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By Nicholas J. Grant, Italo S. Servi

SPECIAL polishing and etching techniques were developed during an investigation of the high temperature mechanical properties of high purity aluminum (99.995 pct Al).* Electrolytic polishing was done successfully in the following electrolyte: 5 ml perchloric acid (72 pct), and 95 ml glacial acetic acid. No special precautions need be taken during the preparation of the electrolyte since no appreciable heat of mixing is evolved. Although the electrolyte is not an explosive, it is recommended that Jacquet's safety rules' be followed during the polishing operation. A voltage of 25 to 60 v gives a good polish in about 2 min at room temperature after preparation on 3/0 metallographic paper. Most of the grain boundaries are visible under the microscope after polishing. Since the current is controlled essentially by the resistance of the bath, it is necessary to keep the anode-to-cathode distance as constant as possible. Accordingly, polishing of irregularly shaped pieces will be difficult. A cooling bath and a stirring system are advisable in order to keep the temperature of the bath uniform and constant. Coarse-grained samples can be macroetched in a few seconds by lowering the voltage below 10 v. This is done after electrolytic polishing, without removing the sample from the bath, Fig. 1. The specimen can be repolished in less than 1 min by raising the voltage above 25 v. The "galvanic etching" technique, which has been described elsewhere,' was found to be helpful not only for macroetching, but also for microetching coarse-grained specimens. In fact, the different orientations of adjacent grains provide good contrast at the grain boundaries, when the sample is observed under polarized light. If the specimen is only partially etched, Fig. 2a, the grain boundaries can be located without completely destroying the appearance of the surface of the specimen. The unetched surface appears black under polarized light. Excellent color contrast is obtained by using a "sensitive tint" plate in the optical system of the microscope. In this case, the unetched surface has a magenta color, while the etched part of the sample assumes different colors varying from green to brown, according to the orientation of the grains. Etch pits were produced on high purity aluminum by using the technique suggested by Lacombe and Beaujard." Good results also were obtained by substituting 70 pct nitric acid for the fuming nitric acid recommended. This gave an etching reagent of the following composition: 70 ml nitric acid (70 pct), 50 ml hydrochloric acid (37.5 pct), and 3 ml hydrofluoric acid (48 pct). An example of the results is shown in Fig- 2b. The outline of the etch pits is revealed sharply if the specimen is observed under polarized light, as shown in Fig. 2c. These metallographic techniques are not suitable for the examination of commercially pure (2s) aluminum. References 'P. A. Jacquet: Metal Finishing (Nov. 1949) 47, p. 62. 21. S. Servi: Metal Progress (1950) 58, p. 732. 3 P. Lacombe and L. Beaujard: Journal Inst. of Metals (1947) 74, p. 1._________________________

Jan 1, 1952

By P. D. Merica

IN connection with other investigations on the properties and characteristics of chilled iron car wheels, the question as to the best range of annealing temperatures was raised. Chilled-iron wheels are cast with a chill against the tread and the inside of the flange, the remainder being in sand. The composition of the metal is so chosen that under these conditions the tread and inside of the flange will show white iron to a depth of from 5/8 to 7/8 in. (15 to 22 mm.), the remainder of the wheel becoming graphitized or gray. In order to relieve the stresses set up during cooling under such drastic conditions, the wheels are stripped from the mold, while still red hot, piled in a soaking pit, and allowed to cool very slowly from their temperature at stripping. Obviously the most suitable temperature for this annealing is the highest at which no formation of graphite occurs within the white tread and at which the wheels can be stripped from the molds. Inasmuch as no direct determinations have been made of the temperatures at which the' formation, of graphite takes place in white iron of compositions used in car wheels upon annealing, it was considered worth while to determine these temperatures as a means of establishing the maximum temperatures at which the annealing of the wheels may be carried out. In the course of this work, some incidental observations were made which are of interest in connection with the theory of graphitization in white iron. The literature on the subject of the formation of graphite both during cooling at casting and upon annealing is very extensive and can be best studied by reference to a comprehensive discussion of the subject by Hatfield. 1 Perhaps the most important contributions of previous investigation are the following: 1. Whether a given mass of molten iron becomes white, mottled, or gray upon casting, depends on its composition and its rate of cooling through the temperature range of solidification and immediately below.

