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By Bahrein Petroleum Company

In Comodoro Rivadavia, well 8. 132, drilled in zone No. 2, has discovered between 5205 and 5297 ft., the dcepest pool yct found in this field. The oil production in Bahrein for the year 1939 totaled 7,588,554 bbl., a decline of 709,444 bbl. from the 1939 production of 8,297,998 bbl. The production for the first seven months of 1939 remained fairly constant, the daily average by months during this period ranging between 20,000 and 22,000 bbl. per day. The daily average rose in August to the year's high of 23,800 bbl. per day, then dropped gradually to the year's low of 18,787 bbl. per day for November. The daily average for the year was 20,791 bbl. At the end of 1939 there were 59 wells producing and 8 wells drilling.

Jan 1, 1940

By Bahrein Petroleum Company

In Comodoro Rivadavia, well 8. 132, drilled in zone No. 2, has discovered between 5205 and 5297 ft., the dcepest pool yct found in this field. The oil production in Bahrein for the year 1939 totaled 7,588,554 bbl., a decline of 709,444 bbl. from the 1939 production of 8,297,998 bbl. The production for the first seven months of 1939 remained fairly constant, the daily average by months during this period ranging between 20,000 and 22,000 bbl. per day. The daily average rose in August to the year's high of 23,800 bbl. per day, then dropped gradually to the year's low of 18,787 bbl. per day for November. The daily average for the year was 20,791 bbl. At the end of 1939 there were 59 wells producing and 8 wells drilling.

Jan 1, 1940

By Clifford C. Hanninen, Allan H. Caverson

Within the past nine years a means for measuring the distance between mine roof and floor was developed at the White Pine mine which yields relevant information utilized in the mining operation. The technique known as "convergence" is an efficient, low cost way for obtaining large quantities of data for predicting roof falls, caving activity and overall mine stability. Since 1964 the activity of convergence measurements has expanded to become a production tool found in all sections of the mine. The program involves four types of activity: 1) monthly measurements in areas known to be active and in sample blocks scattered throughout the mine for a long-term stability study; 2) semi- monthly measurements along vital travel roads, belt drifts and compressor sites; 3) weekly measurements in areas where men are working; 4) daily measurements in pillar-recovery and caving operations.

Jan 5, 1973

By Nicholas Kowall, K. L. Clark

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 I938, Burns, Moore and Archer published & curve? 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 rallge found in construc-tional S.A.E. compositions. Some of the deeper hardening types investigated, however, contained carbon to a maximum of only o.2o 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 a that could be prepared for Brinell indentations. The test piece was quenched immediately after solidi fication was complete and hardness readings were taken, so that the carbon content could he 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 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 I938, Burns, Moore and Archer published & curve? 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 rallge found in construc-tional S.A.E. compositions. Some of the deeper hardening types investigated, however, contained carbon to a maximum of only o.2o 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 a that could be prepared for Brinell indentations. The test piece was quenched immediately after solidi fication was complete and hardness readings were taken, so that the carbon content could he 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 Robert C. Stephenson

LARGE deposits of titaniferous magnetite occur associated with anorthosite and gabbro in the Lake Sanford area, Essex County, New York. The ore, gabbro, and anorthosite show consanguineous relations. Anorthosite grades through gabbroic anorthosite into gabbro but is locally intruded by gabbro. Structural and petrographic evidence suggests that gabbro was differentiated from anorthosite by filter pressing. Field and laboratory study of ore occurrences indicates that an ore residuum concentrated in the gabbro through magmatic segregation by normal crystallization and flowage. Ore occurs as bands which grade into gabbro, and also as large masses which replace anorthosite. Ore in the gabbro is finer grained and richer in ilmenite than ore in anorthosite.

