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By Henry Fay

LAWRENCE ADDICKS, New York, N. Y., (communication to the Secretary *).-There are two points regarding gun erosion on which I want to say a few words: The first is about the analogy to hardening of wire by drawing and the second the possible role played by thermal conductivity of the metal. The ductile metals do not necessarily become brittle when cold-worked as it is possible to draw copper from 3. in. in diameter soft rod down to the finest hair wire without annealing. This results, as stated in the paper, informing a hardened core with a very hard skin. The electrical conductivity is depressed some 3 per cent. and the tensile strength nearly tripled. A soft copper wire 0.08 in. in diameter and 6 in. long may be twisted 150 or more turns before the wire will snap under torsion. A hard-drawn wire will break after perhaps a dozen twists, the skin breaking down at one spot. Just wiping the wire with a cloth clamp with dilute nitric acid has a remarkable effect in increasing the number of twists without appreciably lowering the tensile strength, showing the skin to be very thin. On the other hand, pickling the rod, from which the wire is to be drawn, in dilute nitric acid also greatly increases the number of twists which can be applied to the resulting wire. This indicates that the copper oxide scale produced when the wire bar is rolled hot is more or less rolled into the rod and may have much to do with the skin effect. We also know that if the conditions of drawing are not correct, the heat of deformation in the die may produce quite an annealing effect. The application of this analogy to what occurs in a gun to produce the effects noted offers some difficulty. The second point is that as the temperature of the surface of the gun bore has undoubtedly a great deal to do with the amount of erosion, one natural remedy would be to conduct the heat away fast enough to keep this temperature within desired limits. This brings up the question of the thermal conductivity of the metal of which the gun is made. We know that the conductivity of pure metals is greatly altered by alloying and that the alloy is usually, though not always, lower in conductivity than the metal before alloying. This is interesting when it is considered that the high-nickel and manganese-steel alloys show greater erosion as stated. Would it not be instructive to study the question from the point of view of heat conducted away from the eroded surface?

Jan 3, 1917

By W. R. Wilcox

The camphor-anthracene system was chosen as a transparent low-melting analog of the zirconium carbide -graphite system. Camphor and zirconium car -bide both grow nonfaceted, while casting of mixtures yields platelets of both anthracene and graphite. Zone melting of thin layers of organic was observed under the microscope. Irregular lamellar structures were produced at high values of the ratio of the temperature gradient G to the zoning rate V. The anthracene invariably led the camphor, indicating lower kinetic undercooling for the anthracene. The lamellar spacing was an order of magnitude greater than typical spacings for metal eutectic systems. Exact behavior depended on orientation of the anthracene. Oriented dendritic structures were produced at low values of G/V. Transient and oscillatory behavior were also observed—much of it unexpected. A.RC-CAST refractory carbide-graphite mixtures are promising thermal-shock resistant materials. Oriented structures of these materials would be superior to arc-cast materials for many applications. Mollard and Flemings1 and Cline2 have shown that aligned structures can be obtained for a wide range of Pb-Sn alloys. However, these metals both solidify in a nonfaceted manner while graphite yields platelets or flakes. In addition only small diameter samples of Pb-Sn alloys were produced because it was necessary to avoid free convection and to have high temperature gradients. The purpose of the present work was twofold: 1) To observe the solidification of a transparent low-melting analog of carbide-graphite systems and 2) to see if larger diameter samples can be produced. EXPERIMENTAL PROCEDURE When zirconium carbide-graphite mixtures are cast, the resulting structure naturally depends on composition. Carbide-rich mixtures yield metal-like nonfaceted carbide dendrites in a eutectic matrix. Graphite-rich alloys have graphite platelets in a eutectic matrix. Empirically it was found that camphor-anthracene mixtures produce similar structures with camphor being nonfaceted and anthracene forming plates. The organic eutectic melted at 116°C and was composed of 78 wt pet camphor.3 The camphor used was U.S.P. grade from Fisher Scientific Company; the anthracene was 98+ pet fro Aldrich Chemical Co. The impurity content is judged to be on the order of 1 pet. Mixtures ranging from 50 to 88 wt pet camphor were employed for the experiments. All but one of the experiments were performed on the microscope-stage zone melting apparatus described in detail elsewhere.4 The organic mixtures were contained in horizontal cells made of microscope slides or cover glasses. In most of the cells the organic was present as a very thin layer, thus giving almost two-dimensional growth behavior. The cells were moved slowly under a heated wire, which caused a molten zone to move through the solid at rates ranging from 0.01 to 5.4 cm per hr. The temperature gradient was estimated before moving the zone by measuring the distance between the line where all solid was melted (freezing point) and that where solid first began to melt (eutectic temperature). The temperature gradient was found to be 465°C per cm in the thinnest cells used, which were made by pressing together two microscope cover slips in the organic melt and then rapidly withdrawing them. RESULTS The experimental results are described in four parts: simultaneous growth, dendritic growth, irregular growth, and transients and erratic phenomena. Steady state data are summarized in Fig. 1. Except where noted all comments are for the cells containing a thin layer of organic. A) Simultaneous Growth. Simultaneous and roughly parallel growth of anthracene and camphor was obtained over the full range of compositions investi-

