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By J. E. Burke, C. S. Barrett

THE fine lines shown in Fig 1 are typical of markings that may be detected after polishing and etching deformed specimens of alpha brass and other alloys. Although they have long been the subject of discussion by metallurgists their nature is still uncertain and the names that have been applied to them, such as deformation lines or strain markings, indicate this uncertainty. In this paper which reports the results of a further investigation of their nature, they will be called strain markings. INTRODUCTION Matthewson and Phillips1 in 1916 concluded that strain markings appeared only after deformations that exceeded 20 pct. They objected to the markings being called slip lines believing this term should be reserved for surface markings produced by plastic deformation. In 1921, Vogel2 described similar striations which appeared after polishing and etching the roughly ground surface of numerous alloys. He reported that the markings were crystallographic in nature, and since they resemble Neumann bands in iron, at least superficially, he assumed them to be mechanical twins. In 1928, Matthewson3 reported work by Phillips which indicated that the lines were more readily produced by impact than by slow deformation and that in many cases the twins inside recrystallized grains were parallel to strain markings in the original deformed grains. This was taken as evidence that the markings coalesce into annealing twins, and hence that they themselves are mechanical twins. Many attempts have been made to [ ] demonstrate directly that the markings are mechanical twins. In 1934, Samans4 described the results of X ray studies of two deformed crystals of alpha brass. Evidence was obtained which could be interpreted to indicate that the strain markings are mechanical twins, and this remains the only direct evidence to this effect. Several other attempts to obtain similar evidence by X ray diffraction have failed5,6,7 although in no case was the original method of Samans employed. An

Jan 1, 1948

By M. Gensamer

ALTHOUGH a large number of X-ray photograms of cold-rolled steel have been published, two circumstances have led to the experimental work reported in this paper. The first is that no complete study, making use of the pole-figure method of Wever1, has been made of cold-rolled low-carbon steel. Wever has published pole figures of mild steel sub-jected to plane parallel deformation1,2 and undoubtedly he has applied the method to cold-rolled mild steel, but the authors have not found these data published. Kurdjumow and Sachs3 have applied the method to the study of rolling and recrystallization textures in electrolytic iron; their results will be referred to later. The reason for this dearth of papers using the pole-figure method is obvious; a greater number of photograms and more analytical work (although this work is quite simple and straight-forward) are required to construct a pole figure than most investigators have felt worth while, despite the fact that no other method of which the authors are aware will satisfactorily depict the orientations of the crystal-lites in a polycrystalline aggregate. The second circumstance that led to the work reported in this paper was the appearance of a paper by Wayne A. Sisson4 on the same subject. In his valuable study of the factors influencing the development of pre-ferred orientations in cold-rolled mild steel, Sisson made one observation that required confirmation; that is, that at some stage of the rolling proc-ess the type of preferred orientation changed from the type that gives a photogram characterized as a "six-point" X-ray pattern to that known as a "four-point" pattern. A similar observation had been made by Tam-mann and Heinzel5, who studied the orientations developed in the rolling of steel by the specular reflection of light from the etched surface of rolled samples. These workers also found that the type of preferred orientation

Jan 1, 1936

By John Chipman, Minu N. Dastur

This paper presents equilibrium data on the reaction of water vapor with vanadium dissolved in liquid iron at 1600°C. The thermo-dynamic behavior of vanadium and oxygen when present together in the melt is discussed. A deoxidation diagram is presented which shows the concentrations and activities of vanadium and oxygen in equilibrium with V209 or FeV2O4. STUDIES of the chemical behavior of oxygen dissolved in pure liquid iron1-3 have served to determine with a fair degree of accuracy the thermody-namic properties of this binary solution. The practical problems of steelmaking, however, involve not the simple binary but ternary and more complex solutions. Only a beginning has been made toward understanding the behavior of such systems. The silicon-manganese-oxygen relationship was studied long ago by Korber and Oelsen4 and more recently by Hilty and Crafts." The carbon-oxygen reaction was investigated by Vacher and Hamilton6 and by Marshall and Chipman.7 A number of deoxidizing reactions have been studied empirica1lys'10 with the object of determining the appropriate "deoxidation constants." The work of Chen and Chipman" afforded a clear-cut view of the effect of the alloy element, chromium, on the thermodynamic activity of oxygen in liquid ternary solutions. These investigators determined the oxygen content of experimental melts which had been brought into equilibrium with a controlled atmosphere of hydrogen and water vapor and were able to show that the presence of chromium decreases the activity coefficient of oxygen. They determined also the conditions under which the two deoxidation products, Cr2O3 and FeCr2O4, were formed and showed that the activity of residual oxygen is considerably less than its percentage. It was the object of this investigation to apply a similar method to the study of molten alloys of iron, vanadium, and oxygen. Vanadium was once considered a moderately potent deoxidizer, but this is now known to be erroneous, in the light of its behavior in steelmaking practice. Its reaction with oxygen retains a certain amount of practical interest in that a high percentage of one element places a limit on the amount of the other that can be retained. As a deoxidizer it will be shown that vanadium lies between chromium and silicon. Experimental Method The apparatus was that used by the authors3 in their study of the equilibrium in the reaction: H2(g) +O = H2O(g);K,= [1] PII., ao Crucibles of Norton alundum or of pure alumina were used. The latter were made in this laboratory and were of high strength and low porosity. Under conditions of use they imparted no significant amount of aluminum (less than 0.01 pct) to the bath. Temperature measurements were made with the optical equipment and calibration chart of Dastur and Gokcen.= The charge was made up of calculated amounts of ferrovanadium (20 pct V) and clean electrolytic iron totaling approximately 70 g. The first few heats were made in alumina crucibles with an insufficient amount of vanadium so that no oxide of vanadium would be precipitated under the particular gas composition. All the heats were made at 1600 °C under a high preheat and with four parts of argon to one part of hydrogen in the gas mixture to prevent thermal diffusion. The rate of gas flow was maintained constant at 250 to 300 ml per min of hydrogen. The time for each heat was three quarters of an hour after the melt had melted and attained the required temperature (1600°C). The water-vapor content of the entrant gas mixture was gradually raised in succeeding heats, keeping the vanadium content of the melt constant. This was controlled by manipulation of saturator temperature. A point was reached when for a given H2O:H2 ratio some of the dissolved vanadium was oxidized and appeared as a thin, bright oxide film on top of the melt. By raising the temperature of the melt it was possible to dissolve the oxide film which reappeared as soon as it was cooled down to 1600°C. The temperature readings taken on the oxide film were consistently higher by 80" to 85 °C as observed by the optical pyrometer. The heat was allowed to come to equilibrium under a partial covering of this oxide film. At the end of the run the power and preheater were shut off and the crucible containing the melt was lowered down into the cooler region in the furnace. This method of quenching proved quite

