viewpoint of supply and demand of all the non-ferrous metals. Copper, it is thought, will come back to its own when European affairs are stabilized, although at that time competition from Chile, Peru, and Katanga, in particular, will be more severe than in pre-war days. The future for silver and for zinc is uncertain. New uses are developing for zinc, and the market has remained better than many expected, but the stabilization of world markets will bring in foreign competition instead of relief. The cost of producing zinc from simple zinc ores, by the retort process, will, from the nature of the labor required and the increasing cost of fuel, increase steadily. As a result, the small producers of purely zinc ores around Joplin are shutting down their mines, even with a good market price for zinc; on the other hand, the producer of lead from complex ores, in the Rocky Mountain states, is confident of a profit from the sale of his lead, and is seeking means to make the zinc in his ore pay some part of the cost of treatment. However, the tonnage costs for mining and ore dressing are much higher in the Rocky Mountain states, as may be seen by comparing tax-return statements from the various states. Even before the recent drop in the price of silver, many mines were operating on a very slender margin of profit; labor and supplies cost more. Mining at greater depth has shown most orebodies to grow increasingly more complex, so that improvements in mining and ore-dressing practice have not been sufficient too compensate for the additional expense involved in beneficiating these ores. The smelters have had to meet the same general economic situation, so they can only give

Jan 3, 1924

By Charles N. Bell

The Telluride mining district of southwestern Colorado is defined by the 37" 45' and 38" parallels of latitude and 107" 45' and 108" meridians of longitude. Telluride was never a boom camp, but has had a steady growth. In recent years, notwithstanding the business depression of 1920, the business has been the same as in normal years. The first prospector is said to have appeared in 1875, in which year locations on the Smuggler vein were made. Shipments were made in 1877 and 1878, and in 1879 milling the ores was attempted. While the district produced high-grade ores, it did not become important until 1890, when the Rio Grande Southern R. R. was completed from Ridgway to Telluride. The railroad has since been extended to Durango. In the fall of 1896, 400 stamps were in operation, and the annual production was $3,000,000.00, two-thirds of which was gold. The total production from 1875 to 1923 was: gold $58,274,527; silver 41,-830,920 oz., valued at $31,016,893; copper 15,258,866 lb., valued at $2,533,291; lead 166,056,484 Ib., valued at $8,324,910; zinc 18,141,182 Ib. valued at $1,323,787; or a total production of $101,473,408. All claims are held in fee. Most of them are 1500 by 300 ft. but claims located within the last few years are 1500 by 600 ft. General supplies are obtained at Telluride, Denver, and Salt Lake. The largest mines are within 6 miles of the town of Telluride. Denver is 422 miles and Salt Lake is 439 miles, by rail, from Telluride. One-half of the distance to Denver and one-sixth of the distance from Telluride to Salt Lake is by narrow-gage railroad. The labor is efficient. The best miners are Italians and Austrians, then Slavs, Greeks, and Mexicans follow in the order mentioned. There are no labor unions. There are no serious mine pumping problems, the drainage being through adits. The Tomboy and Smuggler companies pump water from their reservoirs, the former for milling and domestic purposes and the latter for milling, power, and domestic purposes. BIBLIOGRAPHY A partial bibliography of the Telluride District is: Geologic Atlas Telluride No. 57; Preliminary Report on the Mining Industries of the

