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By David Sinclair, Philip B. Bucky

THE dimensions and shapes of mine structures may at present be determined by (1) field experience, (2) structural calculations, and (3) barodynamic tests.§ None of these, however, provide information as to the stresses, their direction and distribution in a mine structure. For the design of pillars, the placing of openings relative to working places such as gangways, haulage levels, etc., this information is desirable. Photoelastic methods provide this and, while relatively new, their application in all engineering fields is assuming increasing importance. This paper, therefore, will present the method with a few applications to mining, and with sufficient reference for further study by the reader. PART I THE PHOTOELASTIC METHOD The photoelastic method of stress measurement determines the stress distribution in a two-dimensional model by optical means. It makes use of the fact that when a piece of isotropic transparent material, such as glass, celluloid, or Bakelite, is stressed and viewed in polarized** light a picture is seen which indicates by its color bands of light, or fringes, the magnitude of the stresses, their direction and their distribution. GENERAL EXPLANATION The stress at any point 0 in a structure (Fig. 1), may be resolved into two components, P and Q, each a pure tension or compression, at right angles to each other, called principal stresses.1 To fully identify the stress, the values of P and Q and their directions or angle [0] must be known.

Jan 1, 1940

By John V. Beall

Probably it won't happen to us again in a thousand years, but it was very embarassing at the time. It is only because of certain matters that have come up this month that we tell you at all about it. At the beginning of our trip to Peru and Chile last summer, we were flying with Bill Haddon from Lima to Tacna aboard Fawcett. Being an old hand at foreign travel, particularly in South America, we felt obliged to explain some of the special features of travel in Latin America and the niceties of etiquette in particular and were so engaged when the plane landed at the airport. We led the way briskly into the terminal, expecting at any moment to have a representative of Southern Peru Copper pop up and present himself. However, this didn't happen so we repaired to the baggage arrival station to wait. All the bags were quickly picked up, but ours were no where to be seen. Bill was slightly agitated because the plane was being buttoned up for take off. However, rising to the emergency with our usual aplomb, we took charge of the situation. Brandishing the claim checks under the nose of the porter who pointed to them and said, "si, Tacna," we nodded briskly and in our serviceable Spanish said "si se[n]or, vayase viejo, rapido." He was off and back with our suitcases quickly enough.

Jan 1, 1970

By J. B. Seabrook

The accompanying Fig 1 is a graphical scheme of intermediate accuracy for expediting interconversions of mol, weight, and volume percents. This chart consists of a family of curves of mol or atomic or volume percent plotted against weight percent, each curve in the family providing for a certain ratio of molecular or atomic weights or densities. Thus, the whole range of variations is presented in a very familiar format, and the conversion is effected simply by choosing the proper curve and reading off the required values. An entire series of conversions for a given binary system can be found by following the appropriate curve. It is interesting to examine the analytical geometry of the plots. The curves, which must fit into a square and all join at the 0 and 100 pet points, may be shown to be hyperbolas with their centers on the extension of the diagonal of the square which they intersect. Multiplying out the expression x A atomic fraction of A = y = ------ where x is the weight fraction of A, and A and B are atomic weights, we get xy+A/By- A/Bxy=x Upon rotating and translating axes and avoiding imaginaries, it is found that the angle of rotation is —45°, the origin moves upv2/2 units andv2/2(A/B+1/A/B-1) units to the right, and the standard form is Thus the curves are equilateral hyperbolas, their centers are units away from their intersection with