Jan 1, 1952

By B. G. Bunting, D. L. Abata, J. Robb, J. H. Johnson

Toxic gases produced by the detonation of six explosives were measured in an underground hardrock metal mine during mining operations. The explosives included two semi-gelatin dynamites, three slurry explosives, and an ammonium nitrate, fuel-oil/ammonia dynamite combination. Explosives were detonated at the face of a drift and toxic gases produced by the detonation were trapped at the end of the drift by a bulkhead located a short distance away from the face. Toxic gas concentrations were then measured with direct readout instruments and together with the containment volume, the toxic gas volumes per mass of explosive were calculated. Toxic gas measurements were found in the following ranges (ft3/1bm): NO, 0.0100-0.035; N02, 0.003-0.019; CO, 0.08-0.30; SO2, 0.00-0.05; and CO2, 0.7-1.8. Results showed that toxic gas production (ft3/lbm) correlated with the densities (kg/m3) and energy densities (kJ/kg) of the explosives tested.

Jan 1, 1983

By G. Donald Emigh

Nothing is more important to life-plant and animal-than phosphate. Its compounds are essential to the energy functions of all living systems and for the formation of bones and teeth. Animals get their phosphate from eating plants and other animals, or domestically from feed supplements. Plants get their phosphates from the soil. Man's most important use of phosphate is for fertilizer; approximately 95% of the world's phosphate rock production is consumed by fertilizers. Most of the balance is processed in electric furnaces into elemental phosphorus, the important raw material for making industrial phosphates. Recovery of uranium from phosphates has been possible but not widely used. However, recent significant developments have generated interest in such recovery in the US and elsewhere. Phosphate occurs in all igneous and sedimentary rocks, and in all fresh and salt water. However, economical recovery is limited to deposits where natural concentration of the phosphate mineral has occurred. Occasionally natural concentration is great enough that the material can be used as mined; generally, however, the ore is low grade_ and must be concentrated. Phosphate rock is produced in 31 countries. Fig. 1 shows the location of major phosphate rock producers as well as some of the known phosphate deposits not yet in production. In the last decade the world phosphate industry has experienced steady growth. World production rose from 98 Mt of phosphate rock in 1973 to 140 Mt in 1982. Fig. 2 shows the growth curve of rock production and graphically illustrates the almost straight-line rise since 1945 in both US and world production. Table 1 gives the breakdown, by countries, of world rock production, 1974 through 1979. Table 2 shows US rock production by producing areas. Definitions of Terms Used in the Phosphate Industry Phosphate Rock: Commonly called rock in sedimentary deposits and apatite in igneous deposits. Those expressions generally include any mined, or mined and beneficiated, fluorine-containing calcium phosphate used as the raw material for the next stage of manufacturing. The average phosphate content in rocks is 0.1 to 0.2% P2O5, as documented by McKelvey (1973). About 200 minerals contain more than 1 % P2O5. However, the important mineral in igneous rocks is fluorapatite, [Ca5 (PO4),3 F], containing about 42% P205 and 3.8% F2; in sedimentary rocks the important mineral is francolite, a carbonate fluorapatite containing up to 2% molecular CO2. Both are in the apatite family of minerals. Most phosphate rock, whether beneficiated or not, is a fine-grained material. The expression phosphate rock has no relation to its phosphate content. For example, phosphate rock from Idaho used in the production of phosphorus may contain about 24% P205, whereas rock from Morocco may contain 36.6% P2O5. Phosphorite: A deposit of phosphate directly or indirectly of sedimentary origin, which is of economic interest. Grade of Phosphate Rock: The calcium phosphate content of phosphate rock is expressed in different world areas by one of the following terms: BPL (bone phosphate of lime) TPL (triphosphate of lime) P2O5 (phosphorus pentoxide) P (phosphorus-not commonly used) An illustration of relationship is: 80% BPL = 80% TPL = 36.6% P5O2 = 16% P

