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By G. R. Heckman, H. J. Murphy, C. T. Sims

An incestigation has been made of the effects of heat treatment and alloy composition on the long-time stress-rupture properties and structural stability of the similar nickel-base alloys Udimet-500, Lrdimet-520, and Udimet-700. Rupture test data are presented at stresses ranging from 4 to 50 ksi at temperatures from 1450° to 1900°F for times up to 14,000 hr. Ductility response is emphasized. Optical and electron tnicroscopy were complemented by X-ray diffraction analyses of extracted phases to relate microstructural stability to the observed rupture properties. Particular attention is paid to Udimet-520 since structural characteristics of this alloy appear to vary somewhat from its sister alloys. Both cast and wrought performance of Lrdimet-500 are discussed. The computerized PHACOMP calculational technique, based on electron-vacuncy theory, is discussed and related to structural stability where appropriate. Electron microscopy and microprobe techniques were used to conduct evaluation of the oxidation characteristics of Udimet-500 exposed in air for 16,100 hr. The steady advance in strength and reliability of nickel-base superalloys continues to be one of the high points of modern metallurgy. The stress capability of these materials has increased steadily, allowing higher and higher operating temperatures in the highly sophisticated aircraft and industrial gas turbines now on the market. The attendant increase in efficiency, of course, means greatly improved power output. Gas turbines for industrial and marine use have long been designed with these objectives paramount the usual design requirements in terms of time of service being 100,000 hr. High-efficiency, long-life aircraft such as the supersonic transport require superalloy engine materials with high-strength and long-time structural stability. Thus, materials studied for and operating experience from industrial gas turbines provide a good reservoir from which technology of high value to the SST program can be drawn. This study is one such case. Three prominent nickel-base super alloys—Udimet 500, Udimet 520, and Udimet 700 were extensively evaluated for industrial gas turbine bucket use. Particular attention was directed toward structural stability as a requisite property. Within the present context, structural stability is defined as freedom from the propensity to form strength-robbing or embrittling phases such as u,p,x,or Laves, and the ability to maintain useful rupture strength and ductility throughout design life. MATERIALS The three alloys, cast Udimet 500 (U-500C), Udimet 520, and Udimet 700, were chosen for detailed evaluation based on preliminary studies which indicated that U-500C and U-520 possessed comparable rupture strength capabilities, and that U -700 had a greater strength capability but somewhat poorer ductility than wrought U-500. The nominal compositions of the three alloys, along with the compositions of the heats investigated, are presented in Table I. PROCEDURE Dimensionally rejected U-520 buckets from Special Metals Corp. heat 63370 were heat-treated using the four cycles delineated in Table 11. Cycle A was investigated to determine the effects of a shortened 1700°F primary age. Cycle B was considered a "standard" treatment. Cycle C investigated a higher solution temperature in combination with a shortened primary age, while cycle D assessed the effect of the higher solution temperature alone. These heat treatments were designed to produce optimum combinations of rupture strength and ductility through maximum y' development, the development of a y' grain boundary cushion, promotion of MC carbide degeneration reactions, and agglomeration of resultant M23CB. Since one of the premises of the evaluation of U-520 was that rupture strength would be equivalent to U-500, forged U-500 buckets from Special Metals Corp. heat 62916 were heat-treated with cycles A, B, and C to provide comparison. The heat-treated structures of U-520 and U-500 are illustrated in the 8700 times electron micrographs of Fig. l. The U-700 tested was all from 3-in.-diam hot-rolled and centerless-ground rod from Special Metals Corp. heat 2-1426. Two heat-treatment cycles were employed, E and F of Table 11. Cycle E is a standard four-step, triple-age treatment intended to provide an optimum match of strength and ductility through well-developed matrix and grain boundary y', as recommended by U-700 vendors. Treatment F is a shortened , single-age cycle which could provide a significant processing cost reduction should adequate strength and ductility be maintained. Following heat treatment, rupture specimens of U-500 and U-520 were machined from the buckets and tested. Standard rupture bars of U -700 were machined from the heat-treated rod and rupture-tested. Failed and withdrawn rupture bars were prepared and examined by optical and electron microscopy. Select specimens were electrolytically digested, and the residues analyzed for carbide and topologically close-packed phases using CrKa or CoKo radiation. Of the six different U-500C heats evaluated, five were cast by Misco Precision Casting Co. and one was cast by Haynes Stellite Co. Cast-to-size rupture bars

Jan 1, 1968

Resonance re-emission from nickel vapour affords a convenient method for isolating the resonance lines at 3415A, 3515A, and 3524A. The vapour is generated by cathodic sputtering and is illuminated by light from a nickel atomic spectral lamp. The resonance lines thus isolated can be usefully employed for absorption measurements on mineral samples where the nickel concentration is too high for measurements with the more sensitive line at 2320A. A spectrophotometer employing a resonance lamp as monochromator possesses several advantages where a great number of determinations are made under routine conditions. The wavelength setting is stable under even the most rigorous conditions and with the provision for automatic setting of full scale deflection the instrument requires virtually no adjustment. The instrument has been used under routine conditions for the determination of nickel (in the range O· 05-2 per cent) in mineral samples.