Jan 7, 1919

By L. D. Jaffe, D. C. Buffum, F. L. Carr, M. Goldman

IN an earlier investigation by Jaffe and Buffum,' a time-temperature transformation diagram for isothermal temper embrittlement of an SAE 3140 steel showed some suggestion of two overlapping "noses." These authors mentioned, as a possible explanation, that their specimens embrittled at 525°C were slightly softer than expected, perhaps because of some slight unknown variation in tempering treatment. Because a double nose would be of considerable importance in elucidating the mechanism of the temper brittleness reaction,' it appeared worthwhile to redetermine the portion of the diagram near 525°C. The same heat of SAE 3140 steel was used as in the previous work, and experimental procedures were the same.' Blanks were austenitized 1 hr at 900°C, water-quenched, tempered 1 hr at 675°C, and water-quenched. Groups were then embrittled isothermally at the temperatures and for the times shown in Table I, and water-quenched. For comparison, one series was tempered various times at 675°C, water-quenched, and given no further treatment. V-notched Charpy impact specimens machined from the blanks were tested over a range of temperatures. Energy absorption and percentage of fibrous fracture were plotted vs test temperature for each group, utilizing both the new data and those for the same treatment obtained in the earlier work,' except that the earlier data at 525°C were discarded.* are given in Table I. After a small correction (-0.28°C/BHN) for the variation of hardness" from Rockwell C24, the transition temperatures were plotted against embrittling time for each embrittling temperature, using the data of Table I for the range of treatments covered there, and using previous dataL for other treatments. By cross-plotting, Fig. 1 was finally obtained. It appears from this figure that if there are two noses to the time-temperature-transformation diagram for isothermal temper embrittlement of SAE 3140 steel, the upper nose must lie above 575°C. As interest had been primarily in the region near 525°C, a thorough study of embrittlement above 575°C was not made. Fig. 1 shows that such a study is needed, especially since preliminary measurements at the tempering temperature of 675°C reveal much more rapid embrittlement than would be expected from the data at lower temperatures. The transition temperature increased, approximately, as the logarithm of the tempering time (about 81/2°C, after correction for hardness, for each doubling of the time).& Since three tensile specimens tempered 240 hr at 675°C and water-quenched had an average yield-tensile ratio of 0.844, with 70.7 pct reduction of area, it is assumed1 that the tempering temperature is not above Ae1. The omission of a quench-and-reheat operation below Ae1, for the groups tempered at 675°C, as compared to groups embrittled at lower temperatures, should not affect results." More detailed investigation of embrittlement above 575°C is now under way.

Jan 1, 1954

By AIME AIME

WEST TEXAS, New Mexico and Northern Mexico form one of the most interesting regions in America for geologists and mining men and are full of points of historical and human interest for others. Including as the region does, a representative portion of the high plateau of Mexico, the front range of the Rocky Mountains and the great down-dropping plains of Texas, there is variety as well as interest in the geological and mining problems there to be studied. Gold and silver mining were the pioneer industries and are yet of high rank in importance. Among the papers to be presented at the El Paso meeting of the Institute this month will be two dealing with silver mining and ore treatment at the Shafter mine in Texas, that most un- usual property which has for so many years been the largest mining enterprise in its region. West Texas is now better known for its petroleum and gas, and in another paper will be described the problems involved in uding natural gas for smelting at the well-known El Paso smelter of the American Smelting and Refining Co. In still other papers, presented at the session sponsored by the West Texas Geological Society and cooperating organizations, the general geology of the region, the potash and the sulfur deposits will be de- scribed. At El Paso the refineries of the great com- panics will be available for visits.