Jan 1, 1983

By C. D. Woodward

PRIOR to 1902, the tramming of ore from the stopes to the shafts, in the Butte mines, was done by man or animal power, but the demand for greater tonnage and the need for more improved methods of tramming the ore resulted in the installation of the compressed-air locomotive in a few mines. Some of the objections to animal haulage were thus eliminated, but this locomotive was not generally adopted, because of a number of limiting features. It was superseded by the electric trolley locomotive. The early types of trolley locomotives were not satisfactory from the operators' viewpoint, but. they had many economic advantages and after a number of years, in which improvements were constantly made in the structural details, they became dependable, so that the use of animals for main haulage in the mines has now been practically abandoned. There are now operating in the Butte mines of the Anaconda Copper Mining Co., 185 trolley-type locomotives, each of which has replaced five animals. It cost approximately $50 per month to keep an animal, hence the economies that resulted fully justified the expenditure of electrifying the haulage systems. The haulage conditions in this company's mines possess many advantageous features that are not always found in underground mine workings. The drifts and crosscuts are large, approximately 5 ft. (1.5 m.) wide by 7 ½ ft. (2.3 m.) high, and have curves of no less than 18 ft. (5.5 m.) radius; and the roadbeds of the drifts and crosscuts have a uniform grade of 0.5 per cent. toward the shaft, or in favor of the loaded trips. In all of the mines, except two, the track gage is 18 in. (45.7 cm.), and all tracks in the main haulageways are laid with 25-lb. (11.3 kg.) rails. The stations at the shaft are large, well-lighted, clean, and cool. The average temperature of ,the stations, however, is about 75° F. (24° C.), while the average temperature in some of the drifts and crosscuts is 92° F. (33.5° C.).

Jan 2, 1922

By C. D. Woodward

PrioR to 1902, the tramming of ore from the stopes to the shafts, in the Butte mines, was done by man or animal power, but the demand for greater tonnage and the need for more improved methods of tramming the ore resulted in the installation of the compressed-air locomotive in a few mines. Some of the objections to animal haulage were thus eliminated, but this locomotive was not generally adopted, because of a number of limiting features. It was superseded by the electric trolley locomotive. The early types of trolley locomotives were not satisfactory from the operators' viewpoint, but they had many economic advantages and after a number of years, in which improvements were constantly made in the structural details, they became dependable, so that the use of animals for main haulage in the mines has now been practically abandoned. There are now operating in the Butte mines of the Anaconda Copper Mining Co., 185 trolley-type locomotives, each of which has replaced five animals. It cost approximately $50 per month to keep an animal, hence the economies that resulted fully justified the expenditure of electrifying the haulage systems. The haulage conditions in this company's mines possess many advantageous features that arc not always found in underground mine workings. The drifts and crosscuts are large, approximately 5 ft. (1.5 m.) wide by 71/2 ft. (2.3 m.) high, and have curves of no less than 18 ft. (5.5 m.) radius; and the roadbeds of the drifts and crosscuts have a uniform grade of 0.5 per cent. toward the shaft, or in favor of the loaded trips. In all of the mines, except two, the track gage is 18 in. (45.7 cm.): and all tracks in the main haulageways are laid with 25-lb. (11.3 kg.) rails. The stations at the shaft are large, well-lighted, clean, and cool. The average temperature of the stations, however, is about 75" F. (24" C.), while the average temperature in some of the drifts and crosscuts is 92" I?. (33.5" C.). As the orebodies lie at varying distances from the hoisting shafts,

Jan 1, 1923

By C. D. Woodward

PrioR to 1902, the tramming of ore from the stopes to the shafts, in the Butte mines, was done by man or animal power, but the demand for greater tonnage and the need for more improved methods of tramming the ore resulted in the installation of the compressed-air locomotive in a few mines. Some of the objections to animal haulage were thus eliminated, but this locomotive was not generally adopted, because of a number of limiting features. It was superseded by the electric trolley locomotive. The early types of trolley locomotives were not satisfactory from the operators' viewpoint, but they had many economic advantages and after a number of years, in which improvements were constantly made in the structural details, they became dependable, so that the use of animals for main haulage in the mines has now been practically abandoned. There are now operating in the Butte mines of the Anaconda Copper Mining Co., 185 trolley-type locomotives, each of which has replaced five animals. It cost approximately $50 per month to keep an animal, hence the economies that resulted fully justified the expenditure of electrifying the haulage systems. The haulage conditions in this company's mines possess many advantageous features that arc not always found in underground mine workings. The drifts and crosscuts are large, approximately 5 ft. (1.5 m.) wide by 71/2 ft. (2.3 m.) high, and have curves of no less than 18 ft. (5.5 m.) radius; and the roadbeds of the drifts and crosscuts have a uniform grade of 0.5 per cent. toward the shaft, or in favor of the loaded trips. In all of the mines, except two, the track gage is 18 in. (45.7 cm.): and all tracks in the main haulageways are laid with 25-lb. (11.3 kg.) rails. The stations at the shaft are large, well-lighted, clean, and cool. The average temperature of the stations, however, is about 75" F. (24" C.), while the average temperature in some of the drifts and crosscuts is 92" I?. (33.5" C.). As the orebodies lie at varying distances from the hoisting shafts,

