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By C. E. Shoenfelt

Wildcat drilling in the Rocky Mountain region did not suffer as large a decline in 1942 as was anticipated. The drilling program laid out by the Government at the beginning of the year stressed wild-catting operations and called for reduction of drilling in proved fields. The increased wildcatting campaign did not yield a great many new discoveries, nor important extensions to old fields. Several interesting wildcat wells were drilled in Colorado in 1942 but no new fields were discovered. The Wilson Creek field was extended and about 400 acres added to its reserves. In Montana two new oil fields and two small gas fields were discovered. The developments in the marketing situation had improved, however, making the prospects especially bright for 1943, as will be shown presently in the section on Montana in this report. In New Mexico eight wells were completed, which constituted discoveries ol either oil or gas but none of these was of major proportions. In Wyoming one new oil field and one new gas field were discovered, and one old oil field and one old gas field were extended. Most important was the disco-very of prolific oil producers in deeper sands in three old oil fields, of which one at least, Elk Basin, probably is of major proportions. Government Action On Dec. 26, 1942, President Roosevelt signed the O'Mahoney bill, calling for a flat 12.5 per cent royalty on lands in the public domain. It is expected that the enactment of this bill will encourage wildcatting in the public land states. Opportunity for a full discussion of the problems of reserves and production was afforded at the hearings conducted on the O'Mahoney bill by the minerals subcommittee of the Senate Committee on Public Lands and the statements submitted at these hearings last fall placed the situation, its causes and the logical remedy, clearly on record. It was established at the hearings that for several years the volume of oil discovered per wildcat well drilled has steadily declined; new fields discovered have not been of major proportions; drilling costs have advanced rapidly; a sharp decline in exploratory drilling took place in 1942, while the proportion of dry holes increased; the inescapable conclusion is that to find new reserves the search for oil must be intensified and much more wildcat drilling ' must be done. To ensure an adequate drilling campaign, the Petroleum Industry War Council, the Interstate Compact Commission and other representative oil organizations have voiced by resolution their opinion that an upward revision of crude prices is necessary to provide an incentive to the prospector to undertake the hazards of wildcat drilling, since statistics prove that only ope in five or six wells drilled results in actual production. Former Price Administrator Henderson rejected the recommendations for price increases and declared himself unalterably opposed to a general price advance, On the ground that such advances would contribute to inflation. Now that Mr. Hender-

Jan 1, 1943

By B. W. Dyer

IN 1924, the Crescent Eagle Oil Co., while drilling the salt section of the Paradox formation in Grand County, Utah, encountered a salt that did not appear to be sodium chloride. This salt was analyzed and showed the presence of potash minerals, both sylvite (KC1) and carnallite (KMgC12.6H20). Because of the high potash content of the sample, there was considerable speculation: (I) as to whether the hole had been salted, and (2), if not, the extent, richness, and the depth at which the deposit occurred. The discovery caused a large amount of activity in the area. During the next few years, 68 potash prospecting permits were issued by the Government, 24 under the Act of 1917 and 44 under the Act of Feb. 7, 1927, each including about four sections of land. Several holes, all shallow, were drilled for potash. A number of holes were drilled for oil into the salt horizon and the cuttings collected at the oil wells were examined petrographically and chemically. The shallow test holes were not sufficiently deep to reach the potash horizon and revealed nothing of value, but several of the oil test holes gave some indication of where potash might be found. LOCATION AND GEOLOGY OF DEPOSITS The potassium and magnesium salts have been found in various places from the Denver and Rio Grande Western Railroad tracks about seven miles west of Thompsons, in eastern Utah, to Cane Creek, a tributary of the Colorado Rivera distance north and south of about 35 miles. In this locality, there appear to be five separate deposits: the Crescent Eagle area, which is in T. 22 S., R. 19 E.; the Salt Valley area, in the vicinity of the north-south line of T. 23 S., between R. 20 E. and R. 21 E.; the Seven Mile area, in the eastern part of T. 25 S., R. 2o E.; the Cane Creek area, on the Colorado River, in T. 26 S. and T. 27 S., R. 2o E. and R. 21 E.; and the Salt Wash area, in T. 22 S. and T. 23 S., R. 16 E. and R. 17 E. (Fig. I.) The Crescent Eagle and Salt Valley areas are in the Salt Valley anticline, some of the wells being in the fault graben and others outside. Structurally, the Salt Valley anticline is very complex, and can be described in general terms as a northwesterly plunging collapsed anticline about 15 miles long. In the Crescent Eagle area, the valley graben is about 1 mile wide and the salt probably forms a plug, the apex of which is in the vicinity of the Crescent Eagle well. Owing to the complex structure, there has been every opportunity for flowage in the salt to cause local thinning or thickening of beds. The regular succession of formations in the general area* is: [Cretaceous Mancos Dakota Jurassic Morrison Summerville Entrada Carmel]