Jan 1, 1945

By H. Sato, R. J. Lipp, I. Iwasaki, K. A. Smith

Selective desliming holds much promise for upgrading low-grade, finely disseminated iron ores that are not readily amenable to conventional flotation. The process is extremely sensitive to the presence of calcium and magnesium ions that are in process water or are released by constituent minerals. The effects of these two alkaline earth ions on quartz were compared through streaming potential measurements, flocculation and cationic flotation tests, abstraction tests and scanning electron microscope studies. Calcium ion, adsorbed as CaOH+, and magnesium ion, attached by heterocoagulation as Mg(OH)2 precipitate, were responsible for the flocculation of quartz suspension and for the depression in cationic flotation of silica in alkaline pulp solutions. Magnesium hydroxide coating could be removed, similarly to adsorbed calcium ion, by complexation with EDTA and polyphosphates.

Jan 1, 1980

By H. F. Yancy

PooR results in coal washing and in ore concentration are sometimes attributed to the shape of the particles in the feed. It is well known that the shape of a particle influences its rate of fall in water. This is evidenced by the value of the constant C in the Rittinger equation for the velocity V of settling in water, V = C-D(d- z ), where C has the following values: 2.73 for roundish grains, 2.37 for long grains and 1.92 for flat grains. This report, which is based upon data obtained during the course of coal-washing investigations conducted by the U. S. Bureau of Mines in cooperation with the College of Mines of the University of Washington, gives the results of a method or procedure of screening in which the particles are separated into three shapes and shows the deportment of these shapes when coal is treated on a coal-washing table. The method consisted in first screening the coal with Tyler standard square-hole sieves, followed by screening tests of each of these products with screens of rectangular opening. For this purpose Tyler "Ton-Cap" screens were used; each square-hole product was subsequently sized with two Ton-Cap sieves so selected that their shortest dimensions were approximately 75 and 50 per cent., respectively, of the opening of the square-mesh sieves. For example: A product which is through 8 mesh (0.093 in.) and on 10 mesh (0.065 in.) is screened on slotted sieves which have openings 75 and 50 per cent. of the 0.065-in. opening in one direction and an opening of not less than 0.065 in. in the other direction. For convenience in discussion, the particles retained on the first slotted screen are termed "cubical"; those retained on the second slotted screen are termed "prismatic" and those passing the second screen are called "flat." (See Fig. 1.) The square-mesh screens separate particles according to two dimensions, length and breadth; the slotted screens divide them further according to the third dimension, or thickness. Prismatic particles have a mass of about two-thirds, and flat particles of about one-half, that of cubical particles of the same square-mesh size. The screen-

Jan 1, 1931

1 Healthy and active Local Section organizations are vital factors in promoting the vigor and growth .of the Institute 2 Activity on the part of Local Sections should be recognized and stimulated by appropriation of funds, from the Institute's treasury, and these appropriations should be as large as is consistent with the relative needs for other activities 3 As between different Sections, the amount of such appropriations should be based primarily on the extent of activities as reflected in the number and character of meetings held and the attendance of the members at such meetings 4 In making a request for funds for any year, the officers of a Local Section should submit a report on the printed form approved by the Directors at their meeting on November 19, 1937

Jan 1, 1952

1. Healthy and active Local Section organizations are vital factors in promoting the vigor and growth of the Institute. 2. Activity on the part of Local Sec¬tions should be recognized and stimu¬lated by appropriation of funds from the Institute's treasury;. and these appropriations should be as large as is consistent with the relative needs for other activities. 3. As between different Sections, the amount of such appropriations should be based primarily on the extent of activities as reflected in the number and character of meetings held and the attendance of the members at such meetings. 4. In making a request for funds for any year, the officers of a Local Section should submit a report on the printed form approved by the Directors at their meeting on November 19, 1937.

Jan 1, 1941

US 4,194,729 - Sintering of iron oxide ore on a straight sinter belt. The upper strand of the belt is divided into sintering and cooling sections with windboxes for removing their respective gases. The main for collecting cooling gas is located beneath the lower strand and is connected to opposite sides of the windboxes, while the main for collecting sinter exhaust gas is located beneath the lower strand and connected to sinter section windboxes. Both mains are exhausted via gas-evacuating fans and pipes to a flue. Space requirements are lessened and plant accessibility can be maintained at optimum conditions. K. Wacker and F. Feigk, assigned to Dravo Corp. Mar. 25, 1980. 8 pp. (266-144). Filed: 10-30-78 (956,058). Priority: West Germany, 12-16-77 (2,756,082).

