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By Richard H. Jahns

GRANITIC pegmatite deposits are the chief source of commercial feldspar, sheet mica, beryllium, tantalum-columbium, and lithium minerals, and certain types of kaolin. They also have yielded significant quantities of cassiterite, gems, scrap mica, molybdenite, tungsten minerals, uranium-thorium and rare-earth minerals, and zircon, either directly or as the sources of placer deposits. The output from pegmatite mines in the United States is small as compared to other mineral products in terms of bulk or value, and much of it comprises minor metals and nonmetals. Nevertheless, pegmatite minerals play a vital part in domestic industrial economy, particularly in the ceramic and electrical industries. Numerous special purpose uses also are important, even though they require small quantities of raw materials. Never was United States dependence upon pegmatite mining more clearly emphasized than during World War 11, when greatly expanded demands and uncertainties of foreign sources of supply caused much concern. Such commodities as beryl, tantalite, and sheet muscovite remained high on the critical list for months at a time, and for some minerals there was a real struggle to achieve and maintain a favorable ratio of supply to demand. Satisfactory stock piles of certain sizes and qualities of sheet mica, for example, were not built up until late in 1944, when wartime requirements already had begun to level off or even to decrease. Production of all the strategic pegmatite minerals from domestic deposits during World War I1 constituted only 10 pct or less of the total domestic consumption of these minerals, but the importance of this contribution should not be minimized. Domestic production often represented the difference between increase and further reduction of existing stocks of commodities already in seriously short supply, and in the early stages of the war it was the only assured source if imports were cut off. During the recent war period, the U. S. Geological Survey carried on a program of pegmatite studies in the New England and Southeastern States, in the Black Hills area of South Dakota, in the Rocky Mountain region of Wyoming, Colorado, and New Mexico, and in various parts of Washington, Idaho, Utah, Nevada, Arizona, and California as shown in Fig. 1. Several papers and reports already have appeared as an outgrowth of this work,'-= and others are in preparation. This paper outlines some results of data obtained by the writer during the period 1942 to 1946, when he was engaged in studies of pegmatites in the Southeastern, Southwestern, and Rocky Mountain States. Beryllium Minerals Beryl is the present commercial source of beryllium metal and beryllium compounds, which are used in ceramics, in the preparation of X-ray tubes and fluorescent lamps and screens, in special processes of paint and textile manufacture, and in the optical systems of some electrical instruments. The metal also is used in nuclear physics, chiefly as a source of neutrons. Beryllium is alloyed with aluminum for certain light-metal uses and is a constituent of some nickel and iron alloys. Currently the chief demand, however, is for copper-base alloys, which are exceptionally resistant to fatigue and wear, are responsive to hardening treatments after

Jan 1, 1952

By Charles H. Addison, Robert W. Shields, James W. Sweeney

GIPSY: Is user oriented. Is flexible in applications. Is an ITERATIVE question answering system. Has an adaptable retrieval mechanism. Has both a batch and a teleprocessing version. Allows the user to "browse" through his information. Has ability to answer "ad hoc" queries. Is a currently working and proven system.

Jan 1, 1969

By K. L. Clark, Nicholas Kowall

MAXIMUM furnace efficiency and close control of final steel composition demand that the steel melter be able to follow closely the variations in the carbon content of the bath. For many years, the fracture test has been used by melters for estimating carbon, because it requires only a very short time to pour a sample into a chill mold, cool it in water, break it with a sledge hammer, and observe the fracture. After long experience gained from the observation of such fractures, most melters are able to estimate the carbon content of steel with amazing accuracy, particularly in the lower carbon ranges. Notwithstanding the utility of the fracture test, there has been widespread interest in other methods for rapid carbon determination to supplement it and to ensure against possible errors in human judgment. Several methods, based upon measurement of magnetic properties as functions of carbon content, have been described in the literature1-6 and have been found to give reasonably reliable results in plant practice when scrap composition is known and controlled. A difficulty encountered in the use of analyzers of the magnetic type is that alloying elements do change the relationship between carbon content and magnetic properties and it becomes necessary to establish calibration curves for all the expected combinations of alloy residuals that are not oxidized in the bath. The work reported here is of an investigation of a method that is independent of alloying elements normally present in constructional steels, being based upon the relatively well-known fact that in plain carbon and low-alloy steels martensitic hardness is a function of carbon content alone. WORK OF OTHER INVESTIGATORS In 1938, Burns, Moore and Archer published a curve7 that showed that the hardness of martensite is a function of carbon from 0.10 to 0.50 per cent and is independent of grain size or alloy content, at least within the range found in constructional S.A.E. compositions. Some of the deeper hardening types investigated, however, contained carbon to a maximum of only 0.20 per cent. Using this principle, Kern8 developed a method of rapid carbon determination for S.A.E. 43xx steels. His procedure consisted of chill-casting a test bar that was large enough to give a surface that could be prepared for Brinell indentations. The test piece was quenched immediately after solidification was complete and hardness readings were taken, so that the carbon content could be read from an experimentally determined curve giving the relationship between as-quenched hardness and carbon. EXPERIMENTAL WORK Although Kern's work had been done with a relatively deep-hardening steel, it

