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By J. M. Mwase

The platinum group metal (PGM) industry is currently reliant on the crush-mill-float-smelt-refine route to process PGM ores. However, there are many instances where this route would not be feasible. An alternative process route has been developed which involves heap bioleaching to extract base metals followed by heap reclamation and a water wash step, leading into heap cyanide leaching to extract precious metals. This process was evaluated through test work on samples of Platreef ore using laboratory scale columns. After 304 days 75% Ni and 93% Cu were extracted in the bioleach experiment at 65°C, and after 60 days 58% Pt, 99% Pd and 90% Au in the follow-up cyanide leach experiment at 50°C. A preliminary process flow sheet has been developed around this. Analysis via a mineral liberation analyser showed that the remaining Pt was in the form of the mineral sperrylite, which appeared to be slow leaching in cyanide in comparison to the other mineral types. Analysis of cyanide effluent solution showed high levels of thiocyanate, which present an environmental risk for disposal and high consumption of cyanide. Further studies to develop the process for commercial application in the South African PGM industry are outlined.

Jan 1, 2014

By V. Rajaram

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, 1977

By S. C. Termes

As part of an effort to provide basic data on the fundamental scientific and engineering principles of minerals beneficiation, the Bureau of Mines is conducting research on the flocculation of mineral fines. This paper presents results of studies using crosslinked starches containing carboxyl, diethanolamine, iminodiacetic acid, and xanthate groups to flocculate hematite, goethite, chromite, manganrte, pyrolusite, cuprite, and cassiterite fines. The carboxyl and xanthate derivatives flocculated all minerals except cassiterite; the latter was flocculated by only the diethanolamine derivative. The iminodiacetic acid derivative flocculated hematite, goethite, chromite, cuprite, and pryolusite fines. Zeta potential measurements were made to help define the reaction mechanism responsible for flocculation. These measurements indicate that electrostatic attraction probably is not involved, except possibly in the case of the diethano lamine derivative. The separation of hematite from quartz by selective flocculation with chelating cross- linked starches under two pH conditions and with two dispersing agents is described. Best recoveries and grades were found when either the carboxyl or xanthate derivatives was added at the natural pH of the pulp in the absence of a dupersing agent.

Jan 1, 1983

The introduction of nitro-carbo-nitrate (NCN) blasting agents has been one of the most significant innovations in the explosive industry in the last twenty years. The most commonly used blasting agent is a rather narrowly proportioned mixture by weight of 94% ammonium nitrate (AN) and 6% No. 2 diesel fuel oil (FO) that is generally designated as ANFO. Other formulations have been developed but none of these have been as extensively used as ANFO. The relative safety of the nitro-carbo-nitrate (NCN) blasting agents almost immediately suggested bulk loading techniques to obtain economies in materials handling. The first attempt at bulk handling was to pneumatically load boreholes with ANFO. When the initial experiments were made in 1957, it was apparent that there were three problem areas which needed study to minimize potential hazards. These were: 1. Static Electricity 2. Fumes 3. Safe Handling Procedures Since those early days, considerable work has been performed in evaluating these problem areas and in arriving at procedures and recommendations that would provide the required safety. Despite the relative insensitivity of ANFO type products, all normal practices for the safe handling of explosives should be obselved. Smoking should not be tolerated in the vicinity of blasting agents and misfires should be handled in the same manner as a misfire with a dynamite charge. The purpose of this Technical Report is to discuss the problems of static electricity and fumes and the solutions that have been developed. Safe handling procedures have been discussed by the Bureau of Mines and are specified by various state and local regulations. Since regulations vary from state to state, the local, applicable regulations must be followed within the area of their jurisdiction. General information is contained in a U. S. Bureau of Mines report, IC 8179, "Safety Recommendations for Sensitized Ammonium Nitrate Blasting Agents" (1963).