Jan 1, 1950

By Stanley Gill

The apparatus is composed of sections of small diameter, seamless steel tubing welded into a continuous flexible tube. At the bottom end a 1/4-in. pipe nipple with a 10 to 15-lb. weight is attached, together with a registering thermometer and a pair of ball check valves. The entire length of tubing is coiled in a single layer upon a drum 4 ft. in diameter which can be attached to the platform of a truck and provided with devices for winding and unwinding the tubing. Connections are made with the upper end of the tubing through a stuffing box, thence to a gas manifold to which a pressure gage is connected. Hydrogen gas is carried in standard 2-ft. cylinders and readings are taken by admitting gas into the tubing from one (or both) of the hydrogen cylinders until the pressure has been built up above that to be measured. At this time the gas supply is cut off. Excess gas escapes through the open end of the tubing and when equilibrium is reached, the pressure is read at the surface gage. Corrections are made for the weight of the column of gas. The advantages claimed for the apparatus include accuracy and the ability to measure the pressures at any number of points without removing the gage. Among the disadvantages of the apparatus are the somewhat bulky size of the equipment and its relatively high initial cost.

Jan 1, 1933

Professor Somasundaran has given an excellent presentation of the numerous problems which remain to be solved before the selective aggregation of fine particulates is likely to see broad commercial application in the beneficiation of mineral fines. However it is useful, I think, to reiterate some of the major problem areas. The over-riding factor which has limited the development of selective aggregation techniques is that processes such as coagulation and flocculation tend to be inherently non-selective. Conditions which favor the aggregation of one kind of fine particles usually favor the aggregation of all kinds of particles. As Professor Somasundaran has pointed out, the state of aggregation of a fine-particle dispersion is primarily determined by the forces of interaction between the individual particles. In most systems, the dominant forces are: 1. van der Waals - London Dispersion forces between the particles themselves 2. electrical double layer forces 3. steric forces between adsorbed layers on the surfaces of the particles. The London Dispersion forces between like particles are always attractive, but for dissimilar particles dispersed in a fluid medium can, in some cases, lead to a net repulsion. Electrical double layer forces always lead to repulsion between like particles but can, again, cause either attraction or repulsion for dissimilar materials. The steric forces, which are by far the least understood of the three types, can also lead to attraction or repulsion depending on condi-

Jan 1, 1979

By Ramkrishna Agarwal

The problem of the measurement of in situ stresses in rock masses has, in recent years, become one of the prime concerns of investigators and researchers in the field of rock mechanics. Numerous instruments have been developed for that purpose and various techniques have been used to determine the absolute values of these stresses at a point.l The "stress-relief" technique has gained the widest acceptance. In its usual application it relies on one of the two following principles: (1) Measurements of the changes in a "solid inclusion" in a borehole,2 or (2) Measurements of the diametral deformation of a borehole with a free boundary." The theoretical development, in the case of the latter, is based upon an evaluation of the deformation of a circular hole in an infinite plate under the action of a uniaxial stress field. Expressions for the deformations may be obtained by using either the plain strain or the generalized plane stress theoretical approach of the classical theory of Elasticity, which assumes that the material is linearly elastic, homogeneous and isotropic. The solution for the case of a biaxial stress field is obtained by the Principal of Superposition. The circular hole becomes elliptical after deformation takes place under the action of a uniaxial or biaxial stress field applied to the plate. In the practical application of the technique, the reverse procedure is applied. A borehole is drilled in the rock and a deformation-measuring

Jan 1, 1968

By Robert Lindsay

A NUMBER of detailed investigations of the physical changes accom-panying age-hardening have raised the question as to the possibility of some phenomenon preceding the actual process of precipitation. There is considerable evidence to indicate that in the first stages of the aging process there is a pronounced distortion of the crystal lattice. This is particularly marked in duralumin. It would be of considerable theo-retical interest to know the nature of this distortion as compared with that produced in other ways and to find out whether, in supersaturated alloys, it is a necessary antecedent to the formation of a second phase by precipitation. It was believed that a study of the age-hardening char-acteristics of a normally aged alloy compared with one that had been mechanically distorted might supply some useful information on these points. In addition, information would be obtained regarding the effect of a mechanical distortion on any subsequent stage in the aging process. Duralumin was chosen as the material for this investigation because the various aspects of its aging behavior can be shown in detail by suit-able variations of the aging temperature. Also, probably more work has been done on this class of alloys than on any other. In spite of the many published results, it was felt that the experiments would be significant only if all of the work were done on samples from the same source and if they were examined under identical experimental conditions.

