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By Arthur Notman

(San Francisco Meeting, September, 1915) SACRAMENTO HILL is a mass of granite porphyry intruded along a fault between Paleozoic sediments and pre-Cambrian schists in the Bisbee district, Cochise County, Arizona. The intrusion invaded both walls of the fault to a large extent, and the accompanying extensive mineralization of the Paleozoic limestones is the locus of the great high-grade copper orebodies of the Bisbee mines. Prior to 1909, although the presence of ore in the mass of the hill itself had long been suspected, systematic exploration had not been attempted. A few shallow pits on the surface here and there had disclosed some chalcocite with associated carbonates as stringers in a mass of strongly brecciated, silicified, and iron-stained porphyry. The workings in the surrounding limestones had penetrated the porphyry in a dozen or so places for some distance from the contact but had disclosed no ore. However, the rock had been largely altered to quartz and sericite and very thoroughly impregnated with pyrite and traces of the copper sulphides. A close geological study of the conditions, both surface and underground, strengthened these suspicions, and plans for prospecting the hill were made in 1909. Reference to the accompanying illustrations, Figs. 1 and 2, will give an idea of the general appearance of the surface. The mineralization is more intense in two main zones, one at the west end and the other at the east end of the hill. The outcrop of the hill is elliptical and approximately 3,000 ft. long by 1,400 ft. wide. The Sacramento shaft, which is the main hoisting shaft of the mine and situated at the east end of the hill, as shown by the accompanying map (Fig. 3), offered a convenient base for prospecting that end of the hill, while the workings from the Holbrook shaft offered a similar opportunity at the west end. The choice of level for the first work was determined by analogy with the most favorable depth for enrichment below surface observed in the other disseminated deposits of the Southwest.

Jan 8, 1915

By Myron K. Rodgers

In rock- or ore-crushing tests all data, in order to be valuable for study and comparison, should be obtained and tabulated under conditions as uniform as possible. The results of many such tests have no value for comparison, because of incomplete data and the lack of uniform conditiops, screens and scale of sizing, etc. The purpose of this paper is to suggest a form of standard specifications which may be developed by the Milling Committee and approved by the A. I. M. E. for rock-crushing tests. It is not intended to discuss any theories of rock crushing. Reports of rock-crushing tests should include the following details: 1. Description of the machine employed (jaw or gyratory crushers, rolls, stamps,tube mills, Chilean mills, etc.), 2. Method and material (timber, concrete, etc.) of foundation. Much power is dissipated in the vibration of poor foundations. 3. Locality from which the rock or ore was obtaincd, and geological, mineralogical, and physical characters of the material. 4. The power consumption of the machine running with no load and with full load, the unit of power being 1 hp. per 24 hr, 5. The capacity of the machine in tons (of 2000 Ib.) per 24 hr. 6. The duty in tons per horsepower-day. 7. The screen analysis of feed and product by the proposed A. I. M. E. standard screen scale. On the foregoing statement, the following remarlrs are offered. Toughness of Rock Table P shows the relative crushing duty of the same machine on three different characters of rock, all other crushing conditions being the same. This table indicates that the specific resistance of the rock to crushing, may affect the crushing duty of a unit of power as much as 300 per cent. Perhaps this quality may be called toughness. It is not a function of hardness only. For comparison of tests, rocks should be divided into

Jan 1, 1916

By Olin G. Bell

At the beginning of the year 1935 the older fields in Southwest Texas, and particularly those discovered during 1934, had been practically delimited and only normal development continued. As a result, operations in this area were somewhat slowed down. Shortly after the first of the year, however, activity in the area was greatly accelerated, due largely to the fact that the Loma Novio field, discovered during the last few days of 1934, indicated the presence of a new productive trend east of and parallel to the Government Wells field and also indicated the presence of a new productive horizon, the Loma Novio sand, approximately 100 ft. lower than the Government Wells sand zone. Other discoveries during the year greatly augmented the activity in the district. During the year there were 651 oil wells, 53 gas wells and 275 dry holes drilled in this area during the year. Most of the operations were in the Government Wells, Cole, Loma Novio, Seven Sisters and Lopez fields. New Fields Four new fields were discovered during 1935 as follows: Seven Sisters and Piedra de Lumbre in Duval County; Loma Alto in McMullen County; and Lopez in Webb County. Seven Sisters Field.—The Seven Sisters field, opened in May, was the direct result of a systematic search for new productive areas northeast of the Loma Novio field. The first producer, Harvey & Henderson NO. 1 Chernosky, survey 226, was completed in the Labbe (Chernosky) sand at 2220 ft. However, the second producer, Santa Clara Oil Co. No. 1 Welder in survey 385, drilled about one mile south of the discovery well, failed to find production in the Labbé sand and was carried on down and completed in the Government Wells sand at 2473 ft. with an initial production of 20 bbl. of oil per hour. These two discoveries, in the Labbé and Government Wells sand, started an active leasing and drilling campaign in this part of Duval County and drilling operations continued especially active throughout the remainder of the year.