Jan 1, 1970

By Paul A. Farrar, Harold Margolin

The system Ti-Cr has been re investigated From 40 to 100 pct Cr. The high-temperature modification of TiCr, was found to exist in the temperature range from 1365 where it terminates in the eutectoid reaction TiCr,(TI)* — HE chromium-rich region of the Ti-Cr system was investigated by Vogel and Wenderott,' Mc Quillan,' Van Thyne et dl.,' and Cuff Duwez and Taylor determined the crystal structure of the low-temeperature modification of TiCr, to be fcc a = 6.943A and Levinger' discovered the existence of a second (high-temperature) modification of TiCr, and determited its crystal structure to be hexagonal a = 4.932A, c/a = 1.617i. No information was obtained as to the temperature range over which each modification of TiCr? existed; therefore the present investigation was initiated. I) Experimental Techniques Alloys employed for the delination of this system were prepared from iodide titanium and high-purity chromium. The purity of these materials is as follows: Iodide titanium: purity 99.99 pct; major impurities—carbon 0.0001 pct; oxygen 0 to 0.002 pct; nitrogen 0 to 0.002 pct; silicon 0 to 0.005 pct; manganese 0.001 pct; copper 0.001 pct (Foote Mineral Co., Lot 609-29). Chromium #1: metallic purity 99.997 min.; interstitial content—oxygen 0.27 to 0.46 pct; hydrogen 0.028 to 0.038 pct; nitrogen 0.0002 pct (Ave-quipo Inc.). Chromium #2: purity 99.9 pct; major impurities—carbon 0.01 pct; oxygen 0.013 pct; nitrogen 0.02 pct; silicon 0.01 pct; sulfur 0.03 pct; iron 0.01 pct (Fulmer Research Institute Ltd.). A total of sixteen alloys of thirteen different compositions was prepared in the range from 40 to 95' *All percentages are given in weight percent. pct Cr. The compositions of the alloys prepared were as follows: Ti-40, 45, 50, 60, 62, 64, 66, 68, 70, 80, 85, 90, and 95 pct Cr. Two buttons were prepared of the 66, 90, and 95 pct Cr alloys. The 40 pct Cr and one of the 66 pct Cr alloys were prepared from the chromium # 2. All the other alloys were prepared from chromium #1. The alloys were arc-melted as 25-g buttons in a copper-hearth glass-walled furnace7 under an inert atmosphere of high-purity helium. The alloys were sintered at 250 amp and melted twice at 350 amp for 30 sec with the buttons being turned over between melts. Weight losses during melting were determined and in the range 45 to 68 pct Cr they were found, in all cases, to be less than 1.25 pct of the total alloy weight. A number of the high-chromium alloys shattered during cooling from either the first or second melt, which made the weight loss considerably larger than usual. The 70 and 80 pct alloys lost approximately 5.7 pct of their total weight, the 85 pct alloys 1.5 pct, the 90 pct alloy 2 pct, and the 95 pct alloy 3 pct. However, it is felt that the actual composition of the alloys in this region is probably within approximately 1 pct of the intended composition, as a large portion of the material lost was that due to shattering after melting. Nominal compositions were therefore used in plotting data and referring to the alloys. The alloys were cut into specimens, wrapped in molybdenum sheet, and encapsuled in argon-filled quartz or Vycor tubes for heat treatment. The heat-treatment times and temperatures are given in Table I. The specimens were quenched in iced brine (I.B.Q.) following heat treatment. The standard techniques of grinding, polishing., and etching were used in preparing the specimens for metallo-graphic examination. For alloys below 68 pct Cr

Jan 1, 1963

By M. E. Learmont, I. Iwasaki

Grinding with steel media adversely affects the flotation response of galena. Electrochemical measurements, flotation tests, and AES, XPS, and STEM examinations were employed to identify interactions between galena and mild steel. Iron oxide, hydroxide, or sulfate species that formed on the galena surface upon contact with mild steel decreased its floatability, with the time of contact and aeration condition affecting the severity of the flotation depression. Parallel tests performed with an active metal, magnesium, indicated that floatability was also affected by the presence of a surface coating involving lead species.

Jan 1, 1985

International Trade in Nonmetallic Minerals. BY J W FURNESS AND E W PEHRSON (Man &. Met, Sept, 432 2500 words) International trade in nonmetalic minerals (exclusive of fuels) is dominated largely by fertilizer raw materials such as phosphate rock, potash, nitrates, sulphur and pyrites and the miscellaneous group of minerals including asbestos, mica, graphite, fluorspar and china clay Cost of trans¬portation deters any substantial movement of the building materials which usually occur widely in nature and are thus available near consuming centers at relatively low cost This paper, which presents a summary for 1932 of the world production, consumption and principal trade relations of asbestos, china clay, fluorspar, graphite, gypsum, mica, phosphate rock and potash illustrated by world charts, is based on an original study of 15 nonmetallic minerals conducted by the U S Bureau of Mines Practical and Legal Aspects of Mme Financing See METAL MINING Economic Significance of High-grade Concentrates See MILLING AND CONCENTRATION

Jan 1, 1937

By Yasushi Ishikawa

The fact that the degree of granulation and the state of granulated particles of sinter raw mixtures are the influential factors in ensuring coke combustibility and permeability during sintering has been clarified. Based on this knowledge, Nippon Steel developed the divided coke-addition process and the technology to utilize binder, and applied them on a commercial scale. Productivity and sinter quality are thereby greatly improved with a significant reduction in fuel consumption.