Jan 1, 1982

By R. E. Somers

THE Appalachian field is notable for four tests drilled in recent years to depths of over 7000 ft. and for one commercial gas well at 6822 ft. The latter is the Ligonier well and produces from the Oriskany FIG. I.-NATURAL GAS PRODUCTION OF PENNSYLVANIA AND WEST VIRGINIA. sandstone. Together with several other comparatively deep tests, these holes were drilled in search of natural gas, to make up for the decline in production of the field. The production curve of Pennsylvania FIG. 2.-EAST WEST SECTION OF APPALACHIAN FIELD. (AFTER ASHLEY AND ROBINSON, PENN. G. S.) and West Virginia from 1907-21 is given in Fig. 1 to illustrate the heavy decline from the peak of 1917. This diminishing supply has also been shown by Moyer,1 on the basis of decreasing rock pressures.

Jan 3, 1924

By J. G. Koenigsberger

THE electrical specific resistance of rocks in the field is measured by sending a current through a medium of great volume, compared to the electrodes, whose resistivity should be measured. The whole resistance can be determined by the Wheatstone bridge and the specific resistance calculated by a well-known formula. The resistivity of some rocks in place in Germany and in Switzerland is given; first, of a rock near the surface, and especially near electrodes. Practical applications are made in the determination: (1) of the continuity of a conducting orebody; (2) of the surface area of an orebody; (3) in the detection of a water-bearing fault in a salt mine. Preliminary observations are described: (1) on the influence of the depth of ground-water table; (2) on the detection of gas under high pressure in coal seams. The observations in this paper of the electrical resistivity of rocks and soil in place are along the lines of the very interesting method and results of the Messrs. Gish, Rooney, Hotchkiss and Fisher.1,2 All the work described has been done since 1920.

Jan 1, 1928

By D. F. Stoneburner, G. Derge, Ling Yang

PREVIOUS investigations in this laboratory have shown the existence of electronic conduction in several molten metal sulfides and the specific conductance of a number of these has been measured as a function of temperature.' In order to better understand the electronic nature of these melts, the thermoelectric power of a molten FeS-solid tungsten thermocouple was measured and a value of approximately 55 µv per "C was obtained in the temperature range from 1200" to 1400c2 These studies have been continued and the thermoelectric power of several other molten metal sulfide-solid tungsten thermocouples have been obtained. The experimental arrangement is shown in Fig. 1. A Kanthal furnace was used, doubly wound to prevent any undesirable effects of an external field. A 1/2-in. McDanel tube was fitted with two vertical 5/8-in. McDanel tubes as shown. These tubes were about 2 in. apart. A graphite boat was used to hold a re-crystallized alumina boat in which the prefused sulfide was placed. Two probes were made using

Jan 1, 1960

By William E. Ford, Edward Salisbury Dana

The important BARITE GROUP is the only one among the anhydrous sulphates and chromates. Mascagnite. Ammonium sulphate, (NH4)2S0,. Orthorhomhic. Usrially in crusts and stalactitic forms. p = 1.523. Occurs about volcanoes, as at Etna, Vesuvlus, etc. Taylorite. 5K2SOa.(N&)ySOd. 111 small compact lumps or concretions. From the guano of the Chincha Islands. Thenardite. Anhydrous sodium sulphate, Na2S04. In orthorhombic crystals, pyrarnidal, short prismatic or tabnhr; also as twins (Fig. 384, p. 160). White, to brpwnish. 0 tically +. p = 1.477. Soluble in water. Often observed in connection with salt lates, as on the shores of Lake Balkhash, Central Asia; similarly elsewhere; also in South America in Tarapaca, Chilc. In the United States, forms extensive deposits on the Rio Verde, Aria. In Cal., at Borax Lake, San Bernardino Co. Aphthitaiite. Arranite. Glmerite. (Ii,Na)&O1. Rhombohedral; also massive, in crusts. Color white. From Vesuvius, upon lava; at DouglashaU near Weateregeln, Ger- many, in hloditc; Stassfurt, Germany; Rocalmuto, Sicily.

