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By J. P. Murphy, T. E. Leontis

During the last few years, the trend in the aircraft and automotive industries has been toward higher and higher operating engine temperatures. This has created considerable interest in the effect of temperature on the properties of alloys. In the magnesium field, it has been recognized for many years that the addition of cerium imparts high strength and good resistance to creep at elevated temperatures. Beck,' in his treatise on magnesium, has summarized the work of German investigators. This includes the unpublished data of Menking, showing the increase in strength and hardness of extruded alloys containing 2 to 20 per cent Ce at temperatures from 20' to 300°C. (68" to 57z°F.) and the results of Vosskiihler, who demonstrated the improved resistance to creep of alloys containing 6 per cent Ce plus 2 per cent Mn and 0.5 per cent Ce plus 2 per cent Mn at 150°C. (302°F.). Wellinger and Kei12 have also reported the creep properties of a forged magnesium-cerium-man-ganese alloy at 200' and 250°C. (392' and 482°F.). Haughton and Prytherch have determined the tensile properties of various forged magnesium alloys containing cerium, cerium plus manganese, cerium plus calcium, cerium plus nickel, cerium plus nickel plus manganese, and cerium plus cobalt plus manganese at temperatures up to 290°C. (554OF.). Magnesium-cerium alloys have been used in some commercial applications. It is reported that an alloy containing 3 per cent Ce plus 0.5 per cent Mn plus 0.5 per cent Ca is being used on a forged impeller in Great Britain. Two forged parts made from an alloy with a nominal composition of 5 per cent Ce and 2 per cent Mn have been found on the German BMW-8o1D aircraft engine. These two forgings consist of a supercharger impeller and a rear cam-follower guide. In this country, several types of pistons have been made experimentally in both the cast and the forged conditions from an alloy containing 6 per cent Ce plus 2 per cent Mn and in the cast condition from an alloy of magnesium plus 10 per cent Ce. The cast pistons have been tested in various types of internal-combustion engines, with promising results. This paper presents the results of an extensive investigation on the properties of various cerium-containing magnesium alloys in both the cast and the forged conditions. Data are presented to show the beneficial effects of increasing amounts of cerium on the mechanical properties of magnesium at at temperatures' The effects of heat-treatment on the properties of these alloys and the attendant changes in the microstructure are discussed. The alloys investigated most extensively are

Jan 1, 1946

By H. E. Elliott, R. S. Busk, A. T. Peters

ONE of the problems of the fabricator of metals and alloys is the propensity of some composition ranges toward abnormal grain growth during certain stages of fabrication. In this respect magnesium alloys are no exception among alloys. Fortunately, convenient foundry control methods have been developed by which the abnormal grain growth possible in certain magnesium-alloy castings can be suppressed. An unusual characteristic of magnesium alloys, however, is that castings of some composition ranges are subject to local grain growth during heat-treatment without the necessity of intentional mechanical stressing of the part prior to heat-treatment. This effect occurs only under certain critical casting conditions, and only in certain alloys of greater than about 8.5 per cent aluminum content, such as C alloy (Mg, o per cent Al, 2 per cent Zn, 0.2 per cent Mn) and G alloy (Mg, i0 per cent Al, 0.2 per cent Mn). The first observation of this phenomenon in cast magnesium alloys occasioned much surprise, since it is not observed in other metals. Jeffries and Archer' have stated that "the grain size of cast metals, provided they have not been plastically deformed, cannot be changed by heating below the melting point." The study of the conditions leading to abnormal grain growth in cast magnesium alloys, and of the mechanism of this phenomenon, has led to some very interesting observations. Perhaps the most significant of these was the observation that stresses originating from cooling contraction in magnesium-alloy castings are the only stresses necessary, under certain conditions, to cause local recrystallization and subsequent grain growth in the casting during heat-treatment. of abnormal local grain growth was a definite problem in the production foundry on C alloy sand castings. Illustrated (Fig. r) is a picture of a casting scrapped because of this defect. A mottled effect is produced in coarse-grained areas by suitable etching solutions. The properties of metal in the affected area are much impaired by such grain coarsening. Ultimate tensile strengths of half the normal value have been measured in metal of this nature. In this paper are described the techniques that have been developed by The Dow Chemical Co. for studying, and in large measure solving, this production problem. Also discussed are studies of the mechanism by which excessive grain coarsening occurs, and the fundamental conditions that produce this effect. The abnormal grain growth discussed in this paper will be referred to as "germination," since this term has been defined' as any process leading to an abnormally coarse grain size. This paper deals only with abnormal local grain growth that may occur during the solution heat-treatment of certain magnesium-alloy castings, as dis-

Jan 1, 1945

By E. J. Duggan

The mine and mill of the Climax Molybdenum Co. are at Climax, Colorado. Climax is on Fremont pass directly on the Continental Divide, at an elevation of 11,400 feet. Description of Ore The Climax ore-bearing rock is essentially an altered and highly silicified granite, fully half of the gangue being quartz. Molybdenite is the only mineral of economic consequence and most of it is intimately associated with quartz in the form of fine veinlets and stringers. Other minerals are molybdite, pyrite, and chal-copyrite. While the molybdite may be readily extracted by hydrometallurgical methods, its content is too low to make such operations profitable. The pyrite content ranges from 2 to 5 per cent and that of the chalcopyrite from 0.03 to 0.05 per cent. There is not enough copper to make its recovery attractive and one of the metallurgical problems is the elimination of it and the pyrite from the product. On account of the close association of the molybdenite with the quartz and the necessity of eliminating the pyrite and chalcopyrite from the final product, fine grinding followed by flotation is the only feasible method of concentration. History Construction of the first milling unit was started in 1917 and it was operated during parts of 1918 and 1919. In the postwar years, there was almost no demand for the product and production was at a standstill until 1924. The Company's research campaign to develop the use of the metal began to show results in that year. From r926 to 1932 production ranged from 500 to 1200 tons per day. In 1931 an additional mill section was built and production was gradually increased until in 1934 and 1935 about 3000 to 4000 tons was milled per day. This tonnage overtaxed the milling facilities, and as the demand for inolybdenum was growing constantly, additional milling equipment was needed. In 1936 and 1937 another crushing plant, six additional mill sections and the necessary auxiliary plants were constructed and brought into operation. This plant was designed to mill I0,000 tons per day, but it was not long before 12.500 tons was being treated during periods of peak demands. During the summer of 1941, to meet defense needs, the mill has been required to treat 15,500 tons per day. This has been accomplished with little plant expansion and at no loss in recovery, as will be described later. TO increase capacity still further, one more primary section is now being built. This will bring capacity to 18,000 tons per day, which can be stretched to 20,000 tons at a small sacrifice in recovery. Crushing There are two crushing plants: No. I, of 5000 tons capacity (flowsheet in Fig. I) and No. 2, of 15,000 tons capacity (Fig. a).

