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By Nicholas J. Grant, Noboru Komatsu

Electron-micrographic studies and hardness tests were made of an internally oxidized dispersion-strengthened Cu-12 vol pct SiO2 alloy follozuing longtime annealing at elevated temperatures. The rate of coarsening of SiO2 particles and the relationship between hardness and interpavticle spacing were Dispersion -strengthened alloys exhibit a remarkable stability of structure and properties at elevated temperatures compared with conventional alloys; nevertheless, when they are exposed to high measured. The rate of coarsening of SiO2 particles is controlled by the decomposition of SiO, rather than by the diffusion rates of silicon or oxygen through the copper matrix. The mechanism of coarsening was also studied by using a diffusion-couple technique. temperatures, weakening takes place as a result of coarsening of the dispersed phase. The theoretical treatment of the coarsening of dispersed phases has been treated by Greenwood,1 wagner,, and others3 by considering the interfacial energy of dispersions and the diffusion of solute atoms. Recently, experimental work on the coarsening of relatively insoluble, finely dispersed cobalt particles in copper was reported by Livingston,4 and on aluminum oxide in nickel by Dromsky, Lenel, and Ansell;5 according to these investigations, the rate

Jan 1, 1964

By Earl Oliver

CONTENTS PAGE A.I.M.E. Stabilization Committee Activity 3 Definition of Capture Rule: Robert E. Hardwicke 4 Westmoreland Natural Gas Co. vs. DeWitt 5 Kelly vs. Ohio Oil Co 5 Bernard vs. Monongahela Gas Co 6 Definition of Ownership in Place 7 Prospective Stabilization Remedies 7 Dean Roscoe Pound's Four Tests of Practicability 7 I: Mechanically Feasible 8 Capture Rule 8 Ownership in Place 10 Mechanical Separation Method 10 Engineering Appraisal Method. 11 II. Economically Advisable. ., . 13 Capture Rule 14 Ownership in Place 14 III. Politically Wise 14 Capture Rule 14 Ownership in Place 17 IV. Legally Sound 18 Capture Rule 18 Ownership in Place 19 Dean Henry M. Bates' Analysis 19 Resume 22 THE A.I.M.E. Stabilization Committee was named in 1932 to ascer-tain whether some practical substitute could be devised for the Rule of Capture, which was generally credited with being the major cause of instability in the Petroleum Industry. After considerable intercommittee correspondence a letter was received from. E. DeGolyer under date of Jan. 25, 1935, in which he discussed the possibility of modifying rather than discarding the Rule of Capture. He summarized his proposal as follows:

Jan 1, 1937

On Feb. 16, 1948, the Board of Directors of AIME authorized the publishing of "Technical Notes" in METALS TECHNOLOGY. The purpose is to provide prompt publication of wry short items of the following general types: 1. Results of short investigations which do not warrant a paper. 2. The conclusions of extensive investigations of insufficient general interest to justify a regular paper. 3. Conclusions arising in the course of an investigation, which, because of interest to others in the field, the author wishes to present prior to completion of the investigation. 4. Pertinent factual comment (not mere argument) on the subject matter of previous "Notes." Such Notes will be subject to the approval of the Auxiliary and AIME Publications Committees, but can be handled more promptly than regular papers because they need not be referred to readers. The recommended maxi- mum length is 500 words; notes in excess of 1,000 words will not be considered for this type of publication. A graph or photograph may be included as part of the note when particularly illustrative. As with regular papers, contributions to the new section should be submitted to the Secretary of the AIME.

Jan 1, 1948

By F. P. Schwarz, A. J. Erickson, S. M. Weber

The Mount Hope stockwork molybdenum deposit, Eureka County, Nevada, occurs In a small igneous cauldron complex 32 to 38 mybp in age. The deposit is characterized by alteration zones and mineralized shells symmetrically distributed around multiple intrusive. For samples from the 25000 meters of 1981-82 drilling, an appraisal of error in in-house sample preparation and in commercial assaying has been made. After splitting, drill core is crushed and reduced in volume (8: 1 at 10-mesh, 8: 1 at 70-mesh, 6: 1 at 200-mesh) to supply 25 grams of 200-mesh pulp for replicate analyses. A 0.5 g portion of the pulp 1s used for dissolution and atomic absorption analyses. Factors which initially generated unacceptable data variances have been minimized by planning, repeat analyses, introduction of standards, and routine monitoring. Assuming that error between replicate assays defines a Gaussian distribution with its average ideally equal to zero, precision (from preparation including core splitting and analysis of 8400 pairs of molybdenum samples) is on the order of ± 25%. The error distribution is not based. Accuracy is approximately 4% lower than absolute as determined by replicate assays of commercially prepared samples.