Jan 1, 1923

By H. I. Young

Inasmuch as there has been a great deal of activity in this district recently, a paper of this kind should treat of all the various phases of mining, namely, prospecting, developing, and operating. Prospecting .. Where ore is found at a depth of 100 ft. (30 m.) or more, the prospect work is done by churn drilling. Several makes of churn drills are used in this work, both steam- and gasoline-driven machines being used. The drilling is usually started with a 6-in. bit, and the size of the bit is reduced, if necessary, as the hole is advanced. It is general practice to drill from 100- to 400-ft. holes, but this is governed entirely by the location and formation of the ground. In drilling sheet ground, close spacing of drill holes is unnecessary, but in narrow orebodies, the holes are spaced from 15 to 50 ft. (4.6 to 15 m.) apart. Ten years ago, very few assays were kept of the drilling, but during recent years records have been kept very accurately, showing the location, elevation, assays, and also the vertical section of the hole. After the orebody is reached, cuttings are taken every 2 or 3 ft. (0.6 to 0.9 m.) samples being sometimes taken by pouring the water off the cuttings and taking a portion of the coarse material for assay. It has been found, however, that very often the sludge material poured off with the water contains high mineral values. To overcome this, cuttings from each 2 or 3 ft. are put in a container, and, after the water is evaporated, sample for assay is taken by means of Jones samplers. Permanent records of cuttings showing various formations are kept in glass jars or glued on large cards. Drilling at present is costing from $1.25 to $1.50 per foot. In pre-war times, the drilling costs ran from 75c. to $1 per foot. Development After proving property by drilling, shafts are put down to the ore-body. These are usually vertical shafts, either single or double compart-

Jan 1, 1918

US 4,192,851-Recovery of elemental sulfur and the metal values from a complex sulfide ore containing two or more of the metals zinc, lead, copper, silver, gold and/or other metals. A mixture of ore and sulfuric acid and/or spent electrolyte is flowed at optimum temperature and pressure in a quiescent zone to dissolve selected metals and sulfur and coalesce the sulfur. The coalesced sulfur and unreacted sulfides are separated by flowing the leach slurry with an upward velocity component The separated materials are discharged and further processed by conventional methods as war- ranted. H.E. Hirsch, J F. Higginson, EG. Parker, and G M Swinkels, assigned to Sherritt Gordon Mines Ltd. Mar. 11, 1980. 6 pp. (423-28) Filed. 3-14-78 (886,368). Priority. United Kingdom, 3-15-77 (10800/77).

Jan 1, 1982

By Haim H. Chiswik, Ralph Hultgren

In recent years considerable attention has been devoted to the development of new commercial uses for silver, chiefly because of lowered prices and large stocks of the metal. This has led to increased interest in the phase diagrams of silver alloys. The silver-lead diagram is reported' to be of the simple eutectie type, but no measurements of the solubility of lead in silver have been made. The solubility of silver in lead has been estimated2 from diffusion experiments and resistance measurements to vary with temperature from 0.09 to 0.18 atomic per cent (0.05 to 0.10 weight per cent). Silver-rich silver-lead alloys have recently been recommended as high-strength bearing metals3 The silver-bismuth diagram is similar.' The solubility of bismuth in silver. has been estimated to be about 5.5 weight per cent on the basis of X-ray work.4 Matthiessen6 found a solubility of silver in bismuth from 0.25 to 0.50 per cent by conductivity measurements. Silver and thallium form the same type of diagram,' with no data on their mutual miscibilities. We have studied the first two of these diagrams by X-ray methods, verifying their main features and determining the solubilities of lead and bismuth in silver at several temperatures. We also determined the solubility of thallium in silver at one temperature. The solubilities of silver in lead and in bismuth were found to be too low to be detectable. Materials and Methods Mallinckrodt precipitated silver, analytical reagent, was used. Maximum impurities listed on the label were: chloride, 0.005 per cent; copper, 0.001; iron, 0.002; other heavy metals (as Pb), 0.002; and sulphate (SO³), 0.05. The lattice constant was found to be a0 = 4.0782 $., in good agreement with the value of Jette and Foote,6 a0 = 4.0779 A., for

Jan 1, 1940

By Ralph Hultgren, Haim H. Chiswik

In recent years considerable attention has been devoted to the development of new commercial uses for silver, chiefly because of lowered prices and large stocks of the metal. This has led to increased interest in the phase diagrams of silver alloys. The silver-lead diagram is reported' to be of the simple eutectie type, but no measurements of the solubility of lead in silver have been made. The solubility of silver in lead has been estimated2 from diffusion experiments and resistance measurements to vary with temperature from 0.09 to 0.18 atomic per cent (0.05 to 0.10 weight per cent). Silver-rich silver-lead alloys have recently been recommended as high-strength bearing metals3 The silver-bismuth diagram is similar.' The solubility of bismuth in silver. has been estimated to be about 5.5 weight per cent on the basis of X-ray work.4 Matthiessen6 found a solubility of silver in bismuth from 0.25 to 0.50 per cent by conductivity measurements. Silver and thallium form the same type of diagram,' with no data on their mutual miscibilities. We have studied the first two of these diagrams by X-ray methods, verifying their main features and determining the solubilities of lead and bismuth in silver at several temperatures. We also determined the solubility of thallium in silver at one temperature. The solubilities of silver in lead and in bismuth were found to be too low to be detectable. Materials and Methods Mallinckrodt precipitated silver, analytical reagent, was used. Maximum impurities listed on the label were: chloride, 0.005 per cent; copper, 0.001; iron, 0.002; other heavy metals (as Pb), 0.002; and sulphate (SO³), 0.05. The lattice constant was found to be a0 = 4.0782 $., in good agreement with the value of Jette and Foote,6 a0 = 4.0779 A., for