Jan 1, 1944

By E. V. Kleber, V. F. Novy, R. C. Vickery

The constitutional diagram has been determined for the system gadolinium-nickel. Nine intermetallic compounds have been found at compositions corresponding to the following gadolinium-nickel ratios: 3:1, 3:2, 1:1, 1:2, 1:3, 2:7, 1:4, 1:5, 2:17. The GdNi and GdNi5 compounds have congruent melting points of 1300' and 1500°C, respectively while the remaining compounds melt in-congruently. Eutectics exist at 15 wt pct Ni, 31 1/2 wt pct Ni and 87 wt pct Ni with melting points of 6703 8803 and 1220°C, respectively. IN a continuing investigation of the properties of rare earth alloys, a study has been made of the gadolinium-nickel system. Previous work encompassed the iron containing alloys and a subsequent paper will deal with the constitution of the gadolinium-cobalt system. Vogel,1 examined alloys of nickel with lanthanum and cerium. R3Ni, RNi, RNi2, RNi3, RNi4, and RNi5 compounds were found. Endter and Klemm,2 Fulling et al.3 Heumann,4 and Nowotny5 found the 1:2 compositions of this series to exist in a C-15 (face-centered cubic) structure, and the 1:5 compositions in a hexagonal system. Jepson and Duwez6 more recently examined these 1:2 and 1:5 compositions and generally confirmed earlier data while Wernick and Geller7 most recently have given additional data on the GdNi5 compound. Comparisons with our results will be made in the appropriate section of this report. EXPERIMENTAL Methods of alloy preparation, annealing procedures, and experimental techniques have been given in our earlier paper.8 Chemical analyses of the alloy samples were made by dissolving the specimen in nitric acid, precipitating the gadolinium as hydroxide and the nickel with dimethylglyoxime. Both precipitates were ignited to oxide and weighed. RESULTS Microstructure— Metallography of alloy specimens in this series has been conducted on both arc-melted and annealed materials. Etchants used have been 5 pct nital with approximately 10 pct distilled water added, for high gadolinium samples; Carapella's ferric chloride solution for intermediate compositions; and Marble's (copper sulfate) reagent for high nickel content alloys. Because of difficulties encountered in the grinding and polishing of specimens containing 40 to 75 wt pct Ni, no photomicrographs were made of such specimens. The microstructure of an arc-melted 5.3 wt pct Ni alloy is shown in Fig. 1. Light etching primary grains of gadolinium are embedded in an eutectic matrix. The microstructure of an alloy of 9.55 wt pct Ni alloy, Fig. 2, annealed 50 hr at 700°C, consists almost entirely of the intermetallic compound Gd3Ni. The structure of an arc metal alloy of approximately 19 pct Ni, Fig. 3, consists of grains of the compound GdNi embedded in the Gd3Ni2-Gd3Ni eutectic. The arc-cast structure of the 38.7 wt pct Ni alloy is shown in Fig. 4. Large primary grains of a compound rest in a matrix structure of coarse GdNi-GdNiz eutectic. Because of the occurrence of several peritectic compounds in the central region of the diagram, identification of the primary structure in this alloy is not certain. As has been indicated above, microstructures of alloy specimens containing between ca 40 and 75 wt pct Ni have not been photographed. These specimens were highly brittle, and macro- and micro-cracking were impossible to control in the grinding and polishing procedures. Prolonged annealing did not alleviate this condition. Visual observations in small specimens did, however, provide evidence for a multiplicity of phases and peritectic dissociations of compounds although rationalization of structures was not possible.