Jan 1, 1943

By E. J. Duggan

The mine and mill of the Climax Molybdenum Co. are at Climax, Colorado. Climax is on Fremont pass directly on the Continental Divide, at an elevation of 11,400 feet. Description of Ore The Climax ore-bearing rock is essentially an altered and highly silicified granite, fully half of the gangue being quartz. Molybdenite is the only mineral of economic consequence and most of it is intimately associated with quartz in the form of fine veinlets and stringers. Other minerals are molybdite, pyrite, and chal-copyrite. While the molybdite may be readily extracted by hydrometallurgical methods, its content is too low to make such operations profitable. The pyrite content ranges from 2 to 5 per cent and that of the chalcopyrite from 0.03 to 0.05 per cent. There is not enough copper to make its recovery attractive and one of the metallurgical problems is the elimination of it and the pyrite from the product. On account of the close association of the molybdenite with the quartz and the necessity of eliminating the pyrite and chalcopyrite from the final product, fine grinding followed by flotation is the only feasible method of concentration. History Construction of the first milling unit was started in 1917 and it was operated during parts of 1918 and 1919. In the postwar years, there was almost no demand for the product and production was at a standstill until 1924. The Company's research campaign to develop the use of the metal began to show results in that year. From r926 to 1932 production ranged from 500 to 1200 tons per day. In 1931 an additional mill section was built and production was gradually increased until in 1934 and 1935 about 3000 to 4000 tons was milled per day. This tonnage overtaxed the milling facilities, and as the demand for inolybdenum was growing constantly, additional milling equipment was needed. In 1936 and 1937 another crushing plant, six additional mill sections and the necessary auxiliary plants were constructed and brought into operation. This plant was designed to mill I0,000 tons per day, but it was not long before 12.500 tons was being treated during periods of peak demands. During the summer of 1941, to meet defense needs, the mill has been required to treat 15,500 tons per day. This has been accomplished with little plant expansion and at no loss in recovery, as will be described later. TO increase capacity still further, one more primary section is now being built. This will bring capacity to 18,000 tons per day, which can be stretched to 20,000 tons at a small sacrifice in recovery. Crushing There are two crushing plants: No. I, of 5000 tons capacity (flowsheet in Fig. I) and No. 2, of 15,000 tons capacity (Fig. a).

Jan 1, 1943

By B. N. Bose, M. F. Hawk

SINCE Davenport and Bain' introduced the isothermal transformation technique for the study of austenite decomposition in steels, a new field of investigation has opened up. Extensive research has been carried out on many different steels, but relatively little work has been done on eutectoid transformations in analogous alloy systems. The researches of Smith and Lindlief,² Mack,³ and Klier and Grymko²0 on the beta-phase transformation in copper-aluminum alloys, of Hibbard, Eichelrnan, and Saunders4 and Smith5 on the kappa-phase transformation in copper-silicon alloys, of Chaudron and Forester6 on the decomposition of "FeO," and of Wasserman7 on similarities between the iron-carbon, copper-aluminum, copper-tin, and copper-beryllium systems essentially comprise the field. The iron-nitrogen system, in view of its remarkable similarity to the iron-carbon system, is particularly attractive for the study of eutectoid decomposition. The present investigation is concerned with the study of isothermal transformation, proceeding by the familiar nucleation and growth processes, and of martensitic transformation characteristics of pure iron-nitrogen alloys. The kinetics of transformation and the morphology of the transformation products have been investigated, for these must be the factors determining the properties and behavior of the final product. The Iron-Nitrogen System he binary iron-nitrogen phase diagram has been a matter of considerable disagreement among vari01.1s investigators. However, the phase diagram according to Eisenhut and Kaupp8 and Lehrer10 is now considered essentially correct as reproduced in fig. 1. The important values, 2.35 pct nitrogen and 591°C, for the co-ordinates of the eutectoid point (obtained from this diagram and used in the re- search to be described) were confirmed in a concurrent study of Paranjpe, Cohen, Bever and Floe." The eutectoid decomposition involves the transformation of the ? face-centered cubic interstitial solid solution of nitrogen in iron to the a body-centered cubic interstitial solid solution of nitrogen in iron and the ?' nitride of iron. This nitride is essentially the compound Fe,N; it also possesses a face-centered cubic lattice but a considerably larger one than the ?; the nitrogen atoms in ?' are arranged in an ordered way in the centers of the unit cubes.8,10,11 A martensitic structure has also been reported8,12 in iron-nitrogen alloys and was studied in the research to be described here. Materials and Methods The specimens used in this investigation were prepared by nitriding "pure" iron. This iron was supplied by the Westinghouse Research Laboratories and is the product bearing their trade name "Puron"; it contains about 0.04 wt pct total impurities, the major portion of which is oxygen. Specimens were ribbons several inches long, a tenth of an inch wide, and 0.125 mm thick; this was the

