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GENERAL Broken Hill lies at latitude 31º58'S longitude 141º27'E on the semi-arid western plains of New South Wales. From discovery in 1883 until the end of 1969 the lead-silver-zinc orebody has yielded 107,570,000 tons of ore for an overall grade of 13.1% Pb, 6.9 oz Ag/ton and 9.4% Zn.* The orebody currently supports the activities of four mines which are, from north to south, North Broken Hill Limited, Broken Hill South Limited, The Zinc Corporation, Limited and New Broken Hill Consolidated Limited. It is estimated that in 1969 these mines produced about 8 ½ % of world lead production and about 6% of world zinc production. In 1905 The Zinc Corporation, Limited was founded to recover zinc from tailings dumps and moved into mining in 1911 on leases purchased from Broken Hill South Limited at the then southern extremity of the "line of lode". New Broken Hill Consolidated Limited was formed in 1936 to explore and mine for deep ore in the leases to the south of The Zinc Corporation which were purchased from Barrier South Limited. The Zinc Corporation, Limited and New Broken Hill Consolidated Limited mines are both managed by Conzinc Riotinto of Australia Limited, which wholly owns The Zinc Corporation, Limited and has a 32% interest in New Broken Hill Consolidated Limited. * Throughout this paper tons referred to are long tons of 2,240 lbs.

Jan 1, 1970

By J. R. Hassemer, T. T. Chao, University of Georgia, K. C. Watts, R. F. Sanzolone

Secondary oxides of Fe-Mn have been used in mineral exploration from the time gossans were first recognized Since gossans are conspicuous features and are largely explored, it is necessary to look for more subtle indication of blind mineralization. Sampling materials used in these geochemical studies consist of secondary Fe-Mn oxide-rich products of hydrothermal mineralization, and "in situ" weathering found in fracture fillings-as selvages along joints and disseminations in host rock. These materials were selectively collected and studied in the Silver City mining region. Two independent sampling methods were compared. The difference in the sampling methods was mainly in the ways samples were obtained and processed. One method involved systematic sampling of fracture fillings and coatings from which secondary Fe and Mn oxides and associated trace elements were then selectively extracted by chemical methods. The second approach involved collection of composite stream sediments and physical extraction of Fe-Mn oxide materials by gold panning, bromoform concentration, and electromagnetic separation. The source of the Fe-Mn-rich materials in the stream sediments is considered to be fracture fillings and coatings that mechanically entered the drainage basins. Map distributions of the two-sample types were compared. Both methods showed generally supportive patterns of anomalous metal dispersion, although anomaly-to-background contrast seems better in joint coatings. Both were useful in distinguishing geochemical differences between mining districts in the region. For example, the Pinos Altos district may contain more hydrothermally-introduced iron than the Central district, whereas the Central district has lead and zinc enrichments that are less on the amount of iron enrichment than is the case in the Pinos Altos district. The methods were qualitatively compared relative to time, expense, and other advantages and disadvantages.

Jan 1, 1984

By John Garcia

IN some districts of the bituminous coal field the problem of construct-ing bulkheads to seal off water under pressure is becoming increasingly important. Recently this matter has been brought very much to the front by the loss of a large Illinois mine due to failure of a bulkhead that separated it from several old, flooded mines. As this great misfortune has provoked much inquiry about proper bulkhead design, it-is felt that a description, of the successful and extensive water-sealing practice at three mines that have different natural conditions will be of considerable interest to those connected with properties having a present or future water problem and to engineers that may have to design safe bulkheads of economical construction. These three mines are the Saxton and Dresser, near Terre Haute, Ind., and the Hegeler, near Danville, Ill. All three have water conditions that make it necessary to regularly seal off all worked-out sections of the mine, and there are considerably over a hundred bulkheads in each. As far as the writers know, these three mines are the only ones in the bitu-minous coal fields of the United States with anything like so large number of water seals and experience, although a number of other mines are known to have a few bulkheads. More detail will be included herein on the Saxton mine than on the others, as the writers are more familiar with it.

