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By B. A. Cheadle, K. P. Steward

Axial tensile, ring tensile, closed end burst, and free end burst tests were done at room tempe.vature and 300°C on three batches of Zircaloy-2 sheathing zuith different textures. Knoop hardness tests were also done on all batches. The mechanical properties of the tubes were largely dependent on the percentages of cold work, but were also markedly affected by the textures, particularly with respect to deformation behavio'r. The deformation behavior observed confirmed Picklesimer's predictions, zuhereas Knoop hardness results could be correlated with texture and yield strength anisotropy after the ,method of Wheeler and Ireland. From the mechanical properties, and from efjectiue strain values deterrlzined at the fractures using a photoqid technique, it zuas concluded that tubing witlz a single preferred orientation of radial basal poles best combines strength and ductility for any given deqee of cold work. THE mechanical properties required in collapsible Zircaloy-2 fuel sheathing for water-cooled power reactors are strength to resist wrinkling deformation by coolant pressure and ductility to accommodate a small amount of deformation in service without rupturing. Zircaloy-2 tubing during fabrication develops pre- ferred orientations of the a Zr grains due to aniso-tropic deformation behavior, and these textures markedly affect mechanical properties. Picklesimer' had predicted the deformation behavior of tubes with various textures, but the texture required to provide the optimum strength and ductility for a given degree of cold work has not been reported. To investigate this problem, tests at three transverse to axial stress ratios were done at room temperature and 300°C on three batches of Zircaloy-2 tubing covering a wide range of textures and percentages of residual cold work. Knoop hardness values were also measured to correlate with preferred orientation and yield strength anisotropy after the method of Wheeler and relland.' 1) MATERIAL For this investigation, three batches of tube-reduced tubing were chosen from the Zircaloy-2 sheathing produced for the Douglas Point Reactor. Individual tubes were 191/2 in. long, 0.600 in. OD, and 0.0165 in. nominal wall thickness. The identities of the batches, together with their textures, are shown in Table I. The tubes had the normal Zircaloy-2 composition3 of 1.5 wt pct Sn, 0.3 wt pct Fe, Ni, Cr combined with the following oxygen concentrations: Batch VII 1140 to 1390 ppm 0 Batch VIII 1400 to 1750 ppm 0 Batch IX 880 to 1320 ppm 0

Jan 1, 1968

By J. T. Richards

ELASTIC constants, including E-modulus, G-modulus, Poisson's ratio, and compressibility, are affected by temperature, but not necessarily to the same degree nor in the same direction. Theoretical expressions relating the temperature coefficients for the various elastic constants have been introduced by Gruneisen. In considering the thermoelastic characteristics

Jan 1, 1955

By R. S. Rickard, H. D. Peterson, J. D. Miller, M. C. Fuerstenan

Pure chrysocolla is floated with chelating agents that form insoluble complexes with copper at ambient temperature. Complete flotation is obtained with potassium octyl hydroxamate as collector at pH 6. Flotation response is enhanced with increased temperature when low additions of hydroxamate are involved. A natural ore was floated with 0.4 1b per ton octyl hydroxamate at pH 6.5 and 58°C, and a flotation recovery of 76% was obtained with a concentrate grade of 31.6% copper. The flotation characteristics of the oxide copper minerals, malachite, azurite, and cuprite, have not presented the difficulty for concentration as have those of the copper silicate, chrysocolla. The copper carbonates and oxides respond reasonably well to flotation with conventional collectors, whereas chrysocolla will not respond to flotation with fatty acids or xanthates under normal flotation conditions. In this view then, other reagents will have to be devised to function as collectors for chrysocolla. The most obvious general class of reagents for this purpose would seem to be the organic copper chelating compounds. The utility of chelating agents as collectors in flotation systems has already been demonstrated. For example Vivian1 has floated cassiterite using ammonium nitrosophenylhydroxylamine. Holman2 studied the flotation of nickel oxide ores with dimethylglyoxime and also suggested the use of taurine on oxidized lead ores. A rather detailed study on the application of certain chelating agents to some flotation systems was presented by Gutzeit.3 This work indicated that the formation of surface insoluble chelates is probably responsible for flotation in many cases. The role that soluble chelating agents assume was also presented, that is with effective removal of polyvalent cations by complex formation, effective depression of quartz can be obtained. DeWitt and Batchelder4,5 have shown that oximes function well as collectors for chalcocite, malachite, azurite, and cuprite. Ludt and DeWitt6 have presented the possibility of using dyes, such as octyl malachite green, as a collector for chrysocolla. These works presented by DeWitt et al suggest that organic copper chelating compounds offer considerable promise for concentrating chrysocolla, but that the most suitable chelating reagent from the standpoint of cost and flotation response has yet to be determined. The present investigation was undertaken to study the flotation response of chrysocolla to selected copper chelating compounds, that is ethylenediamine, hexamethylenetetramine, potassium octyl hydroxamate, dimethylglyoxime, and benzoin a-oxime. EXPERIMENTAL MATERIALS Chrysocolla: The chrysocolla used in the microflo-tation studies was from New Mexico and analyzed 20.8% copper. X-ray diffraction showed this material to be amorphous in character, but some faint lines of quartz were noted. A natural oxide copper ore from Utah was also used in the investigation. This ore contains malachite principally but also contains chrysocolla and tenorite together with some sulfide copper. The sulfide copper comprises from 15 to 20% of the total copper content of the ore. Water: Conductivity water was used in the microflo-tation experiments, while Golden tap water was used in the experiments with the natural ore. Reagents: Reagent grade n-amyl alcohol was used as frother in the experiments with pure mineral, while MIBC was used in the work with the ore. Ethylenediamine, hexamethylenetetramine, dimethylglyoxime and benzoin a-oxime were reagent grade in quality. Pure potassium octyl hydroxamate was prepared as follows: 1) 1.0 mole of KOH in 140 cc of methanol was combined with 0.6 mole of hydroxyl-amine hydrochloride in 240 cc of methanol at 40°C (KC1 precipitates under these conditions and to effect complete removal of KCl, the system was cooled to 10°C and filtered), 2) a light methanol wash was then given the KC1 cake, 3) the filtrate was agitated at room temperature and 0.33 mole of the methyl ester of the organic acid (i.e. methyl octanoate) was

