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By Attilio Ligasacchi

The production of magnetite in copper smelting has been the subject of wide investigation in the past.1-9 It is accepted that most of the magnetite is produced in the converters and returned to the re-verberatory furnace with the converter slag. Part of this magnetite is circulated back to the converters in the matte. As a result, if proper fluxing practice is not followed, and temperatures in the converting process are not strictly controlled, an undesirable circulating load of magnetite may occur. This might ultimately lead to saturation in the reverberatory bath with consequent settling of the magnetite at the furnace bottom. This paper contains the cumulative results of a series of investigations on the formation and control of magnetite presently being conducted by the metallurgical department of the Chino Mines Division of Kennecott Copper Corp. THE METHOD USED FOR THE DETERMINATION OF MAGNETITE AND OTHER MAGNETIC MATERIALS Conventional wet chemical magnetite analyses are neither reproducible nor theoretically sound. These analyses are sensitive to time, temperature, and heating rate-all factors which tend to decrease their accuracy and reproducibility. To overcome the unreliability of the above method, H. W. Mossman1 developed an inductance bridge magnetite "meter" which completely replaces the wet chemical analysis with the advantage of quicker and reproducible results. Fig. 1 is a schematic diagram of the meter in use in the Chino metallurgical laboratory. When a pulverized specimen with magnetic properties is placed in coil A of the inductance bridge circuit, the permeability of the core is increased, causing a voltage drop across the coil. The unbalance is amplified to operate the balancing motor which adjusts the movable iron core in coils C and D to bring the bridge back to balance. An indicator arm connected to the movable iron core indicates directly the percent, or weight, of the magnetic material in the specimen. Coil B acts as a reference coil and a zero adjustment. The meter is standardized with a set of various amounts of -100 mesh pure magnetite crystals (99.8 pet Fe3O4) thoroughly mixed in a test tube with -100 mesh quartz sand. These mixtures are combined with inert transoptic powder and heated to 140° to 160°C (melting point of the powder) and subsequently cooled to room temperature, solidifying the whole mixture, in this manner eliminating any possible preferential orientation of the magnetite grains. In order to determine the effect of the particle size" of the magnetite and other magnetic materials on the meter determinations, five size fractions were obtained by wet screening of the 99.8 pet pure magnetite and several reverberatory matte and slag samples. The following size fractions were investigated: -80 + 100; -100 + 150; -150 + 180; -200 + 250; -250 + 300 and -100 mesh. The deviation of the meter readings for the various sizes of each sample never exceeded ±0.3 pet. This deviation is considered well within the accuracy needed for common smelter operation procedures. Further investigation proved also that grinding slag and matte samples in our laboratory disc grinder normally produced a powder constituted of 95 pet -200 + 300 mesh. For practical purposes a - 100 mesh size was used as standard for our studies. It was also found that for rapid determinations tamping of the sample in the test tube was sufficient and gave comparable results with those samples solidified with transoptic powder. For the purpose of this study we define the magnetite content in copper smelter slags and matte as the equilibrium amount of crystalline Fe3O4 existent in the specimen at a given reference temperature, excluding any secondary magnetite precipitated in the specimen during nonequilibrium conditions. MAGNETITE DETERMINATION IN SLAGS Since it is impossible to ascertain the status of equilibrium of a conventional slag sample, due to