Jan 1, 1939

By John W. Pack

At present the manufacture of metallic zinc, or spelter, in Missouri, is carried on only at the establishments located at Carondelet, or South St. Louis. Although the development of the industry has not yet reached that fulness which it has attained elsewhere in the United States, still the commanding advantages of position of these establishments are so evident that the prospective importance and magnitude of spelter manufacture in this State, and especially at this locality, can hardly be doubted. A study of the chemical and technical aspects of the business of these points cannot be without interest to the metallurgist as well as to the capitalist. I have endeavored to investigate, as far as was practicable, within the limits of a paper of this character, some of the problems connected with this industry, at the same time making a few comparisons of the results attained at some of the Carondelet works with those of other establishments with regard to which information could be obtained. In the prosecution of these studies I have been kindly aided by the managers of Carondelet establishments, and by Prof. Charles P. Williams, Director of Rolla School of Mines. To the latter I am especially indebted for assistance in regard to methods of analysis. To all these gentlemen I return my thanks for their valuable aid. Other sources of information will be duly credited in their proper places.

By W. W. Tyler, A. C. Wilson, L. B. Nesbitt

INVESTIGATIONS of thermal conductivity and impact strength of the titanium alloy RC-130-B and 316 stainless steel were undertaken because of interest in strong, nonmagnetic, commercially available alloys of low thermal conductivity for use in low temperature experiments. Measurements of electrical resistivity and thermoelectric power were also made for some of the samples studied. The titanium alloy designated as RC-130-B is manufactured by Rem Cru Titanium Inc. It contains 0.14 pct C, 3.99 pct Al, and 4.7 pct Mn. A general discussion of properties of the two phase Ti-4Mn- 4A1 alloys is given by Finlay and Vordahl.' The alloy is machinable and has a yield strength greater than 130,000 lb per sq in. at 0.2 pct offset. The 316 stainless steel sample used for both conductivity and impact strength measurements was obtained from the Allegheny-Ludlum Steel Corp. and is designated as Allegheny metal 18-8M, Type 316, Grade 316. The sample had received 25 pct minimum final cold reduction and had a Brine11 hardness rating of 255. Several impact tests were made on a sample of 316 stainless which had not received the 25 pct cold reduction. Also several data points are reported giving thermal conductivity and electrical resistivity for a sample of 304 stainless steel taken from stock. Figs. 1 and 2 give thermal conductivity and electrical resistivity data for the titanium alloy and for

Jan 1, 1954

By P. K. Chatterjee

The overall success of many strip coal mining operations depends primarily upon the efficient use of draglines to remove overburden. These machines require enormous capital investment and unless used efficiently the profitability of a venture is adversely affected. It is important that the dragline works continuously and it is imperative that the walking path and other facets of its operation be predetermined exactly so that the desired production rate is achieved with a minimum of non-productive time. Details of dragline operations which are of particular interest are walking path, prediction of best cut and positioning to maximize production, the angle of swing which produces the swiftest operation, optimum fill factor allowable for the type of material and conditions of ground, the maximum depth from which it can excavate and operating level with respect to the elevation of the high wall. The aims of the present paper are: 1. To establish a cut-off point in the cost-depth ratio. 2. Predict the most economic method of stripping in a given area using graphical plots of walking path implemented with information necessary to ensure optimum production. The optimum operating efficiency of the dragline in relation to the terrain and other conditions imposed on its operation will be evaluated. The model is based upon operating data which has been collected from site observations of a large strip coal mining operation in Central Queensland, Australia.