Jan 1, 1984

A list of publications of the United States Bureau of Mines, complete from its establishment to the end of June, 1931, may be had upon request. In addition a monthly leaflet of new publications is issued and is sent to those on the mailing list of the Bureau. Publications are separated into three main divisions: 1. Sales Publications.-Those for which a charge is made. Any orders or remittances in payment for sales publications should be sent directly to the Superintendent of Documents, Government Printing Office, Washington, D. C., and not to the Bureau of Mines. Sales publications are classified into (1) Bulletins, (2) Technical Papers, (3) Economic Papers, (4) statistical reports of the mineral resources of the United States, (5) Monographs, (6) Handbooks, and (7) Schedules. Bulletins and Technical Papers present the results of scientific and technical investigations. Economic Papers are analytical studies of production statistics, sources, resources, .distribution, and industrial flow of mineral commodities. The Annual Report, entitled "Mineral Resources of the United States," includes chapters, published separately, on the production and consumption of metals and of nonmetallic minerals. Monographs give detailed results of extensive cooperative investigations of special

Jan 1, 1933

By D. M. Waldorf

Steam permeability measurements have been made in the laboratory on several samples of natural reservoir materials. The steam temperatures and pressures were selected to simulate conditions which might exist in a reservoir during the injection of steam. For each sample tested, the experimental permeability to superheated steam was comparable to that measured with air and no evidence of plugging was detected. Some samples were exposed to water at various temperatures and plugging was found to occur in materials which contained significant quantities of monmorillonite clay. Temperature had little effect on the degree of plug-ning between 75 and 325 F. The measured pemeabilities tended to increase slightly with temperature, but the changes were small compared with the initial loss of per~neability on wetting. Sequential pemzeability measurements were made on two samples using air, water, steam, water and air, in that order. Both samples were water-sensitive and plugged extensively after the initial injection of water. Upon exposure to superheated steatm the samples dehydrated and their permenbilities to superheated steam were comparable to those initially measured with air. The remaining measuretnetzts with water and air confirmed that the water plugging was reversible and that the samples were not seriorrsly damaged during the tests. INTRODUCTION The swelling of water-sensitive clays during water floods has long been recognized as a potential source of reservoir damage. The recent extensive application of steam injection and stimulation has compounded this problem since both hot water and steam (as well as fresh water at reservoir temperatures) are, at sume time, in contact with the producing zone adjacent to the bore of a steam injection well. The purpose of this paper is to present data which compare the sensitivity of some natural sedimentary rock samples to water at various temperatures, and to super-heated steam. Some properties of montmorillonite clay are briefly reviewed, and comparisons are drawn between empirical data and the predicted behavior of the montmorillonite known to be present in the samples. PROPERTIES OF MONTMORILLONIT E CLAY Water initially adsorbs on dry N a -montmorillonite clay in discrete layers in the interlaminar space between clal platelets. The platelet spacing, which is 9.6 A (angstroms) for a dehydrated clay, has been observed to expand in discrete steps to 12.4, 15.5, 18.4 and 21.4 A spacings, indicating the formation of four discrete layers of regularly oriented water molecules.' The first two layers are easily formed by hydrating a dry sample to equilibrium in an atmosphere with carefully controlled humidity. The formation of the higher layers is more difficult. The usual X-ray diffraction patterns of the more highly hydrated samples indicate a gradual increase in the average spacing betwcen 15.5 and 19.2 A, followed by a discontinuous expansion to 31 A when the weight ratio of water to dry clay is between 0.5 and 1.2.' Platelet expansion above 31 A proceeds monotonically as the moisture is increased and no regular arrangement of the platelets ib observed. Water-sensitivity in sedimentary rocks is usually associated with Na-montmorillonite clay when it is in the noncrystal-line state. Mering3 found that the average lattice spacing of sodium montmorillonite hydrated at 68 F and 70 per cent relative humidity was 15.5 A, and that the spacing, at 92 per cent humidity was 16.5 A. The water adsorbed at the higher humidity has the same free energy as liquid water at 65.6 F. Kolaian and Low' used a tensiometer to measure the thermodynamic properties of water in diffuse suspensions of montmorillonite clays relative to pure water. They observed that water in suspensions as dilute as 6 per cent clay became partially oriented when left undisturbed. The bonding associated with this orientation was not extensive because the free energy difference between the water in suspension and pure water was only a few millicalories per mole. They also found that the measured free energy difference decreased rapidly with temperature and became negligible above 100 F. This evidence indicates that montmorillonites contained in sedimentary rocks would dehydrate to a crystalline structure when exposed to superheated steam, and that the rock permeability measured with steam would be equivalent to that measured with air. The effect of elevated temperatures on the swelline of montmorillonite clays in aqueous suspensions has not been investigated. The Gouy-Chapman diffuse-ion-layer theory has been used to predict the swelling pressure of clay suspensions in dilute salt solutions at room temperature with reasonable success. theory also correctly predicts the direction of the thermal response of Na-mont-morillonite swelling pressures in dilute salt suspensions, 9 Over the temperature range of 33 to 68 F, an increase in

