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By E. J. Rapperport, M. F. Smith

A presentation of the W-Ru constitution diagram is given. Techniques utilized in the determination of phase boundary values include electron micro-probe analysis of two-phased alloys and diffusion couples, as well as normal metallographic and X-ray methods. The primary features of the diagram are: 1) a terminal solid solution of ruthenium in tungsten with a maximum solubility of 23 at. pct Ru at 2300°C; 2) a terminal solid solution of tungsten in ruthenium with a maximum solubility of 48 at. pct W at 2205°C; 3) a o phase of maximum breadth about 6 at. pct based on the composition W3Ru2 which forms peritectically from the melt at 2300°C, and which decomposes eutectoidally at 1667 °C to form a twigs ten and 0 ruthenium; 4) a eutectic at 45 at. pct Ru and 2205°C with the products being o plus ß ruthenium. THE W-Ru diagram has previously been studied only in a cursory fashion. Raub and alter' obtained a 1400°C isotherm in which they observed no intermediate phases, and on which they established the limits of solubility as 36.5 at. pct W in ruthenium and about 1.5 at. pct Ru in tungsten. In addition, Obrowski2 found a o phase forming peritectically from the melt and existing only above 1650°C. Below this temperature the phase was presumed to decompose eutectoidally. The present work finds the diagram as given in Fig. 1. I) EXPERIMENTAL PROCEDURE The materials used for alloy preparation in determining the W-Ru constitution diagram were 99.9 pct pure ruthenium powder supplied by Baker Chemical Co., and 99.9 pct pure tungsten powder from General Electric Co. Typical analyses of these elements are given in Table I. Initial alloys at 10 at. pct intervals were prepared from the metal powders by the following method. Powders sufficient for 25 g of the alloys were weighed out with an accuracy of 0.1 mg and blended mechanically. After blending, the powders were compacted, in a steel die, at approximately 30,000 psi. The compacts were sintered in an electric vacuum furnace in order to remove adsorbed gases and to achieve partial densification prior to arc-melting. Vacua of 10-4 mm Hg or less were maintained in sintering as the furnace temperature was raised to approximately 2000°C. Sintering times ranged from 10 to 20 hr. The sintered compacts were arc-melted under a protective atmosphere of purified helium. Melting was conducted on a water-cooled copper hearth, utilizing a nonconsumable tungsten electrode. In the melting process, each alloy was turned over and re-melted on opposite sides from four to six times to ensure complete melting and to eliminate gross in-homogeneities. The arc-melter used had a vacuum capability of 5 X 10-6 mm Hg, and a leak rate of about 20 -liters per hr. Chemical analysis techniques for refractory metal-platinum group metal combinations are not well-established; therefore, composition control and determination depended principally upon weight-loss observations and calculations. This consisted in weighing each alloy after sintering and after arc-melting, and calculating the maximum and minimum composition values, assuming the total weight losses to be first all tungsten, and then all ruthenium. Since composition uncertainty was directly related to weight loss, care was taken to minimize losses in handling, compacting, and melting. Prior to homogenization and equilibration the as-arc-melted alloys were analyzed in several

Jan 1, 1964

By Leo F. Reinartz

Part II of a four-part series on the history of steelmaking in the US, points out the inadequate safety and living conditions that existed in steel mills at the turn of the Century. Also defined are furnace and process developments. OPERATIONS in steel plants today are highly mechanized. Men work in light, clean, orderly melting shops, making it difficult for old timers to convince young men that primitive, hazardous conditions existed in steel plants at the turn of the century. Working conditions then were very poor as compared to present day standards. In small plants especially, sanitary, locker, and washroom facilities, first-aid practices and stations were un- known Accidents were frequent and severe. Workers had a fatalistic attitude toward getting hurt. He who had an accident was looked upon as a hero. A dirty bandanna often served as a bandage. Infections were frequent. Electric cranes were in their infancy and broke down often Cables had not as yet replaced chains. Pig iron and scrap iron were loaded by hand in the stockyard, and stockyard locomotives were un- known; mules served as the usual motive power. It was not unusual to see recorded a delay of ½ hr in charging a furnace because of a balky mule. Furnace operations A few plants had primitive charging machines, but most furnaces were charged by placing scrap or pig iron on the paddle of a long peel, which rested on a bar across the furnace door opening. Laborers at the handle end of the peel, using the bar as a fulcrum, would heave the material into the furnace by a down and sideward motion of the peel handle. In time they became expert in placing these materials in the furnace, but it was hard, hot work, and a long time was required for charging. Cold charges of 25 tons required more than 12 hr for melting and re- fining the steel. Ports, doors, and frames were not water cooled. The charging and working area in front of the furnace was covered with steel plates. They were hot and often warped by the intense heat of the un- insulated checker chambers directly below. In the summer, working conditions on the charging floor were almost unbearable. Silica refractories were of poor quality. Because of this, and the inadequate training of furnace men in fuel control and furnace operations, roofs, front and back walls, and ends burned out rapidly. Dolomite machines were unknown; consequently, furnace banks and hearths were fettled with dolomite by the use of hand shovels. The round system required six or more men. Each man took a shovelful of dolomite and, in his turn, deposited it on the back wall and bank by a dexterous forward swing and twist of the shovel. The upward swing of the shovel partially protected his face from the searing heat of the furnace coming out through the wide-open door. Considerable skill and stamina were required to do this job properly. Reverse valves, usually of the cast-iron butterfly type, were located below the charging floor. They were operated by long levers on the charging floor level men they became warped, because of heat and abuse, great strength and skill were required to reverse them. Furnace operations were difficult. The quality and quantity of producer gas coming from irregularly stoked, hand-operated gas producers was uncertain and unreliable. Furnace Linings and ports were quickly burned out. Poor bottom and side-wall refractories, indifferent and inexperienced crews, as well as irregular re-

