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By John C. Bilello

The brittle fracture behavior of cold-worked sintered tungsten was studied over the temperature range 4.2° to 298°K using a high-sensitivity strain measuring system and electronfractography. Similar observations were made on a swaged electron beam zone-refined monocrystal. In sintered tungsten irreversible plastic deformation was observed during cyclic load-unload tests at stress levels well below the fracture stress for all temperatures, but general microyielding could be detected only down to 202°K. For the zone-refined samples macroyielding occurred at all test temperatures with evidence for twinning below -202°K. The fracture stress of the sintered tmgsten was virtually independent of temperature, while the zone-refined crystal showed a 2.3 times increase over the same temperature range. Electronfractography confirmed the presence of numerous rod-shaped and spherical submicroscopic voids which ranged in diameter from 1400 to 4300A in the sintered tungsten; no voids could be found in the zone-refined tungsten. Contrast effects observed on the replicas in the vicinity of certain voids indicated that plastic deformation could be induced by the local stress concentration. It has been suggested that the presence of these voids may be responsible for the low-temperature brittle failure of sintered tungsten. Based m this suggestim und on the evidence obtained here, a dislocatim model is presented to account for the brittle behavior of sintered tungsten. In this model slip, which is induced by the local high stress concentration in the region at the edge of a favorably oriented void, could cause the void to grow to a microcrack of critical size. STUDIES of brittle fracture in bcc metals have led to the well-known experimental relationships between grain size, yield stress, fracture stress, and temperature which have formed the basis for the various dislocation pile-up1-3 or interaction4'= models for slip-induced microcrack nucleation. While microcracks can be nucleated by deformation twins,6,7 there has been no direct evidence furnished by transmission electron microscopy to support conclusively either the Zener pile-up or Cottrell dislocation reaction models for producing micro-cracks in all "brittle" materials. In addition to the "inverse" grain size relationship for yield and fracture stresses the cottrel14 theory predicts that the fracture stress below the transition temperature should behave in a fashion similar to that of the yield stress above this temperature. Such behavior has been verified for several bcc metals.8-10 With reference to both grain size effects and the tem- perature dependence of the fracture stress below the transition temperature, the behavior of sintered tungsten appears anomalous. Early work by Bechtold and Shewrnon 11 showed no apparent temperature dependence of the fracture stress below the ductile-brittle transition temperature (DBTT). They attributed this result to the intergranular nature of the fractures observed. More recent work by Wronski and Four-deux12'13 on considerably purer material did not show any systematic relationship between the fracture stress and temperature below DBTT. The dependence of flow and fracture stresses on grain size is also not clearly established for sintered tungsten. Koo, for example, has shown that the DBTT for sintered tungsten depended chiefly on the annealing temperature and was relatively insensitive to the actual grain size achieved. Using electrofractography and transmission electron microscopy, Wronski and Fourdeuxl3 showed that numerous spherical and rod-shaped submicroscopic voids could be found in sintered tungsten but not in melted tungsten of nominally the same purity. They suggested that these voids could be responsible for the temperature insensitivity of the fracture stress below the DBTT. In the present work the temperature dependence of the fracture stress for high-purity commercially sintered tungsten has been determined. The presence of submicroscopic voids in sintered materials was confirmed, and these were studied in detail to examine the role they could play in nucleating brittle fracture. A dislocation model is suggested which could cause an inherent spherical void to lengthen into a Griffith crack of critical size. EXPERIMENTAL PROCEDURE Commercially sintered tungsten rod was obtained in the as-swaged condition from Sylvania. A zone-refined crystal was obtained from the same source. This crystal was grown by giving three zone passes (at 25.4 cm per hr) to a sintered rod of high-purity tungsten. The rod axis prior to cold working was -15 deg from the [110] direction. Originally the zone-refined rod was -6 mm in diam; it was reduced to -3 mm by eight swaging passes, at high temperatures, with each step having about the same reduction of area. The final swaging step gave a 7.5 pct reduction of area at 1050°C. All swaging operations were performed in a hydrogen atmosphere. For the sintered rod a similar working schedule was employed. Metal-lographic examination of the sintered material revealed that the cold-worked structure had an apparent grain diameter of -25 u transverse to the swaging direction (obtained by the intercept method). In the longitudinal direction cold-worked grains were approximately 1.5 to 2 times their diameter. No distinct fiber structure could be observed optically for the zone-refined rod. The cold-worked structure in the