Jan 1, 1968

By Gerald W. Elger

To determine the feasibility of removing nonferrous metal impurities from automobile scrap by thermal treatment in a rotary kiln, the Bureau of Mines conducted four series of tests with synthetic scrap mixtures heated at various temperatures under oxidizing and reducing conditions. The treated scrap mixtures were melted in an electric-arc furnace and cast into small ingots for impurity evaluation. Analyses showed that the ingots were essentially free of residual metal impurities except for copper. Test data indicated that in an oxidizing atmosphere the percentage of copper removed increased with treatment temperature. Percent of copper removed in a reducing atmosphere was found not to be temperature dependent. A significant finding was that copper was embrittled under some of the operating conditions and was mechanically removed by fragmentation.

Jan 1, 1968

By William A. Wallace

Common mineral resources (sand, gravel, crushed stone, etc.), which are so necessary for the construction of metropolitan areas, are rapidly being depleted or otherwise rendered unavailable in the very areas that need them most. However, the problem of planning for these resources involves a number of independent and dependent variables that must first be defined and related. Finally, a dollar value must be assigned where possible. Complex interrelationships between the variables and their dependence on outside factors has made mathematical "solution" of the problem of planning for non-renewable mineral resources difficult at the present time. Therefore, the use of computer simulation is suggested as a means by which this complex problem can be investigated. The purpose of this paper is to report on a continuing research program whose objectives are: (1) to delineate the factors involved in planning for the utilization of common mineral resources in urban-suburban environs; (2) to construct a planning model for these materials amenable to computer analysis, (3) evaluate the model by using test cases, and (4) perform a sensitivity analysis to determine the initial parameters in future planning for these materials.

Jan 1, 1968

By M. E. Wadsworth, K. C. Bowles, H. E. Flanders, R. M. Nadkarni, C. E. Jelden

The kinetics of precipitation of copper on iron of various purity were carried out under controlled conditions. The rate of reduction has been correlated with such parameters as copper and hydrogen ion concentration, geometric factors, flow rate, and temperature. The character of the precipitated copper as a function of flow conditions and rate of PreciPitation has been observed under a variety of conditions. ThE precipitation of copper in solution by cementation on a more electropositive metal has been known for many years. Basile valentine' who wrote Currus Triumphalis Antimonii about 1500, refers to this method for extraction of copper. Paracelsus the Great2 who was born about 1493 cites the use of iron to prepare Venus (copper) by the "rustics of Hungary" in the "Book Concerning the Tincture of the Philosophers". Agricola3 in his work on minerals (1546) tells of a peculiar water which is drawn from a shaft near Schmölnitz in Hungary, that erodes iron and turns it into copper. In 1670, a concession is recorded4 as having been granted for the recovery of copper from the mine waters at Rio Tinto in Spain, presumably by precipitation with iron. Much has been published in recent literature on the recovery of copper by cementation, the majority of the articles being on plant practice.5-24 The rest include articles on investigation of the variables involved25-28 and a review of hydrometallurgical copper extraction methods." This literature has established: a) The three principal reactions in the cementation of copper are Cu + Fe — Fe+4 +Cu [ 11 One pound of copper is precipitated by 0.88 lb of iron stoichiometrically. In actual practice about 1.5 to 2.5 lb of iron are consumed. 2Fe+3 + Fe — 3Fe+2 [21 Fe +2H'-Fe+2 + H2 [3] Reactions [2] and [3] are responsible for the consumption of excess iron. Wartman and Roberson'28 have established that Reactions [ I] and [2] are concurrent and much faster than Reaction [3]. b) Acidity control is important in the control of hydrolysis and the excessive consumption of iron. he commercial workable range is approximately from pH = 1.8 to 3." c) Iron consumption is closely related to the amount of ferric iron in solution. Jacobi" reports that, by leaving the pregnant mine waters in contact wi th lump pyrrhotite (Fe7S8) for 3 hr, all the iron was reduced to the bivalent condition and scrap iron consumption was cut to 1.25 lb scrap per pound of copper precipitated. He also reported that SO2 has been used successfully to reduce ferric iron to the ferrous state. d) The ideal precipitant is one that offers a large exposed area and is relatively free of rust. e) High velocities and agitation show a beneficial effect upon the rate of precipitation, as it tends to displace the layer of barren solution adjacent to the iron and also dislodges hydrogen bubbles and precipitated copper to expose new surfaces. Little work, however, has been published on the reaction kinetics of copper precipitation on iron. Cent-nerszwer and Heller20 investigated the precipitation of metallic cations in solutions on zinc plates. They found the cementation reaction to be a first-order reaction. The rate constant was independent of stirring for high stirring rates and they concluded that the rate is governed by a diffusional process at low stirring speeds and by a "chemical" process at higher stirring speeds where the rate reaches a constant value. This conclusion has been challenged by King and Burger30 who could not find any region where the rate was independent of the stirring speed, although the rate constant they had obtained for high stirring speed was greater than the maximum value of the rate constant reported by Centnerszwer and Heller (by a factor of six). King and Burger, therefore, concluded that the rate of displacement of copper was controlled only by diffusion. Cementation of various cations on zinc has been summarized by Engfelder.31 APPARATUS A three-necked distillation flask of 2 000-mm capacity was used as a reaction vessel. A pipet of 10-mm capacity was introduced through one of- the side necks, the sample of sheet iron, mounted in a rigid sample holder, through the other, the stirrer being in the middle as shown in Fig. 1. The whole assembly was immersed in a constant-temperature bath. The stirrer was always placed at the same depth in the solution. EXPERIMENTAL PROCEDURE Reagent-grade cupric sulfate (J. T. Baker Chemical Co., N.J.) was used to make up a stock solution containing 10 g of copper per liter which was then diluted to various concentrations as required. Experimental data were obtained by measuring the amount of copper and iron ions in solution at successive time intervals. The initial volume of the solution was always 2000 ml, 10-ml aliquots being removed each time for chemical analysis. Because the total volume change of the solution was less than 10 pct, no correction was used for solution volume change. Nitrogen was bubbled through the solution before and