Jan 1, 1977

Abbott, Robert H., (S'42) Agricultural & Mech. College of Texas, College Sta.. Texas. Abrahamson, Guy C., (S'43) Univ. of California, Berkeley. Calif. Abrego, Alfredo, (S'43) Texas College of Mines & Metallurgy, El Paso, Texas. Ackermann, K. G., (S'43) Univ. of Alabama, University, Ala. Adamec, Lew, (S'42) Colorado School of Mines, Golden, . Colo. Adams. Charles E., (S'42) Univ. of California, Los Angeles, Calif. Adams, Charles W., (S'30) Asst. Met., Canada Foundries & Forgings Ltd., Welland, Ont., Canada. Adams, John W., (S'42) Univ. of Texas, Austin, Texas. Adams, Karl S., (S'43) Univ. of New Hampshire, Durham, N. H. Adamson, Charles R., (S'41) Univ. of Utah, Salt Lake City. Utah. Adler, A. G., (S'41) Met. Engr., Flotation Operator Helper. Utah Copper Co.. Garfield, Utah. Adler, Frank J., (S'42) Colorado School of Mines, Golden, Colo.

Jan 1, 1943

By R. J. Quigg, G. S. Doble

Commercial stress -relieved TD Nickel bar was shown to retain room- and elevated-temperature tensile strength after exposure up to 2501°F. Cold swaging increased both room -temperature and 2000°F tensile strength. After annealing at 2500°F the strengthening due to swaging was retained at 2000°F hilt eliminated at room temperature. Annealing produced changes in hardness and X-ray half peak width indicating the presence of recovery processes as 1071° as 1000°F but no recrystallization of swaged material was noted at any temperature. In contrast to swaging, rolling induced a recrystal-lized structure after annealing. The tensile strength of this recrystallized structure was comparable to the cold-worked condition. High-temperature tensile properties of as -received bar were highly anisotropic with the transverse tensile strength being one fifth the longitudinal value. The aniso-/ropy is affected by working direction and may he partially reversed by changing the direction of metal flow. The divergence in tensile strength, beginning above 550°F or- approximate one third the absolute melting point, is strain-rate dependent. T D Nickel is a commercial dispersion-hardened alloy containing 2 vol pct thoria. The dispersion, consisting of spherical particles 0.030 to 0.050 in diameter with an interparticle spacing of less than 1 is reported to maintain stable properties up to 2400°F.1 This stability of second phase results in maintenance of elevated-temperature strength at higher temperatures and longer times than normal nickel-base superalloys.2 The purpose of this paper is to describe the effect of various mechanical working operations on the strength and microstructural stability of TD Nickel bar. MATERIAL AND PROCEDURES All material used in this study was commercial TD Nickel bar. This material is produced by a chemical process which results in a nickel powder containing a dispersion of thoria particles. The powder is then pressed, sintered, extruded, and subsequently worked to bar stock. Three starting materials from three separate lots were used: as-extruded bar. 1-in.-diam stress-relieved bar, and 1/2-in.-diam stress-relieved bar. Since TD Nickel bar stock is cold-worked without a recrystalliza-tion anneal, the accumulated deformation or degree of cold work in these materials increases as the bar diameter decreases. Some of the 1/2-in.-diam bar was swaged to 1/4 in. diameter at room temperature in order to produce an as-worked condition for comparison with the stress-relieved stock. Tensile testing was performed on an Instron Tensile Tester at a constant crosshead speed of 0.020 in. per min. The 0.2 pct offset yield strength was measured from the load-crosshead movement plot. Specimen gage dimensions were 0.080 in. in diameter by 0.40 in. in length, producing a strain rate of approximately 0.050 min-1. Specimens were tested in air and heated within a resistance-wound furnace controlled to ±5°F. A 15-min soak at temperature was employed before testing. Samples were heat-treated in air and specimens machined after exposure with sufficient material removed to eliminate any surface contamination. X-ray line breadth was determined from a diffractometer scan of a transverse face of a bar using copper K, radiation. Metallographic preparation utilized standard mechanical polishing with Carapella's etch. Specimens for electron microscopy were electropolished in a 1:7 sulfuric/methaol solution and chromium-shadowed collodion replicas prepared. RESULTS AND DISCUSSION I) Effect of Elevated-Temperature Exposure on the properties of TD Nickel. The effect of various elevated-temperature exposures on the room-temperature tensile strength of TD Nickel is shown in Table I. In the unexposed condition the tensile strength, reduction in area, and hardness all increase with increasing accumulated deformation while the elongation decreases. After exposure at 2500°F the strength of all three materials decreases to about 65,000 psi and the elongations increase slightly. The apparent increase in strength of the 1-in. bar after a 2000°F treatment is probably experimental scatter. These results indicate that the room-temperature strengthening due to additional deformation is annealed out upon elevated-temperature exposure. In contrast to the room-temperature data, the 2000°F tensile strengths increase in order of increasing deformation even after exposure. Although some loss of strength occurs after exposure, much of the effect of working is still maintained at 2000°F. The room-temperature hardness after various