Jan 1, 1965

By H. M. Bannerman, E. N. Cameron

INTRODUCTION DURING the years 1942-1944, about 125 New England deposits were mined for sheet and punch mica, and many others were briefly prospected. During this period the Geological Survey, United States Department of the Interior, carried on detailed studies of the deposits and the pegmatite bodies that contain them. The primary purpose of the studies was to provide geological information that would contribute toward efficient mine development and operation. The studies were aimed directly at practical production problems. Detailed maps showing the structure of the deposits were prepared, and geological findings were closely correlated with data on specific yields and costs of mining and processing. The result is information that permits a reasonably accurate appraisal of the mica deposits of New England and the mining industry that they support. At a time when the future of the industry is in doubt, it seems desirable to submit this appraisal for consideration. Domestic mica deposits supply only a small fraction of the country's needs in normal times, for only the richest domestic deposits can compete with the low-cost mines of India and Brazil. However, the possibility that this country may be cut off from its supplies in time of war gives domestic deposits an importance much greater than their peacetime production would imply. New England supplied about 22 per cent of domestic output in 1943 and 1944, the peak years of wartime production. Its actual contribution to the war effort was greater, for the proportion of sheet mica of high quality in the New England product is higher than the average for domestic mica. The data analyzed below were collected for the Geological Survey by D. M. Larrabee, A. H. McNair, J. J. Page, V. E. Shainin, G. W. Stewart, and the co-authors of this paper. The cooperation of officials of Colonial Mica Corporation and of mine operators and owners in furnishing information is gratefully acknowledged. D. M. Larrabee, A. H. McNair, and V. E. Shainin have made various suggestions based on critical reading of the manuscript. ANALYSIS OF WARTIME OPERATIONS In considering the data presented in this report, it must be remembered that the scale of mica operations is very small compared with that of many other mining industries. The typical New England mica mine of 1943 and 1944 was worked by a crew of five or six men. Equipment was varied but on the whole extremely simple. The first stage of operation at a deposit was normally opencut mining. Drilling was done mostly with jackhammers powered by portable compressors driven by gasoline engines. Muck was shoveled by hand into buckets with a capacity of 1/3 to 2/3 ton and commonly hoisted by derrick to a dump adjacent to the cut. As operations were carried to greater depth, and the transition to underground mining was made, these methods were modified to a degree depending largely on the attitude of the deposit mined. At steeply dipping deposits,

Jan 1, 1946

By Arthur Hockman, Howard W. Jaffe, Howard F. Carl

THE problem of establishing practical techniques for evaluating natural corundum ores arose from the desire to improve the existing purchase specifications for crystal corundum procured by the Federal Government for stockpiling. Such purchase specifications had been developed for a large number of products, including minerals and ores considered to be critical and strategic because of the country's dependence on foreign sources of supply. It will be apparent to anyone considering the subject of purchase specifications that the determination of whether or not a submittal meets the specifications is a prime consideration. Consequently satisfactory specifications for minerals should not only incorporate physical, chemical, and mineralogical requirements that are practical but should also establish the means by which both buyer and seller can be assured that materials meet stated requirements. The Munition Board's Material Purchase Specification for corundum, dated February 1954, covered two grades of crystal corundum intended primarily for abrasive use. It established limits of size and of composition: Grade A, at least 95 pct +3 mesh and 92 pct alumina (Al2O3); Grade B, at least 95 pct +7 mesh and 90 pct alumina. It also specified that "of each lot of material, not less than 95 percent shall have a hardness equal to or exceeding nine (9) on Moh's Scale." These specifications were unsatisfactory for several reasons. They did not allow the purchase of lower grades of corundum being used by industry. Neither did they specify exactly what a corundum ore actually was, except that it should contain so much alumina and have a certain scratch hardness. Nothing was said about the abrasive qualities of the material that was to be purchased primarily for abrasive use. During the period 1946 to 1948 supplies of the two grades defined in the then current specifications continued to decrease. Early in 1949 industry recommended that the finer sizes of corundum known as "crystal corundum concentrates," ¼-in. to 16-mesh material, be added to the stockpile specifications and that lower grades of crystal corundum also be included. In the spring of 1949 the National Bureau of Standards and the Bureau of Mines were asked by the Munitions Board to cooperate in developing more practical specifications for grading natural corundum ores. The National Bureau of Standards indicated that it would investigate physical test methods for determining abrasive characteristics of corundum, and the Eastern Experiment Station of the Bureau of Mines at College Park, Md., stated that it would consider the mineralogical aspects of the problem. Members of these two agencies, in consultation with representatives of the Office of Materials Resources of the Munitions Board and of the Federal Supply Service of the General Services Administration, and with the cooperation of industrial suppliers and consumers of abrasive corundum, developed, in a fairly short time, more practical specifications for six grades of corundum ores. The new specifications, issued January 1951, were for corundum, natural crystals, as by this time high-purity synthetic corundum was available and widely used. Nevertheless, for certain specific applications the natural product was preferred over the synthetic material. It has been extensively used in forming snagging wheels. It breaks into more or less cubical particles, whereas artificial corundum fractures into splintery shapes. These produce irregular cuts in glass, while the more symmetrical shape produces a more uniform ground surface. For this reason natural corundum has been preferred for certain types of lens grinding. Pure corundum is clear, colorless alpha alumina (A12O3), but it is rarely found in nature in this form. The most important gem varieties include the blue and yellow sapphires and the ruby. Minute impurities of titanic oxide impart a blue color,

Jan 1, 1955

By J. Ostachowicz, B. Holynska, M. Lankosz

The paper presents an analyzer and the method for the continuous determination of weight percentage of ore grains with diameter smaller than 75 pm in mineral slurries. The method is based upon the measurement of characteristic x-rays of copper excited by primary radiation of two different energies 16.5 keV and 60 keV from Pu238 and Am241 sources respectively. Additionally the backscattered primary radiation is measured in order to correct the variations of the solids content in the slurry.