Jan 1, 1962

MORE than 5000 miners and suppliers descended upon Denver to make the American Mining Congress' four-day metal mining show one of the most extravagant equipment displays ever assembled in one place at one time. The most recent developments in equipment for mining, milling, and processing ore were shown by the 146 exhibitors at Denver's new City Auditorium which covers 57,000 sq ft of floor space. Other displays were placed in the open air opposite the auditorium site. Registration desks were opened Sunday, Sept. 21. A field trip to the Colorado School of Mines at Golden was the featured activity of the day. Official opening of the show took place on Monday, and presided over by Howard I. Young, president of American Zinc, Lead & Smelting Co.; Otto Herres, vice president, Combined Metals Reduction Co.; William J. Coulter, vice president, Climax Molybdenum Co.; Charles B. Stainback, Westinghouse Electric Corp.; and Merrill E. Shoup, president, Golden Cycle Corp. Convention welcoming addresses were delivered by a representative of Mayor James Q. Newton, of Denver, and Gov. Daniel V. Thorton of Colorado. Following the formal opening ceremonies a round table discussion dealt with the "Paley Commission Report" formally called Resources for Freedom. Participating in the panel were: Arthur H. Bunker and George R. Brown, members of the Paley commission; H. I. Young, president of the American Mining Congress; Horace M. Albright, president of U. S. Potash Co.; Evan Just, vice president, Cyprus Mines Corp.; Donald H. McLaughlin, president, Homestake Mining Co.; E. H. Snyder, president Combined Metals Reduction Co.; Simon D. Strauss, vice president, American Smelting & Refining Co.; Sen. H. C. Dworshak (R.-Idaho) ; Ira B. Joralemon, consulting engineer; Jess Larson, De fense Materials Procurement Agency; and Andrew Fletcher, president of St. Joseph Lead Co. The panel discussed the report for six hours, adding a great deal of information to the already voluminous amount which has been gathered concerning it. Three objections to the report frequently mentioned were: 1-the multilateral contract; 2-international buffer stocks; 3-international buffer stocks combined with limited quota arrangements. Points on which the panel commended the report were its recommendations for acceleration of topographic and geologic mapping of the United States and Alaska; recognition of the principle of percentage depletion for metals and minerals; and advocation of removal of the present limitations on the expensing of exploration costs applicable to minerals. Technical sessions were held throughout the four days of the meeting. Included in the program were: Progress in Mechanication; Small Mines; Public Lands; Open Pit Mining; Manpower-Labor Relations; Shaft Sinking; Roof Support; Taxation, Gold, Silver and Monetary Policy; Advances in Mill Practices; Special Conference on Strategic Materials; Uranium Mining-Atomic Energy; Prospecting and Exploration; New Metallurgical Processes; and Rock Breaking. About 45 papers and several panels were presented during technical sessions. Formal and informal social functions consumed the remaining time of the convention. Three locations were needed to handle the huge throng attending the Mining Jamboree Monday evening. The only other sponsored social function took place Thursday evening. A great many informal gatherings, chiefly convivial, were held in manufacturers' courtesy rooms-called wet stopes. Field trips included Cripple Creek, Pueblo, Climax -Leadville-Gilman, Colorado Plateau-Grand

Jan 1, 1952

By W. A. Binsacca

The concentrator treats sulfide ore containing lead, copper, zinc, gold and silver, at the rate of 850 tons per 24 hr., and produces lead, copper, zinc and iron concentrates by selective flotation methods. The ore occurs below the oxidized zone along a main fracture, the wall rock of which is either greywacke or calcareous shale. The predominating sulfide minerals are galena, sphalerite, pyrite and chalcopyrite; the others are quartz and calcite. In minor amounts, arsenopyrite, pyrrhotite and hematite occur, and such secondary minerals as smithsonite, chalcocite, covellite, bornite, cerussite and anglesite are detected in the ore, the last two named occurring principally as surface alterations of the galena. The ore is hauled from the mine bins in 10-ton cars which pass over the track scales before entering the car dumper ahead of the crusher plant.' A conveyor belt delivers the crushed ore to the sulfide bin, which has a capacity of 2800 tons. The primary grinding unit consists of two 6 by 12-ft. Marcy rod mills operating in parallel and in open circuit, each taking 425 tons per day. One rod mill discharges into an 8 by 25-ft. Dorr classifier with a 12-ft. bowl and the other into a 6 by 25-ft. Dorr duplex classifier. These classifiers are arranged so that each unit rakes the sands into a 6 by 14-ft. Traylor ball mill, which discharges to the bowl classifier only. The duplex classifier therefore operates in open circuit and the bowl classifier in closed circuit, the overflow of both classifiers furnishing the feed for the flotation section. Other groupings have been tried, but this has been found the most satisfactory. The Marcy mills are driven by 150-hp. slip-ring induction motors with speed reducers to give 17 r.p.m. The Traylor mill operates at a speed of 24 r.p.m. and is driven by a 200-hp. slip-ring induction motor, direct connected to pinion and gear. The bowl classifier operates at a speed of 22 r.p.m., with the bowl rake making 4.5 r.p.m. and the duplex classifier at 31 r.p.m. High-carbon steel rods of Mexican manufacture, 12 ft. long by 3-in. diameter, are used in the Marcy mills, with a resulting consumption of 1.52 Ib. per ton ore. The Traylor mill is fed 3-in. cast-iron balls cast in