Jan 1, 1966

By W. F. Chiao, R. B. Gordon

Tile sharp-yield point found in magnesium crystals in the solulion-treated and aged condition is studied by dislocation internal-friction experiments. The results show that the sharp yield is not file to the sudden release of pinned dislocations hut is movc likely due to the rapid multiplication of an initially small number of dislocations. Recovery or the dislocation internal friction after deformation is also studied. This yecovery results from the re-pinning of dislocations by a solute, presumably nitrogen, which moves with a relatively small activation energy. SHARP-yield points, when they occur, are a striking feature of the stress-strain curve generated during a tensile test. Although commonly associated with steel, sharp yielding has been found in a variety of metallic and nonmetallic crystalline materials. In particular, sharp-yield points have been found in zinc"' and cadmium3 containing nitrogen. With this background, Geiselman and Guy4 investigated the tensile properties of magnesium single crystals containing nitrogen to see if sharp yielding also occurs in this system. They found that sharp yields did indeed occur in solution-treated and aged specimens tested at elevated temperature but were not able to give conclusive proof that the sharp yield was caused by nitrogen, a yield drop being observed even in their purest crystals. Sharp-yield points have also been found in various polycrystalline magnesium alloys.7'8 In the study of the sharp-yield phenomenon it is desired to observe the behavior of dislocations in the earliest stages of the deformation process. Internal-friction experiments are useful for this purpose because dislocation damping is sensitive to the mobility of free-dislocation segments. At low strain amplitudes the damping, A, due to the the forced vibration of dislocation segments of average length L is ? =KAL4 [1] where A is the dislocation density and K, if the applied frequency is well below the resonant frequency of the dislocation segments? is a constant for the sample under observation.5 Dislocation damping, because of the fourth-power dependence on L, is particularly sensitive to the creation of free-dislocation segments during deformation. Since sharp yielding is associated with the sudden release of pinned-dislocation segments, marked changes in the dislocation damping are expected at the yield point.6 The use of the dislocation-damping observations to help elucidate the incompletely understood mechanism of yielding in magnesium is the primary objective of the experiments reported here. PROCEDURE Many investigations have shown that very marked and rapid changes occur in the dislocation damping of of a deformed material as soon as the straining is stopped.5 It was quite essential, then, for the purpose of this investigation, to make the damping measurements during the deformation of the samples. This can only be accomplished through the use of the ultrasonic-pulse method. In this method traveling sound-wave pulses are used and, in contrast to resonating-bar methods, only the sample ends are set in vibration. Thus, the sample can be gripped along its sides in the tensile-test machine without disturbing the damping measurements. In the pulse method, the decrease in the amplitude of a sound pulse is measured as it travels back and forth through the sample. If A is the amplitude after traversing a distance x and A. is the initial amplitude, A=Aoe-ax [2] and a is called the attenuation. It is commonly measured either in units of cm-I or as db per µ sec. The observed attenuation in a metal sample is due to a number of causes. These include scattering by grain boundaries and impurity particles, thermo-elastic damping, diffraction effects, stress-induced ordering of solute atoms, and dislocation damping. The total observed attenuation in a given sample usually cannot be resolved into these various components, but changes in a due solely to changes in dislocation damping can be accurately determined, provided the experiment is arranged so that all other sources of damping are held constant. It is desired to reduce the extraneous sources of attenuation to a minimum and for this reason the experiments are done on single crystals of high purity. Magnesium crystals offer the further advantage that, when properly oriented, only a single set of slip planes is active during deformation. Crystal Preparation. The method of sample preparation is similar to that of Geiselman and Guy.4 The starting material was high-purity, sublimed magnesium rod supplied by the Dow Chemical Co. Melting under Dow 310 flux was used to reduce the nitrogen content of the starting material: the fluxing was done under an argon atmosphere and the

Jan 1, 1965

By I. H. Warren, E. A. Devuyst

The selective dissolution of pyrolusite (MnO2) in presence of goethite (FeO•OH) in aqueous ammoniacal ammonium carbamate solution has been investigated: various reducing agents were studied, in particular sodium sulfite (Na2SO3,) and hydrazine hydrate (N2H4•H2O). Sodium sulfite was found to be an unsatisfactory reducing agent for both goethite and pyrolusite, for the leaching rate decreased steadily with time to an impractical level because of the limited solubility of the reactions products. Hydrazine hydrate was an effective reducing agent for pyrolusite even at low temperature, whereas goethite required much higher temperatures for any appreciable dissolution. A 1-hr leach at 35°C dissolved 90% of the pyrolusite but only 0.1% of the goethite. An activation energy of 17.0 Kcal per mole was found for the dissolution of pyrolusite with hydrazine. A reaction mechanism for the leaching of pyrolusite with hydrazine is proposed in which a reduction reaction on the surface of the mineral is the rate-determining step. The application of ammonium carbamate to the beneficiation of ilmenite is briefly described.

Jan 1, 1973

By J. Landau, A. Dim, R. Houlihan

Recent developments in the application of solvent extraction in hydrometallurgical processing make it desirable to reassess the present state of availability of suitable equipment for these applications. The range of solvent extraction applications now includes very large scale applications with a modest demand on separation performance (the treatment of some base metals) and applications in which the decisive factor is a very high requirement on separation performance. The extraction column to be described in the present paper is of the type in which mechanical energy is provided for the two- liquid system inside the column. The active elements for this are reciprocating sieve plates designed and mounted so as to uniformly load the driving mechanism, to eliminate vibration of the plant, to have sufficient control over the degree of dispersion of the dispersed phase, and to reduce axial mixing effects, which are highly detrimental to the separation performance of production-scale plant. The operating features of the reciprocating-plate column will be illustrated mainly by experimental results obtained on a 4" diameter column in the extraction of uranyl nitrate with TBP. Some mechanical features of the operation of reciprocating-plate columns will also be discussed.