Jan 1, 1925

By H. J. Rahilly

MINE FIRES, in the Butte District, have been a source of trouble and expense for the past thirty years, for while the actual fire area in most of the mines has been comparatively small, the handling of the gas has generally been a much larger problem than the actual putting out of the fire. The chief causes of these fires have been: Defective electrical equipment, incendiarism or carelessness, and spontaneous combustion. While fires from the first two causes have been numerous, they have generally been discovered and extinguished before they became very serious. Spontaneous combustion has been the cause of most of the large fires. Sufficient heat has been generated by ground movement, high rock temperatures, and decomposition to set fire to inflammable materials (tarred ropes, canvas, dry timber, manure, and hay) left in the gobs some years ago. Also, the heat resulting from the oxidation of the fine broken sulfide ore is sometimes sufficient to set fire to the timbers. In 1906, a fire was discovered on the 1100-ft. level of the Minnie Healy mine about 400 ft. (122 m.) west of the Minnie Healy shaft, which presumably originated, in one of the upper levels, from spontaneous combustion. The fire was walled off by concrete bulkheads and a pillar of ground 100 ft. (30 m.) thick was left below and mining resumed underneath. During subsequent operations, this pillar became cracked and broken and the fire passed into the new workings. It travelled downward and spread rapidly until, in 1917, it had become necessary to wall off portions of the Tramway, Leonard, and West Colusa mines on the 1300, 1400, 1500, 1600, 1800, 1900, and 2000-ft. levels, and the top of the 2200-ft. raises were sealed. The fire area now consists roughly of a block 1000 by 1200 ft. and from the 600-ft. to the 2200-ft. level. This block is composed largely of a series of parallel northwest-southeast nearly vertical veins and stringers that form a large orebody, with no well-defined walls but badly fractured and faulted, and known locally as "Horsetail Ore." These veins, or orebodies, are mined by the square-set or the rill method.

Jan 2, 1922

By D. J. Carney, C. W. Boquist, E. C. Rudolphy

Effect of variations in sinter feed composition on sinter strength, bulk density, re-ducibility, chemical composition, and microstructure were determined by sintering experimental samples on a production sintering machine. Increasing amounts of roll scale, ore fines, return fines, and blast furnace slag were most beneficial to feed permeability, sinter bulk density, and strength. Burnt lime additions improved feed permeability but were not beneficial to sinter strength or bulk density. Sinter reducibility was adversely affected by all additives. DEVELOPMENT of methods for evaluating sinter quality, which would in some way predict the behavior of the sinter during charging and smelting in the blast furnace, has been given considerable attention in recent years. In a previous investigation at South Works of the United States Steel Corp., standard sinter sampling and testing procedures were developed.1,2 By modifying the sinter sampling device, a method of sintering experimental mix sinter samples upon a production Dwight-Lloyd sintering machine was also developed. This technique afforded a rapid and controlled method of investigating the effects of the various raw materials and additives on sinter quality and was used in this present investigation. Since the beginning of the present study in 1953, the results of numerous sinter investigations have been published, most of which were concerned with production tests of iron ore sinter, both here and abroad. Three groups of investigators reported results of experimental sinter studies that were related to this investigation. Voice et al.3 studied the effects of controlled variables on sinter quality by producing and testing experimental Northants iron ore sinter using an experimental sintering unit. Mor-rissey and Powers' determined the relationship between iron ore sinter quality and the moisture and coke content using a small laboratory sintering system. Burlingame et al.5 studied the effects of "additives" upon iron ore sinter using a laboratory sintering apparatus and laboratory grade raw materials. At South Works, it was considered desirable to study the effects of sinter mix composition and additives upon the quality of a flue dust-base sinter produced on a production sintering unit. Extrapolation of controlled laboratory test data to sintering plant operation lacking such precise control is not altogether satisfactory. Therefore, the present study was conducted in a manner which approximated production conditions as closely as possible. The raw materials used were those commonly encoun- tered in the production of flue dust and flue dust ore-type sinters and these were varied within extremes encountered in this type of sinter production. Experimental Procedure The experimental sinters were produced from 100 lb mixtures of sinter feed. The principal raw materials and additives used, their particle size, and approximate chemical composition are listed in Table I. The mixing of the raw materials was accomplished by means of a miniature single shaft pug mill shown in Fig, 1. The use of the pug mill as a mixer was decidea upon after encountering difficulty in reproducing the mixing and chopping effect of the sinter plant pug mill with other types of available small mixers. The miniature pug mill was constructed, consisting of 31/2x2x1/4 in, blades spaced 3 in. apart along a 3 ft shaft. Preliminary tests were run with this small mixer to establish the proper rotation speed and the required number of passes through the pug mill to thoroughly mix and distribute all the raw materials in a manner approximating the production Pug mill- Although the effects of varying the mosture content were determined in one particular series of tests, the amount of moisture added was changed as the composition of the experimental mix was varied. The aim in making water additions was to achieve a permeability as high as possible for each particular

