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By John W. Cahn, John E. Hilliard

Single crystals of copper and silicon-iron were cold rolled in orientations chosen to produce individually the major components of the poly crystalline deformation texture. The orientation dependence of the recrystallization kinetics was studied relative to the primary recrystallization textures of these specimens. It is not possible to rationalize the poly crystalline re crystallized textures on this basis. The results suggest an important role of the interaction of adjacent crystals during the deformation of aggregates. BRICK and Williamson1 first noted evidence that the recrystallization temperature was different for straight-rolled and cross-rolled copper given comparable reductions. Michalak and Hibbard2 investigated quantitatively the effect of rolling procedure on the kinetics of recrystallization of cold-rolled copper and found that material cold-rolled the same amount by straight-pass, cross-pass, and compression-pass techniques developed different deformation and recrystallization textures, different 1-hr recrystallization temperatures, and different recrystallization kinetics. However, the temperature dependence of the rate of recrystallization was essentially the same for all techniques. Similar results were obtained on iron. Dunn and Koh3 in studying the recrystallization textures of cold-rolled silicon-iron single crystals reported large differences in the annealing temperatures and times required to recrystallize specimens of different orientations cold-rolled the same amount. Liu4 and Liu and Hibbard5 utilized the concept of different recrystallization temperatures for different orientations of cold-rolled crystals to rationalize the difference in recrystallization textures found in various face-centered-cubic metals. Their explanation predicted a significant difference in the recrystallization kinetics of deformed (110) [112] crystals as compared to (358) [352] crystals, and, in fact, Liu4 reported evidence that this difference existed at least qualitatively. Verbraak6 who rolled and recrystallized a series of copper single crystals found that the double (112) [111] rolled orientation is related to recrystallized cube texture formation. The effect of rolling intensity on the relative amount of cube component suggests an important role of recrystallization kinetics. Walter and Hibbard7 while trying to relate the behavior of rolled and recrystallized single crystals of silicon-iron to the behavior of polycrystal-line silicon-iron again noted that differences in recrystallization kinetics were necessary to rationalize their results. The purpose of the present investigation was to obtain quantitative kinetic data on the recrystallization of single crystals of both copper and silicon-iron rolled to initial isolated individual orientations corresponding to those found in the polycrystalline deformation textures. These data might indicate the importance of the deformation orientation, i.e. the range of available nuclei, the deformed matrix orientation into which these nuclei grow, and the orientation dependence of their growth rate during primary recrystallization on this texture. I. COPPER Experimental Procedure—A single crystal of 99.98 pet purity copper, grown by the Bridgman technique, was purchased in the form of a bar 1 1/2

Jan 1, 1962

By Scott Turner

AS IN OTHER lines of engineering, progress in mining was influenced during 1931 by the world-wide economic depression. Low-metal prices ? resulted in active efforts to reduce production costs of base-metal mines. Probably the chief factors in reducing costs were the greater efficiency of labor, due to better relations between management and workmen, to the scarcity of jobs, reduced wages in most base-metal mines, and to lower overhead expenses secured by drastic economies. The use of mechanical equipment continued to increase, due to more efficient designs and a better practical understanding of the applicability of such equipment to requirements. With one exception, there were no startling innovations in stoping methods, but there was notable progress in the better adaptation of mining methods. In the United States, no large new base-metal or silver mines came into production during the year. At a number of mines, output was curtailed, and operations were discontinued at several important producers. On the other hand world-wide interest in gold was stimulated, as evidenced by increased output from producing mines, the reopening of some old properties, and intensive prospecting for new deposits. Mining methods at several gold mines in the United States and Canada were modified or changed to obtain a higher extraction of ore or to meet the need for additional support of the mine workings at depth. Permanent record of improvements in mining practices has been made during the year by the Federal Government; the industry thus has available for its use more detailed information than ever before. This work was done through cooperation of the mining companies and their representatives with the United States Bureau of Mines, whereby many papers descriptive of practices and costs at individual mines have been published. The Bureau's program of describing methods and costs at the more important mines (those producing in excess of $100,000 annually) is nearly completed, but papers will be issued concerning such additional mines as may possess particular interest because of novel methods, exceptional conditions or operating results, and others to supplement reports already issued. In this way, an interesting record of the results of changing conditions, or innovations in methods, will be made available.