Jan 1, 1968

By J. P. Matoney, E. J. Sandy, D. A. Dahlstorm

INTRODUCTION Before an understandable discussion concerning coal-dewatering processes can be initiated, it is necessary to define some terms of usage. The many different meanings and interpretations of terms preclude development of standard definitions so that the terms which are defined in this chapter should be regarded mainly as working terms intended to facilitate communication. A coal slurry ' might be defined as a watery suspension carrying particles of fine coal and other assorted material ranging upward in size from the finest clay particles. Some particles may be in the colloidal sue range and exhibit characteristics of suspended colloids. The dilution of the system generally is such that it is in a condition of independent particle subsidence. In some coal mining areas a slurry is regarded as a suspension of fine coal and other materials having a dilution that cannot be economically dewatered by filtration. A coal slime may be regarded as a slurry containing particles of such size range that 50 per cent or more (by weight) will pass a 200-mesh sieve. Slime suspensions generally are difficult to handle without special treatment in conventional sedimentation equipment. A coal sludge is defined as a slurry that has been partly dewatered by sedimentation usually to a thick or viscous consistency where further dewatering can be most readily facilitated by filtration. Culm and silt are terms characteristic of coal-preparation practice which should be defined. In anthracite terminology, culm is the generally coarse residue or waste accumulation of coal, bone and rock from preparation plants most of which are no longer functional. Culm has a wide range of sizes, some rather coarse, and except to differentiate it from silt, the term is of limited interest in this discussion. In anthracite terminology, silt is the accumulation of waste fine coal, bone and slate settled out from preparation plant water in excavated basins. Silt is generally made up of particles ranging in size from 3/32-in. round-opening screen to the very finest sues. Silt is also referred to at times as sludge, fines, slush, and mud and is the partly dewatered derivative of what has been previously defined as slurry. In the terminology of the bituminous coal producing areas, the word culm commonly corresponds to slurry or slime, depending upon the size distribution of the suspended solids. Editor's Note: Because of the numerous and varied contributions of the associate authors of this chapter, the text does not differentiate between sections authored by each individual as is the case in most chapters of this book.

