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By R. R. Klimpel Discussion by C. C. Harris, L. G. Austin

C. C. Harris (Columbia University) — The authors ' have presented relationships for the random division of a magnitude into r + l parts taking account of the order of selection. Interpreting their model in comminution terms, their Eqs. 7, 9 and 11 refer to the one-dimensional case; that is, to the subdivision of a long thin rod at random. It is assumed that the fragments may be indefinitely small. Real materials, however, are limited in the degree of subdivision which can be attained through the intervention of practical restrictions. One in fine grinding is the depletion of microflaws as material becomes finer. Another is the

Jan 1, 1969

By W. L. Zeigler

THE gravity concentrator of the Hecla Mining Co. was originally constructed in 1888 by the Milwaukee Mining Co., which was operating the Gem of the Mountains mine. It was purchased by the Hecla Mining Co. in 1900, and placed in operation 2 years later. At that time [ ] the capacity was only about 200 tons a day, but many additions and changes in equipment have been made so that the present capacity is about 800 tons. One of the outstanding improvements made was the substitution of Callow flotation cells for vanners, which occurred in 1915. The recent building of a flotation plant for treating jig tailings, and the construction of a modern surface plant at the mine, following the

Jan 1, 1928

By M. L. Fuller

IN connection with an investigation in this laboratory on the high-zinc side of the copper-zinc system, it was observed that well developed segre-gate structures of the Widmanstätten type were formed when a secondary phase precipitated from the solid solution of copper in zinc. This paper presents an analysis of the crystallographic relationship between the segregate and the solid solution matrix. The data to be presented are an interesting addition to the literature on segregate structures in that the plane of segregation is one of the less densely populated planes. In agreement with the generalization of C. H. Mathewson and D. W. Smith1 the plane of segregation in the matrix con-tains the direction of closest atomic packing of the lattice. Furthermore, the matrix and the segregate are both hexagonal close-packed, which has not been reported hitherto in the literature.2 The increasing com-mercial importance of zinc alloys containing copper makes this funda-mental study of value to the metallography of zinc alloys.

Jan 1, 1933

By J. S. Wakeman

The techniques of testing the physical properties of green pellets produced in a batch balling test are described. It has been found that these physical properties, i.e. drop resistance, wet compressive strength, and plastic deformation under load, are generally related to the moisture content of the wet balls. A "criterion" method of analyzing data from a series of batch tests is discussed. This method facilitates the comparison of results of various test series. A time-sharing computer program, which correlates the test data from a batch series, generates the "criterion" values for subsequent comparison and analysis, and produces X, Y plots of the various moisture-strength relationships, is presented. Examples of computer output and use of the "criterion" evaluation method are given.

Jan 1, 1973

By B. D. Thomas

GRAVITY concentration is a general term designating processes for separating and sorting granular material by means of forces that depend on the density, size and shape of the particles. When these forces are applied to the particles the latter are caused to move, those of a given density along one path and those of a different density along another, until ultimately they are sufficiently separated to be removed from the operation of the process. The forces producing this separation are in general complex and, unfortunately, no completely rigorous analysis of them has as yet been devised. The science of the hydrodynamics of viscous fluids deals with the little that is known about the problem. Every observer of nature is familiar with the fact that an object moving in a fluid encounters a force of resistance. We have only to walk against a brisk wind or stir a cup of coffee, or observe the slow fall of a grain of sand in water, to experience directly the fact that such forces exist. The exchange of force between an object and a fluid in which it is moving operates on the fluid as well as on the object. Thus a sailboat may be set in motion by the force exerted by the wind on the sail; but the sail also deflects the wind-furthermore, the water in which the boat floats is set in motion by the force exerted by the boat as it cleaves through the water. The wind is thus enabled to do work on the water through the intermediary of the boat. In general, an object moving through a fluid encounters a force that opposes the motion and also acts to change the motion of the fluid. In gravity concentration we are dealing with this force of resistance acting on the granular particles that are to be separated. Furthermore, the motion induced in the fluid by a particle will in turn affect the motion

