Search Documents

By William C. McLaughlin

In the deep vein mines of the Coeur d'Alene mining district, rock bursts are a potential hazard to the mine structure and underground personnel. Damage repair costs are estimated by one company to exceed $1 per ton of ore mined. The Bureau of Mines, in cooperation with the mining companies, has conducted research intermittently over the past 10 years to help reduce bursts. Onsite inspections of major rock bursts were conducted, and reports were submitted to mine management; these included the geology and geometry of the affected area. The paper discusses the development and improvement of microseismic and surface monitoring equipment. The underground microseismic network, when operated on a regular basis and the results plotted daily, is capable of detecting stress concentration in certain areas. The surface seismographs record rock bursts, blasts, earthquakes, etc., throughout the district and show approximate location, time, and relative intensity of the event.

Jan 1, 1976

By J. Brett, S. Friedman

A study of the diffusion of nickel into both fibrous and recrystallized 0.065-in.-diam silica-alumina doped tungsten wire at 1200°C has been conducted. The diffusion profiles were determined by chemical dissolulion of successive circumferential layers and spectro-photometric determination of nickel in the etchant. It was shown that the diffusion of nickel into tungsten is markedly structure-sensitive. No significant amount of nickel could be introduced at 1200°C into tungsten which had first been recrystallized at temperatures of 2300°C, leading to an upper limit estimate for the bulk diffusivity of nickel in tungsten of 10-11 sq cm per sec at 1200°C. However, nickel did diffuse into initially fibrous wires, caused re crystallization, and was alsays present at the advancing recrystallization front. The accumulation of nickel in an initially fibrous region ceases when the recrystallization front arrives. The characteristics of the resulting diffusion profiles are explained in terms of the relation between diffusion processes and micro structural changes. WHILE it is well-known that the presence of nickel and certain other metals causes low-temperature recrystallization of the cold-worked fibrous structure of doped tungsten,''' the character of the phenomenon is not well understood. Recently it was shown that the recrystallization reaction can be induced at low temperatures by the presence of solid nickel on the surface of doped wire, but not by exposure to nickel vapors.3 Once recrystallization was initiated, a continued source of nickel was required for propagation of the recrystallization front. The phenomenon appeared to be a complicated solid-state reaction since, in addition to the change in structure of the tungsten from fibrous to equiaxed grains, diffusion of nickel from the surface into the recrystallized and fibrous structures was occurring with possible chemical reaction between nickel and tungsten at the surface and interaction of nickel with the dopants which ordinarily stabilize the fibrous structure within the wire. The objective of the present work was to study the diffusion of nickel into fibrous and recrystallized tungsten structures in order to clarify the relationship of the diffusion process to nickel-induced recrystallization. Studies of interdiffusion in the Ni-W system4"7 have been principally concerned with the mobility of tungsten in nickel. Information on diffusion of nickel in tungsten is meager, and there seem to be no studies of the mobility of nickel in tungsten which elucidate the structural aspects of the phenomenon. The present experiments were designed to determine the diffusivity of nickel at 1200°C in fibrous tungsten, in large-grained tungsten prerecrystallized at high tem- perature, and in tungsten recrystallized at 1200°C due to the presence of nickel. Although the concentration profiles were determined in these experiments, unexpected changes in boundary conditions or complex diffusion paths complicated the analysis of these profiles so that the interpretation could not be readily expressed in terms of simple diffusivities. EXPERIMENTAL PROCEDURE The experiments were conducted on Sylvania 0.065-in.-diam silica-alumina doped commercial tungsten wire, hereafter designated as ordinary doped wire. A special lot of 0.065-in.-diam silica-alumina doped low-nickel wire was also used. Impurity analyses of the wire are given in Table I. The experimental design is shown in Fig. 1. All heat treatments were conducted in vacuum. Two groups of ordinary doped wire were prepared for diffusion with nickel. One group in the as-received (fibrous) condition was elec-tropolished, nickel-plated, and annealed at 1200°C for 20 and 40 hr, or was exposed to nickel vapor at 1200°C for 20 and 40 hr. The second group was recrystallized to an equiaxed grain structure at 2300°C for 3 hr, electropolished, nickel-plated, or exposed to nickel vapor for anneals at 1200°C for 20 and 40 hr.

Jan 1, 1969

By M. C. Irani

The Bureau of Mines, in cooperation with the Mine Safety Appliances Co., has developed a new methane analyzer system for underground applications. Methane enters coal mine ventilation air from the breakup of coal at the active face, from the collapse of roof rock during retreat mining, and from the ribs abutting virgin coal. Each source contributes varying amounts to the total emission, depending upon rate of mining, type of mining, and the character of the coalbed and adjacent strata. The evaluation of individual parameters of methane emission requires the continuous monitoring of individual mine sections over a long period of time. The methane analyzer system was developed to meet this need. The system has been installed and operated in an active mine in the Pittsburgh coalbed. The system and details of its installation and calibration are described. Data are presented to substantiate its reliability.