Jan 1, 1961

By M. A. Whiting, H. Kenyon Burch

One of the advantages presented by electric drive in many classes of work is the ease with which the electric motor can be controlled automatically. In a large number of cases certain features of the control are automatic—for example, the rate of acceleration may be limited automatically or the equipment may be stopped automatically at the limit of travel—but the equipment is started and ordinarily is stopped by hand. In other cases the motion of the machinery is utilized to start, control the speed, and stop the motor automatically, independently of any operator. A considerable proportion of the large mine hoists now in use have certain automatic features, particularly protective devices against overwinding, and, in some classes of electric hoists, devices for preventing excessive acceleration or retardation. The large automatic hoists discussed in this paper, however, are completely automatic, i.e., capable of making their trips without the presence of an operator at the control levers. According to circumstances, various advantages may be obtained . by automatic control, chief of which are decreased power consumption, increased precision and safety of operation, and decreased cost of attendance. The first step in the analysis of a prospective automatic mine hoist is to determine whether automatic operation is feasible at all. If men are to be hoisted, or levels changed, the attention of an operator is required for these purposes; but under some conditions it may be entirely practicable and advantageous to build the equipment so that, while provision is made for hoisting men or changing levels, ore can be hoisted automatically from any one level. If, however, an operator's attention is required every few minutes for changing levels, handling men or drills, or other work requiring hand control, it is obvious that automatic operation between times will not be of any practical benefit.

Jan 1, 1917

By B. M. Larsen, W. E. Shenk

This paper describes a method of reversal control of the open-hearth furnace that obtains in practice those effects considered below as essential to a completely automatic control, without appreciable interference with the natural rise and fall in temperature of the regenerative portions of the furnace system. Growing out of some studies of radiation pyrometry in open-hearth regenerators, it was developed during 1934-1938, and has been successfully applied to a number of commercial furnaces. The goal of open-hearth furnace operation is the highest rate of production of steel of proper quality consistent with good refractory life and fuel economy. This requires rapid heat transfer from furnace to charge, which in turn is dependent upon heating the furnace refractories to the highest safe operating temperature. The greater the heat input to the melting chamber, the sooner this limiting temperature will be reached, so that control methods in general that are designed to protect against overheating of refractories should help to maintain maximum fuel input and production rate. For the typical open-hearth system, with fixed regenerator capacity and with rate of fuel input usually restricted in its range of variation, our basic assumption is the idea that the only other important variable —that is, the time interval between successive reversals—should also be held constant or within a small range. The present reversal control was designed therefore so that, under normal operating conditions, no arbitrary limitation is imposed other than to keep the reversal interval within the optimum time range. However, since a near approach to completely automatic operation involves protection of refractories through the balancing of furnace end temperatures as well as emergency protection against temperature peaks above some upper limit, it was also felt essential to employ, as an integral part of the control unit, a temperature-measuring instrument to register the true temperature of the refractory surfaces at some critical region in the hot ends of the regenerative zones. As the basic elements of the control, we thus have one "maximum" and one lLminimum" time relay and a potentiometer recorder-controller, combined with switches and relays to operate as follows: I. Reversal normally occurs within an optimum range limited by the maximum and minimum settings to about 4 to 6 min. variation, but the actual interval usually is less variable and closer to the minimum setting. 2. The margin between minimum and maximum time is utilized, together with a "floating temperature limit" in the potenti-ometric control instrument, to correct any tendency toward temperature unbalance between ends of the furnace. 3. A second "maximum temperature

Jan 1, 1945

By C. H. Mathewson

ABOUT fifty pages of Henry M. Howe's profound treatise, "The Metallography of Steel and Cast Iron," are devoted to twinning with special reference to the origin, nature and general significance of the Neu-mann bands in ferrite. Howe believed with Osmond and Cartaud1 that the Neumanns are mechanical twins and his careful observations leave no doubt that these straight-sided narrow bands habitually occur parallel to trapezohedral planes of form {211}. Attempts to develop the structure of the bands by various methods so that their identity could be established beyond question have not been conspicuously successful. Howe thought that they deflected slip bands. Some of the etching figures which have been developed within and adjacent to Neumann bands support the contention that they are twins. A good example of this effect in ferrite containing 0.6 per cent. of nickel and 1.3 per cent. of phosphorus, originally due to Harnecker and Rassow,2. was reproduced in the 1928 lecture before the Institute of Metals Division on twinning in metals.3 In this case, the sides of the figures might represent the traces of cubic planes laid bare by etching a properly oriented grain of ferrite, twinned along a plane of form 12111. Our own observations in this direction may be represented by Fig. 1 which shows in a deeply etched cavity in the boundary region between a Neumann band and the original crystal two small crystal surfaces which resemble the faces meeting at a reentrant angle in the simple cube twinned along a bisecting plane of form {211} as sketched in Fig. 2. Rosenhain and McMinn4 in 1925, after a careful study of slip bands in ferrite containing Neumanns previously produced by shock, concluded