Jan 1, 1973

By D. Paktunc, S. P. du Preez, J. P. Beukes, P. G. van Zyl, A. Jordaan

"The chromium (Cr) content of stainless steel originates from recycled scrap and/or ferrochrome (FeCr), which is produced mainly by the carbothermic reduction of chromite ore. The oxidative sintered pellet production process is one of the most widely applied FeCr processes. The supplier of this technology specifies that recycling of chromite-containing dust collected from the pellet sintering off-gas and fines screened out from the sintered pellets (collectively referred to as pre-oxidized chromite fines) should be limited to a maximum of 4 wt% of the total pellet composition. However, the results presented in this paper suggest that recycling of such fines up to a limit of 32 wt% of the total pellet composition may improve the compressive and abrasion strengths of the cured pellet. In addition, electron microprobe and quantitative X-ray diffraction (XRD) analyses demonstrate that chromite grains present in the pre-oxidized chromite fines consist, at least partially, of crystalline phases/compounds that will improve the metallurgical efficiency and specific electricity consumption (i.e. MWh/ton FeCr produced) of the smelting process. Introduction Stainless steel is a vital modern-day alloy that is well-known for its corrosion resistance, which is mainly due to the inclusion of chromium (Cr) (ICDA, 2013). Stainless steel is mostly produced from recycled scrap and ferrochrome (FeCr), a relatively crude alloy of Cr and iron (Fe). FeCr is predominantly produced by the carbothermic reduction of chromite, a mineral belonging to the spinel group characterized by the unit formula [(Mg,Fe2+)(Al,Cr,Fe3+)2O4] (Haggerty, 1991; Paktunc and Cabri, 1995; Tathavakar, Antony, and Jha, 2005). Although Cr can occur in 82 different minerals, chromite is the only source of new Cr units that can be exploited in commercial volumes (Motzer and Engineers, 2004). Approximately 95% of mined chromite is used in the production of various FeCr grades, of which high-carbon and charge grade FeCr are the most common (ICDA, 2013)."

Feb 1, 2019

By Irshad A. Rana

In a modern copper smelter, the capital cost of a sulfuric acid plant constitutes the largest single cost item of the total investment. It is thus essential to properly size the acid plant in order to reduce its capital cost and enhance the economic viability of a new smelter project. Whereas the off-gas from a smelting furnace is continuous and generally uniform, the gas flow from the Peirce-Smith converters is intermittent with significant fluctuations. The converters off-gas volume is dependent upon a number of interrelating factors. The most significant factors are the matte feed grade, the system air infiltration, the converter's size and blowing rate, the maximum number of converters simultaneously blowing and the gas cooling system employed. The acid plant size, therefore, is heavily influenced by the converter off-gases. Several of these factors are discussed, and their impact in determining the acid plant size is explored.

Jan 1, 1993

By Olin M. Hart

Uranium ores occur in the Lower Cretaceous Inyan Kara group of heterogeneously stratified fluvial and fluvial-marine sandstones in the Black Hills of western South Dakota and northeastern Wyoming. There are three principal mining districts, each in the ancestral and present drainage area of a major river partially responsible for stripping the region to its present topographic form. Primary minerals in the deposits are coffinite and uraninite with minor amounts of paramontroseite and haggite. The ore minerals coat sand grains and fill interstices of complexly cross-stratified sandstone along solution fronts similar to "roll" type deposits of the other districts. Minerals of oxidized deposits are typically carnotite and tyuyamunite with different proportions of secondary vanadium accessory minerals. Ground water was the transporting medium and deposition of primary uranium and vanadium minerals occurred in reducing environments produced and controlled by physio-chemical characteristics of the sedimentary rocks.

Jan 1, 1968

By R. K. Young

Producing a sound plant design for a major project requires hundreds of engineers and many drawings. Economical accomplishment of this task is based upon careful and orderly organization of the design team so that at all times there is a complete and workable staff but at no time a surplus of costly talent. This paper will describe the various stages in the development of plant design which normally follow the laboratory and pilot plant investigations discussed in other papers today. An outline of the procedures used in the assembling of a project design group, within an established engineering organization will be presented. Actual procedures may vary according to the size and character of the plant, the special requirements of the owner, and the make-up of the engineering organization performing the design, but most of the points covered will be found to be basic to any plant design project.