Jan 1, 1932

By Karl V. Lindell

THE Jeffrey mine of the Canadian Johns-Manville Co., Asbestos, Que. has operated for a number of years, supplying the parent company, Johns-Manville, raw material for asbestos products. The mine is situated in the 70-mile-long serpentine belt running from Asbestos, Que. on the west to East Broughton on the east. This district is the most important producing area in the world of quality spinning-fiber asbestos, with 11 operating mines supplying 70 pct of the world's needs. The Jeffrey mine, located 90 miles from Montreal and approximately 35 miles southwest of Thetford, accounts for 50 pct of the Canadian asbestos output. Production from the Canadian serpentine belt is the chrysotile asbestos, which is considered the best available for spinning. Consumers in the United States prefer the clean, fine fibers of the Canadian chrysotile of the type produced by the Jeffrey mine. Mining In 1881, when the mine was first opened, all work, including drilling, was done by hand. The deposit, located on a hillside, was first worked as a sidehill cut by hand drilling 15-ft holes and blasting with black powder. The fiber was chiselled from the broken rock. Hand derricks, later powered by horses, were used to raise the rock as the pit deepened. Eventually, the pit became so deep that derricks were, by necessity, replaced by aerial tramways. In the late 1930's, further deepening of the open pit, with the resulting constriction of the pit bottom brought about the need for altering the mining system then in use. The high ratio of overburden to be handled to mill ore mined and the value of surface structures, not company property, that would be destroyed in expanding the area of the pit, definitely indicated vertical rather than horizontal expansion would have to be used. One exception to this was that a small area on company property to north and east of the pit could be opened up. The mining problem then resolved itself into two phases; make the small lateral expansion and as rapidly as possible choose a mining method that would expand the mine vertically. Several methods for vertical expansion were studied and rejected. Methods considered included shrinkage stoping, block caving, glory holing, and various modifications of open workings. Block caving was finally accepted as the most suitable method of underground development. Cost factors and production were important factors in the decision, also, the asbestos mines in the Thetford area were already having success with this method. Original plans provided for the lateral expansion of the open mine where possible and beginning the underground operation. This program was based on the open pit being worked out in 1954, with the underground development and production gradually increasing until the open mine was depleted. In 1949, the plan was changed to allow underground development to progress at maximum so that underground output would be 550 tons per hr by 1951. Any deficit in ore would be mined from the open pit. This change permitted extending the life of the open pit through 1964 and in this time would make available a large quantity of readily attained ore. Block Caving at The Jeffrey Mine Plans for the underground operation were formulated on a 12,000-ton-per-day basis, and the adaptability of block caving methods to high production presented a desirable situation. As shown in the main-haulage plan, a continuous loop was laid out for smooth operation of the underground railroad from the loading points to the underground crusher. A feature encountered at the Jeffrey mine, as well as other asbestos mines using caving methods, is the large size of caved material, requiring that ore be crushed before hoisting.

Jan 1, 1952

By C. H. Herty Jr, C. H.

FEW subjects have attracted the attention of metallurgists more than oxygen in steel. From the days of Mushet and Ledebui interest in this subject has been increasing, and as additional knowledge has become available, the problem has naturally grown more complex. Instead of using the simple term "oxygen" we now distinguish between iron oxide, silicates of various kinds, oxysulfides, oxygen as gas and oxygen in solid solution in steel. There are five general methods for determining oxides in steel: hydrogen reduction; vacuum fusion; various wet-extraction methods, including electrolytic methods; methods depending on volatilization of the iron away from the oxides; and metallographic methods. For oxygen in solid steel each of these methods has both advantages and disadvantages. The hydrogen-reduction method is of no use on steels above about 0.20 per cent. carbon; 1 furthermore, it gives only FeO and possibly some MnO. The vacuum-fusion method2 is expensive and gives total oxygen, with the exception of some A1203, and does not differentiate between the various oxides in which the oxygen exists. Most of the wet-extraction methods3 give only the more insoluble oxides SiO2 and A1203, though the iodine method gives MnO to an uncertain degree (information that may be more misleading then no information

Jan 1, 1957

By A. Gatti, R. L. Fullman

A very fine dispersion of aluminum oxide is produced by internal oxidation of solid-solution alloy of 0.14 pet A1 in Ag. The particle size of the aluminum oxide is approximntely 50 to 100A in radius. The yield strength of the alloy is increased markedly by internal oxidation. A further increase in strength is produced by cold working the internally oxidized alloy. Recrystallization is retarded by the finely dispessed aluminum oxide particles, so that the strength increase resulting from cold work is retained on annealing at temperatures 14 to about 700°C. MANY workers'-3 in the past have studied various aspects of the internal oxidation of aluminum-silver alloys. This paper is an extension of these studies with emphasis placed on the effect of time and temperature of annealing on the strength of these alloys after oxidation and subsequent cold working. Two general conditions are necessary to internally oxidize an alloy. First, oxygen must diffuse through the base material more rapidly than does the addition; otherwise oxidation will take place as a surface layer. Secondly, the affinity of oxygen for the addition must be greater than for the base material. After internal oxidation of certain alloys takes place, a marked increase in hardness accompanied by higher yield stress and improved creep properties is noted, presumably as a result of the highly dispersed oxide within the base material. Meijering and Druyvesteyn1 also noted that the internally oxidized portion of a partly oxidized alloy failed to recrys-tallize under annealing conditions that led to coinplete recrystallization of the unoxidized part. EXPERIMENTAL-METHODS AND PROCEDURES Few alloys can be made to contain a second phase that is extremely stable at high temperatures. Silver plus aluminum in solid solution was chosen for these internal oxidation studies because of the high rate of oxygen diffusion through silver and the very stable nature of aluminum oxide. Two alloys were vacuum cast. The nominal compositions were: Alloy A—1 pct Al, balance Ag; Alloy B—0.1 pct Al, balance Ag. Chemical analysis, which does not distinguish between aluminum and aluminum oxide, showed the conlposition to be: Alloy A—1.6 pct Al, and Alloy B—0.14 pct Al. The ingots were machined for surface cleaning, swaged and drawn to 0.020-in. diam wire. A sample 20 ft long of the 0.020-in. dianl wire of each composition was annealed 24 hr at 800°C in pure dry hydrogen. Each wire was then cut into two equal pieces. Photomicrographs of the 0.14 pct A1 alloy are shown in Fig. 1, the annealed 0.020-in. wire at the left and the oxidized wire to the right. The oxidation treatment for the first set of data was 1000 hr at 800°C in air. After this treatment the 1 pct A1 proved to be brittle. It is assumed that high alunlinum oxide concentration at the grain boundaries was responsible. The 0.14 pct Al wire remained ductile and all further data were derived using this alloy. One-half of this wire, about 5 ft, plus 5 ft of as-homogenized wire, was then drawn cold to 0.005 in. diam. All tensile tests were conducted with an Instron Engineering Corp. tensile-testing machine, Model TT-B. Unless otherwise indicated, the tests were made at room temperature with a strain rate of 0.1 per min. All metallographic samples were etched with an aqueous solution of 2 pct each of CrO3 and H2SO4 . EXPERIMENTAL RESULTS AND DISCUSSION PARTICLE SIZE DETERMINATION A study was made of the particle size of the aluminum oxide produced in the samples of Ag + 0.14 pct Al, oxidized 1000 hr at 800°C. A cross section of the as-oxidized wire was mounted in bakelite, polished, and etched with an aqueous solution of 2 pct each of CrO3 and H2SO4. The specimen was then thoroughly cleaned by stripping successive coatings made by applying 10 pct nitrocellulose in amyl acetate. The final replica of the cross section was made by applying 2 pct nitrocellulose in amyl acetate. The replica was stripped, transferred to a copper screen, shadow cast with chromium at 10 deg and photographs taken using a Phillips Metallix electron microscope at an accelerating potential of 100 kv. A photograph of an etched sample of the as-oxidized material is shown in Fig. 2. We believe the pits in the photograph are places were A12O3 inclusions were sitting in the matrix. By inspection, it appears that the volume fraction ob-

