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By Peter R. Morris, Alan J. Heckler

THREE angles are required to specify the orientation of a crystallite with respect to a physical reference frame. The distribution of crystallite orientations in a polycrystal is thus a function of three angular variables. The most widely used experimental techniques for studying orientation in polycrystals lead directly to the pole figure representation, i.e., the distribution of the poles of certain crystallographic planes in terms of two angular variables. In recent years1-5 methods have been developed which permit determination of the (three-angle) crystallite orientation distribution from several (two-angle) pole figure distributions. In this work Roe's method has been applied to the study of orientation in hcp materials. The method is illustrated for commercial purity titanium sheet (Ti-70) which was cold rolled (65 pct reduction), annealed at 1450°F for 3 min, and air cooled. The grain shape was observed to be equiaxed after this treatment. EFFECTS OF PHYSICAL, CRYSTALLOGRAPHIC SYMMETRY In Roe's method the crystallite orientation distribution, w(?,?,F), is expanded in a series of generalized spherical harmonics 11(?,?,F) = E E E W^Zirmtye-tote-in* [l] 1=o ,,,=-I ,,=-I where { = cos 8. The set of Euler angles employed here is illustrated in Fig. 1. The axis for each rotation is denoted by a double arrowhead. The positive sense of each rotation is that of a right-handed screw advancing in the direction of the double arrowhead. The X, Y, and Z directions correspond to the rolling direction, cross direction, and normal direction, respectively. In the initial orientation (10.O), (12.O), and (00 . 1) planes are perpendicular to the X, Y, and Z directions, respectively. The IC/ rotation about the Z axis is carried out first by rotating X into X', Y into Y', and leaving 2 unchanged, i.e., Z' = Z. The 8 rotation about the Y' axis is carried out second by rotating X' into X", 2' into Z", and leaving Y' unchanged, i.e., Y" = Y'. The I$ rotation about the Z" axis is carried out last by rotating X" into X"', Y into Y"', and leaving 2" unchanged, i.e., 2"' = 2". Any specified orientation of the X'", Y'", and Z'" crystal-fixed axis system relative to the X. Y, and Z physical axes (rolling direction, transverse direction, and sheet normal direction, respectively) can be obtained by appropriate IC/, 8, and (F rotations. The Zl,, of Eq. [l] are the Jacobi polynomials, augmented by the square root of the weight function. The Zl,, are symmetric in m,n, i.e., Zl,,= Zlnm. For orthotropic physical symmetry and hexagonal crystallographic symmetry, the coefficients, W!,,, of the series are all real, W!mn = Wzfi, = Wlm~ = Wlfi~, 1 and m are even and n is restricted to 6k, where k = ...,-2,-1, 0, 1, 2, .-.. The determination of the Wlmn from pole figure data has been previously described.'~~ The Zl,, may be written in multiple angle form

Jan 1, 1970

For the year ending February, 1926 PRESIDENT J V W REYNDERS, District 0 NEW YORK, N Y PAST PRESIDENTS E P MATHEWSON, District 0 NEW YORK, N Y WILLIAM KELLY, District 5 IRON MOUNTAIN, MICH FIRST VICE-PRESIDENT E DEGOLYER, NEW YORK, N Y TREASURER , CHARLES F RAND, NEW YORK, N Y SECRETARY FREDERICK F SHARPLESS, NEW YORK, N Y

Jan 1, 1923

By F. Rosenblum, P. Spira, F. Kitzinger

The possibility of increasing the efficiency of mineral processing plants by means of computer control has prompted metallurgists to examine their flowsheets more critically in order to develop practical control strategies. Control schemes in use to date generally rely on the automation of traditional and previously manually regulated control loops, e.g., the addition of reagents to maintain a constant assay or a constant pH. This approach is predicated on the availability of well established primary sensors such as pH electrodes or on-stream analyzers. Noranda Research Center, in cooperation with Noranda Group concentrators, has developed a froth level monitor and a pulp density meter adaptable to this type of control. Although some of the basic principles on which they are based have been known for some time, their incorporation into the design of reliable, direct-reading instruments which can be interfaced with a computer is believed to be novel.