Jan 1, 1973

By Cyril Wells, Robert F. Mehl

THE two earlier papers in this series1,2 presented data on the rate of diffusion of carbon and of manganese in gamma iron. Apart from their scientific interest, these [] data are needed chiefly in order to treat data on carburization, on the rate of formation of pearlite, and on the rate of austenizing in a quantitative way. 1,2,9,10 In the present investigation rates of diffusion of nickel in -?-Fe over wide temperature and concentration ranges have been determined, and the effects of carbon, of impurities, and of grain size on these rates have been studied. Claussen,3 using the data of Fry,4 has calculated the diffusion coefficient of nickel [ ] in -?-Fe as 9.2 X 10-11 sq. cm. per sec. at 1200T., but had no data from which to calculate the variation of D with concentration, temperature, and percentage of carbon. METHOD AND MATERIALS Method.-Nickel was diffused along the axis of a cylindrical specimen across a concentration gradient, concentration-penetration curves were determined and D values calculated from Grube or Matano solutions.5 Details of the method are given

Jan 1, 1941

By Paul Billingsley

THE mining districts of the first and second order1 of the western United States (and borders) are those named on Fig. 1. These fall into four groups: (1) in the eastern outliers of the Rocky Mountain system; (2) in the Rocky Mountain system itself; (3) in the Great Basin; and (4) in the Sierras and Coast ranges. Of these four groups, the first three are almost entirely of Tertiary age and are within a belt of Tertiary compres-sive folding which we shall call the Rocky Mountain-Great Basin thrust arc. The backbone of this belt is shown by the line BAC. The position of the ore districts in this belt indicates a conformance to linear elements of the continental pattern. These are additional to the peripheral elements emphasized by Butler.2 NATURE OF THE THRUST ARC The thrust arc separates regions of contrasted kinds. To the east of it are flat-lying plateaus interrupted by earlier mountain folds; to the west, sunken basins, in which block-faulted ranges lie like an anchored fleet in a sea of desert wash or lava. The cross-sections are as shown in Fig. 2.

Jan 1, 1933

By John M. Logan, John Handin

Quasi-dynamic triaxial compression tests have been done for the first time at confining pressures to 7 kb. The intermediate strain-rate apparatus employs a gas loading cylinder which allows axial strain rates up to 102/sec on a sample 2 cm in diameter and 4 cm long. Samples can be deformed at confining pressures to 7 kb. Strain gages bonded to the loading piston and to the jacketed specimen allow internal measurements of load and sample strains respectively. Westerly granite has been deformed at confining pressures to 7 kb, room temperature, and axial strain rates of 10-2 to 1/sec. An increase of ultimate strength with confining pressure was found as expected. The ultimate strength was also found to vary directly with increasing strain rate; the rate of rise increases with confining pressure. Brittle deformation has dominated the sample behavior. Solenhofen limestone has been deformed at confining pressures to 3 kb, room temperature, and axial strain rates of 10- to 10/sec. The brittle-ductile transition was found to take place at about 1.5 kb confining pressure at a strain rate of 10/sec.

Jan 1, 1971

Dr. Oldshue has provided a useful summary of a voluminous subject and my task will be to select and direct attention to those areas of mixing theory and practice which are germane to mineral processing in general, and to fine particle treatment in particular. Pulp mixing in impeller actuated reactors occurs in mineral processing in several different applications: (1) emulsification of reagents; (2) mixing pulp with 'reagents as in conditioning for subsequent operations (such as flotation, flocculation or agglomeration) ; (3) high intensity agitation, as in (a) disintegrating and dispersing aggregates, and (b) aggregating particles as in shear flocculation or in selective agglomeration; (4) hydrometallurgy; (5) hydrometallurgy with gas phase (e.g., Arbiter process); . (6) flotation in sub-aeration machines. Attention is invited to 3 above in which two opposite effects can be induced by proper choice of chemical treatment and hydrodynamic conditions. Successful processes for treating mineral fines require excellent aggregate dispersion in order to fully accomplish the liberation stage. Some processes depend further upon selective aggregation following dispersion. The term “dispersion” is often used in different senses which for present purposes will be clarified at the bottom of the next page.

