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By Ira Joralemon

THE sampling of disseminated copper deposits has been described often but the method of combining assays, to give the true shape and value of the orebody as it will be mined has received less attention. As the ore mined during five or ten years at several of the great disseminated properties has averaged materially lower in grade than the published estimates, the question of the sampling and estimating of these orebodies seems timely. In this paper, attention is given particularly to factors that may cause errors in the final estimate. Sampling of diamond-drill holes, churn-drill holes, and underground workings is briefly described in the first part of the paper; then the method of combining assays to give the average grade and tonnage that will be mined is taken up in some detail. The necessity of study of the geology of the deposit and of probable costs is emphasized. Finally, the methods of calculating tonnages are outlined. DIAMOND-DRILL SAMPLING There are three main requisites for accurate diamond-drill sampling. First, the core should be removed and the hole cleaned out at the beginning of every sampling interval, usually 5 ft. (1.5 m.). After the rods are let down, water should be run through them until it becomes clear. The water must be clear before drilling starts. In this way the material knocked down from the sides of the hole by the descending rods is washed away, instead of being left to salt the sludge, sample.

Jan 2, 1922

YEARS ago, when metal mining was more an adventure than a well-organized business, it was often said (with some color of truth) that unless a mine could stand bad management or mismanagement, it was not much good. Today, the natural excellencies of an ore deposit are merely a challenge to the engineers to exploit it as skillfully, as efficiently, and as profit- ably as possible. A vast amount of competent and imaginative engineering management (which includes economic analysis no less than the technologic arts of mining ore and treating it) has been required to make New Cornelia the smooth-running and successful operation that can be seen at Ajo today. New Cornelia was acquired by the Phelps Dodge Corporation when it absorbed the Calumet and Arizona Mining Company in 1931. Next to Morenci, it doubtless is the corporation's biggest asset. It in no way detracts from the achievement of Phelps Dodge engineers to say that they had an admirable ore deposit to work on. New Cornelia ore, as mined, is relatively low in grade and the deposit is by no means the largest of the Porphyries; but it has these attractive features : (1) It is peculiarly suitable for opencut mining because: (a) The overburden of waste rock lying above the ore deposit was (it has long since disappeared) almost negligible. (b) The deposit is roughly circular in horizontal section, with the horizontal dimensions four to five times as great as the maximum thickness. (Nevertheless, eventually some underground mining may be desirable.)

Jan 1, 1957

By Lawrence A. Garfield

From the bottom of a shallow fissure the near-naked man-animal hacked out a hand-sized chunk of the red rock-like material which, when beaten between other rocks, could be drawn out to the thinness of a flint edge. Unlike flint, however, it did not shatter when, as the point for a spear or arrow, it went wide of its mark and fell amongst the rocks or tree branches. For this reason and others, the red rock- like material was specially sought and much time was spent in trying to break it from the real-rock in which it grew. Only infrequently was a chunk broken free and in this area many hours had been spent to win but a few fragments. What luck then, to remove so large a piece where before nothing but real-rock dust formed whenever the stone hammer hit. Why did this happen? Did yesterday's food-fire, burning on top the red rock, loosen its hold on the real-rock and cause it to break free when struck with the stone hammer? It is not a matter of recorded history that the first heat assisted extraction of native copper from country rock occurred under the circumstances or in the manner related but it is known that crude mining operations using these techniques were conducted by primitive man. In this way the first mineral production may have been achieved and the original example of rapid excavation unknowingly given to the world. Rapid excavation is not a method of removing rock or ore from an insitu condition nor does the term refer to a type of equipment which is specifically employed in mining and underground construction. It is, rather, the nomenclature currently popular in industry-primarily in underground construction- relating to a comparative rate of performance.