Jan 1, 1969

By Cyril Wells, Robert F. Mehl

THE practical importance of a knowledge of the rates of diffusion of carbon and of alloying elements in steel has often been pointed out 1,13 This importance ties chiefly, though by no means only, in the study of carburizing and in the study of reactions involved in the eutectoid inversion in steel The present paper is one of a series in which the rates of diffusion of carbon and of alloying elements in y-Fe and their mutual effects are measured with precision The present paper reports the results of meas¬urements of diffusion coefficients D of manganese in -y-Fe over wide ranges of temperature, and concentration, and of the effect of carbon and impurities and of grain size upon these diffusion coefficients [$] Data on the rate of diffusion of manganese in y-Fe have been reported by Fry2 and by Paschke and Hauttmann 3 Claussen4 calculated the diffusion coefficient D from Fry's data as 3 X 10-10 sq cm per sec at 960°, which will be shown to be incorrect by many orders of magnitude Paschke and Hauttmann gave a rough value of 9 6 X 10-8 sq cm per sec at 1400° Neither of these workers considered the variation of D with concentration and with temperature, and neither studied the effect of carbon METHOD AND MATERIALS Method -The method employed is identical with that used earlier 5 Owing to the volatility of manganese and the consequent loss of manganese from the outer surfaces of the welded diffusion bars, these surfaces were discarded The diffusion anneals were performed in argon, except one (test 18) in which hydrogen was employed for purposes noted below The temperatures reported are accurate to about 3° and constant within I°C , the diffusion times are reported to the nearest half hour The specimens were furnace-cooled after the diffusion anneal at about 2° per min Layers, usually 0 004 in thick, parallel to the welded interface, were machined from the specimens after the diffusion anneal and analyzed for manganese to 0 01 per cent Mn, the distances of these layers from the interface was measured to ±0 0002 in The concentration-penetration curves obtained were analyzed by both the Grube and the Matano solutions e The D values calculated by these two methods do not differ appreciably 5 The Grube solution was used except in tests in which the effect of concentration upon D was greater than 50 per cent, in such cases the Matano method, which explicitly provides for the variation of D with concentration,1 is the more reliable In general, the number of layers machined from the zones of variable composition were large enough to permit the use of the average layer composition as that of the center of the layer In 3 of the 30 tests, however, this is not justified, and the D values

Jan 1, 1941

By P. E. Demmler

PHOSPHORUS combines with copper in various proportions, forming true alloys, some of which are of commercial importance. These materials find wide application as deoxidizers and as a means of introducing phosphorus into other alloys, as in phosphor-bronze. Phosphor-coppers containing 10 and 15 per cent. of phosphorus are the commercial grades that are most generally offered. Each has certain advantages when used in making other alloys. The 10 per cent. grade of phosphor-copper has an advantage over the 15 per cent. in that it has a much lower melting point and can be prepared by certain methods with a much lower loss in phosphorus. The 15 per cent. grade has the advantage of lower freight rates per unit of phosphorus and, by the method to be described, a uniform product can be prepared with practically no loss of phosphorus. Alloys of copper and phosphorus containing any desired percentage of phosphorus lower than 15 per cent. can be prepared by melting together the requisite amounts of copper and 15 per cent. phosphor-copper. Processes for making phosphor-copper may be divided into two classes as follows: (1) Those depending on the smelting of phosphate rock or superphosphate of calcium with copper or copper-bearing materials, and coal or other carbonaceous material; (2) those depending on the direct combination of metallic copper and elemental phosphorus. A number of formulas for preparing phosphor-copper according to the first method have been published. The Metal, Industry' gives-the following: Superphosphate of calcium, 60 lb.; granulated copper, 301b.; finely powdered coal, 10 lb. Similar formulas are given by Brannt2 and others, and detail 'variations are covered by patents, such as those of L A Jeffs3 and H A Webster.4

Jan 8, 1920

By Donald N. Rosenblatt

I would like to commend the author on his description of Pinto Valley's plant, and its interesting innovations. The author's discussion of 18 ft in diameter by 21 ft long primary ball mills (the largest wet ball mills made to date) is of considerable importance to those who have been engaged in the field of studying ball mill liner wear as it relates to various grinding installations. While it is stated that the mills have operated on a fixed tonnage and therefore it has been difficult to determine the best liner pattern, calculations from the data in the paper indicates that for mills 1, 2, 5, and 6, the tonnage per hour varies from a low of 223 for mill No. 1, up to a high of 314, for mill No. 2, while mills 5 and 6 calculate 285 and 246, respectively. Analysis of the wear patterns for the single wave liners used in mill No. 1 as compared to the double wave liners in mill No. 2, suggests that the author's data may tell more than he suspects about liner wear to be expected and thus what should be a best pattern selection from what may appear to be only limited hours of operation. [Fig. A] is a reproduction of author's [Fig. 10], to which wear forecast patterns [F-1 and F-2] have been added. Forecasts are based on many previous studies of large diameter ball mill operations over many years of field service. Calculations from the first-wear pattern provide an initial wear rate of only 13 lb of liner per 100 sq ft of shell liner surface per day, or 0.031 lb per to: ground. However, the second wear pattern is ac-