Jan 1, 1975

By Howard N. Eavenson

The mines of the United States Coal & Coke Co. are located in the Pocahontas coal field, in McDowell County, West Virginia. Twelve plants have been opened and equipped, of which, by reason of the present business depression, only nine are now in operation. These twelve plants serve eighteen mines; some of the plants having several openings, in either the same seam or in different seams, tributary to the same tipple. Only nine of these mines are now being worked at the plants in operation. Construction work was begun in 1902, and coal from the first three plants started was shipped in December of that year. An additional plant was opened in 1903, two in 1904, two in 1905, two in 1907 and the last two in 1908. On Jan. 1, 1915, the plants have been in operation an average period of 8.8 years. The rules of the company, which have been in operation since work was first begun, are similar to those in use by the H. C. Frick Coke Co. at its mines in Pennsylvania, in which " Safety First" was incorporated as early as 1907; and it has always been the policy of both companies to look carefully after the safety of their employees. Although the field is an extension of the old Pocahontas field, the mines, located upon a new branch railroad, are away by themselves, and, as is usual in such cases, the class of labor attracted at first was temporary in character. The rapid development of the mines required the employment of many new men and officials each year; and, while the accident record from 1904 to 1909 was as good as the average of the field, it was felt to be not as good as it could be made, and a determined campaign was inaugurated for preventing accidents of all kinds. Fig. 1 shows the tonnage of coal produced per fatality, both total and for inside accidents only, at our mines; the tonnage per fatality of all West Virginia mines, and of those in the Pocahontas field. The purpose of this paper is not one of congratulation on the results so far accomplished, since the operating officials are not at all satisfied that the maximum is in sight, to say nothing of its having been reached; but to describe the organization and methods that have produced these

Jan 1, 1915

By Qi Jinduo, Gong Min

On the basis of actual parameter of wall control blast in Nanfeng mine, China, the process of dynamic stress changing between two column charges was studied recently for a presplit-cushion blast by holographic photoelasticity. In the experimental model, two holes were simultaneously detonated from both ends (four ignition points). The bottom of the holes were loaded more than other parts (heavy charge). Under these conditions, four consecutive isochromatic fringe patterns at different times were acquired in one loading run, and the characteristics of the stress distributions were compared at different places and times in the holes. It was found that interaction types of stress waves vary along the holes. The theory is posed that the stress wave which is formed by the interaction of earlier producing P wave and later S wave along a distributed line charge is the most important part in all stress waves. Research indicates that a heavy charge in the bottom of the holes is crucial to producing a presplit-cushion effect at the bottom. "End Effect" doesn't affect the magnitude of stress along linking lines between the bottoms. The chief fields of the "End Effect" are also explained in the paper.

Jan 1, 1998

Albert R. LEdoux, New York, N. Y.—I can add a little to the information which has been given, by saying that it has been our business for some years, among other things, to inspect outgoing copper from some of the works here in the East, and to find out why there are variations not only in the conductivity of the wire-bars, but also in the character of the cathode-copper shipped; and we have found two things: These impurities which have been mentioned are largely upon the surface of the cathode. Samples taken of the inside, even of the nodules or " berries " which grow on the outside of the cathode, show that they do not contain more impurities than the denser material in the interior. In other words, it is a superficial deposit or contamination. There is still another reason for impurity in some of the copper which finds its- way to the manufacturers, namely, carelessness in the handling of molds or in casting. We have found copper which was comparatively pure, as far as the copper itself was concerned, but contained, mechanically intruded in the interior of the ingots,

Jan 1, 1913

By X. Tang, N. Ripepi

The Langmuir model has been widely used for the coal-methane sorption process through an isothermal test. However, even though the temperature-dependent Langmuir model was recognized theoretically and experimentally, the quantitative relationships between the Langmuir constants a and b and temperature have not been clarified and confirmed by laboratory test data. This paper collects 158 methane-coal sorption data under different temperatures that apply the Langmuir model to the relationships between the Langmuir constants a and b and temperature. Even though the Langmuir model cannot be used to show the physical state of methane adsorption on coal, it is widely used because of its simplicity and the reasonable explanation of its parameters a and b. The results from these published isothermal tests indicate that (1) there is no consistent relationship between Langmuir constant a and temperature, (2) the Langmuir model is a temperature-dependent model whose temperature-dependent feature is mainly shown by the relationship between the Langmuir constant b and temperature, and (3) the relationship between the Langmuir constant b and temperature can be described by both exponential and linear relationships with dried coal. This paper provides a database for the temperature-dependent Langmuir model that can be used for the reservoir simulation of coalbed methane reservoirs and for the coal seam degasification modeling of underground coal mines, considering the heating effects induced by geothermal and heat injection through factors such as hot water, hot steam and ultrasonics.