Jan 1, 1940

By John C. Sawyer

The mechanism of catastrophic oxidation of chromium and 446 stainless steel is examined. Data are presented to show that accelerated oxidation of these two materials, as caused by lead oxide, can occur in the absence of a liquid layer contrary to presently accepted theory. An alternate theory is proposed in which the rate of accelerated oxidation is a function of the rate at which lead oxide destroys the protective oxide formed on the base metal. An example of the application of the theory is given for the catastrophic oxidation of chromium in the presence of lead oxide. WHEN stainless iron-, nickel-, or cobalt-base alloys are heated in air to moderate temperatures in the presence of certain metallic oxides, oxidation will proceed at an accelerated rate. This phenomenon, often called "catastrophic oxidation", is most pronounced for the stainless steels. With these alloys the condition is so severe that large masses of oxide will form on the surface of the alloy in 1 hr or less at temperatures of 1200o to 1700oF. While a number of oxides are known to cause this effect, PbO, V2O5, and Moo3 are the most familiar, having been the subject of one or more investigations which have appeared in the literature.1-7 In presenting the results of these investigations, many of the authors have offered possible explanations to account for the more rapid rate of oxidation observed; however, the liquid layer theory as proposed by Rathenau and Meijering 2 has been the most commonly accepted mechanism. The liquid layer theory proposes that a low-melting oxide layer is formed on the surface of the alloy as the result of the interaction of the alloy oxide and the contaminating oxide. When the temperature of oxidation is above the melting point of the oxide on the surface, a liquid layer will form and oxidation will proceed at an accelerated rate. At temperatures below the melting point of the surface oxide, oxidation will proceed more slowly in the normal manner. It is argued that the rates of diffusion of oxygen and metal ions through the liquid layer are extremely rapid thereby accounting for the high rate of oxidation. Various experimental data have been presented to show that the temperature at which accelerated oxidation first becomes apparent coincides with the melting point of the eutectic oxide which would be present on the surface. Some exceptions have been observed, e.g., silver will oxidize in the presence of Moo3 at temperatures below the lowest melting eutectic; on the other hand, stainless steel will not be catastrophically oxidized at 1500oF in a molten bath of PbO and SiO2. In reviewing the various theories which have been used to explain catastrophic oxidation, Kubaschewski and Hopkins 8 favor the liquid layer theory, but note that, ".. .as experimental observations are not altogether in agreement with this theory (liquid layer theory), one should consider it a necessary but not a sufficient condition." In contemplating the liquid layer theory, it appears that sufficient evidence has not been presented to establish the theory beyond question. As a means of further clarification, a program of research was undertaken to determine in greater detail the mechanism of accelerated oxidation as caused by lead oxide. The first part of the program deals with a comparison of the oxidation of both AISI 446 stainless steel and chromium metal in the presence of lead oxide, vs the oxidation of these two materials in air alone. These comparisons are made at a number of different temperatures, most of which are below the melting point of the surface oxides. The second part of the program is concerned with a presentation of an alternate theory of accelerated oxidation exemplified by the system Cr-PbO-Air. PROCEDURE AND RESULTS Several experimental methods are commonly used to follow the progress of oxidation. One of these, the weight-gain method, was chosen for this work. This procedure requires that a specimen of the alloy be weighed, oxidized for a given period of time at an elevated temperature, and reweighed—the difference between the two weights being noted. The weight gain of the specimen represents the amount of oxygen acquired from the atmosphere to transform a portion of the specimen to oxide. In those cases where there is a tendency for the specimen or oxide to volatilize at the testing temperature, additional data must be collected so that a correction factor can be determined. This factor must be applied to the weight change in order to ascertain the actual amount of oxidation which has taken place. The specimens used for this work were 1 1/2 in.

Jan 1, 1963

Have your name and address on the first page of your manuscript. Typewritten manuscript is preferred, but is not essential. If you have the manuscript typewritten, have it double spaced and written on one side of the page only; send two copies to us if convenient; only one copy of the illustrations is desired. In typewritten manuscript, formulas are better inserted by hand. Keep a copy of your manuscript in case of loss in the mail. ILLUSTRATIONS.-Photographs reproduce best when printed on glossy paper. Solio is one of the best varieties. A good print is preferable to a negative. Blueprints, drawings, or pen or pencil sketches can be used for line engravings, but care should be exercised to make them legible and clear, especially in the case of blueprints. Tracings or photographs of drawings are preferable to blueprints. Rough sketches can be used, if necessary. Photographs should be sent flat, not rolled. Do not put reference letters or other marks on photographs; if such letters or marks are necessary, fasten a piece of tracing paper to the top edge, trace a rough outline of the picture upon it and then place all letters, etc. on the tracing paper lithe exact position you wish them to appear. Restrict the number of micrographs as much as possible on account of the considerable expense involved. Standard magnifications for non-ferrous metals and alloys are recommended as follows: 10, 25, 50, 75, 100, 150, 250, 500, 750, 1000, 1500. Micrographs should be trimmed to 2 1/4 X 2 1/4 in. (six micrographs to a plate), or, if larger, up to 3 1/2 X 4 in. (two to a plate). The smaller size should be adopted if consistent with adequate representation of the subject. With each micrograph should be attached an explanatory title, together with the actual magnification, etching medium, treatment, etc., indicating what the author intends to show.