Jan 1, 1965

By W. W. Dudley

Inflow of ground water is an important engineering and safety consideration during construction of large openings underground. The initial step in predicting groundwater inflow involves hydraulic tests in exploratory drill holes. Zones within the area of interest are isolated in the drill hole by inflatable packers and are tested by measuring the water level responses to applied hydraulic stresses. These responses may then be translated into significant hydraulic characteristics of the tested rocks such as transmissivity, hydraulic conductivity, hydraulic potential, and storage coefficient by using a type-curve solution. Once the geometry and necessary hydraulic characteristics have been determined for the rock in the vicinity of the proposed opening, a model can be developed using certain assumptions that will lend itself to treatment with available mathematical methods. The mathematical method applied to the model considers conditions of partial penetration and nonsteady-state, leakyartesian, constant-drawdown discharge of ground water. A type-curve solution results in a curve that gives the variation of discharge (inflow) with time. This technique of predicting ground-water inflow has been used in planning construction of cylindrical chambers for use in underground nuclear experiments by the U.S. Atomic Energy Commission. These chambers have been constructed in low-permeability rocks at depths as much as 6000 ft and under hydraulic heads of thousands of feet.

Jan 1, 1973

By E. L. Ickes

DURing the summer and winter of 1918 eleven standard rigs were erected in the United Kingdom to test the petroleum prospects of- ten structures, eight of which were in England and two in Scotland. By the fall of 1921 ten of the wells were completed; the remaining one, the D'Arcy in Scotland, was stopped some months later. The tests were deep ones, five of the wells being 4000 ft. or more, the rest varying in depth between 1810 and 3918 ft. The total footage drilled was 40,047 ft. The holes were put down with standard or cable tools purchased in the United States (except the boilers). The larger sizes of casing, 10-in. and above, were also from America, while the smaller sizes were secured in Scotland. The Hardstoft well in England found a small production of high-grade oil and the D'Arcy well also encountered what is reported as a favorable showing at a depth of 1810 ft. The Werrington and West Calder wells had to be abandoned on account of drilling difficulties. The Apedale well encountered great thicknesses of ash in the Carboniferous and had to be abandoned on account of depth. The results might be summarized by saying that of the ten structures drilled upon, two yielded encouraging showings; three cannot be considered as having been adequately tested; and five produced dry holes, although in some of these small oil showings and gas were met. The total cost of the work amounted to about half a million pounds sterling, which sum includes the cost of all equipment, subsequently sold by the government. The work, under the superintendence of V. L. Conaghan, took place for the most part in the period immediately following the war—a period of high prices, labor and transportation difficulties, and unsettled conditions generally; factors tending to retard the work and affect the costs. The writer, as a member of the staff of S. Pearson & Son, Ltd., had charge of the administration of the work during its later stages and

Jan 1, 1924

By D. W. Jessup

ONLY during the past few years, have the old-fashioned methods for treating ores and byproducts progressed to any marked degree. The advent of multiple-hearth roasting, blast roasting, the baghouse, and the Cottrell plant indicate this change. It is the ability to roast and smelt sulfide ores and concentrates that gave this later advance. Further investigations that will solve the problem of efficient handling of flotation concentrates and their attendant ills are of the utmost importance. With future developments, the metallurgist will be able to smelt more economically and to treat still more refractory ores, making the early methods appear small by comparison. GROWTH OF SMELTING Well within the memory of pioneer smeltermen, the ore was charged directly into the blast furnace as it came from the mine;, only the richer, ores were smelted, the lower grade and sulfide ores were undesirable. Matte was, at first, thrown away and only two products) were desired-slag and lead bullion. Scores of the early smelting companies failed because of improper reduction of ores, high costs, short- furnace campaigns, inability to treat sulfide ores, and ores containing-zinc. With the failure of weaker companies, consolidation eliminated many others, until today the field is dominated by a comparatively few organizations, each strong financially. Formerly, a few thousand dollars would erect a small plant, whereas the modern smelter costs over a million dollars. Ore and products to which formerly no attention was paid are now treated with comparative ease and at a good profit. Mechanical improvements have modernized smelting, furnace tonnages show an increase, and metal recoveries have made enormous strides. Even though costs have decreased, they have not dropped in proportion to the improvements, because of the higher wages, greater costs of fluxes and coke, more undesirable ores smelted, etc.