Jan 1, 1960

By J. F. Enrietto

Internal friction measurements were used to determine the effect of manganese on the solubility and precipitation kinetics of nitrogen. Manganese, in concentrations up to 0.75 pct, has little effect on the solubility at temperatures above 250°C. On the other hand, at Concentrations as low as 0.15 pct, manganese inhibits the formation of iron nitrides, especially Fe4N, even though it may not form a precipitnte itself. The precipitation and solubility of carbides and nitrides have been extensively investigated in the pure Fe-C and Fe-N systems.1-3 In recent years, some effort has been ispent in studying the influence of substitutional alloying elements on the behavior of carbon and nitrogen in ferrite.4 -7 In particular Fast, Dijkstra, and Sladek have investigated the effect of 0.5 pct Mn on the internal friction and hardness during the quench aging of Fe-Mn-N alloys.', ' They found that at low temperatures (below 200°C) the presence of 0.5 pct Mn greatly retarded quench aging. For example, after 66 hr at 200°C very little precipitation had taken place in the iron alloyed with manganese, whereas precipitation was complete after a few minutes in a pure Fe-N alloy. The effect of varying the manganese content and the details of the precipitation process were not mentioned in these papers. Fast' postulated that manganese causes a local lowering of the free energy of the lattice with a resulting segregation of nitrogen atoms to these low energy sites. The segregated nitrogen atoms are bound so tightly to the manganese atoms that they cannot form a precipitate. The internal friction measurements of Dijkstra and Sladek tended to confirm the concept of segregation of nitrogen around manganese atoms, and the increase in free energy on transferring a mole of nitrogen atoms from a segregated to a "normal" lattice site was computed to be - 2800 cal. Dijkstra and Sladek9 distinguished between two types of precipitates: ortho, a nitride of appreciably different manganese content than that of the matrix, and para, a nitride with a manganese content essentially that of the matrix. With each type of precipitate a solubility, again designated ortho or para, can be associated. Since the internal friction maximum in alloys which were aged several hours at 600" C dropped almost to zero, Dijkstra and Sladek9 concluded that the ortho solubility must be very low. The effect of temperature on the ortho and para solubilities has no1: been investigated. There are obviously several gaps in our knowledge concerning the influence of manganese on the behavior of nitrogen in a-iron. It was the purpose of the experiments described in this paper to determine the following: 1) The ortho and para solubilities of nitrogen as a function of temperature. 2) The details of the precipitation process at elevated temperatures. 3) The effect of varying the manganese concentration on the above phenomena. EXPERIMENTAL PROCEDURE Internal friction is conveniently employed in studying the precipitation of nitrides and/or carbides from a -iron because it is one of the few parameters, perhaps the only one, which is not affected by the presence of the precipitate itself. For this reason, internal friction techniques were heavily relied upon in the present experiment. A) Preparat of -. All specimens were prepared from electrolytic iron and electrolytic manganese. Alloys containing 0.15, 0.33, 0.65, and 0.75 wt pct Mn were vacuum melted and cast into 25 lb ingots. After being hot rolled to 3/4 in. bars, the ingots were swaged and drawn to 0.030 in. wires. The wires wen? decarburized and denitrided by annealing at 750° C for 17 hr in flowing hydrogen saturated with warer vapor. To obtain a medium grain size, - 0.1 mm, the wires were then heated to 945oC, allowed to soak for 1 hr, furnace cooled to 750°C, and water quenched. Subsequent internal friction measurements showed that this procedure reduced the nitrogen and carbon concentrations of the alloys to less than 0.001 wt pct. The wires were nitrided by sealing them in pyrex capsules containing anhydrous ammonia and annealing them for 24 hr at 580°C, the nitrogen being retained in solid solution by quenching the capsule into water. Immediately after quenching, the wires were stored in liquid nitrogen to prevent any precipitation of nitrides. By varying the pressure of ammonia in the capsule, it was possible to produce any desired nitrogen concentration. B) Internal Friction. The internal Friction measurements were made on a torsional pendulum of the Ke type,'' a frequency OF 1. or 2 cps being used. For