Jan 1, 1977

HENRY M. HOWE, Bedford Hills, N. T. (communication to the Secretary?).-The authors valuable results as to the effects of the air-hardening temperature on high-speed steel may be summed up thus: Influence of Rising Air-Hardening Temperature on. High-Speed Steel Air-hardening microstructure Cutting Properties temperature S Austenite Grain Free Carbide Grains Boundaries Too low Small or Narrow Maximum Too soft undeveloped Intermediate, Well-developed Intermediate Little or even Best correct none Too high Coarse hide, even with Minimum . Weak, brittle, three-rayed crumbling stars Here the suggestion is that as the air-hardening temperature rises it causes two prominent effects, one helpful and the other harmful, the increase of the former exceeding that; of the latter up to a certain point, at which the steel is most useful, and then in turn being outrun by it. The first is the progressive dissolving of the free carbide in the austenite, increasing the stability of the red-hard state. The second is the progressive coarsening of the grains, and thickening of the intergranular cement, developing at last into spandril-like three-rayed stars of the 1,288° specimen. (2,350° F.) of Plate D, thus giving clear proof of incipient fusion, that is of crossing the solidus. This causes intergranular weakness. The individual grains may have great red-hardness, but they do not cohere. They approach the condition of a bag of emery grains.

Jan 6, 1917

By D. L. Harris, A. M. Gaudin

THE following results, presented here in condensed form,1 were obtained in a preliminary study of the adsorption of n-hexane thiol, hexyl mercaptan, on sphalerite, zincite, willemite, and quartz, from aqueous solution and from a gas. Interest in this subject was aroused by a Belgian report2 of effective use of hexyl mercaptan for flotation collection of oxidized zinc minerals. The relatively low boiling point, 149°C, of the mercaptan3 suggested the desirability of extending the usual measurements of partition of collector between aqueous solution and gas and between gas and mineral. It is believed that this paper presents the first measurements of this type on a flotation system. Attempts were made to carry out the measurements at equilibrium, but as the work progressed it became increasingly doubtful that this desirable condition had been achieved. To control composition and extent of the gas phase, the apparatus was a wholly-enclosed thermally-controlled glass system. Because of these constraints and the desirability of dealing with pure minerals, a scale of operations was chosen in which a few grams of deslimed mineral were used in each test. It was also necessary to choose a particularly sensitive method for mercaptan analysis, and in fact a method that would permit the experimenters to follow the approach to equilibrium. For these reasons mercaptan marked by radiosulphur 35 was used. An analysis was made for the radiosulphur by a modification of the method of Gaudin and Carr.4

Jan 9, 1954

By LeRoy Scharon, P. Uhley

TEST gravity surveys were made in the Washington County barite district of Missouri on properly owned by the Baroid Sales Division of the National Lead Co. This property is located just northeast of Richwoods in the northeastern corner of Washington County, Fig. 1. The area to which the surveys were confined comprised approximately 5000 acres, of which some 525 acres were surveyed gravitationally. Gravity observations were made at 2600 points within the area, observations being confined to relatively clear and gently sloping ground. Part of the area was heavily wooded, and the terrain too rugged for either the occurrence of a commercial barite deposit or a feasible gravity survey. The relief along the central drainage, Ditch Creek, was about 140 ft, the maximum difference in elevation being 400 ft in a distance of 3½ miles. The purpose of the test gravity survey was to determine whether the gravity method of geophysical prospecting might be applied in the exploration for barite deposits in the Washington County barite district, since a satisfactory systematic procedure had not been devised to explore and ultimately determine barite ore reserves with desired accuracy. No previous geophysical work with respect to barite is known to have been done in this area. Stratigraphy: The formations over which the barite deposits occur' are Paleozoic in age, representing rocks involving sandstones and dolomites unconformably underlain by pre-Cambrain granites and rhyolite porphyries. The areas covered by the granite survey were directly underlain by almost