Jan 8, 1925

By R. T. C. Rasmussen, L. H. Banning, W. E. Anable

In the rapidly growing industry of elemental-phosphorus production from western phosphates, most of the vanadium and chromium contained in the phosphate rock collect in the byproduct ferro-phosphorus. Results are presented of a completed laboratory project, which developed a tristage crystallization and hydrolysis process for recovering strategic vanadium and chromium, as well as a valuable phosphorus product, after extracting these elements from the ferro-phosphorus by roasting and leaching. THE Phosphoria formation in Idaho, Montana, Wyoming, and Utah contains the Nation's largest reserve of phosphate rock. A unique feature of the Phosphoria beds is their content of a fraction of a percentage each of vanadium, chromium, nickel, and molybdenum. Vanadium is the most important as to quantity and value. Small-scale tests by the Bureau of Mines at Albany, Oregon, in 1947, indicated that most of the vanadium in the phosphate rock collects in the ferrophosphorus product of smelting. Subsequent electric smelting operations to produce elemental phosphorus from western phosphate rock (experimentally by TVA and industrially at Pocatello, Idaho) have shown that the vanadium and other metals in the rock are to a large extent recovered in concentrated form in the ferrophosphorus byproduct. This paper reports the results of completed laboratory research on the recovery of vanadium from ferrophosphorus, which was undertaken by the Bureau of Mines at Albany in 1948 as the first phase of a project entitled, "Vanadium and Fluorine from Western Phosphates." The various vanadium-recovery methods investigated, including the roast-leach method that showed most promise and was studied in greatest detail, are discussed in an earlier publication.' Subsequent systematic study of the roast-leach method of extracting vanadium from western ferrophosphorus developed the more effi- cient tristage crystallization process, which is the subject of this paper. Process Development The investigations were made on ferrophosphorus produced in the electric smelting of elemental phosphorus from western phosphate rock. The TVA provided two sample lots of ferrophosphorus produced in pilot plant smelting of phosphatic shale from the Fort Hall Indian Reservation in Idaho. The Westvaco Chemical Div. of the Food Machinery & Chemical Corp. supplied two sample lots of ferrophosphorus produced by its phosphorus smelter at Pocatello, Idaho. The analyses of all four lots are shown in Table I. Westvaco lot B was the starting material for the more recent tests. The roast-leach process for recovering vanadium from western ferrophosphorus, as originally developed, employed the following principal steps: Roasting of a mixture of pulverized ferrophosphorus, soda ash, and salt; extraction of the water-soluble vanadium, phosphorus, and chromium compounds from the calcine by leaching, settling, and decanta-tion of the pregnant solution; primary crystallization of trisodium phosphate from the pregnant solution; purification of the trisodium phosphate crystals by dissolution in water and secondary crystallization; purification of the pregnant vanadium solution from the primary crystallization step by adding calcium chloride to precipitate calcium phosphate; and hydrolysis of vanadium red cake from the puri-

Jan 1, 1954

By M. E. Kukura, L. G. Stevens

As described in a previous presentation and in various patents, the Minerals Sciences Div. of UOP, Inc., has developed a modified reduction roast ammonia leach process for nickel laterites. This process gave considerable improvement in extraction over the conventional Caron approach as practiced in Cuba, Australia, and the Philippines. This greatly improved response was obtained with a wide variety of ores. This paper describes the pilot plant flowsheet and reviews the design features unique to the UOP process. Operating results from pilot plant campaigns are compared with bench scale results. Operating problems and their solutions are also discussed.

Jan 1, 1976

By V. Rajaram, I. P. Nielsen, H. D. Raymond

The Parachute Creek member of the Green River formation in the Piceance Basin, Colorado, contains vast reserves of oil shale, nahcolite, dawsonite, and other accessory minerals. The dry alkali process of sulfur dioxide removal using nahcolite (naturally occurring sodium bicarbonate) has great potential A room and pillar mining scheme has been designed to extract a nahcolite zone occurring at a depth of 472 m, from the lease application area of the Yankee Gulch joint venture. Geotechnical parameters affecting mine design will be discussed. A preliminary development plan for mining at the rate of 1000 t/d will be described in detail.