Jan 1, 2016

By G. Fehr, B. B. Panda, R. Bansberg, K. Arnold, T. Freiman

To evaluate the potential for process solutions to contaminate groundwater outside of the area of the Oxide Pit, it is necessary to predict the ultimate maximum pit lake elevation once pit-related mining activities have ceased. A water balance model was developed based on the existing pit geometry, the groundwater flow equation, and assumed hydrologic input parameters. The model assumed that at any point in time, total inflow into the system (i.e., direct precipitation, surface water and groundwater) minus outflow from the system (evaporation from the lake surface) was equal to the change in the pit water volume. The pit lake depth over time was predicted by assuming a succession of steady- state water balance conditions over short time increments. An analytical method using a spreadsheet and computer model was employed in this study to model the filling of the lake in the Oxide Pit. A sensitivity analysis was performed to evaluate uncertainty associated with the input parameters in the model. The sensitivity analysis indicated that the model was most sensitive to values of precipitation and evaporation and to the static water table.

Jan 1, 2003

By R. J. Wysor

Discussion of the paper of R. J. WYSOR, presented at the New York meeting, February, 1916, and printed in Bulletin No. 106, October, 1915, pp. 2161 to 2170. LEONARD WALDO, New York, N. Y.-Will Mr. Wysor kindly give us more information as to the pyrometers used and the temperature measurement? R. J. WYSOR, So. Bethlehem, Pa.-We used standard Bristol pyrometers with bare fire ends. These were standardized both before and after the tests with salt and pure aluminum. We also interchanged the pyrometers. J. W. RICHARDS, So. Bethlehem, Pa.-Did you attain any results which gave you approximately the value of the heat insulation at any of the furnaces? R. J. WYSOR.-In the first installation we were afraid to put in the insulation throughout the hot-blast main for the reasons mentioned in the paper, but we used the insulating brick in two 8-ft. sections in straight lengths of our hot-blast mains. Owing to the high conductivity of the steel shell, the temperatures which were taken on the outside were not representative of the two temperatures resulting from heat flow through the insulating brick. I believe that when a hot-blast main is insulated

Jan 5, 1916

By C. J. Fleisch, C. P. Clingerman

THE recent installation of a combination dust catcher, gas washer and precipitator at Carrie blast furnaces of the Homestead Steel Works has given very satisfactory results. The following description of the gas-cleaning installation is based on actual operating experience. When Carrie blast furnace No. 3 was rebuilt the decision was made to fine-clean all the gas produced by the furnace, because the management wanted fine-cleaned gas for fuel in the stoves and boilers. In order to keep the installation cost as low as possible, the gas-cleaning system was streamlined. All by-pass lines and goggle valves for bypass lines were eliminated from the system. A radical departure from the use of 8-in. tubes in the Cottrell-type precipitators was made by using 12-in. diameter tubes in a single compartment, the single compartment being divided into two units by a single partition wall in the top header. THE FURNACE PROPER A few of the characteristic points and dimensions of the furnace proper are: [Hearth diameter 26 ft. o in. Bosh diameter 29 ft. 1 3/4 in. Stock-line diameter 20 ft. o in. Large-bell diameter 114 ft. 8 in. Small-bell diameter 6 ft. 6 in. Height of furnace from center of iron notch to bottom of large bell, closed 94 ft. 4 in. Height of furnace from center of iron notch to main platform 105 ft. o in.] The furnace top is equipped with a McKee revolving distributor, the operation of which is electrically interlocked with the skips, bell hoists, and coke-weighing and charging apparatus through a Freyn automatic charging control. The gas leaves the furnace first through four offtakes, 5 ft. g in. in diameter, then through uptakes that are approximately 85 ft. high, which feed into a single down-comer that is 9 ft. in diameter. DUST CATCHER The primary dust catcher installed (Fig. I) may be described as a single-cone type. The inlet pipe at the top of the dust catcher is g ft. in diameter; it is flared to a conical shape as it extends down inside the dust-catcher shell, which is 35 ft. in diameter, 37 ft. high on the straight side, and has a conical top and bottom. The slope of the bottom is 50° with the horizontal. The cone-shaped pipe inside the dust-catcher shell is 42 ft. high and is 19 ft. 7 in. in diameter at its bottom lip where it releases the gas in-