Jan 1, 1928

By F. G. Clapp

Introduction.......................................................... 915 Scope of Discussion................................................... 915 Literature and Acknowledgments....................................... 915 Geographic Distribution of Petroleum in South America................. 916 Geographical Comparison with North America.......................... 917 Geological Inferences Regarding South America......................... 918 Quality of South American Oil........................................ 918 South America's Position in the World's Production.................... 919 Political Conditions in South America................................. 920 Peru.................................................................. 920 Distribution of Peruvian Fields................................ :...... 920 Surface Indications.................................................. 923 Geological Conditions................................................ 925 Quality................................................,............ 927 Production......................................................... 929 Argentina............................................................. 932 Distribution of Argentina Fields...................................... 932 Surface Indications.................................................. 933 Geological Conditions............:................................... 935 Quality .......................................................... 936 Production.......................................................:938 Venezuela................................................. 939 Distribution of Venezuela Fields...................................... 939 Surface Indications................................................. 939 Geology of Venezuela Fields.......................................... 941 Quality........................................................... 942 Production.......................................................... 943 Colombia.............................................................. 944 Distribution of Colombia Fields....................................... 944 Surface Indications.................................................. 945 Geological Conditions............................................... 948 Quality............................................................ 950 Production......................................................... 950

Jan 1, 1918

By W. A. Ver Wiebe

The year 1940 was singularly unmarked by sensational developments in Kansas. Routine operations were carried on in a systematic, orderly fashion and the efforts of oil producers were concentrated on extending known fields. In Kansas an arbitrary yardstick for wildcats has been set up. A well drilled mile or more from a known pool or well is now considered a wildcat. A "rank wildcat" is one that is drilled at least 2 miles from any known producer. During 1940, rank wildcats resulted in the completion of 116 test wells, among which 16 were successful in finding new oil pools and the remaining I00 were dry holes. The ratio of successful wells to dry holes, therefore, was approximately I:6. During the year, 1890 wells were completed in eastern and western Kansas. This figure is somewhat lower than that given in several trade journals, because it does not include wells that were deepened or wells that were recompleted in a different geological horizon. About three fourths of these (1423) were completed as commercial oil wells (I220 in western and 203 in eastern Kansas). The commercial gas wells completed number 58 of which 10 are in eastern Kansas and 48 in western Kansas. Of the remzining completions 147 are dry holes in eastern and 262 are dry holes in western Kansas. Based on daily potential capacity, the new discoveries of the year account for a cumulative initial production of 46,000 bbl. in eastern and 2,128,000 bbl. in western Kansas. The state of Kansas attained a new peak in production, with the total of 66,245,000 bbl. for the year 1940, the number of contributing wells being 20,779. Thus the increase over 1939, when about 58 million barrels was produced, is considerable. The previous peak occurred in 1937, when 70,761,000 bbl. was marketed. In another still earlier peak, in 1917, slightly more than 45,000,000 bbl. was produced and sold. The production of gas probably reached a new peak also during 1940, with its total of 85 1/2 billion cubic feet. Between the peak of the year 1908, when over 80 billion cubic feet was produced, and that of 1940, the production dropped to a low point of 16 billion cubic feet in the year 1921. The number of test wells drilled was larger than in 1939; that is, 1890 compared with 1458. The first peak was reached in 1904, when 2782 wells were drilled. The number dropped off rapidly, to 368 three years later, but rose to the second and highest peak in 1918, when 4671 test wells were completed. In the period between 1904 and 1912 more gas wells were completed than oil wells. Between the high peak of completions in 1918 and somewhat lower peak of 1937, the low point was reached during 1931, with the completion of only 470 test wells. In the number of new pools discovered, Kansas again ranks high among the states. The exact number depends somewhat upon the interpretation of a "new" area— whether it should be called a new pool or a long extension of an old pool. Unfortunately, the matter of securing the right kind of production allowable also enters into this question. Often the decision regarding a new pool cannot be made until other wells