Jan 1, 1971

By T. S. Fuller

The tensile properties of steels at elevated temperatures have been studied by numerous investigatorsll primarily for the purpose of determining their suitability for structural uses. Tests with this objective have been confined largely to the temperature range of approximately 20" to 500' C., because of the rapidly decreasing tensile strength at the latter temperature. Tests have also been extended to higher temperatures2 for the purpose of determining the most suitable forging range. This temperature range is also of theoretical interest. The phenomenon if increased tensile strength and decreased ductility .in the so-called "blue-heat" range, approximately 200" to 300" C., is well known. It was suggested to the Bureau early in 1926 that a study of the properties of rail steels in this temperature range might prove of interest in relation to the studies of transverse-fissure failures in rails. There were available from another investigation3 several new rails from several different heats made to approximately the same specification requirements, the complete manufacturing histories of which were known. It was decided to determine, at least in the preliminary series of tests, only the ultimate tensile strength, elongation and reduction of area, because of the difficulty, time and cost involved in determining the proportional limit and yield point at elevated temperatures.

Jan 1, 1930

By D. J. DeLazaro, D. W. Levinson

Observations were made of the isothermal transformation and quench and reheat transformation characteristics of binary titanium alloys containing nominally 6 wt pct and 10 wt pct Mn at temperatures of 700°, 600°, 500°, and 400°C. A large change in electrical resistivity attends the beta to alpha transformation in these alloys. The correlation between the resistivity and microstructure provides a very sensitive means of following the transformation. IN a recent paper, Wyatt' determined the electrical resistivity of several grades of unalloyed titanium metal as a function of temperature. In addition to the expected discontinuity accompanying the a-B transformation, it was shown that s-Ti has a much larger temperature coefficient of resistance than 8. The result would be a very large change in resistivity attending ß?a: transformation if it were possible to retain the ß structure at room temperature in pure titanium. From these data, it was reasoned that this very large resistance change should accompany the decomposition of the ß phase in alloys in which the ß phase can be retained by quenching to room temperature from the ß field. This effect is illustrated schematically in Fig. 1. Binary Ti-Mn alloys containing more than 5 wt pct Mn can be quenched to retain ß from the ß field. While the ß phase would be expected to transform in these alloys to a + TiMn via a eutectoid reaction,' it has been observed that the eutectoid decomposition does not occur readily in hypoeutectoid alloys, but rather the decomposition of the ß occurs by rejection of proeutectoid a only." Thus, the resistivity should show a marked decrease, as the a: phase is rejected from ß and a study of the resistivity of solution treated and isothermally transformed or quenched and reheated alloys should provide an excellent means of establishing the transformation kinetics of these alloys at various temperatures. The usual metallographic method of determining the transformation temperature-time characteristics of alloys of this type is very satisfactory for deter- mining the time required to initiate the rejection of the a phase at temperatures relatively close to the ß/a: + ß boundary when the rejected a is coarse, and a typical Widmanstaetten structure is produced. The metallographic method is less satisfactory for this purpose at lower temperatures where a fine nodular decomposition product is observed and is very unsatisfactory for the determination of the time required to complete the transformation at any temperature. Accordingly, specimens were prepared for resistivity measurements in order to determine the transformation characteristics of the alloys.

Jan 1, 1955

By J. Ellzey Hayden, Lucien Eaton

The Cliffs Shaft mine of the Cleveland Cliffs Iron Co., located in the city of Ishpeming, Mich., is the largest producer of hard hematite ore on the Marquette iron range. The two shafts, A and B, lying 820 ft. (250 m.) apart on the east-west trend of the ore formation, were sunk in the early eighties, and, except for four years, have been steady producers of iron ore. Their location, on a hill overlooking the general offices of the company on the one side and the city of Ishpeming on the other, has made the shaft houses landmarks. In the spring of 1919, as the old wooden shaft houses had become shaky and out of line, and would soon be unsafe, it was necessary to replace them with the least possible delay. Three plans of construction were, therefore, considered: To replace the old shaft houses by somewhat similar structures made of wood; to use steel and radically change the design; or to build reinforced-conerete shaft houses outside of the wooden structures, completely enclosing them. The first plan was disapproved, because it is anticipated that the mine will have a long life and the proximity of other buildings makes the danger from fire rather great. Delay in receiving material, and the necessity for closing the shafts during erection, were other factors in the situation. The second plan was disapproved on account of the high cost of steel, slow delivery, and interference with hoisting during the period of erection. The presence near one of the shafts of a large bed of hard gravel suitable for concrete made the cost of the third plan considerably less than the second, and little, if any, delay in hoisting was expected. Our expectations in this regard were fully realized. Furthermore, the work could be done by unskilled labor, which was plentiful, and the erection could be quickly started. When the proposition was submitted to W. G. Mather, president of the company, he recommended that, on account of the prominence of the buildings due to their location, an effort should be made to combine in the design as far as practicable something of architectural beauty. Following his recommendation, the original plans were submitted to the