Jan 1, 1980

By Reinhard Fischer

The consumption of lead for batteries in some western countries and Japan amounts to 870,000 T. annually. Battery life is 2-3 years. Therefore after a short time a considerable quantity of lead flows back to smelters. The production of lead from scrap batteries is discussed from the following points of view: 1. Separation of the acid contained in the batteries. 2. Separation of the components which are free of lead from the components containing lead, e.g. cases, separators. 3. Separation of metallic lead from lead compounds. 4. Avoidance of manual-work. A process has been developed and perfected at a plant, which began operation in 1965. The procedure consists essentially of the following steps: 1. Breaking the cases and removing the acid. 2. Crushing the batteries in an impact mill. 3. Screening off separators. 4. Separation of slurry. 5. Gravity separation of metal and organic material. The plant has a one-shift capacity of -24,000 T. batteries/year.

Jan 1, 1970

FRank FirmstoNe, Easton, Pa.: The effect of lead on brass seems to have been recognized by Berthier, and the facts published by him as early as 1818 (Ann. des Mines, 1st ser., iii., 1818, p. 347 et seq.). He there says expressly that copper containing lead makes " dry " (see) brass, and that, for the same reason, blast-furnace

Jan 1, 1898

Jan 1, 1949

By F. Rosenblum, P. Spira, F. Kitzinger

The possibility of increasing the efficiency of mineral processing plants by means of computer control has prompted metallurgists to examine their flowsheets more critically in order to develop practical control strategies. Control schemes in use to date generally rely on the automation of traditional and previously manually regulated control loops, e.g., the addition of reagents to maintain a constant assay or a constant pH. This approach is predicated on the availability of well established primary sensors such as pH electrodes or on-stream analyzers. Noranda Research Center, in cooperation with Noranda Group concentrators, has developed a froth level monitor and a pulp density meter adaptable to this type of control. Although some of the basic principles on which they are based have been known for some time, their incorporation into the design of reliable, direct-reading instruments which can be interfaced with a computer is believed to be novel.

Jan 4, 1979

TO metallurgists generally, Arthur S. Dwight is no stranger even to those who do not know him personally. He is one of those contributors to technical progress whose names will go down to posterity because of their being attached to a successful machine or process, such as Dorr, Hardinge, or Marcy, or Wedge, MacDougall, or Herreshoff. The roasting and sintering method and equipment developed by Colonel Dwight and his associate, the late Richard L. Lloyd, may be found in lead smelters throughout the world, and also in many metallurgical works dealing with other ores, including those of iron. It is ordinarily used to desulphurize and agglomerate fine ores for subsequent smelting. Colonel Dwight's citation as James Douglas Medalist reads: "For his contributions to the art of smelting nonferrous ores; and particularly for his pioneer work in developing equipment and technique for sintering such ores and metallurgical products." The medal was awarded at the last Annual Meeting of the A.I.M.E. but unfortunately the medalist was unable to leave Florida at the time to receive it in person.

Jan 1, 1942

By Joseph Jensen

California's outstanding contribution to unit operation is the plan of development now established for the North dome of the Kettleman Hills. Beginning April 1, 1931, the Kettleman North Dome Assn. will control the unified operation and development of 10,800 acres of proven and semiproven oil land, and at the same time the Standard Oil CO. of California will operate as another unit its fee land of 9460 acres of similar character. The holdings of the two companies are in a checkerboard mile-square pattern. In addition to this, 410 acres of land may yet be included in the Kettleman North Dome Assn. unit and 530 acres of land are definitely out of both units. The owners of some of this land have expressed their intention of cooperating in a reasonable way with these two units. Cooperative agreements are now in force as to most of this field. Under the definitions of a unit pool and a near-unit pool,' the operation at Kettleman Hills will be a near-unit operation, but because of the size of the structure and its proven highly productive character, the arrangement. concluded on Jan. 31, 1931, in the approval of the Kettleman North Dome Assn. Agreement by Secretary of the Interior Ray Lyman Wilbur and by California State Oil and Gas Supervisor R. D. Bush is of outstanding importance to the entire oil industry. No other major unit operation plans are under way in California at the present time. There has been some little discussion of a plan in the North Belridge field and a feeling that the discovery of oil in the Lost Hills field and also in the South Belridge field would necessitate consideration of unit plans. So few data are available for these areas, as to the land that should be included in such unit plans, that little constructive action is now possible. The beginning of drilling on the Middle dome of the Kettleman Hills also makes it an area deserving consideration for unit operation. All four of the above-named areas lie on the west side of the San Joaquin Valley, in Kings and Kern counties, to the south of the