Jan 1, 1935

By T. M. Howell

JET piercing is a licensed process developed by Linde Air Products Co. Experiments with this method lapsed during World War II, but in the decade that followed the process was expedited. Two types of drills mount the jet piercing equipment for blastholes. The turntable of one machine rotates the complete stem system as well as the blowpipe, which emits three individual flames at different levels. Depth penetrated is limited by length of the blowpipe mounted in the rotary mechanism. This machine has successfully drilled blast- holes in Minnesota taconite.

Jan 6, 1957

By J. L. Bray

IT is well known that iron markedly improves the physical properties and casting characteristics of aluminum bronzes. The use of 1 to 4 per cent iron as the principal modifying addition has become common practice in many foundries melting aluminum bronzes. Although the beneficial effects of iron are unquestioned, there is some uncertainty regarding the structural changes caused by it in the basic copper-alumi-num system. It is agreed that a new constituent appears in abundance when the iron content reaches 2 to 4 per cent. This constituent, which frequently occurs in shapes resembling clover leaves, is sometimes assumed to be an aluminum-iron intermetallic compound. If this were correct we might expect a change in the structural relationships of the matrix in the direction of decreased aluminum content. On the other hand, it has been reported that iron has a negligible effect in altering the fundamental relationships of copper-aluminum alloys1. Others2,3 have reported an additive coefficient. Apparently it will be necessary to know the equilibrium relationships between the phases of the copper-aluminum-iron alloy system to establish any such theory as fact. When this has been done it may very well be that a further revision in the structural relationships may be necessary to describe the changes to be expected in commercial cast alloys. It was with this latter problem before them that the authors attempted to

Jan 1, 1936

By P. Nelson, K. L. Gunsallus, A. R. Ingraffea, J. F. Beech

INTRODUCTION Fracture toughness, KIC, is an intrinsic material property and is a measure of the energy required to create new surface area in a material. Fracture toughness measurements can be made for a wide range of rock types (Ouchterlony, 1980). As a measure of energy of comminution, fracture toughness might be used for more sensitive predictions of Tunnel Boring Machine (TRM) performance than are possible with other index measures in current use. This paper describes part of an ongoing, comprehensive, analytical/experimental program aimed at evaluation of KIC in such a role. The program includes efforts to: 1. Provide a firm analytical basis for a test specimen geometry: the core-derived short-rod. 2. Develop simple, inexpensive testing equipment and techniques. 3. Evaluate the accuracy of the above by testing rock and other materials and comparing the measured fracture toughness with those obtained by other methods. 4. Measure fracture toughness of a substantial number of different rocks from three ongoing TBM projects. 5. Compare fracture toughness results with other strength measures. 6. Compare all test results with observed TBM performance in the three projects. Presented here are summaries of all but the last of these efforts. Comparative evaluation of KIC as a more senstive rock property for TBM performance prediction will be the subject of the oral presentation and a subsequent paper.