Jan 1, 1965

By Herman Van Fleet, Frederick W. Neil, O&apos

The object of this paper is to describe the present status and possil~ilities of liquid oxygen as an explosive based upon the investigations, research and practical work of the Ingersoll-Rand Co., and of the Air Reduction Co., from early in 1922 to date. The following work was done. 1. A study of the history and physical theory of L. 0. X. as an explosive. (No attempt will be made in this paper to give the history or theory, as this has already been covered by the literature on the subject.) 2. An investigation of the use and the practice with L. 0. X. in the iron mines of Lorraine where L. 0. X. has its largest application in Europe. Although L. 0. X. is extensively employed in the iron mines of Lorraine, many of the mines using it exclusively, and blasting with it a total of approximately three million tons of iron ore per year, the fact that the mining practice in Lorraine1 is to drill comparatively shallow holes and blast only a few holes at a time, renders the data obtained there of very little value in estimating the possibility of replacing dynamite with L. 0. X. in American mining methods. In fact, in the iron mines in Lorraine, L. 0. X. replaced black powder, or its equivalent. 3. Laboratory research work on properties of absorbent materials. 4. Work in the Bureau of Mines explosive laboratory at Pittsburgh, Pa., on the properties of L. 0. 3. cartridges. 5. Practical work underground with L. 0. X. cartridges in the Kitherbee-Sherman iron mines at Mineville, N. Y. 6. Practical work in the quarries of the Calcite Quarry Co., Myers-town, Pa. 7. Practical blasting in several quarries and open-pit mines.

Jan 1, 1927

By R. S. Handy

AT THE TIME of my first visit to Bolivia in 1927 the tin-mining industry was prosperous, the tin price at London being more than £300 per long ton of tin, and the operators were making every effort to bring their plants up to the very highest point of capacity as well as of efficiency. Any device or piece of equipment or method that gave promise of increasing production was welcomed regardless of the cost, and the plants were being modernized as rapidly as human ingenuity could make it possible. At the time of my second visit in 1932, however, conditions had changed materially. The price of tin had fallen to a little over £100 but costs had not decreased anywhere in proportion and operators were at their wit's end to cut the operating losses that were everywhere prevalent. Charles L. Bradbury, manager of the Empresa Minera de Huanuni, at Huanuni, Bolivia, had been recently called from Mexico to make all analysis of the situation and to attempt to work out a remedy for the economic conditions that threatened to close the mine. His analysis brought out the following points:

Jan 1, 1938

By Robert H. Richards

This truly remarkable machine was built on a preliminary scale in May, 1895. The first full-sized table was built by Mr. A. R. Wilfley, and was used in his own mill in Kokomo Colo., in May, 1896. The first table sold for installation was placed in the Puzzle mill, Breckinridge, Summit county, Colo., in August, 1896. The mill enthusiasts at first hailed it as the cure for all the ills that flesh is heir to in the milling line. A little later it was found to make losses which were serious, and on this account the table succeeded only to a limited extent in displacing the vanners of the gold-mills. Still later, mill-men in a number of districts throughout the country made special studies of the faults of the machine, and devised a number of ways of grouping supplementary machines to overcome as far as possible the losses, and at the same time retain the benefit of the extraordinarily large capacity accompanied by the production of clean concentrates for which the machine has become so justly famous. I hope to make an exhibit of some of these methods in an appendix to my book on ore-dressing which is now in preparation. These experimenters have not written up the subject, and if they possess all the facts they have not given them out for the benefit of the mining profession at large. The object of this paper is to obtain the facts and to present them so clearly that their bearing can be seen by all. To this end two complete series of tests have been planned. One (the present paper), to study concentration of galena in presence of quartz; the other (to follow shortly), to study concentration of chalcopyrite in presence of quartz. Some authorities claim that the table does its best work when treating natural products; by this phrase I mean products which have been crushed to pass through a limiting

Jan 1, 1908

By C. D. King

THE key to maximum production of ingots for the war effort is maximum production of pig iron. For any given furnace and ore, the most important single influence on blast-furnace production is the quality of the furnace coke. It is generally recognized that undoubtedly deterioration of Pittsburgh coking coals will be accelerated by the depletion of some of the better grades' of coal; the extension of mine mechanization, with attendant degradation of coal quality; and the opening of new coal fields, some of which are known to be fairly high in sulphur. All of these factors, contributing as they do to higher ash and sulphur, and not infrequently to inferior quality of coke, made it desirable that an extensive study be undertaken to determine the effect of washing some coals that closely approximate the average chemical composition of coking coals to be expected in the future by the subsidiaries of the United States Steel Corporation in the Pittsburgh district. It was deemed advisable to study the improvement obtained by washing such coals and to determine the need for supplementing the existing coal washery at Clairton to assure continued maximum production of pig iron from presently available furnace stacks. The existence of the coal washer at Clairton made it possible to conduct tests on coals used in raw form and on similar coals after washing. This study covers an investigation of the quality of furnace coke as affected by washing coking coals, and is confined to the use of 100 per cent high-volatile Pittsburgh seam coals from Fayette and Greene Counties in the manufacture of furnace coke. It covers the improvement in chemical and physical properties as well as the degree of uniformity in coke obtained by washing these coals, and includes the effect on blast-furnace production and practice. The test period involved is four months; the plants, Clairton by-product coke plant, and the Carrie No. I and No. 2 blast furnaces at Rankin, Pa., Carnegie-Illinois Steel Corporation. CLAIRTON BY-PRODUCT COKE PLANT AND COAL WASHER The Clairton by-product coke plant carbonizes 30,800 net tons of coal daily in 22 batteries containing 1482 ovens. Three oven sizes are used, commonly known as wide, medium, and narrow types, recognizing the difference in oven width. These ovens also differ in height and length. The present coal washer has a daily capacity of- approximately 14,000 tons, leaving 16,800 tons to be carbonized in raw form. Washed coal is used on all the narrow ovens and on three of the six batteries with ovens of medium width, raw coals being used on all the remaining ovens. The customary arrangement is