Jan 1, 1937

By H. E. Gross

Recently, areas of abnormal rock pressure have been drilled on the Gulf Coast of the United States. These pressures may be caused by the recent and pronounced raising of some of the structures without loss of the formation pressure that existed when the reservoir was developing and the producing sand much more deeply buried. It is possible also that a permeable fissure may connect a shallow accumulation of gas with the gas cap of a much deeper reservoir of oil, gas and water. The pressures are so great that dependence on blowout-prevention equipment alone is hazardous to life and property. Fortunately, wells with excessive casing-head pressures, such as the Stanolind Oates No. 1 of the South Houston field, an 8700-ft. gas well with 6000 Ib. per sq. in., and the near-by Stanolind Candelari No. 1, and 8100-ft. gas well with 5000 Ib. per sq. in., have not blown out and cratered. A case is on record of drill pipe in a well in Harris County, Texas, (Oates No. 1) rotating for 8 hr. through blowout-prevention rams holding a back pressure of 2900 Ib. per sq. in. at the casinghead after the mud was altered by salt-water intrusion. Such conditions warrant the use of extremely heavy muds having low viscosity, made from galena (PbS) or specially prepared mixtures of hematite (Fe²O³) and galena suspended by bentonite. In some Gulf Coast wells, sodium silicate mixed with concentrated brine is used to drill through heaving shale formations. Such a fluid inhibits heaving remarkably, but it is expensive and costs as much as $10 per barrel. Barite has been used to weight this mixture. However, this mineral too rapidly increased an already excessive viscosity and it was thought that galena might be better for weighting such drilling fluid. The operator was anxious to try the latter, but none was available in the district. Laboratory Study of Heavy Muds To foster the use of the plentiful and extremely heavy mineral, galena, research has been done recently at the University of Oklahoma to determine the mud-making properties of this substance. For comparative

Jan 1, 1938

By John C. Calhoun, Raymond G. Loper

Theoretical calculations for the decline of pressure and the variation of instantaneous producing gas-oil ratio with increased cumulative production have been made for reservoir systems under various producing drawdown values and for various spacings. These variables have been included by a modification of previously Published techniques. This consists essentially of utilizing a radial system flowing gas and oil in a succession of steady state calculations. The results of the calculations do not show any variation in the predicted behavior of the internal gas drive reservoir when either the drawdown or the spacing are changed. The prediction of performance on an internal gas drive reservoir has been presented by various authors. ',"' These predictions are in the form of a pressure decline and an instantaneous producing gas-oil ratio as a function of cumulative oil withdrawal. In making these predictions a basic assumption has been that the saturation of the reservoir is uniform throughout at any time, or that the pressure differential imposed on the reservoir system is zero. Because of these assumptions the validity of such predictions has been questioned. Their application to actual systems, where saturations are not uniform and where producing differentials exist, has been a hazardous procedure. The authors cited have used different methods of approach to the derivation of equations for making their predictions and for arriving at a solution of both equations, but basically the same relationships are utilized in each case. In all instances the instantaneous producing gas-oil ratio is calculated from the equation: In utilizing this equation an average reservoir pressure and an average reservoir saturation must be known, the former to define ß, v, s, and uo/ug and the latter to define kg/ko. Predictions can be made, therefore, only for the conditions of a uniform reservoir saturation and a uniform reservoir pressure. This restriction of requiring a uniform oil saturation can be resolved by applying two-phase steady state flow for the radial system to the reservoir's history. Radial steady state flow is defined when the ratio of phases flowing,

Jan 1, 1949

By C. L. Horn

All the tunneling machines discussed in this chapter are Calweld machines. I have divided the machines designed for soft-to-medium formations into three groups, correlated with typical formations and estimated compressive strengths: 1) Running sand and silt requiring blade cutters. 2) Chalk and clay, requiring drag-type cutters, for compressive strengths ranging from 0 to 2000 psi. 3) Sandstones, hard clays, and limestones, requiring disk cutters, for compressive strengths ranging from 2000 to 20,000 psi. All of the soft-to-medium-formation machines are powered by electric hydraulic or diesel hydraulic pumps. The pumps in turn drive hydraulic motors for the torque reaction. The soft-to-medium-formation machines are enclosed in a 360º shield with a cutting shoe, a center portion of the shield housing the mechanical equipment, and a tail shield. Tunnel supports are usually required, and the supports are normally erected in the tail shield. Our first machine was built in 1963, and all but five of the machines illustrated in the figures with this chapter were built in 1966 and 1967. Some of the machines manufactured will be discussed in the following sections; specific features as development has progressed will be pointed out. HARD-ROCK MACHINE The Calweld hard-rock machine has been designed along basic and accepted principles for a hard-rock mechanical borer. The features of this machine are as follows: 1) Direct electric motor drive through a planetary gear reduction ring and pinion gear, and then to the cutting head through a hollow drive shaft.