Jan 1, 1960

By AIME AIME

THIS year the Petroleum Division holds its fall meeting at Houston, Texas, Oct. 2 and 3, with head- quarters at the Lamar Hotel. Technical sessions will be held in the morning and afternoon of both days. A smoker on Friday afternoon will afford an opportunity to get together socially. Saturday evening is left free for private parties to the beach at Galveston, where a wide variety of entertainment is available. On Oct. 4 there will be an excursion to Sugarland oil field, with luncheon at Boling and a visit to Boling sulfur mine and plant in the afternoon. There are nine technical papers on the program for Friday. Saturday morning will be devoted to oil production control and it is planned to make the discussion more

Jan 1, 1931

By B. H. Kear

All the possible ways of forming simple two-dislocation boundaries in multiple slip orientations are deduced. It is shown that the principal differences in work hardening behavior of crystals plastically deformed in these orientations can he accounted for in terms of the likelihood of formation of diffuse boundaries, or deformation bands, consisting of the products of dislocation reactions of the Lomer type. Also, it is pointed out that the break-up of boundaries under the applied stress is more likely to yield interstitial jogs than vacancy jogs, whereas glide dislocations cutting throuqh dislocations trapped in particularly stable boundam'es can acquire both types of jogs. USING Frank's' grain boundary formula, Ball and Hirsch2 determined the parameters of all the possible boundaries that can be built from two sets of glide dislocations in the fee structure. This paper deduces the geometrical possibilities for the formation of these two-dislocation boundaries in the different multiple slip orientations, and discusses the role of boundaries in work hardening and in jog formation. Formation of Two-Dislocation Boundaries in Mutiple Slip Orientations. The parameters of the possible two-dislocation boundaries for any crystal orientation can be deduced most conveniently using the boundary formulae due to Amelinckx,3 in conjunction with the stereographic projection shown in Fig. 1. Suppose that slip occurs in a-BC and ß-CA. According to Amelinckx, when the two systems of glide dislocations are parallel, the rotation axis, u, of the boundary is parallel to (a x ß) and the unit normal, u, defining the boundary plane is parallel to (a x ß) x (BC x CA). On the other hand, when the glide dislocations form a crossed grid, u is parallel to (BC x CA) and u is parallel to (a x CA) x (ß x BC). In Fig. 1, (a x ß) is the pole of the great circle passing through a and ß, so that u is parallel to DC, i.e., parallel to [110]. Furthermore, (a x ß) x (BC x CA) is the pole of the great circle passing through DC and 6, so that u is parallel to [110]. Hence, when all the glide dislocations are parallel, the boundary is pure tilt with parameters u = [110], v = [ 110]. Similarly, it may be shown that the corresponding crossed grid of dislocations is a mixed boundary with u = [111], u = [111]. Consider the case of a crystal compressed in the [001] orientation. In this orientation, according to Fig. 1, there are eight available slip systems. In what follows, the different types of two-dislocation boundaries that are possible in this orientation will be examined by taking different combinations of two slip systems out of the available eight, with a-BC always one of the systems. Case (i)—Slip Systems a-BC and d-CB. The formation of a tilt boundary in (101), which consists of a crossed grid of edge dislocations with vectors BC andCB, is illustrated in Fig. 2(a). As the figure shows, slip is required in the system a-BC in one part of the crystal and in d-CB in the other part, with both sets of dislocations entering the boundary from opposite sides. The rotation axis of the boundary lies in (101), depending on the relative densities of the two sets of edge dislocations in the boundary. Case (ii)-Slip Systems a-BC and ß-CA. The two possible boundaries are shown in Figs. 2(b) and (c); boundary (b) is tilt with u = [110], u = [110], and