Jan 1, 1956

By J. Brett, L. Seigle, L. Castleman, T. Montelbano

Impurity-induced low-temperature recrystallization of cold-worked tungsten was inuestigated with emphasis on the influence of nickel on the reaction. Palladium, nickel, aluminum, manganese, platinum, and iron greatly lower the recrystallization temperature of doped tungsten, which zs normally very high, but the recrystallization temperature of electron-be am zone-refined tungsten wzre is slightly raised by conlacl with nickel. Recrystallization can be induced at low temperature by the presence of solid nickel on the surface of doped tungsten wire, but apparently not by exposure to nickel vapors alone. Approximately 200 ppm of Ni dijjused into 10-mil wires at 1200 from a deposit of nickel on the surface produced total recrystallization, whereas more than 600 ppm of Ni could be absorbed frotn a vapor source without altering the fibrous structure of cold-worked tungsten. Once initiated, nickel-induced recrystallization required a continued source of' nickel for propagation of the recrystallization front. The solubility of nickel in fibrous 10-mil W wire was approximalely 500 ppm at 1150' C, and the activation energy for penetration of the recrystallization front was 52 kcal per mole. In many applications the usefulness of tungsten depends on critical control of its structure. Cold-worked tungsten with the fibrous structure developed by suitable thermo-mechanical treatment has a low, but technologically significant, ductility. It has long been known1 that traces of nickel, and perhaps other metals, are profoundly deleterious in doped tungsten, because they induce recrystallization at low temperature, which produces a brittle, equiaxed grain structure. This effect appears to be an exception to the general observation that recrystallization is impeded and the recrystallization temperature raised by the presence of impurities.2"9 Previous studies7-'' of the annealing and recrystallization of tungsten wire have divided the phenomenon into prior recovery stages, primary recrystallization and secondary recrystallization. The present investigation is concerned principally with primary recrystallization which is defined here as the replacement of the fibrous structure of deformed tungsten by equiaxed grains. The objective of this study was to explore the nickel-induced recrystallization reaction in tungsten and attempt to elucidate its mechanism. As well, an effort to define which other elements give rise to low-temperature-induced recrystallization was carried out. EXPERIMENTAL PROCEDURE The procedure adopted for these experiments was essentially to bring nickel and other elements into diffusive contact with cold-worked tungsten wires. The process of recrystallization was followed as a function of time and temperature by light and electron microscopic observations. First the influence of nickel on the recrystallization temperature of arc-melted, zone-refined, and variously doped tungsten wire was determined by electroplating a deposit of nickel on the surface of the wire and annealing at a variety of temperatures for 3 hr. The chemical analyses of the tungsten wires used in this investigation are given in Table I. The surface of the tungsten wire was etched with Murakami's slution' and approximately 0.005 in, of Ni was deposited from a Watts-type low pH bath14 for the conditions of these experiments. Variations in plating thickness from about 0.001 to 0.005 in. had no discernible influence on the resulting structures. The wires were then annealed in an atmosphere of dry hydrogen to establish the recrystallization temperature. Concurrently, un-plated specimens were annealed to establish the recrystallization characteristics of nickel-free wire. The criterion of recrystallization was that the fibrous structure be completely replaced by equiaxed grains after a 3-hr treatment of temperature. This provided more reproducible results than use of the first recrystallized grain or a fixed proportion of re-crystallized structure as the critical observation. The structures encountered in longitudinal and transverse sections were examined by both light and electron microscopy at magnifications up to X32,000 using parlo-dion-carbon replicas shadowed with platinum for the latter method. Second, the influence of a variety of metals on the recrystallization temperature of 0.010 in. D alumina-silica doped tungsten wire, AW136-64, was determined. The elements were applied by electroplating whenever possible. Alternatively, they were vapor-plated on the tungsten wire and a greater thickness built up by coating with a dispersion of metal powder in nitrocellulose lacquer. Elements not amenable to either of these procedures were merely slurry coated on the tungsten. The recrystallization temperature was determined as above. Third, the nickel-induced recrystallization process in doped wire was studied more closely by electroplating 8 mils of Ni on 65-mil alumina-silica doped tungsten wire, AW153-NS10, and exposing the wire to temperatures of llOO°, 1200°, or 1300°C for various times in a hydrogen atmosphere. A circular recrystallization front, 'Onsisting of equiaxed grains, developed at the periphery Of the coated tungsten wire, and the advance of this front into the fibrous interior was studied. These experiments employed relatively coarse 0.065 in. D wire because the 0.010 in. D wire recrystallized too quickly to permit observation of the pene-