Jan 1, 1941

By Stephen Krickovic

THERE is today no proven continuous mining machine that can be used under all the varying conditions found in most bituminous coal mines. During the last five years, however, both the machines and methods of using them have been improved. Coal operators can now exercise a fair degree of selectivity, except those who must struggle with thick and hard partings and operate in seams less than 40 in. thick. It must be realized, then, that more than one type of continuous miner may be used advantageously in the same coal mine. Although this appears to violate the standardization generally sought after, the gain can more than offset added maintenance and, to a lesser degree, operating problems. It is equally important to realize that most coal mines will require one or more conventional loader setups in the plan of total mechanization. Seam variations, adverse physical conditions, and special designs of main headings for haulage and ventilation, to name only three reasons, may render 100 pct use of continuous miners uneconomical. Of course, this situation may change. In one mine, prior to 1954, machines that ripped coal from the face achieved only average results, as compared to the impressive performance of boring-type units in another coal mine. A boring-type unit was therefore selected for the first mine in the belief that the chance of success would be greater if it were used in a combined cutting and wedging operation, cutting a full face in its forward movement. The miner was located in a part of the mine where a special projection could be readily developed, a solid area scheduled for mining according to the overall progress plan. All openings surrounding the particular area were carefully investigated for the presence of sulfur balls. Fig. 1 (opposite) shows the representative seam section, containing the several pyritic bands 1/4 to 1/2 in. thick; a characteristic Pittsburgh seam parting averaging 5 to 6 in. of slate, coal, and slate; and the occasional py-rite lenses 2 to 3 in. thick. Under normal conventional mining methods, the top 10 or 12 in. and the bottom 4 in. are left in place to offer roof protection

Jan 1, 1958

By J. W. Hickman, E. A. Gulbransen

In a previous paper' the authors have investigated the structure of the oxide films formed on most of the metals that make up the alloys of this study. The metals were studied in order to provide basic information on the structures, both physical and chemical, of the oxide films and to determine how these structures are effected by the temperature, time of oxidation, and surface preparation. It was felt that an understanding of the physical and chemical structure as well as the stability of the oxide film might furnish clues as to the nature of the reaction process and the protective quality of the film. The oxidation of the metals was studied over the temperature range 300' to 7o0°C. except for copper, wherc the range selected was 100' to 500°C. The results of these studies were presented in graphical form as existence diagrams of the oxides on a time-temperature scale. For some of the metals the existence diagrams were simple and showed few chemical transitions, but there were numerous cases where the physical state of the oxide surface was a function of time and temperature. In general the physical state of the oxide surface changed with increasing temperature so as to increase the sharpness of the diffraction patterns and to cause orientation effects to be more pronounced. Deviatiois in lattice Darameters from X-ray values were noted. In general these deviations were of positive nature and may be due to solid solution of the metal in the oxide lattice. This effect might be expected in thin oxide films. In a study of the oxidation of alloys containing two or more metals, there may arise the complicating factor of identification of the oxides formed. A thorough understanding of the oxides formed on the pure metals, therefore, was, essential before investigation of the oxidation of alloys. In this paper it is our purpose to present a study of the following problems: 1. The existence diagrams of various alloys. 2. The effect of the structure of the alloying metal on the existence diagram of iron. 3. The effect of the percentage of chromium on the oxides formed on Fe-Cr alloys. 4. The relationships, if any, between the oxides formed and the protective quality of the oxides. The following alloys are included in this study: alloys of iron with body-centered cubic, face-centered cubic and other metals, 13 Cr-Fe, 18-8 stainless steel, K4²B, Nichrome V, Hipernik, Inconel, Stellite "²I," Refractaloy, Kovar, mild steel, a series of Cr-Fe alloys and a series of Co-Fe alloys. Since many of the commercial alloys in this list contain more than two metals, various complicating factors in the identification of the oxides formed may arise.

Jan 1, 1947

By Charles D. Borror, George K. Foster

The Jeffrey mine of the Canadian Johns-Manville Co., Limited, is in the town of Asbestos, situated approximately 100 miles northeast of Montreal and about the same distance southwest of Quebec, in Richmond County, Quebec. Mining operations were started in 1881 on outcrops on a hill, as a side-hill cut, followed by a second and third cut. This development was the forerunner of the present large open-pit operations, the mine now ranking as the largest open-pit asbestos mine in the world. Operations were first carried on by hand, then by horsepower and later by stem cableways. By 1924 the derrick spans, 2000 ft. or more long, became unwieldy. To overcome this, and also to eliminate hand labor as much as possible, steam shovels and railroad haulage were introduced. The steam shovels were replaced in 1928 by larger electric shovels of the full-revolving type. The Ore Body The ore body is a serpentinized peri-dotite rock mass. The chrysotile fibers form a network of veins throughout, varying from microscopic width to two or more inches measured across the veins (Fig. I). These veins may be continuous for a few or many feet; they may increase or decrease in width within a few feet. The veins in which the fibers occur per- pendicular to the veins are known as cross fiber. Those in which the fibers lay parallel to the veins are known as slip fiber. The cross fibers are of better quality, and more in demand. The majority of the fiber