Jan 1, 1962

By Ralph W. Edie

"IntroductionTHIS PAPER deals with chemical and mineralogical changes in wall-rocks associated with pitchblende mineralization in the Gold-fields area of Saskatchewan. The localities at which the rock specimens studied were collected, and descriptions of the various rock-types referred to, are given in a previous paper by the author (5).The geological field work upon which this paper is based was carried out while the writer was employed by the Eldorado Mining and Refining Company during the summers of 1948, 1949 and 1950. The laboratory work§ consisted largely of quantitative spectrographic analyses for both major and minor elements, supplemented by an examination of 250 thin sections of both altered and unaltered rocks.Character of the AlterationHydrothermal alteration, with associated pitchbende mineralization, is widespread in the Goldfields area of Saskatchewan. The most intense alteration is restricted to the immediate vicinity of fault or breccia zones, but large areas are affected to a minor extent.In detail, the relationship between alteration and pitchblende mineralization is complex, as individual veins do not in general have separate alteration halos. Pitchblende generally occurs in gash-like calcite veins or stringers in wide, fractured zones associated with faulting. Large, lenticular and tabular masses of slightly to intensely altered rock occur in the same wide fracture zones as the mineralized veins. However, vein deposition appears to be-long to a later fracturing period, after hydrothermal alteration was more or: less completed. Generally, the veins transect and are confined to highly altered rock, but on the other hand many highly altered zones intersected in diamond drill-core are barren of mineralized veins."

Jan 1, 1953

By D. R. Gagnon

Mining companies are continually looking for product-ivity and efficiency improvements with their equipment to reduce operating costs. This paper will review the results of a productivity analysis conducted at the Luscar Ltd. Boundary Dam and Bienfait mines near Estevan, Saskatchewan using a Computer-Aided Earthmoving System (CAES) installed on a track-type dozer. The CAES TTT system is a Global Positioning System that provides the operator with constant survey guidance. The study includes a productivity comparison between two similar test sites, one with the aid of the CAES system and the other, without. The CAES TTT system shows a productivity improvement of between 20 and 35% in the reclamation slope leveling application. Even with the CAES TTT system deactivated, some of the advanced features of the system were used to: retain terrain data for volume calculations; track the equipment position; and, accurately record and separate idle time from working time.

Jan 1, 2002

By B. F. Buie

In South Carolina and Georgia an area about 20 miles wide situated near the inner margin of the Coastal Plain and extending from the vicinity of Columbia, S.C. southwestward about 180 miles to the vicinity of Macon, Georgia is the principal kaolin-producing area of the world. It is especially important as the world's major source of clay used for paper coating. Essentially all of the land known or likely to be productive of quality kaolin in this area is now owned or controlled by producing companies. The least-fully developed portion is that in the vicinity of Wrens, Georgia which has been explored and developed since 1961. For the two decades following the end of world war II, demand for kaolin increased at approximately twice the rate for other industrial minerals. From 1945 to 1965 production increased four-fold. Since 1965 the rate of increase has been less, but the outlook now is that production and demand will double at least once again before the year 2000. A substantial part of this increased demand has come, and will continue to come, from industrial development, especially in the paper industry, outside the United States. The general effect, in addition to a continuing increase in production in the U.S., will be to cause: 1. Intensive research for development of more effective and more economical methods of beneficiation; 2. Concerted research effort to find an economical way of modifying high-viscosity kaolin so that it can be used for paper coating; 3. More active exploration in the U.S. and overseas, especially for deposits to supply the foreign markets; 4. More intensive study of the geological factors responsible for the accumulation of commercial deposits of kaolin; 5. Some modest rise in price, relative to the cost of other industrial minerals. The effect on kaolin producing region of Georgia and South Carolina will be to cause: 1. Working of progressively lower-grade deposits; 2. An increase in the acceptable thickness of overburden; 3. Mining of deposits farther down-dip, the use of which is now inhibited by large volumes of groundwater; 4. Increased threat of invasion of the kaolin in industry's market by substitute materials; 5. A substantial increase in concern over environmental factors; 6. More attention to be paid to the large opportunity offered for mining of silica sand and other co-products.

