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By H. O. Hofman

With the exception of the exhaustive paper on the Father de Smet mill, by its designer, Mr. A. J. Bowie, Jr. (Bans., x. 87), nothing, so far as the writer is aware, has as yet appeared on the stamp-mills of the Black Hills of Dakota, although they have been steady producers for the last ten years. Within the small area of about 6000 by 1600 feet, $2,271,341.14 was produced in 1887† from rock averaging $4 per ton in free gold. I. The Ores. Character of the Ores.—The gold of the district is found in quartz and pyrites finely distributed through vast bodies of mica- and amphibole-schists, argillites and phyllites, and also impregnating the schists themselves. The " Belt," embracing the section of Lead City, Terraville and Central City, is the only part worked at present. The principal associated mineral is iron pyrites, with some arsenopyrite and chalcopyrite, garnet and asbestos. The ores from open cuts and upper levels are more free-milling. than those from underground workings below water-line. Hence

Jan 1, 1889

By F. J. Plecity, J. T. Michalak, W. C. Leslie

Isothermal recrystallization and grain growth in zone- and vacuum-melted irons and Fe-Mn alloys, up to 0.60 pct Mn, were studied in the range 480° to 650° C, after 60 pct cold reduction. In initial stages, rate of grain growth and rate of recrystallization of iron decrease with time. The recrystallization is typical of a growth-controlled process, and rate of growth is determined by the extent of recovery. Mn decreases rates of growth and of recrystallizatzon. The recrystallization process changes at about 0.30 pct Mn and nucleation may become time-depetzdet~t. In recent years, considerable effort has been expended in determining the effects of solute elements on recrystallization and boundary migration in fcc metals. The results have indicated that the effects produced by single solute additions are dependent upon both the element added and its concentration.'-' In contrast, there have been very few attempts to determine the characteristics of recrystallization and boundary migration in high-purity bcc metals, especially after heavy deformation, and the effects thereon of single solute elements.9-11 This study was undertaken to determine the recrystallization characteristics of various "high-purity" irons and the effects of manganese additions at two levels of base purity. It was hoped that the information obtained would improve our understanding of the recrystallization of pure metals and aid in formulating a theory for the effect of solute elements. The interest was not entirely academic, for the annealing of low-carbon steels, which is of very great commercial importance, is but poorly understood. MATERIALS The compositions of the irons and iron-manganese alloys used are listed in Table I. The zone-melted iron and Fe-Mn alloys were made by Battelle Memorial Institute. Iron S-1 was arc-melted in a water-cooled steel mold in an argon atmosphere. The ingot was forged into a bar, then given two horizontal zone-refining passes in an alumina boat. Iron V-4 was treated in a similar manner, but was not zone-refined. The iron for the zone-melted Fe-Mn alloys was induction melted in vacuum in MgO crucibles and cast into alumina molds. The ingots were forged into bars, machined to shape, and a groove milled down one side of each. The best available electrolytic Mn was placed in the grooves, and the bars were zone melted. The vacuum-melted Fe-Mn alloys were induction melted in this Laboratory in MgO crucibles and poured into cast-iron molds. Iron V-5 was purchased from National Research Corp. in the form of a small vacuum-cast ingot. The low-carbon steel was made by induction melting in air at the U.S. Steel Corp. Applied Research Laboratory. The history of the materials prior to the final cold reduction differed; these details are given in the Appendix. The penultimate grain size of the principal materials was kept in the range ASTM 2 to 4, except for the low-carbon steel. PROCEDURES The cold work prior to the final recrystallization anneal was kept constant at 60 pct. It is known that rolling procedure can influence the kinetics of recrystallization of ironI2; therefore, all specimens were rolled in one direction only, between clean,

Jan 1, 1962

By C. F. Jr. Tolman

IN February 1913, Prof. L. C. Graton and Dr. Joseph Murdoch1 presented to the American Institute of Mining Engineers a notable contribution to economic geology under the title The Sulphide Ores of Copper. The value of the work was recognized by mine operators, and Mr. Graton was assisted in his plan to extend his investigations,. by the organization of a commission to undertake a "secondary enrichment investigation." In this work lie secured the cooperation of the Geophysical Laboratory of the Carnegie Institution of Washington. Their report 2 on the chemical phases of the investigation has just been published. Incidental to investigations 3 carried on in my laboratory by advanced