Jan 1, 1968

By H. J. Gluiskoter

The chlorine content of the coals in the Illinois Basin ranges from 0.00% to more than 0.60%. The chlorine content of the Herrin (No. 6) Coal has been mapped on a regional scale and, in general, increases with the depth of the coal. The depth-chlorine correlation exists because the coal is in apparent equilibrium with the composition of the ground water associated with it, and the salinity of the ground water generally increases with depth. At least part of the chlorine can be easily removed from the coal in the laboratory. In a natural weathering experiment, chlorine values decreased markedly during an 8-week period. Results to date indicate that none of the coals studied has a sufficiently high chlorine content to make it unusable in high-temperature steam boilers, although special steps may be necessary in the preparation or utilization of some of the highest chlorine coals. Investigations into the occurrence and distribution of chlorine in Illinois coals have been in progress at the Illinois State Geological Survey for over 35 years. Since 1948, chlorine analyses of face channel samples and of drill core samples of coal have been made routinely. The increased interest in chlorine and alkalies in coal in the U.S. followed that in Europe, where power plants during World War II were called upon to produce at higher levels than previously and with less down time for maintenance. Higher steam temperatures were reached, resulting in increases in the amount of fouling of external heating surfaces and in corrosion of boiler tubes when high chlorine coals were used. Early studies of the problem showed that coals with high chlorine content were more likely than those low in chlorine to cause difficulties in installations fired with powdered fuel. Crossleyl reported that the first rule of thumb developed for British coals was that coals considered to be high in chlorine (more than 0.30%) caused the most trouble, those intermediate in chlorine content (0.15% to 0.30%) were less likely to cause difficulties and those low in chlorine (less than 0.15%) generally were not associated with alkali bonded deposits and corrosion. However, this relatively simple picture was not adequate to characterize the difficulties that could be expected during the utilization of a large number of coals and Crossley1 developed another scheme for assessing the chances of superheater corrosion. This scheme took into consideration the observation that coals high in sulfur as well as chlorine are more likely to cause corrosion and fouling than coals low in sulfur and high in chlorine. Crossley also considered the ash content. When two coals had the same chlorine and sulfur contents, the one with the greater amount of ash would be the less likely to cause difficulties. Knowing only the amount of chlorine in a coal obviously will not give all the answers. Indeed, the significance of the chlorine content has been much discussed and it has been suggested that perhaps the total alkalies are a better indicator of possible troubles. The observation that the deposits that form

Jan 1, 1968

By Henry G. Dorsett

Dust explosion data obtained in laboratory tests by the Bureau of Mines are presented for 73 chemical compounds and mixtures, 29 drugs, 27 dyes, and 46 pesticides. Information is given on ignition temperatures of cloud and layer, minimum igniting energy, minimum explosive concentration, percent of inert dust required to prevent flame propagation, limiting oxygen concentration in the atmosphere to prevent ignition, and pressures and rates of pressure rise at dust concentrations of 0.1, 0.2, 0.5, 1.0, and 2.0 ounces per cubic foot. Explosibility indexes are computed where data are available to permit comparison of the relative explosion hazard. Variations of explosibility parameters with chemical composition are discussed. General means for minimizing the dust explosion hazard are reviewed.

Jan 1, 1968

By J. Campbell

The negative pressure developed within a solidifying sphere of pure iron is investigated theoretically assuming an elastic-plastic model. The maximum hydrostatic tension attainable is shown to be an order of magnitude smaller than that required for the homogeneous muclealion of pores in the liquid cove, and four orders of magnilude smaller than that predicted from) a rigid shell model. It is well-known that liquids can withstand large hydrostatic tensile stresses, or negative pressures. The various experimental investigations of the tensile strengths (often called the fracture pressures) of liquids are reviewed by Dean,1 and the theoretical attempts at estimating fracture pressures are critically assessed by wakeshima.2 Using Fisher's3 quation, the fracture pressure of pure liquid iron is about -70,000 atm, which may be too large by as much as a factor of 4, but is certainly correct to within an order of magnitude.' In view of the great importance of the problem of the nucleation of shrinkage cavities in castings it is of interest to determine exactly what tensile stresses can exist in the residual liquid in a solidifying casting; it has often been assumed that, because of the very low strengths of solid metals near their melting points, no interior stresses are developed at all. Nussey4 has determined theoretically the pressure in the liquid core of a solidifying metal sphere assuming that the solidified shell does not deform (i .e., is perfectly rigid), so that because of the contraction accompanying solidification (a) (about 3 pct for most metals) the progressive deposition of solid onto the inner surface of the shell causes the remaining liquid to be expanded to make up this difference in volume. This leads to a relation between the pressure P in the liquid, the initial pressure, PO, the bulk modulus of the liquid, K, and the inner and outer radii of the solid shell, o and b, respectively:

Jan 1, 1968

By Kenneth J. Kurry

12.2-1. Introduction. Successful management constantly strives to improve its methods and equipment in order to produce a better product at reduced cost. It is not enough that managers be cost conscious and industrious in these days of rapid, dramatic technological development. They must keep abreast of these developments-new or improved methods, machines, and equipment. Most of the machines and equipment have been carefully designed and perfected by reliable companies. However, improvements and progress often evolve from a definite need and are most successful in a particular operation. What may be the "answer" to the requirements of one company may be totally useless or inefficient to those of another. The manager of today must continuously evaluate the myriad proposals for change that result from modern technology-in terms of the particular needs and objectives of his company-to determine correctly which will best satisfy those needs and reach those objectives. Each new method or piece of equipment must receive careful study to make certain it is compatible with the entire operation. It may solve a problem in one department only to create a new problem in another. There are many pitfalls to be avoided in obtaining the necessary facts, and often these problems are unrelated to the actual use of the equipment or method being studied. All facets of the operation being considered must be thoroughly studied to determine if the method is compatible to the entire operation. For example, in considering a possible recommendation that a certain method and type of equipment be used to transport ore, some of the factors that should receive close scrutiny are: blasting procedure, maintenance, turning radius, percent grades, weather extremes, dumping problems, tire problems, length of haul, operator acceptance, or mismatched equipment. Failure to consider every factor-large and small, present and future-in evaluating a proposed change can mean a large investment in a new method or machine that will have to be continued for years at higher-than-antici-

Jan 1, 1968

Jan 1, 1968

By J. P. Van Kleunen

9.3-1. Introduction. The demands of industry for handling materials at higher rates and at reduced costs have had a very significant effect on belt conveyor technology. Although the general appearance of the belt conveyor today is essentially the same as it has been for the past several decades, the similarity ends there. Each component comprising the conveyor system has been continuously improved through design and materials technology to enable present conveyor systems to operate at ever-increasing rates and reliability. For example, twenty years ago the strongest commercially available, fabric-reinforced conveyor belting had a tension rating of 50 lb per ply-in. Currently, fabric-reinforced belts are available with ratings of 350 lb per ply-in. and steel cable reinforced belting is available with tension ratings of 3000 lb per in. of belt width (3). These technological advances have therefore enabled the belt conveyor to not only attain acceptance as a preferred method for in-plant movement of bulk materials, but also to be used for long distance transportation of bulk materials, particularly in areas of adverse terrain. The information contained in this chapter is intended to assist the reader to make basic decisions regarding the use and application of a conveyor system. The design of an overland conveyor transportation system or an in-plant process conveyor is accordingly beyond the scope of this article. Many comprehensive technical works covering the design of a belt conveyor are currently available from the manufacturers of materials handling equipment (6, 7, 9, 11). The design handbook published by the Conveyor Equipment Manufacturers Association is particularly recommended (2). 9.3-2. Conveyor Capacities. One of the most important factors in determining the proper size of a conveyor system is the rate at which material must be handled. Although tables and charts are available to the conveyor designer to assist him in his selection of conveyor components, only the

Jan 1, 1968

By M. M. Tilman

The objectives of this research were to determine the practicability of using cobalt as a means of controlling the amount of ferrite in the micro-structures of semiaustenitic stainless steels, and to determine the effects of reduced ferrite content on mechanical properties of these steels. Cobalt additions of up to 3 weight-percent were made to type 17-7 PH2 (AISI 631) stainless steel. Ferrite contents were determined for alloys in the aged condition, and for alloys quenched from the hot working temperature. Ferrite can be completely eliminated from the microstructure of 17-7 PH stainless steel by additions of cobalt, but complete elimination of the ferrite phase results in lower tensile strength, yield strength, and hardness. Tensile properties, hardness, and impact strength were determined for aged material. A subzero temperature treatment before heattreating was necessary to obtain maximum strength in the alloys containing cobalt. Addition of 2 weight-percent cobalt enhances mechanical properties of 17-7 PH stainless steel.