Jan 1, 1970

By S. Katz, M. E. Nicholson, J. J. Kelly, D. R. Curran

A series of wedges of 1020 steel (2 1/2 by 6 by 8 in.) were explosively loaded, as shown in Fig. 1. A slab of explosive on the surface of the steel wedge was initiated simultaneously along one edge, producing an essentially two-dimensional oblique shock in the metal. Pressure and density in the metal were measured as a function of distance from the explosive-metal interface by a method described elsewhere.' While for pressures below 130 .kbars the technique produces accurate results, for greater pressures the presence of two shock waves in the metalzy3 makes interpretation of the data uncertain. However, the location of the transition in pressure at 130 kbars can be readily identified from the data. The assumption of a single shock in the region above 130 kbars overestimates the pressure computed on a multiple-shock model. After firing, the wedges were sectioned, lapped, and etched with 2 pct Nital. A photograph of an etched specimen is shown in Fig. 2. The specimens were examined metallographically. The dark region, at the top of the specimen, was heavily banded, Fig. 3, while the lighter area was comparatively free from banding, Fig. 4, the boundary between the two regions being quite abrupt. The very light regions at an angle of about 45 deg to the explosive-metal interface show virtually no banding. The origin of these light regions, which are not Luder's bands, is not yet explained. The thickness of the heavily banded area was measured and compared with the pressure at the boundary between the heavily and lightly banded regions. The results of these measurements and calculations are given in Table I. For all shots, the pressure at the boundary is approximately the same

Jan 1, 1960

By L. M. Barker

THE New Cornelia Branch of the Phelps Dodge Corporation is at Ajo, Pima County, Ariz. It is at the southern terminus of the Tucson, Cornelia and Gila Bend Railroad, which connects with the Southern Pacific Railroad at Gila Bend, Ariz., approximately 43 miles to the north. HISTORY Early history of the Ajo district has been related by A. W. Allen1 and by T. A. Rickard.2 Briefly, steps looking to the large-scale development of the ore body were instituted as early as 1912. This work culminated in the equipment of the property for open-pit mining by steam shovels. Ores initially mined carried economic amounts of copper carbonates as the principal copper-bearing mineral. Treatment methods developed for the extraction of the copper content involved leaching and a 5000-ton leaching plant was constructed and placed in operation in early 1917. Description of methods and equipment employed in this plant has been given by A. A. Tobelmann and James A. Potter.3 As exhaustion of the carbonate ore body neared, and mining operations exposed an adequate tonnage of sulphide ores, a 5000-ton concentrator was constructed for their treatment. That plant has been described by H. Kenyon Burch.4 Construction was completed and the plant was placed in operation in early 1924. Changes made in the original plant to improve practices and increase production will be the subject of subsequent paragraphs of this paper.

Jan 1, 1939

By R. Janes, F. Everard

Pilot plant studies have been conducted on a variety of iron ores of differing composition and grain size to test their amenability to dry autogeneous grinding and dry magnetic concentration. A general description of the pilot plant and its equipment is given with particular reference to the Aerofall mill and the dry magnetic separators developed by the Ontario Research Foundation. Test results are reviewed in detail with emphasis on power consumption, mill speed, the use of ball charges, types of ores, moisture content, separator speeds, and design. In 1957 the Ontario Research Foundation installed a pilot plant (Fig. 1) for the study of dry autogenous grinding and dry magnetic concentration of iron ores. A 61/2-ft Aerofall mill was installed as the dry autogenous crushing and grinding medium. The Cavanagh fast drum and the Double Helix, two dry magnetic separators developed at Ontario Research Foundation, were also installed. Iron ore samples of 10 to 150 tons have been investigated. These ores varied widely in mineralogy and grain size. Taconite (-325 mesh), fine-grained magnetite (200 to 325 mesh), and medium-grained magnetites (65 to 150 mesh) have been treated with varying degrees of success. Lately, considerable research has also been conducted on the metamorphosed magnetite-hematite complexes of the Labrador Trough. Operational and metallurgical data have been compiled from these tests. The effects of ore type, air flow, mill speed, and ball charge on mill operation are discussed. Metallurgical data are also presented to illustrate the operation of the dry magnetic separators. PILOT PLANT DESCRIPTION Fig. 2 depicts the normal flowsheet used. Minus 6-in. ore from a vibrating feeder is fed to the 6%-ft Aerofall mill powered by a 50-hp 550-v induction motor. The main blower, a 25-hp 550-v fan rated at 7000 cfm, draws air through the mill. Finely ground ore is conveyed by the air stream to a horizontal classifier, where expansion and a change in direction cause the +I50 mesh fraction to fall onto a vibrating