Jan 1, 1979

By H. C. Gatos, J. T. A. Pollock

It is well known that the superconducting critical current densities of many alloy superconductors may be increased by cold working and in some cases further enhanced by a short heat treatment. This latter enhancement has been attributed to the redistribution of dislocations into cell-like networks' and to the precipitation of second phase particles,2'3 which act as flux pinning centers. In a manner analogous to dislocation pinning in precipitation hardening alloys,4 it is expected that here also a critical distribution of the pinning centers should result in maximum pinning effect. Concentration inhomogeneities exist in most or all commercial alloys yet there have been only a few attempts made to determine their effect on critical current capacity in the absence of cold working. Sutton and Baker,5 and Kramer and Rhodes6 have found that the complex precipitation processes occurring during the aging of Ti-Nb alloys can result in critical current density enhancement. Livingston7-10 has clearly shown, for lead and indium based alloys, that the distribution of precipitated second phase particles is of critical importance in determining magnetization characteristics. However, these '(soft" alloys age at room temperature and the time involved in specimen preparation prevents metallographic examination in the state in which the superconducting measurements are made. Thus results with such alloys are expected to be biased towards larger precipitates and interpar-ticle spacing. The present study of Ta-Zr alloys was undertaken to examine the influence of second phase precipitation, as controlled by heat treatment, on the critical current capacity of well annealed polycrystalline material. A study of the published phase diagram11 indicated that annealing supersaturated samples containing up to 9 at. pct Zr at suitable temperatures would result in the precipitation of a zirconium-rich second phase. It was MATERIALS AND PROCEDURE The alloys were prepared from spectrochemically pure tantalum and zirconium. Analysis was carried out by the supplier. Major impurities in the tantalum were: 12 pprn of 02, 17 pprn of N2, 19 pprn of C, and less than 10 ppm each of Mo, Nb, Al, Cr, Ni, Si, Ti. The crystal bar zirconium was pure except for the following concentrations: 15 pprn of 02, 17 ppm of C, 23 ppm of Fe, 11 ppm of Cu, and less than 10 pprn each of Al, Ca, N2, Ti, and Sn. Samples were prepared in the form of 8 to 10 g but-tons by arc melting using a nonconsumable electrode on a water-cooled copper hearth in a high purity ar-gon atmosphere. Each button was inverted and re-melted three times to ensure an even distribution of the component elements. The samples were then homogenized at temperatures close to their melting points for 3 days in a vacuum furnace maintained at 5 x 10-7 mm Hg. After this treatment the buttons were cold rolled to sheets approximately 0.020 in. thick from which specimens were cut, 0.040 in, wide and 1 in. long suitable for critical current density (J,) and critical temperature (T,) measurements. These strips were then recrystallized and further grain growth was allowed by an additional vacuum heat treatment at 1800°C for 60 hr. Some second phase precipitation occurred during cooling of the furnace and a solution treatment was necessary to produce single phase supersaturated samples. This treatment was successfully carried out by sealing the samples together with some zirconium chips in quartz tubes under a vacuum of 5 x 10-7 mm Hg, heating at 1000°C for 5 hr and then quenching into water or liquid nitrogen. The samples were then heat treated at either 350" or 550°C and quenched into water or liquid nitrogen. All samples which were heat treated at 350°C were quenched in both cases by cracking the capsules in liquid nitrogen. The samples treated at 550°C were quenched by dropping the capsules into water. Analysis for oxygen in randomly selected samples indicated that the oxygen content was in the range of 175 to 225 ppm. Values of Tc were determined by employing a self-inductance technique. Jc measurements were made at 4.2oK by increasing the direct current through the wire in a perpendicularly applied field until a voltage of 1 pv was detected with a null meter. The risk of resistive heating at the soldered joints during these latter measurements was reduced by first plating the ends of the wires with indium and then soldering to the copper current leads using tin. Metallographic examinations were performed after mechanical polishing of the same samples and etching in a 4H20:3HN03 (conc):lHF(conc) solution.