Jan 1, 1968

By Klaus Detert

Fifteen and 18 pct Ni maraging steel and several binavy and ternary alloys of the iron-rich corner of the Fe-Co-Ni system have been studied. After annealing in the austenite range, these alloys were deformed slightly by cold rolling and subsequently aged. Compavison of experimental measurements at various processing stages indicates that small degrees of deforn~ation (5 to 10 pct reduction in thickness) do not influence hardness and strength or the aging kinetics. Electrical resistivity and ductility are somewhat redu]ced and the coercive force is substantially lower when compared to identical samples which were not deformed. The results are explained in terms of retained austenite which transforms into martensite with the small amount of deformation. RECENTLY there has been increasing interest in maraging steel for applications in electric power generators requiring a high ratio of power to weight.' Fifteen pct Ni maraging steel has been investigated to evaluate its properties and performance for application as high-strength magnetic rotor steel,' and a thorough investigation of the precipitation and transformation processes in this alloy has been conducted in this laboratory.3 The influence of deformation, which preceded the aging treatment, was also studied. It was found that a small deformation in the order of 5 pct has a rather striking effect in reducing the coercive force. Other interesting effects on the properties caused by such deformation have led to the more detailed studies reported herein. EXPERIMENTAL METHOD The methods used to produce the samples from 15 pct Ni maraging steel have been described elsewhere.3 The general procedure of hot forging and cold rolling to sheet has been followed. The composition is included in Table I which also contains the composition of the 18 pct Ni maraging steel grade 250 studied. More data about the material and the processing of the 18 pct Ni maraging steel have been recently reported.4 The experimental alloys of binary and ternary Fe-Ni-Co alloys were made by levitation melting in an argon atmosphere and casting into rod-shaped ingots 7 mm thick weighing 20 g. From these ingots 25-mm-long rods were machined to study the phase transformation by a dilatometer. These rods were then cold-rolled to strips, 2.4 mm thick. Annealing for austenitizing was done in tube furnaces in an argon or helium atmosphere followed by cooling in the water-cooled portion of the tube. Aging was done in a salt bath containing a neutral blend of Alkali nitrates and nitrites. Vickers hardness was measured using a load of 50 kg for 15 sec. Tensile tests were carried out on a hard beam tensile tester at a strain rate of 5 X lo-' per sec using flat samples with a gage length of 37.5 mm and a cross section of 1.25 by 6.25 mm. Estimated sensitivity was 5 K x strain and 0.35 kg per sq mm stress. Magnetic saturation was determined on small cylindrical samples, 2.5 mm in length and diameter, by measuring the force exerted by the gradient of a magnetic field of 1000 oe per cm in a mean field of 11,500 oe. The measured values could be reproduced within *1 pct. Coercive force was measured by a precision-type magnetic field probe in a magnetic coil as described by Foerster.5 The magnetizing field was 1300 oe. The samples were 5 cm long, 1 cm wide, and 2.4 mm thick. he coercive force was measured to within +0.1 oe. Electrical resistivity was measured by using a potentiometer on flat strips with a gage length of 100 mm and a cross section of 2.5 by 0.5 mm. The accuracy of the measurement was 0.1 pct but the reproducibility of the measured specific resistivity among different samples was in the order of 1 pct. The method used to prepare the samples for electron transmission has been reported elsewhere.3 RESULTS Fig. 1 shows the influence of deformation after annealing on the resistivity, hardness, and coercivity. The samples were annealed for 30 min at 1000"C,

Jan 1, 1968

By J. R. Mihalisin

Phase changes in as-cast alloys in the Ni2 CoCr-Ni, Ti-NSAl system containing 0.1 wt pct C were studied after heat treatment at 1650°F. It was found that a vegion of CrCo-type s was developed in this system after I1000 hr. The tendency for s formation was dePendent upon the aluminum and litanium content, the s -forming tendency generally becoming more pro-nounced as the latter two elements are increased. s lended to form in interdendritic regioues and was associated with solutioning- of- carbide phases. Electron- vacancy computations for prediction of s formation on these alloys mere in sufficient agreement with what was observed experimentally to indicate that the method should be of value in assessing a-forming potential in cast alloys. However, the correlation of electrotz- vacancy numbers may not be as favorable in cast as cormpared to wrought alloys. THE increasing use of high-temperature alloys for longer times at higher temperatures has resulted in a real need for obtaining information on the phase changes taking place in these alloys since these changes often have a direct effect on properties. This paper reports on a study of the phase changes in Ni-Cr-Co-Al-Ti alloys after prolonged heating at 1650°F. The alloys were selected from the pseudo-ternary system Ni2CoCr-Ni3Ti-Ni3Al and this system was chosen because it is the basis of many of the newer cast commercial superalloys. The attempt here was not to define accurately the boundaries of s formation in the NizCoCr-Ni3Ti-Ni3Al system but to delineate the phase transformations taking place upon heating alloys covering a wide range of chemistries in this system. An addition of carbon was made to all alloys to further simulate commercial alloys. It was hoped that the information generated in this manner would be of more direct use to superalloy designers than an equilibrium diagram approach since commercial alloys generally have outlived their usefulness when equilibrium is attained. EXPERIMENTAL PROCEDURE The alloys were vacuum-melted from carbonyl-nickel pellet, vacuum-grade chromium, electrolytic cobalt, high-purity aluminum and titanium, and spec-trographic-grade carbon.