Jan 1, 1936

By Charles Legrand

The power plant of the Burro Mountain Copper Co. is located near Tyrone, N. M., at 5,950 ft. elevation. It is interesting because it uses the largest stationary Diesel engines in the United States. The general layout of the plant is shown in Figs. 1 and 2. The building is of steel-frame construction with hollow-tile walls and corrugated-iron roof; the floor is concrete and all windows have steel frames, making a fireproof building. The building is made to accommodate one more electric generator unit which is being installed; also two 4,000-cu. ft. air compressors direct-connected to three-cylinder engines with the same size cylinders as the electric units. The power plant consists of two 815-kva., 60-cycle, three-phase, 6,600-volt, 180-r.p.m. generators, direct-connected to five-cylinder, two-cycle Diesel engines; the necessary circulating pumps for cooling water, cooling towers and oil storage tanks. A portion of the power is used in the same building as the generating units to run one of two 200-kw. rotary converters delivering 260-volt direct current, and a 2,500-cu. ft. air compressor, delivering air at 95 lb. pressure, direct-connected to a 400-hp., 6,600-volt, three-phase synchronous motor. The remainder of the power is used to run a 1,500-ton concentrating mill 3 ½ miles from the power house, various hoists, pumps and motors about the mines and the lighting and water-works of the town of Tyrone. The direct current is used for electric traction in the mine, also to run hoists and motors that were installed before the new power plant was built. Due to the large hoists that take starting peaks of 250 kw. and the 10-ton electric locomotive that takes at times 150 kw., the load is extremely variable, as shown in. Fig. 3.

Jan 9, 1916

By G. H. Fancher

Improving economic conditions are reflected in the statistical picture of the petroleum and natural gas industry for 1933. Prices were better, demand was greater and the volume of production increased. The increase in the production of gas has been due mainly to the utilization of outlets to the new prolific gas fields of Potter and Tioga counties; of oil, to the growing demand for Pennsylvania grade lubricants. It should be emphasized that nowhere is volume of production more subject to control due to the extensive use of secondary methods of recovery and regional peculiarities than in Pennsylvania. A summary of developments in production for Pennsylvania in 1933 of necessity is brief. The data listed in Table 1 are all too few in number and not all that is desirable from the standpoint of accuracy. No state agency for the collection of data exists, no reports are compulsory. Nevertheless, because of the hearty cooperation of many individuals and public spirited corporations, it is believed that the data are as reliable as are obtainable at the present time. Furthermore, records of the past too often are lost, were never in existence or are fragmentary, to say the least. Illustrative of the condition is the fact that no thorough study of the oil and gas-producing regions has ever been made. The publications of the Pennsylvania Topographic and Geologic Survey upon the subject are noteworthy and valuable, especially the most recent one.' The Survey has been handicapped in the work by lack of time, personnel and funds in addition to the difficulties mentioned previously. It is obvious, therefore, that Table 1 cannot be completed for Pennsylvania. The data simply are not in existence. Officially there are 328 oil and gas pools or fields known by name and 58 distinct sands or horizons, one or more of which are productive of oil and gas in the various pools, but reliable data for only three general regions could be assembled.

Jan 1, 1934

By F. E. Lathe, G. A. Guess

This investigation was started with the idea of determining whether copper-nickel mattes might not have a lower flowing temperature than copper mattes, and thus perhaps aid in accounting for the difficulty so far experienced in attempts at pyritically smelting copper-nickel ores. We have used the term flowing temperature to avoid confusion with the usual melting temperature. The idea at first was that there might be a greater viscosity range in the one matte than in the other. In the early experiments it was in our minds to determine the relative fluidity of the mattes at a given temperature. Looking to this end we tried pouring equal quantities of matte at the same temperature down an inclined graphite slab, and comparing the distances traveled. Results from such experiments were not satisfactory. We next tried pouring equal quantities at the same temperature through a drilled hole in an Acheson graphite crucible, timing the flow with a stop watch, the whole operation being carried out in the muffle. The flowing temperatures of the mattes tried in this way appeared to be about the same, and there was no marked difference in their fluidity when well fused. Oxidation gave some trouble. These experiments finally led to the adoption of the following apparatus which we thought at the time was wholly original with us, but which we have since found was described by W. McA. Johnson.l The tray used was a slab of graphite 8 in. long, 2 in. wide and 1/4 in. thick. It had six holes, into each of which sat a cup of Acheson graphite. Centrally in the bottom of each cup was a vertically drilled hole 3/16 in. in diameter and 1/2 in. long. The mattes to be tested were put into the cups, in a solid piece. The cups were covered with inverted Battersea "A" cups. The tray was put into the muffle of a gas-fired furnace. Supports on each end held the tray about 2 in. from the floor of the muffle. Under

Jan 1, 1917

By Olin G. Bell

At the beginning of the year 1935 the older fields in Southwest Texas, and particularly those discovered during 1934, had been practically delimited and only normal development continued. As a result, operations in this area were somewhat slowed down. Shortly after the first of the year, however, activity in the area was greatly accelerated, due largely to the fact that the Loma Novio field, discovered during the last few days of 1934, indicated the presence of a new productive trend east of and parallel to the Government Wells field and also indicated the presence of a new productive horizon, the Loma Novio sand, approximately 100 ft. lower than the Government Wells sand zone. Other discoveries during the year greatly augmented the activity in the district. During the year there were 651 oil wells, 53 gas wells and 275 dry holes drilled in this area during the year. Most of the operations were in the Government Wells, Cole, Loma Novio, Seven Sisters and Lopez fields. New Fields Four new fields were discovered during 1935 as follows: Seven Sisters and Piedra de Lumbre in Duval County; Loma Alto in McMullen County; and Lopez in Webb County. Seven Sisters Field.—The Seven Sisters field, opened in May, was the direct result of a systematic search for new productive areas northeast of the Loma Novio field. The first producer, Harvey & Henderson NO. 1 Chernosky, survey 226, was completed in the Labbe (Chernosky) sand at 2220 ft. However, the second producer, Santa Clara Oil Co. No. 1 Welder in survey 385, drilled about one mile south of the discovery well, failed to find production in the Labbé sand and was carried on down and completed in the Government Wells sand at 2473 ft. with an initial production of 20 bbl. of oil per hour. These two discoveries, in the Labbé and Government Wells sand, started an active leasing and drilling campaign in this part of Duval County and drilling operations continued especially active throughout the remainder of the year.