Jan 1, 1943

By Carle R. Hayward

SulphuR has long been one of the banes of the steel manufacturer and often no effort and expense have been spared in order to reduce it to a small per cent. in the finished product. This condition is due to a general conviction that in many cases where steels have failed in service, sulphur has been the cause. But there has been a growing feeling in recent years that the verdict against sulphur has been unnecessarily severe. In cases of segregation it was present in. augmented amounts along with other impurities, but it had not caused the segregation. High sulphur in pig iron is caused by poor furnace conditions and the sulphur is merely one indication of an iron that has not been properly reduced. No amount of subsequent treatment under oxidizing conditions in the open-hearth furnace can remedy the defects, although the per cent. of sulphur may be considerably reduced. In other words, the causes of bad steel can frequently be traced back to bad pig iron, and sulphur is merely one indication that the pig iron is bad. The writer recently visited a steel plant where a mass of evidence had been accumulated which substantiated this fact, and the superintendent was emphatic in stating that high sulphur was not harmful provided the steel was not otherwise poor due to insufficient reduction in the blast furnace. The presence of a moderate amount of sulphur is desirable from the standpoint of the man who machines the steel. The low-sulphur material drags and the production of a smooth surface is very difficult. A slight increase in sulphur enables the machinist to produce a smooth surface without difficulty. Since, therefore, such large quantities of steel are subjected to machining, it becomes highly important that the sulphur controversy should be settled, and if its presence is proved to be harmless the ban on it should be lifted. Among the recent papers on the effect of sulphur on steel is one by Dr. J. S. Unger, Manager of the Central Research Bureau, Carnegie Steel

Jan 1, 1917

By F. H. Wilson, R. M. Brick

With the papers of Palmer and Smith1 and of Burghoff and Bohlen,2 published in 1942, understanding of the problem of the development of ears on deep-drawn brass cups was brought to the point where, from a practical standpoint, producers of brass sheet could keep earing under control. However, these very practical results raised questions concerning the reasons for the observed behavior. Since plastic deformation is fundamentally a function of crystallographic slip, these reasons must be considered in the light of the textures to be found in the annealed sheet. Various attempts have been made. to interpret the mechanism of ear formation by correlation with the preferred orientation and the anisotropy of the sheet. However, none of these has satisfactorily explained why ears are usually found in the rolling and transverse directions for copper but at 45' to these directions for brass. This paper offers additional data on these two related subjects and has been divided into two sections The first section provides a survey of the recrystallization textures of brass as affected by annealing temperatures and prior reductions, and an account of the caring behavior which accompanies these textures. The second section reports new data on the anisotropy that accompanies a characteristic texture for brass and endeavors with partial success to establish the factors that account for the difference in earing behavior between copper and brass Earing BehavioR oF Brass Review of Textures The recrystallization texture of severely rolled brass was first reported by Bass and Glocker.3 The preferred orientation to which this texture, obtained from metal annealed at 500°C., was most akin was (II3)[I12] This texture has been confirmed by Bauer, von Göler and Sachs;4 Brick;' Brick, Martin and Angier;6 and Cook and Richards7 who, in general, used annealing temperatures under 500°C. Bass and Glocker3 also reported the recrystallization texture at 850°C. to be the same as at 500°C. They analyzed their textures by means of single photograms obtained with white radiation. The photo-grams for both temperatures are reproduced in their paper, and there is a strong similarity between the two. However, for the latter temperature, the number of spots registered on the film was remarkably large for the grain size to be expected, and the authors made no mention of using a technique that would integrate a large enough area of the specimen to produce so many spots. The only other attempt to determine textures resulting from high temperature