Jan 1, 1962

By H. S. Martin

THE Phosphate Recovery Corporation operates three flotation plants, Nos. 1 and 2 concentrators about three miles northeast of Mulberry, Florida, and No. 3 plant at Wales, Tennessee. These plants represent the first commercial phosphate flotation operation and are also believed to be the largest nonmetallic flotation operation in the world at the pres-ent time. The details of this paper will be confined to plant No. 2, this being the newest and largest concentrator in Florida, and the flow sheet being practically the same as at plant No. 1. The No. 3 plant has been oper-ated but a short time and has been shut down since December, 1932, on account of the decrease in phosphate rock production. The phosphate washers usually are located centrally on a known deposit so that about two hundred acres of ground can be mined eco-nomically to each washer location. The washers are moved to new areas when the distance becomes too great for economical pumping. The flotation plants are built either adjacent to a washer, so that current debris may be utilized, or on the site of a former washer where there is sufficient accumulated debris available for mining, and the flotation plants must also be moved from time to time. Most of the water used in the Florida flotation plants is recovered after passing through a circulating system where most of the fine sus-pended matter is settled out, but some make-up water is obtained from deep wells near the plant. Power is obtained from the Tampa Electric Co. through the dis-tribution facilities of the International Agricultural Corporation. Flotation concentrate is hauled from the plant by trolley over the International Agricultural Corporation's trolley system, to the drying plant at Prairie, one mile northwest of Mulberry.

Jan 1, 1933

By R. S. Archibald

The subject of this paper is particularly appropriate, since Daniel C. Jackling was active in early exploitation of taconites on the Mesabi Range and contributed greatly to their later economic development. After his success in developing the low grade porphyries in the West he looked for more worlds to conquer, and so undertook the concentration of low grade taconites, from which he hoped to produce commercial ore. Mesabi Iron Co., organized in 1919, actually did produce merchantable sinter from taconites in 1922. The enterprise did not prove commercial at the time, as cost of production was high and the surplus of iron ore in the Lake Superior District already contributed to a low market price, but this same property has since been developed by Reserve Mining Co. The work done by Jackling had much to do with the success of this later venture. Iron ore was first discovered on the Marquette Range in Michigan in 1845. The first ore from this range came from the old Jackson mine in Negaunee in 1848. During these early years this property and others on the Marquette produced limited tonnages for transportation to Lower Lakes and for consumption by charcoal furnaces in the area, where a plentiful supply of hardwoods furnished the charcoal for iron smelting. The Marquette and other ranges tributary to Lake Superior did not produce much ore for transportation to Lower Lakes until the locks at Sault Ste. Marie were constructed, but from the time the first lock at the "Soo" was completed in 1855 these ores were transported through the locks to consumer centers in the East. The Marquette Range has a history of continuous production from 1848 to the present day.

Jan 5, 1959

By D. W. Mitchell

Mine fires are a serious hazard; surveys show that the coal-mining industry lags considerably behind industry in general in planning and training for fighting fires, and providing adequate fire-protection facilities. The results of the experiments discussed in this paper emphasize that every effort must be made to extinguish a fire in its incipient stage. The research also demonstrated that extinguishing agents and techniques, superior to those presently used in most operating mines, are available. An underground coal mine fire, if not extinguished quickly, can develop rapidly, create a serious hazard, and cause loss of life and property. The problem of controlling a fire increases in direct relationship to the time interval necessary to initiate control measures; as the fire increases in size and intensity it becomes progressively more difficult to cope with roof control, visibility, ventilation, and explosion prevention. Despite the constant vigilance of the industry, the number of coal mine fires is increasing. During the eight-year period, July 1952 to July 1960, following enactment of the Federal Coal Mine Safety Act, the Bureau of Mines investigated 401 fires that caused 30 fatalities and 75 injuries. More than half of these fires burned for more than one shift; 20 pct could not be extinguished by direct attack and had to be sealed. Agents and techniques for extinguishing simulated mining-machine and underground coal fires have been investigated in the Bureau's experimental coal mine. The research shows that visibility in the fire area is a primary factor affecting control operations. Associated with good visibility is accessibility to the fire; the closer the attack can be made, the less time and quantity of agent are required for extinguishment. Approach to the fire and visibility are hindered by the smoke and hot gases backing up against the ventilating current. In open entries an increase in air velocity assists in driving smoke ahead; at low airspeeds approach can be made by placing a brattice across the lower two-thirds of the entry, pushing the smoke ahead with water sprays, or discharging rock-dust from a rock-dust distributor. In a dead-end entry, fires can be approached by coursing fresh air along an airtight line brattice. However, it is safer, easier,