Jan 1, 1970

By Eckhard Nembach

The phase diagram of the system Pb-In has been investigated between -27° and + 40°C, using nzainly X-ray dijfraction. In accordance with t her mo dynamic measurements by Heumann and Predel, a segregation occurs at low temperatures, though not in the form of a nziscibility gap. THE phase diagram of the system Pb-In has been the subject of extensive investigations,1&apos;1 but recently Heumann and prede13 concluded from their thermodynamic data that a new feature should occur below room temperature. These authors observed that the maximum values for the enthalpy and entropy of mixing, which occurred at a composition of 50 at. pct Pb, were +400 and —1.7 cal per g-atom deg, respectively. From this the authors estimated that a miscibility gap should occur below 30°C, centered at 50 at. pct Pb. Resistivity measurements seemed to support this view. These authors proposed the phase diagram outlined in Fig. 1. Three phases exist at 30°C: the tetragonal indium phase with c/a > 1, the tetragonal intermediate phase a, with c/a < 1, and the fcc lead phase. During an investigation of the superconducting properties of Pb-In alloys. it has been observed4 that aging a specimen with 50 at. pct Pb for 14 days at -18°C decreased the superconducting transition temperature about 0.13"K and tripled the transition width. In this paper, the results of an investigation of the Pb-In phase diagram in the temperature range from — 2T to +40°C are reported. Superconductivity and X-ray methods have been used. 1) SPECIMEN PREPARATION The materials were provided by the American Smelting and Refining Co. According to the manufacturer their purity was 99.999 pct. The weighed amounts of the constituents were sealed in quartz tubes under an atmosphere of 10 torr helium, mixed for 24 hr in a rocking furnace at 380°C, quenched in ice water, and homogenized at 20" to 30°C below the solidus line, established by Heumann and Predel. The annealing times were 144 hr for specimens containing Less than 30 at. pct Pb and 36 hr for the remainder. 2) SUPERCONDUCTIVITY EXPERIMENTS The specimens were quenched from the homogeniza-tion treatment into ice water and their superconducting transition temperatures T, measured. The procedure used has been described in Ref. 4. The transition was detected by the change of the mutual induc- tance of two coaxial coils containing the sample. T, was defined as the temperature at which 50 pct of the total change in inductance had occurred. The repro-ducibility with which T, could be measured was i0.002"K. Then the specimens with lead contents between 38 and 75 at. pct were aged for 7 days at temperatures between -30" and 40°C. If this treatment caused T, to change by more than 0.005"K or the width of the transition to increase by more than 0.002"K, it was concluded that the specimen had undergone a phase change and no longer consisted only of the fcc lead phase: as it did immediately after homogenizing. The result is shown in Fig. 2. From this one can estimate at what temperatures and concentrations phase changes occur. The X-ray measurements were based on these preliminary results. 3) X-RAY EXPERIMENTS Because of the softness of the material, relatively coarse powders. 75 p, had to be used, which were filed in a helium atmosphere from homogenized specimens. The powders were annealed at least 30 min at temperatures between 120" and 16OJC, depending on their concentration, and quenched in ice water. Then their X-ray patterns were taken at -178°C with a Picker diffractometer, model 3488K, and a cold stage. on which the specimen was in thermal contact with a liquid-nitrogen reservoir. In this way the following relation was established for the fcc lead phase: a = 4.697 + 0.00247C for 40 5 C 5 75 11 where n is the lattice constant (A) and C is the at. pct of lead. The coarseness of the powder made it impossible to use lines with 0 > 75 deg; therefore n was averaged from lines with 45 deg 5 0 5 75 deg. The results were reproducible to within i0.05 pct. Relation [I] is very similar to the one found by Heumann and Predel at room temperature. Following this, homogenized specimens with compositions between 15 and 56 at. pct Pb were aged for at least 10 days at temperatures between -27" and

Jan 1, 1970

By Charles Catlett

Much has been done of late years to facilitate preliminary stratigraphical investigations, and for examination at considerable depths and in a certain character of material the diamonddrill, in its general forms, certainly stands pre-eminent among the tools for such work. But there are large classes of deposits —indeed, I may say the larger proportion in which ordinary. prospecting is done—which lie near the surface and are interbedded with soft and fine material. The method usually employed for prospecting these is by means of small shafts. These are sunk with considerable slowness and at considerable expense, depending largely upon the character of the material encountered, and are greatly interfered with by water. In this region the smallest are 3 by 4 feet, but they are usually considerably larger. Having had occasion during the past year to do a large amount of prospecting work, I have found the use of a hand-auger and drill of immense value in this respect, and in my practice it has largely superseded, and always preceded, the other forms of investigation. I believe that the information desired mas

Jan 1, 1898

By P. N. Richards, M. K. Ormay

The present Paper extends the previous work on cold reduced, low carbon steels to preferred orientations developed after various heat treatments. In recrystal-lized rimmed steel, cube-on-comer orientations increased with cold reductions up to 80 pct. Above that {111}<112> and a partial fiber texture with (1,6,11) in the rolling direction dominated. During grain growth, cube-on-corner orientations have been observed to grow at the expense of {210}<00l>. In re-crystallized Si-Fe (111) (112) and cube-on-edge type orientations are dominant near the surface and the (1,6,11) texture near the midplane for reductions up to 60 pct. With larger reductions {111)}<112> and the (1,6,11) texture are dominant. In cross rolled capped steel a relationship of 30 deg rotation was observed between the (100)[011] of the rolling texture and the main orientations after re crystallization. Most orientations present in recrystallized specimens can be related to components of the rolling texture by one of the following rotations: a) 25 to 35 deg about a (110) b) 55 deg about a (110) C) 30 deg about a (Ill) THE orientation texture of recrystallized steel is of interest where the product is to be deep drawn, because preferred orientation is related to anisotropy of mechanical properties such as the plastic strain ratio (r value);1,2 and in electrical steel applications where a high concentration of [loo] directions in the plane of the sheet improves the magnetic properties of the material. It is interesting to note that both these aims are to a large extent achieved commercially, even though the orientation texture of cold rolled steel does not show large variation3 and the recrystallized orientations are generally given as being related to the as rolled orientations mostly by 25 to 35 deg rotations about common (110) directions.4-6 There is, as yet, no single completely accepted theory on recrystallization. The three mechanisms that have been investigated and discussed are: a) Oriented growth b) Oriented nucleation c) Oriented nucleation, selective growth Largely from the observations of the recrystalliza-tion process by means of the electron microscope,7-11 there is now considerable evidence that the "nucleus" of the recrystallized grain is produced by the coalescence of a few subgrains to form a larger composite subgrain, which finally grows by high angle boundary migration into the deformed matrix. From the intensive work on the recrystallization of rolled single crystals of iron, Fe-A1 and Fe-Si al-loys4-" he following observations have been made: 1) The change in orientation during primary recrys-tallization can usually be described as a rotation of 25 to 36 deg about one of the (110) directions. 2) The (110) axes of rotation often coincide with poles of active (110) slip planes. 3) If several orientations are present in the cold rolled structure, the (110) axis of rotation will preferably be a (110) direction that is common to two or more of the orientations. 4) With larger amounts of cold reduction (70 pct or more) departure from these observations became more frequent. 5) After larger cold reductions, rotations on re-crystallization about (111) and (100) directions have been observed. K. Detert12 infers that a rotation relationship of 55 deg about (110) directions is also possible, by stating that the recrystallized orientation {111}<112> can form from the orientation {100}<011> of cold reduced partial fiber texture A.3 The observation by Michalak and schoone13 that (lll)[l10] formed during recrys-tallization in fully killed steel containing (111)[112],— as well as (001)[ 110] which is related to the {111}<011> by a 55 deg rotation about <110>-implies a possible 30 deg rotation relationship about the common [Ill]. Heyer, McCabe, and Elias14 have recrystallized rimmed steel after various amounts of cold reduction, by a rapid and by a slow heating cycle and found that the preferred orientations strengthened with increased cold reduction. The most pronounced orientation up to about 70 pct cold reduction was found to be {1 11}< 110>, after 80 pct cold reduction both {111}<110> and {111}<112>, after 85 and 90 pct cold reduction, {111}<112>, and after 97.5 pct cold reduction it was {111}<112> and (100)(012). In the present work, the orientation textures of the recrystallized specimens are examined under various conditions of steel composition, amount and method of cold reduction, and method of recrystallization. The relationships between the preferred orientations of the as rolled and recrystallized specimens, and the conditions for the formation of the various orientations during recrystallization are investigated.