Jan 1, 1968

By G. S. Cole, G. F. Bolling

Fluid flow strongly influences ingl structure and the columnar -to-equaaxed transition. Artificial flow patterns siwzilar to the nuturul ones act to induce this transition, while dampening forces act to suppress this transition. It is shown here how simple mechanical forces can be applied to a systerrz in order to induce or slipPvess relative fluid flow and the change both the structure transition and the exact structures obtained. The example used is the effect of slow rotations and oscillations 012 a cooling- ingot (of laboratory scale). The details of rotution and oscillation for various cooling rates, lenlperal~ire gradients, and sizes of ingot are related to other solidzfication variables. THE grain structure of a casting can be changed by altering the fluid motion during solidification. Just how important these changes are depends directly upon the degree to which the fluid motion can be controlled. An early step in understanding the nature and influences of fluid motion was taken by studying natural thermal convection; when a static mechanical device was used to suppress natural flow the result was opposite to that obtained when an electromagnetic device was used to augnlent flow in a pattern similar to the natural one. ''2 Suppression allowed more columnar growth to occur, but "augmented natural convection" brought about an earlier columnar-to-equiaxed transition (CET). Since the solidification of a free ingot must have characteristics somewhere between those displayed during suppression and augmentation, we know that natural convection must influence the CET. Further, since heat transfer in the liquid is always some time-dependent combination of convection and conduction, it can easily be guessed that the temperature gradient in the liquid is the vital factor affecting the CET.1,2 It is obvious that the structure arising from the unadulterated solidification of an ingot, without external influence, is rarely if ever the best possible one. Although the pattern of the natural fluid flow may be considered efficient, the magnitude of the flow and the heat transfer decrease freely from the outset. For a

Jan 1, 1968

By P. E. Cavanagh

"The Davis tube test has been used for many years as a laboratory method for determining the magnetic iron re-coverable from a magnetite iron orebody. This paper de-scribes a method for determining the recoverable iron from ores of the Labrador Trough type, with the usua1 flow sheet utilizing spirals followed by magnetic separation.The mechanical structure of a metamorphosed iron ore, resulting from recrystallization over long periods of time, is the basis for the laboratory method developed. Similarities between the structures of such recrystallized ores and the structure of annealed and recrystallized steel are noted.A laboratory technique to determine the size of the different grains of gangue and iron ore minerals is de-scribed and the application of this information to arrive at recommended grinding techniques and flow sheets is demonstrated. The use of the method to determine recoverable iron in such ores is compared to actual iron recovery in the pilot-plant and commercial concentrations of the same ore.The use of a specified lower limit of recoverable iron as determined by this method, in order to design open-pit limits, achieves practical results when compared to designing a pit based on an arbitrary lower limit of total soluble iron. The Ungava Iron Ore deposits are used in giving an example of the resulting pit design changes."

Jan 1, 1968

By Noel Jarrett, Allen S. Russell, Bernard M. Starner, Stanley C. Jacobs

A process has been developed to refine high-grade commercial aluminum to 99.99 pct purity. This enzploys precipitating titanium, vanadium, and zirconiu~ as borides. The upgraded liquid is partially crystallized under conditions that prevent massive freezing. The resulting crystals are compacted and washed free of adhernig impure liquid aluminum by melting the top crystals while draining off the liquid. Finally, the bottorn portion of the crystal bed is melted and removed as the pure product. Leakage from the crystallizat~on vessel is prevented by a layer of alumina granules that are not wetted by the aluminum. ALUMINUM of 99.99 pct purity is desired in a variety of applications. These include electrolytic capacitors, catalyst carriers, decorative trim for automobiles, aluminum powder, and high-strength alloys. This market was for many years filled by refining commercial-purity aluminum in a three-liquid-layer electrolytic cell of the type originally proposed by Hoopes. To meet the expanding need for lower-cost high-purity aluminum, a refining process based on chemical precipitation and fractional crystallization was developed. The availability of this super-purity metal was announced in November 1961, and three patents1-3 relating to the process were issued in 1965. An alternate process, comprising continuous fractional crystallization of a portion of a liquid-aluminum feed stream under conditions of strong agitation at the surface of the growing crystals, was published by Dewey4 in 1965. Earlier proposals by Larsen 5 and by Regner6 also emphasized the advantage of rapid agitation of the melt in the region of the crystallization zone. johnson 7 more recently proposed extracting purified aluminum from an alloy by mixing crystals of pure aluminum into the molten alloy, allowing them to grow, and removing the pure aluminum as by casting. Aamot's 8 recent patent describes a freeze refining process that involves controlled partial freezing against cooled moving retort walls. The Alcoa process to produce high-purity aluminum is schematically described in Fig. 1. Relatively pure aluminum is treated with boron in a furnace (a) to precipitate high melting point impurities, the supernatant liquid is transferred to a crystallization vessel (b), the liquid is partially crystallized with mechanized "tamping" (c), the remaining impure liquid is tapped out and the crystal bed partially and directionally re-melted to wash the underlying crystals (d), and the balance of the crystals is melted and withdrawn as high-purity aluminum (e). PRINCIPLES OF FRACTIONAL CRYSTALLIZATION Commonly encountered impurity elements form two types of systems with aluminum. Titanium, vanadium, and some other transition elements in periodic groups IV, V, and VI are the high melting point impurities. Initial solidification of aluminum containing small percentages of these elements will produce solid markedly enriched in them at temperatures slightly above the freezing point of high-purity aluminum. Most other elements, such as silicon and iron, produce eutectic type reactions with aluminum. In this case the first solid formed on initial solidification at temperatures slightly below the freezing point for high-purity aluminum is markedly depleted while the remaining liquid is enriched in these elements. The equilibrium change in composition during solidification of aluminum contaminated with silicon, iron, or titanium is illustrated in Fig. 2. Here, for clarity, the temperature scale is expanded beyond the