Jan 2, 1916

By R. J. Teitel

The Pb-U system has been investigated by X-ray, thermal, and microscopic analyses. Two pyrophoric intermetallic compounds were found; UPb3 and UPb. The crystallographic structure of UPb3 is reported. A phase diagram was drawn for the system showing three eutectic and one syntectic reaction. AS a result of the interest in uranium metallurgy, the Pb-U system has been investigated. Practically no quantitative data appears in the literature concerning this system. Chips were machined from bars of high-purity uranium obtained from Ames Laboratory and the lead was 99.9 pct high-purity grade from Bel-mont Smelting & Refining Co. The chips were pickled in a dilute solution of nitric acid, washed in water and then alcohol, and dried prior to use for alloy preparation. The lead was simply sheared from the pig with no chemical treatment. Lead and uranium were placed in graphite crucibles and loaded into an induction furnace. In order to insure good alloy formation, the lead was loaded above the uranium to wash the uranium chips into the melt. After the charge was held at the desired preparation temperature for 15 to 30 min, it was allowed to cool in the crucible. The entire melting operation was accomplished in an atmosphere of helium (double charcoal refined grade with no further treatment). The procedure was to outgas the furnace by first evacuating it to 10-% m Hg, admitting helium to 8 psi gage and sealing the furnace off. An optical pyrometer focused on the charge through a hole in the crucible cover was employed for thermal measurements. Usually a 50° to 70°C correction had to be added to the instrument value. The most suitable alloy preparation temperature range was found between 1220° and 1280°C. The reason for this is explained by the phase diagram, Fig. 7. Above this temperature range two liquids separate preventing alloy formation upon cooling at a reasonable rate. On the other hand, below this range the uranium was coated with a layer of both compounds and the rate of reaction was diminished by diffusion processes. The fastest reaction rate occurred in this narrow range of temperature because only UPb coats the uranium and it evidently does not protect the uranium as well as UPb,. Apparatus and Procedures The development of apparatus and techniques was determined by the peculiar properties of the alloys. All the alloys were pyrophoric, and, consequently, the alloys had to be protected from oxidation by handling them in a dry box or inert atmosphere furnaces. Other operations performed outside of this equipment had to be done as quickly as possible. Thermal analyses were conducted in a furnace and arrangement similar to that described by the author.' Graphite crucibles having a thermocouple well in the bottom were used to contain the prepared alloy, while a helium atmosphere protected the melt from oxidation. The furnace was outgassed by pumping a 10-3 mm Hg vacuum until the furnace had been heated to 400°C. Then helium was admitted and the furnace sealed under 8 psi gage pressure. Chromel-alumel thermocouples were used for thermal analysis and the accuracy of thermal measurements was judged to be k 5°C. At first, an attempt was made to use platinum-platinum-rhodium thermocouples, but evidently lead vapors attack it at high temperatures forming low melting alloys. These lead vapors had direct access to the thermocouple because the graphite crucible was porous. A differential temperature control was used to regulate thermal analyses. The thermal gradient across an alundum tube placed between the windings and the crucible was maintained constant by a controller.

Jan 1, 1953

By Maurice L. Pinel, Thomas T. Read, Thomas A. Wright

THE erroneous, but until recently widely prevalent, belief that iron castings were first made in Europe in the fourteenth century has been adequately refuted in a number of earlier papers;1,11,12 but except for an unpublished metallographic study by the late William Campbell, and a phosphorus analysis by T. A. Wright of the metal of the Han dynasty cast-iron stove described by Laufer,2 nothing was known of either the chemical composition or the metallographic structure of the metal of any ancient iron casting, although data on castings of recent manufacture are abundantly available. The metal of the stove, which had been buried in a grave for at least 15 centuries, was so corroded that it seemed inadvisable to publish the results on it until more and better specimens from other ancient castings could be obtained. During a journey through China, extending from Peking in the north to Canton in the south and Cheng-tu, Ssu-chuan, in the west, in the late summer and autumn of 1936, one of us (T. T. Read) was fortunate enough to obtain, and bring home for study, nine castings, all more than 1000 years old, of which the date of manufacture is precisely known because of inscriptions cast in them, another that lacks a dated inscription, but of which the date, as explained below, can be otherwise established, and a specimen from the largest iron casting ever made," which is also dated. The period covered by this suite of specimens extends from 502 to 1093 A.D. In addition, a sample was obtained from a casting of date unknown, but which was certainly cast before 1000 A.D. and possibly as early as the third century A.D. A detailed description of these specimens is as follows: 1. 502 A.D. A pair (right and left) of recumbent lions (Fig. 1). Base 7 ¼ by 14 3/8 in., height over-all 5 ½ in., weight 26 lb. each. The translation of the inscription on the base is: "Made on the twenty-fourth day of the seventh month of the third year of Ching Ming of Great Wei" (Sept. 11, 502 A.D.).