Jan 11, 1979

I. MCLAUGHLIN, R. P.-Protecting California Oil Fields from Damage by Infiltrating Water. Discussed by M. E. Lombardi, A. F. L. Bell, A. C. McLaughlin, R. P. McLaughlin, William A. Williams, Mark L. Requa, C. D. Keen 2413 BEST, W. N.-Petroleum as Fuel Under Boilers and in Furnaces. Discussed by William A. Williams, Hennen Jennings, David T. Day, Mark L. Requa, A. F. L. Bell, W. N. Best 2420 JOHNSON, ROSWELL H.-Sliding Royalties for Oil and Gas Wells. Discussed by William A. Williams, A. C. McLaughlin, A. F. L. Bell, Roswell H. Johnson 2423 BELL, ARTHUR F. L.-Important Topping Plants of California. Discussed by William A. Williams, David T. Day, A. F. L. Bell 2426 LOMBARDI, M. E.-The Cost of Maintaining Production in California Oil Fields. Discussed by C. D. Keen, Mark L. Requa, H. M. Bacon, M. E. Lombardi 2427 HUNTLEY, L. G.-Oil, Gas, and Water Contents of Dakota Sand in Canada and United States, Discussed by E. W. Shaw 2428

Jan 12, 1915

By C. H. Mathewson

CONSIDERABLE progress has been made during the last few years in analyzing the action of plastic deformation in metallic crystals. This is due largely to the development of X-ray spectrographic methods for studying changes in the orientation of single crystals, or of conglomerates, as they occur during the process of plastic deformation, but partly to the widespread knowledge of suitable technique for preparing large (single or variously combined) crystals for direct crystallographic observation under stress or in various conditions of strain. These two methods of studying changes in the crystalline structure of metals may of course be used in conjunction with features of mutual support, but unfortunately the advantage of direct crystallographic observation is lost when we proceed to the study of severely cold-worked structures, owing to the occurrence of real or apparent crystalline discontinuities which become more and more complicated as the amount of plastic action increases. Furthermore, the X-ray methods do not appear to be adequate, at least in their present stage of development, to fix definitely the character of structural alteration in the parent crystal lattice by plastic deformation. The principal question at issue concerns the nature of the crystalline particles that remain after plastic deformation. These are generally known in our American metallurgical literature as crystalline fragments,1 and they seem, indeed, to diffract as individuals causing the Hull pattern of a, severely cold-worked metal to resemble the pattern of a fine powder,2 with certain features of preferred orientation among the particles determined by the manner and intensity of cold working.

Jan 1, 1927

By K. D. Jacob

MONTANA Phosphate Produucts Co., a subsidiary of The Consolidated Mining and Smelting Co. of Canada Ltd., operates three properties near Garrison, Mont., known as the Anderson, Graveley, and Luke mines. All three are underground operations, mining the same narrow bed at points several miles apart. The Anderson, the oldest and largest of the three, has produced about 700,000 long tons since 1929. The Graveley has produced slightly over 100,000 long tons since 1940, and the Luke, acquired in 1943, is still in an early stage of development. The great bulk of the output has been shipped to the Trail, B. C., plant of Consolidated Mining and Smelting Co. for use in the manufacture of fertilizers. The phosphate seam is the basal member of the Permian Phosphoria formation. In all three mines it has a uniform thickness of 3 to 4 ft. of oulitic phosphate, with a few shaly partings. The overlying part of the formation comprises about 50 ft. of chert and the immediate footwall consists of a few feet of shale and sandstone. underlain by the Quadrant quartzite.