Jan 1, 1951

By Frank Foote, E. R. Jette

In recent years the constitution of the high-silver aluminum-silver alloys has been extensively investigated. Hansenl has reviewed the literature to 1935. More recently, Obinata and Hagiya,2 Hofmann and Volk,3 Taziri4 and Tishchenko5 have confirmed the general features of the phase diagram in the region around 25 atomic per cent aluminum. In this paper we present the results of high-precision measurements of lattice constants of the silver-rich alpha solid solution in the homogeneous range and the neighboring two-phase regions. These results are used to establish the nature of the solid solution, the identity of directly measured densities with those calculated from lattice constants and the homogeneity limits of the alpha solid solution with respect to three different neighboring phases. A study of the earlier investigations indicated that the last two subjects in particular required new and accurate data. Experimental Procedure Preparation of the Alloys.—The alloys were made from high-purity silver and aluminum. The silver was "Proof Silver," 99.999 per cent pure, supplied by the U. S. Metals Refining Co. The aluminum was 99.97 per cent pure (contained Si, 0.009 per cent; Fe, 0.0016 per cent; Cu, 0.004 per cent) and was supplied by the Aluminum Company of America. The lattice constants of these two materials have been reported by Jette and Foote.6 Weighed amounts of the two metals were placed in alundum crucibles and melted in vacuo in a high-frequency induction furnace. The melts were allowed to cool in the crucible, the ingots thus obtained weighed about 10 grams. These ingots were then filed clean, hamered, again cleaned and given a homogenizing anneal in vacuo of from 6 to 15 days at temperatures ranging from 500" to 695°C. The ingots were air-cooled from the annealing temperature. Lattice-constant Measurements.—Carefully prepared filings for X-ray analysis were sealed into evacuated quartz or Pyrex tubes and annealed for various periods of time at suitable temperatures. The furnaces used were vertical, rapid-quenching furnaces, the samples being quenched by crushing the sample tube under water by means of a heavy plunger. The general X-ray technique has been previously described6 The cameras were of the symmetrical, back-reflection, focussing type. Ka, radiation from a cobait-nickel alloy target was used. The wave-length values were taken from the second edition of Siegbaum's book.7 A correction for the index of refraction was applied and the lattice constants were calculated by the method of Cohen.8, 6 The lattice constants were calculated to a common temperature of 25°C., using the value of the linear expansion coefficient of pure silver as 18.9 X 10-6. Presumably the expansion coefficient for

Jan 1, 1941

By Frank Foote, E. R. Jette

In recent years the constitution of the high-silver aluminum-silver alloys has been extensively investigated. Hansenl has reviewed the literature to 1935. More recently, Obinata and Hagiya,2 Hofmann and Volk,3 Taziri4 and Tishchenko5 have confirmed the general features of the phase diagram in the region around 25 atomic per cent aluminum. In this paper we present the results of high-precision measurements of lattice constants of the silver-rich alpha solid solution in the homogeneous range and the neighboring two-phase regions. These results are used to establish the nature of the solid solution, the identity of directly measured densities with those calculated from lattice constants and the homogeneity limits of the alpha solid solution with respect to three different neighboring phases. A study of the earlier investigations indicated that the last two subjects in particular required new and accurate data. Experimental Procedure Preparation of the Alloys.—The alloys were made from high-purity silver and aluminum. The silver was "Proof Silver," 99.999 per cent pure, supplied by the U. S. Metals Refining Co. The aluminum was 99.97 per cent pure (contained Si, 0.009 per cent; Fe, 0.0016 per cent; Cu, 0.004 per cent) and was supplied by the Aluminum Company of America. The lattice constants of these two materials have been reported by Jette and Foote.6 Weighed amounts of the two metals were placed in alundum crucibles and melted in vacuo in a high-frequency induction furnace. The melts were allowed to cool in the crucible, the ingots thus obtained weighed about 10 grams. These ingots were then filed clean, hamered, again cleaned and given a homogenizing anneal in vacuo of from 6 to 15 days at temperatures ranging from 500" to 695°C. The ingots were air-cooled from the annealing temperature. Lattice-constant Measurements.—Carefully prepared filings for X-ray analysis were sealed into evacuated quartz or Pyrex tubes and annealed for various periods of time at suitable temperatures. The furnaces used were vertical, rapid-quenching furnaces, the samples being quenched by crushing the sample tube under water by means of a heavy plunger. The general X-ray technique has been previously described6 The cameras were of the symmetrical, back-reflection, focussing type. Ka, radiation from a cobait-nickel alloy target was used. The wave-length values were taken from the second edition of Siegbaum's book.7 A correction for the index of refraction was applied and the lattice constants were calculated by the method of Cohen.8, 6 The lattice constants were calculated to a common temperature of 25°C., using the value of the linear expansion coefficient of pure silver as 18.9 X 10-6. Presumably the expansion coefficient for