Jan 1, 1943

By G. R. M. Del Giudice

The term "slime-coating" is not new in the art of flotation; the phenomenon has been observed and described by Taggart;(l)† Taggart, Taylor, and Ince;(2) and by Ince.(3) Notwithstanding that flotation was introduced for the treatment of finely crushed ore, the adverse effects of slimes have been recognized since the earliest days of the process, and the Elmore, Delprat, Potter, and other processes actually specified desliming of the ore prior to treatment. The cause of this trouble has been studied and described by Taggart;(1) Taggart, Taylor, and Ince;(2) Ince;(3) Morrow and Griswold;(4) and by Gaudin and Malozemoff.(5) Old Theory of Slime-coatings At present, so far as published work shows, there seems to be but one theory for the mechanism of slime-coatings. Ince(3) states that they are due to attraction between electrostatic charges of opposite sign on the sulfide and on the slime particles, supporting this theory by migration experiments in the Burton tube. He also used the microscope in conjunction with a glass cell employed by Beans and Eastlack(6) in studying migration, but met with interference from endosmosis. Several attempts have been made in the Department of Mineral Dressing at Columbia University to duplicate Ince's experiments with the Burton tube, but the results have never been convincing. Formation of precipitates which settled through the pulp levels, and evolution of gas at the electrodes, which disturbed the interface between the pulp and the distilled water above it, seriously interfered with observations. However, by use of the migration cell shown in Fig. 1, endosmosis effects and the disturbances due to precipitation and gas evolution were avoided, and distinct and reproducible migrations or absence of migration were observed. The cell was made of bakelite and had platinum electrodes. Objectives were employed which had a working distance of at least three millimeters,1 and the parts of the mounting which came in contact with

Jan 1, 1935

By Frederick Laist

THE ore from the Butte mines of the Anaconda company is quite siliceous; that is, it contains considerably less iron than is needed for the fluxing of the silica. The direct smelting of this ore, therefore, requires the addition of considerable fluxing material. The only flux available in sufficient quantity at Anaconda is limestone containing no metallic minerals. This necessarily makes the direct smelting of the ore so expensive that it is more profitable to subject the ore to a preliminary treatment by concentration. However, as the losses in the concentrator were very high, compared with the losses in the blast furnaces, it was found, by calculation, more profitable to send ores containing more than a given percentage of copper to the blast furnaces, in spite of the higher costs of treatment. The dividing point was dependent on various factors, the chief of which was the prevailing market price of -copper. It was customary, therefore, to segregate the ore as mined into two classes. Ore in the first class generally contained 5 per cent. or over of copper;: this was sent directly to the blast-furnace department. Second-class ore contained less than 5 per cent. of copper, and averaged around 3 per cent.; it went to the concentrating department. With the introduction of the flotation process, it was found possible to maintain an average recovery, as concentrates, of 96 per cent. At the same time, the cost of reverberatory smelting was very materially decreased by the use of pulverized coal. These two changes in practice made the blast furnaces unable to compete with the reverberatory furnaces on a cost basis. The distinction between first-.and second-class ore was therefore abandoned, and the ore was treated by concentration. Obviously, on ores as high in iron as the Butte ores, the concentrator, produces a product that is self-fluxing; in fact, it is possible to produce a

Jan 1, 1920

By Dan White

Stress measurements taken at Climax, El Teniente, Henderson, Lakeshore and Urad mines indicate that the deposits cited are generally subject to an inclined stress field that can be highly anisotropic. The horizontal stresses vary significantly between deposits and exceed the measured vertical stresses at Henderson and El Teniente mines. Experience at Henderson, Lakeshore and Urad mines is used to suggest a relationship between cavability and the premining stress. In poorly fractured, high strength rock masses, high stresses can assist the caving process. In well fractured, low strength rock masses, caving is ensured by breakage along fracture planes. The relationship between ground weight and the premining stress is also investigated. Ground weight problems appear to be most related to the competence of the ground rather than the magnitude of the premining stress as supported by experience at Climax and El Teniente mines. Recent developments in block caving favor the extraction of poorly fractured, high stressed rock. Accompanying the development of these deposits are new problems such as rock bursts. These pose particular problems to mine designers in that no experience currently exists in combatting rock burst problems at block caving mines.