Jan 1, 1919

By H. Margolin, E. Ence

In order to understand the effect of zirconium on properties of Ti-Cu-A1 alloys, Ti-Zr alloys were examined for the presence of ordering or compounds at the following compositions in weight percent: 24.1 pct Zr (lZr:GTi), 32.2 pct Zr (lZr:4Ti), 38.8 pct Zr (lZr:3Ti), 49.0 pct Zr(1Zr:ZTi). Alloys were prepared as 15-g buttons by non- consumable arc melting under argon atmosphere from Bureau of Mines titanium (Bhn 63) and Reactor Grade zirconium (Bhn 150). Weight losses during melting did not exceed 1 pct of the initial button weight. Prior to heat treatment, buttons were hot-rolled at 600" to 700°C to rods of about 6 mm diam. Contamination after hot-rolling was found to extend to a depth of less than 0.5 mm. Specimens for heat treatment were wrapped in molybdenum sheet, annealed in argon-filled quartz capsules, and quenched by breaking the capsules under iced brine. Annealing times were as follows: 700°C — 7 days; 600°C— 14 days; 575°C-1 and 2 months; 525°C-2 months; 500°C-2 months. Prior to heat treatment, all Ti-Zr alloys were vacuum annealed at 900°C to remove hydrogen. The reanneal of 575°C specimens for an additional month produced no observable microstructure changes. The results obtained by microstructure and X-ray diffraction are shown in Fig. 1, together with data of Hayes et al.' No other phases than a or P were found. Small amounts of retained P were detected by X-ray in the 49 pct Zr alloy. The data of the present investigation suggests that ß and a transus boundaries are at considerably lower temperatures than those of Hayes et al. The work of Hayes et al. is based on sponge titanium and Bureau of Mines zirconium, both of which contained 0.15 pct 0. Since melting was performed in

Jan 1, 1962

By W. A. Backofen, D. L. Holt

Push-pull fatigue tests have been carried out at 4.2°K, 77oK, and room temperature on two poly crystalline materials of widely different stacking-fault energy (?): pure copper (? - 70 ergs per sq cm) and the Cu-8 wt pct A1 alloy (? - 2.8 ergs per sq cm). Constant stress-amplilude was imposed and measurement was made of the plastic-strain amplitude (ep) at saturation. Lives extended from 104 to 106 cycles. Designating lives at the various temperatures by NRT, N77, and N4.2. the ratios N77/NNT and N4.2/N77 ranged from 3.5 to 18 under the condition of common Ep . Metallo-graphic examination revealed different crack morphology in Cu-8 Al fatigued at room temperature, and at 77" and 4.2oK. At room temperature, cracks lay in or near grain and lain boundavies; at 77o and 4.2oK. cvacks were transcrystalline. Tests on single crystals of Cu-8 A1 showed that such a change in the cracking mode in polycrystallitle material accounted for a factor of- about 3.25 in N77/NRT . The longer life at lower tewperatztre (conslant cp) has heels attributed to two deuelopinents: a reduced production of the dislocation tangles and subgrain boundaries which serve as paths of rapid cracking, and suppression of oxygen chetni-sorption at the crack tip It was concluded that in both materials the luller accounted for an extension of the life at 4.2oK beyond that at room temperature by a factor of 15. XV ECENT experiments on the fatigue of Cu-A1 alloys in the so-called high-cycle range (greater than lo4 cycles) have emphasized the importance of stacking-fault energy (y) as a quantity affecting crack propagation rate and fatigue life.1,2 It was found in comparisons at essentially fixed plastic-strain amplitude that crack growth rate decreased by a factor of about 5 over the composition range from copper (? - 70 ergs per sq cm) to Cu-8 wt pct Al (? - 2.8 ergs per sq cm). The argument was made that, when stacking-fault energy is high, cross slip and climb are favored, so that dislocation tangles and/or subgrain boundaries form more readily under cyclic loading. Since the boundaries and tangles act as paths of rapid crack propagation ,3, 4 life is shortened as a result. However, when stacking-fault energy is reduced (as by alloying), cross slip and climb become more difficult, with the result that substructure formation is retarded and growth rate is also reduced. A purpose of the present work was to investigate the substructure effect in relation to temperature. As temperature is lowered, ? is varied only slightly (if at all), but decreased thermal activation can interfere with cross slip and climb. Thus substructure formation could be curtailed and life increased. Fatigue life in the high-cycle range is also known to be strongly influenced by environment. Working with copper, Wadsworth and Hutchings observed that life in a vacuum of 10-8 mm Hg exceeded life in air by a factor of 20.5 They isolated oxygen as the agent that furthered cracking. While the details are still unclear, a requirement in any mechanism of oxygen-accelerated cracking is that there be chemisorption at the crack tip. That could prevent welding on the compression half cycle,= interfere with reversal of slip,1, 6 or aid in breaking metal-metal bonds at the crack tip.5'7 In the work being reported here, temperature was lowered by immersion in liquid nitrogen and helium, which also served to reduce both the oxygen concentration and chemisorption rate. A possible effect upon life, i.e., a lengthening, had to be recognized. Several researchers have determined fatigue lives at low temperatures presenting their results in the form of stress amplitude (S) vs cycles in life (N) curves.8-11 Such curves reflect, primarily, the fact that metal is strengthened by lowering temperature; effects of substructure and changing environment tend to be masked. The difficulty can be overcome by comparisons based on identical plastic-strain amplitudes, and in the present work the dependence of life on both plastic strain and stress amplitude was established. EXPERIMENTAL Materials. The principal materials were polycrystal-line copper (? - 70 ergs per sq cm)" and the Cu-8 wt pct Al alloy (? - 2.8 ergs per sq cm),I3 the latter being near the limit of solubility of aluminum in copper and having, therefore, the lowest stacking-fault energy in the CU-Al system. Specimens were machined from 0.118-in.-diam cold-swaged rods of high-purity (99.999 pct) copper and the Cu-8 Al alloy, the latter produced initially in a graphite boat by induction vacuum melting a mixture of 99.999 pct Cu and 99.99 pct Al. The machined specimens were annealed to produce mean grain diameters of about 0.070 mm in copper and 0.190 mm in the alloy. Specimen dimensions are given in Fig. 1. Values of the tensile yield stress, ultimate strength, uniform strain (determined by the Considgre construction), and reduction of area, for both materials at 4.2oK, 77oK, and room temperature, are listed in Table I. The tensile apparatus in which these results were obtained has already been described.14 Apparatus. Specimens were fatigued in push-pull with a machine that is illustrated schematically in Fig. 2. The specimen is first soldered into the top grip (1) with Woods metal, and the grip is then screwed into the inner tube (2) which is connected to the drive rod of the Goodmans vibration genera-