Jan 1, 1922

By T. A. Rickard

In a previous paper (ante, p. 411) some description was given of the occurrence of the auriferous alluvium, extensive deposits of which lie among the highlands of the province of Otago, New Zealand. The present paper will describe some of the methods by which that alluvium is exploited. The alluvial mining of New Zealand is not yet hindered by " debris legislation." The mines are for the most part situated in a country of little agricultural value, and large rivers with rapid currents act as tailings conveyors. In time, however, steps will have to be taken to restrict the discharge into the Clutha of the tailings which are slowly raising the river-bottom. The methods of California have been followed in Otago with such alterations as peculiar local conditions require. The distinctive feature of the alluvial mining of Otago is the prominence given to the hydraulic elevator. The all-important factor in this form of mining is the control of an abundant water-supply at a suitable height above the level where it is to be utilized; and in this respect the gold-fields of the south island of New Zealand are most favora-

Jan 1, 1893

By A. M. Gaudin

UNTIL recently little attention has been paid to the effect of particle size on flotation. This has been especially true of material finer than 200 mesh.1 Particles of different sizes must behave differently in a flotation circuit; increased information along this line would be of practical use as well as of theoretical interest. The object of this study has been to determine what effect particle size has on floatability. The problem has been approached in two ways. One method consisted in a study of samples of the final products of several mills. These samples were sized and each size-product was analyzed for its important constituents. Bakelite briquettes2 of some of the products were made and studied under the microscope. This investigation is being continued, with particular reference to quantitative microscopic analysis of intermediate products of flotation plants. M In the other method of study, mixtures of pure minerals were ground to different degrees of fineness and floated. The products were then sized and analyzed. A study of the behavior of mixtures of pure sized minerals would have been illuminating, but after trial it was considered impractical on account of the tediousness of the large amount of elutriation required and the fact that the mineral particles would oxidize while being sized, preparatory to flotation. Broadly speaking, the following conclusions have been reached: 1. Results obtained by the two methods of study are in agreement. 2. The usual notion about the relative ease of flotation of very fine particles does not agree with the facts: 3. There is a time sequence of flotation with regard to particle size, the medium coarse particles floating first. 4. No successful method of floating extremely fine pulps has been found. 5. Recovery is optimum in a certain well-defined size range. 6. Selection is optimum in another well-defined size range.

Jan 1, 1931

By H. W. Graham

THE young metallurgist of today who thinks casually of the technical literature of the steel industry might conclude that little has been published concerning the Bessemer process. This conclusion is true as relating to the last decade or two, but there is a fairly voluminous Bessemer literature in the period of 1860 to 1910, Since that time, however, an entirely new level of metal-lurgical knowledge of steelmaking has been reached; and the present paper is simply an effort to look broadly from this new level and to bring the recorded history of the process up to date, It is an effort to appraise the acid Bessemer method of steelmaking in the light of today's technical knowledge thereof. In this paper matters of history will be dealt with only insofar as they contribute to an understanding of today's situation. Attention will be directed to the apparent causes of past developments in seeking to perceive the true direction of trends now in existence and effective as bearing upon future developments. The paper will discuss the economics of the Bessemer process, but only to the extent that will bear upon the metallurgist's understanding of his respon-sibility. The problem of the quality of Bes-semer steel will be reviewed and examples will be given of the technical data upon which the reasoning of the paper is based, Matters of engineering design, mechanical maintenance, operation and metallurgical investigation will be surveyed. Compari-sons will be made between the Bessemer and open-hearth processes for the sake of clear and ready understanding,