Jan 1, 1931

By Donald L. Katz

The equilibrium constants developed by Souders, Selheimer and Brown1' have been very useful tools in predicting vapor-liquid equilibria during the past five years. Their equilibrium constants were computed by assuming ideal solutions and recognizing the deviations of vapors from ideal gas laws. The same fundamental concepts were used by Lewis and co-workers8 for predicting vaporization phenomena by means of fugacities. The equilibrium constant is defined by equation 1: y\x =K [1] in which K = equilibrium constant, y = mol fraction of a constituent in the vapor phase, x = mol fraction of the constituent in the equilibrium liquid phase. The equilibrium constants are a function of temperature and pressure and might be considered as replacing the ratio of the vapor pressure to the total pressure of Raoult's law. They may be used to compute the vapor or saturation pressure of a liquid or the dew point of a vapor for any pressure or temperature from the analysis of the mixture much as Raoult's law is used. Likewise, the quantity of a mixture that will vaporize at any equilibrium temperature and pressure and the composition of the vapor and liquid may be calculated. The purpose of this paper is to review the available equilibrium data of interest in petroleum production, to discuss the auxiliary physical properties of the hydrocarbons, and to present typical uses of the equilibrium constants. The particular applications chosen are the computation of the results of stage separation of crude oil and natural gas, the calcula: tion of a pressure-volume curve of a crude oil-natural gas mixture, and information gleaned from a consideration of reservoir equilibria.

Jan 1, 1938

NAME "Utah" is derived from the name of the Indian tribe, variously spelled "Yuta," "Ute," "Youta." "Uta." "Eutaw," and finally "Utah." It means "in the tops of the mountains," or "on the heights." The state emblem is the "Beehive," typical of industry. State nickname is "Beehive State." AREA Utah is the tenth state in area. It contains 84.990 square miles, of which 2.806 miles are water. When admitted as a territory in 1850. Utah included all the area from the east line of California to the summit of the Rocky Mountains between the 37th and 42nd parallels, which embraced practically all of the present state of Nevada, all of western Colorado, part of Idaho and part of Wyoming, in addition to the present area of Utah.

Jan 1, 1925

By C. Richard Tinsley

Mineral economists debate whether to call the deep-ocean nodules "manganese nodules," "nickel nodules," "polymetallic nodules," or even "ferro-manganese nodules." It is nickel and copper that are generally regarded as the main targets in the nodules. Processing considerations are thought to virtually dictate that Deepsea Ventures will produce high-purity manganese metal (at least if it follows a hydrogen chloride leach), whereas other groups have been focusing on the selective extraction of copper, nickel, cobalt, zinc, and molybdenum, while rejecting manganese to tails. Solvent extraction appears to be the primary multimetal extraction technique (except for manganese). These processing considerations indicate that metal production f, or Deepsea Ventures is essentially a co- product system (manganese recovery is necessary to recycle chloride ions) while the other groups can more easily approach the metals as selective co-products (e.g. recovering nickel and copper, and rejecting cobalt). Some zinc may be produced as a co-product, as it may have to be removed in the solvent extraction process.

Jan 4, 1975

By E. H. Jr. Dix

THE success of the Charpy impact test in the steel industry has led those interested in aluminum alloys to investigate the possible applica¬tion of this test to aluminum and its alloys. In this paper are set forth the results of a few preliminary tests made at the Lynite Laboratories of the Aluminum Manufactures, Inc. In order to study more thor-oughly the significance of the Charpy test, slow-bending tests have been made duplicating the arrangement of the impact machine. Tests have been made on both notched and unnotched specimens of a series of copper-aluminum alloys. APPARATUS The standard American-made Charpy impact machine delivering a blow of over 200 ft.-lb. was- much too large to test aluminum-alloy specimens of the same type used for steel, so that it was necessary either to adopt a larger specimen or to have a special light-weight hammer made. Since there is no known relation between specimens of different sizes, even though geometrically similar, it was decided to adhere to the 10 by 10 mm. specimen. Accordingly, Sauveur and Boylston, the American makers of the machine, were asked to construct a special light-weight pendulum adapted to their standard machine, this pendulum to have one-tenth the capacity of the standard. The writer wishes here to acknowledge his indebtedness to Mr. H. M. Boylston for the personal interest and care exercised in constructing this pendulum. The machine with, the light-weight hammer in place is shown in Fig. 1. It is mounted on a concrete foundation with the concrete covering the flange on the base of the machine. Vibration is further prevented by four 5/8 -in. (15.8 mm.) foundation bolts. The large standard hammer shown against the wall was also used for some of the unnotched bars that requited more than 20 ft.-lb. to rupture.