Jan 1, 1978

By J. A. Holmes

SHUTTING-IN the Rangely gas well was an interesting problem because of the high rock pressure and the volume of gas developed, as well as the difficulties encountered. After nearly a week's open flow, the rock pressure was 1275 lb., which corresponds with a 2950 ft. hydrostatic head. The volume of gas was between 45,000,000 and 50,000,000 cu. ft. per day. The Rangeley oil field, which now has a daily production of 100 bbl. of shale oil from shallow depth, lies approximately 100 miles north and 30 miles west of Grand Junction, Colo.; not far from the Utah line. The, well we are considering was drilled on the apex of a large clearly defined. Structure1 in the SE.1/4 sec. 30, T. 2 S., R. 102 W., and entered the gas sand at 2954 ft. on March 2, 1925. The condition of the well at the time the gas was encountered was as follows: 20 ft. of 20-in. conductor cemented with ten sacks at 40 ft. The 15 1/2-in. casing was pulled when the 12 1/2-in. was cemented. 1166 ft. of 12 1/2-in. casing, cemented with fifteen sacks. 2531 ft. of 10-in, casing, cemented with ten sacks; neither the 12 1/2-in. nor the 10-in, casing shut off water but they were cemented for protection. 2938 ft. of 8 1/4-in. 36-lb. casing, hanging on a spider in the collar with a forged-steel, high-pressure bradenhead between it and the 10-in. casing. An 8 1/4-in. drilling, or master, gate and a control head were in place on the 8 1/4-in. casing, and all was in readiness for the bringing in of the well.

Jan 1, 1926

By C. A. Heberlein

INTRODUCTION THE present war in Europe seems to have stimulated the demand for quicksilver. In July last, the price ranged around $35 per flask of 75 lb., while to-day it seems to fluctuate between $47.50 and $50. The use of quicksilver in the form of fulminate, containing 70 per cent., and as corrosive sublimate, containing 73.8 per cent., must be extensive and a further market advance may be expected. With such an advance, some revival in quicksilver mining maybe looked for, particularly in California, where many abandoned properties exist. What can be done with low-grade quicksilver ores under favorable conditions, particularly with low mining cost, may be seen from the following description of the Oceanic mine, near. San Luis Obispo, Cal. Its operations date back to 1876, when rich sand ores were discovered. In three years 7,400 flasks of quick-silver were produced, but since then the deposit has been only sporadically worked. Until two years ago various attempts had been made by the Oceanic Quicksilver Co. to mine the more refractory "mud rock," which was encountered lying beyond the "sand rock." Mud and sand rock in varying quantities were treated together with poor results, but operations were successful with sand rock of fair percentage. About two years ago,, when all the sand rock had been exhausted, Murray Innes purchased the Oceanic mine. He found large quantities of low-grade mud rock, varying from 6 to 8 lb. of quicksilver per ton, which at the prevailing low price of quick-silver demanded very cheap mining costs, in conjunction with high but cheap metallurgical extraction. At that time the extraction of quicksilver from mud rock ranged between 40 and 50 per cent., as far as I am able to, learn.

Jan 2, 1915

By Z. F. Oszter, D. Vincent, W. K. Behrands

With the expansion of open pit operations, belt conveyors are going to be used in the 13 608 to 18 144 t/h (15,000 to 20,000 stph) capacity range, which calls for a review of some of the horsepower calculation methods. This paper presents methods (based on German research data, field tests and theoretical considerations) for the evaluation of the Ky factor in the CEMA formula for belt conveyors of large carrying capacity, which fall beyond the limits of the data given in tables in the CEMA book. (The CEMA limits are 407 N\\m (300 lb ft) and Tave = 7.3 Mg (16,000 lb). At these large loads, the impression resistance of the belting on the idlers plays a major role, which in turn influences the magnitude of the drive horse power required. An example will illustrate the order of magnitude difference of the horsepower values obtained by using a conventional calculation method and the suggested method, as well as the beneficcia1 influence of the 4-roll idler in comparison to the standard 3-roll unit for a large caving capacity belt conveyor. This paper concerns itself with the analysis of the resistance to motion of belt conveyors, emphasizing the evaluation of the frictional resistance to motion due to load and belt pressure on the idlers and the flexing resistance of the belt and material when passing over the idlers. In the case of long and heavily loaded belt conveyors, the aforementioned resistances reach extremely high values calling for close analysis of the phenomena, presently not calculable with normally used formulas. This paper establishes correlation between experimental and empirical data presenting practical formulas a tool for the designer of high-capacity belt conveyors. The application of the formula is illustrated in an example in the Appendix.