Jan 1, 1922

By C. D. Rubert, W. J. Parton

A flotation plant was placed in operation in 1945 at the Tamaqua colliery of the Lehigh Navigation Coal Co. Inc., to recover fine anthracite which is discharged from the cleaning plant with the washery water.‡ In addition to the recovery plant, facilities were provided for the complete clarification of the washery water, recirculation of this clarified water for breaker use, and disposal of the refuse solids in a waste impounding dam. Fig I shows a view of the settling tanks and the flotation plant. Flow Diagram The flow diagram for the complete recovery project is given in Fig 2. All the waste water from the cleaning plant is collected in a sump A outside the breaker structure, from which a 7000 gpm pump B delivers it through a 16 in. line to a 75-ft diam hydroseparator C. The hydroseparator, acting as a classifier, is set to give a separation at approximately 200-mesh. The minus 200-mesh overflow is discharged by gravity into the 180-ft thickener D for final settling of the solids. The classifier underflow sludge is pumped to the flotation plant by a 6-in. quadruplex diaphragm pump E. A 10-ft diam hydroseparator F is used to make a second classification on the sludge solids at approximately 28-mesh. The underflow from this classifier containing the coarse particles is elevated by a 6-in. diaphragm pump G and is discharged on two 4- by 6-ft vibrating screens II. These screens are dressed with approximately 28-mesh cloth. Screen oversize product flows directly to the centrifuge that dewaters the cleaned froth. The screen underflow and the overflow from the 10-ft classifier flow to the flotation circuit. The flotation feed is conditioned in a 12 by 12-ft agitator tank J at a pulp density of I:2.33 (30 pct solids). Reagents are fed to the circuit by reagent feeder I. The conditioned pulp is then diluted to a pulp density of approximately I: 5 (18 pct solids) and is fed to two banks of four 100-cu ft froth flotation cells K for primary coal recovery and cleaning. Additional reagents from reagent distributor L are added to the feed weir-box of Nos. 2, 3, and 4 cells of each bank of flotation machines. Clean coal removed from these cells flows directly to the clean-coal sump. Dilute tailings from the primary cells is re-thickened in a 30-ft diam thickener M and is then retreated in a scavenger circuit for final recovery of coal. The scavenger circuit consists of a 6- by 6-ft agitator tank N and two banks of four 24-cu ft froth flotation cells 0. Coal froth from these cells flows to the dewatering equipment and the tailings flows to a vertical refuse pump which delivers it to the 180-ft diam waste thickener D. Dewatering of the coal products is accomplished in a 54- by 72-in Bird centrifugal filter P. The cake product is dropped onto a conveyor and is loaded