Jan 1, 1970

By F. C. Langenberg, J. Chipman

New data on the distribution of silicon between slag and carbon-saturated iron at 1600oand 1700oC are presented which, in combination with previously published data, permit the determination of silica activities over a broad range of compositions in the CaO-Al2O3-SiO2 system. The distribution of silicon between graphite-saturated Fe-Si-C alloys and blast furnace-type slags in equilibrium with CO has been described in previous publications.1"3 In this past work the silica-silicon relation was established at temperatures of 1425" to 1700°C for slags containing up to 20 pct Al2O3. This paper presents the results of additional studies at 1600" and 1700° C which extend the silicon distribution data at these temperatures for CaO-A1203-SiO2 slags over a range from zero pct A12O3 to saturation with A12O3, or CaO.2A12O3. The upper limit of SiO, is set by the occurrence of Sic as a stable phase when the metal contains 23.0 or 23.7 pct Si at 1600" or 1700°C, respectively. The activity of silica over the expanded range is determined directly from the distribution data.3 Recently, 4-7 other investigators have studied the activities of SiO, and CaO, principally in the binary system, using different methods and obtaining somewhat different results. EXPERIMENTAL STUDY The experimental apparatus and procedure have been fully described in previous publications.1, 3 Six new series of experimental heats have been made, four at 1600° and two at 1700°C. Master slags of several fixed CaO/A12O3 ratios were pre-melted in graphite crucibles, and these were used with additions of silica to prepare the initial slag for each experiment. Slag and metal were stirred at 100 rpm and CO was passed through the furnace at 150 cc per min. The initial sample was taken 1 hr after addition of slag at 1600°C or 1/2 hr after addition at 1700°C. The run was normally continued for 8 hr at 1600°C or 7 hr at 1700°C, and the final sample was taken at the end of this period. Changes in Si and SiO2 content indicate the direction of approach to equilibrium, and in a series of runs where the approach is from both sides this permits approximate location of the equilibrium line. Fig. 1 shows the results of such a series of 15 runs at 1600°C for slags of CaO/Al2O3 = 1.50 by weight. Figs. 2 and 3 record other series at 1600°C and Fig. 5 a series at 1700°C with fixed CaO/Al2O3 ratios. The results of the experiments at 162003°C have been reported in part in a preliminary note.3 In the experiments recorded in Figs. 4 and 6, the slags were saturated with A12O3 (or with CaO.2A12O3 within its field of stability) by suspending a pure alumina tube in the melt during the course of the run. The final slag analyses were used to establish the liquidus boundaries8 in the stability fields of CaO.2Al,O3 and of A120,. ACTIVITY OF SILICA The free-energy change in the reaction has been calculated by Fulton and chipman2 from recent and trustworthy data including heats of formation, entropies, and heat capacities. The more recent determination by Olette of the high-temperature enthalpy of liquid silicon is in satisfactory agreement with the values used and therefore requires no revision of the result which is expressed in the equation: SiO, (crist) + 2C (graph) = Si + 2CO(g.) [1] &F° = + 161,500 - 87.4T The standard state for silica is taken as pure cristobalite and that of Si as the pure liquid metal. Since the melts were made under 1 atm of CO and were graphite-saturated, the equilibrium constant for Eq. [I] reduces to K1 = asi /asio2 The value of this constant is 1.77 at 1600°C and 16.2 at 1700°C. Through K1, the activity of silica in the slag is directly related to the activity of silicon in the equilibrium metal.