Jan 1, 1969

By Leo F. Reinartz

Part II of a four-part series on the history of steelmaking in the US, points out the inadequate safety and living conditions that existed in steel mills at the turn of the Century. Also defined are furnace and process developments. OPERATIONS in steel plants today are highly mechanized. Men work in light, clean, orderly melting shops, making it difficult for old timers to convince young men that primitive, hazardous conditions existed in steel plants at the turn of the century. Working conditions then were very poor as compared to present day standards. In small plants especially, sanitary, locker, and washroom facilities, first-aid practices and stations were un- known Accidents were frequent and severe. Workers had a fatalistic attitude toward getting hurt. He who had an accident was looked upon as a hero. A dirty bandanna often served as a bandage. Infections were frequent. Electric cranes were in their infancy and broke down often Cables had not as yet replaced chains. Pig iron and scrap iron were loaded by hand in the stockyard, and stockyard locomotives were un- known; mules served as the usual motive power. It was not unusual to see recorded a delay of ½ hr in charging a furnace because of a balky mule. Furnace operations A few plants had primitive charging machines, but most furnaces were charged by placing scrap or pig iron on the paddle of a long peel, which rested on a bar across the furnace door opening. Laborers at the handle end of the peel, using the bar as a fulcrum, would heave the material into the furnace by a down and sideward motion of the peel handle. In time they became expert in placing these materials in the furnace, but it was hard, hot work, and a long time was required for charging. Cold charges of 25 tons required more than 12 hr for melting and re- fining the steel. Ports, doors, and frames were not water cooled. The charging and working area in front of the furnace was covered with steel plates. They were hot and often warped by the intense heat of the un- insulated checker chambers directly below. In the summer, working conditions on the charging floor were almost unbearable. Silica refractories were of poor quality. Because of this, and the inadequate training of furnace men in fuel control and furnace operations, roofs, front and back walls, and ends burned out rapidly. Dolomite machines were unknown; consequently, furnace banks and hearths were fettled with dolomite by the use of hand shovels. The round system required six or more men. Each man took a shovelful of dolomite and, in his turn, deposited it on the back wall and bank by a dexterous forward swing and twist of the shovel. The upward swing of the shovel partially protected his face from the searing heat of the furnace coming out through the wide-open door. Considerable skill and stamina were required to do this job properly. Reverse valves, usually of the cast-iron butterfly type, were located below the charging floor. They were operated by long levers on the charging floor level men they became warped, because of heat and abuse, great strength and skill were required to reverse them. Furnace operations were difficult. The quality and quantity of producer gas coming from irregularly stoked, hand-operated gas producers was uncertain and unreliable. Furnace Linings and ports were quickly burned out. Poor bottom and side-wall refractories, indifferent and inexperienced crews, as well as irregular re-