Jan 1, 1936

By John Chapman, J. C. Vaughan

Although a considerable amount of practical importance attaches to systems involving gases and molten metals, little is known regarding the effects of alloy elements upon the solubility of gases in liquid iron. The solubilities of hydrogen1 and nitrogen2,3 in pure liquid iron arc known and it has been shown that small amounts of silicon and aluminum3 exert only a small effect upon the solubility of nitrogen but greatly increase its rate of solution. This paper presents the results of a study of the solubility of nitrogen, at pressures approximately one atmosphere, in molten iron containing up to 15.8 per cent silicon. EXPEBIMENTAL METHOD There are two general methods by which the solubility of a gas in a molten metal may be determined. In the first, which Sievertsl employed, the gas is measured from a burette into the enclosure containing the metal and the amount absorbed is found by subtracting from the total volume that of the dead space in the container. The second method, which was used successfully for pure liquid iron, is to expose the molten metal to the gas until absorption ceases, then to solidify and analyze the metal. In either method the stirring produced by inductive heating prevents the development of a stagnant layer at the metal surface and ensures actual attainment of equilibrium. Obviously the second method is accurate only when the saturated metal is capable of solidifying without gas evolution. Since the rate of solution of nitrogen in iron is increased by the presence of silicon, it was to be expected that the rate of evolution would be correspondingly increased and for this reason the first method was selected. A sketch of the furnace is shown in Fig. 1. A small high-frequency coil having 17 turns fitted closely around a fused silica tube, 2 in. in diameter, in which was placed, on a bed of 60-mesh alumina sand, an

Jan 1, 1940

By J. C. Vaughan, John Chapman

Although a considerable amount of practical importance attaches to systems involving gases and molten metals, little is known regarding the effects of alloy elements upon the solubility of gases in liquid iron. The solubilities of hydrogen1 and nitrogen2,3 in pure liquid iron arc known and it has been shown that small amounts of silicon and aluminum3 exert only a small effect upon the solubility of nitrogen but greatly increase its rate of solution. This paper presents the results of a study of the solubility of nitrogen, at pressures approximately one atmosphere, in molten iron containing up to 15.8 per cent silicon. EXPEBIMENTAL METHOD There are two general methods by which the solubility of a gas in a molten metal may be determined. In the first, which Sievertsl employed, the gas is measured from a burette into the enclosure containing the metal and the amount absorbed is found by subtracting from the total volume that of the dead space in the container. The second method, which was used successfully for pure liquid iron, is to expose the molten metal to the gas until absorption ceases, then to solidify and analyze the metal. In either method the stirring produced by inductive heating prevents the development of a stagnant layer at the metal surface and ensures actual attainment of equilibrium. Obviously the second method is accurate only when the saturated metal is capable of solidifying without gas evolution. Since the rate of solution of nitrogen in iron is increased by the presence of silicon, it was to be expected that the rate of evolution would be correspondingly increased and for this reason the first method was selected. A sketch of the furnace is shown in Fig. 1. A small high-frequency coil having 17 turns fitted closely around a fused silica tube, 2 in. in diameter, in which was placed, on a bed of 60-mesh alumina sand, an

Jan 1, 1940

By F. Cadena

HIWASSEE Dam, now under construction by the Tennessee Valley Authority on the Hiwassee River, a tributary of the Tennessee River, will require aggregate for approximately 800,000 cu. yd. of concrete. Near the damsite deposits of natural sand or gravel are not available and graywacke, a rock that is found in abundance, suggested itself as a likely source of manufactured aggregate. Graywacke is a metamorphosed sandstone composed principally of a mixture of quartz (65 per cent), mica (25 per cent), and feldspar (10 per cent). Other minerals are present in negligible amounts. The rock varies in different parts of the quarry from very fine to a coarse grain containing particles of about 1/4 in. maximum size, although the bulk of the deposit is medium grain. Extensive tests showed that graywacke would be suitable as a source of both coarse and fine aggregates. The aggregate plant available for use at Hiwassee Dam consisted of the coarse-aggregate and sand plant used on the Norris project. The coarse-aggregate plant had also been used at Chickamauga Dam. Although most of this plant equipment is now in use at Hiwassee, the present flowsheet is not only different from that at Norris and Chickamauga but is also unique as compared to the flowsheet of the average crushed-stone aggregate plant. It is hoped that this paper will show the importance of proper arrangement of equipment if the optimum in flexibility and capacity is to be attained. FLOWSHEET Rock is loaded by 3-yd. electric shovels into 12-yd. dump trucks, which carry the rock to the primary crusher, a 42-in. Superior McCully gyratory unit set at 4 ¾ in. (Fig. 1). The primary crusher discharges directly onto a 42-in. inclined belt conveyor, which carries the product to a surge storage pile with a maximum live storage capacity of approximately 3000 tons. A concrete tunnel under this storage pile houses the feed end of a 36-in. belt conveyor (conveyor B) fed by a 36 by 66-in.