Jan 1, 1940

By Howard S. Bryant

The year 1928 has recently.passed from the picture and it is at this time that the various divisions of the oil industry are giving thought to plans for the present year. The outstanding characteristic of the industry in 1928 was the successful curtailment of oil production to the market's needs. It has been thought advisable to look ahead and endeavor to anticipate the oil demand for the coming year, and thus determine the volume of oil that can be safely produced without causing major additions to surface stocks. The year has been one of smaller additions to stocks than in 1927, a record demand for oil products, and a further developed spirit of cooperation among oil producers, as well as various other achievements. It is well to pause and take stock of ourselves. Present Status of Crude Oil Supply and Demand The total daily new supply of oil is at this time1 about 2,960,000 bbl. per day, made up of 2,585,000 bbl. domestic crude production, 125,000 bbl. casinghead gasoline, and 250,000 bbl. of imports. With the present low consumption, due to the falling off in the winter season demand, it is estimated that about 150,000 bbl. a day are now being run to storage, and that the first three months in 1929 will see large-sized additions to storage. Consumption plus exports of oil have increased at a regular rate from year to year, and although oil production in 1928 passed the 1,000,000,-000 bbl. mark for the second time in the history of the United States, with a production of 25,000,000 bbl. more than in 1927, only 30,000,000 bbl. were added to storage during 1928. This is compared to an addition of 65,500,000 bbl. in 1927.

Jan 1, 1929

By J. R. Long, E. L. Anderson, R. S. Dean, F. S. Wartman

TITANIUM has been estimated to comprise about 0.65 per cent of the earth's crust and ranks fourth in abundance among the metallic elements suitable for engineering uses. In spite of this, applications of titanium for structural purposes have not as yet been developed. Its commercial exploitation has been largely confined to the chemical industries and the production of paints and pigments; no doubt because of the difficulties that lie in the way of preparing the pure ductile metal. Published reports, however, indicate that ductile titanium can be prepared and possesses some unique properties. This, together with the occurrence in this country of several important titaniferous deposits, has led the Bureau of Mines to investigate processes for the production of metallic titanium, 'methods required for its fabrication, and the properties that may be produced in this interesting metal. METHODS OF PREPARING METALLIC TITANIUM Many early investigators claimed to have isolated metallic titanium; but in the light of present knowledge, it seems that they really had produced various mixtures of carbides and nitrides that have a metallic appearance but are brittle, hard, and unworkable. The first metallic titanium pure enough to be malleable when cold was produced by Hunter1 in the early part of the twentieth century. Kroll,2 van Arkel,3 and Fast,4 subsequently confirmed the facts that pure titanium is a ductile metal and that small amounts of impurities were responsible for previous reports of brittleness. When heated, titanium reacts chemically with various gases, such as hydrogen, oxygen and nitrogen; if the volume of gas thus absorbed is too great, the metal becomes brittle and unworkable. The principal difficulty in making ductile titanium is prevention of such contamination, and the success of a given process may be judged by the completeness with which it solves this difficulty in a practical manner. Of the gases mentioned, hydrogen is the least objectionable, since its absorption by the metal is completely reversible and, although dimensional changes occur and absorption of hydrogen embrittles the metal, the gas may be removed readily by heating in a high vacuum for a short time. On the other hand, the absorption of oxygen or nitrogen results in the formation of permanent 'solid solutions of the oxide and nitride, which cannot be decomposed by the strongest reducing agents2 with sufficient completeness to restore the inherent ductility of the metal. Because of