Jan 1, 1962

By D. W. Lillie

It has been demonstrated that considerable bend ductility exists in bulk specimens of polycrystalline high-purity silicon. The possibility of hot-forming at 1200°C is suggested. EXCELLENT corrosion resistance in many media and low cross section for absorption of thermal neutrons (0.13 barn) would make silicon of interest to nuclear engineers were it not for extreme brittle-ness and the difficulty of fabrication by any reasonable means. The use of silicon for structural purposes also has been considered in view of its light weight and oxidation resistance. Johnson and Han-sen' have investigated the properties of silicon-base alloys and concluded that there was no way of making pure silicon or silicon-rich alloys ductile at room temperature. In view of reports of appreciable ductility in germanium single crystals above 550°C'." and some plastic deformation in single-crystal silicon above 900oC,' the present investigation was undertaken to define more precisely the limits of high-temperature ductility in pure silicon. After this investigation was begun torsion ductility in both germanium and silicon was reported by Greiner." Through the courtesy of F. H. Horn, a small bar of cast extra high-purity silicon was obtained and small bend specimens were made from it by careful machining and grinding. All of the reported tests results were obtained from samples from this bar (bar No. 1) and one other of similar source (bar No. 2). No complete analysis was obtained but, based on analysis of similar semi-conductor grade material, metallic impurities were under 0.01 pct total. Vacuum-fusion analysis for oxygen showed a value of 0.0018 2 0.0003 pct for the first bar tested and metallographic analysis showed no evidence of a second phase. Bend tests were carried out on an Instron tensile machine using a bend fixture with a 1 -in. span loaded at the center. Supporting and loading bars were 0.250 in. round and the load was applied by downward motion of the pulling crosshead of the machine. Specimen thickness and width were approximately 0.10 in. and % in. respectively. Loading rate was controlled by holding crosshead motion constant at 0.02 ipm. In some cases a smaller specimen was used on a 5/8-in. span with a 0.129-in.-diam loading bar. The entire bend fixture was surrounded by a hinged furnace and all heating was done in air atmosphere. Temperature measurement was made with thermocouples fastened directly to the bend fixture within less than 1 in. from the specimen. Autographic stress-strain curves were recorded during each test, and breaking load, total deflection, and plastic strain could be obtained from these curves. Stress was calculated from the beam formula S = 3PL/2bh2, where P is the load in pounds, L the span in inches, b the specimen width in inches, and h the specimen thickness in inches. This formula is strictly correct only in the elastic range but has been used to calculate a nominal stress for convenience in the plastic range. The stress given is the maximum stress in the specimen. Results The results of the complete series of tests are shown in Table I. The first group of tests (specimens Nos. 1-6) showed the beginning of plastic flow at a test temperature of 900°C, so two additional tests (Nos. 8 and 9) were made at 950°C on small-size specimens from bar No. 2. Specimen No. 8 was tested in the as-machined condition, and No. 9 was heat-treated in hydrogen at 1300°C for 2 hr, cooled to 1200°C and held 1 hr, cooled to 1000°C and held 1 hr, cooled to 900°C and held 1 hr, and finally cooled to a low temperature before removal from the hydrogen. It is apparent that the heat-treatment had a significant effect on yield strength and ductility. In addition, the magnitude of the yield point was conslderably reduced in the heat-treated specimen as is shown m Fig. 1 by tracings of the stress-strain curves. After obtaining a furnace capable of reaching higher temperatures specimens Nos. 10 to 13 were tested at 1100 and 1200°C. Strain rate was increased by up to a factor of 10 to see whether the ductility observed was excessively strain sensitive. Specimen NO. 10, strained at 0.02 ipm and 1100oC, was still bending at a deflection of 0.322 in. when the load rate was increased to 0.2 ipm, resulting in immediate