Jan 1, 1968

By Samuel J. Sims

The Grace mine magnetite deposit, located 2 miles north of Morgantown in Berks County, Pennsylvania, was discovered in 1948 by an aerial magnetometer survey. It is situated on the southern border of the Triassic lowlands section of the Piedmont province. Cambrian sandstones, shales, and limestones overlie Precambrian crystalline rock and were folded and thrust-faulted during the late Paleozoic Appalachian revolution. Late Triassic continental sediments were deposited on the deformed basement rocks and were intruded by Late Triassic diabase dikes and sills before regional tilting and normal faulting occurred. The Grace mine magnetite ore is characteristic of the Cornwall type. The ore has replaced a Cambrian limestone lens isolated between Triassic diabase footwall and Triassic sedimentary rock hanging wall. The ore body is roughly tabular in shape, dips 20° to 30°NE and plunges about 20°N80°E. The ore is granular, fine- to medium-grained, typically consisting of unevenly distributed magnetite in a matrix of light green to white serpentine gangue. Magnetite is the major ore mineral, pyrite and chalcopyrite are common accessory minerals, and pyrrhotite occurs locally. Sphalerite, marcasite, galena, hematite, digenite, and goethite are uncommon. Serpentine, talc, and chlorite are the major gangue minerals; calcite and dolomite are common, and phlogopite, tremolite, and biotite are present locally. Apatite is a common accessory; sphene is rare. Calcium-magnesium silicates were formed first by contact metamorphism of impure limestone by the intruding diabase. Later, the silicates were altered hydrothermally to the serpentine- talc-chlorite assemblage now present. Magnetite, the first ore mineral, formed by replacing serpentine and was followed by pyritepyrrhotite and then by chalcopyrite-galenasphalerite. Marcasite, secondary pyrite, goethite, and hematite are secondary minerals resulting from alteration of pyrrhotite and magnetite. It is estimated that confining pressure was about 1500 bars and the temperature range was 500° to 675°C during ore formation.

Jan 1, 1968

By C. A. Rowland

Wet grinding rod mills have been used for 50 years to grind ores and to make specification sand. The application of wet grinding rod mills is well understood. Until recently, there have been very few installations of dry grinding rod mills. The basic principles learned from wet grinding rod mills that were used in the application of dry grinding rod mills are 1. It is possible to extrapolate the performance of 5' and 6' diameter wet grinding rod mills into larger diameter rod mills with the larger mills performing as predicted. Wet grinding rod mills as large as 14' diameter (inside shell) by 20' long using 19.5' long rods are in use operating satisfactorily. 2. Wet grinding rod mills generally grind more efficiently when the fines are left in the mill feed than when the fines are removed from the feed. 3. Wet grinding rod mills produce little tramp oversize and generally can be operated in open circuit except when very close control on the top size in the product is required. When operated in closed circuit, the circulating load is normally less than 100%. 4. The power required for the desired grind can be accurately determined from the work indices obtained from rod mill grindability tests on the material to be ground. Where required it is necessary to, apply inefficiency factors for oversize feed and for larger or smaller than normal- ratios of reduction. Recent applications for rod mills have developed where it is required that dry grinding be used. These recent applications cover the grinding of 1. Lead sinter, lead slag and limestone. 2. Iron ore. 3. Silica for making glass sand. 4. Cement clinker. 5. Coke.

Jan 1, 1968