Jan 1, 1946

By J. de la Vergne, L. O. Cooper

The hydrostatic steel mine shaft liner (HSL) Provides a permanent wall lining for drilled shafts. It is watertight and suitable for bad ground conditions. After a shaft has been drilled to its full depth, the HSL is lowered into it and secured in place with cement grout. The liner consists of a cylindrical steel shell usually reinforced with exterior stiffening rings. The shell is basically designed for compressive strength and the rings are provided to give the shell added resistance to buckling. There are no published standards for the correct procedures to design an HSL. This paper gives a method that appears logical. A design solution can be complex with increased opportunity for error. This paper presents simple formulas to produce sufficient accuracy for construction design. Two new concepts are presented, referred to as transition pressure and critical pressure. An example demonstrates use of the formulas and concepts presented. To facilitate comprehension and use of the formulas, Greek letters are avoided and most of the English alphabet symbols used refer by association to their definitions. An appendix shows derivation of the formulas.

Jan 1, 1984

By A. T. Tye

REGARDING the results of preferential flotation at Cananea, Weinig has stated that "The concentrating mill of the Cananea Consolidated Copper Company at Cananea, Mexico, furnishes an excellent example of modern flotation practice. The complete figures are given because they present so forcibly the advantages of modern selective flotation."' L. O. Howard notes that "Perhaps the outstanding example so far published of improvements in results through the use of selective flotation is that at Cananea, Mexico." The following notes indicate the conditions under which the results were obtained at Cananea; also the effect of preferential flotation at the concentrator and at the smelter. In the majority of cases the full benefit of selective flotation is not fully realized, as the concentrates are shipped from the mill to smelters owned by other companies. The saving made at a certain concentrator by this method of flotation may be well understood but the saving resulting at the smelter from the results of preferential flotation at the mill is not so apparent, as the data are contained in the smelting records of some other company. Even at the smelter the great gains following preferential flotation may not be noted, as a variety of ores and concentrates from various sources are received and the difference from the changed concentrator operations of a certain mill may be obscured. As noted by Professor Weinig and Professor Howard, the results obtained at Cananea brought about a veritable metallurgical revolution at the smelter. There are probably plants at which a better preferential separation is being made than at Cananea. Many ores contain barren iron pyrite which, when depressed, does not carry copper into the tailing. Some concentrators use clean uncontaminated water for milling and in others the ore is ground much finer than at Cananea. All of these items are concerned in perfect separation. The details of preferential flotation at Cananea, therefore, are not presented on account of the perfection of the

Jan 1, 1928

By William Alden

A GREAT landslide occurred on June 23, 1925, in the valley of Gros Ventre River, about 35 miles south of Yellowstone National Park (Fig. 1). The relations of the north-easterly dipping rock formations of the slide scarp and of the dam formed by the slide are shown in the diagrammatic cross-section of the valley (Fig. 2). This generalized section is based on unpublished maps and notes by Eliot Blackwelder, in the files of the U. S. Geological Survey. FIG. 1.-MAP SHOWING SCARP AND DAM (LARGE DOTS) AND LAKE (CROSS-LINED) FORMED BY LANDSLIDE BLOCKING GROS VENTRE RIVER. (Scale 1, in. = 1 mile; contour interval 100 ft. From Grand Teton and Mt. Leidy topographic maps). Heavy rains and melting snow in the Gros Ventre Mountains had saturated clay layers in the Carboniferous strata, which dip toward the valley at angles of 18° to 21°, consequently an enormous mass of rock at the end of the north spur of Sheep Mountain became loosened and, on the afternoon of June 23, slid suddenly down into the valley. Within a few minutes this mass of debris-estimated as 50,000,000 cu. yd.-carrying

Jan 1, 1928

By E. R. Force, W. F. Cannon

Many large high-grade manganese deposits occur in marine-transgressive sedimentary sequences deposit fed on stable platforms, although the manganese mineralogy varies from carbonate to oxide facies and host lithologies vary from carbonate- to clay-dominated sections. Examples include the Nikopol and related deposits of the Soviet Union and Groote Eylandt, Australia. Recent work has shown that high sea-level stands are synchronous with stratified and stagnant oceans. We suggest that during transgressions and consequent anoxic events, the anoxic deep waters rich in dissolved manganese were dilute ore-forming fluids. Manganese was precipitated on the oxidized side of oxidation and alkalinity interfaces on shallow shelves. Where the precipitate was preserved, manganese ac- cumulated into ore deposits. Sedimentary manganese deposits have not been widely explored for in North America, nor are they always obvious in outcrop. Large areas of North America are underlain by rocks that we consider broadly favorable for such manganese deposits, and the disparity between the high potential but significant reserves of the United States is difficult to reconcile. Important undiscovered deposits seem likely. An area of Cretaceous rocks in South Dakota is presented as a possible location for a United States deposit analogous to foreign deposits described herein.