Jan 1, 1943

By S. J. R. Lowrie, J. S. Edwards, A. D. Jones

A small scale model has been constructed to simulate air and gas flows on a full scale retreat longwall coal face. Scaling relationships were derived to define how the main aerodynamic properties of the full scale could be preserved in the small scale model. These scaling requirements include: a minimum value for the Reynolds number for the flow on the face in order to maintain turbulent flow with a constant non-dimensionalised coefficient of turbulent dispersion; a constant Richardson number to maintain similitude for the formation of layers of buoyant gas; scaling of the permeability of the waste so as to obtain the same proportion of seepage flow through the waste; pressure gradients due to the ventilation and to the density difference (between the air and the gas layer) were kept in proportion; and in the waste, the relative contributions of inertial dispersion and molecular diffusion were approximately in proportion. The complementary roles of computational fluid dynamics (CFD) and aerodynamic scale models for simulating mine ventilation are discussed. The physical model is described and an example presented of simulations of the effect of changes in mining condition on the effectiveness of gas control in retreat longwall coal faces.

Jan 1, 1995

By A. C. Hitchins, C. N. Orssich

The Eagle zone is a gold-bearing, sheeted, quartz vein porphyry deposit hosted by the Cretaceous Dublin Gulch biotite granodiorite stock, located in central Yukon, 50 km north of Mayo. The deposit occurs at the western end of the stock and has been drill tested over a 1000 m by 500 m area, to a depth of 150m. Mineralization consists of 1 cm to 2 Cm wide, parallel, grey and white quartz veins with accessory gold, arsenopyrite, pyrite, pyrrhotite, chalcopyrite, native bismuth, bismuthinite, and scheelite. Vein densities range from two to fifteen veins per metre and average approximately five per metre. The majority of the veins have potassic and or phyllic alteration envelopes. Alteration of the granodiorite becomes pervasive as vein densities increase. Mineralization outside of the Eagle zone, but spatially related to the Dublin Gulch stock, includes: (i) scheelite bearing sheeted quartz vein zones within the east-central portion of the stock; (ii) a swarm of gold-bearing quartz-sulphide veins up to a metre wide in a zone along the northern contact of the stock and extending 7 km further west; (iii) the Mar scheelite skarn located on the south side of the stock; and (iv) cassiterite-bearing breccias located 2 km north of the stock. A geological potential resource of 64.5 Mt tonnes at a grade of 1.03 g/t Au has been estimated for the Eagle zone from widely spaced core and reverse circulation drill holes. Mineralization is open at depth, on strike to the west and beneath the hornfels to the north.

Jan 1, 1995

By A. H. Geisler, R. F. Mehl, C. S. Barrett

The complicated nature of the property changes that accompany age-hardening has made it necessary to reconsider and to elaborate the simple dispersion theory.l It has been apparent for some time that more direct information is needed concerning the atomic mechanism of precipitation from solid solution if the theory of age-hardening is to be developed past a purely qualitative stage.‡ Fortunately, in recent years information has been developed which allows us to trace in detail the lattice changes accompanying the process of precipitation from solid solution. This information relates chiefly to the sequence of the several stages of lattice alteration by which the matrix lattice is transformed to the equilibrium precipitate lattice, and permits reasonable inferences to he drawn concerning the states of internal strain that accompany these stages. This information is most complete for the solid solution of copper in aluminum. The equilibrium precipitate is the 0 phase, "CuAl2." This forms in plates, parallel to the {100} matrix planes. The atom pattern and atom spacing on the plane in 0 lying parallel to this plane are roughly similar to those opposite it in the matrix.3 The formation of 0, however, is preceded by the formation of a transition lattice 0': which again lies parallel to the matrix {100} plane, but in this case the matching of atom pattern and spacing across the matrix-precipitate interface is nearly periect; thus there is lattice coherency across the interface and the interface is a plane of separation in only a very limited sense.'8 Particles of 0' may be recognized microscopically and form a well-defined Wid-manstatten figure.* The 0' lattice is recognized by the occurrence of diffraction lines on powder photo-grams or of spots on Laue photograms which may be analyzed in the usual ways to determine the lattice type and the lattice spacings. Very recent research 6, 7, 1 has shown, however, that streaks occur on the Laue photogram at an earlier point in time during the aging process. These streaks have been attributed to a preferential clustering of copper atoms into small platelike elements of only a few atoms in thickness and a lew hundred atoms in diameter, probably of the composition of " CuA12," which may be designated as Guinier-Preston zones or aggregates.1 It is difficult if not impossible to determine the lattice type and lattice spacing in these aggregates. It is possible1 that these aggregates are in fact ?' in a high State of dispersion; the inclination to argue this is strong, as we shall see later. Never-