Jan 1, 1955

By Walter W. Lilly, Issa S. Oweis

Application of rock engineering in geotechnial consulting practice considered herein is in areas of: (a) bedrock verification for foundation support, (b) bearing capacity and settlements, and (c) excavations. A routine geotechnical investigation usually provides data on depth to rock, rock classification, and rock quality. In cases of rock outcrop, such outcrops are mapped for geologic structures and rock mass description. In addition, the regional geology and the general aspects of the groundwater regime are usually known from either published literature or previous experience. The predominant technique for ground and site investigation are usually drilling and geologic reconnaissance. Other techniques involving seismic and geophysical soundings, borehole camera, and oriented cores are used by by no means routine. Performing laboratory strength and compressibility tests is often made to be considered as routine. The use of the point load test is gaining increasing use in the United States and would, perhaps, become a routine field or laboratory test due to its simplicity and, more importantly, its relatively low cost. The purpose of this paper is to describe cases where mostly routine investigation and testing were used to arrive at engineering decisions. Bearing Capacity and Settlements The allowable bearing values for foundation support on rock is usually dictated by local building codes which presumably should reflect local experience. The interpretation of the code, however, can present a problem, especially if the interpretation is made by a designer under the delusion of knowledge in rock engineering. For

Jan 1, 1982

By C. M. Loeb, A. M. Gaudin, J. H. Brown

THE object of most size reduction operations in the mineral industry is to liberate the grains of valuable minerals in the ore from those of the gangue. This is usually accomplished by crushing and grinding the entire mass of ore until there is only a small probability that any single particle contains more than one mineral. During this size reduction only limited control exists over size or composition of the particles exposed to the breaking action, and there is no control over the paths followed by cracks generated during the operation. This lack of control usually results in overgrinding and in production of large quantities of very fine material. The first detriment, overgrinding, is costly in itself, but when combined with the second factor it is doubly so. Not only is the fracture of a free particle unnecessary-the fracture of these particles may also make subsequent separation operations difficult, inefficient, and wasteful. It has been pointed out' that if the object of size reduction is to liberate the valuable mineral component of the ore then, ideally, fracture should follow intergranular paths to the exclusion of trans- granular ones. This would result in liberation of the valuable minerals with as little size reduction as possible. This ideal comminution operation is referred to as intergranular comminution, and it was the object of the investigation to determine the extent to which it could be developed by heat treatments.

Jan 4, 1958

THE Institute of Metals Division of the A. I. M. E. has joined with the American Society for Steel Treating and the American Welding Society in support of National Metal Week in Philadelphia, Oct. 8 to 12. Individual and joint technical sessions, plant inspection trips, and a general exposition to be held in Commercial Museum have all been arranged. With the coming of the Institute of Metals Division into the circle, the scope of the exposition has been broadened to cover non-ferrous metals, and exhibits of much interest are promised. Headquarters for the Institute of Metals and the American Society for Steel Treating will be at the Benjamin Franklin Hotel, and for the American Welding Society at the Bellevue-Stratford. The American Society for Steel Treating and the Welding Society will hold technical sessions each forenoon at their hotel headquarters. The Institute of Metals Division will hold sessions Tuesday morning and Wednesday and Thursday afternoons; that for Wednesday being a joint session with the American Society for Steel Treating. The latter society will hold independent afternoon sessions on Thursday and Friday. Registration and information desks will be open at the hotels throughout the week, and an attractive program of entertainments has been arranged.

Jan 1, 1928

By Arthur F. Taggart

MR. CHAIRMAN: Congratulations! Your four-ring milling show this year was a dandy. It cleared our minds, for a few hours at least, of what Hitler, Hirohito, the New Deal, and the tribe in the Treasury are trying to do to strangle American enterprise. We mustn't forget this, but it's a relief to get our thoughts away from it occasionally. GRINDING-There was a further contribution to the excellent work that the Allis-Chalmers laboratory staff has been doing for the grinding fraternity in compiling-and publishing-a carefully quantitative list of comparative resistances of ores and other materials to comminution (T.P. 1579, Bond-Maxson). A diagnostic accuracy of ± 10 per cent was claimed for estimates based on these figures. Are they really that good? How about some of you men in the field writing M&M about it?