Jan 4, 1920

For the year ending February, 1919 PRESIDENT SIDNEY J. JENNINGS NEW YORK, N. Y. PAST PRESIDENTS L. D. RICKETTS, NEW YORK, N. Y. PHILIP N. MOORE ST. Louis, Mo. FIRST VICE-PRESIDENT C. W. GOODALE, BUTTE, MONT. TREASURER GEORGE C. STONE, NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 11, 1918

For the year ending February, 1919 PRESIDENT SIDNEY J. JENNINGS NEW YORK, N. Y. PAST PRESIDENTS L. D. RICKETTS NEW YORK, N. Y. PHILIP N. MOORE ST. Louis, Mo. FIRST VICE-PRESIDENT C. W. GOODALE BUTTE, MONT. TREASURER GEORGE C. STONE, NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 9, 1918

By H. A. Hancock, L. M. Pidgeon

Equilibrium carbon monoxide pressures were measured over the reaction between chromium oxide and a number of solid ferrochromium alloys in the composition range 0.4 to 4.8 pct C and 0 to 49 pct Fe. Measurements were also made for the carbides Cr23C6 and Cr7C3 which agreed well with previous investigations. Between 1050°and 1400°C the pvessures varied from 0.1 to 56 mm and increased markedly with the iron and carbon contents of the alloys. The data were used to estimate the activity of carbon in the alloys and to calculate the equilibrium conditions for the decarburization of a useful range of ferrochromium alloys. WHEN ferrochromium is produced by the reduction of chromite with carbon in an electric arc furnace it invariably contains up to 10 wt pct C. For many purposes such as the production of stainless steel, it is necessary that the carbon content be as low as from 0.02 to 0.05 pct. Thus an important part of the ferrochromium industry consists of the production of low carbon ferrochromium. The classical Bessemer steelmaking technique cannot be used to oxidize low carbon contents in chromium and ferrochromium alloys without also oxidizing the chromium. Recently a new commercial process2-4 has been introduced for oxidizing carbon from high chromium content alloys which consists of heating the solid alloy with such oxidizing agents as Cr2O3, Fe2O3, or SiO2 in a retort at reduced pressures. By maintaining the carbon monoxide pressure below the equilibrium value for the system, the carbon can be removed as carbon monoxide without oxidizing the chromium. The equilibrium conditions for the decarburization of solid chromium carbon alloys have been determined by Boericke5 who measured the carbon monoxide pressure over the reaction between the various chromium carbides and chromium oxide. A typical reaction is shown below. Cr23C6 + 2Cr2O3 =u 27Cr + 6CO [1] These values are not applicable to the decarburization of commercial ferrochromium alloys which invariably contain major amounts of iron. The present investigation was therefore undertaken to measure the change in the equilibrium carbon monoxide pressure brought about by additions of iron to the Cr-C-0 system, thus extending the work of Boericke into the region of the production of low carbon ferrochromium. MATERIALS AND METHOD Materials. Measurements were made on two carbides of chromium, Cr233C6 and Cr7C3, and fifteen Fe-Cr-C alloys. The chromium carbides were made