Jan 1, 1941

By H. L. Eiselstein, F. P. Huston, B. B. Betty

An extensive program for the establishment of creep data on high-nickel alloys has been in progress during the past seven years. This paper presents the accumulated data on two solid solution alloys, cold-drawn, annealed Monel and cold-drawn, annealed Inconel. Data on these two alloys in other conditions will be published at a later date. Monel, a nickel-copper alloy, is normally considered a corrosion-resistant material, but it will be shown that it also has considerable creep strength, validating its use at temperatures up to and including 900°F. Inconel, a nickel-chromium-iron alloy, is definitely a heat-resisting alloy possessing good creep strength and oxidation resistance up to iiooOF., and because of its oxidization resistance has been used successfully at much higher temperatures for lightly stressed parts. The literature contains but meager data on the creep properties of high-nickel alloys. Howevcr, Bennett and McAdam have presented a substantial quantity of creep data for cold-drawn Monel.1 The material as tested was not representative of mill production for it was cold-drawn to a reduction of area of 40 per cent as against 13 per cent, which is the mill standard for Monel. Twenty-two individual tests were run on each alloy in the investigation described in the following pages. The data and curves presented herein represent an integration of all the tests to obtain the most accurate picture of the creep properties of these alloys. Neither of the two alloys was found to be embrittled by the combination of temperature and stress, as evaluated by room-temperature tensile and impact tests that were made following creep testing. These data indicate that no tendency toward embrittlement exists. It is recommended that 6300 lb. per sq. in. be used as a working stress for cold-drawn, annealed Monel at 900°F. and 13,200 lb. per sq. in. for cold-drawn, annealed Inconel at the same temperature. Table 8 lists recommended working stresses, based on 80 per cent of the stress to produce a minimum creep rate of 0.01 per cent per 1000 hr., for Monel and some steels. Equipment The equipment used for these tests consists of Colville creep-testing machines manufactured by the Tinius Olsen Testing Machine Co. The load is adjusted, depending on the stress level, to give an error in the stress of not more than ± 0.1 per cent. This is based on considerations of lever sensitivity and the stress used for the standard (A.S.T.M. Tentative Standard E22-38T) 0.505-in. diameter creep specimen having a 2-in. gauge length. The single-specimen furnaces are provided with primary and secondary windings, from

Jan 1, 1945

By Leslie F. Tedsen, Alan E. Flanigan, John E. Dorn

IT is necessary occasionally to use aluminum-alloy sheet where moderately elevated temperatures are encountered. Considerable attention has been directed toward determining the influence of "artificial aging" on the room-temperature properties of the precipitation-hardenable alloys, as testified by numerous company reports and by references 1 to 4. Investigations on the properties at elevated temperatures are few, however,5-7 and have not always covered the range of times and temperatures of greatest interest. The present investigation was instituted to overcome this deficiency. The work was done for the Office of Production Research and Development of the War Production Board, under the supervision of the War Metallurgy Committee, as a part of the "restricted" Project NRC-548. It has been released for publication by the Office of Production Research and Development. As is well known, the high-strength aluminum alloys achieve their remarkable properties as a result of precipitation-hardening. In production they are subjected to a solution heat-treatment followed by quenching, to retain the supersaturated solid solution. The solution treatment is followed by "aging" (precipitation-hardening) either at room temperature or at a suitable elevated temperature. A considerable increase in tensile and compressive yield stresses results from precipitation at room temperature ("natural aging"). Through the elevated-temperature process ("artificial aging") it is possible to obtain values of yield stress considerably higher than those attainable by natural aging. The increase in yield stress is accompanied by a smaller gain in ultimate tensile stress and by a decrease in elongation. During [TABLE I.-Sources of Materials Used in the Testing Program MATERIAL ORIGIN AND TREATMENT 24S-T Alclad.... From Lockheed stock. 24S-RT Alclad... Direct from mill. 24S-T80 Alclad.. 24S-O Alclad from Lockheed stock, solution-heat-treated (925°F., water quench) and aged at 375°F. for t0 t % hour. 24S-T8I Alclad.. 24S-T Alclad from Lockheed stock, plant stretched up t0 I per cent and aged t0 ± % hr. at 375°F. 24S-T86 Alclad.. 24S-RT Alclad from Lockheed stock aged 534 ± 34 hr. at 375°F. 6IS-W (bare).... From Lockheed stock. 6IS-T (bare) 6IS-W (bare) from Lockheed stock aged 8 hr. at 350°F. XB7SS-T Alclad. From Lockheed stock.] the first stages of artificial aging the yield stress increases steadily until it reaches a maximum value. In this condition the material is said to be "fully aged." Further exposure results in "overaging," attended by a steady decrease in yield stress. In the production of the artificially aged materials, temperatures and times are selected to achieve full aging. The following important characteristics are associated with the process: I. The higher the temperature, the more rapidly is the fully aged condition attained.

Jan 1, 1945

By L. S. Richardson, N. J. Grant

Iodide-grade titanium, two oxygen alloys, and two aluminum alloys were studied by means of creep-rupture tests from 1000° to 2000°F. From the test information an evaluation was made of, 1) the relative creep-rupture strengths of the u (hexagonal-close-packed) and 0 (body-centered-cubic) forms of titanium and some of its alloys; 2) the effects of solid-solution strengthening by oxygen and aluminum on the u and 0 structures; and 3) the extent and effect of atmospheric oxygen alloying on rupture life in tests above about 1000°F. THE use of titanium alloys at temperatures above 1000° F has been considered unlikely by most investigators because of low creep strength (based on a requirement for room-temperature ductility, formability, and weldability) and low oxidation resistance. The results of this testing program do not entirely uphold this pessimism in terms of strength and oxidation resistance. The observations described below are based entirely on stress-rupture results, although some creep tests were also carried out on these alloys. Three items of primary importance are covered: 1) Stress-rupture data in the form of the Larson-Miller parameter curves for several titanium alloys at temperatures up to 2000°F; 2) The relative strengths of the hexagonal-close-packed a structure and the body-centered-cubic 0 structure; 3) The effects of solid-solution alloying on the creep-rupture properties of titaniu'm at elevated temperatures. Only two investigatons have reported the creep- rupture properties of titanium at temperatures above 1000° F. Lunsford and rant' tested iodide titanium; their values are also utilized in the paper. EXPERIMENTAL PROCEDURE After a few tests had been made in a conventional creep-rupture test machine, it became clear that some sort of atmospheric protection would be necessary for short-time tests conducted at temperatures above 1600°F, or for times greater than 100 hr at 1200°F or above. Several furnace units and test machines were constructed, the most successful of which is shown in Fig. 1. Certain experimental difficulties peculiar to titanium were encountered; for example, the use of molybdenum holders was dictated because titanium forms low melting-point eutectics with conventional high-temperature alloys containing appreciable amounts of iron, nickel, or cobalt. This same difficulty made the use of chrome l-alumel thermocouples in direct contact with a test specimen impossible, above about 1500" F. The high-temperature high-vacuum furnace shown in Fig. 1 was capable of maintaining a vacuum of better than 10"5 mm of mercury at 2000°F (pressure measured in cold part of system) and 5 X lo-' mm at room temperature. Most of the tests eonducted in vacuum were at temperatures