Jan 1, 1982

By W. A. Clark

THE production of sand in an oil well increases operating costs because of abnormal wear in subsurface equipment, the necessity for frequent cleanouts, and the need for a means of disposing of the sand. Moreover, removal of sand from the zone can bring about the creation of cavities from which bodies of formation, sand or shale, may slough into the hole, endangering the shutoff, impeding production or collapsing the liner. The procedure known as gravel packing is attracting attention as a means of controlling these factors and contributing to the productive life of a well. That gravel packing is now substantially beyond the preliminary stage on the Pacific Coast is reflected in the 191,000 bbl, of oil produced monthly by the 66 gravel-packed wells in 11 different producing sectors. REASONS FOR GRAVEL-PACKING Gravel packing, if properly carried out, can be expected to provide the following benefits: 1. Prevent the movement of sand and thus eliminate sand production and sand fills, and prevent the formation of cavities. 2. Provide a practical, relatively inexpensive, large-diameter hole, which will provide well-known theoretical advantages. 3. Support the walls of the hole by completely filling the space between the liner and the formation, regardless of its irregularities, and afford a support for liners. 4. Provide for more efficient pumping operations in wells by: (a) possibly utilizing the gravel as a gas trap in pumping gaseous fluids, (b). allowing deep submergence of the pump into the oil zone.

Jan 1, 1939

By John E. Sherborne, William M. Newton

THE relation between the properties of electric logs and the fluid used in drilling a well is briefly discussed in this paper, and the fact that the resistivity of the drilling mud and its filtrate can appreciably affect such logs is shown. Apparatus was designed and a procedure established to determine the effect of various factors on the resistivity of drilling mud. Five muds commonly employed in California were tested and the following observations were made: I. The effect of raising the temperature from 80°F. to 180°F. is to decrease the resistivity of the mud or filtrate approximately 50 per cent. 2. The resistivity of the mud in most cases closely approximates that of its filtrate. 3. The change in the resistivities of muds caused by the addition of chemical is not the same function of the amount of chemical added for each mud. 4. The effect produced by increased sodium chloride content is to reduce markedly the resistivity of the mud and its filtrate. 5. Weighting materials, such as Baroid and limestone, tend to increase the resistivity of drilling mud. 6. Cement and counteracting reagents reduce mud resistivity.

Jan 1, 1942

By Nelson Severinghaus

THIS Rock Chapel plant of Consolidated Quarries Corporation (Fig. 1) is three miles northeast of Lithonia, DeKalb County, Georgia. It was opened about eight years ago for crushed stone aggregate. This paper reviews a number of experiments that have been tried in drilling and blasting, and gives the practice in use today. It also present, several theories on the action of explosives in this type of blasting. [ ] The rock worked is a bare dome of granite gneiss about 3000 ft. in diameter, rising 150 ft. above the surrounding ground (Fig. 2). It is uniform in composition and quality, without seams, and extends downward to unknown depth below the quarry floor. A water well drilled 600 ft. remained in the same rock. The principal difficulty encountered in blasting is an easy split, which tends to break clown the rock in large blocks.

Jan 1, 1938

Jan 1, 1891

By F. W. Jessen, N. Mungan

The plastic flow characteristics of clay water suspensions were first recognized by Binghaml in 1916 and further studied by Ambrose and Loomis' in 1931-1932. Many physical and chemical properties of clay suspensions are deeply influenced by particle size distribution as well as by the exchange cation. Separation of a number of fractions is particularly helpful in making a detailed study of a suspension. A limited amount of work has been conducted on the effects of particle size on specific properties of mud drilling fluids. A knowledge of particle size distribution is essential for a better understanding of fundamental properties of clay suspensions, particularly viscosity and gel strength. The purpose of this investigation was to study the effect of particle size on the viscosity and gel properties of clay suspensions and to determine any changes in mineral composition accompanying variation in size. EXPERIMENTAL PROCEDURE Numerous methods may be used to fractionate a poly-dispersed clay suspension into nearly mono-dispersed systems. Particles larger than 44 micron (325-mesh) may be obtained by wet screening. For sizes from 44 to 1 micron, the fractionation may be accomplished by sedimentation, elutriation plus microscopy,' or turbidimetry.6 When dealing with systems which contain a major portion of particles below l-mi-cron size, slit ultramicroscopy,7 centrifuge methods of Svedberg,5 eams,9 and McBain,l0 and X-ray methods" may be employed. The Sharples super centrifuge has been proved suitable for the economical separation of suspended particles of submicron range.12,13,14 Three-hundred and forty-five gal of 1 per cent by weight Aquagel suspension was mixed in a high-speed 5-gallon mud mixer and the suspension was allowed to stand in 5-gal glass bottles for 30 days to assure full hydration. All particles larger than 44 microns were removed by wet screening. Five fractions in the range of 44 to 1 micron were obtained by sedimentation. The Sharples super centrifuge method described by Hauser and Reed.13 Norton and Speil,14 Ha user and Lynn,15 and Hauser and Schachman,10 as employed to yield five fractions of submicron size. A super centrifuge operation chart prepared by Fancher, Oliphant, and Houssierre12 was used to determine operating conditions for the desired particle ranges. The clay suspension, after removal of all material above 1-micron size, was centrifuged. During rotation of the bowl, the particles were deposited on a thin plastic liner which fit closely inside the bowl. After passing 5 gal of suspension through the centrifuge, the liner was removed and the particles on the liner were scraped off, remixed and recentrifuged. This was repeated five times. Thus, Fractions H, I, K, and L were obtained. The finest fraction, M, remained in an approximately 0.4 per cent suspension. Water was evaporated under reduced pressure from this suspension to yield the finest particles. Results of the fractionation are included in Table 1. In order to achieve proper orientation and humidity conditions for X-ray diffraction analysis, the following procedure was employed. The dilute suspensions were placed on glass slides and allowed to dry at room temperature. This was repeated several times. Previous to measurement each sample first was placed in a water desiccator for half an hour and then allowed to stand for 15 minutes at room temperature. thus yielding an equilibrium condition of about 52 per cent relative humidity. The relative humidity of the room in which the X-ray diffraction was carried out was maintained at approximately 50 per cent so that there was no change in the spacings during the X-ray examination. Samples