Jan 1, 1945

By R. G. Knickerbocker, R. R. Lloyd, W. T. Rawles

In July 1041, the Experiment Station of the Bureau of Mines at Boulder City, Nevada, began a study of methods of producing magnesium metal from magnesium oxide, with particular emphasis upon the direct use of magnesium oxide in a molten chloride electrolyte. The program was extended to include pilot-plant study of chemical methods for the preparation of pure magnesia from dolomites and magnesites. Preliminary work on the production of magnesia from dolomite was done with the cooperation of Kobert D. Pike and the Harbison-Walker Refractories Co. These investigatipns included a cooperative arrangement whereby the Bureau tested certain steps of the Harbison-Walker-Pike process. The process finally developed by the Bureau includes the precarbonation mixing step of the H.W.P. flowsheet prepared by Mr. Pike. Two magnesium-reduction plants using MgO as a source of magnesium were being constructed in the West, and they enormously stimulated interest in various dolomite deposits as possible sources of the magnesia needed by them. This paper describes one phase of this program—the operation of a pilot plant for producing cell-grade magnesia from dolomite from Sloan, Nevada. The process developed for this purpose is an adaptation of a well-known process first proposed by Clossonl and modified by others,2"1 involving the use of calcium chloride and carbon dioxide. It is based on the following chemical reactions: MgCl2 + Ca(OH)2 = CaCl2 + Mg(OH)2 [1] Mg(OH)4 + CaCU + CO2 = MgCl2 + CaCO, + H2O [2] The first reaction proceeds almost completely to the right because of the much greater solubility of calcium hydroxide as compared with magnesium hydroxide. Under equilibrium conditions, when only the four components shown in reaction I are involved, the ratio of magnesium to calcium in solution, according to solubility-product relationship, will be: This reaction is the basis of present commercial processes for recovering magnesium from sea water and dolomite. The second reaction is, in effect, a reversal of the first reaction produced by adding COz. This reaction also proceeds nearly to completion, the solubility relationship being: Ca where P indicates partial pressure of COz, in atmospheres.

Jan 1, 1944

AT the fall meeting of the Iron and Steel Division, Oct. 4, 1934, in New York, a symposium was held on Slag Control in the Making of Iron and Steel. The chairman was J. H. Nead and the vice chairman, G. B. Waterhouse. The latter presided at both morning and afternoon sessions. The papers and discussions were presented in the order in which they appear on the following pages. To meet space requirements, much of this material has been considerably condensed. CONTENTS [ ]

Jan 1, 1935

By G. B. Walker

THE sink-float methods designated by heavy-media separation processes were pioneered by C. Erb Weunsch for the treatment of base metal ores as an improvement over jigs. The work of Weunsch was further developed by Victor Rakowsky and The American Zinc, Lead and Smelting Co. Early in the development of the processes, the inherent unsuitability of galena as the solid constituent of the medium was recognized and ferrous media amenable to magnetic recovery and control were developed. The high efficiency and low cost of magnetic recovery and cleaning of ferrous media regardless of particle size, slime contamination, or surfacial oxidation had led to the adoption of ferrous media by all of the sink-float plants operating under the heavy-media separation processes patents controlled by American Zinc, Lead and Smelting Co. Approximately 2,000,000 tons of base metal and nonmetallic minerals are treated each month by these methods.