Jan 1, 1945

By R. G. Gifkins

Mean boundary migration depended linearly upon creep extension under various conditions. Prolonged annealing or air-casting increased the proportion of immobile boundaries at a given stage of tests. Grain growth during annealing followed a power law. The linking of migration and sliding in creep and models for migration are examined; activation energies are calculated from these models. Segregation of oxygen to boundaries appears to be a controlling factor. THE idea that boundary migration and boundary sliding during creep are linked has often been suggested,'-5 especially when evidence has been obtained for an alternation between the two processes. In simple bicrystals sliding can occur without any migration6 but in more complex bicrystals7 it is observed. McLean' and Couling and Roberts 5 made measurements of both sliding and migration; McLean concluded that there was no linking of the two processes whereas Couling and Roberts supported the idea. McLean' also developed a model for migration during creep and annealing. The present work was initiated as part of a study of the recrystallization of lead during creep9 but has been extended to examine some aspects of the mechanism of migration. MATERIALS AND METHODS Specially refined high-purity lead* was used; the total of impurities, excluding oxygen, was 0.0008 wt pct. Oxygen was removed as far as possible by melting in vacuo, treating at 550" to 600°C with hydrogen and then casting at 450°C under a vacuum of 10-2 mm Hg; the oxygen was then believed to be 0.00005 wt pct. Specimens were made from extruded strip and then annealed at the required temperature in an air oven, controlled to 5 lac. They were then polished in a mixture of acetic acid and hydrogen peroxide. At this stage some specimens were etched to give grain contrast and their grain sizes determined by the intercept method. Migration of boundaries during creep was measured on the surface of polished (not etched) specimens, directly loaded at room temperature (22°C) or 50°C (52"C) to initial stresses of 300 to 700 1b per sq in. Twenty six vacuum-cast hydrogen-reduced specimens were used and, in addition, two specimens were from material air cast after hydrogen reduction ("partial" air cast) and two from air-cast material not treated with hydrogen ("full" air cast). Duplicates were made in the majority of tests. At intervals through the creep tests, specimens were unloaded and the migration measured, normal to the direction of migration at the point of measurement, for each boundary along standard traverses. Usually between 110 to 180 boundaries were measured at each of some twelve stages of the tests. Migration was measured on the projected image (X100) using prism illumination. Fig. 1 illustrates the method of measurement and shows the kind of variation of migration found from boundary to boundary and along particular boundaries. Fig. 2 gives an example of more extensive migration. The mean value of distance migrated was generally reproducible to *10 pct but occasional points gave a scatter of *20 pct. The correctibn applied by McLean8 to allow for the contribution sliding makes to the apparent distance of migration could not be used, for the sliding at most boundaries was too small to measure with the equipment available. There were two reasons for supposing the correction unnecessary in the present work;

Jan 1, 1960

By A. Paul Bond

Two series of 17pct Cr iron-base alloys with small, controlled amounts of carbon and nitrogen were vacuum-melted in an effort to detertmine the meclz-uniswls of inter granulur corrosion in ferritic stain-less steels. An alloy containing 0.0095 pct N aid 0.002 pct C was very resistant to intergranular corrosion, even after sensitizing heat treatments at 1700" to 2100o F. However, alloys containing more than 0.022 pct Ni and more than 0.012 pct C were quite susceptible to intergranular corrosion after sensitizing heat treatments at temperatures higher than 1700°F. This corrosion was observed after the usual exposure tests and after potentiostatic polarization tests. Electronmicroscopic examination of the alloys susceptible to intergranular corvosion revealed a small grain boundary precipitate; this precipitate was absent in the alloys not susceptible to such corrosion. Thc electronmicrographs indicate that intergranu1ar corrosion of ferritic stainless steels is caused by the depletion of chromium in areas adjacent to precipi-tates of chromium carbide or chromium nitride. It also seems likely that the precipitates themselves are attacked at highly oxidizing potentials. Confirma-tion of the proposed mechanisms was obtained in tests on air-melted ferritic stainless steels containing titanium. The titanium additions greatly reduced susceptibility to intergranular corrosion at moderately oxidizing potentials but had no beneficial effect at highly oxidizing potentials. A major obstacle to the use of ferritic stainless steel has been their susceptibility to intergranular corrosion after welding or improper heat treatment. It appears that sensitization of ferritic stainless steel occurs under a wider range of conditions than for austenitic steels. In addition, a greater number of environments lead to damaging intergranular corrosion of sensitized ferritic stainless steels than to sensitized austenitic steels. The chromium depletion theory of intergranular corrosion is widely accepted for austenitic stainless steels'" although there: are some objections.3 On the other hand, several alternative mechanisms proposed for ferritic stainless steels include precipitation of easily corroded iron carbides at grain boundaries,' grain boundary precipitates that strain the metal lat-tice,5 and the formation of austenite at the grain bound-arie.6 The application of the chromium depletion theory to ferritic stainless steels has been discussed extensively by Baumel.7 The present investigation was undertaken to determine which of the proposed mechanisms can be sub- A PAUL BOND IS Research Group Leader, Climax Molybdenum Co of Michigan, Ann Arbor, Mich. stantiated with experimental data obtained on ferritic stainless steels. High-purity 17 pct Cr alloys containing small controlled additions of carbon or nitrogen were therefore prepared, and then examined electro-chemically and metallographically. EXPERIMENTAL PROCEDURES Materials. Two series of experimental alloys were prepared from electrolytic iron and low-carbon ferro-chromium using the split-heat technique. In this technique, the base composition is melted, and part of the melt is poured off to produce an ingot. To the balance of the melt, the required addition is made and the next ingot cast. This process is repeated until a series of the desired compositions is cast. By this procedure the impurity levels are essentially constant within each series. All the alloys in the carbon-containing series were melted and cast in vacuum. The base composition in the nitrogen series was melted and cast in vacuum; subsequent ingots in the series were melted with additions of high-nitrogen ferrochromium, and cast under argon at a pressure of 0.5 atmosphere. Two additional alloys were produced starting with normal purity materials. They were induction-melted while protected by an argon blanket and cast in air. Table I gives the composition of the alloys. The 2-in.-diam ingots produced were hot-forged and hot-rolled to a thickness of 0.3 in. and then cold-rolled to 0.15 in. All specimens were annealed at 1450°F for 1 hr. The indicated sensitizing heat treat-s s ments were performed on annealed material. All heat treatments were followed by a water quench. Specimen Preparation. For the 65 pct nitric acid test, 1 by 2 by 0.14-in. specimens were wet-surface ground to remove surface irregularities and polished through 3/0 dry metallographic paper. For the modified Strauss test, $ by 3 by 0.14-in. specinlens were similarly prepared. Immediately prior to testing, the Table I. Compositions of the Alloys Composition, pct Alloy Cr hio C N 270A 16.76 0.0021 0.0095 270B 16.74 0.0025 0.022 270C 16.87 0.0031 0.032 270D 16.71 0.0044 0.057 271A 16.81 0.012 0.0089 27 IB 16.76 0.018 0.0089 271C 16.69 0.027 0.0085 271D 16.81 0.061 0.0O71 4073' 18.45 1.97 0.034 0.045 4075† 18.5 2.0 0.03 0.03