Jan 1, 1944

By B. L. Averbach, M. Cohen, G. P. Conard

IT has been frequently observed that, when metal crystals are bent and annealed or when they are bent at elevated temperatures, the asterism of the Laue spots is split discontinuously into tiny intensity maxima. This finding indicates that segmented crystallites or subgrains are produced, which are relatively undistorted within themselves but which differ slightly in orientation from their neighbors. The following viewpoints have been put forward concerning the nature of this segmentation process: 1—Crussard' has described the phenomenon as "re-crystallization in situ." According to this mechanism, the deformed lattice recrystallizes on heating into an aggregate of comparatively strain-free subgrains separated from one another by low-angle boundaries and having nearly the same orientation as the original crystal. This process differs from the classical type of recrystallization in that the latter involves the formation of grains having quite different orientations from that of the mother crystal. 2—A similar but more detailed picture has been advanced by Cahn' who adopted the term "polygonization." In this interpretation, the plastic bending of lattice planes results in an excess of dislocations of one sign, but at suitable temperatures these dislocations migrate along slip planes and collect in localized regions to form an array of low-angle boundaries. Concurrently, the lattice segments between the boundaries lose their curvature and elastic strain. 3—The "cell formation" concept of Wood and co-workers: unlike the two hypotheses cited, postulates that the segmentation of the lattice is basically a mode of deformation and is not an annealing phenomenon. Cell formation appears to compete more effectively with respect to the normal slip process as the deformation temperature is increased and as the strain rate is decreased. The present work was performed on 3.2 mm diameter 99.99' pct Zn single crystals, grown from the melt in a gradient furnace. The major impurity was 0.003 pct Fe. The crystal orientations ranged from those with basal plane parallel to the rod axis to those with the basal plane almost perpendicular to the rod axis. The specimens were bent on templates to effective radii varying from 14.2 to 1.3 cm at the temperatures from —196" to 100°C. In each case, the axis of bending was parallel to the basal plane. Subsequent annealing was carried out at temperatures from —196" to 400°C. Back-reflection Laue pictures were taken on the convex surface of the bent specimens, before and after annealing. This procedure was found to yield better resolution of the detail in the diffraction spots than did the previously used Laue transmission technique. Some X-ray pictures of rods bent at —196" and —78°C were taken at these respective temperatures without intermediate warming to room temperature. In addition, bent crystals were acid cut" parallel to the basal plane, and double-crystal spectrometer rocking-curves were obtained from the etched (0001) face before and after increment an-

Jan 1, 1954

By Paul D. Foote

Most of the treatises on metallurgy intimate that simultaneously with the development by the atomic physicist of a really satisfactory theory of the atom will be inaugurated a new epoch in the science of metals. Metallurgically and metaphorically, we shall dwell in the Utopia of Sir Thomas More. It is my privilege this afternoon to demonstrate that this state has not arrived. An atom is a miniature planetary system consisting of a positively charged nuclear sun about which revolve electrons each carrying the negative charge e. The charge on the nucleus is + Ze where Z is the atomic number and the number of planetary electrons in a neutral atom is equal to Z. These electrons are arranged in several groups having different binding energies. Ordinary x-ray phenomena relate to processes occurring deep within the atom, usually with electrons in the so-called K or L shells. Such electrons in the heavier atoms are so closely bound to the nucleus that the forces exerted by neighboring atoms in a solid are relatively inappreciable. For most practical x-ray investigation, the atom may be considered as in the gaseous phase completely isolated from its neighbors. The K radiation from an element in the gaseous state, in the solid or liquid phase, or even in combination with other elements in all its possible valences, is almost identical.‡ Visual and ultraviolet spectroscopy is concerned with disturbances of the most loosely bound outer or valence electrons of the atom, always in the vapor state. The remarkable progress of the last year in both theo-

Jan 1, 1926

The American Society of Mechanical Engineers extends an invitation to members of the Institute to participate in an exceedingly interesting excursion on Saturday, November 11. Permission has been secured for a visit to the plant of the Electric Boat Co. at New London, Conn. There will be run a special-test on a high-power 8-cylinder, 4-cycle Diesel engine. A large number of submarine and other engines in various stages of construction will be seen, also the boring of torpedo tubes, cylinders and other equipment for submarines. The drafting rooms and foundry mill also be open for inspection. The party will have an opportunity to see at close range the submerging of several submarines, and an attack on a vessel on the surface, an exhibit which is being arranged by courtesy of Rear Admiral A. W. Grant, who is in command of the submarine forces of the United States. The Boston members will leave South Station on train No. 7 at 8.30 A. M. Those from Providence will board this train at 9.36 A. M. The Worcester members will leave on train No. 745 at 8.36 A. M. The New York contingent will leave the Grand Central Terminal at 8.31 A. M. on train No. 8. This train will leave New Haven at 10.30 A. M. Upon arrival at New London, each group will go directly to the Mohican Hotel, where a "get-acquainted" luncheon will be served