Jan 1, 1948

By M. F. Hawkes, R. F. Mehl

The rate of isothermal transformation of austenite to pearlite depends upon the rate of nucleation, N, and the rate of growth, G, of pearlite in austenite. Values of N are given in terms of the number of nuclei forming in unit time per unit grain boundary area of unreacted austenite; values of C are given in terms of the linear rate of radial growth. Variations in the isothermal rate with temperature result from variation of N and G with temperature. Depth of hardening of a steel depends fundamentally upon values of N and G; changes in carbon and alloy content effect changes in N and G and thus affect depth of hardening. Quantitative studies are available on N and G for the formation of pearlite in plain carbon eutectoid steels.3 Systematic studies in this field are necessary if the phenomena are to be well enough known to furnish a proper basis for full rationalization and for theory. Accordingly, the studies are continuing, both with respect to the effect of alloying elements upon the values of N and G in the formation of pearlite and to the values of N and G for the formation of ferrite in hypoeutectoid steels. The present paper is the first relating to the effect of alloying elements upon the values of N and G for pearlite. It offers special interest since cobalt is known to have an anomalous effect upon the rate of formation of pearlite, accelerating it, whereas all other elements retard it.4 It will be shown that cobalt increases both N and G for pearlite and that this effect is inherent in the Fe-Co-C system and not dependent upon factors relating to austenite heterogeneity nor upon any recognizable adventitious factor. Inasmuch as the rate of diffusion of carbon in austenite and the interlamellar spacing of pearlite are variables related to G and possibly to N (in a manner not yet certain), measurements of the effect of cobalt upon them are also reported here. In the course of the work, measurements were made on the effect of cobalt upon the marten-site temperature and these are given. COBALT AS AN ALLOYING ELEMENT IN STEEL Properties of Cobalt Cobalt resembles iron more closely than does any other chemical element. Its atomic number is 27, hence it is the element immediately following iron in the periodic system. The two differ in atomic structure only in the fact that cobalt contains seven electrons instead of six in the third, or transition, level of .the third shell. The next shell, which is the

Jan 1, 1948

By T. S. West

Completion and production data presented for three wells in the Oakville area of Live Oak County, Texas, which were completed near the gas-oil or water-oil contact, indicate that coning may not be as prevalent a cause of failure in such cases as is commonly assumed. Failure in the cases discussed is indicated to be due instead to: (I) erosion of the formation, (2) flowing out of mud filter cake, or (3) failure of the cement. An open-hole gravel-pack type of completion procedure is proposed for preventing failures of this kind by preventing movement of all solid material in the space in which completion is made. Various combinations of layers of gravel, sand, and cement are utilized for this purpose. Experimental results and theoretical discussion as to the applicability of gravel pack completion are included. Introduction This paper is primarily a study of the reasons for failure of oil-well completions near the gas-oil or oil-water contact, and suggests a procedure for increasing the efficiency of this type of completion. The value of improvement in completion effectiveness near the gas or water zone is not confined, however, to wells of relatively thin oil columns. Thick oil columns become thin as depletion progresses. It would seem to follow that the minimum distance from the gas or water zone at which completion can be made in a new well indicates the limit to which depletion may be carried in a well having an oil column of any initial magnitude. Only four ways can be postulated in which high gas-oil or water-oil ratio can initially occur if the zone exposed for production is within the oil column: 1. Failure of the cementing material. 2. Vertical coning. 3. Failure along the boundary between the cement and the wall of the well. 4. Failure of the formation comprising the wall of the well. Cementing materials such as portland cement and plastics have reached a high stage of development. Failures of this type are probably due almost always to extraneous causes such as mud contamination rather than to faulty cementing material. Vertical coning can and obviously does occur. However, the usual occurrence of thin impermeable streaks in sand sections and the success with which open-hole drill-stem tests can be made near the gas-oil contact suggest that over-all effective vertical permeability, and in turn vertical coning, is less prevalent than frequently is assumed. Much has been written on failure by flowing out of the mud filter cake between cementing material and the formation. A filter cake is always present if, prior to cementing, mud has come in contact with a permeable formation at pressures exceeding the pressure head of the fluid it contains. Mechanical methods are in use for removing filter cake during the cementing operation? which undoubtedly are of

Jan 1, 1947

By George K. Foster, Charles D. Borror

The Jeffrey mine of the Canadian Johns-Manville Co., Limited, is in the town of Asbestos, situated approximately 100 miles northeast of Montreal and about the same distance southwest of Quebec, in Richmond County, Quebec. Mining operations were started in 1881 on outcrops on a hill, as a side-hill cut, followed by a second and third cut. This development was the forerunner of the present large open-pit operations, the mine now ranking as the largest open-pit asbestos mine in the world. Operations were first carried on by hand, then by horsepower and later by stem cableways. By 1924 the derrick spans, 2000 ft. or more long, became unwieldy. To overcome this, and also to eliminate hand labor as much as possible, steam shovels and railroad haulage were introduced. The steam shovels were replaced in 1928 by larger electric shovels of the full-revolving type. The Ore Body The ore body is a serpentinized peri-dotite rock mass. The chrysotile fibers form a network of veins throughout, varying from microscopic width to two or more inches measured across the veins (Fig. I). These veins may be continuous for a few or many feet; they may increase or decrease in width within a few feet. The veins in which the fibers occur per- pendicular to the veins are known as cross fiber. Those in which the fibers lay parallel to the veins are known as slip fiber. The cross fibers are of better quality, and more in demand. The majority of the fiber