Jan 1, 1960

By W. C. Ellis, M. E. Fine

In the iron-cobalt system there are several property-composition relationships of theoretical importance. The alloys are ferromagnetic exhibiting a maximum saturation at approximately 33 at. pct cobalt;' the interatomic distances at room temperature show large positive deviations from Vegard's rule;2 and in the region of 50 at. pct cobalt there is an order-disorder transition2 which has a large effect on other properties. The thermal expansion data for the system have been reported only from room temperature to 100 C and for this temperature range a minimum in coefticient in the rcgion of 50 at. pct cobalt is well established.3,4,6 This paper reports the expansion properties in the iron-cobalt system for temperatures from 30 to 850°C, shows the correlation with other physical properties, and proposes an explanation for the tcrrelation. Experimental Procedure The thermal expansivities of iron-cobalt alloys in 10 pct steps in composition were determined from 30 to about 850°C. The major series of alloys was prepared by induction melting from Armco iron and cobalt rondelles with the addition of about 0.6 wt pct manganese. This series was supplemented by three compositions: high purity electrolytic iron, high purity electrolytic cobalt, and an alloy of 52.1 wt pct cobalt prepared from the high purity electrolytic iron and electrolytic cobalt by vacuum-melting. The compositions of both series of alloys are given in Table I. The specimens for measurement were prepared from the cast ingots by first hot-swaging followed in most instances by cold-swaging to 0.180-in. diam rod. Some alloys in the region of 5c pct cobalt, because of inherent cold-brittleness, were swaged hot to the final diameter. The expansion specimens were approximately 2 1/2 in. long with flat-ground and polished ends. Before measurement they were annealed in hydrogen for I hr at 900°C. In the apparatus used for the thermal expansivity measurements (Fig I), a modification of that designed by Hidnert and Sweeney,? the differential expausion between the specimen and vitreous silica was measured by a dial micrometer reading to 0.001 mm. An invar fixture supported the dial gauge, and this fixture, in turn, was connected to a split invar collar which supported the outer silica tube. A pyrex "T" was placed over the outcr silica tube and was sealed to the invar collar by Apiezon Q sealing compound. A movable hollow vitreous silica rod which rested on top of the test specimen slid through a flexible rubber diaphragm cemented to the top of the pyrex "T." The specimen rested On a vitreous silica pedestal fused into the outer tube and was kept centered by a silica sleeve. A nonoxidizing atmosphere was obtained by admitting hydrogen into the

Jan 1, 1949

By L. C. De Jong, J. F. Shirley, M. L. Campbell

At the Southern Peru Copper operation in Toque-pala, Peru, a new process flowsheet for the recovery of byproduct molybdenite has proved successful in dealing with complex and highly variable ores. This paper describes the process and the functions of each of the chemicals used. The Toquepala concentrator of the Southern Peru Copper Corp., located approximately 720 miles southeast of Lima near the Chilean border, processes a daily 36,500 tons of ore containing between 0.50 and 3.00% copper. The molybdenite content in the ore also varies greatly ranging from essentially nothing to as high as 0.15%. The 1966 yearly averages were approximately 1.20% copper and 0.03% molybdenite. The Toquepala porphyry deposit is a mushroom-shaped ore body consisting of a flat-lying enriched zone of predominant chalcocite with a stem-like extension of hypogene chalcopyrite ore in depth within and around a large breccia pipe.1 The underlying chalcopyrite ore has not been reached; however, due to the presence of a major post orebody fault, predominantly chalcopyrite ore is present in the north side of the pit. Most of the molybdenite occurs either as small, fine granular, pulverulent masses in vugs or empty voids of breccia, or as thin foliated masses and narrow thread-like filling in rock joints and fractures. The normal occurrence of quartz gangue with the molybdenite gives some basis for correlating the molybdenite mineralization to some later periods of silicification. On April 18, 1962, the molybdenite recovery plant at Toquepala went on stream, approximately 27 months after the copper concentrator had been in production. The plant was designed and built by Southern Peru Copper Corp.'s engineering and mechanical departments. The basic method chosen for separating the molybdenite from the copper concentrate was the sodium hypochlorite-sodium ferrocyan-ide process. The selection of this process was based on the results of an extensive testing program performed by the Colorado School of Mines Research Foundation, Inc. and the economic conditions of the area. The originally designed process could never be fully implemented due to a lack of sodium hypo-chlorite and has had to be continually modified to satisfy the requirements of the kaleidoscope of ores from the mine. The three basic problems that plague the operation of any molybdenite recovery plant are all present at Toquepala in large measure. Both the quantity of plant feed and the quantity of molybdenite contained in the plant feed are continuously changing. Even more detrimental to an efficient operation is the fact that the copper mineralization in the feed frequently changes once in every 24 hours and occasionally once a shift. From the point of view of the molyb-