Jan 1, 1983

By R. Hogg

Sintering is a process in which the pore structure of an agglomerated powder is modified. For many applications, it is desirable to be able to control the pore structure in order to optimize such properties as mechanical strength and reactivity (availability and accessibility of solid surfaces to reactant gases, for example). In general, these properties will be determined by the total porosity and the pore size distribution of the agglomerate. In the work described in this paper, a physically realistic mathematical model for the sintering process has been developed. The model is based on the usual assumption that the pore system in an agglomerate can be treated as a network of interconnecting, cylindrical pores of continuously varying size. It is further assumed that the total pore length is conserved during the course of the sintering process. Using standard expressions for the rate of shrinkage of an individual pore, the model can be used to predict the changes in total porosity and pore size distribution as sintering proceeds. Experimental pore size distributions, obtained by mercury intrusion porosimetry, for the sintering of oxides appear to be in general agreement with the predictions of the model.

Jan 1, 1977

By John S. Bell, J. M. Shepherd

pressure difference of 280 psi measured initially on opposite sides of the major fault in the Hawkins Field led to pressure determinations in the Woodbine sand throughout the East Texas basin. Considering the large area, there is unusually good correlation between pressure losses and points of major withdrawals, these losses indicating that the basin pressure has been materially reduced by withdrawals, primarily from the East Texas Field and secondarily from the old fault-line fields of Limestone and Navarro counties, with the pressure loss varying inversely with the log of the distance from these two main areas of basin withdrawals to the measurement points. Apparently faults located throughout the basin serve as local blocks to continuous pressure gradients. INTRODUCTION The pressure anomalies found in the Hawkins Field, Wood County, Texas,' shortly after discovery have led to an area-wide investigation of the pressure distribution within the Woodbine sand of the East Texas basin. These pressures were obtained by drill-stem tests made for that sole purpose while drilling wildcat wells to deeper horizons. The Woodbine sand of Gulf Cretaceous Age is or has been productive of oil and gas in 42 different fields, with the 28 oil fields currently active having produced 118,000,000 bbl of oil during 1949. With one exception, producing energy for all Woodbine reservoirs has been from water drive provided predominantly by expansion of the tremendous volume of water contained in the Woodbine sand. This producing mechanism was recognized at an early date and was described mathematically by

Jan 1, 1951

By John S. Bell, J. M. Shepherd

pressure difference of 280 psi measured initially on opposite sides of the major fault in the Hawkins Field led to pressure determinations in the Woodbine sand throughout the East Texas basin. Considering the large area, there is unusually good correlation between pressure losses and points of major withdrawals, these losses indicating that the basin pressure has been materially reduced by withdrawals, primarily from the East Texas Field and secondarily from the old fault-line fields of Limestone and Navarro counties, with the pressure loss varying inversely with the log of the distance from these two main areas of basin withdrawals to the measurement points. Apparently faults located throughout the basin serve as local blocks to continuous pressure gradients. INTRODUCTION The pressure anomalies found in the Hawkins Field, Wood County, Texas,' shortly after discovery have led to an area-wide investigation of the pressure distribution within the Woodbine sand of the East Texas basin. These pressures were obtained by drill-stem tests made for that sole purpose while drilling wildcat wells to deeper horizons. The Woodbine sand of Gulf Cretaceous Age is or has been productive of oil and gas in 42 different fields, with the 28 oil fields currently active having produced 118,000,000 bbl of oil during 1949. With one exception, producing energy for all Woodbine reservoirs has been from water drive provided predominantly by expansion of the tremendous volume of water contained in the Woodbine sand. This producing mechanism was recognized at an early date and was described mathematically by