Jan 1, 1984

A regular feature of the December issue is to be abstracts of graduate theses in the mineral industry field presented during that year. The following abstracts were submitted for this first article in the series.

Jan 1, 1975

By R. T. O’Brien, J. M. W. Mackenzie

A microelectrophoresis technique has been used to measure the zeta potential of quartz over a range of pH and Ni (11) and Co (Ilj concentrations. Results have been discussed in terms of adsorption of Ni (11) and Co (11) cations and hydroxide precipitates. Possible relationships between the experimental results and the formation of lateritic nickel deposits have been discussed. The adsorption of metallic cations to the surface of silicate minerals is of significance in many industrial and natural processes. In an earlier publication,' the adsorption of Fe (111) to the quartz surface, a phenomenon of importance in flotation, was studied qualitatively using microelectrophoresis techniques. This paper reports the extension of this work to an investigation of the adsorption from aqueous solution of Co (11) and Ni (11) to the quartz surface. The adsorption of these metals was of interest for two reasons; firstly, the importance of such an adsorption process in the formation of nickel deposits by the lateritization of nickeliferous rocks, and secondly, the comparison of electrophoresis data for these metals, whose hydroxides precipitate in the pH range 7-8, with similar data for Fe (111) where the hydroxide first precipitates at pH 2.8. The development of laterites is essentially a near-surface geological process involving vertical and, in part, horizontal redistribution of elements derived from rock-forming minerals. This redistribution of elements leads to the formation of layers within the lateritic profile which are enriched in one or more of these elements and, depending on the nature of the original rocks, continued lateritization may give rise to iron ores, bauxites or nickeliferous laterites. The mechanisms discussed in this paper deal with the last mentioned type of deposit although the considered factors are applicable to laterites in general. Nickeliferous laterites are derived from basic and ultrabasic rocks containing ferro-magnesian silicates. These rocks may be partly or wholly converted to serpentinites. Besides their high Mg, Si and Fe contents, they also contain small amounts of Mn, Al, Cr, Ni, Co, Cu and Zn. The nickel content is usually near to 0.2-0.3%, but for economic use this must be increased during lateritization to over 1% and preferably over 2%. The zone of nickel enrichment is usually at some depth within the lateritic profile. Unpublished work by Mr. O'Brien on nickel-bearing laterites in eastern Australia indicated four visually different types of material which were separated from crushed samples under a stereo-microscope. Although chemical analyses indicated that all four types of fragments contained 2-4% nickel and smaller amounts of cobalt, X-ray diffraction and optical studies revealed only quartz, hematite and chromite as well as, in one of the types, a serpentine mineral. No distinct, nickeliferous minerals were detected. Furthermore, it was possible to extract some 60% of the nickel content of the laterites with cold 0.5N hydrochloric acid. It was therefore postulated that much of the contained nickel was present as amorphous, adsorbed material. In considering this fact, as well as the problem of the actual method of transfer and fixation of elements within the lateritic profile, it was further postulated that the transfer of these elements probably took place partly as solutions and partly as colloids and that the fixation of these was caused by adsorption and flocculation. The existence of nickel in solution in water draining from serpentinites has been confirmed by Smurov.2 Although we have no evidence for the transportation of nickel in the colloidal state, it is well accepted that colloids are important in the formation of laterites. Previous work by Mr. Mackenzie' has already indicated that iron may be adsorbed on quartz under conditions which could be expected in a lateritic profile, but no information was available for nickel or cobalt. Although adsorption possibly also takes place on minerals other than quartz, the latter is significant because silica is an important constituent of the silicate parent rocks. During lateritization, it is released to form free quartz and it is likely that it is initially extremely fine-grained. This would provide abundant opportunities for adsorption and it was de-