Jan 1, 1981

By W. N. Lacey, B. H. Sage

In recent years there has been an increase of interest in the flow of gases at relatively high pressures. Hydrodynamic calculation of the energy losses in the flow of gases in conduits, as well as through the porous solid materials constituting natural petroleum reservoirs, requires a knowledge of the viscosity of the fluid at the pressure and temperature involved. Although there are numerous publications concerning the absolute viscosity † of hydrocarbon gases at atmospheric pressure, there appears to be little information available relating to the effect of pressure upon the viscosity of these gases. Voge133 determined the viscosity of methane at 32° F. and atmospheric pressure. His measurements at 32° F. were later substantiated by the measurements of Rankine and Smith20 at 63° and 212° F. Ishida14 also reported values for the viscosity of methane at atmospheric pressure. Trautz and Kurz30 measured the viscosity of propane at atmospheric pressure, from 83° to 530°F., by the use of a short capillary tube. Rap-penecker2' determined the viscosity of gaseous isopentane at elevated temperatures. Day6 made an accurate investigation of the effect of pressure upon the viscosity of n-pentane and isopentane at pressures from 2 lb. per sq. in.‡ to the vapor pressure at 77° F. (approximately 9.8 and 13.3 lb. per sq. in., respectively). Earhart7 reported data upon the viscosity of several natural gases measured by the long capillary-tube method. The viscosity of air, at atmospheric pressure and 73.4° F., was measured by Harrington9 by the rotating-cylinder method. Kellstrom15 has rec,ently made an elaborate investigation of the viscosity of air at atmospheric pressure. The latter work is perhaps the most accurate investigation of the viscosity of a gas that has been made.

Jan 1, 1938

ONE of the problems that confronts the chronicler of the Porphyry story is to determine the date from which Morenci should be regarded as one of the group. The mines have the distinction of being the first operated in Arizona for copper. A small smelter was in operation as early as 1873 and in the eighties two smelters accounted for a substantial production ranging from 3,000,000 to 6,000,000 lb. per year. The first concentrator was built in 1886, but the ores were principally oxidized, and direct smelting ore still supplied most of the production. As early as 1893, the mining of somewhat leaner porphyry ores, containing copper in the form of the sulphide mineral, chalcocite, was commenced; but these still were of comparatively high grade and the concentrators were plants of 100 to 400 tons daily capacity. Moreover, the backbone of operations was still the production of rich oxidized ores for direct smelting. They assayed 10 to 15 per cent copper and the sulphide milling ores assayed 3 to 4 per cent. A significant comment appears in the Copper Handbook for 1908. Speaking of the Arizona Copper Co., Ltd., which was to become the most important component of the present Morenci enterprise, the editor, Horace Stevens, says: "A tremendous amount of ore is in sight, ore reserves . . . being estimated at 10,370,600 tons . . . " It seems fair to infer from this that the property was not yet regarded as an immense low-grade mine, but that the copper content of perhaps 70 lb, to the ton made an ore of "medium " grade even according to the standards of the time. Although the concentrating ore was typical of that in the porphyry group of mines (except for its greater richness), no one seems to have the least inclination to take from Utah the

Jan 1, 1933

By W. H. Schacht

IN THE Lake Superior District, the air indoors must be heated continuously during eight months of the year and occasionally during the remaining months. Incident with mining in this district, therefore, there is need for heating many of the buildings connected with these operations. In addition to the mine buildings, that is, shops, engine, houses, offices, change houses, etc., such public buildings as schools, library, and theater, when close to the mines, are often supplied from the mine heating mains. At the Copper Range Company's mines, Champion, Trimountain and Baltic, the heating surface thus supplied from the mine mains is over 50,000 sq. ft. (4645 sq. m.) which requires a steam consumption, at times, of 18,000 lb. (8165 kg.) per hour, or the equivalent of a rate of over 50 tons of coal per day (were live steam used). This figure is based on a consumption of 1/3 lb. per square foot of heating surface during the coldest weather, and provided the system is not wasting steam by blowing it to the atmosphere or into the return line on account of leaky traps, which so often is the case. Under the latter conditions, steam consumptions of three to four times the above rate are not uncommon. This shows that the cost of heating is of enough importance to be given serious consideration, especially at this time of rising prices of fuel. The power and heating value of exhaust steam are appreciated by most engineers, and its application for such purposes is general. At our stamp mills, the exhaust from the stamps is used to operate low-pressure turbines, thus reducing the former water rate per horsepower developed by more than 50 per cent.