Jan 1, 1963

By A. E. Bibb, F. W. Kunz

A platelet form of zirconium hydride was found in zirconium and ZY-1 wt pct U single crystals containing hydvogen in the range of 50 to 100 ppm. The habit planes for the hydride plateletg in the zirconium crystals were found to be {1012}, {1121}, and (1122) while the habit planes in the ZY-1 wt pct U crystals were {1121), {1123}, and (1.231). With the exception of the {1231} plane, these have been identified as the twin planes in zirconium. The different effect of hydridc on the mechanical puoperlies of zirconium at high and low strain rates has been explained in terms of the defornzation mechanism and the habit planes of the hydride. ZIRCONIUM and zirconium-base alloys are considered for many nuclear reactor applications, where the pick-up of hydrogen is a distinct possibility, if not an unavoidable occurrence. An excellent example of this is the absorption of hydrogen by zirconium and its alloys during aqueous corrosion, where as much as 30 pct of the hydrogen produced by the corrosion reaction is picked up by the metal. Under the proper conditions, the absorbed hydrogen would precipitate as zirconium hydride and consequently alter the mechanical and physical properties of the zirconium-base alloys. The knowledge obtained from a study of the crystallographic aspects of the hydride precipitation is necessary for the interpretation of the observed changes in the mechanical and physical properties. The deleterious effect of hydrogen on zirconium-base materials is not always observed in normal slow tensile loadings at or above room temperature, but becomes immediately obvious under impact loading, where the energy absorbed decreases with increasing hydrogen content,' and in notched specimens where triaxial loadings are attained.2 This effect is of serious consequence in the applications of Zr where shock loads or high strain rates are experienced. The purpose of this investigation was to determine the crystallographic planes of the Zr and Zr-1 wt pct U matrices upon which zirconium hydride will precipitate and to correlate these with the observed mechanical property data. PROCEDURE Crystal Growth—Single crystals of Zr and Zr-1 wt pct U alloy were used in this investigation. The Zr crystals were made from sponge that had a typical analysis as shown in Table I. Large grains were grown in this material by rapid cooling an arc-melted charge in a button furnace. This operation undoubtedly lowered the volatile impurity concentration below those listed in Table I. Back-reflection Laue patterns of these large grains showed the presence of considerable substructure and lattice distortion within each grain. It was found that an 18-day anneal in an argon atmosphere at 840°C (a high a heat-treatment) followed by furnace cooling, resulted in the further growth of the large grains and removed the detectable substructure ana lattice distortion. Equiaxed crystals with a cube edge of approximately 1/4 in. were produced in this manner. Large crystals of Zircaloy-2 (1.5 wt pct Sn, 0.15 wt pct Fe, 0.1 wt pct Cr, 0.05 wt pct Ni) also were produced by this technique but the large amount of substructure formed could not be removed by annealing. The Zr-1 wt pct U solid solution crystals were produced from an alloy rod consisting of Westing-house-Foote hafnium-free crystal bar zirconium and depleted uranium. The chemical analysis of the alloy is also given in Table I. Three-inch sections were cut from an 0.120-in.-diameter alloy rod and tapered to a fine point on each end. The samples were sealed in evacuated Vycor tubes, homogenized for 5 hr at 1000°C in the ß-phase field, and slowly lowered in a gradient furnace into the a phase (800°C), annealed for 60 hr at this temperature to produce grain growth and furnace cooled. This technique produced large grains approximately 1/2 to 3/4 in. long over the entire cross section of the rod, which were free of observable substructure. Metallographic examination up to X1000 did not show the existence of any second phase in these grains. Crystal Orientation—All crystals were abraded on fine emery paper to produce two flat surfaces 90 deg to each other. The crystals were analyzed by the standard Back-Reflection Laue technique to obtain the crystal orientation with respect to the abraded surfaces. The Back-Reflection Laue Photograms of all crystals used were clear and sharp indicating that the crystals were free from any substructure that could be detected by these means. Hydriding—Only samples containing four to five grains were used for hydriding. Samples that exhibited fine grained patches were discarded. The samples were hydrided using the following technique. After etching in 48 vol. pct HNO3, 48 vol. pct H2O, and 4 vol. pct HF (48 pct) solution, the specimens