Jan 1, 1939

By Francis Church Lincoln

I. Situation and Surroundings, The Promontorio mine is situated at the northern end of the Sierra San Francisco de Coneto, in the town of Promontorio, Partido of El Oro, State of Durango, Mexico. As shown in the sketch-map, Fig. 1, the nearest railroad station is Chin-acates on the Mexican International Railroad, 82 miles north of the city of Durango. The mine is 16 miles north of the sta-tion by air-line. It is reached by means of a good wagon-road which first crosses the Guatimapé Plain, passing the ranches of San Antonio and San Julian, to Estacion—a distance of about 15.5 miles—and then entering the mountains crosses the Sierra to Promontorio—a further distance of 11.5 miles— making in all a distance of 27 miles by road from railroad to mine. Promontorio is just beyond the summit of the range, at an elevation of about 8,000 ft. above sea-level, or 1,350 ft. above the Chinacates station. The Castillo de San Francisco, the highest peak in the Sierra, has an altitude of 10,000 ft., and the Promontorio road crosses the summit of the ridge at an elevation of 9,000 ft. by a pass just below this peak known as the Puerto del Almagre. The Promontorio mill is situated at Santa Inés, 2 miles by tram or 3 miles by wagon-road to the north of Promontorio and about 600 ft. lower. The Sierra San Francisco de Coneto decreases in height towards the north and west till it comes to an end at the Mel-chor Arroyo on the ranches of Melchor and Ramos. Beyond this arroyo another range, the Sierra de la Candela, begins. In the vicinity of the Promontorio mine the hills are very rugged and the surface is furrowed by ravines which contain running streams during the rainy season-—July, August and

Jan 1, 1908

By R. G. Baughman

With the constantly increasing sales competition, coal to be sold today must meet the test of quality in every respect. The producers must be able to make all marketable sizes that will meet such general requirements as follows: 1. Ash content must be consistently low, depending upon the use to be made of the coal. 2. Sulfur content must be controlled accurately according to requirements. 3. All sizes must be positively free from visible impurities. 4. Free moisture of washed sizes must be reduced to a minimum. 5. The freezing of wet coal in cars must be prevented. 6. The percentage of fines in small mixed sizes must be controlled to give the uniform and proper combustion when used on various types of automatic stokers. 7. The undersize particles or degradation caused by handling must be kept to an absolute minimum in all sizes loaded. Many difficulties may be met in bringing any particular coal to meet these quality requirements, because the extent to which the quality of a coal may be controlled is determined largely by its physical characteristics. Preparation of an Impure Coal Bed The application of modern and scientific methods in the controlled preparation of bituminous coal from a bed in the mid-western field will illustrate the results that can be accomplished by adequate preparation: The bed referred to contains coal inherently excellent as to low ash and other desirable characteristics; in fact, the coal itself is one of the best in the field. It is, however, divided into four layers by dirt bands of soft shale 1 to 2 in. thick. It also contains much sulfur in the form of sulfur lenses and laminated sheets. Horsebacks or rolls varying from 6 in. to 12 ft. in width are encountered in the mining of the bed and heretofore have rendered it practically unworkable. The mines operating in this

Jan 1, 1931

By Kenneth L. Adams

10.3-1. Introduction. Equipment replacement or maintenance is of major concern to every company today. It can be the difference between an efficient and profitable operation or an inefficient and struggling one. Mining equipment, as everyone knows, will not last forever. Some equipment becomes obsolete before it wears out while some may be doing its intended job, yet not economically. It is a major problem for management to make the decision as to whether a piece of equipment should be repaired or replaced. There are numerous approaches to this problem; using formulas, charts, and graphs. These would be very good if all conditions were stable. Since conditions and requirements are constantly changing, an accurate observation cannot be derived from a set formula. A formula does, however, serve as a reminder to include most of the items that should be considered when evaluating old and new equipment. In the field of mining there are several questions which enter into the reasoning that are difficult to put into an equation. Some of these are: 1. Will the present equipment produce the required output of the mine, or an increase if necessary? 2. Are reserves adequate to support the purchase of new equipment? 3. Can the old equipment be repaired to efficiently continue the mining operation? 4. What is the stability of future markets for the product? Depreciation rate, or the write-off life, is a factor that can directly effect decisions on replacement. If the initial life expectancy is too long and the price of equipment is not written off when discarded, then the original investment has not been recovered. If the write-off time is too short, then the equipment is written off before replacement is even considered. In this case, the depreciation accrual is usually used to finance some other phase of the operation. In view of the increasing prices, the amount of depreciation fund is generally too small for much incentive to replace an older unit

Jan 1, 1968

By C. A. Heberlein

C. A. HEBERLEIN,* New York, N. Y.-The results stated by Rey and Brevers are so startling that they are of great interest, as the concentration of a low percentage of cinnabar by differential flotation yields a high-grade concentrate in the presence of either arsenical or iron pyrite. The authors say: "Cyanide can thus be used to depress arsenopyrite and make a good cinnabar-arsenopyrite separation. A cinnabarpyrite separation could probably be effected in the same way." Corrosive sublimate at the present price of mercury would be a very expensive reagent but the expense would be justifiable if a high rate of concentration could be obtained with a high extraction. On my request, special tests were made in the Punitaqui mill in Chile along the line suggested by the authors, without any improvement of either grade or extraction. As the recovery of the cinnabar in a complex sulphide of chalcopyrite and pyrite gave unsatisfactory results, I had tests made at the testing laboratory of the American Cyanamid Co. at Stamford, Conn. As these tests turned out to be highly satisfactory, not only at Stamford but later at the mine, they are presented here. [AMERICAN CYANAMID TEST FEED PER CENT Si02 66.54 A12032.08 CaO0.70 MgO 0.00 Alkalis1.78 Fe15.63 Cu0.44 S9.42 Hg0.45 OZ. PER TON Ag0.95 Au0.151 Screen Analysis of Tailings, Per Cent Plus650.0 Plus 1001.32 Plus 15020.75 Plus 20019.85 Minus 20058.08] The pulp had a density of 22 and a pH of 7.8. Total time of conditioning was one minute. The reagent added was Texas fuel oil, 0.116lb. Of 33.7 Bé. gravity containing 0.9 per cent sulphur. Frother, 0.062 lb. of No. 5 pine oil. Rate of concentration of mercury was 25.7: 1 [ ]