Jan 1, 1948

By R. H. Hiltz, R. W. Douglass

Large-grain specimens of iodide titanium prepared metal-lographically were stain etched using the technique of New York University as modified by Watertown Arsenal Laboratories. Orientations of grains showing an abnormal response to stain etching were determined by back-reflection X-ray techniques. X-ray results showed that a-titanium grains, oriented such that their basal planes were parallel to the polished surface, have a slower reactivity to stain etching than any other orientation. Grains oriented such that their basal planes made small angles with the polished surface exhibited reaction rates between that of the true basal orientation and the normal rate. As the angle with the surface increases the reactivity increases up to a maximum angle of 14 deg. Basal planes making an angle with the surface of greater than 14 deg show normal reactivity to stain etching. These data, plus work on polycrystalline specimens, indicate that the oxidation rate of titanium might be reduced by correct alignment of crystal planes. ThE earliest observed phenomenon in the micrography of titanium was the occurrence of a grains which exhibited no birefringency. Even though a titanium possesses a hexagonal-close-packed structure and should be optically anisotropic, it can appear optically isotropic, when the crystal is so oriented that its intersection with the polished surface is perpendicular to the axis of symmetry. During the develoment of color staining techniques for titanium: it was noted that the a phase did not stain uniformly. Staining of specimens of commercially pure titanium resulted in a micro-structure of blue-colored grains, among which were randomly oriented a few grains exhibiting colors between the initial yellow and the final blue color. Under polarized light, these off-colored grains appeared to be optically isotropic. More intense study with polarized light, however, showed only the yellow grains to be isotropic. The intermediate colored grains exhibited weak birefringency, which at first glance is not detectable due to the strong birefringency of the surrounding structure. Aminoff2 and Straumanis3 have previously shown that in zinc the basal orientation is less reactive than other orientations. Leidheiser4 showed the same thing to be true for the hexagonal-close -packed configuration of cobalt. Thus, it would appear that the basal-plane orientation is responsible for the abnormality in stained titanium. Later work by Leidheiser5 on cobalt has shown that other planes besides the basal plane exhibited reaction rates slower than the normal rate. Reported planes were the (100), the (1011) and several planes making small angles with the basal plane. The last observance appears not to be due to the reactivity of the reported plane but due to the reactivity of the basal plane which is very close to being parallel to the surface. There are, then, two possible explanations for the range of colors observed in stain-etched a titanium. Since extensive research on the effect of orientation on surface reaction has failed to provide any definite trend, these two explanations are not adequate in themselves. Planes showing the retarded reactivity differ not only for different crystal structures but for metals of the same crystal structure and even for different reactions of the same metal. Tragert,6 Leidheiser,7 Tammann,6 and wagner9 have shown copper to exhibit retarded reactivity on the (111) plane. However, Leidheiser10 has shown that under other conditions the retarded reactivity of copper is associated with the (100)

Jan 1, 1960

By A. E. Bellis

ROBERT J. ANDERSON, Cleveland, Ohio (communication to the Secretary *).-The paper by Messrs. Bellis and Hardy was interesting to me and has led me to make a few remarks concerning some of the points brought out. The question of employing correct hardening temperatures is one that is sadly neglected, particularly in many large plants that forge and treat their machine tools for private use. As is most aptly remarked in this paper, "The custom of using one, high-speed temperature for all tools is very poor practice;" still, such practice is more common than otherwise. An instance came to my attention some time ago, in connection with some work with the standardization of high-speed steels for machine tools, where there were no less than six different brands of alloy steels being used for machine tools such as lathe, shaper, planer, boring mill and cutters of like nature. All of these different steels received identical heat and forging treatment-or at least that was the aim of the tool hardener. That the results were highly unsatisfactory goes without saying. That the hardening department of many plants is conducted on a rule-of-thumb fashion is the reason for a great deal of the trouble and disappointment which seems to be the lot of many tool-steel users. Exceedingly crude execution is the rule rather than the exception, and it is no small wonder that the results are as good as they sometimes happen to be. It would seem that at the present price of alloy steels the subject should receive a closer scrutiny by purchasers than it does. One not familiar with the workings of souse plants that disdain to lend an ear to scientific heat treatment would scarcely give credence to some of the methods employed, not only in the treatment of the steel but also in its selection and purchase. Heating for hardening should be conducted under close pyrometric control only after the correct hardening temperature has been determined.