Jan 10, 1916

By E. T. Turkdogan, P. Grieveson

Experimental results are given for the rate of oxidation of ferrous iron to ferric iron in pure molten iron oxide by carbon dioxide + carbon moloxide mixtures at 1550°C. It is shown that the rate-controlling process is the interdiffusion of iron and oxygen atoms within the melt. The inter-diffusivity of iron and oxygen in the melt is obtained from the results and the value of (5.0 * 1.0) x 10-5sq cm per sec is recommended for the temperature of 1550°C. Similarly, it is also found that the rate of reduction of molten iron oxide is con -trolled by diffusion in the melt; however, apparent interdiffusivity values from these experiments are 10 to 20 pct higher than those obtained in the oxidation experiments, by virtue of convection arising from density difference. The results of the oxidation experintents are used to calculate an estimated self-diffusivity of iron in molten iron oxide of (1.5 * 0.5) x sq cm per sec. BECAUSE of the industrial importance of iron oxides, the study of the kinetics of both the reduction and oxidation of the solid oxides has received a great deal of attention. However, knowledge of the kinetics of similar reactions in the liquid state is very meager. Dancy 1 studied the kinetics of reduction of molten iron oxide by carbon in pig iron and found that the reaction is very fast. It was concluded from the results that the reduction of molten ferrous oxide is a first-order reaction up to 80 pct reduction, while

Jan 1, 1964

By William Fink

SINCE so many different curves have been published for the solid solubility of zinc in aluminum, it seems desirable to definitely establish the correct curve by two or more independent methods. The curve published in part I1 was based entirely upon X-ray measurements because the other methods employed at that time were not satisfactory. The present paper (the seventeenth of this series on high-purity aluminum alloys) describes the determination of the solid solubility of zinc in aluminum by the measurement of electrical resistivity at temperature and by microscopic examination. Since the publication of our part I in 1932, an investigation of the solubility relations in the aluminum-zinc system has been reported by Schmid and Wassermann2, who obtained their solubility results from lattice-parameter measurements on heat-treated and quenched speci-mens. The diagram that they published is shown in Fig. 1. In this investigation they also found by X-ray measurements that the parameter of the gamma phase changed continuously with zinc content and at such a rate that it would be identical with that of the beta phase at 60 atomic per cent zinc. It was concluded therefore that the beta and gamma phases, from the point of view of structural relationship, are one single phase. They also suggested a gap of immiscibility between 270° and 350° C. The complete boundary in this region could not be deter-mined satisfactorily by the method employed and therefore was not shown in their diagram.

Jan 1, 1936

Jan 1, 1961

By John Fritz

THE John Fritz Medal was presented to Ambrose Swasey of Cleveland, Ohio, in the Auditorium of the Engineering Societies Building, in New York, on April 23. Charles F. Rand, Chairman of the Board of Award, presided and, after speaking very briefly of Mr. Swasey, whose friend he has been for a great many years, ,introduced Gen. William Crozier, formerly Chief of Ordnance, U. S. Army, who spoke most entertainingly of, Mr. Swasey's accomplishments in designing and manufacturing instruments of precision, particularly for the use of artillery in range finding: Dr. William Wallace Campbell, Director of the Lick Observatory, and President of the University of California, described Mr. Swasey's, contribution to astronomical advancement by his notable development of the largest telescopes in this country.