By D. M. Hausen

The amenability of a given vanadium ore to any given treatment depends largely on the mineralogic combinations of vanadium in the ore. Quantitative data on vanadium mineralogy provide not only an objective basis for selection of proper treatment, but also may eliminate many time-consuming amenability studies whose results are empirical, at best. Vanadium is distributed through the interstices of mineralized sandstone ores in the form of oxidized vanadates, reduced oxides, and silicates. Oxidized vanadates, e.g., carnotite, tyuyamunite, etc., are most readily beneficiated by simple acid leaching. Reduced oxides are more slowly solubilized, but relatively amenable to most acid treatments. The layered silicates, roscoelite, mixed layered mica-montmorillonite, and chlorite, are least amenable to most acid extractions, and constitute an assemblage of vanadium- bearing clays that are common to many sedimentary deposits. Vanadium is combined principally as layered silicates in the clay fractions of many sandstone ores. Mineralogic studies in this paper are largely confined to clay minerals, and to their amenability characteristics in low pH liquors.

Jan 1, 1985

By C. J. Bise, E. K. Albert

Mathematical modeling and computer simulation are the two primary techniques used for production analysis of underground coal mine layouts. Oftentimes, however, the selection between these two techniques is not based on an awareness of the level of effort needed for input formulation versus the suitability of the desired output. This paper will review mathematical modeling and two of the more prominent simulators (Virginia Tech's FACESIM and Penn State's UGMHS) used in underground coal mine production analysis. A hypothetical section will be analyzed by these programs and, based on the results of the aforementioned study, their advantages and disadvantages will be discussed.

Jan 1, 1985

By Y. L. Yao

The solubility limit of oxygeu in a titanionn at 850°C has been determined by magnetic measurements as 12.5 + 0.5 pct (29.0—30,9 at. pct). Also in the susceptibility-co~centmtion curve, there is n distinct but not sharp maximum at 19.0 * 0.5 z~t pet (40.5--42.1 at. pct), which indicates the presence of the 6 phase. The magnetic susceptibilities of the alloys of the titanium-oxygen system were determined byEhrlich in 1939.' is alloys were prepared by sintiring mixtures of titanium and its oxide at high temperatures. On the titanium-rich side, despite the fact that the alloy compositions he measured crossed two phase boundaries, the limited results obtained

Jan 1, 1960

By A. Boltax

H. Herman and M. E. Fine (Northzcesteriz University)—The author is to be complimented on the quality and completeness of his work. Of special interest to us was the exponent of time in the exponential rate equation, n = 0.28 ± 0.03, since it is consistent with results for the early stage of quench-aging in A1-2 at. pct Cu, n = 1/3, first determined in this laboratory."' In that work we attributed the early kinetics to attraction of vacancy - solute atom complexes to the plate-shaped zone due to the strain field about the zone and the lowering in free energy. To our knowledge, Hirano et 1.' were the first to