Jan 1, 1941

By R. W. Huber, R. C. Wiley, V. C. Petersen

"Three arc- melted ingots, two of a t itanium-7 percent manganese all oy and the third of unalloyed titanium, were forged and rolled into 3/ 4-inch plate; comparative data were obtained on these processes. The finished plate, part of which was used by the Naval Bureau of Ordnance, was tested for mechanical and other properties.These properties were correlated with sponge purity, forging technique, rolling temperature, and cooling rate from the rolling temperature. For the alloy material, transformation data were obtained, and their age-hardening characteristics were studied. The temperature-impact relationship was established for rolled sections from all three ingots.INTRODUCTIONArc -melted ingots of unalloyed titanium and a titanium-manganese alloy were fabricated into plate under closely controlled conditions by personnel of the Metals and Alloys Section, Physical Metallurgy Branch, Bureau of Mines, College Perk, Md. This program was cosponsored by the Naval Bureau of Ordnance. Bureau of Mines interest lay in correlating the processing procedures with the mechanical properties of the finished plate.Considerable data have been published recently on constitution diagrams and properties of titanium-manganese alloys in genera1. 3/ 4/5/6/ However, little if any correlation between processing schedules and end results has been published, particularly with respect to the present commercial production of the proprietary titanium manganese alloys . Several factors in the production of titanium and titanium alloys have a pronounced influence on the physical and mechanical properties of the finished product: (1) The degree and nature of impurities in the base materials, ( 2) the amount of impurities introduced during the melting cycle and their distribution, (3) the homogeneity of the alloy, (4) forging, (5) rolling, and ( 6) final heat-treating cycles. All of these item£ are important from a metallurgical standpoint in producing the desired end properties in the metal."

Mar 1, 1955

By R. F. Mehl, C. S. Barrett, A. H. Geisler

The complicated nature of the property changes that accompany age-hardening has made it necessary to reconsider and to elaborate the simple dispersion theory.l It has been apparent for some time that more direct information is needed concerning the atomic mechanism of precipitation from solid solution if the theory of age-hardening is to be developed past a purely qualitative stage.‡ Fortunately, in recent years information has been developed which allows us to trace in detail the lattice changes accompanying the process of precipitation from solid solution. This information relates chiefly to the sequence of the several stages of lattice alteration by which the matrix lattice is transformed to the equilibrium precipitate lattice, and permits reasonable inferences to he drawn concerning the states of internal strain that accompany these stages. This information is most complete for the solid solution of copper in aluminum. The equilibrium precipitate is the 0 phase, "CuAl2." This forms in plates, parallel to the {100} matrix planes. The atom pattern and atom spacing on the plane in 0 lying parallel to this plane are roughly similar to those opposite it in the matrix.3 The formation of 0, however, is preceded by the formation of a transition lattice 0': which again lies parallel to the matrix {100} plane, but in this case the matching of atom pattern and spacing across the matrix-precipitate interface is nearly periect; thus there is lattice coherency across the interface and the interface is a plane of separation in only a very limited sense.'8 Particles of 0' may be recognized microscopically and form a well-defined Wid-manstatten figure.* The 0' lattice is recognized by the occurrence of diffraction lines on powder photo-grams or of spots on Laue photograms which may be analyzed in the usual ways to determine the lattice type and the lattice spacings. Very recent research 6, 7, 1 has shown, however, that streaks occur on the Laue photogram at an earlier point in time during the aging process. These streaks have been attributed to a preferential clustering of copper atoms into small platelike elements of only a few atoms in thickness and a lew hundred atoms in diameter, probably of the composition of " CuA12," which may be designated as Guinier-Preston zones or aggregates.1 It is difficult if not impossible to determine the lattice type and lattice spacing in these aggregates. It is possible1 that these aggregates are in fact ?' in a high State of dispersion; the inclination to argue this is strong, as we shall see later. Never-