Jan 8, 1920

By E. H. Jr. Dix

THE success of the Charpy impact test in the steel industry has led those interested in aluminum alloys to investigate the possible applica¬tion of this test to aluminum and its alloys. In this paper are set forth the results of a few preliminary tests made at the Lynite Laboratories of the Aluminum Manufactures, Inc. In order to study more thor-oughly the significance of the Charpy test, slow-bending tests have been made duplicating the arrangement of the impact machine. Tests have been made on both notched and unnotched specimens of a series of copper-aluminum alloys. APPARATUS The standard American-made Charpy impact machine delivering a blow of over 200 ft.-lb. was- much too large to test aluminum-alloy specimens of the same type used for steel, so that it was necessary either to adopt a larger specimen or to have a special light-weight hammer made. Since there is no known relation between specimens of different sizes, even though geometrically similar, it was decided to adhere to the 10 by 10 mm. specimen. Accordingly, Sauveur and Boylston, the American makers of the machine, were asked to construct a special light-weight pendulum adapted to their standard machine, this pendulum to have one-tenth the capacity of the standard. The writer wishes here to acknowledge his indebtedness to Mr. H. M. Boylston for the personal interest and care exercised in constructing this pendulum. The machine with, the light-weight hammer in place is shown in Fig. 1. It is mounted on a concrete foundation with the concrete covering the flange on the base of the machine. Vibration is further prevented by four 5/8 -in. (15.8 mm.) foundation bolts. The large standard hammer shown against the wall was also used for some of the unnotched bars that requited more than 20 ft.-lb. to rupture.

Jan 4, 1920

US 4,190,436 - In the cyanide leaching of gold ore in tailing or ore dump piles, or gold ore in vats or on pads, the ore is agitated and oxygenated by introducing timed bursts of air, along with cyanide in a cyclic or regulated manner. The leach liquor is drained from the material by providing a continuous flow of air. Fines are homogenously mixed, thereby reducing channelling In the ore bed. Yield is improved and cyanide consumption lessened. R M. Hughes Feb. 26, 1980. 7 pp. (75-105). Filed. 12-20-77 (862,335).

Jan 1, 1982

By K. C. Sclater

GAS as a factor in the efficiency of oil production, might be a better title for this paper as it deals in general with the significance of the gas-oil ratio as an index of the efficiency of oil production and briefly discusses oil production methods with reference to the gas-oil ratio in wells, particularly during the early life of a field. In the recent hearings held at Washington before the Federal Oil Conservation Board the fuller utilization of the energy contained in the gas occluded in or associated with the oil underground was stressed by some of the speakers when referring to greater ultimate recovery of oil. One speaker commenting on this point said in part, "There is ample evidence indicative that if the gas associated with the petroleum in our fields were conserved and elevated gas pressure maintained in the oil sands during their productive life, the ultimate production of oil could be greatly increased."

Jan 1, 1926

By Bernard York, John J. Reed

J. P. Zannaras (U.S. Tungsten Corp., Congress, Ariz.) —In the investigation described in the paper by Bernard York and John J. Reed, the 8x8x8-in. square block was subjected to compressive forces from three sides, top, side, and rear. Let us refer to the stresses set up by these forces as Sz due to top pressure, Sy due to side pressure, and Sx due to rear pressure. At the section across the 2-in. hole (when failure occurred at 317 psi) the compressive stress Sy was equal to 317 x 8/6 = —422 psi, the top compressive stress S; is of the same intensity, —422 psi, and the rear compressive stress S, equals —317 psi. The true stress is T = Sy — S — S Taking as 0.2,* Taking the case when the opening was ½ in. and failure occurred at 517 psi, 8 Sy - 517 x -----= —537 psi 7.5 8 Sz = 517 x-----= —537 psi 7.5 Sx = —517 psi The true stress T = Sy — Sz — S, T - —537 + 0.2 x 537 + 0.2 x 517 = —327 psi. It can be shown that the above fundamental formula holds good not only for the above two examples but for all sizes of openings used, because when this formula is expressed in terms of the external pressure and size of the opening it agrees perfectly with the experimental results obtained by the authors and given in Fig. 12 of their paper. General formula: T = Sy — s: — S....

Jan 1, 1955

By David E. Van Dillen

INTRODUCTION Current design practices for deep tunnels make extensive use of plasticity solutions by Newmark (1970) and Hendron and Aiyer (1971). These solutions are applicable to a circular tunnel subjected to a hydrostatic stress state in a Mohr-Coulomb plastic medium. The role of rockbolts is introduced into these solutions as a uniform internal pressure equivalent to the yield stress of the rockbolt pattern. The application of these solutions is hampered by their inability to consider the biaxial nature of the in-situ stress field or any surcharged stress, such as due to blast loading. As a means of considering the biaxial stress field, designers have turned to relatively costly alternatives, such as the finite element method. The recent work of Detournay (1983) simultaneously provided two generalizations to the state of the art of the analysis of circular tunnels. Whereas the solution of Newmark applies to nondilatant Mohr-Coulomb materials, and that of Hendron and Aiyer applies to materials having associated flow rules, the solution of Detournay covers materials of arbitrary dilatancy. Secondly, Detournay's solution is valid for biaxial stress states, as long as the problem remains statically determinate (St. John, Detournay, and Fairhurst, 1984). The topic of this paper is an investigation of various alternatives for introducing the effects of rockbolts into simple tunnel design charts developed using Detournay's solution. The study was conducted using the BMINES finite element code, into which rockbolt elements have been added (St. John and Van Dillen, 1983). These rockbolt elements allow for plastic deformation of the bolt, bolt