Jan 1, 1968

By J. J. Strohl, H. J. Schwellenbach

This paper relates the results obtained by decreasing the size of feed to a rod mill screen circuit. As would be expected, added production was gained and a finer grind with no tonnage loss was made possible. THE MacIntyre mill of the National Lead Co. has four parallel sections in which magnetic and gravity separations are made. Ore from a 5000-ton bin is fed by Hardinge constant weight feeders to a 6x12-ft open-end Marcy rod mill in each section. Rod mill discharge is bucket elevated to two 4x10-ft Tyrock screens whose oversize is returned to the rod mill. Screen undersize is pumped to Crockett separators for magnetite removal, and the Crockett tailings are sized and tabled to make an ilmenite concentrate. Minus 200-mesh material, overflowed by the Crockett and Dorrco sizers is thickened, de-slimed, and concentrated by flotation.' By 1948, the development of a successful slime flotation process and numerous improvements in the gravity circuit of the mill had increased the capacity of the available concentrating equipment. At the same time, improvements in the operating techniques of the dry crushing plant and improved feeding of the crusher by the mining department had appreciably increased the production rate per operating hour in that plant. Therefore, it was decided to take advantage of the added crusher capacity to produce a finer rod mill feed and in that way increase grinding capacity. At approximately the same time, finer screens were installed in the rod mill circuits to give finer grind and thus improve liberation of the magnetite and ilmenite from the gangue and from one another. Prior to the first part of 1948, a 3/4-in. limiting screen was used for sizing rod mill feed. The first reduction in crushing plant screen size was to 1/2 in. With this screen, the circulating load in the tertiary crushing circuit was too high and plant capacity dropped below a practical hourly rate. A 9/16-in.-sq opening screen, installed next, proved satisfac-

Jan 1, 1951

By H. J. Schwellenbach, J. J. Strohl

This paper relates the results obtained by decreasing the size of feed to a rod mill screen circuit. As would be expected, added production was gained and a finer grind with no tonnage loss was made possible. THE MacIntyre mill of the National Lead Co. has four parallel sections in which magnetic and gravity separations are made. Ore from a 5000-ton bin is fed by Hardinge constant weight feeders to a 6x12-ft open-end Marcy rod mill in each section. Rod mill discharge is bucket elevated to two 4x10-ft Tyrock screens whose oversize is returned to the rod mill. Screen undersize is pumped to Crockett separators for magnetite removal, and the Crockett tailings are sized and tabled to make an ilmenite concentrate. Minus 200-mesh material, overflowed by the Crockett and Dorrco sizers is thickened, de-slimed, and concentrated by flotation.' By 1948, the development of a successful slime flotation process and numerous improvements in the gravity circuit of the mill had increased the capacity of the available concentrating equipment. At the same time, improvements in the operating techniques of the dry crushing plant and improved feeding of the crusher by the mining department had appreciably increased the production rate per operating hour in that plant. Therefore, it was decided to take advantage of the added crusher capacity to produce a finer rod mill feed and in that way increase grinding capacity. At approximately the same time, finer screens were installed in the rod mill circuits to give finer grind and thus improve liberation of the magnetite and ilmenite from the gangue and from one another. Prior to the first part of 1948, a 3/4-in. limiting screen was used for sizing rod mill feed. The first reduction in crushing plant screen size was to 1/2 in. With this screen, the circulating load in the tertiary crushing circuit was too high and plant capacity dropped below a practical hourly rate. A 9/16-in.-sq opening screen, installed next, proved satisfac-