Jan 1, 1959

By S. G. Cupschalk, J. J. Wert, R. A. Buchanan

The uniaxial deformation of thermally ordered and disordered polycrystalline Cu3Pt was studied by means of the X-ray line - broadening analysis according to Warren and Averbach and the extension of this analysis to ordered fcc materials by Mikkola and Cohen. Because of the heat treatment history, extinction had a pronounced effect on the X-ray spectra of ordered and disordered C%Pt at small plastic strains. After an appropriate correction for extinction, the long-range order in thermally ordered ChPt was found to decrease at a slow constant rate with plastic strain. Furthermore, the antiphase domain probability increased at a constant rate to 17.5 pct strain. The effective particle size behavior indicated that the stacking fault energy is lower in ordered than in disordered Cu3Pt. Analysis of the stress-strain curves shouled that ordered Cuzt has a slightly lower yield Point but a much higher work-hardening rate than disordered Cu3Pt. THE presence of long-range order in a solid-solution alloy has a marked effect on its mechanical properties. While this effect has been known qualitatively for many years, it was not until recently that detailed investigations have been performed to determine the exact role long-range order plays in this strengthening mechanism. The development of an advanced, quantitative. X-ray diffraction analysis by Warren and Averbachl and the extension of this analysis to the L1, type super lattice by Mikkola and cohen2 have greatly accelerated research in this field. The research reported in this paper consisted of two primary phases. The first phase was to determine the effect of long-range order on the tensile properties of polycrystalline Cu3Pt. This objective was accomplished by comparing the stress-strain behavior of thermally ordered CusPt to that of thermally disordered CusPt. The second phase of the research was to determine the difference between the atomic arrangements in thermally ordered and thermally disordered Cu3Pt as a function of uniaxial deformation and thereby gain a deeper insight into the mechanism by which long-range order affects the tensile properties. This second objective was accomplished by applying the Warren-Averbach method of peak profile analysis to the X-ray diffraction patterns obtained from ordered and disordered Cu3Pt after given amounts of uniaxial deformation. EXPERIMENTAL PROCEDURE The Cu3Pt was prepared by vacuum melting and casting. After a homogenization anneal, the ingot was cold-rolled to sheet form. Two tensile specimens with gage sections of 2.50 by 0.500 by 0.115 in. were carefully machined from the sheet. The specimens were polished with a final step of 600-grit paper to insure smooth diffracting surfaces. Finally, one specimen was heat-treated to yield an average grain diameter of 0.016 mm and an initial degree of long-range order, S, of 0.825. The other specimen was water-quenched from above the critical temperature, 645"C, to yield an average grain diameter of 0.017 mm and zero long-range order. The heat treatment history of each specimen is shown in Table I. The tensile tests were performed utilizing a Research Incorporated Model 900.95 Materials Testing System. This unit employs a closed-loop feedback system which maintains a constant strain rate through an extensometer clipped to the gage section of the tensile specimen. A strain rate of 1.32 i0.02 x 10"4 sec-' was employed in testing both specimens. In the X-ray diffraction analysis, a General Electric XRD-5 diffractometer equipped with a pulse-height analyzer set for 90 pct efficiency was employed. The goniometer speed selected was 0.2 deg, 20, per min. Filtered Cu radiation was used for all peaks and all peaks were chart-recorded. Because of nonuni-form grain size. it was necessary to spin the specimens during X-ray analysis in order to obtain reproducible integrated intensities. The spinning rate was 2000 i100 rpm. The application of the Warren-Averbach method of peak broadening analysis to a diffraction pattern is very time consuming if done manually. In this research, the calculations involved were performed with the aid of a computer program by wagner.3 As reported by Wagner, the program is written in Fortran TV computer language. It was modified to Fortran I1 so as to be handled by the IBM 7072 computer at Van-derbilt University. In the X-ray diffraction analysis of uniaxially deformed Cu3Pt, the 100, 200. 400. 111, and 222 reflections were recorded from the initially ordered sample after 'plastic strains of 3.0, 6.0, 9.0, 12.0,

Jan 1, 1970

By A. J. Heckler, J. A. Peterson

A capsule technique was successfully employed to investigate the effect of nickel on the activity of nitrogen in Fe-Ni-N austenite in the temperature range 600" to 1200°C. This technique consisted of equilibrating nitrogen among various Fe-Ni alloys within a sealed silica capsule. Nitrogen transfer among the specimens occurred by N, gas at 900°, lOOO? and 1200?C. Nitrogen gas pressures within the capsules were estimated to be as high as 22 atm. The activity coefficient of nitrogen, fN , in Fe-Ni-N austenite is adequately described by the linear interaction equation: log . wt pct Ni where the standard state is chosen such that fN = I as wt pct Napproaches zero in binary Fe-N. This relationship was determined over the temperature range 873" to 1473°K and for nickel contents of 0 to 35 wt pct. ALTHOUGH chemical thermodynamics of liquid iron alloys have been extensively studied, experimental data for the solid state are needed. These thermody-namic data will provide a basis for understanding phase transformations, precipitation reactions, metal-gas equilibria, and so forth. The interaction of sub-stitutional alloying elements with the interstitial elements is of particular interest. In this investigation the thermodynamic behavior of Fe-Ni-N austenite has been studied. The solubility of nitrogen gas in iron austenite is known to obey Sieverts&apos; law up to about 65 atm.1-6 In addition, the solubility of nitrogen in Fe-Ni austenite has been investigated5"8 using the classical method of equilibrating Fe-Ni alloys with nitrogen gas at 1 atm. A capsule technique similar to that used to study the activity of carbon in alloyed austeniteg&apos;&apos;&apos; was employed in the present work to determine the effect of nickel on the activity of nitrogen in Fe-Ni austenite over the temperature range 600" to 1200°C. EXPERIMENTAL PROCEDURE A series of Fe-Ni alloys up to 35 wt pct Ni was vacuum melted and cast into 1 by 3 by 6 in. ingots. Chemical analyses at the top and bottom of each ingot demonstrated that the ingots were homogeneous with respect to nickel content. The nickel contents are given in Table I. Additional chemical analyses showed that wt pct Si < 0.05, s < 0.01, C < 0.01, Al < 0.006, 0 < 0.004, Mn < 0.002, and P < 0.002. A 2 in. section of each ingot was cold rolled to 0.015 in. The material was then decarburized to a carbon content of less than 0.004 wt pct. A portion of the material of each nickel content was nitrided to various levels in a H2-NH3 gas atmosphere to provide a source of nitrogen during subsequent equilibration. The experimental technique consisted of equilibrating the series of Fe-Ni-N alloys in a partially evacuated sealed silica capsule at the temperature of interest. Both Vycor and quartz capsules were used. In general, the final equilibrium nitrogen content for each Fe-Ni alloy was approached from both higher and lower nitrogen levels. The criterion for establishing that equilibrium was attained was that the final nitrogen content for each Fe-Ni alloy was the same irrespective of the initial level. A schematic drawing of the sample configuration in a capsule is shown in Fig. 1. The samples were arranged so that there was a minimum of physical contact. The samples were also dusted with a fine, high purity alumina powder to help prevent sticking. Several different types of furnaces were used in this study. In each case, a thermocouple was placed immediately adjacent to the capsule during equilibration and the temperature was controlled to within *4?C of that reported. At each equilibration temperature, the following times were found to be more than sufficient to attain equilibrium: 600°C-250 hr, 900°C-150 hr, 1000°C-150 hr, and 1200°C-50 hr. After equilibration the capsules were quenched in water and the nitrogen contents of the specimens determined by a Strohlein analyzer. Analyses of samples after equilibration at 1000" and 1200°C showed no silicon pickup from the silica capsules. RESULTS AND DISCUSSION Transfer Mechanism. The mechanism by which nitrogen was transferred among specimens in an initially hydrogen flushed and partially evacuated capsule equilibrated at 1000°C was investigated. After equilibration the gas in the capsule was collected over water and an estimate of the pressure at temperature