Jan 1, 1949

By J. E. Nelson, R. J. Bonnis

Recent completion of Cyprus Bagdad's $240-million modernization and expansion program has registered a 700% increase in ore production with only a 50% increase in labor. Elements of this remarkable achievement include the application of large-scale mining equipment as well as the selection of the latest in processing hardware. Most important, however, was the early recognition that Bagdad's labor personnel is its most important asset.

Jan 4, 1978

By L. L. Wyman

Since the presentation, by the writer, of the initial paper on the embrittlement of copper,1 the subject has been investigated further along two separate lines. The first series of investigations involves the "double-deoxidized" coppers, while the second series is devoted to single deoxidizers other than those used in the investigations reported upon last year. The object of these experiments is to develop a type of copper that will show the minimum of detrimental effects after having been exposed to alternate oxidation and reduction. The fabrication of this material necessitates the use of alternate oxidizing and reducing atmospheres, at temperatures ranging up to 900" C. Following this treatment it is essential that the soundness and strength of the copper be unimpaired, even in sections of only a few thousandths of an inch in thickness. Materials The ensuing report embodies three separate groups of materials, which may be classified as follows: 1. Double-deoxidized copper using silicon and calcium boride. 2. Copper deoxidized with calcium. 3. Double-deoxidized copper using constant calcium content (0.075 per cent) plus silicon, or calcium boride. Last year, T. S. Fuller, of the General Electric Research Laboratory, suggested that if a properly deoxidized copper had sufficient deoxidizer residual in the material, this excess material might increase the resistance of the copper to the oxidation reduction cycle. In consequence of this suggestion, two small lots of "double-deoxidized" copper were prepared. The first, lot A, was made by adding 0.03 per cent silicon as the deoxidizer, following this by an addition of 0.55 per cent calcium boride immediately before pouring. The second, lot B, contained the same ingredients, but these were added in the reverse manner. Inasmuch as these lots were tested separately from the materials about to be described, it must be borne in mind that the materials cannot be grouped together, and are not directly comparable.

Jan 1, 1933

By C. A. Hansen

The furnace used for experimental work is shown in Fig. 1. One fireclay sagger, or pot, was set within another and the space between the two filled with Silox heat insulation. The hearth is a cast-iron plate with an imbedded ribbon of nichrome wire; this wire heater is connected to a potential regulator, which permits a very close voltage control. A mechanically driven arm is fitted with rabble blades so arranged that a uniformly thick ore bed may be maintained indefinitely. This arm is usually driven at about one revolution per minute but its speed of rotation can be varied as desired. Compressed air is led into the furnace through a meter, and it was found necessary to preheat the air in order to secure the definitely isothermal conditions sought. With this arrangement, it is possible to maintain any desired temperature constant within about 5" C. for any desired length of time and to

Jan 1, 1921

By J. A. Retty

IN the Labrador iron fields two concessions, totaling nearly 24,000 square miles, have been staked out and commercial-grade deposits delineated. The Newfoundland-Labrador concession, owned by the Labrador Mining and Exploration Co. Ltd., is a 20,000-square-mile tract in the upper basins of the Hamilton and N askaupi Rivers which drain into Lake Melville. The New Quebec licensed area is 3900 square miles, owned by the Hollinger North Shore Exploration Co. Ltd., lying to the northwest of the northwestern part of the Labrador concession. It includes the upper basin of the Swampy Bay River and part of the upper basin of the Whale River, both of which drain into Ungava Bay. Both of the above-named companies are controlled by Hollinger Consolidated Gold Mines Ltd. with The M. A. Hanna Co., of Cleveland, holding a minority interest. When exploration was first undertaken in 1936, the only published map of the area was that prepared by A. P. Low in 1895. It showed only the main watercourses and gave only a rough, general idea of the geology. The numerous lakes of this vast area had to be first sketched and then mapped. Since then, extensive geological and topographical surveys have been conducted by the Labrador company, work which is normally done by Government branches. The object of the work was to examine the area and gradually eliminate unfavorable or less favorable prospecting ground. With this object in view, geological