Jan 1, 1961

By Sam N. Dewitt, Albert S. Trube

This paper presents a discussion of the pressure maintenance operations which were begun in the New Hope Field. Franklin County. Texas. in 1944. The project has required the injection of extraneous waters at depths from 7.300 to 8.000 ft with intake well-head pressures up to 4.000 psi in three different reservoirs — the Bacon. Hill. and Pittsburg. Records of oil and water production. water injection and the GOR have been kept for each reservoir and reservoir pressures were taken at regular intervals. These data indicate that the Bacon Reservoir had no apparent water encroachment up to the time of water injection. However. the Pittsburg and Hill reservoirs had some natural water influx hut not sufficient to prevent pressures from declining below the bubble point. The Bacon and Hill reservoirs responded almost immediately to water injection. while the Pittsburg which is the least permeable. has shown good pressure response only since .August, 1948. The principle objective of the project has been to increase ultimate recovery. Success of the project to date also has resulted in reduced lifting costs. Esti- mates based on the initial water breakthrough patterns indicate that the primary objective of substantial additional recovery will he accomplished, and there is a possibility that the original estimates elf oil recovery with pres-sure maintenance will he exceeded. INTRODUCTION This pressure maintenance project was one of the earliest primary pressure maintenance programs to he attempted on a multiple zone field. There are three producing reservoirs into which water is being injected for the purpose of maintaining pressure and increasing the ultimate recovery- from each. This paper is limited in scope to al1 account of the development of the project. the pressure production relationship prior to the injection of water and the effect of water injection on the producing reservoirs. Also discussed are the nature of the injection system and the indicated results on initial water break-through in the Bacon Reservoir. FIELD CONDITIONS The New Hope Field, which is located about 12 miles northeast of Winusboro, Franklin County, Texas, is an elongated symmetrical anticline containing four known oil reservoirs. The reservoirs are of the Trinity group of the Comanchean or Lower Cretaceous period and are found in Table I. The oil productive portion of each reservoir is not present in all of the producing wells because their areas and positions vary with respect to one another. Fig. 1 shows the relative position of the four reservoirs and illusIrate? how some wells could penetrate all four, while others are restricted to three. two. or perhaps one. depending on structural location. The first three reservoirs contain undersaturated oil. The deepest. the Elledge, has a primary gas cap. Although this reservoir covers a considerable area of the field. it has a very thin section and a low order of permeability. Elledge producing wells have generally been characterized by an early increase in GOR, making it necessary to recomplete them in other reservoirs. (At present. one well is completed in the Elledge. which is still producing.) Because of the difficulties en-countered in producing oil from this reservoir. and the small quantity of oil actually present. future attempts at producing it will probably be on a salvage basis during the later life of the program. For this reason, the remainder of this report will be confined to a discussion of the Bacon, Hill and pius-burg reservoirs.