Jan 1, 1970

By A. U. Seybolt

The solubility limit of oxygen in columbium has been determined in the range between 775&apos; and 1100°C by means of lattice parameter measurements and microscopic examination. The solubility is a function of temperature and varies, in the range given above, from 0.25 to 1.0 pct O, respectively. BECAUSE of the marked deleterious effect of oxygen upon the mechanical properties of some of the transition metals, it is desirable to know something about the solubility of oxygen in these metals. The brittleness caused by oxygen in solution is particularly marked in the case of the group VA elements, vanadium, columbium, and tantalum. The solubility of oxygen in vanadium has already been reported in an earlier paper,&apos; and Wasilewski2 has given a value (0.9 wt pct) for the solid solubility of oxygen in tantalum at 1050°C. Brauer3 in 1941 investigated the Cb-0 system up to Cb2O5, but made no real effort to investigate the extent of oxygen solubility in the metal. He made the observation, however, that this solubility must be less than 4.76 atom pct (0.86 wt pct) oxygen. This estimate was made from X-ray diffraction results on the alloys CbO, CbO, and CbO; all alloys consisted of the terminal (Cb) solid solution plus CbO, but the last alloy containing 4.76 atom pct 0 showed only three very weak CbO lines. It is surprising that Brauer, by examining only three alloys, arrived at an estimate of the solubility which agrees very well with the results to be reported herein. Experimental Procedure A columbium strip obtained from Fansteel Metallurgical Products was cut into strips, 0.020x1/2x2 in. Two holes, about 3/16 in. in diameter, were made near the ends of the strips in order to hold them against a flat steel block for mounting in a General Electric X-ray spectrometer for lattice parameter measurements. The same holes were used to hang the specimens inside a fused silica vacuum furnace tube which was part of a Sieverts&apos; gas absorption apparatus. The apparatus and method of adding oxygen gas has been previously described.1 According to the supplier, the columbium obtained had the analysis given in Table I. After degreasing the samples, approximately 0.001 in. was etched from each side of the samples in order to remove possible surface impurities from the last rolling operation. For this purpose the following cold acid pickle was found satisfactory: 8 parts HNO3, 2 parts H2O2 and 1 part HF. Various Cb-O compositions were obtained up to 0.75 wt pct O by the gas absorption and diffusion technique. After the sample had absorbed all the oxygen gas added at 1000°C, an additional 24 hr was allowed for homogenization. This treatment appeared to be adequate, as shown by the linearity of the lattice parameter-composition plot. More concentrated alloys were prepared by arc melting mixtures of Cb and Cb2O5 since it was very time-consuming to make Cb-0 alloys in the neighborhood of 1 pct O, or over, by the diffusion method. When the flat strip specimens were used, they were ready for the X-ray spectrometer after cooling from the Sieverts&apos; apparatus. The cooling rate obtained by merely allowing the hot fused silica furnace tube to radiate to the atmosphere (when the furnace was lowered) was sufficiently fast to keep the dissolved oxygen in solution. Arc-melted alloys were reduced to —200 mesh powder in a diamond mortar, wrapped in tantalum foil, sealed off in evacuated fused silica tubes, and then heat treated as indicated in Table 11. The fused silica tubes were quickly immersed in cold water without breaking the tubes after the heat treatments. The tantalum foil prevented reaction between the fused silica and the sample; there was no reaction between the powdered samples and the foil at 1000°C, but some trouble was experienced at 1100°C. At this temperature level a reaction between the sample and the foil was sometimes observed, which resulted in erroneous parameter values. Experimental Results Hardness Tests: Since most of the X-ray samples were in the form of flat strip, it was convenient to obtain Vickers hardness numbers as a function of oxygen content. Compared to the V-O case,&apos; oxygen hardens columbium much more slowly, presumably because of the larger octahedral volume in colum-bium (about 12.0 compared to 9.3Å3 in vanadium), hence, requiring less lattice strain for solution. The plot of VHN vs wt pct O is shown in Fig. 1.