Jan 1, 1980

By Georges Caraghiaur

INTRODUCTION A small, independent mining enterprise (SIME) is an independently owned and operated business concern engaged primarily in mineral development, from the exploration to the production stage. A SIME may or may not be listed on stock exchanges. By definition, a SIME is not dominant in its field and has no long-term financial backing. As such, it is not a major producer of minerals, nor is it a petroleum company, a government organization or a subsidiary of such organizations. The survival and growth of a SIME is most often controlled by an independently minded entrepreneur, who not only conceives and carries out new projects, but is materially affected by the success or failure of these projects. Usually, a SIME does not have a large or constant cash flow. Such a lack of long-term financial backing forces the SIME to meet the challenge of finding capital for its activities on a step-by-step basis. Its survival strategy is thus based on finding funds at the right time, of the right type and in the right quantities. The purpose of this paper is to show that the type of venture in which a SIME is involved affects the difficulty of raising new capital and the choice of possible sources of funds. The Small, Independent Mining Enterprise The SIME, also called small miner, junior mining company, speculative mining company, and pennystock mining company, is not a figment of the imagination of financial speculators. In Canada, there are more than 1,800 small mineral enterprises which spend on the average less than $1,000,000 per year on activity which is directed at bringing forth new mineral supply. In the United States, 64 percent of the non-fuel mining operations are conducted by nine or fewer men, and the coal industry is characterized by several thousand smaller independent producers, still predominantly family-owned or controlled. In Chile, 80 percent of the mines can be classified as small mines. In the Philipines, approximately 60 percent of metal mining operations are classified as small mines. The SIME is actively engaged in mining all over the world, and very much so in the Pacific Rim. The Mineral Supply Process The whole process of bringing forth new mineral supply involves a dynamic sequence of activities, ranging from the initial exploration for a mineral occurrence to the production of a marketable product. A typical sequence is outlined in Figure 1. At the grass-roots exploration stage, a series of geological, geophysical and geochemical tests is aimed at locating a mineral occurrence. Especially in the early phases of such activities, the uncertainty (risk) surrounding a venture is high, since only general geological information exists on which to base a judgement of the economic viability of the venture. Such risk is attractive to few investors.

Jan 1, 1982

By Richard J. Fruehan

ThE thermodynamic activities of nickel and chromium in liquid Ni-Cr alloys have not been previously reported. There have been several investigations on the solid alloys.1-3 In the present investigation the activity of chromium in liquid Ni-Cr alloys at 1600° C was determined by the use of the following galvanic cell, The use of galvanic cells employing solid oxide electrolytes for determining the activity of metals in solid alloys was first demonstrated by Rapp and Maak4 on Cu-Ni alloys between 700° and 1000°C. Recently Schwerdtfeger5 tested the performance of the ZrO2(CaO) electrolyte at 1600°C and found it satisfactory for oxygen pressures as low as 10"12 atm. He also demonstrated the use of solid oxide electrolytes for determining the activities in liquid metal systems in measuring the activity of manganese in Fe-Mn alloys at 1500°C. Extensive investigations have been carried out in this laboratory, exploring the oxygen partial pressure lower limit at which ZrO2(CaO) electrolyte can be used satisfactorily in oxygen galvanic cells at 1600°C. In a paper to be published at a later date,9 it is demonstrated conclusively that ZrO2(CaO) exhibits insignificant electronic conductivity at oxygen pressures down to about 3 x 10"13 atm which is lower than the oxygen partial pressure in equilibrium with Cr-Cr2O3 at 1600°C. Therefore, the activity of chromium can be related to the measured reversible electromotive force of the cell in the present investigation since no electronic short circulating will occur. Fig. 1 is a schematic diagram of the cell used. The Cr-Cr2O3 electrode was made of equal weights of chromium and Cr2O3 powders which were mixed and packed into a recrystallized alumina crucible. A Pt-wire lead was embedded into the Cr-Cr2O3 compact to insure good contact. A ZrO2(CaO) crucible, supplied by the Zirconium Corp. of America, contained the Ni-Cr melt equilibrated with solid Cr2O3. The ZrO2(CaO) crucible was placed on the Cr-Cr2O3 electrode and additional Cr-Cr2O3 mixture was packed around it. Contact with the Ni-Cr alloy was made with a Cr2O3 tube, which is a weak electronic conductor. A platinum wire lead was attached to the Cr2O3 tube. The galvanic cell was lowered slowly into the hot zone of the furnace tube in order to avoid too large a thermal shock which could break the ZrO2 (CaO) crucible. The furnace was con- tinuously flushed with purified argon during the experiment. The temperature was measured with a Pt-Pt/10 pet Rh thermocouple and maintained at 1600° ± 5°C. The electromotive force was measured with a recording potentiometer. The furnace was turned off when measurements were being made in order to avoid induction effects and the reversibility of the cell was demonstrated in the usual manner. The electromotive force was measured several times over a period of approximately 1 hr. During that period the electromotive force remained constant within ± 3 pet and did not continuously drift in any one direction. After the experiment the alloys were analyzed for chromium in the usual manner. The measured electromotive forces of the cell at 1600°C, (2912°F), are listed in Table I. The activity of chromium, with solid pure chromium as the reference state, (a), was calculated using Eq. [l], , n F E I, n lna RT- U] where E is the measured electromotive force, F is the Faraday constant, and n is equal to 3, the number of equivalents per mole, (nF/RT = 18.59 volts'1 at 1600°C). The resulting activities are listed in Table I. The activity of chromium relative to pure liquid chromium was also calculated. The free energy of fusion of chromium at 1600° C was calculated using