Jan 1, 1970

By E. G. De Coriolis

The development of huge production facilities and of new or improved processes for manufacturing magnesium from its raw sources has been an outstanding achievement of this war. Furthermore, at least one new method has reached a stage of pilot production that offers promise. Its potentialities seem to indicate that a reduction in cost and simplification or elimination of problems incident to the use of at least one of the present processes are quite within the realm of possibility. Although magnesium of very high purity (99.9 per cent and higher) is obtained, and the rate of recovery reasonable (60 to 70 per cent). the ferrosilicon reduction process is open to a serious objection, which at the time its use was proposed was thought to be sufficient to raise some doubts as to its success, at least on a high production basis. The temperature range at which the reaction is carried out—namely, 2100" to 2150°F.—is very close to the failure temperature of the material of which the retort is made. It is so close that for a time it was assumed it might make commercial use of the process an impossibility. However, at the time under discussion, the demand for magnesium was so great that it was felt by those who had to go ahead and produce this essential metal that the emergency warranted their taking a chance on this process. Subsequent developments have fully justified the soundness of their decision. Fortunately for the war effort, when the plants were put into operation it was discovered that although the retorts did collapse in rather short periods of time, as predicted, they could be blown back into operable shape by application of high-pressure air. This practical method of operation so relieved the situation that the problem disappeared. Nevertheless, if the process had not been successful, or the production of magnesium by the electrolytic process had not been able to keep pace with demands, our war program would have been seriously impaired. Fireless Cooker'' Process For this reason a program was set up and assigned for the development of a new method that had been suggested to the War Production Board in 1941. It is believed justifiable in terming the method "new" for several reasons: (I) while utilizing the same (ferrosilicon) process as the Pidgeon, hence involving similar reactions, the type of retort or furnace is essentially different, (2) the method of operation, reaction temperatures, etc., differ materially, and, most important of all, (3) the problems to be overcome in making the process successful were not and could not have been anticipated by anything previously known about the Pidgcon process. As will be shown later, the briquetting process, the condenser, the furnace lining

Jan 1, 1949

By W. W. Harvey, F. O. Dudas

Toward hot hydrochloric acid, the usual order of reactivities of the common copper sulfide and associated minerals is reversed, and the rates of H2S formation vary as [ ]. The iron component of chalcopyrite and bornite reports to the solution as ferrous chloride, while pyrite remains essentially unreacted. If a pressure of H2S is maintained in the reactor, copper solubilization is suppressed, and the primary copper sulfides are converted to finely divided secondary sulfides (principally covellite). The HCl leach reside then consists mainly of covellite, pyrite and acid-insoluble gangue. Copper can be selectively leached from this upgraded concentrate to yield a clean, strong copper sulfate solution for direct electrowinning. Preliminary analysis indicates competitive economics with respect to established hydrometallurgical processes. Other concentrate treatments based on an initial HC1 leach are proposed and relative advantages compared. The common denominator of the major process routes considered is the requirement to regenerate HC1 from an FeC12 solution. Five distinct concentrate compositions were employed in the experimental study, which included some attention to the fates of selected minor constituents of the copper concentrate, especially gold, silver, molybdenum, arsenic and selenium. Significant mineralogical features of reactants and products are described.

Jan 1, 1978

By W. G. SWART

THE best estimate on reserves of iron ore in the Lake Superior district is that made, in 1920, by Mr. R. C. Allen, amounting to 2,947,225,000 tons of assured and probable ore. This includes direct- shipping or so-called merchantable ores, and those capable of beneficiation by demonstrated processes. De- ducting from this the 287,000,000 tons shipped since 1920, leaves a present reserve of approximately 2,500,- 000,000 tons, or; about 50 years' supply. The assured ore in this estimate is given as 1,560,500,000 tons, which checks Mr. Lake's estimate of 1,528,948,000 tons, or about 30 years' supply. This is not a long time in the life of the steel industry, and it can be readily appreciated that the matter is important enough to war- rant the attention it is beginning to receive. The first question that engages our attention is, What is merchantable ore? In 1902 the average of all Mesabi shipments was 56.07 per cent iron and 4.35 per cent silica. Twenty-five years later it had dropped to 51.99 per cent iron, with silica up to 7.92 per cent. It has remained around these figures for' ten or twelve years and, except for a probable rise in silica, can stay there for an indefinite period. Most of these figures I am giving cover the Mesabi Range. Including the other ranges does not change the figures greatly, and the Mesabi Range commands the situation, since it produces about 65 per cent of the total annual tonnage and, according to Mr. Allen, contains 81 per cent of the assured reserves, 50 per cent of the probable reserves, and 66 per cent of both the assured and the probable reserves.