Jan 1, 1930

By Frank V. Hicks

THE following paper-in no sense a technical paper-is a summary of a safety campaign instituted by a coal-mining company to improve an unfortunate safety record. The experience should be suggestive equally to coal and metal-mining companies. With few precedents to follow in the beginning, the course was charted by trial and error. The endeavor, often disheartening, finally resulted in the capture of the most coveted safety trophy in the mining industry, "The Sentinels of Safety," awarded by the Hercules Powder Co. of Wilmington, Del., through the U. S. Bureau of Mines. The period described covers the 10-year interval, 1924 to 1933, the year 1933 being that for which the award was made. The coal company considered has produced annually for a number of years an average of 2,750,000 tons of coal, employing at various times from 1.800 to 3000 men. Prior to 1924, the

Jan 1, 1935

By Oswald J. Heinrich

The responsibility resting upon the owners and managers of mines where fire-damp is generated, renders it a matter of imperative duty that a frill and correct statement of any explosion that occurs should be given to the public. But such a statement must be based on the testimony of impartial eye-witnesses or trained experts. Then a sad experience may result in the adoption of effective preventive measures. In the absence of any official and professional body of mining experts in the State of Virginia, the writer desires to submit to his professional brethren of the American Institute of Mining Engineers an account of an explosion which recently took place in a colliery under his management, and earnestly desires a thorough and impartial discussion on the Fats submitted. Description and Plan of the Mine.—The "Grove" shaft is situated at the nearest point 825 feet from the last old workings upon the Midlothian property, south of the old Pump shaft works. (See Plate 111.) The shaft was sunk by the former company, some thirty years ago, to the depth of 622 feet. An incline over 230 feet long, starting in a northwest direction at a depth of 105 feet above the shaft bottom, had been driven to explore the coal on the dip. A return of very small dimensions had been driven round the shaft on the south side, entering the upcast chamber. With the information obtained from the former company that a seam of coal about four feet thick, at a depth of 490 feet, had been found, and with the information obtained by the present proprietor, R. T. Burrows, of Albion, N. Y., by means of two boreholes on the dip west of the old shaft, in both of which workable seams of coal at various depths had been ascertained, the clearing out and thorough retimbering of this shaft were commenced in March, 1873. Borehole No. 1, at a depth of 4773 feet from surface, revealed a seam of coal. This borehole was afterwards carried to a depth of 1140 feet to the granite, without finding any other seam of coal. Borehole No. 3, at a depth of 608 feet, revealed the first coal-seam, 14 1/2 feet thick; at 633 feet, the second, 12 feet thick; at 662 feet the third, 1 foot thick, and at 692 feet the fourth, 43 to 5 feet thick. The borehole was stopped at a depth of 715 1/2 feet.

By E. M. Murphy

Eight years ago the Hecla mine, a lead-silver producer, situated at Burke, Idaho, was producing ore from but two levels, the 300- and the 600-ft. All hoisting was done with a 12- by 16-in. slide-valve, double-reel, hoist. The hoist was being worked to its capacity and was unsuitable for hoisting from greater depths. As the work of opening a new level was about to be started, it became necessary to remodel the then-existing equipment or install a new hoist. The recent advent of electricity from Spokane had made available a cheaper power than steam. By a series of tests conducted throughout the Cæaur d'A1ene district, it was found that it cost $109 per year to generate a horse-power with steam. Electric power was to be had for $50 a horse-power per year. It was decided to substitute for the engines a motor-drive, of sufficient capacity to operate from the 900-ft. level, and ultimately install an entirely new hoist. After disconnecting the engines, installing a new shaft, and making a few minor changes, a 300-h-p., 2,300-volt, 514-rev. per min., variable-speed motor of the induction type was geared to the reel-shaft. The reels were supplied with 3/8- by 4-in. flat rope, and the duty of the hoist was about as follows: Cage, 1,700; ore, 2,600; car, 1,400; rope, 2,250; total, 7,950 pounds. The Bristol ammeter chart, Fig. 1, shows the combined current-consumption of the hoist- and mine-motors. The large intermittent load is clearly shown; this produced harmful fluctuations in the voltage of the long, lightly-loaded, 60,000-volt transmission-line from Spokane to the Cæmur d'A1enes. The power company received no compensation for the increased cost of producing power for this intermittent or fluctuating load. In order to protect its system from similar excessive

Jan 1, 1913

By C. H. Herty Jr, C. H.