Jan 1, 1969

By James C. Fulton

Since publication of the First Edition of "Basic Open Hearth Steelmaking," in 1944, this book has been a major reference on the subject of steelmaking. The Second Edition of 1951 was so fundamental that it has retained its general usefulness to the present date. However, recently some of the material has been updated in connection with the writing of a companion book, "Electric Furnace Steelmaking." The sponsor of these two books, the Physical Chemistry of Steelmaking Committee, has felt that the new material should be made equally available to purchasers of either book. Accordingly the subject matter of Chapters 14, 15, and 16 of this new edition is duplicated by corresponding chapters in "Electric Furnace Steelmaking." It was also recognized that the use of oxygen in the open hearth and in the new basic oxygen processes represents a major development that should not be omitted from any basic reference. Thus the major new feature of this Third Edition is the supplement on "Oxygen in Steelmaking." The cooperation of the Iron and Steel Division's Acid Converter and Basic Oxygen Steel Committee (now merged to form the National Open Hearth and Basic Oxygen Steel Committee) is specifically recognized. In addition to the authors of chapters listed elsewhere, it should be noted that Arthur B. Wilder was the Committee Chairman. Although the changes in the Third Edition are important, the Committee cannot overlook the classic character of the Second Edition. This edition was edited by W. O. Philbrook and M. B. Bever in collaboration with H. B. Emerick and B. M. Larsen. It is anticipated that the Third Edition will maintain the value of the book until the current rapid changes in all basic steelmaking processes stabilize themselves sufficiently to justify a complete revision of the entire text in Part I. The experienced service of Wesley Burr in incorporating the new material in the index is also recognized.

Jan 1, 1964

By B. S. Tani, R. V. Schablaske, M. G. Chasanov

In the Ti-Cd system two intermediate phases, TiCd and Ti Cd, have been found and characterized by X-ray diffraction powder techniques. An earlier reference' had reported the existence of the compound Tisd. No structural details, however, were given nor was there any indication of the possible existence of other binary compounds. Studies of the solubility of titanium in liquid cadmium2 led to the discovery of both TiCd and Tisd. The solid phase in equilibrium with saturated solutions of titanium in liquid cadmium at temperatures below 620°C is TiCd, whereas TizCd is the equilibrium solid phase above 620°C. Both thermal analysis and X-ray studies show that a peritectic reaction between the y phase (~isd) and cadmium to form the 6 phase (Ti Cd) occurs at 620°C. X-ray diffraction powder photographs of material isolated from the ingots used in the solubility measurements as well as material prepared by a direct heat of the appropriate stoichiometric amounts of titanium and cadmium can be indexed on the basis of a tetragonal unit cell with a = 2.904 ± 0.002A, co = 8.954 * 0.004A, c/a = 3.083. No variation of lattice parameters indicative of a range of composition is evident. With four atoms in the unit cell the calculated density of the intermetallic is 7.05 g per cm3; the observed value is 7.07 g per cm3. The TiCd lattice is primitive as indicated by the fact that there are no systematic absences among hkl reflections. The absence of all hko reflections for which h + k = 2n + 1 is also evident. This systematic absence indicates the following two space groups, C\h — P4/n and D&~4/nmm; both groups, however, have the same two- and four-fold positions. Stoichiometry, symmetry and space group indicate two likely structure types. They are the PbO-litharge3 (B10) type and the Ti CU (B11) type. Spatial considerations favor the B11 structure with atoms placed in the following positions: 2Ti (c) 0, 1/2, Z; l/2, 0, Z 2Cd(c) 0, 1/2, Z; 1/2, 0, Z The TiCd structure may be summarily described as a layered structure in which double cadmium layers alternate with double titanium layers along the c-axis. The best agreement between calculated and observed intensities is obtained for the values ZTi = 0.608 and ZCd = 0.130. Calculated and observed powder intensities as well as other pertinent powder data are recorded in Table I. Interatomic distances for the proposed structure are recorded in Table II and are to be compared with the distances of closest approach for titanium and cad-