Jan 1, 1948

By B. G. Klugh

(New York Meeting, February, 1912). IN a paper before the Institute at Wilkes-Barre, Pa., June 1911,1 Mr. James Gayley discussed the application of this process to iron-bearing materials. The same author2 described the results of operations at the plant at Birdsboro, Pa. The purpose of the present paper is to present further discussion of some technical details involved in the operation of this plant, and of the theoretical and practical relations of this product to blast-furnace practice. Since Oct. 1, 1911, the Birdsboro plant has been in operation at the blast-furnace of the E. & G. Brooke Iron Co. The results have been highly satisfactory, although the material treated, being chiefly the flue-dust currently made by the furnace or taken from the accumulated stock-pile, was excessively high, and yet not uniform, in carbon, so that the desirable control or regularity of the amount of fuel in the mixture treated could not be maintained. Nothing could more forcibly demonstrate the flexibility of the process than the fact that, under these conditions, the sinter produced was, in all cases, of excellent quality. The Dwight & Lloyd process, as such, and its present highly-developed mechanical appliances were described by Mr. Gayley in the paper above mentioned. While the repetition of some particulars will be unavoidable in this paper, it will be confined to features bearing upon the metallurgical principles involved. According to the principle of the process, the finely-divided iron-bearing material to be sintered is intimately mixed with

May 1, 1912

By H. K. Najarian

AT Josephtown, Pa., on the south hank of the Ohio River about thirty miles northwest of Pittsburgh, is the Josephtown electrothermic zinc smelter, which operates as a custom smelter receiving both domestic and foreign concentrates. Constructed in 1930, the plant was designed to produce zinc oxide and to process 124 tons per day of zinc concentrate obtained mainly from the Company's New York State mines. Zinc condensing equipment was developed in conjunction with the St. Joe electrothermic. furnace and commercial production of zinc metal started in 1936. Expansion of the plant and equipment during 1939 and 1940 brought the processing. capacity to upwards of 300 tons of concentrate per day; and the plant operated at peak capacity during the war years, earning the Army-Navy "E" award and three subsequent stars. A postwar plant expansion is now under way, designed to increase the capacity to 500 tons per day of concentrate, with an estimated daily production of 160 tons of zinc metal of various grades, about 100 tons of zinc oxide, and 425 tons of sulphuric acid as major products.

Jan 1, 1947

By PHILIP N. MOORE

THE development of the power of the Tennessee River at Muscle Shoals has become a matter of political interest as well as engineering possibility. The controversy over it has been so active that the facts have been obscured, the possibilities exaggerated. Although the members of the American Institute of Mining & Metallurgical Engineers are not generally specialists in hydroelectric development, those who visited Muscle Shoals in October, following the Birmingham meeting of the Institute, were interested, and many of them surprised to learn the actual conditions. These have long been familiar to those who have studied the matter through the reports of the U. S. Engineers on the subject. The approved plan contemplates three dams-No. 1, a low dam close to the City of Florence, planned in the interests of navigation, since the construction of the other dams has rendered impossible the use of the river without it. No. 2-named the Wilson Dam is now under construction. Concerning it political argumentation has waged. No. 3 Dam-much smaller, is planned to be erected several miles above No. 2.