FEW subjects have attracted the attention of metallurgists more than oxygen in steel. From the days of Mushet and Ledebui interest in this subject has been increasing, and as additional knowledge has become available, the problem has naturally grown more complex. Instead of using the simple term "oxygen" we now distinguish between iron oxide, silicates of various kinds, oxysulfides, oxygen as gas and oxygen in solid solution in steel. There are five general methods for determining oxides in steel: hydrogen reduction; vacuum fusion; various wet-extraction methods, including electrolytic methods; methods depending on volatilization of the iron away from the oxides; and metallographic methods. For oxygen in solid steel each of these methods has both advantages and disadvantages. The hydrogen-reduction method is of no use on steels above about 0.20 per cent. carbon; 1 furthermore, it gives only FeO and possibly some MnO. The vacuum-fusion method2 is expensive and gives total oxygen, with the exception of some A1203, and does not differentiate between the various oxides in which the oxygen exists. Most of the wet-extraction methods3 give only the more insoluble oxides SiO2 and A1203, though the iodine method gives MnO to an uncertain degree (information that may be more misleading then no information

Jan 1, 1957

By Franklin H. Wilson

COPPER base alloys containing various amounts of aluminum and silicon are of considerable commercial interest. In particular the alloy containing 7 pct aluminum and 2 pct silicon shows an attractive combination of high strength with excellent machinability. Since there is no evidence in the literature that this ternary system has been studied since the recognition by Smith1 and Anderson2 in 1939 of the kappa phase of the binary copper-silicon system, the determination of the equilibrium phase relationships in the copper corner of the ternary diagram has been undertaken to provide a fundamental basis for understanding the behavior of these alloys. Phase boundaries have been determined by the micrographic examination of quenched samples while points on the liquidus surface have been obtained by thermal analysis. The results, of sufficient precision to serve their major purpose of providing a guide for the control of the manufacture of alloys in the region covered, are presented in a series of both isothermal and vertical sections of the diagram. ALLOYS STUDIED For a rough survey of the copper corner of this ternary system the compositions listed in Table I (Series A) were employed. The results of examinations of these alloys indicated that the compositions listed in Table 2 (Series B) would further clarify regions of greater complexity. All alloys were prepared as 1200 g heats, the copper being melted under charcoal, and then first silicon and then aluminum were added. An [ ] excess of 0.05 pct silicon was allowed to cover deoxidation losses. Two small bars 5/8 by 1 ¼ by 1 ¼ in. were cast using Durville type casting equipment. Analyses were made on all alloys using material which was hot-rolled at 800 or 850°C and annealed 17 hr at 650°C. All analyses were found to be within 0.05 pct of the nominal composition. Since the precision of analysis is not much better than this, the points of both isothermal sections and vertical sections at fixed aluminum and silicon contents have been plotted at the compositions indicated by the nominal composition.

Jan 1, 1948

By W. Armstrong Price

INVESTIGATION by German chemists during the World War showed that particles of iron oxide form rapidly in iron pipes carrying hydrogen gas under pressure when the gas contains small amounts of water. Under these conditions, the gas frequently exploded when expanding into a dirigible. The explanation of the explosions lies in the building up of a charge of static electricity in the flow just beyond the orifice and the ignition of the gas by a spark accompanying discharge of the electricity. Friction between the moving particles and the pipe generated the electric charge, which was manifested by a pale blue glow formed in the flow at pressures above two atmospheres. In one experiment, this glow, at eighty atmospheres, extended for a distance of forty to fifty centimetres, but did not ignite hydrogen and air mixtures until the charge was col-lected by a conductor and discharged across a gap between electrodes placed at the side of the column of gas. Autoignition did not occur when this discharge was effected at a distance from the gas column, nor if the gas used was thoroughly dried and free from impurities. The electric charge has been studied by placing various wire and screen conductors in the outcoming stream of gas, Guest having summarized these experiments. The application of these conclusions to fires in petroleum and natural gas issuing uncontrolled from wells is made in the following paper, citing the ignition of a wild gas well in Texas.