Jan 1, 1941

By P. W. Bennett, E. M. Elkin

A new technique for the recovery of palladium and platinum and sludge from go12 electrolyte eliminates many of the drawbacks of the zinc-dust cementation process. In the electrolytic refining of gold by the Wohwill method, the electrolyte contains about 100 gpl gold as AuCl, and 100 gpl free hydrochloric acid. Any palladium and platinum contained in impure gold dissolve and accumulate in the electrolyte. When their concentration approaches that of gold, it becomes desirable to discard the electrolyte and to recover the gold and the palladium and platinum. As practiced at Canadian Copper Refiners until recently, discarded electrolyte was treated with sulfur dioxide to precipitate the gold. 2AuCl3 + 6H2O + 3SO2 —2Au + 6HC1 + 3H2SO4 The gold precipitate was filtered off, washed with water, and melted with scrap anodes. The wash water was added to the gold-free filtrate and treated with zinc dust to cement the palladium and platinum. PdCl2 + Zn — Pd + ZnCl2 PtCl4 + 2Zn—Pt + 2ZnCl2 The precipitate was separated and sold as Pd-Pt concentrate, and the barren filtrate and wash water were discarded. The receipts of palladium and platinum at this company were too small to warrant their refining. The process suffered from a number of disadvantages. Handling the gold-free solution was disagreeable, as it was laden with sulfur dioxide even after blowing with air overnight. Subsequent treatment with zinc dust was also troublesome. A large excess of zinc dust was required. Spray, acid mist, and vigorous evolution of hydrogen accompanied the reaction. The Pd-Pt precipitate was grossly contaminated with occluded unreacted zinc and with yellow granules of sulfur, thought to be formed by the reduction of sulfur dioxide and its derivatives. Repeated boiling of the precipitate with hydrochloric acid and washing with water decreased somewhat, but did not eliminate, the zinc. After drying overnight, the precipitate hardened to a clinkerlike mass that was difficult to grind. Grinding, handling, and packing created heavy dusting. Even weighing in an analytical balance generated dust, indicating that the powder was easily charged with static electricity. The total palladium and platinum content of the powder varied from 56 to 72 pct, with an average of 65 pct. The powder dissolved in aqua regia with difficulty, leaving a small amount of insoluble residue. However, the main drawback of the process was the strongly hygroscopic Pd-Pt product. The powder showed a marked though erratic increase in weight and a corresponding decrease in assay on exposure to air, even during the course of laboratory analysis. Such changes were the source of disagreement between Canadian Copper Refiners and the buyers of concentrate. The cause of the change in weight is believed to be hydrogen, liberated by the action of zinc dust on hydrochloric acid. Some of this hydrogen was adsorbed so strongly by the precipitate that it could not be driven off during the drying. On exposure to air it oxidized catalytically, forming water. Experiments soon showed that the entire process of treatment of discarded electrolyte then in use would have to be changed. A small quantity of apparatus was moved into the gold room, and experimentation was held to a minimum compatible with the development of a new process. PALLADIUM AND PLATINUM PRECIPITATION It was thought that zinc could be replaced with a reagent other than a hydrogen-evolving metal. Semiquantitative experiments showed that platinum and palladium could be precipitated completely from the gold-free solutions with such well-known reagents as sodium formate, formic acid, formaldehyde, and paraformaldehyde. Sodium formate was the preferred reagent, since the other three are volatile and somewhat toxic. The gold-free solutions used were those saturated with sulfur dioxide, partly freed of sulfur dioxide by aerating overnight, completely freed by boiling, as well as strongly and weakly acidic, neutral, and alkaline solutions. The reactions are complex and can be represented by these over-all equations: PdC1, + HCOONa — Pd + NaCl + HC1 + Co2 PtCl4 + 2HCOONa — Pt + 2NaCl + 2HC1 + 2CCX, Strongly acidic solutions required as much as five times the theoretical amount of sodium formate as did solutions neutralized to pH 4.5. Increasing the pH decreased the consumption of

Jan 1, 1965

By Colin Baker, G. C. Smith

Investigation of the initiation and propagation of ductile failure in OFHC copper was undertaken to determine the role of nonmetallic inclusions. The effect of inclusion initiated voids on the formation of the internal cavity and the final shear separation was studied by metallographic eranzination of strained test pieces. A strain anneal technique was used to enlarge the voids under uniaxial stress conditions to elinzinate triaxial stress effects. Measurements of void size us stress and strain were made to show the point at which void im'tiation begins and becomes an important factor in the deformation process. The work of separation of copper-cuprous oxide was determined to attempt to correlate the breakdown of the matrix inclusion interface with void initiation and propagation. The zloid shape and position relative to the tensile axis suggested an interface breakdown mechanisnz of initiation. Evidence is presented that shows a basic similarity between the central cavity propagation and the 45-deg shear portions of the failure. DUCTILE fracture has been studied by a number of workers1-lo and attention drawn to the importance of hard second phase particles in the initiation of the failure. Holes formed at the matrix-particle interface can elongate by plastic deformation and then subsequently expand sideways to link up and produce a major crack. This is usually observed first in the center of the macroscopically necked region of a test-piece where the hydrostatic stresses are at a maximum. As the crack spreads sideways towards the free surface of the specimen, well defined shear zones develop from the crack tip and the final separation is along a direction at approximately 45 deg to the stress axis. This shear failure may also be associated with voids formed adjacent to second phase particles. In this way a cup and cone type fracture is produced. The stage at which separation takes place between particles and the surrounding matrix has not been clearly identified. In addition, although researchers have dealt with anisotropy of tensile behavior" as a result of material fabrication variables, not much is known about the microstructural features of aniso-tropic behavior. In the present work evidence on these points is presented in relation to the behavior of copper containing second phase particles of cuprous oxide. I. MATERIALS AND PROCEDURES EMPLOYED The material used was +-in. diam or 2-in. sq cold-drawn OFHC copper bar which contained 0.6 pct by volume of cuprous oxide inclusions. These ranged in COLIN BAKER, Junior Member AIME, formerly at -mnF of Metallurgy, University of Cambridge, Cambridge, England, is presently Research Scientist Reynolds Metals Co., Richrnand, Va. G. C. SMITH, Member AIME, is Senior Lecturer, Department of Metallurgy, University of Cambridge. Manuscript submitted June 20, 1967. IMD size from approximately 1 to 6 p in length and 1 to 4 p in width. The shape was generally slightly ovoid. Tensile tests were made on specimens having a gage length of 2.5 cm and diameter of 0.643 cm. Metallographic examination was carried out by sectioning deformed and fractured specimens; in addition fracture surfaces were examined optically and with a scanning electron microscope. Some measurements of the work of separation between copper and cuprous oxide were made, using a sessile drop technique which was a modification of that used by Kingery and umenick." The best metallographic results were obtained by using a vibratory polisher, which minimized smearing of the surface. 11. RESULTS A) Initial Experiments. Specimens from the +-in. diam rod were annealed for 2 hr at 650°C in uacuo, at which temperature complete recrystallization occurred without any change in the form of the inclusion. They were then fractured at temperatures from -190" to 600°C. Cup and cone fractures were obtained at all temperatures from -196" to 400°C. With increase in temperature there was, however, a continuous increase in the extent of the central transverse area and a corresponding decrease in the shear portion of the fracture. Above 400°C, the fractures became intergranular. Sections of specimens tested below 400°C revealed extensive small voids which were always associated with inclusions. However, the voids only reached dimensions greater than the inclusion size in the region of the macroscopic neck, where they were many times longer. Lateral expansion was found only near the fracture surface of the test pieces. As observed by Puttick, the voids were either (a) triangular holes initiated in the direction of the tensile axis and elon-