Jan 1, 1941

By Linda Lee, R. E. Reed-Hill, C. R. Smeal

Four fcc metal surfaces, etched to make them responsive to polarized light, have been studied with an electron microscope. Jones'prediction that these surfaces are grooved has been verified. Optical-goniometer measurements made on commercially pure nickel indicate that the groove walls are poorly defined (100) facets. Surface mientations close to either 4001 or {ill).- show no extinctions on the polam'zid-light microscope. An explanation is offered for this orientation dependence. It has also been deduced that polarized-light extinctions on a grooved cubic-metal surface should not be used directly in crystallographic-orientation determinations. The nature of the etching solutions that produce these surfaces is considered. A cubic-metal surface may be made responsive to polarized light in two basic ways."' In one, an anodic film, believed anisotropic, is formed on the surface. A plane-polarized-light beam, at normal incidence, should be reflected from this type of film with an ellipticity that varies with grain orientation. Under crossed polarizers of a polarized-light microscope, each grain may be distinguished from its neighbors by a difference in reflected-light intensity. An alternate treatment,' more generally applicable to cubic metals and of principal concern here, involves etching of grain surfaces. The characteristic features of this surface were first deduced by Jones3 from light-microscope observations. She concluded that, in general, grain surfaces were furrowed so that light was reflected from two parallel sets of etched facets. A grooved surface produces elliptical polarization of a plane-polarized beam because the beam does not strike groove walls at normal incidence. Jones also observed that the furrows must have faces inclined to each other by approximately 90 deg, since the light returns along the incident path, and that a grooved surface should show four maxima and minima of reflected-light intensity during a 360-deg stage rotation of the polarizing microscope. Positions of maximum extinction were predicted to occur when groove axes were parallel to either polarizer or analyzer vibration directions. Because of the limited resolving power of Jones' optical microscope, her deductions were primarily indirect. Proof of the correctness of her conclu-sions, as demonstrated by the electron microscope, will be given as well as evidence concerning the crystallographic nature of the etch furrows and the types of etching solutions that produce them. EXPERIMENTAL PROCEDURE During a comprehensive study of hot plastic deformation in nickel and nickel alloys, an etch was evolved that produced a surface with an excellent polarized-light response on Nickel 200 ("A" Nickel). The etching solution and associated metal-lographic procedures are given in Table I. In evaluating this etch, a study was made of the topological features of the etched surface and their relation to the underlying crystalline structure. As part of this investigation, large crystals (2 mm average diameter) were grown in a 1-cm-sq Nickel 200 specimen. After the surface was etched, the crystallographic orientations of ten grains were determined by the standard back-reflection Laue technique of Gren-inger.4 Maximum extinction positions during a microscope stage rotation were also measured for the ten grains. Groove-wall positions on the surfaces of the ten grains were measured with a two-circle optical goniometer. The technique was essentially that of Barrett and Levenson.5 Several grain surfaces were photographed with a Philips Model 100A electron microscope. All specimens were replicated with collodion, or collodion backed with formvar and chromium shadowed at 18 to 20 deg. The basic material was Nickel 200. However, an electron-micrographic study was also made of surfaces developed by polarized-light etches on other fcc metals (90-10 a brass, Monel 400, and lead). All etching procedures are given in Tables I and 11. EXPERIMENTAL RESULTS Fig. 1 shows typical electron micrographs of three different fcc metal specimens and an optical micrograph of a fourth. All photographs show a grooved structure corresponding closely to Jones'3 predictions. Also, as noted by Jones, extinctions were always observed when groove axes were either parallel or perpendicular to the microscopes' vertical cross hair. The symmetry of the grooves, with respect to the twin boundaries in Fig. 1, implies that furrows have a crystallographic basis. The coarse-grained Nickel 200 specimen was used to study this basis. Facet Orientation. The poles of the ten Nickel 200