Jan 1, 1943

By D. Mills, G. B. Craig

ZIRCONIUM has been float-zone-refined in an electron-beam furnace and the redistribution of oxygen, iron, and tungsten has been measured. The iodide zirconium used in the present experiments initially contained both oxygen and iron in the range 100 to 200 ppm by weight, and tungsten in amounts less than 10 ppm. Float-zone refining of zirconium, using induction heating, has previously been attempted by Kneip and Betterton1 and Langeron.2 Kneip and Betterton were primarily interested in the removal of iron and nickel. They achieved some purification, with respect to both these elements, in material given up to six passes at 150 mm per hr under an argon atmosphere. Langeron reported purification for a large number of elements after four completed passes in a static vacuum system operating at pressures less than 10-6 mm of Hg and with rates of zone travel between 30 and 40 mm per hr. He did not report oxygen concentrations, but stated that there was inverse segregation of this element. westlake5 has also used a minimum of four zone passes to remove iron from zirconium. No rates or conditions were given. Belk6 has shown that tungsten contamination can occur during electron-beam melting. He reported an increase from 0.01 to 0.05 pct by weight tungsten in molybdenum after four complete zone passes. The vacuum system for the electron-beam unit used in the present investigation consisted of a single-stage rotary pump backing a liquid-air-trapped oil-diffusion pump. A pressure of less than 10-8 mm of Hg was obtained with Dow-Corning 705 fluid in the diffusion pump. In order to avoid contamination of the zirconium by evaporation from the tungsten filament, a special focusing cage4 was employed. Three rates of zone travel, 114, 38, and 4 mm per hr, were investigated, with the liquid zone moving from the bottom to the top of the bar. The bars used were 3 mm diam and the total melted length was 130 mm. Oxygen was analyzed by neutron-activation analysis using a neutron flux of 10' neutrons per sq cm per sec to form the isotope N16 by the 016 (n,p) N16 reaction. The standard deviation is quoted for each oxygen determination. The iron and tungsten analyses were performed spectrographically, and the precision is estimated to be ±6 pct. Analyses for tungsten were all below the detectable limit of 10 ppm, confirming the protection given by the focusing cage. No significant redistribution of oxygen was found at the two higher rates of zone travel. The redistribution of oxygen and iron obtained after five passes at a rate of zone travel of 4 mm per hr (1.1 x 10-4 cm per sec) is recorded in Tables I and 11. Burris, Stockman, and Dillon3 have estimated the distribution of solutes during multipass zone refining. Using their curves for an effective distribution coefficient of Keff = 1.5 and 2 for oxygen and Keff = 0.3 for iron, the expected concentrations were estimated for the present material. These are shown in Tables I and 11, along with the experimentally measured values. The calculated concentrations are based on a molten-zone length of 10 pct of the total melted length, whereas in the present experiments the molten zone was approximately 5 pct of the total melted length. The effect of zone length on solute redistribution is most pronounced after a large number of zone passes. Comparison with Pfann's published data8 for solute redistribution for various Keff's and zone lengths indicates only small differences at low numbers of completed zone passes. It is evident that the expected distribution has not been realized in the case of iron. Scrapings of material deposited on the inner surfaces of the electron-focusing cage were found to be magnetic. It is, therefore, concluded that redistribution of iron is masked by evaporation. Deposition of iron inside the focusing cage was observed at all rates of zone travel. The results of the investigation may be summarized as follows: 1) Segregation of oxygen is typical for a solute with a distribution coefficient, Keff > 1. 2) No redistribution of oxygen takes place at high rates of zone travel. 3) The distribution coefficient for oxygen lies between 1.5 and 2.0. 4) Purification with respect to iron occurs mainly by evaporation. 5) The focusing cage is effective in preventing tungsten contamination.