Jan 1, 1972

By B. C. Curson

A comprehensive simulation of .the gas handling system in BHP Copper's San Manuel smelter was developed using AFT Fathom software, with the objective of minimizing SO2 emissions while maximizing smelter throughput. Once verified with plant data, the simulation quickly revealed' the complex interactions occurring between individual converters and the flash furnace. The increased understanding provided by the simulation allowed novel, counter-intuitive control strategies to be developed and tested successfully.

Jan 1, 1999

By M. Board, C. Alexander, M. Ramström, W. Johnson

"Hecla - Lucky Friday is an underground mine that has been in operation for 75 years and produces from depths over 2.3 kilometers (7,500 ft) below the surface. Technical issues at this depth include high rock temperature and seismicity. The use of new innovative mechanization is being examined for ore production. Principal advantages of mechanization are the reduced exposure of personnel, reduced seismic triggers, and increased efficiency. Lucky Friday has partnered with Atlas Copco to design, build, test, and deploy a mechanical miner for primary ore production. We will discuss the background, concept, development and deployment strategy for a mechanical miner. BACKGROUND The Coeur d’Alene mining district in northern Idaho was first discovered over 130 years ago and has been the most prolific silver producer in the US. The Lucky Friday mine of Hecla Mining Company (Figure 1) is the oldest (76 years) and deepest mine in the district, producing approximately 725 tonne per day (800 tons per day) from narrow, vertical lead-zinc-silver veins. Cut and fill stoping is currently employed at depths to about 2.3 km (7,500 ft) below ground surface, making it one of the three deepest mines in the western hemisphere. The #4 Shaft, a winze collared at approximately 1.8 km (5,900 ft) below surface and extending to a depth of nearly 2.9 km (9,600 ft), was recently completed to exploit the high-grade 30 Vein, whose resource has been identified to at least 3 km (9,700 ft) in depth.As with other deep mines worldwide, a number of challenging engineering issues occur, including: high in situ rock stress, squeezing ground, seismicity, high in situ rock temperature that requires refrigeration, diesel equipment that generates diesel particulate matter (DPM) requiring high ventilation airflow rates, and long travel times for worker transport to mining areas."

Jan 1, 2018

By T. F. Anstett

The Bureau of Mines estimated the potential availability of rare-earth oxides (EtEO), including yttrium, and thorium, which is also contained in the rare-earth bearing minerals monazite and bastnasite, from 38 'properties in market economy countries (MEC's). Only nine of the properties evaluated produce or would produce REO as the primary product; the others contain REO as a byproduct, chiefly from mineral sands operations recovering rutile, ilmenite, and zircon. Nearly 77% (2,578,000 mt) of the total 3,355,000 mt of recoverable RE0 evaluated is from producing properties. It is estimated that 21% (705,000 mt) of this total is from properties that could not realize a positive rate of return at the January 1984 market prices for the recovered commodities. At production capacities assumed for this evaluation, the amount of RE0 potentially available from producers ranges from an estimated 46,500 mt in 1986, to a peak of 50,900 mt in 1992, to 49,900 mt by the year 2000. Total MEG production in 1984 was estimated at 40,700 mt. Assuming demand does not increase sharply, producing properties can continue to fulfill overall REO demand through at least the end of this century.