Jan 1, 1951

By H. E. Stauss, J. Hino

INTEREST in silicon has arisen again in the past decade as a result of improvements in crystal rectifiers.' Although the preparation of silicon was first reported by Berzelius in 1880, the early product was of relatively low purity, and only the need for rectifiers in World War II led to the production of a 99.9+ pct pure powder. This material in crystalline form was consolidated into massive silicon for use, and the method developed was to melt it with selected added constituents as "doping" agents. Melting techniques, therefore, are of great importance. There are two basic problems in producing silicon ingots free of doping additions; one is the prevention of spitting and the other is prevention of cracking of the ingot during freezing. The most satisfactory arrangement yet developed for producing massive silicon is to melt and freeze in a cylindrical quartz crucible surrounded by a concentric heating element and concentric radiation shields or insulation. For example, use can be made of a tubular heater with a high frequency generator as the source of power and reflecting shields of alundum cylinders. The spitting of silicon is related to gas evolution, and the gas comes from two primary causes—adsorbed gas and the reaction products of silicon and the crucible. Gas is also released from bubbles contained in the quartz crucible walls. Improved removal of adsorbed gas can be achieved by means of controlled melting and freezing. The seriousness of the problem in vacuo is reduced with an electrically operated mechanical movement of the high frequency power coil. The upper portion of the powder charge is melted first and the high frequency coil lowered until the powder is completely molten. During cooling the high frequency coil is raised slowly. These means also reduce the final nonviolent extrusion of large beads of metal through the ingot top during freezing. Better control of spitting and bead extrusion is obtained when melting is done under helium at. atmospheric pressure instead of in vacuo. The problem of reaction between silicon charge and crucible in practice is confined to the reaction between silicon and quartz. This2 apparently is: Si + SiO2 + 2SiO The part that this reaction plays in spitting has not been isolated for separate study. SiO is a volatile vapor at the melting point; of silicon and is released freely during melting in vacuo, but hardly at all in helium at atmospheric pressure. The cracking of ingots is a major difficulty in melting silicon, and its prevention requires special melting techniques or the addition of "toughening" agents such as aluminum or beryllium.' The cracking of the ingots has been explained as being the result of the expansion that occurs upon freezing; although direct observation of freezing ingots reveals visible cracks on the surface only after a red heat has been reached, suggesting that cracking is the result of differential contraction of silicon and quartz. Silicon wets quartz, and the ingot adheres tightly to the crucible. Therefore as ingot and crucible cool, the two either have to pull apart, or at least one must crack. Surprisingly, in spite of the relative thinness of the quartz and the thickness of the ingot, the ingot and the crucible both crack. Microscopic and X-ray4 studies fail to show any plastic flow other than twinning in the ingots. Slow cooling fails to prevent cracking. Another possible solution to cracking is to weaken the crucible. Use of thin-walled crucibles finally led to success with fused quartz crucibles with a wall thickness of 0.25 to 0.50 mm. With such thin-walled fused quartz crucibles consistently uniform success is secured in producing sound ingots 30 mm in diam from the purest available grade of silicon (99.9+) without the use of any type of addition. Melts are made in the size range of 50 to 100 g. Omission of a deliberately added doping agent is not sufficient to insure pure ingots. The reaction of silicon with crucibles and the resultant solution of impurities in the silicon is well-established." In this laboratory, the presence of Al, Be, and Zr has been found spectroscopically in ingots melted in contact with alumina, beryllia, and zircon. The best crucible materials reported in the literature are MgO and SiO2. Use of MgO in this laboratory has resulted in a heavy deposit of magnesium on the furnace walls, showing that a reduction of the magnesia occurred and the resulting magnesium removed from the melt by volatilization. In the case of quartz, the silica is reduced and SiO liberated to deposit on the equipment walls. There probably is real danger that oxygen is dissolved in the ingot when either magnesia or silica is used as the crucible material. Preliminary analyses by Dean Walter in his vacuum unit in this laboratory6 indicate the presence of oxygen in undoped silicon melted in quartz.

Jan 1, 1953

By Robert H. Richards, Richard W. Lodge

A great deal of speculation, as well as actual experiment, has been devoted to ascertaining the changes in the materials (luring their descent in an iron blast-furnace, affecting (1) the chemical constitution, (2) the mechanical condition, and (3) the arrangement of the materials. With a view to throw some light upon the third question, we constructed a model and tried experiments which are here described. Our model is a vertical section of a furnace, with the lines of the Edgar Thomson furnace D of 1885 for the use of which we arc indebted to Mr. Gayley. The model is 40 inches high, and made to scale (1/2 inch equals 1 foot), and the horizontal section of the space through which the charge falls at any point in the descent is 11/2 in. x d, d being the diameter of the furnace at that place. We are unable to say just where the idea of making this model came from ; perhaps, partly from The Principles of the Manufacture of Iron, and Steel, 1884, I. Lowthian Bell, p. 124 ; partly, also, from

Jan 1, 1888