Jan 1, 1962

By R. C. Himes, K. Zanio, J. B. Wagner, J. W. Moody, J. F. Miller, W. Johnson

The recent research with which this paper deals has been concerned with the preparation of pure PbTe crystals suitable for control of radiative processes and othe.v electronic applications. The research has been directed toward the developrnent of methods for the preparation of puve, homogeneous, loul-ca,wier-density PbTe crystals suitable for use in the fabrication of optically pumped and electrically pumped diode lasers. Steps in the preparation of the crystals include 1) purification of the starting materials, 2) synthesis and purification of the PbTe, 3) growoth of PbTe crystals, and 4) adjustt~zertt of composition of the crystals This Paper describes the general preparation procedure employed and discusses some investigntiotzs of purification processes. THE as-received lead and tellurium are nominally 99.999 to 99.9999 pct pure. Assays furnished by the suppliers, obtained by emission spectrographic analysis, show only the presence of about 2 ppm Mg in the tellurium. Such analyses are not very informative, however, since they give no information on the concentrations of normally gaseous impurity elements such as oxygen. Both the lead and the tellurium in the as-received state usually contain appreciable concentrations of oxygen—primarily in the form of oxides on the surfaces of the material. To reduce the oxygen content, the lead is held in the molten state in hydrogen at -700°C for several hours. For this treatment, the lead is contained in a graphite boat which is rf-heated, and the hydrogen is passed through a liquid-nitrogen trap prior to use. Tellurium is subjected to multiple distillation in hydrogen to remove oxygen and other foreign impurities. If, in conducting the distillation, approximately the last 10 pct of the charge at each "stage" is left as the discard cut, purification of the tellurium proceeds as indicated in Fig. 1.l Tellurium used in this work has been distilled two or three times to reduce carrier concentration to about 10" per cu cm. The PbTe is prepared from the purified elements by reacting them in the molten state in sealed, evacuated, or hydrogen-filled silica ampoules. The charge is usually held above the melting point of PbTe (923°C) at 1000 C for 24 hr to ensure that it has been homogenized. Two methods have been employed for the growth of the required single crystals of PbTe: growth from the melt, which will be discussed first, and growth from the vapor phase. Large single crystals of p-type PbTe can be grown readily from the melt by the Bridgman method. For this method of crystal growth, the PbTe is synthesized in situ from proper proportions of the purified elements. Growth (dropping) rates in the range 1.3 to 6.5 mm per hr are employed. Material near the maximum melting composition (about 50.012 at. pct Te) is utilized to avoid composition change on freezing, and thus to obtain crystals of nearly uniform composition. Crystals prepared by use of procedures described up to this point were sufficiently pure and perfect that they could be used for the preparation of laser crystals in studies at Lincoln Laboratory.2-5 ADJUSTMENT OF COMPOSITION Good n-type crystals of PbTe cannot readily be grown from the melt. Further, growth from the melt of crystals of any compositions (n or p type) other than those near the maximum melting composition is difficult because of the large composition changes that must occur on freezing.'" However, melt-grown crystals can rapidly be brought to other desired compositions by isothermal equilibration through the vapor phase with a two-phase Pb-Te stock material, essentially as described by Brebrick and Allgaier.1 The work to be discussed has been concerned with the preparation of n-type crystals; thus, the two-phase stock which was employed contained excess lead, and all ensuing discussion is of the preparation and properties of n-type crystals. The equilibration was designed to the shift composition to the lead-rich limit of stability at the selected temperature. Initial treatment of the crystals at high temperature was employed to minimize the total time required for the equilibration. Final adjustments of the composition and state of the crystals were made by use of low-temperature heat treatment at temperatures in the range 200" to

Jan 1, 1968

By F. W. Willard

VIEWING with alarm is a preoccupation not exclusively the habit of the political spellbinder. In good faith many of our mineral technologists have been and are genuinely alarmed over the prodigal consumption of our mineral reserves. Most competent observers are cautiously pessimistic. There are sound technical reasons for such caution. It is the purpose of this paper to discuss some of those reasons without benefit of a gift of prophecy. Perhaps the outstanding reason for caution is ignorance of accessible but undiscovered mineral reserves. The petroleum technologists have an edge on their metallurgical brothers for they have better tools for exploration. This is not to say that the mining geologist has to depend on hunches or the divining rod. The outstanding work on orogenesis by Lindgren and others has provided the mining geologist with some sound scientific knowledge as to where accessible metallic minerals are most likely to be found, As Clinton H. Crane has recently observed, most of the accessible areas of the earth have been combed for easily identified outcrops, and those have been or are being actively exploited. To find ore bodies hidden below the surface is still a costly speculation.

Jan 1, 1946