Jan 1, 1938

By Stanley J. LeFond, Neal Davis

Drilling an oil well or most other types of drilling or coring is no longer a simple and uncomplicated operation. Drilling today at depths which exceed 9144 m (30,000 ft) is hazardous and requires personnel with long and varied experience in drilling. It also requires extensive experience and knowledge in the use of materials which are added to the drilling fluid or "mud," more often than not materials utilizing an industrial mineral. The drilling fluid can vary from a simple mixture of water and "mud" to a very sophisticated, scientifically compounded drilling fluid. Industrial Minerals Used in Drilling Fluids Industrial minerals which are commonly used in oilwell drilling and completion are listed in Table 1. The most important minerals, determined by sales, are bentonite and barite. The other minerals listed are either used to achieve a specific purpose or are used regularly but in limited quantities. The main suppliers of drilling fluids internationally are Magcobar Div., Dresser Industries, Inc.; Baroid Div., National Lead Co.; IMC Drilling Mud Co., (a subsidiary of international Minerals and Chemicals Corp. and Halliburton Co.); and Milchem, a division of Baker Industries. Most of the industrial minerals are found in North America, with barite mines and processing plants located in Nevada, Arkansas, Missouri, and Arizona, and bentonite mines near Graybull, WY. Other mines, such as those in Nova Scotia, are capable of shipping to South America and to the European and Middle East countries. Most of the materials processed by any of the suppliers must conform to specifications set by the American Petroleum Institute (API) or the Oil Companies Material Organization (OCMA). These specifications provide for uniform physical and chemical properties of the materials to be sold on the open market. Function of Drilling Fluids In the early days of rotary drilling, the primary function of drilling fluids was to bring the cuttings from the bottom of the hole to the surface. Today it is recognized the drilling fluid has at least ten important functions: 1) To remove the cuttings from the bottom of the hole and carry them to the surface. 2) To cool and lubricate the drill string and drill bit. 3) To build an impermeable cake on the wall of the hole. 4) To control subsurface pressures. 5) To hold cuttings and weight material in suspension when circulation is interrupted. 6) To release sand and cuttings at the surface. 7) To support part of the weight of drill pipe and casing. 8) To reduce to a minimum any adverse effects upon the formation adjacent to the hole. 9) To insure maximum information about the formation penetrated. 10) To transmit hydraulic horsepower to the bit. In order to accomplish some or all of these functions while penetrating formations of various characteristics, several types of drilling fluids systems have been designed. Types of Drilling Muds There are two basic drilling fluid systems-water-base muds and oil-base muds. There is a wide variety of groups within these two main

Jan 1, 1983

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 Waldemar Lingren

CONTENTS. PART I.-GENERAL FEATURES. [ ]

Jan 1, 1902

By O. D. Sherby, J. L. Lytton, C. R. Barrett

Randomly oriented polycryslalline copper of 99.995 pcl was tested in tension at temperatures of 626o, 496o, and 406o. The gvain-size mnge investigated was from 0.03 to 0.7 mm. Grain sizes were produced by two techniques: 1) varying the amount of prior cold work and the amealing time at constant annealing temperature so as to obtain various vecrystallized grain sizes with minimum grain growth, and 4 holding the prior cold work constant while varying the annealing time or temperature so as to obtain varying grain sizes by grain growth. Polycrystalline samples (grain size of 0.03 mm) with a strong. [001](100) texture were also studied. The relationship between the steady-state creep rate, Es, and pain size was found to be the same indepentent of the technique used to prepare the various grain sizes. For specimens with grain diameters above about 0.1 mm ea zuas esse)ztiallj~ independent of grain size, while for smaller grain diameters Cs increased slightly with decreasing grain size. Strongly textured polycrystalline copper, which contained low-angle grain boundaries, exhibited steady-state creep rates that were slightly lower than those observed in randomly oriented copper, of the same gain size. The results are explained by conside?%ng- the contribution of grain boundary shearing to the total strain and the effect of grain size on the resulting creep substructure. EXPERIMENTAL observations concerning the influence of grain size on steady-state creep rates are varied and oftentimes conflicting. Numerous early investigators found that an increase in the grain size resulted in a decrease in the high-temperature steady-state creep rate, i,.'-" Other workers have foundthat ef decreases with increasing grain size up to some optimum grain size and then increases with a further increase in grain size.'- '' It has been suggested that es, decreases with an increase in grain size only because the range of grain sizes studied normally lies to the left of the grain size for optimum creep resistance. However, sherbyl2 and Feltham and his co-worker13, 14 have found that even for small grain sizes 2, does not always decrease with an increase in grain diameter but may be proportional to the square of the grain diameter. A possible explanation for the different creep rate-grain size relationships which have been observed is that in most experimental studies different grain sizes have been prepared by annealing at various temperatures. For metals in which the impurity concentration is high (greater than about 0.1 at. pct) this type of