Jan 1, 1967

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 Takashi Katsura, Avnulf Muan

Equilibrium relations in the system FeO-Fe2O3 Cr2O3 have been determined at 1300°C at oxygen pressures ranging from that of air (0.21 atm) to 1.5 x 10-11 atm. The following oxide phases have stable equilibrium existence under these conditions : a sesquioxide solid solution with corundum-type structure (approximate composition Fe2O3-Cr2O3); a ternary solid solution with spinel-type structure (approximate composition FeO Fe2O3-FeO Cr2O3) and a ternary wüstite solid solution with periclase-type structure and compositions approaching FeO. The metal phase occurring in equilibrium with oxide phase(s) at the lowest oxygen pressures used in the present investigation is almost pure iron. The extent of solid-solution areas and the location of oxygen isobars have been determined. ThE system Fe-Cr-O has attracted a great deal of interest among metallurgists as well as ceramists and geochemists. Metallurgists have studied the system because of its importance in deoxidation equilibria, ceramists because of its importance in basic brick technology, and geochemists because of its importance for an understanding of natural chromite deposits. Chen and chipman1 investigated the Cr-O equilibrium in liquid iron at 1595°C in atmospheres of known oxygen pressures (controlled H2O/H2 ratios). The main purpose of their work was to determine the stability range of the iron-chromite phase. Hilty et al.2 studied oxide phases in equilibrium with liquid Fe-Cr alloys at 1550°, 1600°, and 1650°C. They reported the existence of two previously unknown oxide phases, one a distorted spinel with composition intermediate between FeO Cr203 and Cr3O4, the other Cr3O4 with tetragonal structure. They also sketched diagrams showing the inferred liqui-dus surface and the inferred 1600°C isothermal section for the system Fe-Cr-O. Koch et al3 studied oxide inclusions in Fe-Cr alloys and also observed the distorted spinel phase reported by Hilty et al. Richards and white4 as well as Woodhouse and White5 investigated spinel-sesquioxide equilibria in the system Fe-Cr-O in air in the temperature range of 1420" to 1650°C, and Muan and Somiya6 delineated approximate phase relations in the system in air from 1400" to 2050°C. The present study was carried out at a constant temperature of 1300° C and at oxygen pressures ranging from 0.21 atm (air) to 1.5 x 10-11 atm. The chosen temperature is high enough to permit equilibrium to be attained within a reasonable period of time within most composition areas of the system, and still low enough to permit use of experimental methods which give highly accurate and reliable results. These methods are described in detail in the following. I) EXPERIMENTAL METHODS 1) General Procedures. Two different experimental methods were used in the present investigation: quenching and thermogravimetry. In the quenching method, oxide samples were heated at chosen temperature and chosen oxygen pressure until equilibrium was attained among gas and condensed phases. The samples were then quenched rapidly to room temperature and the phases present determined by X-ray and microscopic examination. Total compositions were determined by chemical analysis after quenching. In the thermogravimetric method, pellets of oxide mixtures were suspended by a thin platinum wire from one beam of an analytical balance, and the weight changes were recorded as a function of oxygen pressure at constant temperature. The data thus obtained were used to locate oxygen isobars. The courses of the latter curves reflect changes in phase assemblages and serve to supplement the observations made by the quenching technique. 2) Materials. Analytical-grade Fe2O3 and Cr2O3 were used as starting materials. Each oxide was first heated separately in air at 1000°C for several hours. Mixtures of desired ratios of the two oxides were then prepared. Each mixture was finely ground and mixed, and heated at 1250" to 1300°C in air for 2 hr, ground and mixed again and heated at the same temperature for 5 to 24 hr, depending on the Cr2O3 content of the mixture. A homogeneous sesquioxide solid solution between the two end members resulted from this treatment. A Part of some of the sesquioxide samples thus prepared was heated for 2 to 3 hr at 1300°C and oxygen pressures of 10-7 or 1.5 x 10-11 atm. Reduced samples (either iron chromite

Jan 1, 1964