Jan 1, 1960

By J. O. Betterton, D. S. Easton

A detailed investigation was made of the phase diagram of silver-zirconium, particularly in the region 0 to 36 at. pct Ag. The system was found to be characterized by two intermediate phases Zr2Ag and ZrAg and a eutectoid reaction in which the -zirconium solid solution decomposes into a-zirconium and Zr2Ag. It was found that impurities in the range 0.05 pct from the iodide-type zirconium were sufficient to introduce deviations from binary behavior, and that with partial removal of these impurities an increase in the a-phase solid solubility limit from 0.1 to 1.1 at. pct Ag was observed. The phase diagram of the silver-zirconium system is of interest as an example of alloying a transition metal from the left side of the Periodic Table with a Group IB element. Silver would normally act as a univalent metal, its filled 4d-shell remaining undisturbed during the alloying. However, there is a possibility that some of the 4d electrons might transfer to the zirconium. An insight into such a question can occasionally be obtained by comparison of phase diagrams. The silver-zirconium system forms part of a more complete review of various solutes in zirconium in which these valency effects were studied.&apos; Earlier work on the silver-zirconium system was done by Raub and Enge1,2 who investigated the silver-rich alloys. After the start of the present experhents, work on this system was reported by Kemper3 and by Karlsson4 which for the most part agrees with the phase diagram presented here. EXPERIMENTAL PROCEDURE The alloys were prepared by arc casting on a water-cooled, copper hearth with a tungsten electrode and in a pure argon atmosphere. Uniform solute composition was attained by multiple melting on alternate sides of the same ingot. Progressive improvements in the vacuum conditions inside the apparatus during the course of the experiments reduced the Vickers hardness increase of the pure zirconium control ingot from 10 to 20 points, observed initially, to negligible amounts at the end of the experiments. Such hardness changes in zirconium are a well known indication of purity. For example, -01 wt pct additions of oxygen, nitrogen, and carbon increase hardness by 6, 10, and 3 VPN respectively. &apos;9&apos; Further verification that the final casting technique did not add a significant quantity of impurities was obtained when pure zirconium was arc cast and then isothermally annealed in the vicinity of the allotropic transition. The transition was always observed to take place over the same temperature range as in the original crystal bar. The alloy ingots were annealed in sealed silica capsules for times and temperatures which varied between 1 day at 1300°C and 60 days at 700°C. The best method found to prevent the reaction of the zirconium with the silica was foil wrapping of molybdenum or tantalum. With this method, samples of pure zirconium were found to be unchanged in hardness after annealing for 3 days at 1200°C. In most of the experiments the protection of these foils was supplemented by an additional layer of zirconium foil inside the molybdenum or tantalum foil. The alloys, foil, and the capsule were outgassed at pressures in the range 10 to l0-7mm Hg in the temperature range 800" to 1100°C before each anneal in order to remove hydrogen and other impurities, and to provide a suitable container for the high purity, inert atmosphere, which is essential in the annealing of zirconium. The temperature measurements were made with Pt/Pt + 10 pct Rh thermocouples calibrated frequently during the experiments against the melting points of zinc, aluminum, silver, gold, and palladium. For the longer anneals the sum of various temperature errors was generally well within ± 2°C. For short-time anneals and during thermal analysis the overall temperature error is considered to be within ± 0.5°C. The compositions of the alloys from the quenching experiments were determined by chemical analysis at Johnson Matthey and Company, Ltd., under the direction of Mr. F. M. Lever. The actual metallo-graphic samples were individually analyzed in every case, and prior to the analyses two or more sides of each specimen were examined to insure that the specimen was not segregated. The sum of the solute and solvent analyses was in each case within the range 99.9 to 100.1 pct. In the course of the experiments, minor impurities in the range 0 to 500 ppm were found to have significant effects on the zirconium-rich portion of the phase diagram. Similar effects had been encountered previously in other zirconium phase-

Jan 1, 1959

By I. Stapf

Systematic investigations on silver-rare earth metal systems have been extended on the Ag-Ce system in order to clarify the discrepancies reported in literature. The phase diagram has been reinvestigated on the base of thermal analyses and of microstructure examination on cast and annealed specimen. All intermetallic phases Ag4Ce, Ag3Ce, Ag2Ce and AgCe show no extended range of homogeneity, they melt congruently fm), or decompose peritectically (d) at 815 °C (d), 1030 °C (m), 855 °C (d) and 855 °C (m), respectively. The system shows eutectics at 793 °C/10 at.%, 780 °C/42 at.%, and about 505 °C/81 at.% Ce. d-Ce dissolves up to 2 at .% Ag and decomposes metatectically at 710 °C. Furthermore, the phase transformation of the intermetallics would be clarified. The phases Ag5Ce and Ag51Ce14 reported in literature could not be verified.

Jan 1, 1984