Jan 1, 1949

By W. O. Philbrook, K. Natesan

A mathematical model was derived for the temperature change in a particle undergoing heterogeneous chemical reaction and heal exchange with a stream of fluid. The model has been applied specifically to the exothermic oxidation of spherical particles of zinc sulfide. Very good agreement was obtained between the theoretical prediclion and experimental observation. It was found that at no stage of the reaction was the particle subjected to a state of thermal instability. In studies of gas-solid reactions, it is generally assumed that the gaseous and the solid phases are at the same temperature throughout the reaction period. This is not strictly true since most of the reactions are either exothermic or endothermic in nature. This paper deals only with heterogeneous gas-solid reactions of noncatalytic type. In the case of exothermic reactions (e.g., roasting of sulfides), there may result an increase in temperature of the particle due to the release of the heat of reaction, and this increase in temperature may enhance the reaction rate and thus cause further release of heat. Such a "spiralling" effect may lead to a thermally unstable situation within the particle. On the other hand, in the case of endothermic reactions (e.g., calcination of limestone), there may occur a decrease in temperature of the particle as the reaction proceeds, leading to a virtual "quenching" of the reaction front. A general discussion of autothermic processes with emphasis on properties and reactor design is given by Van Heerden. 1 Levesque and cubicciotti 2 observed self heating of the sample in the oxidation of thorium. Anous et al. 3 observed self cooling of the sample in their dehydration studies on chrome alum. Cannon and Denbigh, 4 and Ong et al.5 reported self heating of the sample in their studies of the kinetics of oxidation of zinc sulfide. A typical plot of heat generation and heat loss rates with reaction temperature is shown in Fig. 1.'14 The Sigmoid curve represents the heat generation rate while the straight lines represent the heat loss rate. The main objectives of this analysis are to estimate the temperature increase of a single particle undergoing an exothermic reaction and to study the possibility of a thermally unstable situation within the particle. Also, a study of the dependence of the tempera- ture increase on different process variables has been attempted. A "she ll-by-shell" method has been proposed to analyze the problem. The shells may be made as small as necessary, and equations may be set up for heat transfer by various mechanisms. Such equations will have to be solved for each shell, with the boundary conditions for ith shell being obtained from the (i - 1)th shell, using a high speed digital computer. The oxidation of spherical particles of zinc sulfide is considered for this analysis, but the treatment is general enough to be applicable to other reactions and particle shapes. The oxidation reaction can be written as AH =« -115 kcal/mole ZnS [1] Such a reaction has been found to proceed in a topo-chemical manner; i.e., as the reaction proceeds, a progressively thicker outer shell of zinc oxide is formed, while the inner core of unreacted sulfide decreases. It has been found experimentally, both in the present work and in the previous investigations,4-6 that the particle retains its original dimensions. Therefore, at any given time, the particle may be

Jan 1, 1970

By Stanley J. Gasior, Albert J. Forney, Joseph H. Field

Most bituminous coal mined near Eastern industrial areas requiring high-Btu pipeline gas is caking and therefore unsuitable for fixed-bed pres- sure gasification by present techniques. If the caking property of such coal can be destroyed, the resulting fuel can be gasified in a fixed bed at pressure with steam and oxygen as a preliminary step in making a high-Btu gas. To find a practical way to convert strongly caking coals of granular or small lump size to noncaking fuel was the object of this study. In previous work, strongly caking coals of 1/8- to 1½ -in. size were converted to a noncaking coal char by treatment in a static bed in about 3 hours1 and coal of 18-100 Tyler mesh in a fluidized bed in about 5 min.2 An inert gas such as steam, nitrogen, carbon dioxide or a mixture of all three with a small amount of oxygen was used in both studies. In our work a strongly caking bituminous coal from the Pittsburgh seam of 4-8 Tyler mesh size was converted to a noncaking form in free-fall in about 2 sec by dropping it through a countercurrent flow of steam containing 4% to 7% oxygen at 1150º-1200°F and 300 psig. This method should also be applicable to smaller-sized material.