Jan 1, 1962

By A. L. Mincher, W. F. Sheely

Mechanical properties of columbium have been studied over the temperature range of -196 to 1093oC. The decreased strengthening influence of cold-work at temperatures below ambient has been interpreted in terms of the Peierls-Nabarro effect. Maxima in the rate of strain hardening observed during tensile testing in the range 250-600°C. have been correlated with interstitial impurities to indicate the temperature ranges at which carbon, oxygen, and nitrogen, respectively, are responsible for strain aging. THE growing need for structural materials for use above the useful service temperatures of the iron-, nickel-, or cobalt-base alloys has caused the refractory metals to be considered as potential engineering materials. These metals, which include columbium, tantalum, molybdenum, and tungsten, are called refractory because the lowest melting point among them,that of columbium, is about 1000°C higher than the average melting temperatures of conventional high-temperature alloys. They are all body-centered cubic transition metals and, as such, their mechanical properties have basic characteristics which distinguish them from the face-centered cubic metals. For example, all show a much steeper rise in strength with decreasing temperature below room temperature than do the face-centered cubic metals, and their mechanical properties are strongly influenced by interstitially dissolved impurities. In order that these new metals may be used efficiently, it is necessary that their characteristics of behavior be fully known. In this paper, the mechanical properties of columbium will be examined over a wide range of temperatures. In particular, the influences of cold-work and individual species of interstitial impurity atoms on mechanical properties will be described, and basic mechanisms which may control the observed characteristics will be explored. EXPERIMENTAL The material used in this investigation was Union Carbide Metals Co. columbium roundels consolidated to four 4-in. diam ingots, three by consumable-electrode arc melting and one ingot by electron beam melting. Impurity contents of the ingots and methods of ingot conversion and treatment are summarized in Table I. The only metallic impurity occurring in any significant quantity was tantalum at about 0.1 pct. Iron, silicon, titanium, and zirconium were each less than 0.015 pct; boron was 1 ppm or less. This should have no appreciable influence on properties. The electron beam melted material, being the purest, will be used as the basis for comparison in the discussions to follow. Tensile tests were conducted from-196 to 1093oC, on both cold-worked and fully recrystallized arc-melted and electron-beam melted columbium using standard 1/4-in. diam, 1-in. long gage length test specimens. A strain-rate of 0.005 in. per in. per min was employed until the 0.2 pct yield strength was achieved and then the strain-rate was increased to 0.05 in. per in. per min for the balance of the test. Samples were protected in an inert atmosphere at tests above 300°C. The tensile properties obtained on the electron-beam melted columbium, E, in both the cold-swaged and recrystallized conditions are given in Fig. 1. The yield strength data of Dyson, et al.,' obtained on recrystallized electron beam melted columbium and the tensile strength data reported by Tottle2 on powder metallurgy columbium are included in Fig. 1. The material used by Tottle had been purified by vacuum sintering. There is excellent agreement between Dyson's data and those obtained in the present investigation. The tensile strengths obtained by Tottle were slightly greater than those obtained in this investigation on electron-beam melted columbium but varied with temperature in a similar manner. Tottle's data showed a maximum in tensile strength near 500°C, as did our data on electron-beam melted material, and also showed a small maximum at 300°C. The significance of these maxima will become evident later in the discussion. The tensile properties of cold-swaged and recrys-tallized arc melted columbium are plotted in Fig. 2. It was found that the properties of the recrystallized arc-melted columbium from all three heats showed very close agreement except at temperatures between about 500" and 800°C. A reason for this range of disagreement will be suggested in the discussion. The generally good agreement, however, attests to the ability of cold-working and subsequent recrystal-lization to erase the effects of the three different primary breakdown procedures and to produce nearly equivalent structures in the samples derived from the three different heats. wesse13 reported tensile data on columbium having interstitial impurity contents between those of the

Jan 1, 1962

By R. A. Wood, R. I. Jaffee, H. R. Ogden, D. N. Williams

The tensile properties, creep resistance. and thermal stability of highly alloyed Ti-Al-Zr alloys were examined. On the basis of these studies, the Ti-7Al-1ZZr composition was selected for more complete evaluation. The alloy was found to be weldable and free from excessive directionality. In addition, it developed maximum properties without requiring heat treatment other than an annealing operation in the alpha field. The alloy was recommended for scale up and is presently being investigated on a production-level basis. One of the more attractive properties of titanium alloys is their ability to withstand stress at moderately high temperatures, and a considerable amount of effort has been devoted to increasing the maximum service temperature of titanium alloys. This work has suggested that the optimum alloys for high-temperature service will be single-phase a (close-packed hexagonal) alloys containing significant amounts of aluminum. However, the maximum amount of aluminum which can be alloyed with titanium is between 6 and 8 pct,l since at high-aluminum contents an embrittlement reaction occurs in the anticipated service temperature range, 800" to 1100°F. It has been shown that the embrittlement reaction involves decomposition of the high-aluminum a phase to one or more new phases.' Since this reaction does not occur at intermediate or low-aluminum contents, it was felt that intermediate Ti-A1 alloys might be strengthened by a-soluble ternary additions without inducing the embrittlement reaction. The first alloying addition considered was tin, which shows extensive solubility in a titanium and has moderate strengthening tendencies. Unfortunately, it was soon apparent that tin also promoted the embrittlement reaction, and that to obtain a stable alloy, the aluminum content had to be reduced as the tin content was increased. The second alloying addition considered was zirconium, which is similar to tin in its effects on titanium. This element did not contribute to the embrittlement reaction and, in fact, appeared to increase the maximum amount of aluminum which could be alloyed with titanium without inducing instability. This paper describes an investigation of the Ti-A1-Zr a alloy region. Alloys containing from 4 to 12 pct A1 and from 6 to 15 pct Zr were examined. The properties of these alloys are described and the bases for selecting an optimum composition is outlined. This composition, Ti-7A1-12Zr, is presently being scaled up in tonnage quantities, and is being evaluated extensively throughout the industry. In addition to presenting the basis for its selection, this paper presents a description of the properties developed in laboratory material as determined during the alloy investigation. These properties suggest that this alloy can fill an important position in applications requiring light weight, fabrica-bility, weldability, and strength to 1000oF or higher. EXPERIMENTAL PROCEDURES Titanium alloy ingots were prepared by inert electrode arc melting under an argon atmosphere. Alloying elements used were 110 Bhn titanium sponge, high-purity aluminum, and reactor-grade zirconium. Pancake-shaped ingots were prepared weighing approximately 300 g. The composition of the ingots was checked by weight measurements before and after melting. The pancake ingots were forged at 2000°F to approximately half their original thickness to give a flat plate roughly 1/2 in. thick. This plate was then rolled at 1800' to 1600°F to 0.250 in. thick. All of the alloys examined fabricated well. However, alloys containing 15 pct Zr tended to overheat due to exothermic oxidation, and scaling was excessive. As might be anticipated from its effect in decreasing the ß transus, increased zirconium appeared to improve fabricability somewhat, especially during rolling at lower temperatures. Except for a limited study of heat-treatment response, all alloys were examined in the a-annealed condition. Prior to heat treatment the a and ß tran-sus temperatures were determined by metallo-graphic examination of samples quenched after annealing at 50-deg intervals in the transformation region. These data are shown in Fig. 1. Recrystal-lization appeared to occur in about 1 hr in the range 1300º to 1500ºF. Therefore, alloys were annealed for 1 hr at 1550ºF (4 and 5 pct Al), 1600ºF (6 through 7-1/2 pct Al), or 1650°F (8 or more pct Al). This produced an equiaxed a grain structure. In most alloys, a "ghost" structure was visible after the a-annealing treatment, as shown in Fig. 2. This structure apparently resulted from the acicular