Jan 1, 1969

By John E. Dutrizac, Tzong T. Chen

"Laboratory experiments were undertaken to ascertain the behaviour of various ""impurity"" species during the precipitation of hematite directly from ferric sulphate solutions at 225°C and in the presence of 40 or 50 g/L of hematite seed. Copper, nickel and zinc are not significantly incorporated in hematite precipitates. Although the nickel contents increase to 0.22% as the Ni concentration increases to 60 g/L, the solid solution Ni contents are low relative to the bulk Ni contents. Thus, part of the Ni may be present as tiny particles of poorly soluble NiS04.H20. Increasing germanium concentrations to 2,000 mg/L result in products containing up to 0.59% Ge. The Ge occurs either in solid solution in the hematite or is adsorbed on the nanometer-size hematite crystallites. Increasing As(V) concentrations to 10 g/L increase the AsO4 contents of the products up to 16%. However, the products consist of hematite together with As04-containing Fe(SO4)(OH) and an unknown Fe-AsO4 species. All the hematite products contain - 1% SO4 which appears to be adsorbed on the nanometer-size hematite crystallites.IntroductionDissolved iron is a common impurity in most hydrometallurgical processing circuits and, generally, the iron must be eliminated prior to the subsequent recovery of the sought after metals. Simple neutralization of iron-rich solutions yields slurries which are difficult to thicken and filter. To address these concerns, the jarosite, goethite and hematite processes have been developed, and these technologies are able to reject the dissolved iron in a readily filterable form [1]. Despite its higher cost, the hematite process offers several potential advantages. Because hematite is an iron-rich, high-density compound, its formation would reduce the mass of residue and the size of a residue storage pond. Hematite is the thermodynamically stable form of iron under ambient conditions, and this stability would facilitate the impoundment of hematite precipitates. Furthermore, hematite has some market potential for cement manufacture and even for iron making [2]. In all the commercial hematite processes, the dissolved ferric ions are first reduced to the ferrous state. Subsequently, the pH of the solution is adjusted and the solution is then oxidized. The ferric ions gradually generated during solution oxidation hydrolyze and precipitate mostly as hematite, although commercial hematite products also contain trace or minor amounts of jarosite-type compounds. However, there are potential advantages in precipitating hematite directly from ferric ion solutions, as the reduction and subsequent oxidation of the iron are not required. Although the precipitation of hematite directly from relatively concentrated ferric sulphate solutions (up to 0.5 M Fe(SO4)is) was recently demonstrated [3], the behaviour of impurity species during hematite precipitation is largely unknown. To address this issue, systematic laboratory experiments were undertaken to ascertain the behaviour of a number of ""impurity"" species during the precipitation of hematite directly from ferric sulphate solutions at 225°C, and the results are presented in this paper."