Jan 1, 1986

By Ralph Hultgren, Louis A. Carapella

When F. Heuslerl found in 1898 that certain alloys containing only copper, manganese, and tin were ferromagnetic, the discovery excited a great deal of interest and led to numerous investigations. It was early found that tin could be replaced by aluminum, arsenic, antimony, bismuth, or boron without destroying the ferromagnetic nature of the alloys.2 Copper may also be replaced by silver.% All these alloys have come to be known as "Heusler alloys." The aluminum alloys apparently were the most magnetic and have been most extensively investigated. However, no agreement has yet been reached as to the source of the ferromagnetism arising from these nonferromagnetic elements. Absence of reliable quantitative data makes speculation hazardous. The value of much of the earlier work was vitiated by lack of necessary precautions against contamination, and by lack of close control of heat-treatment. It was only recently established that in aluminum Heusler alloys4 the ferromagnetism arose from a single phase, an ordered body-centered-cubic structure. With modern methods of preparation, heat-treatment, and X-ray examination, it is possible to prepare these alloys without contamination, to heat-treat them intellgently, and to determine what phase or phases are present in the finished sample. In the present investigation, a series of pure alloys in the comparatively neglected copper-manganese-tin system have been prepared, which consist of a single, body-centered-cubic structure (the beta phase) and whose compositions vary within wide limits. The magnetic saturation values of these single-phase alloys have been quantitatively determined, so that considerable data on the effect of composition on the ferromagnetism have been made available. In the course of the investigation some information on the extent of the stability of the beta phase and the nature of phases in adjacent regions of the ternary diagram has been accumulated. Anomalies in earlier data. have been explained, and alloys have been prepared that are much more strongly magnetic than any previous Heusler alloys. Previous Work In the original work of F. Heuslerl and coworkers,2 a maximum magnetic saturation value of I = 107 was found at the composition Cu6Mn3Sn, while a value for CusMnAl of I = 443 was early measured. Ross and Gray5 found a second maximum at the composition Cu2MnSn, which was much more magnetic than Heusler's original alloy. F. Heusler6 hen reinvesti-gated the system, confirmed their results,

Jan 1, 1942

By Louis A. Carapella, Ralph Hultgren

When F. Heuslerl found in 1898 that certain alloys containing only copper, manganese, and tin were ferromagnetic, the discovery excited a great deal of interest and led to numerous investigations. It was early found that tin could be replaced by aluminum, arsenic, antimony, bismuth, or boron without destroying the ferromagnetic nature of the alloys.2 Copper may also be replaced by silver.% All these alloys have come to be known as "Heusler alloys." The aluminum alloys apparently were the most magnetic and have been most extensively investigated. However, no agreement has yet been reached as to the source of the ferromagnetism arising from these nonferromagnetic elements. Absence of reliable quantitative data makes speculation hazardous. The value of much of the earlier work was vitiated by lack of necessary precautions against contamination, and by lack of close control of heat-treatment. It was only recently established that in aluminum Heusler alloys4 the ferromagnetism arose from a single phase, an ordered body-centered-cubic structure. With modern methods of preparation, heat-treatment, and X-ray examination, it is possible to prepare these alloys without contamination, to heat-treat them intellgently, and to determine what phase or phases are present in the finished sample. In the present investigation, a series of pure alloys in the comparatively neglected copper-manganese-tin system have been prepared, which consist of a single, body-centered-cubic structure (the beta phase) and whose compositions vary within wide limits. The magnetic saturation values of these single-phase alloys have been quantitatively determined, so that considerable data on the effect of composition on the ferromagnetism have been made available. In the course of the investigation some information on the extent of the stability of the beta phase and the nature of phases in adjacent regions of the ternary diagram has been accumulated. Anomalies in earlier data. have been explained, and alloys have been prepared that are much more strongly magnetic than any previous Heusler alloys. Previous Work In the original work of F. Heuslerl and coworkers,2 a maximum magnetic saturation value of I = 107 was found at the composition Cu6Mn3Sn, while a value for CusMnAl of I = 443 was early measured. Ross and Gray5 found a second maximum at the composition Cu2MnSn, which was much more magnetic than Heusler's original alloy. F. Heusler6 hen reinvesti-gated the system, confirmed their results,

Jan 1, 1942

By N. Tounsi

The use of analytical modeling of continuous chip formation in conjunction with orthogonal cutting experiments was presented in the open literature to identify the coefficients of material constitutive equation within the practical range of stress, strain, strain rate, and temperature encountered in metal cutting. Identification of reliable constitutive data was hampered by a lack of a reliable model for the prediction of the primary shear zone thickness that affects directly the effective strain rate field. An original analytical model to determine the primary shear zone thickness is proposed in this paper. It is based on the mechanics governing the material flow in the primary shear zone. Based on the distribution of the hydrostatic pressure and the forces measured from orthogonal cutting tests, the model that describes the thickness of the primary shear zone is derived. To validate the model, FE simulations of chip formation using DEFORM3D were carried out for different materials and cutting conditions. The results of the analytical model are in reasonable agreement with FEM results.