Jan 1, 1964

By Craig R. Barrett

The influence of the stress dependence of the dislocation density on the overall stress dependence of The steady-state creep rate is discussed. Experimental measurements of dislocation densities and creep rates jor an Fe-3.1 pct Si alloy tested over a wide range of stress are presented which indicate a close correlation between the two quantities. EXPRESSING the stress dependence of high-temperature steady-state creep rates has been the subject of numerous investigations over the past decade. From these investigations have emerged a few general equations which fit most of the available data reasonably well. Garofalo 1 has proposed that for a wide range of stress and temperature the creep rate, i, can be expressed by a relationship of the form: where A, ß, and n are temperature-dependent and is the applied stress. Eq. [I] gives a stress dependence of a at low stresses and exp(nßo) at high stresses, both consistent with experimental observation where n = 5. A number of other investigatorshave proposed a similar expression where: where m and w are in general functions of temperature. Theoretical justification for Eqs. 111 and [2J comes from two different approaches, theories based on dislocation glide3-5 and theories based on the balance between work-hardening and recovery.' Dislocation glide theories predict where p is the mobile dislocation density and V is the activation volume. In order for Eq. [3] to predict a on stress dependence at low stresses with n = 5, it is necessary for p to be a strong function of stress, about proportional to u3 or u4.436 Recovery models of creep start with the general expression:' where r is the recovery rate and h is the work-hardening rate, and then employ a detailed model to determine the stress dependencies of r and h. As example, weertman2 has described a model based on pile-up hardening which results in an expression similar to Eq. [2] with m = 2 and p = 2.5. A recent, seemingly more general approach suggested by McLean is to use Friedels dislocation network growth expression to calculate the stress dependence of r. This model predicts r = p 3,2 and, as h is taken to be a relatively weak function of stress, the stress dependence of i should be about proportional to p3, 2. Once again, it is required that p be a strong function of stress to yield i This recovery model is by no means complete as the stress dependence of network growth is calculated in the absence of an applied stress meaning that r should probably be a stronger function of stress than given by p3, 2 and also some recent work by Mitra and McLean8 suggests that the stress dependence of h may be as large as Because of the importance of the stress dependence of p in determining the overall stress dependence of the strain rate it seems reasonable to examine this relationship in some detail. Measurements made on dislocation densities present during high-temperature steady-state creep generally obey the following relationship a =o0 + aGVWp [5] where uo is usually called a friction stress, a is a numerical constant about equal to unity, G is the shear modulus, and b is the Burgers vector. Depending on the magnitude of uo, data obeying Eq. [5] can give rise to a range of stress dependencies of p. For example, if we assume that the expression where 6 is some constant, adequately represents the stress dependence of p over a range of o, then from Although Eq. [6] obviously breaks down when u 5uo for uo 6 can vary over a wide range of values. In particular, if u > a, > 0 then 6 will be greater than 2. As an example the data of Ishida and McLean are plotted in Fig. 1 showing excellent agreement with dynes per sq cm) and also showing good agreement with a p cc u3 dependence when plotted on a log-log basis. As oo increases 6 tends to increase and correspondingly the stress dependence of the predicted creep rate should also increase,* as-

Jan 1, 1968

By C. G. Dunn, P. K. Koh

THE primary recrystallization texture in cold-rolled silicon iron, which is the matrix texture for developing the Goss texture or the cube-on-edge texture by secondary recrystallization at temperatures near 900°C,1-5,21 has not been adequately described. Thus from the present available information, it is not possible to explain satisfactorily both the grain-growth selectivity of the matrix and the often observed magnetic torque curve, which itself provides some information on the texture. Also lacking is information on the special annealing texture that develops in this material when the annealing temperature is 1200°C or higher and the rate of rise to temperature is extremely rapid. From the work of May and Turnbull5 and from unpublished work, it was known that isothermal annealing near 1200°C tends to reduce the extent of secondary recrystallization and that a much weaker cube-on-edge texture results if appreciable normal grain growth replaces secondary recrystallization. Koh and Dunn6,7 have obtained additional information on complex primary recrystallization textures from further studies made after normal grain growth. In these instances the initial textures were retained during normal grain growth. A similar result reasonably could be expected in the present study except for the presence of a grain growth ihibitor1-5,8,9.21 and its tendency to allow only a few grains to grow. However, any information on the orientations of grains in the special annealing texture, even if far from representative of the initial matrix texture, would provide useful information on the nature of the matrix texture. In the present texture study the method of Newkirk and Bruce,10 which is based on the methods of Geisler" and Schwartz, 12 is used to obtain a complete (110) pole figure of the primary recrystallization texture. The high-temperature annealing texture is determined simply from the orientations of a large number of selected grains. The kinetic nature of the process that produces the annealing texture is treated elsewhere13 and it is shown that a form of secondary recrystallization with a very high rate of nucleation occurs during rapid annealing at high temperatures. EXPERIMENTAL PROCEDURE Commercial 0.014-in. cold-rolled silicon iron strip (3.16 wt pct Si), prepared by two stages of cold rolling with an intermediate short anneal, was given a decarburizing 3-min anneal at 800°C. Me-tallographic studies indicated complete recrystallization. Short-time anneals at 900° C and at higher temperatures proved that secondary recrystallization had not begun at 800°C, in fact, the short additional anneals were still in the induction period of secondary recrystallization. A rapid rise to an annealing temperature of 1260°C (2300°F) was obtained in a BaC12and NaCl fused salt bath. The structures that resulted from anneals in the range 12- to 1000-sec duration were relatively finegrained, even though the growth was a form of exaggerated grain growth13 or secondary recrystallization with a high nucleation frequency.= Many of the grains were large enough for an X-ray study using a 5-mil X-ray beam. A transmission Laue Camera and an optical-mechanical stage for moving the grains into the X-ray beam were used. A total of 325 grains were X-rayed in this manner and the grain orientations determined. Complete (110) pole figures were obtained for the primary recrystallization texture using CoKa radiation at 30 kv in the back-reflection range, such as (220) for (110) poles, as described recently by Newkirk and Bruce.10 The low voltage serves to reduce the spurious white radiation to a minimum. A filter of 0.001-inch iron foil was located in front of the detector slit for transmission and in front of the beam slit for back reflection. A new and improved specimen holder extended the useful tilting angle range for transmission to 70 deg instead of 60 deg as previously reported.' A torque magnetometer was used to obtain the magnetic torque curves for a number of l-in. diam disk specimens. RESULTS The (110) pole figure of the material after recrystallization at 800°C is shown in Fig. 1. The positions of the pole concentrations are found to be