Jan 1, 1984

By A. J. Boynton

THIS paper is not the result of recent research with regard to any particular feature of iron metallurgy, blast-furnace practice or mechanical engineering. It is rather a series of notes with regard to contemporaneous progress in blast-furnace construction and operation, together with some suggestions as to changes and improvements that seem to be desirable. On April 1, 1930, a committee of the Chicago District Blast Furnace and Coke Association presented to that association a rather ambitious study of blast-furnace equipment, together with recommendations for the design of construction of a complete blast-furnace unit for the production of 1000 tons of pig iron per day. This report represented the result of months of study by members of the committee, all of whom were actively engaged in operation or design of blast-furnace plants. It is natural, therefore, that comments on the present state of the art should take this 1000-tons furnace, as recommended by the Association, as a basis for comparison with corresponding features of construction or design. See Table 1. In looking through this report at the present time, the significant difference is in the nature of the gas-washing equipment that today would be specified. In other respects, the installation would remain generally very much as it was outlined in 1930. The change in furnace dimensions would be very slight and of no especial significance, except with respect to changes in stock-line diameter, of which more will be said hereafter. The high-efficiency stove as developed by various designers is thoroughly described within this report, and few changes have taken place since. Blowing equipment shows refinement and reflects the improvement in steam engineering. Hoisting and charging equipment and ladles for the conveyance of iron and slag remain, in general, as they were in 1930. In accordance with a general tendency

Jan 1, 1935

By H. A. Bright, H. C. Vacher, J. G. Thompson

The methods employed for the determination of oxides and oxygen in ferrous materials may be roughly classed in two groups, "wet" methods and "hot" methods, the first group including the iodine, electrolytic, mercuric chloride, hydrochloric acid, nitric acid, and chlorine methods; the second group including the vacuum-fusion and hydrogen-reduction methods. The wet methods depend upon preferential solubility in a selected medium to separate the metallic portion of the sample from the oxygen-containing constituents. Subsequent analysis of the insoluble residue permits the isolation and separate determination of individual oxides and compounds. The hot methods depend upon the reduction of the oxide constituents of the sample by means of carbon or hydrogen at elevated temperatures. With the exception of the recently developed fractional vacuum-fusion method, the hot methods do not identify individual oxides and compounds but yield only a single value representing the sum of the oxygen contents of several or all of the oxide constituents present. With such diversity in the principles and aims of the different groups, it is not surprising that concordance of results by different methods has usually been difficult to obtain. The present cooperative attempt to define more rigorously than has been possible heretofore the accuracy and limits of usefulness of the various methods, originated in correspondence between Dr. John Johnston, Director of Research of the United States Steel Corporation, and other interested metallurgists. The plan was, briefly, to submit identical samples to a number of laboratories for analysis by different methods and to collate the results of these analyses. The project was endorsed by the Iron and Steel Division of the American Institute of Mining and Metallurgical Engineers at the annual meeting in February, 1933, and has been conducted under the joint sponsorship of the Iron and Steel Division and the National Bureau of Standards. The latter organization undertook