Jan 1, 2012

By C. D. Williams, C. E. Ells

The susceptibility of quenched and aged Zr-2.5 wt pct Nb alloy to embritt2ement during irradiation has been examined for a number of solution temperatures and aging times. Material quenched from temperatures approximately 40°C below the transus has high tensile ductility, and this ductility is insensitive to aging at 500°C or to irradiation. If, however, the material is quenched from temperatures above the transus it becomes highly susceptible to loss of ductility either from aging at 500 or from irradiation. Inter granular failure is characteristic of the materials having low ductility. The distribution of the equilibrium phase is found to control the susceptibility to embrittlement by restricting 6 grain growth during heat treatment and thus influencing crack propagation. IN zirconium, as in titanium, -stabilizing alloy additions are used to obtain high strengths via quench and age heat treatments, and the Zr-2.5 pct Nb alloy has been developed1 because of its strength advantage over the Zircaloys. Early in the development of the Zr-2.5 pct Nb alloy the problem of 13 embrittlement was appreciated, and for this reason the solution temperature was chosen below the p transus.' In the course of irradiation studies on quenched and aged Zr-2.5 wt pct Nb alloy it was found' that irradiation introduced an important aspect of p embrittlement, riz., material quenched from the phase and aged 24 hr at 500°C was severely embrittled by moderate doses of neutron irradiation. This effect had not been studied in titanium alloys. In titanium the metallurgical features leading to 0 ernbrittlement were found to be structures with: a) coarse a platelets at the grain bondaries, b) finely dispersed a uniformly distributed throughout the (0) matrix,6 c) Widmanstatten a-13 with more than 50 pct P, d) the presence of some metastable p transformation products,3 and e) large prior -phase grain size.5 Alternatively, the presence of a uniform distribution of coarse a was conducive to high ductility and a structure largely of equiaxed a was very dctile. The detailed mechanisms of the embrittlement have not been worked out for all of these conditions, although weakness at either a-matrix boundaries or prior p grain boundaries have been prominent in the eculation. It was proposed that acicular a might act as a mild notch, and low ductility has been associated with easy fracture along its boundary.' There have been two opposing suggestions for the source of the high ductility associated with equiaxed a phase. JaffeeB proposed that this a would accept a large por- tion of the oxygen, thus increasing the ductility of the matrix, whereas after study of a Zr-Nb-Cu alloy Weinstein and oltz proposed that the a phase, softer than the martensitic matrix, acted to blunt cracks formed in the matrix. In the present work we have studied the effect of neutron irradiation on the ductility, particularly the P embrittlement, of the Zr-2.5 wt pct Nb alloy. By a variation of solution temperature and aging time a variety of metallurgical conditions have been examined, and a range of resultant ductilities obtained. The ductility has been related to the material microstructure and mode of fracture. EXPERIMENTAL The alloy used in the present work came from two separate ingots fabricated into rod of 3/8 or i in. diam, Table I. For both batches the P transus temperature was approximately 890° C. Most of the heat treatments were done directly on lengths of the j} in. diam rod, after which the tensile test specimens were machined. Quenching was achieved by dropping rods from a dynamic vacuum into water, the cooling rate estimated to be 2 100°C per sec. For aging the rods were encapsulated in evacuated silica tubes. Round tensile test specimens, with gage diam and length 0.160 and 1.0 in., respectively, were used throughout and pulled at room temperature or 300°C on Instron tensile machines, at a crosshead speed of 0.05 ipm. Specimens were irradiated in the NRX and NRU reactors, in facilities described in previous publications.'0 The metallurgical conditions examined have been: All tensile test specimens were machined with axes in the axial direction of the swaged rod. Although the specimen had a degree of preferred crystallo-graphic orientation with basal plane normals both parallel with and perpendicular to the tensile axis, the material was comparatively isotropic." The techniques of thin foil examination in the electron micro-

Jan 1, 1970

By Sheldon P. Wimpfen

EVER since the Phoenicians roamed the known world in quest of metals to harden their helmets and precious metals and gems to adorn their ladies, many other nations have sought metals in the far corners of the earth. During the past 75 years American engineers have been among the foremost in seeking for and developing ore deposits. They have been responsible for many of the principal discoveries and for the application of modern methods to mines in the far comers of the earth. American mining engineers with a zest for travel and an insatiable appetite for metals have also introduced throughout the world many articles made of metal which we consider essential to everyday life. Production and consumption of these metals in many foreign countries has brought to these countries an increased standard of living and added tax revenue to their governments. But unfortunately engineers from this country are no longer given ready access to all the countries of the world. This is not only unfortunate for American engineers but also for the countries that have adopted the exclusion policies and especially so since time has proved that in countries where the American engineers have gradually been excluded there has been a significant decline in the progress of the mining industry. Removal of these barriers to professional men would aid immensely in the world-wide development of the mineral industries. New areas brought into production under the guidance of American engineers with their exceptional know-how would provide more jobs for nationals of the countries involved and a better standard of living for the nations as a whole.

Jan 1, 1946