Jan 1, 1961

By K. T. Aust

The relative interfacial energies of symmetrical tilt boundaries in silver of greater than 99.999 pct purity were measured as a function of orientation difference 0 between 9° and 36° about <001>. The results are in good agreement with the dislocation model of the grain boundary. The energy vs H curve may be represented by the Shockley and Read equation in the form Eoe (0.55—In 8). READ&apos; has indicated that an ideal experimental method of testing the predictions of the dislocation theory of the grain boundary would be to measure the interfacial energies of symmetrical tilt boundaries between face-centered-cubic grains that have a common <001> axis, as a function of orientation difference 0. The misfit H should be defined by a rotation of each grain through an angle of H/2 away from the boundary. Such boundaries might be expected, from geometrical considerations, to be made up of a series of edge dislocations, at least for small values of 0. Energy vs H relationships for tin&apos; and lead:&apos; were previously obtained for an asymmetrical tilt boundary separating two grains in which generally only one grain was rotated about a <001> specimen axis through an angle of H away from the boundary, the other grain remaining fixed. It is possible, however, that the boundary atoms in tin and lead may have attained a symmetrical position, in relation to the orientations of the grains on either side of the boundary, during equilibrium annealing. The two sets of measurements on silicon ferrite&apos; were somewhat better suited for comparison with theory, since the boundaries were symmetrical tilt boundaries in which the axis of relative rotation was <110> in the first series and <l00> in the second; but this alloy has a body-centered-cubic structure. Although the grain boundaries in silver" were symmetrically tilted, the axis of relative rotation was not a simple crystallographic direction, and it varied from boundary to boundary. Although the above measurements were in good agreement with the Shockley and Read equation,"&apos;: it appeared desirable to carry out experiments under the ideal conditions specified by Read.&apos; Consequently, the relative energies of symmetrical tilt boundaries in silver between grains that have a common <001> axis were measured. The technique of equilibrating grain boundaries in oriented tricrystals was used rather than the less satisfactory thermal groove method previously employed for silver bicrystals." Experimental Details and Observations The solidification and seeding techniques, described previouslyh for growing tricrystals of controlled orientations, were used to prepare tricrystal specimens from silver of greater than 99.999 pct purity. The silver was obtained from American Platinum Works, Newark, N. J., in the form of poly crystalline rods 10 cm long and 7 mm in diam. These rods were then cold worked by rolling or drawing them into suitably shaped blanks. Single crystal seeds and tricrystals were grown in a high purity graphite boat by means of a movable furnace with globar heating elements. The graphite boat was enclosed in a Vycor tube, which was first evacuated to about l00/u Hg and then filled with a static argon atmosphere. The maximum temperature outside the Vycor tube was 1250°C. A typical tricrystal specimen of silver is shown in Fig. 1. Grains B and C were grown from seed crystals with a <001> specimen axis or longitudinal direction parallel to the direction of growth and with another <001> direction perpendicular to the surface. Each of the two seed crystals was rotated 18" about the <001> specimen axis but in opposite directions away from the boundary. A symmetrical tilt boundary, therefore, separated grains B and C with an orientation difference 8 of 36" about <001>. Grain A in Fig. 1 was grown from the middle seed with a <110> direction parallel to the specimen axis and with a <001> direction inclined at 45&apos; to the surface of the specimen. The interfaces sepa-