Jan 1, 1924

By J. G. Benford, E. B. Stanley

THERE have been numerous papers in the literature1 on the subjects of secondary and tertiary recrystalli-zation in silicon steels. Secondary re crystallization is believed to occur in silicon steel by either a surface-energy phenomenon such as in the usual development of cube texture or by a second-phase phenomenon such as in the usual production of cube-on-edge texture, (110)[001]. Tertiary recrystallization in silicon steel is thought to be a surface-energy phenomenon in which, for example, grains having a (110) plane parallel to the sheet grow at the expense of other grains in the matrix including those having a (100) plane parallel to the plane of the sheet. In all these instances, the orientations involve either a preferred (100) or (110) plane in the plane of the sheet. Until very recently, there had been no experimental evidence reported of the occurrence of a texture by secondary or tertiary recrystallization that involves a (111) plane in the plane of the sheet, although Kohler reported that grains having the (111) plane parallel to the sheet surface can also grow by a surface energy mechanism. Stickels observed a secondary texture in iron described as "near {554}(225)" about 5 deg from {lll}(211).3 Mee reported that in a vacuum-remelted commercial 3 pct Si steel {lll}(hkl) secondary recrystallization took place in a high vacuum and in pure hydrogen.4 Recently in our Laboratory, large-grained structures such as shown in Fig. 1 having an orientation near (111)[211] or (111)[2ii] have been observed. The arrows point to areas of relatively small matrix grains of the kind that the much larger (111) grains consumed while growing. It is of interest that the matrix grains of samples annealed at 2000°F were essentially the same size as those in samples annealed at 2200°F, a matrix-grain-size stability that is characteristic of secondary recrystallization processes. A torque disc taken from Grain 4 of the sample shown in Fig. 1 revealed a very flat magnetic-torque curve, as expected, with a maximum torque of 7000 dyne-cm per cu cm compared to the typical 180,000 dyne-cm per cu cm observed for conventional (110)[001] textured material. A back-reflection Laue pattern for Grain 4 is shown in Fig. 2 and indicates a near-perfect (111)[211] orientation. The other six numbered grains in the sample of Fig. 1 had a similar orientation. The small circles next to each number were the target areas for the X-ray beam. The starting material was an 0.011-in.-thick oriented silicon steel, (110)[001] texture, containing 3 pct Si. It was lightly pickled, cold-rolled to 0.005 in., and annealed 4 hr at 2200°F within a nickel box (not gas-tight) inside a tube furnace through which dry hydrogen was flowing. The samples were heated to 1500°F in 1 hr and then at 60°F per hr to 2200°F. There were other

Jan 1, 1969

By D. M. Hausen

A quantitative x-ray diffraction method has been developed for the analysis of alteration minerals in wallrock. Alteration data are plotted and contoured (analogous to geochemical data). Alteration trends outlined by this technique correlate closely with geochemical anomalies, and in some cases extend well beyond the perimeter of anomalous base metal values. "Monomineralic contouring," applied originally to porphyry-type mineralization, has been extended to other types of mineralization, including volcanogenic massive sulfide deposits. Equipment and techniques used in the quantitative measurement of alteration mineralogy are discussed.

Jan 1, 1980

By R. A. Vandermeer, C. J. McHargue

The (001) fiber-texture component, found in aluminum rods extruded at subzero temperatures, consists of particles of various sizes having extremely irregular shapes dispersed in a nonuniform way throughout a matrix of the (111) orientation. Apparently the (001) texture component is not a result of recrystallization but rather is due to the presence of reimanents of the original grains which fragmented from the main body of material as it reoriented towards the (111) orientation during the extrusion process. Both X-ray line-broadening measurements and electron-microscopic observatwns indicate that, after extrusion, regions having (001) orientations are in a state of relatively less strain and distortion than (111) regions, suggesting that the former have undergone less plastic deformation. A (001) fiber-texture component is also found after complete recrystallization of extruded specimens. Approximately one third of the recrys-stallized volume has this orientation. The (001) fragments, formed during the extrusion process, act as nuclei for recrystallization; i.e., the pain boundaries separating these fragments from the matrix are capable of migrating during annealing. Electron-transmission microscopic observations and X-ray line-broadening measurements indicate that (001) regions recover at a much more rapid rate than (111) regions at annealing temperatures up to 187°C. DURING the extrusion of a rod or the drawing of a wire the individual grains comprising the piece tend to reorient towards a preferred orientation (texture) which is of the fiber type where a particular crys-tallographic direction, (uvw), in each crystallite tends to be aligned parallel to the longitudinal axis

Jan 1, 1964

By Fred Witt, Milton Schwartz

ESTABLISHED methods for obtaining quantitative pole figures for flat sheets1"5 can be extended to apply to thin films on a substrate. The mode of scanning the sample is exactly the same as described in the references? but consideration is given to the fact that the scattered X-ray intensities are due to both the thin film and its substrate with appropriate attenuation factors. The purpose of this paper is to describe a method to obtain the scattered intensities from the film alone for subsequent pole-figure determinations. Fig. 1 shows the four possible general positions of the film (f) and its substrate (s) with respect to the incident X-ray beam (I,). In this paper it will be assumed that the plane of the sample is normal to the plane of the diffractometer. In the diagrams the line jV is the normal to the flat sample and the line P is the trace of the diffracting crystallographic planes in the plane of the diffractometer. The angle of tilt, a, is the positive acute angle measured from the line N to the line P; if this angle is measured clockwise then a is said to be in the positive a region; if this angle is measured counterclockwise then a is said to be in the negative a region. For the reflection cases, the total scattered intensity, at the proper Bragg angle for a particular set of planes, is due to that scattered by the film Vf) and that scattered by the substrate. The beam incident on