Jan 1, 1961

By D. P. Kedzie, R. A. Dodd

The fatigue strength, fatigue hardening, and effect of fatigue deformation on subsequent age hardening of supersaturated Al(Cu) solid solutions have been determined as functions of alloy composition and temperature. The fatigue strength/tensile strength ratios, determined at 150°, 25°, and -195°C, decreased with increase in alloy content for all temperatures, but the F.S./U.T.S. ratios at -195°C decreased much more rapidly than did the ratios for 150" and 25°C. This suggested that strain aging and/or age hardening occurred during tests at higher temperatures. Additionally, the F.S./U.T.S. ratios at 150°C exceeded those at 25°C for all compositions, indicating greater strengthening during fatigue at 150°C. The effect of fatigue or tensile deformation at 150°, 25°, and -195°C on subsequent age hardening showed that the deformatzon increased the rate of precipitation and indicated that mechanically produced vacancies were probably formed during deformation. Fatigue hardening was studied at 150°, 25°, and -195°C, and the effect of room-temperature rests after 10 and 100 cycles was examined. The results confirmed that strain aging occurred at the higher temperatures . DURING the last 15 years various mechanisms of fatigue crack nucleation and growth based on dislocation and vacancy interactions, operating singly or collectively, have been proposed. The probable consensus of present opinion is that the fatigue process in pure metals essentially involves dislocation interactions, and that vacancies formed by such interactions play a minor or inconsequential role. However, there is some evidence that age-hardened alloys tend to overage during fatigue, probably by local vacancy-enhanced diffusion, and strain aging also might be important in selected cases. Furthermore, it has been established that the behavior of quenched-in vacancies in Al(Cu) and other solid solutions is composition-sensitive. Therefore, it seemed worthwhile to investigate various aspects of the fatigue behavior of supersaturated Al(Cu) alloys and to examine the results in terms of vacancy-enhanced effects. EXPERIMENTAL The alloys used in this investigation were prepared from 99.994 wt pet A1 and OFHC copper, the latter containing 0.04 pet 0 as the principal impurity. Six alloys were made, containing, by actual analysis, 0.58, 0.96, 1.96, 2.85, 4.45, and 5.51 wt pet Cu. They were induction-melted in air in graphite crucibles, cast as 7-in. by 7/8-in.-diam rods in graphite molds, and hot-rolled to 5/8 in. diam. The experimental work was a three-part program involving the determination of a) 10' cycle fatigue stresses as a function of alloy composition and temperature; b) the effect of fatigue deformation on subsequent aging of the supersaturated alloys; and c) fatigue hardening as a function of alloy composition and temperature. For determining the 105 cycle fatigue stresses, a portion of the 5/8-in. stock was machined into Krouse rotating cantilever beam fatigue specimens, 2 in. in length by 1/4 in. minimum diameter. These were tested at +150°, 25°, and -195°C (liquid nitrogen) on a Krouse high-speed machine, with special weights to provide lower -than-normal loading ranges, this being necessitated by the small load requirements of those alloys of lower copper content. For the high-temperature tests a small resistance heater was designed to clear the collets and fit in between the chucks, while for the low-temperature tests a hollow nylon cylinder was used, having closed ends drilled to pass a fatigue specimen, and positioned similarly to the heater. A plexiglass container completely enclosed the fatigue machine; rubber gloves fixed to ports in the walls enabled the machine to be operated from outside the box. A tray of magnesium perchlorate dried the air in the container and prevented both atmospheric corrosion fatigue at room and elevated temperatures and troublesome ice build-up at low temperatures. A total of ten to fifteen specimens was used for each combination of alloy composition and temperature. The result of each test was plotted on a standard S-N diagram, and the next stress was selected on the basis of the trends indicated by previous specimens. In this manner a small portion of the S-N diagram was constructed, and the 105 cycle fatigue stress obtained. Small Krouse fatigue specimens were also used to study the effect of cyclic prestrain on subsequent