Jan 1, 1968

By E. E. McGinley, L. D. Woodworth

DURING the past several years has occurred what, in the light of future events, may aptly be called the rebirth of the acid Bessemer process. The increased attention given to the technical and metallurgical details involved in the production of Bessemer steels has been exceedingly fruitful, and indicates the value of further research and plant development. In times like these, when the steelmaking capacity of the country is operating at a maximum rate to supply materials for the national defense program, it behooves the Bessemer operator not only to strive to increase production but also to maintain a high standard of quality. The opportunity is ripe, it seems, to recapture fields of application once considered the birthright of Bessemer steels, but supplanted in recent years by open-hearth grades. This involves cooperation all along the line, from the blast-furnace operator to the metallurgical contact man and salesman. The metallurgist's part in this program involves the study of the many steelmaking variables and the measures necessary to ensure constancy in the finished product. It is equally important that the knowledge gained be disseminated widely to ensure the wise application of Bessemer steels in new fields. The merits of Bessemer steels for certain work are well understood. The combined properties of good weldability, machinability and stiffness are unique and fully explain the strong entrenchment of Bessemer steels in certain fields; e.g., skelp for small butt-weld conduit, screw steels machined in automatics, and certain tinplate applications. It is the purpose of this paper to review briefly the physical properties of Bessemer steels as contrasted with those of open-hearth steels, to discuss control measures now employed in the making of Bessemer steel, and to consider the advantages derived from the use of these control measures. PHYSICAL PROPERTIES OF BESSEMER VS. OPEN-HEARTH STEELS A number of Bessemer blows and open-hearth heats were tested for tensile strength, ductility and impact strength. The steels selected were confined to sections from ¾ to 1 ¼ -in. diameter, inclusive, and the carbon content covered was sufficient to yield parallel ranges in ultimate strength for the comparison. Other factors, such as the extent of deoxidation of the steel and variations in chemistry, were kept as comparable as possible. Machined test pieces of 0.505-in. diameter with an 8-in. gauge length were pulled. The data obtained are shown in Fig. 1, ultimate strength being plotted against carbon content. This graph shows that for equivalent carbon content Bessemer steel has on the average 15,000 lb. per sq. in. greater tensile strength and, conversely, for the same tensile strength Bessemer steel requires on the average 0.14 per cent less carbon. The average phosphorus content for the Bessemer steel was 0.090 per cent,

Jan 1, 1941

By D. S. Eppelsheimer, D. N. Williams

The compression texture of iodide titanium is determined and found to consist of a [0001] texture rotated 15° to 30° from the axis of compression. As the amount of reduction increases, the angle of rotation decreases. The 0001 rotation showed a slight preference for a <1010> rotation axis. RECENT investigation of the cold rolled texture of titanium&apos; has shown this metal to exhibit a new type of rolling texture. This texture can best be described as a (0001) [10i0] with the 0001 planes rotated approximately 30" to the transverse direction around a <10i0> rotation axis. Rather good results in explaining the cold rolled texture have been obtained by other workers&apos; by examination of the tension and compression textures. No information was found giving the tension texture of titanium. Generally the tension texture of a hexagonal close-packed metal is identical with its wire texture. The drawn texture of titanium has been investigatedh nd has been found to be predominately [10?0]. Since this is the common tension texture of hexagonal metals of low c/a ratio, the explanation of the difference between the rolling texture of titanium and the rolling texture of other hexagonal metals is not indicated by examination of the tension texture. Therefore, the compression texture of titanium should be particularly important in the explanation of the unusual transverse rotation of the 0001 planes found in the cold rolled texture. The compression texture of titanium was examined by Yen.",&apos; His results showed titanium to exhibit the usual [0001] texture up to 85 pct reduction. At higher reduction a double texture appeared in which the 0001 planes were rotated from 10" to 30" from the plane of compression. This change in the compression texture seemed unusual since the tendency for hexagonal close-packed metals is to approach the [0001] texture as the idea compression texture. Mechanical twinning generally occurs over a considerable range of reductions beginning at a rather low reduction. The samples used by Yen in his investigations were prepared by two methods. Compression in a testing machine was used up to a reduction of 85 pct. Compression by compression rolling was used at higher reductions. Since the change in texture occurred at the same reduction as the change in the method of compression, a connection between the two seemed likely. To check this possibility and to locate the position of the change in texture definitely, if it was found to exist, the compression texture of titanium was re-examined. An iodide titanium crystal bar (99.9 pct Ti) produced by the New Jersey Zinc Co. and donated by the Titanium Alloy Manufacturing Div. of the National Lead Co. was used in this investigation. Procedure The investigation of the compression texture was carried out in three steps; compression, specimen

Jan 1, 1953

By R. C. Buehl, J. P. Riott, E. P. Shoub

PILOT-PLANT tests have demonstrated that it is possible to produce low-sulphur sponge iron (0.03 to 0.05 per cent sulphur) as a continuous process in an internally fired rotary kiln from iron ore or mill scale; a solid carbonaceous reducing agent; and dolomite to control the sulphur content. The proportion of dolomite employed is small, so that it does not add materially to the cost of the sponge iron. The entire operation is carried out at temperatures well below the melting point of iron, so that the product is discharged in granular form. Compared with other methods for the production of sponge iron, the rotary-kiln method has the advantage of simplicity and low cost of equipment and; in addition, requires little labor for the operation of the process. The pilot-plant equipment used for this work was sufficiently large to demonstrate that the production of low-sulphur sponge iron in rotary kilns is feasible and that the costs are not excessive for applications in which sponge iron has distinct advantages over competing materials. This report constitutes a part of a program by the Bureau of Mines under a special Congressional appropriation for studying gaseous and solid fuel reduction of iron ores. Numerous articles on various phases of these investigations have appeared in Bureau of Mines publications or technical journals. Other articles are being prepared and will be published in the near future. The present program, which is under the supervision of Dr. R. S. Dean, Assistant Director of the Bureau of Mines, was initiated in .1942. However, a considerable portion of the work was a continuation of previous research performed by the Bureau. Previous investigators1-4 utilizing the rotary kiln for the production of sponge iron did not develop a suitable method for controlling the sulphur content. A review of the literature shows that the sulphur content in the product usually exceeded 0.2 -per cent unless reducing agents with very low sulphur contents were employed. This high sulphur value made the product generally undesirable for use as melting stock in electric or open-hearth furnaces. The production of sponge iron in an internally fired rotary kiln has been described in detail in Bureau of Mines Bulletin 2702; consequently, this article will be confined mostly to new features of the process-that is, means for controlling the sulphur content of the sponge iron. Suitable raw materials include iron ores or mill scale; coal or coke for reducing them, and sized dolomite (-20+100-mesh) as the sulphur-controlling agent. A mixture of the raw materials in granular form is fed into the elevated end of the kiln, which is fired axially from the lower or discharge end. In the reducing zone, which is approximately one third the length of the kiln measured from the dis-