Jan 1, 1925

By S. T. Wlodek

The scale md subscale reaction products were identified and their rates of formation were studied in air over the range 1600" to 2000°F (871 " to 1149°C) for periods of up to 400 hr and for hoth the solution-annealed and aged conditions. The effect of prior sltrface preparation on suhscale oxidation was also studied The general oxidation behavior of both Ni-Cr-Mo-Al-Ti type alloys was similar. A surface film of a, Al2O3, forms immediately on exposure Subsequent oxidation continued at a linear rate (QL = 55 * 5 kcal per mole) as colonies of Cr2O3 nucleated at the A12O3/gas interface Further oxidation proceeded at a paraholic rate zvhiclz could he fitted to two successive rate constants. During paraholic oxidation, and depending on temperature, the scale consisted of Cr2O3, NiCr2O4 , and TiO2 with traces of NiO. In the case of Rene 41, the activation energy of both paraholic processes was 66 * 3 kcal per mole suggesting that diffusion of cations tlzrozrgh Cr2O3 was the rate -determining process. An unusual decrease in the oxidation of Udimet 700 at 1900°F where a spinel of Ni(A1,Crh0, zuas the predominant reaction product prevented the accurate assignment of activation energies for this composition. In both alloys internal oxidation of Al2O3 commenced shortly after parabolic scaling was observed. Prolonged exposure prod7tced intemal oxidation of TiN, and in Udimet 700 a complex Mo-Ni nitride was also found. At 1900oF, the subscale reactions in Udimet 700 undergo an inversion which parallels the decrease in surface oxidation; internal oxidation ceases hut is replaced by the formation of "spherodized" 3.' colonies. Surface-preparation techniqtles which introduce appreciable working, such as coarse surface grinding or grit blasting. increase the amount of alloy depletion and internal oxidation in Reni 41. The reverse is true of Udimet 700 for which electropolished or mechanically polished specimens show much more subscale oxidation than strongly worked stirfaces. The strongest commercial nickel-base alloys presently available are generic to the Ni-Cr-Mo-A1-Ti base which exploits the precipitation of Ni3(A1,Ti) as the main strengthening mechanism, while relying on solid-solution strengthening by molybdenum and chromium reinforced by the pre- cipitation of carbides to attain maximum properties. This study characterizes the oxidation behavior of Rene 41, the strongest alloy of the Ni-Cr-A1-Ti type commercially available in sheet form, and Udimet 700, whose higher aluminum and titanium content allows it to exhibit one of the more attractive combinations of high-temperature properties available in a wrought product. The scaling processes of complex, type nickel-base alloys have received relatively little attention. Malamand and vidal as well as Poulignier et al.2'3 have determined the composition gradients across the metal/oxide interface produced by high-temperature oxidation and considered the effect of surface perature, Limited weight-gain data has also been published by Fere 5 for alloys of this type and Radavich6 has identified the reaction products on Udimet 500 and Inco 702 after oxidation at 1832°F. Reference can, of course, be made to the excellent reviews of Kubaschewski and Hopkins7 or Ignatov and Shamgunova8 for a summary of the data available on the oxidation of binary and ternary alloy systems which are related to the more complex alloys considered here. EXPERIMENTAL The analyses of the different commercial heats studied are given in Table I. Using the experimental procedures previously established,9 continuous weight-gain data were obtained on both heats of Rene 41 sheet (A and B) and 150-mil-thick slices of cast Udimet 700. Subscale oxidation reactions were followed by static exposure of cylindrical specimens obtained from swaged Rene 41 (Heat C) and Udimet 700 (Heats E and F). In brief, continuous weight-gain tests were performed on specimens with a surface area of 10 to 12 sq cm. These were abraded through 600 grit Sic paper, electropolished to 2p rms in an electrolyte of 10 pct H2So4 in ethanol, and lightly etched in 10 pct HCl in ethanol before final washing and rinsing in ethanol. All continuous weight-gain data were obtained in dried (-70°F dew point) flowing (1 liter per min) air to an accuracy of +0.1 mg. Subscale oxidation processes were followed by the metallographic examination of 0.5-in-diam by 1.0-in.-long specimens. After an initial center-less grinding, various additional surface treatments were employed to determine the effect of surface preparation on subscale oxidation processes. Before exposure in zirconia crucibles, all samples were lightly etched in 10 pct HCl-ethanol, washed in ethanol, and dried. The depth of internal oxidation was measured to ±0.00025 in. on unetched specimens mounted so as to provide a taper mag-

Jan 1, 1964

By H. B. Pulsifier

THE following report on the structure of copper is the result of work done in the laboratory of the Rome Wire Co. early in 1925. Previous work had indicated to the author that excellent results might be expected if a suitable technique in surfacing and etching could be developed. The resources of the Rome Wire Co. enabled this metal to be studied more intensively than previously, although none of the materials were investigated exhaustively. The material presented is hardly more than a preliminary summary of the most obvious character of the metal; a much longer research would have been necessary to solve many of the pressing problems connected with the casting and working of copper. The Rome Wire Co. has generously released the paper; to Dr. E. H. Darby, technical supervisor of the company, are due particular thanks for his appreciation of the importance of metallographic study of copper and for his effective support in the prosecution of the work and in making its publication possible.