Jan 1, 1957

By N. Schapiro, R. J. Gray, G. D. Coe

A petrographic and chemical investigation was conducted to determine the occurrence and distribution of the organic and inorganic forms of sulfur in various size and specific gravity fractions of a high volatile, A-rank, Pittsburgh seam coal. The investigation was conducted to aid in the resolution of the problem of how metallurgical coke of lower sulfur content can be produced from high sulfur coals. The Pittsburgh raw coal contains about 2.4% S in two dominant forms: pyritic and organic. Pyritic sulfur constitutes about 57% of the total sulfur in the raw coal and occurs in macroscopic and microscopic-size particles. A plant cleaning process mechanically separates between 50 and 60% of the pyritic sulfur, mainly the macroscopic particles. The organic sulfur constitutes 41% of the total sulfur in the raw coal and 55% of the sulfur in the washed coal. Thus, organic sulfur is not reduced by physical methods of separation. Organic sulfur occurs in all the coal entities, but in general, increases as the exinoid content of the coal increases. In this study, it was found that carbonizing certain selected low gravity coal fractions containing an average of 0.45% pyritic sulfur and 1.01% organic sulfur produced cokes containing an average of 0.22% pyritic sulfur and 0.91% organic sulfur. However, the organic sulfur in the coke is probably derived in part from the heating of pyrite in the presence of carbon. Thus, the total sulfur in the coal carbonized is the most important factor affecting the sulfur content of the coke produced. Concentration of microscopic pyritic and organic sulfur in the middling-type coal indicates the necessity for rejecting as much of this material as is economically feasible. Most of the sulfur introduced into the blast furnace originates from the coke. Although the sulfur content of the hot metal can be controlled by the addition of flux, the flux used restricts the productivity of the furnace by displacing ore and requires first to be smelted; therefore, low sulfur coke is highly desirable. Since the sulfur content of coke is dependent upon the sulfur content of the coals from which the coke is produced, low sulfur coals are required to produce low sulfur coke. In the western Pennsylvania area, large quantities of good coking coal are available from the Pittsburgh seam, but this coal unfortunately contains relatively large quantities of sulfur. To provide information that might be useful in reducing the sulfur content of this coal in the cleaning process, an investigation was conducted to determine the physical and chemical forms in which this sulfur occurs and with what petrographic components it might be associated. The Pittsburgh seam coal, like most other coals, contains two dominant forms of sulfur: one occurs as the minerals pyrite and/or marcasite and is referred to as pyritic sulfur; the other is combined with the coal substance and is called organic sulfur. Pyritic sulfur is amenable to physical methods of separation, whereas organic sulfur is not. Pyritic sulfur particles must be freed from the surrounding coal if they are to be removed in the washing process. Generally, this requires crushing; the required degree of crushing being a function of the size and distribution of the pyrite. The present investigation was conducted to 1) determine the size, distribution and association of sulfur-bearing minerals in the coal and 2) to determine whether the organic sulfur has a preferential association with specific coal entities. If a preferential association exists, this knowledge may be useful in devising a method for organic sulfur reduction. In addition, a study was made to determine the extent to which pyritic and organic forms of sulfur in the coal contribute to the sulfur in the coke produced from this coal. A representative 3%-ton sample of raw coal was crushed to —3 in. and screened into square-mesh sizes: 3 to 1 in., 1 to % in., % to % in., % in. to 10 mesh, 10 to 35 mesh, and 35 to 200 mesh. Separate samples of the -200-mesh fraction and the all-size composite were also collected. Each size fraction (except the -200 mesh) was fractionated on heavy liquids of the following specific gravities: 1.280, 1.300, 1.325, 1.350, 1.375, 1.400, 1.425, 1.450,

Jan 1, 1963

By W. A. Klikoff, I. Fatt

The concept of fractional wet wattability is examined. Fractional water wettability of a reservoir rock is defined as the fraction of the internal surface urea that is in contact with water. Capillary pressure and relalive permeability of unconsolidated sand are shown to be functions of fractional wettability. INTRODUCTION The petroleum industry has long recognized that wettability of reservoir rock has an important effect on multiphase flow of oil, water and gas through reservoirs. As early as 1928 the American Petroleum Institute sponsored a study of wettability as part of API Project 27 at the U. of Michigan.&apos; Despite 30 years of research, there is still little exact knowledge of the wettability of reservoir rocks. There are two parts to the wettability problem. After agreeing to a uniform nomenclature in regard to wettability,&apos; the first question to be answered is, "What is the in situ wettability of a given reservoir rock?" If this can he answered the next question is, "What part does wettability play in determining the characteristics of multiphase fluid flow through the rock?" This paper represents an oblique attack on the problem of wettability. No attempt is made here to answer the basic question of wettability in situ. instead the consequences of the concept of fractional wettability are examined. Multiphase flow in sandpacks is shown to he highly influenced by fractional wettability. Jennings&apos; has given 3 definition of wettability and the other terms used in discussing wettability. These terms must be applied to the physical situation existing In reservoir rock. A survey of the pertinent literature from 1928 to 1956 indicates that the concept of a contact angle was applied to reservoir rock in the same way it would be applied to a flat, homogeneous surface. Attempts were made to state quantitatively the wettability of a reservoir rock in terms of a contact angle which was presumably constant at all points on the very rough and heterogeneous interior surface of a porous rock. Calhoun, et al,3-6 prepared synthetic consolidated and un-consolidated porous media in which they claimed there was a known uniform contact angle. They then showed the effects on the capillary pressure and relative permeability characteristics of varying this angle. The API Project 47 at the U. of Texas&apos; and others&apos; have made extensive studies of an indirect approach to the contact angle through the use of heat of wetting data. Even if successful. however, this approach also states the wettability of porous rock in terms of a contact angle which is uniform over the entirc surface. If the angle varies from one part to another on the internal surface, there is no way of determining from the measurements the area distribution of contact angles. In 1956 Brown and Fatt5 suggested that the concept of a contact angle, as applied to reservoir rock, be abandoned. This suggestion was made because it is known that the internal surface of most reservoir rocks is composed of many different minerals, cach with a different surface chemistry and a different capacity to adsorh surface active materials from reservoir fluids. Furthermore, the operation of a contact angle in determining the form of a fluid-fluid interface is difficult to picture in the very complex geometry of a pore. Brown and Fatt proposed that the wettability of reservoir rock be stated in terms of the fractional internal surface area that is in contact with water or oil. All surfaces on which there is water are called water-wet; surfaces on which there is oil are called oil-wet. The fractional water wettability is then stated as a number which represents the fraction of the internal surface that is in contact with water. A symmetrical statement can be made for the fractional oil wettability. The concept of a fractional wettability as previously stated has in its favor the recognition of the heterogeneous mineral composition of most reservoir rocks. Another point in its favor is that fractional wettability can be measured quantitatively with relative ease. Hol-brook and Bernard10 se a simple dye adsorption test to obtain fractional wettability of reservoir rocks. Amott11 uses a combination of imbibition and displacement to arrive at a wettability index of reservoir rocks which seems related to fractional wettability in the range 0.25 to 0.75 fractional water wettability. Jennings" has shown the changes in relative permeability that take place when a porous material is changed from unity to zero fractional water wettability. He also shows that reservoir rocks in their natural state, but at room temperature and atmospheric pressure, have relative permeability characteristics which would indi-