Jan 1, 1946

By E. J. Duggan

THE mine and mill of the Climax Molybdenum Co. are at Climax, Colorado. Climax is on Fremont pass directly on the Continental Divide, at an elevation of 11,400 feet. DESCRIPTION OF ORE The Climax ore-bearing rock is essentially an altered and highly silicified granite, fully half of the gangue being quartz. Molybdenite is the only mineral of economic consequence and most of it is intimately associated with quartz in the form of fine veinlets and stringers. Other minerals are molybdite, pyrite, and chalcopyrite. While the molybdite may be readily extracted by hydrometallurgical methods, its content is too low to make such operations profitable. The pyrite content ranges from 2 to 5 per cent and that of the chalcopyrite from 0.03 to 0.05 per cent. There is not enough copper to make its recovery attractive and one of the metallurgical problems is the elimination of it and the pyrite from the product. On account of the close association of the molybdenite with the quartz and the necessity of eliminating the pyrite and chalcopyrite from the final product, fine grinding followed by flotation is the only feasible method of concentration. HISTORY Construction of the first milling unit was started in 1017 and it was operated during parts of 1918 and 1910. In the postwar years, there was almost no demand for the product and production was at a standstill until 1024. The Company&apos;s research campaign to develop the use of the metal began to show results in that year. From 1926 to 1932 production ranged from 500 to 1200 tons per day. In 1931 an additional mill section was built and production was gradually increased until in 1934 and 1935 about 3000 to 4000 tons was milled per day. This tonnage overtaxed the milling facilities, and as the demand for molybdenum was growing constantly, additional milling equipment was needed. In 1936 and 1937 another crushing plant, six additional mill sections and the necessary auxiliary plants were constructed and brought into operation. This plant was designed to mill I0,000 tons per day, but it was not long before 12,500 tons was being treated during periods of peak demands. During the summer of 1941, to meet defense needs, the mill has been required to treat 15,500 tons per day. This has been accomplished with little plant expansion and at no loss in recovery, as will be described later. To increase capacity still further, one more primary section is now being built. This will bring capacity to 18,000 tons per day, which can be stretched to 20,000 tons at a small sacrifice in recovery. CRUSHING There are two crushing plants: No. I, of 5000 tons capacity (flowsheet in Fig. I) and No. 2, of 15,000 tons capacity (Fig. 2).

Jan 1, 1942

By N. Tiner

IN an article on magnesium and its alloys, Gann and Winston1 stated that manganese has a limited solubility in the liquid state. W. Schmidt2 showed a diagram according to Joseph Ruhrmann indicating that the solubility of manganese in liquid magnesium falls from about 2.65 per cent at 790°C. to about 0.5 per cent at 695°C. The curve was extrapolated to show zero solubility at the melting point of pure magnesium (Fig. I): This work suggested that at the lowest manganese contents it was not possible to detect either a eutectic or the formation of a solid solution, so that manganese was stated to be present in the structure as large individual crystals. Two years after the presentation of these results, Gann3 brought evidence to show that some manganese is capable of dissolving to form a solid solution, any excess of manganese present then assuming chiefly the form of small blue-gray particles scattered throughout the primary magnesium crystals, occasionally in clusters but seldom at the boundaries. He presented micrographs of cast alloys containing o.1, 0.4 and 1.0 per cent manganese that show a small amount of coring around the individual particles due to solid solution, and indicate that the location of the manganese particles is closely associated with the original dendritic structure of the primary crystallization. He also pointed out that the amount of manganese that can be dissolved in magnesium depends on the amount of other alloying elements present, the effect of the second alloying element being to decrease the amount of manganese retained in the alloy. E. Schmid and G. Siebe14 have determined the solid solubility of manganese and its variation with temperature by means of precision X-ray diffraction measurements. They found that the solubility is 3.4 per cent at 645°C and decreases to practically zero at 200°C. It is apparent that the X-ray diffraction measurements of Schmid and Siebel are not in agreement with the results of Ruhrmann as presented by Schmidt. This disagreement, and also the lack of data on magnesium-aluminum-manganese and magnesium-zinc-manganese systems, led the author to the present investigation, to determine accurately the liquid solubility of manganese and its variation with temperature. EXPERIMENTAL METHOD The experimental method for making solubility determinations consists of saturating the molten magnesium or the alloys with manganese at various temperatures and analyzing the dip samples taken from these melts. Melting is carried out in a cylindrical steel pot heated by an electric resistance furnace. The pot had a metallic outside coating to protect the steel against oxidation, and a graphite inside lining to prevent the contamination of the melt by prolonged contact with iron. The inside diameter of the pot was 4 in. and the depth 12 inches.