Jan 1, 1936

YEAR OF r ELECTION 1913 FRANK DAWSON ADAMS Montreal, Canada 1921. WILLIAM CUTHBERT BLACKETT Sacriston, Durham, England 1923 GELASIO CAETANI Washington, D C 1920. HENRY STUROIS DRINKER Menon Station, Pa 1921. FERDINAND FOCH . Pans, France 1922. FEDERICO GIOLITTI Torino, Italy 1888. HATON DE LA GOUPILLIERE Paris, France. 1906. SIR ROBERT A. HADFIELD London, England 1921. FRANK WILLIAM HARBORD London, England 1921. HEINRICH O HOFMAN Cambridge, Mass 1917. HERBERT HOOVER .. Washington, D C. 1915 JAMES FURMAN KEMP New York, N. Y 1905. HENRI LECHATELIER Paris, France 1921. C. McDERMID London, England 1913 EZEQUIEL ORDONEZ Mexico City, Mexico 1909 ALEXANDRE POURCEL Paris, France 1911 ROBERT H RICHARDS Cambridge, Mass 1907. CHARLES D WALCOTT Washington, D C

Jan 1, 1923

By H. M. Crankshaw

THE early methods of mining anthracite in the steep pitching Mammoth bed consisted in driving breasts up the pitch from the gangways and airways driven in the bed along the strike (Plate 2, Fig. 1). Breasts are simply rooms driven up the pitch the full thickness of the bed (Plate 2, Fig. 2), having a width of from 18 to 30 ft., and a manway or traveling way on one or both sides. (For detail of breast method see Whildin, Trans., vol. 50, p. 704). Many difficulties were encountered, and the maintenance cost of the timbered gangways was so great as to be practically prohibitive. To reduce this .expense, the gangways were driven in the thin Skidmore bed underlying the Mammoth, and the coal mined through rock holes. (Plate 2, Fig. 2;-A.) It was found that after the breasts were driven up 80 to 100 ft., the coal almost invariably rushed or "ran away," making good ventilation almost impossible and the extraction of coal from the upper portion of the lift very difficult. The economic length of a lift is from 200 to 250 ft., and the percentage of extraction by the old method above mentioned was often under 50 per cent., while the coal recovered was so badly broken up as to reduce materially the percentage of large sizes.

Jan 7, 1916

By Ali M. Heidarieh Zadeh, Raghu N. Singh

The paper presents a stability investigation of shaft intersections and pit bottom roadways in the vicinity of upcast and downcast shafts at a colliery in the U.K. Aschemeof instrumentation was aimed at monitoring the strata displacement surrounding the pit bottom roadways and shaft intersections with a view to ascertaining the origin of the strata movement and effectiveness of the control measures. The bore- hole instrumentation results together with a theoretical analysis suggested that the cause of instability could be attributed to the drivage of a roadway within the shaft pillar. A semi-empirical technique was used to calculate the amount of support resistance required to reinforce the pillar to take additional abutment load. A rock bolting system was designed to provide a required increase in thrust capacity of the roadway support. The results indicated that roadway closure was effectively controlled after installation of bolts indicating efficacy of the control measures adopted.

Jan 1, 1982

Jan 1, 1897

By H. E. Powell, A. A. Cochran, R. E. Coleman

Infrared spectroscopy, employing the internal reflection method in conjunction with solvent extraction techniques, was used to study surface reactions between aqueous potassium ethyl xanthate and both sphalerite and precipitated zinc sulfide, each activated with aqueous copper sulfate. It was determined that reactions occurring on the sphalerite and zinc sulfide surfaces produce the reaction products ethyl dixanthogen and cuprous ethyl xanthate, some of which are adsorbed on the mineral surfaces. As the pH of the xanthate solution increased from 5.6 to 11.0, the amount of cuprous ethyl xanthate on powdered sphalerite surfaces decreased and the amount of ethyl dixanthogen first increased and then decreased. It is generally accepted that the collector potassium ethyl xanthate will not float the mineral sphalerite (ZnS). However, Gaudin1 showed that sphalerite readily floats if activated with certain metal cations before exposure to the xanthate. Copper sulfate (CuSO4) was found to be the best activator for sphalerite. The over-all flotation reagent reaction, as given by Gaudin,3 is as follows: While this is the over-all reaction, the exact mechanism of the reaction and the intermediate compounds that may be formed are not yet known with certainty. Important work has been done in Russia by Plaksin