Jan 1, 1950

By E. T. Turkdogan, W. L. Worrell

The rate of reaction of hydrogen sulfide with ferrous sulfide was studied by measuring the initial rates of sulfidation of iron strips in hydrogen sulfide-hydrogen-argon mixtures at 670°, 800°, and 900" C. The time-dependent surface sulfur activity is derived from the instantaneous rate of sulfidation with the assumption that diffusion in the sulfide layer is in a pseudo-steady state with the gas-sulfide chemical reaction. The rate of sulfur transfer from hydrogen sulfide to the surface of iron sulfide is proportional to the partial pressure of hydrogen sulfide and inversely proportional to the activity of sulfur at the surface of the sulfide layer. The derived rate equation is based on the assumption that most of the surface sites on the chemisorbed layer of iron sulfide are occupied by sulfur atoms and that the slow rate-controlling reaction is the dissociation of hydrogen sulfide on the chemisorbed layer. The experimental results are in reasonable accord with this reaction model. 1 HE slow approach to parabolic growth rate in the sulfidation of iron in hydrogen sulfide-hydrogen mixtures is a manifestation of slow approach to surface equilibrium between the gas and the surface of the sulfide layer. For example, at 800°C and Fig. 7 in Part I, the parabolic growth rate begins after approximately 1 day of sulfidation time. With decreasing temperature and decreasing partial pressure of hydrogen sulfide, the time necessary to reach gas-sulfide surface equilibrium is much longer. These observations are similar to those reported previously by Turkdogan et al.' on the oxidation of iron to wustite in hydrogen-water vapor mixtures. The slow approach to gas-sulfide equilibrium is well-demonstrated by the results in Fig. 1 where the square of the weight gain per unit area, ( g S per sq cmI2, is plotted against time for gas mixtures having PH g//>H = 1.0 with 0, 25, 50, and 67 pct Ar at 800°C. The value of 1.5 X lo-' (g S per sq cm)' corresponds to almost complete sulfidation of the iron strip (- 0.05 cm thick) to iron sulfide. The points fall on S-shaped curves. If the inflection parts of the curves are considered to be linear, thus indicating parabolic growth rate and the establishment of gas-sulfide equilibrium, their slopes would have to be the same for a fixed ratio in the gas mixture. Such is not the case, and the slopes for the "linear" parts of the S-shaped curves are lower than the value when gas-sulfide surface equilibrium is established. The subject matter of this paper is the kinetics of the surface reaction of hydrogen sulfide with iron sulfide during the early stages of sulfidation of an iron strip. EXPERIMENTAL RESULTS The apparatus and materials used were the same as those discussed in Part I. In the present experiments of relatively short duration, a purified iron strip, 5 by 2 by 0.05 cm, which was suspended in the uniform hot zone of a vertical zircon tube, reacted with a flowing gas mixture of hydrogen sulfide-hydrogen-argon. The sample was suspended from a gold chain attached to a calibrated silica spring. The amount of sulfur picked up by the iron, which formed a layer of iron sulfide, was determined by measuring the displacement of a reference point on the silica spring, using a cathetom-eter. In all cases, the degreased sample was first annealed in a stream of oxygen-free dry hydrogen for several hours to remove any impurities such as oxygen, nitrogen, or carbon which might have been present on the surface of the sample.' The rate measurements were carried out at 670°, 800°, and 900° C in hydrogen sulfide-hydrogen-argon mixtures with pH2 s/Ph2 ratios from 4 to 0.1. In a few experiments of short duration no sulfur deposition was observed in gas mixtures with (comments concerning sulfur deposition at high pH s/ph ratios were made in Part I.) Typical examples of the results obtained are shown in Fig. 2 for two temperatures and two gas compositions. With the present experimental technique, reproducible rate data could be obtained only after a uniform

Jan 1, 1969

By J. W. Spretnak, G. W. Cunningham

Grain growth across the bond region in Pressure bonded copper was found to be mainly dependent upon the presence or absence of microvoids, but it was also found that prior history, bonding pressure, bonding time, and bonding temperature are important variables. An increase in pressure, time, or temperature tends to promote grain growth in the interfacial region. Polygonization is observed after pressure bonding except for specimens previously annealed at temperatures on the order of 1800°F or higher. The dislocation density in bonded specimens was found to be greater in the bond region. THE bonding of metals by the application of gas pressure at elevated temperatures is a relatively new process, having been developed over the past 10 years. The technique, as described by Paprocki, Hodge, and Boyer,l is unique in that assemblies of many parts and complex shapes can be bonded with a negligible amount of deformation. The process thus differs metallurgically from pressure welding, cold welding, and recrystallization welding in that deformation occurs only in a microscopic region whereas, in general, the welding requires severe deformation and may extend the contact surface by a factor of 3 to 10 during the welding. From a practical standpoint, pressure welding is not amenable for bonding large surfaces. During the time in which Paprocki and coworkers were deve1oping the process, West2 established aproc-ess,for bonding aluminum to uranium, and Barnes and Maze? developed a gas-pressure-bonding technique for nickel and copper. Recently, Fugardi and Zambro4 have used equipment similar to that developed by Paprocki and coworkers to establish parameters for bonding stainless steel, aluminum, and zirconium. Most of the investigations on pressure bonding have been empirical in nature and, although methods have been developed for bonding such metals as molybdenum, columbium, titanium, zirconium, and stainless steel, the information concerning the mechanism of bonding is limited. Several workers5"7 have studied the pressure bonding of dissimilar metals in order to gain information on diffusion and formation of inter-metallic phases under application of pressure. Clapson and Robbins8 have shown by a series of annealing studies that voids in the interfacial boundary of roll-bonded copper can prevent movement of the boundary until the voids are spaced far enough apart to prevent pinning. They also indicated that recrystallization and grain growth can eliminate the voids. In this paper it is shown that voids are the major detriment to grain growth across pressure-bonded interfaces, but it is also shown that prior history, bonding pressure, bonding time, and bonding temperature are

Jan 1, 1962