Jan 1, 1968

By Norman P. Goss

What would appear to be a very simple process on paper has proved to be overrun with a multitude of unseen difficulties. For more than 70 years attempts have been made to cast metals in a continuous manner, but it has been only within the last Io years that some degree of success has been achieved.1 Historical Development Bessemer's Experiments—Method I Bessemer was the first to try to cast molten metal in a continuous manner. His method is fully described in U. S. Patent No. 49053, issued in 1865. The patent drawing is shown in Fig. I. In this method the molten metal was poured between a pair of rolls of large diameter, which were cooled by water sprays. Means were provided to prevent moisture from coming into direct coptact with the molten metal. The width of the strip was controlled by the flanges. On paper this should work to perfection, but it is beset with many difficulties still awaiting solution. Bessemer failed to reduce his invention to commercial practice. About 1890 Bessemer's method was revived by Norton and associates (U. S. Patent No. 441375). They formed the Fluid Metal Rolling Co. at Maywood, Ill., and spent $250,000 in endeavoring to develop the technique for this simple method. Finally they had to abandon it. Naturally, they did carry the technical development far beyond anything Bessemer had done, but even so it was far from being a useful commercial success. In recent years it has undergone further development by C. W. Hazelett (U. S. Patent No. 2058447), who has succeeded in obtaining long lengths of copper, brass, aluminum, and even stainless steel. He introduced many' ingenious devices but the greatest obstacle still remained—the disintegration of the roll surface when the surface is heated and chilled in rapid succession. Difficulty is also experienced in maintaining a uniform supply of molten metal to the rolls. The patents pertaining to this method would indicate these to be the major obstacles. Experimental work by Mellen—Method 2 A departure from the method introduced by Bessemer, was tried by Grenville Mellen, of East Orange, K. J., sometime between 1914 and 1920, who obtained a number of patents.2 His method is illustrated in Fig. 2. This method failed to make an impression upon the art; however, it is of value in pointing out the difficulties the inventor ran into and the way in which he tried to meet them. The split mold sections form two endless chains. When going through the center of the apparatus, these sections engage each other to form a complete mold. As the engaged mold section moves downward at a constant speed, molten metal is teemed into it. As this is going on, another set of cooperating mold sections move into position on top of the one being filled. The molten metal is teemed into the mold through a silica tube. According to the teachings of this patent, the level of molten