Jan 1, 1970

By P. G. Shewmon, H. E. Collins

A study has been made to determine the sites at which sulfur adsorption occurs on copper surfaces. measurements were made of the relative torques, Ys, at the intersection of twin boundaries with surfaces near the three low-index orientations, i.e., (100), @lo), and 011), over a range of H2S/H2 ratios. HZS concerztvations j'ro~n 3 to 1500pp)n between 830" and 1050°C were used. It is concluded that sulfur adsorption occurved preferentially though not exclusively at edge sites near the (100) and (110) surfaces in the HzS range — 700 Ppm giving rise to negative torques near these orientations. Beyond this HzS range, adsorption occurred at all sites. Near the (111) surface, 7/y little with HzS concentration up to approxiwzately 75pptn. Above this range, the results indicate adsorption is occurring OH both terrace and edge sites. SCIENTIFIC interest in surfaces and their interactions with a gaseous environment dates back to the beginning of the 19th century. The scientific luminaries of that period—Faraday, Maxwell, Rayleigh, Dewar, and Gibbs—were already concerned about such processes. However, it has only been within the past several decades that adsorption on metal surfaces has been actively studied. This increased interest in adsorption has been brought about by the advent of new and improved experimental techniques and apparatus, e.g., ultrahigh vacuum, and field-emission and ion microscopes. However, most of the work done using these techniques has been carried out at low temperatures. When adsorption studies have been made at either low or high temperatures, they usually gave no indication of the particular surface orientations or type of sites on which adsorption was occurring. In the last few years, there have been a series of studies in which the surface tension, y,, and/or its derivative with respect to orientation, 7, have been studied as a function of orientation and atmosphere.'-7 Nearly all of the work on the relative torque,* ~/y, silver annealed in hydrogen and air.6 Recently Winterbottom and Gjostein" have used a modified and more accurate Mykurian method to determine the y plot of gold in hydrogen The only work in which T/~, has been measured over a range of chemical potentials for a given solute, p2, is that of Robertson and shewmon7 on the Cu-0 system. They measured T/Y, vs Po, (10"" to 10- l3 atm) at 1000°C in various mixtures of Hz0 and HZ. From this work they estimated the value of p2 at which one half of the surface sites are occupied with oxygen, pg, as being in the range 10- l6 to 10- l5 atm of oxygen. They also found that increasing Pa increased the magnitude of ~/y, near the (111) and (100) orientations. This indicates that oxygen is not adsorbed preferentially at step edges, but uniformly over all surface sites. In addition, they did one experiment on sulfur adsorption on copper surfaces, which indicated that sulfur adsorption decreases ~/y, near the (100) orientation, while not affecting ~/y, near the (111). This could be interpreted as indicating that sulfur adsorbs preferentially at step edges near the (100). In this paper the primary objective of the work has been to carry out a study of sulfur adsorption on copper surfaces over a range of temperatures and p,. In conjunction with this work, thermal grooving at grain boundaries has been examined as a method of determining the effect of sulfur adsorption on y,. METHODS Ideally, one would like to have information on the quantity of solute adsorbed on a surface and the types of sites at which it is absorbed as a function of p2. The total quantity adsorbed or the surface excess is given by the thermodynamic equation Thus data on the variation of y, with pz indicates the value of p2 at which adsorption becomes appreciable and the quantity adsorbed. The type of adsorption site is more difficult to deduce but information on this can be obtained from the variation of rz with 8, the angular deviation of the surface orientation. This is obtained from the thermodynamic equationlg Data on t and ys as functions of p2 have been obtained by the following methods. 1) Twin Boundary Grooving—By determining the effect of adsorption on the torque, 7, where T is the variation of surface energy, y,, with orientation, it is possible to obtain some indication as to the preferred sites of adsorption. Experimentally, the torque value measured is the relative torque, 7/ys The twin boundary grooving technique suggested by Mykura'' was used in this study to determine near the three low-index orientations— (loo), (110), and (111). Mykura's equation relates 7 /yS to measurements of the di-