Jan 1, 1967

By W. H. Smith

IN connection with some recent work on the effect of impurities on the ductility of chromium, it appeared desirable to know the solid solubility of carbon in chromium. A literature survey indicated that this information was not available. Although considerable work has been done on the Cr-C phase diagram,&apos;.&apos; previous investigators have been more concerned with the structure and phase boundaries of the carbide phases than with the terminal solid solution. The phase diagram shown in Fig. 1 is taken from the work of Bloom and Grant&apos; and represents the most recent determination. As indicated by the dashed line, the a solid-solubility limit was not determined. Experimental Procedure Alloys of chromium were prepared from hydrogen-treated and vacuum-degassed electrolytic chromium plus spectrographic grade carbon. The oxygen and nitrogen content of the alloys was <0.002 pct. After melting, analysis of the alloys showed them to contain 0.02, 0.08, 0.15, and 0.55 pct C. Pieces of the alloys were heated in a protective atmosphere to various temperatures and then quenched after holding for a time sufficient to insure equilibrium. Microscopic examination of the as-quenched alloys for the presence of a second phase was used as a measure of the solubility limit. The heats were made in a multiple hearth arc-furnace using a zirconium-gettered static argon atmosphere. A zirconium melt was made before each Cr-C heat. Triple melting was used to insure ingot homogeneity as shown by microscopic examination. The alloys were prepared by adding portions of a 4.5 pct C-Cr master alloy to high purity chromium. The carbon contents listed previously were those obtained by analysis. The nitrogen and oxygen contents after arc melting were both <0.002 pct. Sections 1/8X1/4X1/2 in. were cut from the 100-g ingots and a hole drilled in one end in order to suspend the sample from a molybdenum wire. After the surface was carefully cleaned, a sample of each melt was hung in a mullite tube heated externally by a platinum resistance furnace connected to a vacuum system. The lower portion of the mullite tube was sealed to Pyrex and closed off several inches below the furnace. This was filled with sili-cone oil kept cold by circulating cold water around the outside of the Pyrex. Quenching into the oil bath was achieved by melting a fuse wire supporting the sample. It required about 4 sec for the sample to cool from 1400" to 600°C. This severity of quench was considered satisfactory to freeze-in the high temperature equilibrium. For tests made at temperatures of 900" to 1200°C, heating was done in vacuum; for tests above 1200°C, an argon atmosphere was used. The holding time employed ranged from 12 hr at 900°C to 6 hr at 1400°C. Experiments were performed at temperatures of 900°, 1000°, 1100°, 1200°, 1300°, and 1400°C. Microscopic examination for evidence of a second phase was done at X1500. Experimental Result The microstructures of a 0.08 pct C-Cr alloy as-cast and after quenching from 1300°C are shown in Figs. 2 and 3. A 0.15 pct C-Cr alloy quenched from 1300°C is shown in Fig. 4. The data obtained from the quenching experiments is shown graphically in Fig. 5. If the Van&apos;t Hoff equation is obeyed, a plot on a logarithmic scale of the mol fraction of solute vs the reciprocal of the absolute temperature should give a straight line. For dilute solutions the weight percentage can be substituted for the mol fraction without introducing any appreciable error. The Van&apos;t Hoff equation can then be written as where H is the heat of solution in calories per mol. The slope of the straight line on the log pct C vs 1/T plot gives the value of AH. Assuming that the Van&apos;t Hoff equation is obeyed, which is probably justified for the dilute solution of carbon in chromium, the heavy straight line shown on Fig. 5 represents the best fit of the data. This line was obtained as follows. On Fig. 5 the results of the microscopic examination of all alloys following quenching were plotted and designated as to whether one or two phases were seen. Below 1100°C all alloys showed a second phase on quenching. The heavy vertical lines shown in Fig. 5 therefore represent the possible range of the ter-

Jan 1, 1958