Jan 3, 1917

By J. W. Halley, G. L. Plimpton

BECAUSE of the two distinct stages in the solidification of rimmed steel, segregation in the rimmed ingot is more complex than that in the killed or semikilled ingot. In the earlier stage, chemical reactions, resulting in evolution of gas and vigorous stirring of the metal, effect a degree of negative segregation unique to rimmed steel. The composition of this zone constitutes the principal quality advantage of this type of steel. In the later stage of solidification, after the evolution of gas has ceased, the segregation follows the general pattern of a more completely deoxidized steel. However, the composition of the liquid remaining after the first solidification stage varies markedly from that of the original melt, some constituents having been partially removed as reaction products while the concentration of others has been intensified by rejection from the metal solidifying in the first zone. The aim, from the standpoint of segregation, in rimmed steel of high quality is to effect a maximum negative segregation in the rim zone without excessive concentration of undesirable elements at the center of the ingot. To achieve this aim, the composition of the melt may be varied and the furnace and pouring practice may be adjusted within certain limits. It is the purpose of this study to discuss segregation in rimmed steel from the standpoint of the mechanisms that produce it and to survey the phases of open-hearth practice that influence those mechanisms. MECHANISMS PRODUCING SEGREGATION The mechanisms that determine the degree of segregation in the rimmed ingot are closely interrelated, making it difficult to select the primary factors and to determine a satisfactory order for presenting them. For instance, the question of sulphur segregation is relatively simple, since sulphur is not directly involved in chemical reactions in the ingot; but its concentration in the rim zone is dependent not only on its original analysis in the melt, its segregation coefficient, and the freezing rate, but also on the rate of its removal from the impure film on the solidifying surface. This washing action involves all the factors (such as freezing rate, the carbon-oxygen product, pressure, etc.) that determine the rate of gas evolution and hence the efficiency of film removal. Sulphur distribution between the rim and core is affected by the volumetric ratio between the two zones, and its segregation in the core is a function not only of the freezing rate of the core but also of all the foregoing factors that determine its concentration in the metal when solidification of the core starts. To simplify the presentation, it is proposed to treat the mechanisms affecting segregation independently in this section, reserving a discussion of their over-all effects for the section in which actual segregation data are given. The factors affecting segregation will be treated in the following order: (I) differential solidification, (2) removal of constituents as

Jan 1, 1944

By M. S. Burton, G. V. Smith, A. Rosen

The kinetics of re crystallization and the effect of recovery on recrystallization of pure iron were investigated within the temperature range of 517" to 632 OC. Grain growth and activation energies were also studied. Two stages can be distinguished during recrystallization; the first is gvowth-controlled and the second is nucleation-controlled. The extent to which the first stage succeeds before the second stage begins depends on both temperature of recrystallization and temperature of recovery. The softening of cold-worked metals and alloys due to transformation of the deformed crystals to strain-free equiaxed grains during annealing is well-known, and early inestiators established that recrystallization kinetics is strongly influenced by minute quantities of impurities. Generally, it is believed that impurities decrease the rate of recrystallization and the rate of grain growth. To understand the basic phenomena of recrystallization, investigations should be on pure materials. Most of the research on high-purity materials has been on metals having the fee Bcc materials, and especially high-purity iron, have been studied only in recent years. It is known that recovery may influence recrystalliation;" however, no general description of the influence, applicable to all materials, has been presented. This paper presents results of a study of the recrystallization kinetics of high-purity iron, after 60 pct cold deformation by drawing, with particular reference to the influence of recovery on the rates of recrystallization and grain growth. From observations of these rates, conclusions are drawn concerning nucleation. MATERIAL AND EXPERIMENTAL PROCEDURE Preparation of Material. High-purity iron, prepared by zone refining of vacuum-melted electroiytic iron at Battelle Memorial Institute under sponsorship of the American Iron and Steel Institute, was used in this study. Table I gives the reported chemical analysis of the material, taken at a point near the last molten zone and thereby rep- resenting the maximum impurity level for the entire bar. Prismatic specimens, approximately 10 x 10 X 50 mm, were sawed from the 50-mm-diam bar, perpendicular to the zone-refining direction, and turned to cylindrical shape. These specimens were sealed in quartz capsules under vacuum, approximately 10"e mm Hg, austenitized at 930° C for 15 min, slowly cooled, removed from the capsules, and cold-worked in air by swaging to approximately 20-pct reduction of area. The encapsulating, austenitizing, and swaging operations were repeated two additional times, after which the samples were encapsulated, austenitized, and cold-drawn to 60-pct reduction of area. A further vacuum anneal at 630°C for 120 min and cold drawing to 60-pct reduction of area produced wire 2.8 mm in diameter. The drawn wire was electropolished to remove deformed material on the surface, after which it was sawed into 4-mm-long specimens for the recrystallization study. Microscopical examination before the final cold reduction revealed equiaxed grain structure with very fine grains in a thin layer near the surfaces of the specimen and nearly uniform ASTM 3-4 grain size in the center. Recrystallization Heat Treatment. a) Direct Recrystallization of Cold-Worked The 60 pct cold drawn iron specimens were recrystallized at five temperatures, 517, 556, 590°, 612, and 632C, in a lead bath covered with graphite (the temperature was controlled to 1°C). Specimens were treated for twelve different times at each temperature, and all were water-quenched after heat &eatment. b) Recrystallization Following Preliminary Recovery Heat Treatment. After cold working, specimens were sealed into quartz capsules under vacuum, 105 mm Hg, and recovery-annealed at 362", 400", and 440°C for 20 hr prior to recrystallization. No evidence of recrystallization was found