Jan 1, 1955

By Hans Lundberg

GEOPHYSICAL methods as described in technical articles generally fail to answer the questions of prospectors and geologists as to which method they should apply and what information they may expect from their application. This article is an attempt to discuss the use of electrical methods with special reference to the prospecting for orebodies and the map¬ping of geologic structure. Especially on virgin ground, geological reconnaissance should precede electrical prospecting, with the object of outlining carefully the orebearing rock and determining the possibilities of elec¬trical prospecting. No electrical survey will then be carried out on ground which, for geological reasons, may be considered barren or where the electrical meth¬ods are inapplicable. As the success of electrical prospecting depends on the difference in conductivity between the ore and the country rock within which the orebody is inclosed, the conductivity of the two should be considered and de¬termined, if possible. The conductivity of an orebody depends on the distribution of conductive ore minerals and, in addition, on its size (length, width and depth). Most minerals with metallic luster show good electrical conductivity; for instance, the sulfides. Zinc-blende is an exception, but as it is often associated with the ore minerals of good conductivity (for instance, pyrite or galena), there is likelihood also of finding zinc.

Jan 1, 1930

By E. N. Harshman

The Wind River Formation of Eocene age is the host rock for large high-grade uranium deposits in the Shirley Basin. The major deposits are in a northwest-trending belt of sandstones that were deposited in stream channels and that were lithologically favorable for uranium accumulation. Paleotopography influenced the character and position of the belt. The major deposits within the belt are at, or near, the margins of large tongues of altered sandstone formed in the most transmissive parts of thick sandstone beds. At least two tongues of altered sandstone are present in the belt, one of which is 5 miles long, 3 miles wide, and 70 feet thick; the other tongue is somewhat smaller. Ore bodies consist of a few hundred tons to several hundred thousand tons of material containing from 0.10 to about 2.00 per cent U3O8. The ore mineral is uraninite associated with pyrite, marcasite, hematite, and calcite. Deposition is believed to have taken place when neutral to slightly alkaline, oxidizing, uranium-bearing ground water, on entering the basin, encountered a reducing environment. The reductant may have been H2S of biogenic origin. Geology played an important role in discovery, exploration, and development of ore in the Shirley Basin.

Jan 1, 1968

By B. D. Thomas

When the origin and early plans, of Battelle Memorial Institute were described in this journal in October 1929 by R. W. Gillett the first director, the doors of the laboratory had just been opened and the hope of the founder that the institution serve the world by research for industry still existed only as an ideal in the minds of the thirty or so employees who then constituted the staff. Since that time the country has experienced troublous times. A devastating depression plunged the entire world into an unprecedented period of financial and industrial inactivity; and the slow recovery of the late thirties was soon to be overtaken and overwhelmed in the violence of war. Through this time of stress Battelle has continued to grow. The staff has increased to almost 600; buildings and equipment have been added, until now it stands in a place of pre-eminence in the metallurgical and engineering world.

Jan 1, 1944

By Donald L. Ball

The equilibrium of boron nitride, gaseous nitrogen, and solute boron was investigated in Fe, Fe-C, and Fe-Si rnelts by the Sieverts technique. The free ellergy of dissociation of boron nitride, involving -the implied standard states, was evaluated in the range 1400" to 1600°C as: ?Fo = 38,000 - 23.5T, cal ber mole The solute-solute interaction coefficients eBB, ecB , and eg were determined as 0.058, 0.22, and 0.078, respectively. BORON is an important ingredient in some types of steel and cast iron. It was employed at a particularly high level, 0.01 wt pet, in the as-cast malleable iron "CentraSteel".1 In this material, the boron concentration was critical in order to assure graphite, and avoid primary cementite, in the as-cast structure. One possible function of the boron in this alloy was the nucleation of graphite through the agency of boron nitride, which, conceivably, precipitated from the melt during cooling. A research program was instituted to assess the validity of this proposed mechanism. The first undertaking, reported here, was a determination of the thermodynamic possibility of boron nitride precipitation. Data available in the literature on the activity coefficient of solute boron in iron-base melts are inadequate for the present purpose. They will be reviewed briefly, however, so that comparison can be made, when

Jan 1, 1968

By W. L. Zeigler

The mill is a departure from gravity concentration and has gained a reputation for the low initial cost of erection, extreme simplicity and the low cost of milling on the refractory character of the ore which is treated. The structure is of heavy timbers with board walls and corrugated roofing. The floors are concrete and the general layout is of the ground floor only. All the machines are driven by individual motors and the transmission usually found in such a plant is entirely absent. (Fig. 2.) ORE The ore from the Galena mine is sheared Wallace quartzite replaced with quartz, siderite, pyrite, sphalerite, gray copper (tetrahedrite) and very fine-grained argentiferous galena. Much of the silver is undoubtedly associated with the gray copper, the amount, however, apparently varies with different localities in the vein. An average assay of the ore is 6.0 per cent. lead, 1.3 per cent. zinc, 0.3 per cent. copper, 17.5 per cent. iron and 4.5 oz. silver. The concentrates produced are of an average 53 per cent. lead, 40 oz. silver, 8 per cent. zinc and 11 per cent. iron, while the tailings are 0.5 per cent. lead, 0.4 oz. silver. With the present market for zinc no attempt is made to produce a zinc concentrate.