By R. W. Fountain, W. D. Forgeng, G. M. Faulring

Precipitation of the phase Co3Ti (Cu3Au type) from a Co-5 pct Ti a11oy has been investigated using single-crystal X-ray diffraction techniques. Oscillation and transmission Laue patterns of specimens aged for short-time periods at 600" C indicate the formation of titanium-rich and titanium-poor zones coherent with the {100} matrix planes. Longer aging times at 600° C establish that the equilibrium phase also forms on the {100} matrix planes as platelets. These observations are corroborated by electron metallography; electron diffraction studies show the phase Co3Ti to be ordered. A probable sequence of the precipitation reaction is discussed. A previous publication by two of the present authors reported on the phase relations and precipitation in Co-Ti alloys containing up to 30 pct Ti.1 The results of this investigation established the existence of a new face-centered cubic inter metallic phase, ranging in composition from about 17.0 to 21.7 pct Ti at temperatures below 1000° C The decomposition of the fcc supersaturated solid solution was studied employing hardness and electrical resistivity measurements. The changes in hardness upon precipitation in alloys containing 3, 6, and 9 pct* Ti were found to be associated with an initial increase in hardness followed by a plateau and then a second, more pronounced hardness increase. Investigation of this behavior by electrical resistivity measurements suggested that two different kinetic processes were involved, which, when interpreted in terms of the kinetic relation,2-4 indicated that initial precipitation was in the form of thin plates. On continued aging, the plates impinged during the growth process. The general features of these findings have been confirmed by Bibring and Manenc,5 while, in addition, they report the phase to be ordered. The present investigation was undertaken to provide more definite information on the structural relationships between the precipitate and the matrix. EXPERIMENTAL PROCEDURE Single crystals of a (20-5 pct Ti alloy were prepared from the melt employing the Bridgman technique. Poly crystalline rod, 1/2 in. in diam, prepared from vacuum-melted material, was machined to 3/8- in. diam to remove any surface contamination that may have resulted from hot-working. The crystals were grown under a purified hydrogen atmosphere in high-purity alumina crucibles heated by induction. Considerable difficulty was encountered in attempting to grow monocrystals because of the high melting point of the alloy and the high solute concentration. However, one crystal about 6 in. long was obtained which was essentially a single crystal except for one or two very small grains around the periphery. The as-grown crystal was solution heat-treated for 24 hr at 1200°Cin a purified argon atmosphere and water-quenched. One-quarter-in. slices were taken from each end of the solution heat-treated crystal for chemical analyses, and the remainder of the crystal was mounted and oriented by the back reflection Laue Method. The chemical analysis of the crystal was as follows: Pct Ti Pct 0 Pct C Pct N Pct H Pet CO 5.29 0.08 0.004 0.002 0.0003 Balance By proper tilting of the crystal, it was possible to obtain slices 1/32 in. thick of [loo] and [110] orientation. The solution heat-treated crystal slices were sealed in silica capsules for the aging treatments, with titanium sponge placed at one end of the capsule to act as a getter. All slices were water-quenched from the aging temperatures, the capsules being broken under the water to ensure a rapid quench. Thinning of the slices for transmission X-ray studies was accomplished by a combination of mechanical and electrolytic techniques, the final thickness being about 0.1 mm. Laue patterns of the solution heat-treated crystal indicated that no strain was introduced by the thinning technique. ELECTRON METALLOGRAPHY After X-ray examination, the structural changes attending the precipitation were followed by examination of direct carbon replicas of polished and etched surfaces of the single-crystal slices and extracted phases. The earliest indication of significant structural change was observed after aging at 600°C The structure of a heavily etched, solution-treated crystal is shown in Fig. l(a). Aside from the etch pit pattern, no regularity of background structure is observed. On the other hand, in the background of the specimen heated for 500 hr at 600°C, the etching pattern shows a directionality indicating the influence of minute precipitate particles, Fig. l(b). On electrolytic dissolution of this specimen in 10 pct HC1 in alcohol, a large volume of very small, flattened cubes