Jan 1, 1964

By L. A. Delano

During 1916, the St. Joseph Lead Co. milled 2,505,670 tons of ore. This is a daily operating average of 7855 tons. The economic concentration of such a large tonnage necessarily requires a plant equipped with modern machinery and operated efficiently. The milling process used in producing this output has been a gradual development through the long period of years that the company has been in existence. HISTORICAL SUMMARY OF MILLING PRACTICE Ore was first mined at Bonne Terre, Mo., in 1864. The early milling practice was crude. It consisted of breaking the ore into small pieces by hand, pulverizing in a Blake crusher and a pair of Cornish rolls to approximately minus 6 mm., and jigging in the old-fashioned hand jigs. Only the coarse heavy galena was saved, the gangue being shoveled off and discarded. The output for the first year under this method was only 240 tons of pig lead. The first mill of the company was a combination of extensions and additions built from time to time as the mines developed. It was a museum of early milling machinery, such as jigs, percussion tables, buddies, dolly tubs, log washers, etc., following no definite flow sheet. The chats, or tailings, were hauled to waste dumps by mule and ox teams, as much as 500 tons per day being moved in this manner, until a railroad was built in 1880. This mill was burned in 1883, at which time the annual output had reached approximately 7300 tons of pig lead. A new mill of 500 tons capacity was designed and built by C. B. Parsons. This mill has been admirably described by H. S. Munroe.' The ore was crushed in Blake crushers, Cornish rolls, through 6-mm. screens, and treated by jigs of the Parsons type, percussion tables and log washers, or trunking machines, for cleaning the galena. The middlings were recrushed in rolls and treated on Harz jigs. The mill was operated without change, except later installing Gates crushers and en-

Jan 1, 1918

By Charles Eichrodt

THE ore that is being treated by the present plant lies between the leached zone, or capping, and the mixed sulfide and oxide zone. The principal copper minerals are chalcanthite (CuSO4.5H20), brochantite (CuS04 3Cu (OH)2) and atacarnite, (CuC12.3Cu (OH)2). There are, in addition, some other minerals such as cuprite and kröhnkite (CuSO4. Na2SO4.2H20). These minerals, with many others, occur in a greatly crushed granodiorite rock. Most of the copper-bearing minerals occur in the cracks and veinlets, but there are disseminated values and it is probably the relative proportion of these that accounts for some otherwise unexplainable variations in extraction. The entire mineralization of the ore is complex and varies with depth. This variation, the problems presented thereby, and the effect of various constituents of the ore will be taken up in detail. An analysis of an unweighted composite of the ore treated during 1927 follows:

Jan 1, 1930

By R. D. Reiswig, J. M. Dickinson

The 0s-Ir equilibrium diagram was determined. The diagram is of the simple peritectic type, with a peritectic temperature of about 2660°C. The solid miscibility gap is narrower than previously reported, the nearly vertical solvus lines occurring at about 42 and 63 wt pct 0s. Widmanstaetten figures resembling martensite in some of the two-phase alloys account for a previously suspected transformation. In view of the long history of use of such alloys, it is surprising that the 0s-Ir equilibrium diagram has not yet been completely determined. The boundaries of the miscibility gap in this system have been estimated to be between 24 and 39 wt pct 0s and 79 and 100 wt pct OS. It has been predicted3 that alloys of ruthenium, osmium, and rhenium with the fcc platinum metals should solidify peritectically in their two-phase regions. The metallographic examination of natural osmiridium alloys has been said4 to indicate, by the presence of a martensitic structure, the existence of a transformation or a phase separation. On the basis of superconducting transition temperature measurements, a 70 at. pct 0s alloy was found5 to be two-phase prior to annealing. EXPERIMENTAL The elemental components used in this work were obtained from several suppliers as sponge. The purities, stated by each supplier to be in excess of 99.8 pct, were confirmed in each case by a semiquantitative spectrographic analysis. The pure components were premelted in an inert-gas tungsten arc furnace with the evolution of some fume, crushed, and pickled for use as alloy melting stock. Upon arc melting to the final compositions, no fume evolution was observed. Because weight losses of the order of 15 mg or less were observed in preparing alloy buttons weighing 15 g, "synthetic analyses" were used in determining the compositions of the alloys. Alloys used in this investigation contained 15, 20, 33, 40, 42, 43, 45, 50, 55, 60, 63, 64, 66, 70, 79, and 80 wt pct 0s. Heat treatments of the alloy buttons and pieces thereof were performed in a previously described6 tungsten tube furnace under pressures of 105 torr or less. It was found that homogenization treatments on the specimens were essential to remove the severe coring which was present, a 3-hr treatment above 2300°C removing all the metallographi-cally visible evidence of coring. Following the various heat treatments, the specimens were "vacuum-quenched" by melting a tungsten fuse wire and allowing them to drop onto a water-cooled copper plate. In a few instances, specimens were quenched into molten tin for comparison, but no difference was apparent. Vacuum-quenched specimens cooled from 2400°C to below a red heat in less than 60 sec. Typical equilibration times varied from 3 hr above 2300°C to 88 hr near 1100°C. The utilization of successively longer equilibration times and the approach to equilibrium from both directions indicated that the times used were sufficient to give a close approach to true equilibrium. Heat-treatment temperatures were measured with a calibrated Leeds and Northrup optical pyrometer through a 0.120-in. lateral sight hole in the tungsten heater tube. It was known that the assumption of black-body conditions inside the 1-in.-diam by 10-in.-long tube was unwarranted. The empirical results of work with thermocouples and melting

Jan 1, 1964