Jan 3, 1965

By J. C. Allen, E. V. Herring

CHILE EXPLORATION CO's. oxide plant at Chuquicamata, the largest of its kind, started in 1915 with initial operations at the rate of 10,000 tons of ore per day. Anaconda Copper Mining Co. acquired the controlling interest in 1923 and in the next few years modernized the plant and mine, extending operations to a nominal capacity of 490 million lb of electrolytic copper yearly by 1942. Plant production averaging 495.7 million lb of copper per year was maintained for the eight-year period extending from 1941 to 1948 inclusive. During the World War II production reached its highest level when in 1944 the output was 531.8 million lb. The maximum production for any one month was 49.6 million lb, achieved in May 1947. E. A. Cappelen Smith, consulting metallurgist for M. Guggenheim's Sons, worked out the first process for the treatment of Chuquicamata copper oxide ore about 1913, and directed a staff of 20 young engineers operating a pilot plant at Perth Amboy, N. J., on three shifts for an entire year. The copper is extracted from the oxide ore by a hydro-metallurgical treatment described in detail by T. A. Campbell in AIME Transactions, Vol. 106, Copper Metallurgy, 1933. The Oxide Plant is divided into five main operations as follows: (1) Crushing, (2) Leaching, including dechloridizing and sulphur dioxide treatment, (3) Tailing disposal, (4) Electrolytic precipitation, (5) Smelting and melting. Crushing The present Primary Crushing Plant has been in operation 25 years, during which time 4,342,112 cars of 70 tons net capacity have passed through the dumpers. The ore as received from the mine is frequently blocky and up to 5 feet in section. It is reduced to 9-in. size by two 60-in. gyratory crushers, and transported to the east and west ore bins by 60-in. conveyors. In the secondary crushing operation the ore is first reduced to 2 to 3-in. size by five standard 7-ft cone crushers and two No. 10 gyratories. This product is then reduced to 3/8-in. size by fifty-two 48-in. vertical Symons disc crushers and is transported by belt conveyors to the loading bridges from which it is charged° into the leaching vats. Conveyor belt No. 14 which serves the eight vats in the east section of the leaching plant has transported over 125 million tons of ore, which is a record for any type of conveyor. This 60-in. belt travels at a speed of 600 fpm and carries loads up to 5500 tons per hr. Leaching The ore is leached in 14 vats, averaging 13,500 short tons net capacity each. These vats are lined with a natural mastic which adequately resists the sulphuric acid leaching solutions. The leaching process as presently conducted comprises soaking the ore with successive volumes of leaching solution and spent electrolyte and withdrawing successive volumes of enriched solution from the vat to a total of approximately 3.2 million gal. The first 1.6 million gal of this volume withdrawn is called strong solution and contains about 35 parts of copper per 1000. The balance of 1.6 million gal subsequently withdrawn is stored in a

Jan 1, 1952

By J. H. Scaff, H. C. Theuerer

Germanium may be reversibly converted from n to p type by heat treatment. Data for the conversion and the associated changes in resistreatment.tivity are given and the results are interpreted in terms of changes in the donor-acceptor balance. MEANS for controlling the electrical properties of germanium in a predictable manner are of interest because of the increasing utilization of this element as the semiconducting material in electrical devices. Since both the mechanism and the magnitude of the electrical conductivity depend upon the kind and quantity of impurities present, the conductivity usually is adjusted by first carefully purifying the germanium, and then, by standard alloying procedures, adding the elements desired. The elements usually added are from the third or fifth periodic groups depending upon whether p- or n-type germanium is desired. However, in the development of germanium rectifiers during the war, it was found that it was possible also to modify reversibly the conductivity of germanium and even to produce conversion from n to p type by heat treatment.1,5 Since then a detailed study of this effect has been made. The data are presented in this paper and an explanation is offered for the effects observed. Preparation and Experimental Procedure The method used in preparing the germanium ingots for this investigation has been previously described.' The method consists essentially of (1) reduction of GeO2* and (2) preparation of a 50-g ingot from the reduced material. Graphite containers are used in both steps. In the first step the GeO2 is reduced in hydrogen at 650 °C to form a sponge germanium which, to assure complete reduction and to obtain massive materials, is fused subsequently in the reduction furnace by gradually raising the temperature to 1000°C. The button of germanium thus obtained corresponds to a yield of 99.8 pct. The final ingot is prepared by fusion of the germanium button in a helium atmosphere. A cylindrical crucible in a vertical silica tube furnace is employed and the crucible is heated by an external induction coil. The ingot is solidified from the bottom upward by raising the induction coil at a constant rate with power to the coil kept at a fixed value. In such ingots, segregation is normal and most of the impurities are concentrated in the last region of the ingot to freeze. It follows then that the major portion of the ingot is purer than it would have been if freezing had occurred in a random fashion. Moreover the orderly advance of the freezing surface during solidification establishes in the ingot a succession of surfaces of constant composition, if it is assumed that the liquid is homogeneous and that diffusion in the solid is negligible. Therefore, some information on the distribution of impurities in the ingot may be acquired by determining the shape of the solid-liquid interface at different stages of solidification. This is of importance because the concentration of impurities will be seen to affect the response of germanium to heat treatment. Such information is difficult to acquire by direct means, for the impurities responsible for the electrical properties of germanium prepared in this way are present

Jan 1, 1952