Jan 1, 1962

By B. R. Banerjee

MATERIAL used throughout this investigation was high-purity aluminum (99.998 pct). The 1/2-in. cubes were cut out of a cold-rolled slab and annealed at 550°C for 1 hr before deformation. The single crystal specimen was 1 in. in diam x 0.33 in. thick, cut from a cylindrical crystal produced by cooling at about 55°C per hr in a furnace which had a convenient gradient of about 10°C in every 4.5 in. vertical crucible length. Specific data on the ten specimens studied are summarized in table I. Three types of deformation were employed: (I) compression in a hand-operated hydraulic press; (2) impact with a 7-lb sledge hammer; and (3) rolling, using a wedge-shaped specimen&apos; to obtain a gradient of deformations varying from 0 to 50 pct along the length of the wedge. Specimens were either deformed at room temperature, or first cooled in a freezing mixture of dry ice and ether at a temperature of —72°C and then deformed between steel blocks cooled with dry ice. The specimens deformed at the low temperature were ground and polished through 000 emery paper and wheels impregnated with alundum and alumina No. 1. During this entire procedure the specimens were dipped frequently in the freezing mixture of dry ice and ether in order to maintain constantly a frosty surface as insurance against overheating. All specimens were given a final electrolytic polish, using two different electrolytes* to insure that the surface effects observed were not char- acteristic of the polishing technique. With both electrolytes, the annealed specimens gave even surfaces with good polish. Several standard etchants were tried without success. The best results were obtained with an immersion etchant, developed in this connection, containing: hydrofluoric acid, 4 parts; nitric acid, 1 part; glycerine, 3 parts. Discussion of Results Typical strain markings have been observed within deformation bands, as shown in figs. 1, 2, and 4. By stereographic plotting of metallographic measurements, the strain markings within a deformation band in a single crystal of aluminum deformed by compression were found to be traces of (111) planes within a maximum scatter of 6". The edges of the deformation band were found to be traces of the (100) planes also within the maximum scatter of 6" (in agreement with previous workers). At 30 pct deformation, this scatter was considered quite normal because of the fragmentation and rotation of the crystal. This solution, based on the traces on one plane of observation is not unique, but as the planes were observed to be those normally and logically to be expected, further work in this regard was not felt to be necessary. The study of strain markings in a wedge-shaped specimen, rolled to obtain a gradient of deformation from 0 to 50 pct, revealed prominent strain markings at 25 pct reduction in thickness (fig.5). Faint and weak strain markings were visually observable up to a minimum reduction in thickness of about 12 pct. Since strain markings have been observed in other face-centered cubic metals after much smaller deformations;1, 2 and since the rate of recovery in aluminum is high, it is believed that, at lower deformations, self-recovery removes the localized strains at the slip interfaces, thus removing the source of the etching effects that give rise to strain markings. At high magnifications, strain markings sometimes seem to appear as very thin, light-banded re-gions bounded by a pair of dark edges. This so-

Jan 1, 1951