Jan 1, 1945

By E. S. Davenport, R. J. Hafsten, R. A. Grange

The influence of austenite grain size upon the hardenability of steel is now fairly well understood; for a given austenite, increasing the grain size increases the depth of hardening, and, since the latter is related to the fundamental transformation behavior of austenite, it follows that austenite decomposition must, in general, be retarded by increasing grain size. To date, very little quantitative information bearing directly on the effect of austenite grain size upon the progress and result of isothermal transformation has been published. Davenport and Bain,' and Zimmerman, Aborn and Bain2 have shown that the transformation is definitely relarded in hypereutectoid plain carbon steels at temperatures near and above the upper region of rapid transformation (Ar') when the austenite grains are increased in size. More recently, Griffiths. Pfeil and Allen3 investigated the effect of a series of different heating (austenitizing) temperatures upon the progress of isothermal transformation at 1245°F. (675°C.) and 745ºF. (395°C.) in a medium carbon, low-alloy steel; while they reported no measurements of the austenite grain size, their results suggest that increase in grain size retards austenite transformation at 1245ºF. (675°C), but has no appreciable effect at 745°F (395°C.). The present paper deals with the results of a study of the isothermal transformation of austenite in a single commercial alloy steel in which a fine-grained or a coarsegrained state was induced by appropriate selection of austenitizing temperature. The data are presented in the form of isothermal transformation diagrams, which clearly show that coarsening the grains lessens the rate of transformation of austenite to proeutectoid ferrite and pearlite—that is, at temperature levels above about 1000°F. (540°C.)—but is without significant effect at lower temperatures where the transformation product is bainite or martensite. It is to he presumed that the foregoing statement would be valid, at least in principle, for many other grades of steel; it confirms again that the mechanism of transformation to a pearlitic structure is fundamentally different from that to an acicular structure. A number of related observations were made, which seem to throw some light on the transformation process as it takes place in alloy steels, particularly at temperature levels in the vicinity of 1000ºF. (540°C.), where the transition from lamellar to acicular structures occurs. These data are discussed briefly in the belief that they may lead to a clearer understanding of this aspect of the subject. Material and Experimental Procedure The material investigated was a cornmercial grade of S.A.E. 4140 steel, the composition of which was as follows: 0.37 per cent C, 0.77 per cent Mn, 0.98 per cent Cr and 0.21 per cent Mo. It was hot-rolled to a 1 1/8-in. round bar and normalized by air-cooling from 1800°F. (980°C.).

Jan 1, 1941

By R. J. Hafsten, E. S. Davenport, R. A. Grange

The influence of austenite grain size upon the hardenability of steel is now fairly well understood; for a given austenite, increasing the grain size increases the depth of hardening, and, since the latter is related to the fundamental transformation behavior of austenite, it follows that austenite decomposition must, in general, be retarded by increasing grain size. To date, very little quantitative information bearing directly on the effect of austenite grain size upon the progress and result of isothermal transformation has been published. Davenport and Bain,' and Zimmerman, Aborn and Bain2 have shown that the transformation is definitely relarded in hypereutectoid plain carbon steels at temperatures near and above the upper region of rapid transformation (Ar') when the austenite grains are increased in size. More recently, Griffiths. Pfeil and Allen3 investigated the effect of a series of different heating (austenitizing) temperatures upon the progress of isothermal transformation at 1245°F. (675°C.) and 745ºF. (395°C.) in a medium carbon, low-alloy steel; while they reported no measurements of the austenite grain size, their results suggest that increase in grain size retards austenite transformation at 1245ºF. (675°C), but has no appreciable effect at 745°F (395°C.). The present paper deals with the results of a study of the isothermal transformation of austenite in a single commercial alloy steel in which a fine-grained or a coarsegrained state was induced by appropriate selection of austenitizing temperature. The data are presented in the form of isothermal transformation diagrams, which clearly show that coarsening the grains lessens the rate of transformation of austenite to proeutectoid ferrite and pearlite—that is, at temperature levels above about 1000°F. (540°C.)—but is without significant effect at lower temperatures where the transformation product is bainite or martensite. It is to he presumed that the foregoing statement would be valid, at least in principle, for many other grades of steel; it confirms again that the mechanism of transformation to a pearlitic structure is fundamentally different from that to an acicular structure. A number of related observations were made, which seem to throw some light on the transformation process as it takes place in alloy steels, particularly at temperature levels in the vicinity of 1000ºF. (540°C.), where the transition from lamellar to acicular structures occurs. These data are discussed briefly in the belief that they may lead to a clearer understanding of this aspect of the subject. Material and Experimental Procedure The material investigated was a cornmercial grade of S.A.E. 4140 steel, the composition of which was as follows: 0.37 per cent C, 0.77 per cent Mn, 0.98 per cent Cr and 0.21 per cent Mo. It was hot-rolled to a 1 1/8-in. round bar and normalized by air-cooling from 1800°F. (980°C.).