Jan 1, 1963

By R. J. Reynik

A semiempirial small flunctation theory of diff- sion in liquids is presented, which employs a fluctuation energy assumed quadratic for a small atomic or molecular displacement and Einstein's random-iralh model. The resulting diffusion equation is given by In these equations. D is the diffusivity, is the average liquid shite coordination number (at interatomic distance d. cm. T is the absolute temperature, xu. em, is (the diffusive displacement. K, is the quadratic fluctuation energy force constant, and rg, cm, are the radii oj diffusing atoms A and B, respectively. The quantities Xn and K are calculated from the computer-filled values of the slope and intercept. respectively. The radius of self-diffusing atom or radii and of diffusing atoms A and B are eta United and compared with values reported in the literature.. The predicted linear variation of diffusivity with. It tempera lure htm been observed in approximately thirty-iire metallic liquid systems, and in over seventy-fiee other liquid systems, including the organic .alcohols, liquified inert gases, and the molten salts, ALTHOUGH the average density within a macroscopic volume element of liquid is constant for fixed total number of atoms. pressure. and temperature, there exist microscopic: density fluctuations within the respective volume element. As such the microscopic volume available to an atom and its Z first nearest neighbors at any instant of time fluctuates above and below the average volume available to these atoms. If one assumes that liquid state atoms vibrate as in a solid. and further postulates that the mean position of any atom in the liquid state is not stationary. but shifts during every .vibration a distance 0 5 j 5 xo. then every atom in the liquid state continuously undergoes diffusive displacements which vary in the range 0 5 j 5 ro. Mathematically. for a binary liquid system consisting of atcrms A and B. the maximum diffusive displacement. .YO, is defined by the equation: where d is the average liquid state interatomic distance at specified liquid state coordination number Z. and v~ \ and vg are the effective radii of diffusing atoms A and B: respectively. For self-diffusion. r^ equals rg , and Eq. [I.] reduces to: It is interesting to note that Eq. [l] or [2] can be used to compute the radii of the diffusing atoms, provided one had an experimental evaluation of xo. As such. the computed radii could be compared with metallic or crystallographic ionic radii to ascerlain the electronic character of the diffusing atoms. Thus it is proposed that in the liquid state the n~otion of an atom relative to its original equilibrium position of oscillation represents the thermal vibration of any atom and its Z first nearest neighbors. while the small and variable displacements. 0 5 1 5 xc,. of the centers of oscillation represent the complex diffusive motions of the atoms at constant temperature and pressure. This is consistent with data obtained from slow neutron scattering by liquids1 ' and resembles an itinerant oscillator model of the liquid state.'" It is further postulated that the atomic displacements characterizing the liquid state diffusion process are essentially a random-walk process. As such. it nlay be described by Einstein's equation:' where D is the diffusivity. sq cm sec-'. j2 is the mean square value of the diffusive displacement. and i> is the frequency of density fluctuations giving rise to diffusion. FORMULATION OF DIFFUSION EQUATION The effective spherical volume occupied by an atom, as a consequence of a microscopic density fluctuation which enlarges the volume available to any atom, exceeds its average liquid state atomic volume by an amount: where AV is the enlarged spherical volume, v is the radius of the diffusing atom. and j is the elementary displacement distance from the original center of oscillation of the vibrating atom to a new center of oscillation position. For small atomic displacements. where c is a constant whose value depends upon the assumed geometry of the enlarged volume. For a spherical increase in volume, c equals 4nr2. Following the treatment of Furthl' and ~walin." assuming the enlarged volu~nes AL7 for the diffusing atoms are distributed in a continuunl. the probability of finding a fluctuation in the size range 0 5 j 5 xo defined by Where c includes the geometric constant cl and Eij) is the fluctuation energy causing the volume change. But the proposed model assumes all the Z first nearest-neighbor atoms are centers of oscillation. and hence the probability that any of these atoms is adjacent to a fluctuation of magnitude 05j5xo is unity. Thus:

Jan 1, 1970

By R. Costantini

Long-distance transportation of solids by hydraulic pipelines holds promise of great economic benefits. In most mineral processing plants today, moving of solids in slurry-form by pipeline is commonplace. Yet in spite of this, the method is slow in being adopted on a broad scale for moving solids over distances of many miles. This is especially surprising in view of the successful realization of two daring ventures in long-distance solids pipelines in this nation within the last five years. One is the 72-mile long, 6-in. diam. pipeline of the American Gilsonite Co. which has been satisfactorily transporting 700 tpd of gilsonite from the mine at Bonanza, Utah, to the processing plant at Grand Junction, Colo., since April 1957. The other is the 108-mile long, 10-in. pipeline of the Pittsburgh Consolidation Coal Co., which has been transporting about 4000 tpd of finely crushed coal from the mine at Cadiz, Ohio, to the Eastlake Power Plant of the Cleveland Electric Illuminating Co. since January 1958.

Jan 8, 1961

By Ernest Stütz

The problem of increasing blast-furnace efficiency through diminution of flue-dust production while operating with burdens consisting largely of fine ores has of recent years attracted the attention of metallurgists, whether directly or indirectly interested in the economies of iron smelting, and the various methods evolved from theory or practice have been submitted to wide discussion. After the very thorough and, at that time, exhaustive view of the whole subject, which was afforded to the industry by the meeting of this Institute in February, 1912, the subject was again taken up at the meeting of the Verein deutscher Eisenh?ttenleute at D?sseldorf in December, 1912. While American and German conditions are not entirely identical, it may be of interest to give here the words of the gentleman summing up the discussion at the Diisseldorf meeting: " The chief advantage offered by the use of briquettes lies in the fact that disturbances in the furnace, caused mostly by the presence of fine ores in the burden, are avoided, and that blast pressure can be considerably reduced. The resulting economies cannot be overrated, as, with lower blast consumption per ton of product, the installation will be able to take care of increased production. In consequence of lower pressure and speed of blast, heat is more efficiently utilized, flue gas temperature is lowered, and coke particles are less liable to be carried along with the flue dust, of which considerably less is produced. Finally, by increased regularity of operation and higher temperature in the lower parts of the furnace, the quality of the product is improved. The question of briquetting iron ores has grown to be one of the most important in the iron industry, and it is not any more a question of what is the cost of briquetting a ton of ore, but what, in using ore briquettes, is the cost of production of a ton of iron." Dr. A. Weiskopf, of Hannover, admirably condenses in these words

Jan 1, 1914

The 114th(New York) Meeting of the Institute will be held in the third week of February, 1917. The committee on Papers and Publications has set Dec. 1, 1916, as the closing date for the receipt of manuscripts intended for this meeting. . Manuscripts must be received by the Secretary on or before this date. If they are sent through members of the technical committees they must be sent to those committees enough in advance of the time to be forwarded and in the hands of the Secretary by the time specified.

Jan 10, 1916

By C. G. Dunn

WITH respect to theories of recrystallization in metals plastically deformed, it has been said that the present status of this subject is far from satisfactory.1 It may also be said that before any mechanism of recrystallization for metals and alloys can be set forth in a satisfactory manner, there must be made available considerable data on orientation changes that occur during the deformation and recrystallization processes. Although extensive data have been published on recrystallization in single crystals and in polycrystalline specimens, more results of a type that can be classified according to simple orientation changes would be desirable in this complex field. It might even be said that before classifications are made according to types of orientation changes, it may be possible to classify a considerable amount of data into certain kinds of orientation states if groups of common or nearly common orientation occur. Methods for computing the probability of occurrence for various types of groups have been published2 and it has been pointed out in particular that it should be possible to analyze orientation data for high-order twin relationships between old and new grains even when agreement is not at all exact. In this connection, work on recrystallization in silicon ferrite reported in a paper concerned with complex groups of annealing twins' indicated that some data were consistent with primary nucleation occurring according to a second-order or a third-order twin transformation. However, further work in this latter direction was definitely needed. It is, therefore, the purpose of the present paper to report data and analyses for primary nucleation in silicon ferrite following small deformations that have been carried out at the Pittsfield Works' Laboratory of the General Electric Co. Analyses have been made with the aid of standard groups of twins that are reported elsewhere .4 PREPARATION OF SPECIMENS AND EXPERIMENTAL PROCEDURE The material used in the present investigation was taken' from the same heat of steel as that used in a prior report.3 The finished strip in both cases was made by the Allegheny-Ludlum Steel Corporation according to methods that produce a high degree of preferred crystal orientation. Samples with large grains had the following composition: 3.45 per cent Si, 0.003 C, 0.008 P, 0.020 S, 0.075 Mn, 0.031 Al and 0.072 Cu. Thickness of specimens was 0.012 inches. Plastic deformation was produced by cold-rolling the samples on a mill with

Jan 1, 1945