Jan 1, 1962

By Eugene A. Stephenson

Critical analyses of the work expended in producing oil by the utilization of gas energy have appeared in the publications of Shaw,' Pierce and LewisI2 and Herold,3 authors who have ably discussed the factors which must be taken into consideration in comparing energy consumed per barrel in various wells which are flowed by means of gas-lift. However, two distinct phases of oil production are concerned with the ratio of gas energy consumed to oil produced. One of these phases is the gas-lift, which utilizes the differential gas pressures for the purpose of flowing oil, whether these pressures be natural reservoir pressures or be induced by artificial compression of gas or air. The other phase has to do with prorating oil production in pools which are operated either as units, or are subject to such restrictions as those imposed at Oklahoma City by the Corporation Commission, or by similar controlling groups in other fields. An abundance of literature is available relative to the problems of flowing wells by gas-lift, but the first suggestion that the energy of the gas within the oil and gas pool might serve as a basis for proration, appeared in the timely article by Mc Williams.4 Much of the dissatisfaction with proration in certain fields arises because some operators feel that besides the hazard to the wells which accompanies the test, the method of allocating production on the basis of the " potential" gage is inequitable and gives some operators a distinct advantage over others.5 The most severe penalty may be exacted from the most progressive operators or those who attempt to produce their oil with a minimum quantity of reservoir gas. If no difficulties ever developed in drilling, shutting off water, or in well completion, it might

Jan 1, 1931

By M. L. Fuller

OWING to the nature of the die-casting process, freshly cast alloys are undoubtedly not at equilibrium from the standpoint of alloy phase relationships. After casting, therefore, they tend to undergo phase changes, with the ultimate effect of reaching a state of equilibrium at the aging temperature, beyond which no further change takes place. This phase alteration undoubtedly is one of the primary causes of the changes in dimensions and physical properties that zinc-alloy die castings undergo during aging. It is planned to report on this problem in a series of papers of which this is the first. The writers have made a study of commercial zinc die-casting alloys over a period of several years, utilizing the X-ray diffraction technic of determining the phase composition changes in the alloys. Up to the present, two principal phase changes have been observed which are capable of causing dimensional changes: (1) the segregation of secondary constituents from the zinc-base solid solution and (2) the beta aluminum-zinc decomposition. The latter is the subject of the present paper and studies on the former will be reported upon at a future time.

Jan 1, 1934

By Cadwallader Evans

THE American Institute of Mining Engineers was organized in the anthracite region of Pennsylvania by men who were primarily interested in anthracite. Its first meeting, at Wilkes-Barre, Pa., in the Northern Anthracite field, on May 16, 1871, resulted from a call sent out by three outstanding men of the anthracite .industry: Eckley B. Coxe, R. P. Rothwell, and Martin Coryell. The best known of these was Eckley B. Coxe, who was the manager of large hold¬ings operated by him and his family,. and who is remembered as the inventor of a special grate for burning very fine anthracite, known as the Coxe traveling grate, which is still very widely used. R. P. Rothwell was a well-known consulting engineer of the region, as was Martin Coryell, who was associated with another well-known anthracite family, the Pardees. There is no record of the discussions that resulted in this initial meeting, but it is safe to assume that the formation of the Institute was largely influenced, through appreciation by the founders, of the necessity for a free exchange of information covering the whole of the mining industry. One of the rules adopted at the first meeting was:

Jan 1, 1947

The opening session was held on Tuesday evening, June 28th. Mr. F. S. Witherbee, of Port Henry, a member of the Local Committee, welcomed the Institute as follows: Mr. President and Gentlemen and (if I my also add) Ladies of the Institute: In the absence of the Chairman of our Local Committee it is my pleasant duty to give you a cordial welcome once more to the shores of Lake Champlain. I think some fourteen years have passed by since we last had the pleasure of receiving you at a meeting in this vicinity ; but the pleasure of that meeting still lingers in our memory; and the profit which we derived from your discussions and from your presence with us has made us heartily desirous to have you here again. If the truth must be known, we were for a time much embarrassed by the difficulty of providing adeqriate and comfortable shelter for the large number of friends whom we hoped (and, as this assembly indicates, had good reason for hoping) to receive. But the liberality and zealous co-operation of the Delaware & Hudson Canal Company and its hotel manager, in offering to open Hotel Champlain, at no little inconvenience, before the usual time, presented a solution of this difficulty, provided the date originally proposed for the meeting could be changed to a week later. This change was duly authorized; .and I think you will all agree with us that it was wise.. At all events, I am sure, I now need offer no apologies for the roof which covers yau. During the fourteen years which have elapsed since your last visit to us, great strides have been made in the industrial development of this country. The meetings of the Institute, held from one end of the land to the other, have permitted you to witness the transformation of small hamlets? like Birmingham, Ala., into populous and thriving industrial centers. You have seen the Minnesota and the

Jan 1, 1893

By H. W. Clark

Electricity must be safeguarded everywhere that it is used. The conditions that exist underground make the use of safeguards more essential there than almost anywhere else. Electric Shock Electric shock is the greatest danger in connection with the use of electricity in mines, because conditions existing underground are so favorable to its occurrence. Men are often obliged to work in more or less uncertain light near bare wires that are carrying dangerous potentials. The fact that the men are standing on the earth practically connects them to one terminal of the electric generator. The moat dangerous piece of electrical equipment underground is the trolley wire. It is necessarily bare and extends for long distances throughout a mine, often less than a man's height from the track rail. Sometimes the making up of trips of cars must be done near low-hanging trolley wires. All 'bare wires offer the same danger that troIley wires do, although not to the same extent. Apparatus that has accidentally come in contact with the ungrounded side of an electric circuit is almost as dangerous as the trolley wire. A severe and even fatal shock may be obtained by coming in contact with the frame of a motor or a switch box that has become charged with electricity, or "alive," as it is usually termed. It is also possible to obtain . shocks from the frames of locomotives and cars if track sanding, poor bonding or a similar cause has put a high resistance to earth in the path of the current. Fires Caused by Electricity The danger from fires caused by electricity arises principally from defective installation and careless upkeep or from injuries to equipment resulting from falls of roof or similar causes. Fires may be started by unrelieved short cifiuits, or grounds, by the blowing of open fuses, and by the overheating of resistances. Incandescent lamps can produce heat enough to ignite combustible materials if the dissipation of the heat from

Jan 1, 1915

By E. J. Schmitz

Coming from San Antonio, Texas, and following the Galveston, Harrisburg and San Antonio Railroad westwards, one enters soon the Cretaceous formation, which forms a belt of several hundred miles, extending westwards to the boundary of Arizona and across the Rio Grande into the State of Coahuila, Mexico. The members of this formation are very numerous and in petrographical character very diverse—from a whitish or bluish, slaty, impure limestone to a hard, beautiful blue-and-red striped, and a compact heavy-bedded,