Jan 1, 1941

By E. C. Patton

Jan 1, 1947

By E. C. Patton

Jan 1, 1947

By Russell W. Dayton

The metallurgical polarization microscope has been utilized in several researches in the last few years, thus attaining a fair degree of prominence, but little has been written in a manner suitable to a metallurgist concerning the theory of this instrument. In this investigation the theory was carefully studied, and the results are presented here in a detailed manner, yet as simply as possible. The theory is discussed with particular reference to the three chief functions of the instrument: (1) determination of anisotropy; (2) effect of strain; and (3) identification of inclusions. Each of these is investigated experimentally, with especial attention to the mechanism of producing any effect. Where possible, the discussion is supplemented by photomicrographs. The instrument used had numerous defects as a polarization microscope; these and their remedies are discussed. In the microscopic study of transparent mineral sections (chalcography) the use of polarized light has aided tremendously in the identification of a mineral. The determination of strain in transparent substances (photoelasticity) by the use of polarized light has lately become a commercial process, used in testing finished glass articles. The success of the use of polarized light with opaque materials has not been so great. The magnitude of the effects obtained is much less than that of the corresponding effects with transparent materials, and the mechanical difficulties are much greater. Königsberger,"' i in 1909, was the first to apply polarized light to the microscopic study of opaque substances; Endell and Hanemann(2) were the next, in 1913. In 1919 and 1920, Wright(3,4) prepared two papers on the subject. In the first he developed the detailed mathematical theory from the viewpoint of the electromagnetic theory of light, and in the second described the various methods in use, giving improvements of his own. Schwarz(5)

Jan 1, 1935

By Russell W. Dayton

The metallurgical polarization microscope has been utilized in several researches in the last few years, thus attaining a fair degree of prominence, but little has been written in a manner suitable to a metallurgist concerning the theory of this instrument. In this investigation the theory was carefully studied, and the results are presented here in a detailed manner, yet as simply as possible. The theory is discussed with particular reference to the three chief functions of the instrument: (1) determination of anisotropy; (2) effect of strain; and (3) identification of inclusions. Each of these is investigated experimentally, with especial attention to the mechanism of producing any effect. Where possible, the discussion is supplemented by photomicrographs. The instrument used had numerous defects as a polarization microscope; these and their remedies are discussed. In the microscopic study of transparent mineral sections (chalcography) the use of polarized light has aided tremendously in the identification of a mineral. The determination of strain in transparent substances (photoelasticity) by the use of polarized light has lately become a commercial process, used in testing finished glass articles. The success of the use of polarized light with opaque materials has not been so great. The magnitude of the effects obtained is much less than that of the corresponding effects with transparent materials, and the mechanical difficulties are much greater. Königsberger,"' i in 1909, was the first to apply polarized light to the microscopic study of opaque substances; Endell and Hanemann(2) were the next, in 1913. In 1919 and 1920, Wright(3,4) prepared two papers on the subject. In the first he developed the detailed mathematical theory from the viewpoint of the electromagnetic theory of light, and in the second described the various methods in use, giving improvements of his own. Schwarz(5)