Jan 1, 1926

[RECEIPTS Magazine, Advertising $ 32,823.60 Sale of Magazines 3,933.29 Total Magazine $ 36,756.89 Dues, Arrears 5,866.97 Dues Current 100,223.80 Dues of New Members 6,143.29 Dues in advance 1,586.32 Initiation fees 6,820.00 Sale of Transactions 5,464.99 Sale of Binding 5,618.90 Sale of Pyrometry Volume 336.30 Sale of Indexes and Emmons 106.10 Sale of Pamphlets 575.32 Miscellaneous Receipts 105.60 Interest on Bank Balances 1,217.67 Interest on Life Membership Investment 512.18 Interest on James Douglas Library Fund 5,678.67 Total Receipts $177,013.00] [ ]

Jan 1, 1925

By J. L. Gillson

In this past year of our Institute's life, February 1960 to February 1961, we had some major problems to face, as did our members, since businesses in which they were engaged were feeling the recession. The major problems confronting us during this past year were: 1) Financing the new Engineering Center. 2) Keeping our three almost autonomous societies working together and toward a stronger AIME. 3) Cooperation with other engineering societies the Functional Plan. 4) Licensing and registration, and the Model Law. 5) The reorganization of the Council of Section Delegates. 6) Combatting the slump in the appeal of engineering to the young students.

Jan 4, 1961

NEW MEMBERS. The following list comprises the names of those persons who became members during the month of October, 1913: Members. BARNES, KENNETT F., Secty Granby Min. & Smelting Co., St. Louis, Mo. BILLINGSLEY, PAUL, Geol 526 Hennessy Bldg., Butte, Mont. BLANCHORD, RALPH C., Geol 3 Lombard St., London, England. BOYLE, ALBERT C., Jr., Prof. of Min. and Met., University of Wyoming, Laramie, Wyo. BRADFORD, JULIUS S., Min. Engr Chiksan Mining Co., Chiksan, Korea: CLEMES, ALFRED W., Min. Engr P. 0. Box 6,88, Moronic, Ariz. COPELAND, DURWARD, Met Cia. Estamifera de Llallagua, Bolivia, So. America. CRAWFORD, JOHN, JR., Mgr Noble Elec. Steel Co., Heroult, Shasta Co., Cal.

Jan 11, 1913

By L. D. Jaffe, J. H. Hollomon

THE effect of tempering temperature and time upon the properties of quenched steel is clearly a subject of great practical importance, as well as of considerable theoretical interest. It would be very desirable to be able to predict the properties of a quenched steel when given any selected tempering cycle, with a minimum of experimental work upon that heat or even type of steel. Two problems are involved: one consists of relating the structure obtained to the physical properties, and will not be discussed here; the other, with which this paper deals, involves the relations of time, temperature and composition with the structure obtained on tempering. Indentation hardness is perhaps the most convenient quantitative measure of the tempered structure, or of what might be called the "degree of tempering." Undoubtedly, it is not an exact measure, and in some cases (as when temper-brittleness occurs) pieces of the same quenched and tempered steel may have widely differing properties at the same hardness. However, hardness has the advantage of being simple to determine and is certainly the most widely used indication of the degree of tempering. Moreover, for fully quenched steels that are not temper-brittle and do not contain retained austenite when quenched, it appears that, in general, if the hardness of the steel is the same, the tensile and impact properties will also be identical, whether a high or a low tempering temperature is used. The tempering charts available in the metallurgical literature usually give the hardness as a function of tempering temperature for only one tempering time. However, in practice, tempering times frequently vary, and a method of converting tempering curves for one time to tempering curves for some other time would be very valuable. It is also advantageous, in determining the tempering treatment necessary for a given part, not to have to temper samples at several temperatures for the time used for the commercial tempering operation. A more satisfactory procedure would be to employ times of the order of 10 to 30 min., rather than 5 or 10 hr., and if possible to use only one temperature. Furthermore, it is frequently desirable, for reasons such as temper-brittleness,* to obtain a given hardness with short times at relatively high temperatures, and it would be convenient to be able to compute without tests the time required to produce this hardness. Remarkably few quantitative studies of the hardness of quenched steel tempered over wide ranges of temperature and time