Jan 1, 1967

By Bernard Kopelman

THE particle size of tungsten metal powder used to make tungsten wire for use in radio tubes and incandescent lamps must be closely controlled if the highly desirable feature of nonsagging is to be achieved. Our knowledge of factors affecting the particle size of tungsten powder has been limited by lack of any extensive literature on the subject. There are no publications in the English language discussing this problem in any but the most general terms. In this paper the published experimental information on this subject is reviewed. Based on the published data and some experimental data obtained by the author, a general theory of factors affecting the particle size of tungsten metal powder obtained by reduction of the oxides in hydrogen is offered. The various forms of the tungsten oxides and tungsten metal used in the experiments described were those prepared by com¬mercial processes, so that the experimental results obtained on a laboratory scale would be more directly applicable to actual commercial reduction conditions. The effects of time of reduction, temperature, and concentration of water vapor in the hydrogen were observed by counting microscopically the particle distribution obtained. Such a method is very time-consuming, but the data obtained by this method are more reliable and more fundamental than those obtained by any of the several instruments available for measurement of particle size. REVIEW OF THE LITERATURE Until the year 1912, tungsten powder was prepared commercially by reducing tungstic oxide in the presence of carbon or one of its compounds (such as glycerin or ethylene glycol), usually by firing the mixture in a closed fire-clay crucible. The resultant powder contained about 95 per cent tungsten.1 When reduction of tungsten oxides by H2 was introduced commercially, 2.1 several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-13 While these many investigations were in fair agreement on the equilibria there arose considerable controversy as to the chemical composition of the oxide between W03 and W02, because of very poor agreement on the equilibrium constant of this intermediate oxide reduction reaction. The controversy on this intermediate oxide has been in progress for more than 10o years. Thus Malguti,14 in 1835, decided it was W02.56. In 1857, Riche" proposed the formula W308. Usler,16 in 1865, confirmed the existence of W308 and further proposed W4O11. In 1897, Desi17 agreed upon W308 but also found W5014.

Jan 1, 1946

By G. H. Clevenger

(Continuing the discussion of the paper of James Johnston, presented at the New York meeting, February, 1914, and printed in Bulletin No. 85, January, 1914, pp. 107 to 133.) This paper cannot fail of being of great interest and value to all who are interested in the cyanide process, on account of the important developments which it records. Mr. Johnston is to be commended for the large amount of detail which he gives, and the company and its management for permitting the publication of data of this character, which while of great value to others could well be considered private property. It might be discussed from a number of standpoints: First, as an example of recent practice in mill and cyanide plant construction; second, the mill practice; third, the cyanide practice; and fourth, the new features in cyanide treatment involved. Perhaps a more vivid way of expressing it would be : First, the equipment or tools with which the various operations are carried on, are they the best and most efficient which could have been selected for their respective uses; and, second, is the best use in every case made of these tools? It may be well inquired is the highest possible recovery of silver made at the lowest cost per ounce recovered? For after all, the making of the greatest ultimate profit is inseparably associated with successful metallurgical practice; there must therefore be at all times a careful balance maintained between recovery and cost of obtaining it. I wish to call attention in a very general way to the equipment used and to an anticipation of questions which are bound to arise in this connection. However, the. bulk of my discussion will be confined to the presentation of certain additional data, together with a more or less general discussion showing the line of development which leads up to the present practice and .the applicability of certain features of it to similar problems elsewhere. There are a number of vital points of broad general interest involved in Nipissing low-grade practice upon which metallurgists will by no means be agreed to which I wish to call particular attention in the hope that it will lead to the presentation of data y others of practice in other districts which will' assist in reconciling this divergence of opinion.

Jan 7, 1914

By R. H. Smith, A. C. Polk

The physical properties of the materials are listed, together with a short explanation of how this material binds the sand grains together without materially reducing the effective permeability of the sand. The chemical can be used in wells with bottom-hole temperatures ranging from 105°F to more than 350°F A description of the equipment required and the techniques used for applying these plastics to the wells is included. Introduction Recovering oil and gas from unconsoli-dated sand formations offers one of the most troublesome of all production problems. These sands generally present no particular trouble while drilling is in progress, but after the well has been completed and a pressure differential has been established across the face of the producing zone, the formation begins to L'slough," resulting in "sanding up" of the well. The term "sanding up" means that sufficient volumes of sand have moved into the well bore or casing to cause a serious reduction or complete halt of all flow of oil, water or gas. In rare cases a well may produce only a small amount of sand and still continue to flow or pump, the sand being carried to the surface in the fluid stream. However, in such instances, the result may be a costly repair bill due to the effect of the sand on surface and pumping equipment. The difficulty of producing petroleum from sands that are loosely cemented has long been recognized by petroleum engineers but only within the last few years has any new approach to the problem been undertaken. This involves the use of plastics that are capable of bonding the individual sand grains in place without materially reducing the effective permeability of a formation. The successful application of plastics for the consolidation of poorly cemented sands is relatively recent but now it is widely used in many of the more difficult areas on the Gulf Coast of Texas and Louisiana. This relatively new use of plastics1 in the oil fields has been preceded by much laboratory and field research on the use of various chemicals2,3 for solving numerous well-completion and work-over problems. Plastics now are being used successfully to control gas-oil and water-oil ratios,4'6 in zone isolation, the repair of casing leaks, the elimination of caving in cable-tool drilling wells6'7 and in the setting of linerss and casing.9 Sand-consolidating plastics, however, are basically different from all others in that they must not form an impervious seal. Field Practices The approach to the sanding-up problem usually has been the mechanical obstruction of the movement of the sand grains.

Jan 1, 1947