Jan 1, 1935

By L. T. Larson, M. L. Picklesimer

The relationship between the apparent angle of rotation of monochromatic plane polarized light and the tilt of the basal pole from the surface normal has been experimentally determined for zirconium over the wavelength range of 500 to 655 mp. This relationship allows the determination of the spatial orientation of the basal pole of an individual grain in a polycvystal-ling zivrconium specimen to within ±3 deg by three simple tneasurements with a polarized-light metallurgical microscope. The method of measurement is discussed in detail. THE optical anisotropy of materials having noncubic crystal structures has long been used to reveal features by polarized-light microscopy. Petrographers have used measurements of certain optical properties to identify and classify transparent or translucent minerals. More recent work (i.e., Cameron1) has extended such measurements to opaque minerals in reflected light. Few attempts have been made to make similar measurements on noncubic metals. Couling and pearsall2 have reported that a sensitive tint plate can be used in a polarized-light metallurgical microscope to determine the position of the basal-plane trace in a grain of polycrystalline magnesium. Reed-Hill3 has reported that the same technique can be used for zirconium. We have found that the precision of measurement can be increased to about ±0.5 deg by using a Nakamura plate4,5 to determine the exact extinction position after the sensitive tint plate has been used to locate approximately the basal-plane trace. This report describes a method for measurement of another optical property, the apparent angle of rotation. This measurement permits determination of the angle between the basal pole of a grain of a hcp metal and the normal to the surface of the specimen. When the two measurements are combined, the orientation of the basal pole in space can be determined from three simple measurements on a single surface. One to two hundred such determinations will permit plotting of a basal-pole figure for the polycrystalline material with reasonable accuracy. When normally incident, monochromatic, plane-polarized light is reflected from the surface of an optically anisotropic material, the light may be converted to elliptically polarized light, the plane of vibration may be rotated, or both may occur. The el- lipticity, the angle of rotation, and the reflectivity can be related to the indices of refraction and the absorption coefficients of the material.6,7 Ellipticity values can be determined with an elliptical compensator, but not with the ease and precision desirable for the present purposes. Measurement of the angle of rotation requires only the determination of the angle from the crossed position (90 deg to the polarizer) that the analyzer must be rotated to obtain extinction when the trace of the optical axis in the surface is at 45 deg to the vibration direction of the polarizer. The angle of rotation of the analyzer is approximately 6/5 that of the true angle of rotation of the light as reflected from the specimen because there is a small amount of additional rotation produced during the passage of the reflected light through the mirror of the microscope. Since we are presently interested only in determining the tilt of the basal pole, the angle of rotation of the analyzer (the apparent angle of rotation of the light, i.e., uncorrected) can be used. Precision of the measurement can be increased substantially by the use of a Nakamura plate4,5 in determining the extinction position. In an optically uniaxial material (hcp or tetragonal crystal structure) the angle of rotation depends only on the optical properties of the material and the orientation of the optical axis of the grain relative to the plane of incidence of the plane-polarized light.7,8 Thus, in a metal such as zirconium, the apparent angle of rotation at the 45-deg position in any given wavelength of light is a direct measure of the tilt of the basal pole from the normal to the surface. If the optical properties vary with wavelength, the apparent angle of rotation for any given tilt of the basal pole will vary. None of the required information exists in the literature for zirconium nor for any other non-cubic metal. MEASUREMENTS ON SINGLE-CRYSTAL ZIRCONIUM A single-crystal sphere of zirconium 9/16 in. in diam was spark-cut from a single-crystal rod grown from iodide bar by an electron-beam zone-melting process.9 The damaged surface was removed by chemical polishing in a 45/45/10 mixture (by vol) of water, concentrated HNO3, and HF (48 pct) and then electropolishing at 50 v in a bath1' of methyl alcohol and perchloric acid (95/5 by vol) at -70-C. The single-crystal sphere was mounted in a five-axis goniometer stage having a removable eucentric X-ray diffraction goniometer head for the two inner orientation axes. The basal pole of the single-crysta sphere was aligned parallel to a third axis of the goniometer stage by using the sensitive tint method to determine the basal-plane trace at several rotational positions of the sphere. The alignment was then checked by removing the sphere and eucentric gonio-

Jan 1, 1967

By Ogden B. Malin

In conducting the manufacture of extruded brass rods and brass forgings it has been noticed that there is considerable variation in the physical properties, particularly the machinability of different rods and forgings, even though the composition, working temperatures and method of manufacture remain the same. It is the purpose of this paper to attempt to establish the cause and extent of this variation, and also to determine whether variations in composition within certain defined limits influence hardness and machinability to any marked degree. The writer believes that this variation probably is due to the variation in grain size of the metal, therefore the microstructures of several compositions under various conditions of working were examined in an effort to establish this as a fact. Survey of Previous Work in Studying Extrusion Defects Very little has been published concerning defects in extruded and forged brass. In 1921, R. Genders1 $ delivered a paper before the British Institute of Metals, relative to a defect inherent in the extrusion process. This defect, commonly found in extruded brass rod, shows up in the form of a circle in a transverse section consisting of oxides and impurities, and is generally present in the last 25 to 30 per cent of the rod. Genders concluded that the defect is caused by the turning inward of the skin of the billet at the edge of the plunger because the inside of the billet is more plastic than the outside, which is in contact with the cooler container; the outside skin will lag behind to form the rear end of the rod. Genders suggested a movable die as a remedy, and while this met with fair success, it is not used in present practice. About the same time as Genders' experiments, Tucker2 and Rosen-hain3 conducted experiments using colored plasticene in the form of a billet, and found much the same defect as Genders. Dr. Rosenhain State College, Pa.