Jan 1, 1945

By J. L. Lytton, T. E. Tietz

The recovery of flour stress of recrylstallized are-cast molyhdenum after 10 pet prestrain at 150°C was studied for recovery temperatures of 725o 801o and 901oC. The yield phenomenon observed after recovery was such that the yield drop diminished and disappeared as recovery proceeded. A fractional flow-stress recovery parameter fr, was developed and it was shown that, independent of recovery ternperatzwe, equal f, values of about 0.16 produced superposition of stress-strain curves except for the initial yield phenomenon. The activation energy for low degrees oj recovery was found to he 32,600 cal per mole, in close agreement with a reported valzie for difjzdsion of carbon in molybdenum. For values of fr greater than about 0.15 where recovery was thought to predominate over strain aging, the activation energy varied from 43,600 to 82,500 cal per mole and increased with increasing recovery and recovery temperature. A 10 pet pre-strain shifted the ductile-brittle transition temperature, as indicated by tensile elongation, from 10°C. to about -22"C. A 100-hr recovery anneal at 801oC was shown to shift the transition temperature to about —5oC, the major shift occurring during the first hour of recovery. ThE recovery of cold-worked metals is accompanied by changes in the arrangement of the dislocations generated during cold work. In recent years, the use of transmission electron microscopy has allowed direct observation of some of the dislocation configurations formed, such as "tangles", networks, cells, subboundaries, and loops. These observations have recently been reviewed by Keh and Weissmann.' Accordingly, some understanding has been gained concerning the nature of the dislocation rearrangements involved. The relationship between recovery and the decrease of mechanical strength, however, has only recently been explored. Previous efforts of the authors were directed toward investigating the decrease of tensile flow stress of aluminum and Al-1 pet Mg during recovery2 and the effects of concurrent elastic and plastic strain on the flow-stress recovery of aluminum.3 In addition, an investigation of the effect of four different solute additions on the tensile flow-stress recovery of aluminum has been made.4 Many important metals, however, have the bee crystal structure, e.g., iron, molybdenum, tungsten, vanadium, columbium, tantalum, and chromium. These metals might be expected to behave differently during recovery from those with other crystal structures for two reasons. First, the previous and present investigations of aluminum and its alloys have shown that tensile flow-stress recovery is strongly affected by foreign atoms in the lattice. In the bee metals, interstitial impurities are usually present and might be expected to have various effects upon both flow behavior and recovery. For example, heterogeneous yielding might occur during prestraining. The diffusion of these interstitials can also relock dislocations during recovery so that a yield point might be obtained upon restraining (strain aging). Second, some of the bee metals (e.g., iron, molybdenum, and tungsten) undergo the familiar structure-sensitive ductility transition and exhibit brittle fracture at suitably low temperatures. It is of considerable interest to determine the effects of recovery on the transition temperature of such metals. The purpose of the present investigation was to extend our knowledge of flow-stress recovery to the bee metals and to study the effects of recovery on the ductile-brittle transition temperature. Unalloyed recrystallized are-cast molybdenum was chosen as a test material, since it exhibits a well-defined ductility transition near room temperature. As in the previous studies, the degree of recovery was measured in terms of the decrease of tensile flow stress. Prestraining and restraining were carried out at 150°C to avoid the possibility of brittle fracture. EXPERIMENTAL PROCEDURE The are-cast molybdenum sheet used in this investigation was obtained from the Climax Molybdenum Co. of Michigan. It was 0.060 in. thick by 10

Jan 1, 1964

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 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