Jan 1, 1927

By Eric Jette

The nickel-chromium alloys form the base f for many industrial heating alloys, so that this system is of considerable practical importance. The literature on these alloys, however, contains much conflicting evi-dence, not only regarding the solubility limits of the terminal solid solu-tions at different temperatures but even regarding, the number of phases existing in the system. Part of the difficulty undoubtedly arises from the fact that chromium of sufficiently high purity has been available only during the last few years. A second and possibly even more impor-tant difficulty arises from the ease with which chromium reacts with silicon and carbon compounds and the atmosphere to form silicides, carbides, nitrides and oxides. Pilling and kihlgren1 in 1929 reviewed the existing scanty information. They did not consider the diagram by which they summarized the various bits of information to be entirely satisfactory. Matsunaga2 investigated the system by thermal analysis, microscopic examination and other means. Electrolytic nickel of 99.9 per cent purity and thermit chromium containing 0.30 per cent al, 0.40 per cent fe, 0.25 per cent si and 0.04 per cent c were used. A tammann furnace with hydrogen flowing through it was used for melting. Sekito and matsunaga3 reported an x-ray, investigation presumably on these same

Jan 1, 1934

By O. E. KEOUGH

AT the Tooele custom lead-zinc ore concentrator,&apos; two sections, each having a daily capacity of 500 to 600 tons, are operated on slightly different types of ores with but little difference in flow sheet and reagents. The ores comprising the two general classes are the coarsely crystalline type, with low pyrite and sphalerite low in iron content, from the Park City district, and the more finely disseminated higher pyrite ores from Bingham, which are more difficult to treat by flotation. Laboratory testing determines with which general class a new ore will work better. The ores are crushed to minus 1 1/4-in. size at either the Utah Ore Sampling Company&apos;s plant at Murray, Utah, the Tooele smelter sampling plant, or the crushing plant at the concentrator. The ores for each section are mixed to maintain as nearly as possible uniform lead and zinc contents.

Jan 1, 1930

By T. W. Guy

The increased moisture due to water-spraying for coal dust control is of interest even for mines from which the coal is to be wet-washed before screening, because in many cases wet coal dust materially de- 20-mesh X 0 sizes as pct ROM average ............................... 6.3 pct Range 2.3 to 9.5 pct 20-mesh X 0 sizes as pct 3/8 X 0 sizes average........&apos;...................... 18.9 pct Range 12.7. to 23.9 pct creases the loading efficiency of men and equipment at the faces. It also causes a serious increase in the normal wear and deterioration of all equipment with which it comes in contact. It is important to the consumer if it increases his as-received moisture. No attempt will be made in this paper to cover the entire subject of water-spraying of coal for dust control. It will be confined to discussion and data on (I) percentages of dust in bituminous coals, (2) moisture increases due to spraying for dust control in mines or plants by methods which have proved satisfactory for periods of one to five or more years, and (3) a few suggestions for research. Size and Percentage or Coal Dust The U. S. Bureau of Mines1 classifies as coal dust all bituminous coal passing a 20-mesh sieve (0.0328 in. square opening). The percentage of such dust to be found in ROM coal, of course, varies widely with the characteristics of the seam, and with the methods used in the mining and in the preparation of the coal. ROM screen analyses of 12 U. S. coals selected at random from personal files given in Table I show: A few other screen analyses examined indicating 40 pct or more of 20-mesh X 0 dust in 3/8 in. X 0 sizes were not included because of uncertainty that they were representative. The number of results in Table I is not sufficient to give a reliable estimate of the average, or of the range to be expected, but it indicates that in every case the coal dust is a relatively large percentage of the total ROM coal, and, of course, a progressively larger percentage of resultants as the larger sizes are separated for marketing.

Jan 1, 1949

By H. A. Schwartz, A. F. Gorton, H. R. Payne

In a previous paper1 we published what we believed to be a correct stable equilibrium diagram for an iron-carbon alloy containing + 1.20 per cent. silicon. The purpose of the present paper is to record the results of studies concerning the effect of silicon on the location of the eutectoid points of both systems, including also certain incidental observations of general interest. We prepared white cast irons containing roughly 21/2 per cent. carbon, 0.05 per cent. manganese, and 0.03 per cent. each of phosphorus and sulfur, but of accurately known silicon contents which varied from 0.40 to 3.32 per cent. These were completely graphitized, and both A1 points determined, as in our previous work, the specimens being converted from the stable to the metastable condition and vice versa by appropriate heat treatments. Each stable alloy was heated to a few degrees above Arl for 3 to 7 hr., quenched and analyzed for total and graphitic carbon, the difference being the "combined" or, better, agraphitic2 carbon content of the saturated solid solution just above the eutectoid transformation. One specimen was lost through accident, and the 0.40-per cent. silicon material gave an anomalous result ascribed to difficulty in maintaining the stable system in the presence of but little silicon.

Jan 1, 1923

By H. R. Payne, A. F. Gorton, H. A. Schwartz

In a previous paper1 we published what we believed to be a correct stable equilibrium diagram for an iron-carbon alloy containing + 1.20 per cent. silicon. The purpose of the present paper is to record the results of studies concerning the effect of silicon on the location of the eutectoid points of both systems, including also certain incidental observations of general interest. We prepared white cast irons containing roughly 21/2 per cent. carbon, 0.05 per cent. manganese, and 0.03 per cent. each of phosphorus and sulfur, but of accurately known silicon contents which varied from 0.40 to 3.32 per cent. These were completely graphitized, and both A1 points determined, as in our previous work, the specimens being converted from the stable to the metastable condition and vice versa by appropriate heat treatments. Each stable alloy was heated to a few degrees above Arl for 3 to 7 hr., quenched and analyzed for total and graphitic carbon, the difference being the "combined" or, better, agraphitic2 carbon content of the saturated solid solution just above the eutectoid transformation. One specimen was lost through accident, and the 0.40-per cent. silicon material gave an anomalous result ascribed to difficulty in maintaining the stable system in the presence of but little silicon.

Jan 1, 1923