Jan 1, 1937

By S. C. Lindsay, D. J. I. Evans

With each year that passes hydrometallurgical processes are being more widely used to recover base metals from ores and concentrates. Generally these processes involve liquid-solid separation of metal-bearing liquors from barren residues. This may be done by countercurrent decantation, thickening and filtration, or filtration or centrifuging only. Choice of method is governed by chemical and physical characteristics of the pulps; cost of labor, power, materials, and waste disposal; and even by the amount of capital available when building plans are under way. Since all these controlling factors change with time and location and with technological advances, the separation method must be re-evaluated when new plants or expansion programs are contemplated. At the Sherritt Gordon refinery in Fort Saskatchewan, Alberta, an ammonia pressure leaching process recovers nickel, copper, and cobalt from the nickel concentrate produced at Lynn Lake, Manitoba.' Pregnant liquors are separated from the barren leach residues in a thickener-filter liquid-solids circuit. The decision to use this type of separation was based on a summation of economic factors during the pilot plant and design stages. Although countercurrent decantation was not incorporated in the refinery flowsheet, the problems solved in thickening the leach residues and the experience gained in operating the commercial plant are pertinent to countercurrent decantation, particularly where it is applied to slow-settling leach slurries or slurries having a relatively high vapor pressure of a valuable, obnoxious, or poisonous vapor. The nickel sulfide concentrate is leached under pressure with air and ammonia to dissolve the nickel, copper, and cobalt and most of the sulfur, leaving a residue of iron and siliceous material to be discarded.2,3 During a subsequent distillation stage to recirculate part of the ammonia used for leaching, copper is recovered from the solution as a high-grade sulfide. After further purification to remove traces of copper and undesirable sulfur compounds, the nickel is precipitated by hydrogen under pressure at an elevated temperature. The cobalt, together with unreduced nickel, is precipitated as a mixed metal sulfide by hydrogen sulfide for eventual cobalt recovery. The end solution is then evaporated to produce a crystalline ammonium sulfate byproduct. As shown in Fig. 1, the nickel concentrate is leached in a continuous, two-stage, countercurrent circuit. In the first stage, or adjustment leach, the fresh concentrate is partially leached (60 pct) in the liquor produced in the second stage, or final leach. This system is necessary to produce a solution suitable for treatment in the copper sulfide precipitation step. Both stages are carried out at 170" to 180°F under a total pressure, with air, of 100 to 120 psig in large, horizontal, water-cooled autoclaves. The autoclaves are divided by overflow weirs into four compartments to give a certain amount of staging during leaching. In each compartment a relatively slow-speed (100 to 150 rpm) agitator maintains the nickel concentrate in suspension. Adjustment leaching, carried out in two autoclaves in parallel, is followed by a thickener-filter liquid-solids separation. Final leaching is done in two parallel trains of three autoclaves using aqueous ammonia to extract metal values from the adjustment leach residues. This too is followed by a thickener-filter circuit. Here the residues are repulped once with aqueous ammonia and twice with process water and refiltered after each repulping stage, to insure a maximum recovery of soluble metal, before being discarded to the tailings pond. The adjustment leach is followed by a seven-disk Dorr-Oliver American filter, with an agitator in the filter boot to keep the residues in suspension. Agitators have also been installed beneath the four ten-disk filters following the final leach thickener. Slurry Characteristics: A typical analysis of the Lynn Lake nickel concentrate, produced by differential flotation,' is given in Table I. The concentrate comprises 35 to 49 pct pentlandite, (Fe, Ni)S; 3 to 6 pct chalcopyrite, CuFeS,; 1 to 4 pct pyrite, FeS2; and 24 to 42 pct pyrrhotite, Fe1-2S (where x varies between 0 and 0.2) together with various siliceous minerals such as actinolite, hornblende, and talc. During leaching, the sulfur in the pentlandite, chalcopyrite, and part of the pyrrhotite is successively oxidized through the thiosulfate and poly-thionate radicals to sulfate and sulfamate." Simultaneously the nickel, copper, and cobalt are converted to soluble ammine complexes and the iron in the pentlandite, chalcopyrite, and part of the pyrrhotite is oxidized to a spongy hydrated iron oxide. The hydrated iron oxide is readily broken down by the agitation needed to sustain the concentrate in suspension and to maintain a satisfactory mass transfer of the oxygen from the air to the slurry. Table I shows typical chemical, screen, and