Jan 1, 1964

By N. E. Brown, F. L. Versnyder

THE apparent dependency of the electrical characteristics of hexagonal crystalline selenium on microstructure has aroused much interest in microscopical studies of selenium. Microscopic observations on the crystallization of selenium have been made by Escoffery and Halperin,' P. H. Keck,' and other investigators. It is the purpose of this paper to discuss the microstructural changes observed on polished cross-sections of single layers of selenium after various heat treatments. Observations were also made on crystallization of the free-surface layer of these deposits. In general, all of the transformations studied were either transformations of the vitreous selenium to hexagonal selenium or micro-structural transformation of the hexagonal selenium itself. Procedure The selenium used in this work was obtained from the American Smelting and Refining Co. and was approximately 99.96 pct pure. An intentional impurity of 1 part per 2,000 of bromine was added to the material prior to evaporation. A thickness of approximately 0.002 in. of this selenium was vapor deposited on an aluminum base plate. The maximum plate temperature during the vacuum vapor deposition was 140°C. Mounting of the cross-sectional specimens for metallographic study could not be done in plastic mounting media, as is customary, since temperatures in excess of 50°C would cause unwanted transformations. Consequently, a simple clamp-type device was used to mount the specimens for preparation. All grinding operations were then done carefully by hand in order that the specimen not become heated during this operation. Wet polishing was done on the conventional metallographic polishing laps, using successively finer grinding powders. An extremely careful polish is necessary, since observation and micrography of the specimens are done in the unetched condition under polarized light. The two observations of crystallization made on the free surface of vitreous selenium deposits (Figs. 4 and 5) were made on surfaces which were perpendicular to the cross-sections studied. These free-surface layers were examined directly, i.e., no pre- vious metallographic preparation, as obtained from the vacuum vapor deposition. Microscopic Observations A study was made of polished cross-sections of the vitreous selenium as-deposited. It was noted that in all cases there was columnar crystallization adjacent to the base plate, which appeared to occur during the vacuum deposition process. This observation has also been made by Keck? It also was observed that vagrant spherulitic crystallization occurred in the vitreous selenium. The term "vagrant" is used, since these spherulitic grains appear to crystallize at random throughout the vitreous selenium during the vacuum deposition process. Columnar crystallization at the A1-Se interface and a typical spherulite observed in a polished cross-section of "as-deposited" vitreous selenium may be seen in Fig. 1. Cross-sectional samples of vitreous selenium studied after heat treating individual samples for 20 min in 10" steps from 80" to 220°C revealed that crystallization—in this case, columnar crystal growth —proceeds from the aluminum base plate to the surface of the specimen (Fig. 2). Crystallization was microscopically observed to be complete after the 130°C heat treatment. Visual examination of the free surface of the specimen after the 130 °C heat treatment revealed the readily recognizable grey appearance of the completely crystallized selenium, in corroboration of the microstructural observations. No microstructural transformations then appeared to take place between 130" and 190°C. At 190°C the beginning of recrystallization appeared and proceeded until the columnar grain structure had been completely transformed to equiaxed grains between 210" and 220°C (Fig. 3). Naturally, the grain size of the recrystallized grains at the lower temperatures (190" to 210°C) was smaller than is illustrated in Fig. 3. In addition, polished cross-sections of deposits heat treated at 140°C for 10 min to cause complete crystallization and, subsequently, heat treated in 10" steps from 80" to 220°C for 20 min were studied. As expected, no microstructural transformations took place until the beginning of recrystallization was observed at 190°C. A comparison with the previously studied specimens revealed that recrystallization proceeded almost identically in the two experiments although in the first case the deposits were vitreous prior to the series of heat treatments and in the second case they had been crystallized by a previous heat treatment. By heat treating for longer times (180 min) at lower temperatures, the

Jan 1, 1956

By T. Yamasaki, S. Usu

Adsorption of potassium dodecyl xanthate from aqueous solutions on artificial and natural zinc sul-fides was studied by means of infrared absorption spectroscopy. The adsorption species and their stabilities varied depending upon the conditions of the surfaces of the zinc sulfides. Adsorption products were analyzed after they had been removed from the surface with pyridine. Zinc dodecyl xanthate was confirmed for surfaces covered with oxidized products while dodecyl alcohol and carbon disulfide were detected on purified or weakly oxidized surfaces. It is of great significance to study the adsorbed species of collectors on the surface of sulfide minerals with a view of increasing our understanding of the mechanism of flotation. Compared with other methods, infrared spectroscopy promises to be of particular value in determining the nature of the species adsorbed at the mineral/solution interface since it gives direct identification of the adsorption products; and, furthermore, it has an advantage over the electron diffraction technique which has been employed in similar problems in that infrared spectroscopy utilizes radiation of very low energy so that the probability of changing the unstable surface films during examination should be correspondingly decreased. Infrared spectroscopic studies concerned with sulfide mineral flotation have already been reported by several investigators on zinc sulfide-hexanthi01' and lead sulfide-xanthate2,3 systems. The purpose of the present study was to investigate the adsorption of potassium dodecyl xanthate (KDX) at the zinc sulfide-aqueous solution interface by means of infrared spectroscopy. Rarely is the pure zinc sulfide-xanthate system encountered in practical flotation since zinc sulfide is usually activated with small amounts of certain metallic ions, such as copper ion. However, investigation of the pure zinc sulfide-xanthate system appeared promising for studying the fundamental mechanism of the adsorption of xanthate on the sulfide minerals. Although there are few cases where xanthates having an alkyl radical higher than hexyl are employed in practical operations, KDX was used in this study since it was reported that the adsorbability of xanthate on zinc sulfide was increased with an increasing number of carbon atoms of the alkyl radicals.4 EXPERIMENTAL Samples: Experiments were made on artificial zinc sulfide and natural sphalerite. The artificial zinc sulfide was obtained commercially from Dainihon Toryo Co. as a fluorescent pigment of the purest grade A. Considering the fact that there are often cases where the surface of sulfide minerals are apt to be oxidized so that the adsorption of xanthate at sulfide mineral/solution interfaces may be substantially affected, two different procedures were employed in preparing the samples of the artificial zinc sulfide. 1) The zinc sulfide was washed with hot concentrated ammonium chloride solution (300 g per liter) to remove surface oxidation products and followed by washing with deoxygenated hot distilled water by centrifugation until the constant electric conductivity of the solution was reached (Sample I) (specific conductivity of the solution = 8.6 x l0-5 ohm-' cm-'). 2) Sample I in a suspension of 5% by weight was oxidized with a 1.5% aqueous hydrogen peroxide solution for about one hour, and then was washed with distilled water as mentioned in the preparation of Sample I (Sample 11) (specific conductivity of the solution = 1.0 x 10"4 ohm-' cm-'). Both Samples I and II were dried under vacuum and stored in a vacuum desiccator. The specific surface areas of the samples determined by the BET method using carbon dioxide gas were 19 x l04 cm2 per g for Sample I and 35 x l04 cm2 per g for Sample 11. In addition, a sample which was derived from Sample I was also prepared. In 40 ml of 3 x 10-2 M zinc sulfate solution was placed 2 g of Sample I for 2 hours, washed with distilled water by successive centrifugation until no sulfate ion could be detected and dried under vacuum (Sample 111). The purpose of this treatment will be described later. Natural sphalerite was carefully selected by hand, ground in a mechanical agate mortar for about 40

Jan 1, 1965