Jan 1, 1926

By D. J. McAdam

As shown in three recent papers by the author, in two papers by McAdam and Mebs, and in a paper by McAdam, Mebs, and Geil," the technical cohesive strength of a metal, in any particular state as regards mechanical treatment and heat-treatment, cannot be represented by a single stress value, but must be represented by a diagram with the principal stressest as coordinates. Each point on the boundary of such a diagram represents a technical cohesion limit. The technical cohesive strength thus comprises an infinite number of technical cohesion limits, each representing fracture under a specific stress combination. Moreover, neither the yield strength1 nor the ultimate strength can be represented completely by a single stress value, but must be represented by a diagram with the principal stresses as coordinates. All combinations of the principal stresses may be classified in three groups as illustrated by Fig. I. Fig. Ia shows three typical stress combinations with no two principal stresses equal. The magnitude of each principal stress is indicated qualitatively by the length of the arrow. Arrows pointing away from the cube indicate tensile stresses; arrows pointing toward the cube indicate compressive stresses. Typical stress combinations with two principal stresses equal are illustrated in Figs. rb and Ic. Such stress combinations would be produced by subjecting a cylinder to combinations of uniform axial and radial stresses. The uniform radial stress may be resolved into two equal principal stresses. with the mutually perpendicular directions rotatable around the axis of the cylinder. Fig. ib shows stress combinations with Sz equal to The greatest principal stress is in the axial direction, and the stress combination tends to cause either absolute or relative increase in length.* Fig. u shows stress combinations with S2 equal to St. The greatest principal stress is in the radial direction, and the combination tends to cause either absolute or relative decrease in length. The complete representation of either technical cohesive strength, yield strength, or ultimate strength generally requires a three-dimensional diagram. When two of the principal stresses are kept equal, however, the strength of a metal may be represented by a two-dimensional diagram with the coordinates representing the axial and radial stresses.6-II In this paper, attention will be confined almost entirely to stress combinations with two of the prin-

Jan 1, 1945

By M. R. Geer, J. D. Davis, H. F. Yancey

ALTHOUGH the mechanical cleaning of coal is carried out at plants on the surface, preparation is actually begun at the face in the mine. Here the character of the coal and the amount, character, and distribution of the impurities within the bed may be seen. Blasting methods, dust-allaying procedures, location of mining cut with respect to bands of impurity, and the practice of discarding segregated impurities underground, all have an important bearing on the successful operation of surface cleaning units. The most important single characteristic of both coal and its associated impurities from the standpoint of cleaning is specific gravity. Other characteristics related in one way or another to the preparation , of coal are rank, petrographic composition, structure and hardness, and friability. These and still other coal properties are discussed in the first section of this chapter and impurity characteristics in the second. COAL CHARACTERISTICS RELATED TO PREPARATION Rank As a result of work done over a period of several years by committees of the American Society for Testing Materials and the American Standards Association, standard specifications are now available showing the 'classification of coals according to rank and quality of grade.' The term "rank" expresses the degree to which the original coal-forming material has been changed by metamorphism through successive stages from peat to anthracite. Table 1 shows the classification of coals according to rank as devised by the committees of the organizations mentioned. The basic scheme of classification for the higher-rank coals is according to

Jan 1, 1943

By Donald L. Katz

FIFTEEN years ago Dr. Manning published a paper in "Petroleum Development and Technology" on '.Fundamental Research Relating to Petroleum." He tabulated for several industries "the proportion of their present success which can be fairly attributed to the application of information and processes obtained by scientific research," giving petroleum a score of 7 compared to 100 for the electrical and coal-tar industries. Today the petroleum industry as a whole and the producing groups both have raised their score beyond the majority and are climbing toward the top. Present practices are being developed both by fundamental research and the application of the research method in field operation.