Jan 1, 1951

OUTSTANDING symbol of the machine age, the steam shovel needs no introduction. Few individuals there are, in the United States at least, that have not watched with fascination the almost human motion, the more than human strength, the rhythm of the whole steam-shovel cycle of crowding, digging, swinging, dumping, swinging, and crowding again. A mass of steel with some copper and other metals, fed with water and coal, guided by a single alert and dexterous operator, or perhaps two, does the work that would require 50 to 500 men or even more. The largest shovels working in the copper mines have loaded into waiting railway cars as much as 10,000 tons of ore in a single 8-hour shift. With no equipment but hand shovels, it would, in fact, be impossible to duplicate the work with any number of men; first, because they would be in each other's way, and second, because the steam shovel can lift single pieces of rock weighing 5 or 10 tons with effortless ease. Of recent years, internal-combustion engines and electric motors have displaced steam as a motive power in many instances; and of course the detailed design of the shovels has been improved immensely. Whereas the largest dippers used 30 years ago had a capacity of 3 ½ to 4 cu. yd., today the 350-ton shovel used at Chino has an 8-yd. dipper, as has the 320-ton shovel at Chuquicamata. Incidentally, for stripping at coal mines a shovel having an 18-yd. dipper is in use. However, the principle of operation of the modern shovel, regardless of the size and type of motive power, is essentially the same as that of the earlier shovels. It is fair to say that the indispensable of open-cut mining is the steam shovel, or, to be more precise, if perhaps less picturesque, the power shovel. Somehow the electric shovel seems to lack the glamour that

Jan 1, 1933

By B. N. Das, H. E. LaBelle, G. A. Wolf

ZnxHg1-xTe and GUPxAS1-x crystals have been grown from solution by a traveling heater method (THM). In a floating zone type fashion a solution zone sandwich of liquidus composition is made to migrate through feed material of solidus composition by a slow-speed movement of <0.25 mm per hr of the total charge through a stationary radiation or rf heater. ZnxHg1-xTe of composition 0 < x < 0.3 and GUPxAS1-x of composition 0.5 < x < 0.7 have thus been grown from their solution in liquid tellurium and gallium, respectively. A simplified analysis of heat and material transport is given. In this method, Proper adjustment of the temperature distribution along the liquid solution zone axis eliminates instability of the crystal growth front and constitutional supercooling. 1) ZnxHg1—xTe: The solid-solution telluride was grown in sealed quartz tubes at a temperature of 500 to 650°C. For first Preparations mechanical mixtures SINGLE crystals of solid solutions of III-V and II-VI compounds have been grown by various techniques from the melt, from the gaseous phase, or from solutions in of ZnTe and HgTe were used. X-ray determinations showed the resulting crystals to be homogeneous throughout their entire length, except for the end sections. The homogeneity is greatly improved by reusing the ingots obtained from first Preparations as feed material in subsequent crystal growth runs. Ingots of up to 4.5 cm have thus been obtained. 2) GaPxAs1-x: Crystals were grown in a EN crucible at a temperature of 1050°C. For first Preparation a mechanical mixture of Gap and GaAs was cemented together by a minimum amount of liquid gallium through "wet" grinding of Gap and GaAs crystals in the liquid metal and subsequent exuding of excess gallium by compacting of the charge in the EN crucible. Electron microprobe measurements using P-Ka and As-Ka radiation showed uniformity over a length of 0.4 cm. Properties of the various Preparations are described. liquid metals.&apos;-&apos; Their growth from the melt by passing a liquid zone of pseudobinary liquidus composition through a solid rod of solidus composition is generally a convenient method of growth of single crystals of solid solutions of homogeneous composition. This method loses much of its usefulness, however, if the melting point or the vapor pressure of the solid solution is high. In the case of a compound having a high melting

Jan 1, 1969