Jan 1, 1885

By D. L. Albright, R. W. Kraft

High-purity materials have been used in producing as-cast, controlled, colony, and degenerate solidification structures in the Fe-FeS eutectic. Experiments disclosed that this eutectic can be classified as normal and has a natural morphology composed of rodlike iron particles dispersed in a matrix of iron sulfide. The metallography of the various structures was studied, and a preferred crystallography was revealed in the controlled specimens produced by unidirectional solidification. The orientation effects found in these latter specimens are an [001] fiber texture in the -mowth direction of the bcc iron bhase and a texture corresponding to bicrystalline behavior in the hexagonal iron sulfide, with the growth direction near to (2111) poles. The observed texture of the iron phase is considered as indirect evidence that the alloy un-dercooled by at least 75°C before solidification. The unidirectional solidification of binary eutectic alloys has produced materials which exhibit a structure and properties markedly dependent upon the solidification process. In many cases a controlled microstructure with pronounced metallographic and crystallographic anisotropy can be experimentally achieved by proper regulation and balance of the growth rate of the alloy, the chemical purity of the starting materials, and the thermal gradient in the liquid at the liquid-solid interface. The purposes of this investigation were to produce various micro-structures in the Fe-FeS eutectic for subsequent study of their magnetic properties and to correlate the different structures with the solidification conditions in order to obtain a better understanding of the structure of eutectics. The Fe-S equilibrium diagram exhibits a eutectic composed of nearly pure iron and stoichiometric iron sulfide (FeS1.00), with the eutectic reaction occurring at 988°C and 31.0 wt pct S.1 Calculations indicate that this eutectic should solidify with about 9.5 vol pct Fe and 90.5 vol pct FeS, which in turn suggests2 that the micros tructure will consist of a rodlike iron constituent dispersed in a matrix of FeS. This characteristic has in fact been revealed some years ago.3 Thus, controlled solidification of this alloy might yield a material whose micromorphology would consist of very small ferromagnetic iron particles, rod-like in shape and aligned parallel to one another, supported in a matrix of antiferromagnetic FeS. Such specimens, because of the magnetic characteristics of the two phases, would be interesting subjects of study as magnetic materials. Hence the magnetic properties were considered in detail and are reported elsewhere.4 EXPERIMENTAL PROCEDURE The specimens of Fe-FeS eutectic were prepared from ultrapure iron (99.99+ pct) and high-purity sulfur (99.999+ pct). The iron was estimated to contain 60 ppm impurities (99.994 pct Fe) after zone purification.5 The ingots of iron were cut into chips, and the lumps of sulfur were ground into powder. In order to redice any nometallic impurities which might have accumulated during handling, the iron chips were annealed for 5 hr at 750° ± 10°C in a dry hydrogen atmosphere. Immediately after this treatment the chips were blended with the sulfur powder in eutectic proportions; the mixture was tamped into transparent fused quartz tubing and then vacuum-encapsulated under a pressure of 40 to 60µ of Hg. Because FeS expands upon solidification it was necessary to re-encapsulate the initial capsules so that oxidation reactions would be avoided when the inner tube cracked during solidification. For purposes of homogenizing the blended mixtures before solidification, the double capsules were heated to 750° ± 20°C and held for 20 hr; after this treatment the reacted product was weakly agglomerated. Each sample was then loaded into an apparatus for very rapid melting and freezing; this was accomplished by passing a molten zone through the specimen, using induction heating and a traverse mechanism. The resulting specimens solidified in the shape of the quartz tubing. Two sizes of specimens were used in this work, 18 mm diam by 100 mm long and 5 mm diam by 30 mm long. Metallographic examination of several ingots of both sizes after the above consolidation indicated no lack of compositional homogeneity and a random "as-cast" structure, because the travel rate was so rapid that unidirectional solidification was not achieved. Unidirectionally solidified specimens were resolidified in the apparatus shown schematically in Fig. 1, This equipment consisted of a kanthal resistance furnace mounted on the carriage of a zone-melting unit so that the heating element could traverse the length of the sample at a selected rate of speed. Large specimens were solidified with the mechanism tilted at ap-

Jan 1, 1967

By P. A. Larssen, P. R. Gage, R. W. Bartlett

The kinetics of formation of intermediate sili-cide compounds from MoSi2/Mo and WSi2/W couples were studied using a cylindrical sample configuration. Concentration profiles of the constituent metals were deter mined from electron-microprobe analysis of cross-sectioned samples after isotlzernzal diffusion annealing. These data also yielded hand widths of phases. Growth of intermediate phases depends on diffusionin them and obeys a parabolic rate law. The rates of formation of the intermediate phases decrease in the order Mo5Si3 > W5Si3 > Mo3Si. Crowth rates. for the isomorphous phases Mo5Si3 and W5Si3 had the same activation energy. 43 kcal per mole. SILICIDE coatings employed to protect refractory metals from high-temperature oxidation are usually formed by a diffusion process requiring concurrent transfer of silicon to the refractory metal surface. For a simple binary system and a coating thickness of one or two mils, the coatings on molybdenum and tungsten are primarily the disilicides WSi2 and MoSi2, respectively. During use of the coated re- fractory-metal system at high temperatures, in the absence of the silicon source, further diffusion causes growth of lower silicide compounds and depletion of the disilicides. Recent investigations have shown that the lower silicides are less effective than the disilicides in forming a glassy oxide film which impedes oxidation.' Consequently, failure of coatings at high temperatures may coincide with complete conversion of the disilicide phase. The purpose of this part of the study is to investigate the growth kinetics of the intermediate compounds in the W-Si and Mo-Si systems. There are three intermetallic compounds in the Mo-Si system: MoSi2 with a tetragonal structure

Jan 1, 1964