Jan 1, 2006

By Voyle R. McFarland, Robert A. Burmeister, David A. Stevenson

The distribution of lead between phases in the Ag-Sb-Te system was studied using microautoradio -graphy. Two compositions were investigated, both containing an intermediate phase Known as silver antimony telluride as the major phase, and one containing AgzTe and the other SbzTes as the minor phase. For both compositions, two thermal treatments were used: nonequilibrium solidification from the melt and long equilibration anneals of the as-solidified structure. For each composition, lead was segregated in the minor phase of the as-solidified structure, but was distributed in the matrix after anneal. The electrical resistivity and carrier type were insensitive to the distribution of lead in the two-phase structure. ThERE has been considerable interest in the Ag-Sb-Te system because of its thermoelectric properties. The major interest has been in compositions on the vertical section between AgzTe and SbzTes, particularly the 50 mole pct SbzTes composition AgSbTez (compositions are conveniently expressed as mole percent SbzTes along the AgzTe-SbzTes section). One of the major problems in the proper evaluation and utilization of this material is the inability to control the electrical properties through impurity additions: all alloys prepared to date have been p-type, even with the addition of large amounts of impurities. It has been shown Wit all the compositions previously studied contain an intermediate phase of the NaCl st'ructure as a major phase (denoted by b) and a second phase, either AgzTe or SbzTe3, as a minor phase.'-3 One explanation for the unusual electrical behavior of this material is that the impurity additions have a higher solubility in the second phase than in the matrix; the impurity would segregate to the second phase, leaving the bulk matrix essentially free of impurity.4 In order to investigate this mechanism with a specific impurity element, the distribution of lead between the two phases was determined using autoradiography. Lead 210 was chosen because of the suitability of its 0.029 mev 0 particle for autoradiography and also because of the interest in lead as an impurity in this system.5'6 EXPERIMENTAL PROCEDURE Two compositions were taken from the vertical section between AgzTe and SbzTes, 50 mole pet SbzTes (Viz. AgSbTez) and 75 mole pct SbzTes, in which AgzTe and SbzTes appear, respectively, as the minor phase. Lead containing radioactive lead (pb210) was added to the above compositions to provide a concentration of 0.1 wt pct Pb. The material was placed in a graphite crucible in a quartz tube which was then evacuated and sealed. The samples were melted and solidified by cooling at a rate of 8°C per min and then removed and prepared for microa~toradiography. After autoradiographic examination of these samples, they were again encapsulated and annealed in an isothermal bath at 300°C for a number of days and prepared for examination. An alternate method of preparation employed a zone-melting furnace; the molten zone traversed the sample at a rate of 1.2 cm per hr and the solid was maintained at a temperature of 500°C both before and after solidification. This treatment had the same effect as solidification at a slow rate followed by an anneal for several hours at 500°C. In order to obtain the best resolution, thin sections of the alloy were prepared by hand lapping to a thickness of approximately 20 p. Other samples were prepared for examination by lapping a flat surface on the bulk sample. The resolution, although somewhat better in the former procedure, was adequate in both instances and the majority of the samples were treated in the latter fashion. A piece of autoradiographic film (Kodak Experimental SP 764 Autoradiographic Permeable Base Safety Stripping Film) was stripped from its backing, care being taken to avoid fogging due to static-electrical discharge. A small amount of water was placed on the sample, the film applied emulsion side down on the surface of the sample, and the sample and the film dipped into water in order to assure smooth contact. After drying, the film was exposed for 2 to 5 days, the period of time selected to give the best resolution. The film was developed on the specimen and fixed and washed in place. Two major factors must be considered in establishing the reliability of an autoradiograph: the in-

Jan 1, 1964