Jan 1, 1968

By Stuart Croasdale

Not long ago I was called upon to conduct some experiments on the treatment of ores from the New Cornelia copper mine, Ajo mountains, Arizona, for the Calumet & Arizona Copper Co. The problem was a very interesting one and contained some unusual features. Incidental with this problem was the utilization of a large amount of low-grade pyrite in the Bisbee mines of the company, provided this could be accomplished by any feasible method. The New Cornelia mine is situated 45 miles south of Gila Bend, the nearest railroad point, on the Southern Pacific Railroad. It is about 160 miles, almost due west, from Tucson. This section is one of the most arid in the United States. The normal annual precipitation, as given by the United States Weather Bureau covering a period from 1870 to 1901, is 3 to 5 in. During June and July, 1913, the records kept by the company gave the following results. These are all I have available, but they show the enormous evaporation that can be expected, which may be a factor in leaching operations on a large scale. Temperature, Degrees F. High Low Average June...................... 112 62 84.0 ' July...................... 115 71 87.8 Evaporation June July Concrete tank, inches............ 11.7 10.72 Iron tank, inches.............. 14.8 13.07 Rainfall, inches................ None 0.77 Cloudy days................... None 10.00 Aside from several springs about 10 miles from the property, the nearest known water in quantity at the time these experiments were made was the Gila river at Gila Bend, 45 miles distant. Part of the developinent of the property of course included drilling for water in the valley, which was in progress at the conclusion of my experiments. The ore deposit itself is unusual. It consists of of intrusive plug of monzonite or granite porphyry. Chalcopyrite, bornite, and magnetite are finely disseminated throughout the magma in sufficient quantities to make the greater part of the mass commercial ore to a certain depth.

Jan 1, 1915

By Noel S. Christensen

COBALT is a silvery white metal with a slight bluish cast, strongly resembling nickel in its appearance and properties, notably its resistance to corrosion, although its alloys with other metals differ quite decidedly in their properties from those of nickel. The name cobalt was derived from the German "Kobold" meaning goblin and this came to be applied to the cobalt minerals which, although they resembled ores, did not readily yield metal when smelted by the primitive processes available in the Middle Ages. Cobalt minerals were used as pigments by potters and glass workers before the Christian era. Cobalt blue glass was found in the tombs of the Egyptians and in the ruins of Troy, and many colors used by the ancient Greeks and Romans contained cobalt. The ancients were entirely unaware that the colors they used were caused by cobalt and the metal itself was only isolated about the middle of the eighteenth century by Brandt although the preparation of cobalt compounds had been carried on in a small way ever since the opening of the silver-cobalt deposits at Schneeberg, Germany, in 1470. The metal is fairly hard, with a density when pure of 8.81 in the cast state and 8.92 after working. The commercial grade of cobalt has a density of about 8.75 in the cast state. The atomic weight is 58.97. The Brinell hardness of the pure metal is 124; that of the commercial grade varies from as low as 100 to as high as 138, depend¬ing upon the impurities present. Pure cobalt has a sharp melting point at 1478°C. The tensile strength of the pure metal in the cast condition is said to be higher than that of any other pure metal. Kalmus gives it as 34,400 lb. per sq. in. for cast unannealed metal; the effect of annealing at 850 to 900°C. is to raise the strength slightly. The yield point is close to the ultimate strength and the reduction in area and elongation are both low. Mechanical working raises the tensile strength of pure cobalt rapidly and in the form of wire it will be over 100,000 lb. per sq. in. The presence of small quantities of carbon in the commercial metal raises the tensile strength to as high as 61,000 lb. per sq. in., the reduction in area and elongation being raised at the same time to approximately 20 per cent.

Jan 1, 1933

By Stanley F. French, Bruno F. Koch

Although the amount of dust that will be actually recovered in the six main dust-control systems cannot be accurately stated until the tests mentioned previously are carried out, it is estimated that the average air entering the wet collectors will contain around 5 grains of dust particles per cubic foot. This means that the six systems handling a total of about 133,000 cu.ft. of air per minute will return about 68 1/2 tons of dust to the concentrator per day and since the copper in this dust will average around 2 per cent, the total recovery is approximately 1.37 tons of copper every 24 hours. This important copper recovery is not due entirely to the dust-control system since in a plant without control only the duct that is dispersed to the atmosphere represents a loss. A conservative estimate of the recovery of copper solely due to the dust control system would be about half of the total or approximately 0.70 tons of copper per day.