Jan 1, 1961

By R. D. Pehlke, P. D. Goodell, R. W. Dunlap

The rate of dissolution of steel bars in molten pig iron has been measured experimentally in the temperature range 2300° to 2650° F. The rate of solution is shown to be a .function of bath composition, temperature, and stirring. A kinetic model based on carbon diffusion in the liquid phase has been derived to fit the experimental results. THE rate of scrap melting has long been an important variable in steelmaking operations. With the advent of the oxygen steelmaking process and the accompanying shorter heat times, the rate of scrap melting has now become one of the rate-limiting factors in steel production. As observed in commercial practice, the solution rate is influenced by the compositions of liquid and solid, the temperature, agitation, and time. However, no definitive work has been done on the Fe-C system, and there is very little information in the literature regarding the relative effects of these variables in steelmaking systems. A number of questions have been raised in regard to scrap utilization in basic oxygen steelmaking operations. Consideration has been given to the optimum size and shape of scrap, and to the use of preheated scrap as a means for decreasing the pig-iron requirement in oxygen blowing. The determination of an optimum scrap practice for a specific installation depends to a large extent upon the economics of the scrap market and also upon the behavior of scrap in the vessel. The present research was undertaken as a preliminary study in evaluating the behavior of steel in a pig-iron bath under various conditions of temperature, composition, and agitation, as might be encountered in oxygen converter operations or in any steelmaking operation where scrap behavior is an important process variable. Related studies have been carried out on non-ferrous systems. The solution rate of solid aluminum in a molten A1-Si alloy has been studied.' Furthermore, the increasing use of liquid metals has created considerable interest in studies related to dissolution of a solid in a liquid, or mass transfer taking place between a solid interface and a liquid metallic phase.2-10 In an effort to clarify the relative importance of factors influencing the dissolution of scrap in Fe-C alloys, this paper presents the results of a study of the rate of dissolution of a low-carbon steel cylinder in a molten Fe-C bath at various bath compositions, temperatures, and conditions of agitation. An attempt has been made to determine the mechanism of solution, and a model has been derived to fit the experimental results. The rate of heat transfer between the molten pig-iron bath and the solid-steel cylinder has also been studied. EXPERIMENTAL PROCEDURE A molten bath of pig iron (nominal composition 4.2 pct C, 0.5 pct Mn, 0.8 pct Si)* was held in a 200- *In view of the fact that the composition of the pig-iron bath was slowly changing with time because of steel dissolution and reaction with the surrounding atmosphere, intermittent samples of the liquid bath were taken throughout each experiment, Table 1. lb induction melting unit. The internal diameter of the furnace was 8-1/2 in. and the bath depth approximately 14 in. Cold-finished 1020 steel cylinders of 1/2-, 3/4-, 1-, 1-1/2-, and 2-in. diameters were cut into 1 -ft lengths for use as test specimens. One end of each bar was machined to fit a hand-driven, mechanical stirring device which rested on top of the furnace. This fixture permitted 7 to 8 in. of the bar to be immersed in the melt. The steel cylinders were cleaned to free the surface of grease and oxide. The rods, at ambient temperature, were immersed into the molten pig-iron bath. The melt temperatures studied in this investigation were 2300°, 2500°, and 2650°F. Different agitation conditions were achieved by operating with a) the power to the furnace, giving induction stirring; b) induction stirring plus mechanical stirring, using hand rotation with a chain and sprocket assembly at approximately 200 rpm; c) mechanical stirring alone with the power off; and d) the power off and no mechanical stirring resulting in minimum agitation, i.e., only that caused by natural convection currents in the bath. The samples were immersed in the melt for prescribed times ranging from 30 sec up to 6 min. Immersion times were measured with a stopwatch and temperature control of the melt was achieved by power adjustment following temperature measurement with an optical pyrometer. The measurements with the calibrated pyrometer were checked out to within less than 10°F with simultaneous thermocouple measurements. Following immersion, the bars were water-quenched and the diameters were measured with a micrometer at several positions on the reduced area, and by volumetric displacement. The dissolution rates calculated from the

Jan 1, 1965

By A. A. Burr, D. G. Ebeling

The effects of casting texture, grain orientation and grain size upon the performance of Alnico permanent magnets is described. Single-crystal specimens were produced by special sintering and grain coarsening techniques to study the effect of crystal orientation. In addition to texture and orientation effects, an analysis of the results indicates that the permanent magnet performance is impaired by a refinement of the grain size. AN excellent historical review of the development of Alnico permanent magnets has been prepared by Bozorth.1 The desirable permanent magnet characteristics of Fe-Ni-A1 alloys were discovered in 1932 by Mishima.2,3 The work of Ruder' showed that the alloys were age-hardenable, and Betteridge5 defined the best composition and heat treatment for the magnetically isotropic alloy known as "Alnico 3." Horsburgh and Tetley0 increased the energy product by the addition of cobalt and copper, "Alnico 2," and Oliver and Sheddon7 demonstrated that cooling in a magnetic field improved the residual induction of this alloy. Jonas8,9 then disclosed the great practical benefits of heat treating an alloy of higher cobalt content in a magnetic field and the resulting alloy, "Alnico 5," has become the standard of the industry. This paper describes the fundamental aspects of a procedure which can be used to further improve the properties of these anisotropic permanent magnet alloys. A study of the casting techniques used in the production of anisotropic Alnico permanent magnets indicated that the magnetic quality was affected by the as-cast macrostructure. Improved performance was observed in magnets containing a high percentage of columnar grains whose long axes were parallel to the magnetic axis of the casting. McCaig10 studied the effect of such columnar grain structures upon the magnetostriction characteristics of similar alloys, however no data was presented showing the effects on other magnetic properties. The following paragraphs describe two experiments which were conducted to determine the effect of various grain orientations upon the energy product. Special composite molds were prepared of highly conductive and highly refractive components to remove the heat of solidification from the casting in a controlled manner. Representative macrostructures produced by these techniques are shown in Fig. 1, along with the relative volumes of favorably oriented columnar grains. The alloy, Alnico 5, has the highest permanent magnet performance of any commercial magnet material. It has the nominal weight composition of 8 pct Al, 14 pct Ni, 24 pct Co, 3 pct Cu, and 51 pct Fe. A heat of this material was cast into molds producing the type A and B grain structures shown in Fig. 1 and pairs of the resulting magnets were placed in heat-treating boats so as to eliminate any biasing effects of boat position. After a standard heat treatment the type A magnets, with 16 pct of the volume composed of favorably aligned grains, had a maximum energy value of 3,940,000 gauss-oersteds, while the type B magnets with 73 pct aligned grains averaged 5,090,000. This large im-

Jan 1, 1954