Jan 1, 1945

By B. H. Sage, R. T. Carter, W. N. Lacey

The phase behavior of a number of binary systems consisting of parafin hydro-carbons has been determined in recent years. In addition, the composition of the coexisting phases of mixtures of crude oil and natural gas has been investigated.~ However, the latter study did not include information concerning the influence of the concentration of a component upon its distribution between two coexisting phases. Owing to the paucity of such information it was considered desirable to investigate in some detail the composition of the coexisting phases in the methane-propane-n-pentane system throughout the greater part of the two-phase region at a tempera-ture of 100°F. Information of this nature also permits the establishment of the critical behavior of this ternary system. Method The compositions of the coexisting phases in this ternary system at 100°F. were deter-mined by withdrawing samples from a pres-sure vessel containing a heterogeneous mixture of the three components that had been brought 10 equilibrium by mechanical agitation at the desired pressure and tem-perature. The samples were withdrawn under such conditions that the equilibrium was not disturbed and the composition of each of the phases was ascertained by means of the conventional low-temperature fractionation procedure. The apparatus employed in this investi-gation was nearly the same as that utilized in an earlier study of the methane-pentane system.~ Several minor modifica-tions in the arrangement of the apparatus were made in the interest of simplifying the procedure and avoiding the possibility of condensation in the tubing connecting the equilibrium apparatus with the analyti-cal equipment. The pressures were meas-ured by means of a pressure balance with a precision of 0.5 lb. per sq. in. It is believed that the equilibrium pressure was ascer-tained with an uncertainty of not more than 2 lb. per sq. in., even though small varia-tions in pressure obtained during the withdrawal of the samples. The tempera-ture of the equilibrium equipment was maintained by use of an automatically controlled oil bath. The bath temperature was determined by means of a copper-constantan thermocouple, the electromo-tive force being determined by means of a potentiometric circuit of such a nature as to reduce the uncertainty of the tempera ture to less than O.I f. The fractionating column employed in the determination of the composition of the gas phase had a diameter of 0.12 in. and was approximately 4 ft. long, while the column employed in the analysis of the liquid phase was 0.18 in. in diameter and about 5 ft. long. Each column was equipped with the conventional constant-volume receivers, which were maintained at a constant temperature by means of an automatically controlled oil bath. In nearly every case the distillation in thr neighborhood of the transition between

Jan 1, 1941

By L. D. Woodworth, E. E. McGinley

During the past several years has occurred what, in the light of future events, may aptly be called the rebirth of the acid Bessemer process. The increased attention given to the technical and metallurgical details involved in the production of Bessemer steels has been exceedingly fruitful, and indicates the value of further research and p1ant development. In times like these, when the steelmaking capacity of the country is operating at a maximum rate to supply materials for the national defense program, it behooves the Bessemer operator not only to strive to increase production but also to maintain a high standard of quality. The opportunity is ripe, it seems, to recapture fields of application once considered the birthright of Bessemer steels, but supplanted in recent years by open-hearth grades. This involves cooperation all along the line, from the blast-furnace operator to the metallurgical contact man and salesman. The metallurgist&apos;s part in this program involves the study of the many steelmaking variables and the measures necessary to ensure constancy in the finished product. It is equally important that the knowledge gained be disseminated widely to ensure the wise application of Bessemer steels in new fields. The merits of Bessemer steels for certain work are well understood. The combined properties of good weldability, machinabil-ity and stiffness are unique and fully explain the strong entrenchment of Bessemer steels in certain fields; e.g., skelp for small butt-weld conduit, screw steels machined in automatics, and certain tin-plate applications. It is the purpose of this paper to review briefly the physical properties of Bessemer steels as contrasted with those of open-hearth steels, to discuss control measures now employed in the making of Bessemer steel, and to consider the advantages derived from the use of these control measures. Physical Properties oF Bessemer vs. Open-hearth Steels A number of Bessemer blows and open-hearth heats were tested for tensile strength, ductility and impact strength. The steels selected were confined to sections from 3/4 to 1 1/4-in. diameter, inclusive, and the carbon content covered was sufficient to yield parallel ranges in ultimate strength for the comparison. Other factors, such as the extent of deoxidation of the steel and variations in chemistry, were kept as comparable as possible. Machined test pieces of 0.505-in. diameter with an 8-in. gauge length were pulled. The data obtained are shown in Fig. I, ultimate strength being plotted against carbon content. This graph shows that for equivalent carbon content Bessemer steel has on the average 15,000 lb. per sq. in. greater tensile strength and, conversely, for the same tensile strength Bessemer steel requires on the average 0.14 per cent less carbon. The average phosphorus content for the Bessemer steel was 0.090 per cent,

Jan 1, 1941

By W. N. Lacey, R. T. Carter, B. H. Sage

The phase behavior of a number of binary systems consisting of parafin hydro-carbons has been determined in recent years. In addition, the composition of the coexisting phases of mixtures of crude oil and natural gas has been investigated.~ However, the latter study did not include information concerning the influence of the concentration of a component upon its distribution between two coexisting phases. Owing to the paucity of such information it was considered desirable to investigate in some detail the composition of the coexisting phases in the methane-propane-n-pentane system throughout the greater part of the two-phase region at a tempera-ture of 100°F. Information of this nature also permits the establishment of the critical behavior of this ternary system. Method The compositions of the coexisting phases in this ternary system at 100°F. were deter-mined by withdrawing samples from a pres-sure vessel containing a heterogeneous mixture of the three components that had been brought 10 equilibrium by mechanical agitation at the desired pressure and tem-perature. The samples were withdrawn under such conditions that the equilibrium was not disturbed and the composition of each of the phases was ascertained by means of the conventional low-temperature fractionation procedure. The apparatus employed in this investi-gation was nearly the same as that utilized in an earlier study of the methane-pentane system.~ Several minor modifica-tions in the arrangement of the apparatus were made in the interest of simplifying the procedure and avoiding the possibility of condensation in the tubing connecting the equilibrium apparatus with the analyti-cal equipment. The pressures were meas-ured by means of a pressure balance with a precision of 0.5 lb. per sq. in. It is believed that the equilibrium pressure was ascer-tained with an uncertainty of not more than 2 lb. per sq. in., even though small varia-tions in pressure obtained during the withdrawal of the samples. The tempera-ture of the equilibrium equipment was maintained by use of an automatically controlled oil bath. The bath temperature was determined by means of a copper-constantan thermocouple, the electromo-tive force being determined by means of a potentiometric circuit of such a nature as to reduce the uncertainty of the tempera ture to less than O.I f. The fractionating column employed in the determination of the composition of the gas phase had a diameter of 0.12 in. and was approximately 4 ft. long, while the column employed in the analysis of the liquid phase was 0.18 in. in diameter and about 5 ft. long. Each column was equipped with the conventional constant-volume receivers, which were maintained at a constant temperature by means of an automatically controlled oil bath. In nearly every case the distillation in thr neighborhood of the transition between

Jan 1, 1941