Jan 1, 1942

By Arthur E. Hall

Tax operation of "softening" in lead refining is designed, as the word implies, to separate from the bulk of the lead the elements that tend to make lead hard. These elements, which invariably are present in argentiferous lead, interfere with the desilverization, and must be almost entirely absent in refined desilverized lead. They are mainly copper, antimony, arsenic and tin. The properties utilized in accomplishing this separation are the low solubility of copper or copper sulphide in lead at its freezing-point temperature, and the greater and selective affinity for oxygen of the other elements at temperatures of the order of 700° to 900' C., or, in the prcsence of sufficient, alkali, at a temperature of about 500' C. The major problems of softening lead bullion lie in the necessary subsequent treatment of the by-products of the primary operation, which contain, either chemically or mechanically, lead or reagents that must be isolated for market or re-use. Therefore an important objective of the primary operation must be the highest practicable concentration of these elements in the by-products. Within the past three decades, during which the writer has been engaged in lead refining, the technique of softening lead bullion has had as many variations as there were lead refineries. This was the result of the variation in composition and character of lead bullion recived. The writer has received for refining shipments of lead bullion varying as widely as indicated by the following table: Sb, Per CEnt As. Per Cent Sn, Per Cent Cu. Per Cent Ag. Oz. per Ton 1.00 0.05 nil 0.05 70 0.50 2.50 2.00 0.50 200 3.50 0.50 nil 0.30 350 At times these have been received uniformly and at other times irregularly with a variation from week to week as wide as those shown. Under such conditions, establishment of a universal softening technique presented many problems. Such variations existed because refinery tolls too often were based on a ton of bullion, whatever its composition, and

Jan 1, 1937

By F. V. Lenel, G. S. Ansell, M. J. Salkind

An experiment is described in which the growth of interparticle necks in an array of loose spherical silver powder at temperatures near 300°C was determined by measuring changes in the electrical resistance of the array. The activation energy for neck growth of contacts was derived by abruptly changing temperature and noting the change in the rate of neck growth. Since the experiments were run under an external load, the changes in activation energy with stress could he determined. The activation energy was found to decrease rapidly with increasing stress. It is concluded that the material transport in the experiments is one of plastic flow by dislocation motion. The variation of activation energy with stress is typical for cross slip of dislocations, an important material transport mechanism in the temperature range investigated. THE process in which powder compacts or aggregates of loose powder are held at an elevated temperature under an external load is called hot pressing or sintering under pressure by powder metallurgists. In this investigation the early stages of this process as applied to loose spherical silver- powder aggregates were studied. The powder particles were approximately 100µ in diameter and the temperature was near 300°C, i.e., below one half of the melting point of silver in degrees Kelvin, where volume diffusion is not expected to contribute to sintering. In the process, the contact or neck areas between powder particles grow. Since this involves plastic deformation of the particles under a constant external load (even though not under constant stress) it would be termed creep by mechanical metallurgists. On the other hand, the growth in neck area observed in compacts or loose-powder aggregates held at elevated temperature without the application of an external load is termed sintering by powder metallurgists. During sintering the major driving force is the stress due to surface tension. However, even when no load is placed on the compact or powder aggregate, an external stress, i.e., gravity, plays an important role in sintering in addition to those stresses arising from surface tension, as was shown in two previous investigations.'" It is therefore postulated that no sharp dividing line can be drawn between the phenomena of "creep" and "sintering". Different material transport mechanisms may be involved in either of these phenomena, but they will depend upon the temperature and the level of stress, but not necessarily upon the nature of the driving force: surface tension or external load. At the low temperatures of this investigation, an external stress much higher than the stress due to surface tension is necessary to obtain measurable rates of neck growth. In order to avoid misunderstanding this phenomenon will be called "creep". The rate of growth in contact area in the loose silver-powder aggregates was determined by meas-

Jan 1, 1965