Jan 1, 1941

By M. H. Forester, John D. Cooner

ANTHRACITE ALTHOUGH the unmined anthracite will last for approximately 150 years, most of the thicker and cleaner coal beds have been almost entirely first-mined and pretty well robbed, leaving much of the present and future production to come from thin and dirtier beds. Herewith is a section of one of the dirty beds being mined in the Wyoming region [ ] This section shows that 45.8 per cent of the bed is made up of impurities and that the 45 in. of coal in the bed is in five benches, the thickest of which is 19 inches. In some localities of the anthracite region there are 14 beds of minable coal. Orderly and proper mining of the coal makes it necessary to rob or second-mine-almost all beds have already been first-mined-in sequence from the top downward. Therefore the robbing of the few remaining portions of the thicker and cleaner beds is in many instances being held up by the mining of the overlying thin and dirtier coal beds. Impurities Impurities consist of fire clay, slate, rock, and bone. The latter, which is black, contains 40 to 60 per cent carbon and often resembles good coal. In some beds there are also bands of "blue" coal, which, as the name implies, is of a bluish slaty color. Although much of this "blue" coal has a carbon content almost as high as the good anthracite, it is not

Jan 1, 1943

By M. C. Flemings, F. R. Mollard

Two-phase Pb-Sn alloys, ranging in compositiotz from 12 to 26 at. pct Pb, were unidirectionally solidified in a convection-fvee system, with thermal gradients in the liquid of up to 480°C per cm. Plane front solidification Loas achieved in all alloys at sufficiently steep gradient and slow growth rate. Conditions causing breakdown of the interface to a cellular or dendritic structure were roughly as predicted by a sinlple constitutional supercooling criterion. Structures of alloys of near-eutectic composition, solidified with plane front, exhibited a lamellar structure; the alloys furthest from the eutectic exhibited a rod-like morphology. Assumptions used in a previous paper for calculations of solute redistribution in two-phase plane front growth are shown to be reasonable for Pb-Sn alloys. Results of calculations are in good agveement with experiment. These show that variations in growth rate during solidification of the composite produce marked changes in average composition of the solid. IN a previous paper, Part I,' conditions necessary for plane front solidification of two-phase alloys were discussed and calculations given on solute redistribution in this type of solidification. This paper, Part 11, describes experiments on Pb-Sn alloys, designed to check the assumptions of the analyses presented, and to demonstrate their applicability to a given alloy system (Pb-Sn). APPARATUS AND PROCEDURE General. A vertical crystal growing unit was built for the study as described below, and "normal solidification" employed throughout (i.e., the ingot was completely melted except for a portion near the bottom end and then solidification initiated). The furnace was designed to permit achieving very low interface velocities, and steep gradients, in essential absence of convection; it is sketched in Figs. 1 and 2. Simple heat flow considerations indicated choice of a small-diameter specimen (ingot) to achieve high thermal gradients; ingot size chosen was 0.3 cm in diam. The ingots were held inside silica tubes 0.06 cm wall thickness. The requirement for an essentially convection-free system was met by use of the vertical furnace with the heat source over the heat sink, as well as by use of the small diameter ingots. In addition, by selection of tin-rich Pb-Sn alloys, the diffusion boundary layer (lead-rich) was denser than the bulk liquid and would not cause convection. The only apparent driving force for convection in this system was the small transverse temperature gradient resulting from heat flow into the samples from the furnace. Such convection must have been small, however, since 1) no temperature fluctuations in the melt were noted in the recordings, which would have indicated turbulent convection, and 2) experimental results obtained and described below could not have been achieved in presence of significant convection. Ingot Preparation. Pb-Sn alloys ranging from 12 to 26 at. pct Pb were prepared from high-purity lead and tin (99.9999 pct pure metal). Each alloy was prepared by first melting the pure metals in the proper ratio in air, in a Pyrex container. The melt was then stirred thoroughly with a graphite rod and cast into a preheated graphite mold. Ingots were then prepared from these castings for use in the actual experiments; each ingot consisted of a rod of alloy, 15 cm long in a 25-cm-long transparent fused-silica tube, 0.3 cm ID and 0.06 cm wall thickness. One chromel-alumel thermocouple, made with 0.004-in.-diam wire and protected by a two-hole alumina tube, was inserted into each ingot. The 1.5 cm of the thermocouple nearest the bead were protruding from the alumina tube and were coated with a very thin layer of boron nitride paste which provided electrical insulation while allowing good heat conduction. The electrically welded junction size was about that of each wire and the cross section of the two wires represented about 0.3 pct of the sample cross section. Including the coating, the thermocouple cross section still represented less than 0.5 pct of the ingot cross

Jan 1, 1968