Jan 1, 1932

By Donald B. Evans, Robert D. Pehlke

The solubility of nilrogen in liquid binary alloys of iron with Litanium. zivconium, columbium, vanndiurn, and tantalum was measured for alloy composiLions up to the solalbility limils of lhe alloy nitrides. All five alloying agents were found to decrease markedly the activity coefficient of nitrogen in liquid ivon. The metal/nitvogen mole ralios in the alloy nitrides formed were generally .found to be slighlly greater than 1.0, but in no case greater than 1.5. From the experimental data, the standard free energies of fortmation of titanium and zir-conium nitrides have been calculated for the Lemperaluve range 1550° to 1750 C. The solublily Products for columbium, tantalum, and vanadium nitrides are also reported. A number of research investigations have examined the effect of refractory metals on the solubility of nitrogen in liquid iron. Although data on zirconium are not available, investigators are in agreement that titanium, vanadium, columbium, and tantalum markedly increase the solubility of nitrogen in liquid iron. This fact alone makes desirable the acquisition of thermodynamic data for these elements in liquid iron. Since refractory metals are known to be stable nitride formers, they have been suggested as steel denitrifying agents, and some of their nitrides have recently been considered as containment materials for liquid iron and iron alloys. Most available thermodynamic data for these metals relate to their dilute concentrations, but effective thermodynamic treatment of these applications requires data at concentrations near the solubility limit of the alloy nitride. Although some work has been done at relatively high alloy concentrations in liquid iron (particularly for vanadium 2,3 and titanium 2,4), the results have been somewhat contradictory. Disagreement may be partly attributed to the fact that the compositions of most refractory metal nitrides have been shown to be nonstoichiometric, and to vary 2,5-8 depending on the temperature and nitrogen gas pressure with which the solid nitride phase is in equilibrium. One purpose of this study consequently has been to determine the compositions of the refractory metal nitrides precipitated from a liquid iron solution. EXPERIMENTAL PROCEDURE Rao and Parlee2 and Evans and Pehlke 9 have discussed the technique for measuring the solubility product of an alloy nitride phase in liquid iron by finding the point of departure of the nitrogen solubility from Sieverts' law. The method consists of measuring the solubility of nitrogen in a melt of iron containing a known concentration of a second metal as a function of the nitrogen gas pressure over the melt. In this study the second metal was one of the refractory metals titanium, zirconium, columbium, vanadium, or tantalum. When the nitrogen pressure at which the refractory nitride forms is reached, a deviation of the measured solubility of nitrogen in the melt from Sieverts' law is observed in the form of a "pressure halt." The concentration of nitrogen in the melt associated with this breakpoint in the nitrogen-absorption curve is then used to calculate the nitride solubility. The Sieverts method was used to measure nitrogen solubility as a function of nitrogen pressure and temperature. The experimental equipment for this technique has been previously described in detail. 1,9 Charge materials used were vacuum-melted high-purity iron (Ferrovac-E) and the best commercial grades of the refractory metals obtainable (in all cases at least 99.8+ pct pure). Recrystallized alumina crucibles were used to hold all melts except those containing zirconium, for which zirconia crucibles were necessary. Temperatures were measured by a disappearing-filament type optical pyrometer sighted vertically downward on the melt surface through a 1/4-in.-diameter sight hole in the crucible lid. By means of a technique previously described, 9 in which the refractory-metal nitride was precipitated at one temperature then redis-solved by raising the temperature 50°C and precipitated again at a higher temperature, it was possible to obtain data over a temperature range of up to 200°C on a single melt. It was found that this technique could not be used with melts containing zir-

Jan 1, 1965

By Henry J. Miller, Marcella Linderman

During some experiments made by Henry J. Miller, partly in Germany and partly in the United States, in which it was found necessary to melt metals in quantities up to 60 kg. in a vacuum or under low pressures of hydrogen, molybdenum was tried as the resistor in the electric melting furnaces. Molybdenum ribbons 16 by 0.55 mm. and 18 by 0.45 mm. were used as resistors. The furnaces were of the type shown in Fig. 1. About the heating tube, Y, are wound parallel resistors of molybdenum ribbon from the water-cooled electrodes, El, Ez. The whole is within a copper container having outlets for the removal or introduction of gases and a window, W, for observation, the space about the heating tube and electrodes being filled with insulating material. The life of the molybdenum used as the resistor was found to depend very much on the manner of using it, its failure being due in some cases to thinning by evaporation or chemical reaction and in others to hardening, which prevented it from following the expansions and shrinking of the heating tubing without cracking. As such failures are often rather expensive in commercial work, it was thought worth while to determine the causes. The factors influencing the behavior of molybdenum resistors used in this manner may be briefly stated as follows: