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By Michael A. Toole, O&apos

INTRODUCTION The tremendous capital investment required to produce a low grade ore deposit demands a reliable answer to the question: "How much does it cost to drill a well to produce the uranium that geologists have indicated is there in the ground?" However, you will find the answers given will be many and varied, depending on whether they come from the operating company, the drilling contractor, a geologist, a reservoir engineer, purchasing agent, or whoever. Each generally considers only a limited area of the total operation. The operating company usually depends upon the drilling contractors, service companies, and consultants to supply expertise. Because it is often difficult to see the "whole picture" or even to agree upon what the "whole picture" is, planning a well program and its costs is often done piecemeal. Frequently, costs "saved" in one area of the program are needlessly spent in another, because the effect of one area upon the other was overlooked. Since the drilling fluid is such an influential part of the drilling program, it should be given utmost consideration when planning the overall program. As W. D. Lacabanne wrote in 1954: "The drilling fluid system is understandably called the heart of the rotary oil drilling rig. Any other type of rotary rig.... should benefit by the incorporation of mud fluids in the drilling scheme." And G. R. Gray mentions that "The driller recognizes the drilling fluid as one of the useful tools available to solve drilling problems." However, in minerals drilling, only in recent years has the drilling fluid been considered as more than a tool to get through special problem areas. Although there are many similarities between drilling for oil and gas and drilling for minerals, the differences in the drilling equipment used justifies designing specific fluids for the minerals drilling industry. NL Baroid/NL Industries, Inc. has been a leader in introducing such fluids and in providing technical know-how to the minerals drilling industry. The purpose of this paper is: (1) to discuss the selection of drilling fluids to meet specific drilling conditions during both exploration and production and (2) to show the interrelationship among factors present in the exploration and production phases that influence total well costs. DRILLING FLUIDS FOR DRILLING PROBLEMS The drilling fluid is a tool that can be used to improve drilling performance by improving hole cutting, cleaning, stability, and formation productivity. Properly formulated and maintained drilling fluids enable the drilling operation to be carried out with increased efficiency and lower total (overall) costs. However, it should be noted that not all drilling problems can be solved by even the most carefully prepared and maintained drilling fluids. Of the many possible drilling problems encountered in a well before reaching target depth, this paper will discuss only those most likely to be present in the shallow [61 to 610 m (200 to 2000 ft)] drilling operations in South Texas. LOST CIRCULATION Loss of circulation is the most common problem encountered in drilling. Because the losses occur under varied conditions, it is often difficult to determine the exact causes. "Lost circulation" or "lost returns" means the partial or complete loss of drilling fluid to voids in the formation. "Loss of water" while drilling with water may take place into any permeable section and should be distinguished from "water loss" or filtration of fluid through the filter cake of mud solids laid down on a permeable formation. "Loss of water" can frequently be stopped by the addition of colloidal sized clay particles such as high yield bentonites, whereas "water loss" may be controlled with organic polymers. Subsurface conditions that lead to loss of circulation can be classified as: (1) natural fractures, (2) induced fractures, (3) unconsolidated or highly permeable formations (loose gravel), and (4) cavernous formations (crevices and channels). Loss of circulation may occur whenever the borehole pressure exceeds the formation pressure. The greater the differential pressure, the more likely it is that circulation may be lost. To stop loss of whole mud, voids must be bridged so that a filter cake can be laid down on the permeable section. The plugging material must be of the proper size and shape to offer greater resistance to the fluid flow around it than the flow up the annulus. A plugging composition that satisfies these requirements may not be able to be handled by the small rig pump available.

Jan 1, 1979

By Byron E. Eldred

(Pittsburg Meeting. March, 1010.) GENERALLY speaking, the practical study of combustion has been made mainly from the stand-point of the steam engineer. This. narrow view-point has left open a large field for scientific research on the application of combustion in other arts, where the conditions of heat-utilization are widely different from those presented in the steam-generator. The great economic importance of the boiler and the ease of measuring its performance, together with the comparative uniformity of conditions in the steam-generator, is, probably, quite largely responsible for the practical neglect of the study of the use of fuels in other arts save only on the basis of their thermal value. Yet these other arts show quite plainly that a thermal-value basis alone is Dot sufficient. For example, in burning lime, under ordinary conditions of firing, a cord of wood will do as much work as a ton of coal, though the latter affords more than twice the number of heat-units. Similar results are evidenced in burning brick, in the roasting of certain ores, in reheating billets, and in many other arts where heat is to be applied over extended areas to fragmental masses of more or less refractory materials. In these arts much is to be gained by a careful study of the application of the heating-agent in the form of the long flame, and in the production of the heat in contact with, or in direct proximity to, the object to be heated. Of necessity, in boiler-practice, combustion cannot be maintained in actual contact with, or in close proximity to, the object to be heated. Speaking in a general way, heat is imparted from burning bodies to things to be heated in two ways : directly, by radiation, and indirectly, by transfer of the sensible heat of hot gases by convection or contact; by conduction from the hot uses. Both ways are utilized in boiler-practice-directly, by

Jun 1, 1910

By Paul Hunt

UP to June, 1923, the Park-Utah mine had shipped about 94,000 tons of a direet-smelting ore of a gross value of $4,200,000, or about $45. a ton. These values were in gold and silver only, although the ore carried small amounts of lead, copper and zinc. Freight, treatment and deductions had averaged $15.40 a ton. At the expiration of the Pittman Silver Act there was in sight about 30,000 tons of a similar ore with a gross value of about $15 a ton in gold and silver, and a large body of partly developed lead-zinc ore of a gross value of about $20 a ton, 40 per cent. of which was represented by the lead-zinc content and the balance by the silver and gold. Mine costs had been high during the life of the Pittman Act, but as a large part of the profits had gone into equipment of the mine and the orebodies were large and had good walls, we knew that mine costs could be greatly reduced. We were therefore faced by the necessity of getting lower freight and smelter rates or of concentrating the ore. We did obtain better freight rates on lower grade ore, and a favorable smelting rate on the small tonnage of siliccous silver-gold ore, but this smelter rate could not be applied to the lead-zinc ore with any profit to ourselves. The Judge mill of the Park City Mining & Smelting Co., with which we were affiliated, was running to capacity; if we built our own mill it ineant a 5-mile freight haul to a satisfactory millsite and a year's delay. Fortunately, the International Sillelting Co. had just inherited a mill at Tooele which, with some changes, was about double the catpscity required for its own ores. Flotation tests were run on Park-Utah ore and a contract entered into with a low base treatment charge per ton, the tariff being largely fixed by the metallurgical deductions. This contract has been admirably calculated so that the miner can follow a lean orenbody to its limit. Such a procedure has no doubt made it difficult for the smelting company at times, but it has resulted in finding ore extensions that otherwise might have been missed, so In the long run it has profited too. A flat rate per ton would have been like mining up to the claim endlines in a great many of the stopes. In order to offer such a contract it can be inferred that the smelting company must have been able to make high reeoveries and high-grade products on a very lean ore.

Jan 1, 1928

By Arthur La Motte

I NDUSTRIAL explosives, as distinguished from military explosives, include high explosives and blasting powder. The high explosives which are best known are straight dynamite, gelatin dynamite, ammonia dynamite and permissibles. There are two kinds of blasting powder, saltpetre blasting powder and nitrate of soda blasting powder. Blasting powders are mechanical mixtures of nitrate of potash or nitrate of soda with sulfur and charcoal, highly compressed, granulated and glazed. They ignite from a spark and burn with relative slowness, the rate of burning and hence the rate of conversion into gases depending upon the size of the granulation and upon the degree of. confinement under which the powder is placed. High explosives, on the other hand, are chemical compounds which detonate; that is, when the explosive is subjected to a violent shock, provided in practice by a blasting cap or an electric blasting cap, the molecule of the essential ingredient, usually nitroglycerin, is disrupted and the energy and heat released cause any other explosive ingredients which may be present, such as ammoniuin nitrate or T.N.T., to decompose with a resultant evolution of gases at an extremely rapid rate varying from 6000 to 20,000 ft. per second.

Jan 1, 1924

By Edward Wisser

The Pachuca silver district, situated about 100 kilometers northeast of Mexico City (Fig. l), covers roughly the southeastern half of the Sierra de Pachuca. The latter is a mountain range with northwest trend, and forms a part of the northeastern rim of the topographic basin known as the Valley of Mexico. The length of the Sierra proper is about 50 km., its greatest width about 9 km., and it rises to a maximum of 600 meters above the general level of the basin floor. The Pachuca district consists of two contiguous subdistricts, the Pachuca area and the Real del Monte area. The center of the Real del

Jan 1, 1937

By K. E. Brown, F. W. Jessen

By utilizing an 8,000-ft experimental field well equipped with 10 gas-lift valves and 10 Maihak pressure recorders, gas-lift tests were conducted with port sizes ranging from 5/16 through I in. The well was equipped to provide accurate means of measuring surface pressures, temperatures, quantity of injection gas and fluid production. The tests were conducted in 2%-in. OD tubing, and the well was making 95 per cent water. A complete evaluation of gas-lift-valve port sizes shows the relationship of per cent recovery, gas-liquid ratios, minimum pressure created at the operating valve and horsepower requirements for each port. The length of time necessary for the fluid in the tubing to reach equilib.rium conditions after each cycle was recorded. Fallback of fluid at depths of 477, 969, 1,685, 2,493 and 4,290 ft was noted. For each port size, pressure loads of 2.50, 300, 350, 400 and 450 psi were lifted with a valve operating at approximately 550 psi at 6,000 ft. Gas-liquid ratios for each load were varied from excess gas to a gas volume per cycle whereby the load failed to reach the surface. Numerous curves are presented in evaluating the accumulated dara. The results show a 1-in. port to be the most efficient under all conditions. The production of intermittent liquid slugs against different-sized surface chokes was evaluated. These tests were conducted from a 7/16-in. ported valve at 4,072 ft. Tests indicate that, when possible, a %-in. in diameter choke or larger should be used at the surface. In the past few years most of the advancement in gas-lift operations has been made in continuous-flow operations. Yet, it is estimated that at least 70 per cent of the wells on gas lift in the United States are of the intermittent type. Since the term "slug flow" is sometimes used in both intermittent- and continuous-flow operations, it would be well to distinguish between the two types of flow. Continuous-flow gas lift is defined as a method whereby the fluids are produced at a continuous rate at the surface. This generally requires a continuous injection of gas through a surface choke; however, various other control devices sometimes are installed to eliminate freezing, to shut-off gas during natural flow periods, etc. The actual flow of fluids in the tubing may be of the slug type (one of many flow patterns known to exist in continuous flow). Intermittent flow is defined as a method of gas lift whereby the liquid is produced in separate piston-type slugs. Perhaps this type of flow could best be thought of as a ballistic-type flow where the liquid leaves bottom as a piston, propelled by a slug of expanding gas. Gas generally is injected through some type of control at the surface at predetermined intervals. However, the valve may have characteristics whereby gas can be injected through a small choke and still result in a ballistic-type flow. The purpose of the experimental work was to evaluate the most efficient port size to be used on the operating valve for the ballistic type of lift and, in addition, to establish the importance of utilizing a surface choke large enough to allow slugs to be produced without detrimental effects. This work is part of a compre- hensive study of both intermittent-and continuous-flow gas lift, representing a joint project conducted by the Ohio Oil Co., the Sun Oil Co., Otis Engineering Corp, and The U. of Texas. The problem of evaluating port sizes has been given little previous attention. Some work undoubtedly has been done which has not been published to date. Some tests were conducted when the wireline, mechanically-opened valve (Nixon) first came on the market. This valve was capable of utilizing full tubing area as its port size. It is known that this was a very efficient valve, but to the authors' knowledge the results of tests have never been published. EXPERIMENTAL EQUIPMENT These tests were conducted on an actual field well, the Ohio-Sun Unit Well No. 2-E, in the North Markham-North Bay City field, Matagorda County, Tex. The well incorporated 23/8-in. OD tubing and produced 95 per cent water. Since the running of equipment was to be quite elaborate and expensive, a well was selected in which both intermittent- and continuous-flow tests could be conducted. This particular well was capable of producing in excess of 1,000 B/D of liquid (95 per cent salt water), yet with a 3/64-in. in diameter bottom-hole choke, production was controlled to 82 B/D. Most of the intermittent tests were conducted at this low rate. Figs. 1 and 2 show all the surface and down-hole equipment. As can be seen, every attempt was made to insure that ample equipment was available for reliable testing procedures. Fig. 1 shows the surface testing equipment. The input gas was controlled first by a regulator, then

By Paul C. Merritt

Chrysotile asbestos producers in Quebec may soon experience a unique situation-i.e., strong competition from American ore sources for the short fiber market west of the Mississippi River. This com- petition will be forthcoming from Copperopolis and Coalinga, two deposits now being developed on opposite flanks of the San Joaquin Valley in central California. The combined output now planned from both deposits is 100,000 tons annually, equivalent to about 50% of the annual market demand in the western, central and Gulf States, and more than twice the tonnage sold in 1960 by all other American asbestos producers combined. The principal companies involved in these new undertakings are Jefferson Lake Asbestos Corp. (subsidiary of Jefferson Lake Sulphur Co.), Hidden Splendor Mining Co., Coalinga Asbestos Co. (Johns- Manville Corp. in conjunction with Kern County Land Co.), Union Carbide Corp., and Asbestos Corp. Ltd. Jefferson Lake's principal interest is at Copperopolis where the company's new 70,000-ton per yr mill recently went on stream. The company also holds some claims at Coalinga, but this latter area is better known as the site where Hidden Splendor, Coalinga Asbestos Co. and Todd Industries (a local company) have established operating mines and mills capable of turning out 30,000 tons of fiber each year. Coalinga is also the site of exploration by Union Carbide Nuclear and Asbestos Corp. Ltd.

Jan 9, 1962

By A. Ross Rornmel

ABILITY to speak effectively is one of man's most longed for and coveted abilities. It is the ability to stand on one's feet, transfer knowledge and thoughts to others, to reach an objective professionally or otherwise by leading groups through a channel of planned thought. Each day group speaking plays an important part in making or marring success, and the engineering profession often provides this opportunity and requirement. An ability to speak effectively develops courage, poise, confidence, and prestige for the speaker. The technical man cannot be reluctant to face an audience. He is often called upon to do this in presence of employees, supervisors, and other groups. His ability to speak effectively is as much a requirement as the fundamentals of his profession. The three fundamentals of effective speaking are: (1) Enthusiasm and Confidence. These are joined because of their close relation. (2) Preparation. This includes knowledge of the subject. (3) Presentation. By this is meant the features of delivery.

Jan 1, 1946

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

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

Jan 1, 1969

By A. E. Gorum, J. Washburn, E. R. Parker

Experimental evidence was obtained in support of the idea that cleavage fracture can be initiated by dislocation pile-up. The high ductility of MgO crystals when tested in bending comPared to their relative brittleness in tension was explained on the basis that large pile-ups are more likely in a tension specimen. CLEAVAGE fractures have been a problem of major concern for many years. A number of large steel structures have failed in a brittle manner, usually suddenly and without warning; often the failures occurred for no obvious reason and at nominal stress levels well within the generally accepted range. A great deal of data have been collected about factors that contribute to failures,1 but the physics of the fracture process has never been revealed. cottrel12 has recently developed a theory of brittle fracture in ductile materials which was based upon the concept that dislocations moving on two intersecting planes can unite to form a crack nucleus. This theory accounts for the known effect of grain size and for the effect of testing temperature. There has, as yet, been no experimental evidence published that would substantiate this or the earlier theories based on stress concentrations due to piled-up dislocations. The study reported herein was conducted to obtain information that would either substantiate or disprove the

Jan 1, 1960

By AIME AIME

WEDNESDAY night, by long tradition, is al- ways set aside for the annual dinner, even when, as it was this year, it is Ash Wednesday. Whether the somewhat smaller attendance than last year is attributable to that cause, the unexpectedly long persistence of business depression, or whatever may have been the reason, it was a joyous occasion, and the grand ball-room of the Commodore Hotel was as completely filled With diners as * was consistent with com- fort. In the half hour before the dinner was actually served the guests assembled in an adjoining room and not only exchanged greetings but proceeded along the receiving line to greet the guests of honor. The number present was so large that hardly more than half of them had been able to do this before the summons to the dining room sounded and a hearty and immediate response was made to it. Toy balloons at each plate, inflated and directed at the heads of companions or nearby friends, but which were just as likely to carom from the nose of a hurrying waiter, successfully broke the ice as well as not a few plates. It would be interesting to know whether the pleasure the guests derive from these de- vices is in part based on the all-too evident annoyance of the waiters, and what the relative quantitative relationships are.

Jan 1, 1931

By Fred Bond

WHEN some materials are ground dry in a ball mill, a stage of comminution is reached at which the finely divided particles begin to adhere to the balls and to the mill lining. As grinding progresses, a coating accumulates upon the grinding media, which tends to cushion the impacts and thus retard reduction of the material, and finally becomes so thick that all grinding ceases. At this stage, the characteristic noise produced by the grinding media dur-ing normal mill operation changes to a dull, muffled sound. In most instances, the formation of the coating marks the practical limit of size reduction. Industrial requirements for fine grinding frequently meet with this obstacle, and the tendency in many com-mercial operations to grind materials to a higher degree of fineness than formerly makes the solution of this problem an im-portant one. The phenomenon is of far greater importance, therefore, than the limited amount of research and technical discussion devoted to it implies. In order to learn more about the coating of different materials when ground dry to a high degree of fineness, certain labora-tory tests were made from which it was found that different materials form coat-ings at widely different size distributions. It is probable that most materials will coat if they are ground fine enough; the exceptions have inherent lubricating qual-ities, like coal and graphite.

Jan 1, 1940

By H. R. Coles, S. P. Chong

Test work conducted in the 6.4 and 10.5 m (21 and 34 ft) Aerofall mills at the Iron Ore Co. of Canada Carol project showed that conventionally used "deflector" type liners, which form the basic principle of Aerofall Mill grinding, did not necessarily provide the best grinding performance. A new design, using low profile liners incorporating radial ribs of proper height, actually improved the mill throughput 9-20% without sacrificing grinding efficiency. In addition, the new design reduced liner weight and scrap losses, resulting in a 25% reduction in liner consumption. It provided better protection to the mill shell and reduced the overall maintenance cost for the mills.

Jan 1, 1984

By D. Collins, B. Pina, G. Snell

The conversion of moisture and ash free (maf) coal to pyridine solubles and gas was investigated in a microautoclave batch reactor. Two washed Kentucky coal samples (KY # 9 and KY #11) were studied in liquefaction solvents of various donor strength. The liquefaction solvent hydrogen donor strength was varied by changing the tetralin content of a mixed 1 -methylnaphthalene-tetralin mixture. Primary liquefaction conversions in excess of 90 wt% in 10 minutes of reaction time @ 700° K (427OC or 800°F) were achieved with liquefaction solvents of moderate donor strength, i.e. 40% tetralin. A modified irreversible first order rate expression (eq. 1) described the experimental data:

Jan 1, 1986

By T. R. Wright

THE Corporation operates concentrators in four camps: Casapalca. Morococha, Cerro de Pa-co, and Mahr. The present concentrator at Cerro de Pasco is the newest having been completed in 1943. and that at Casapalca the oldest, having been built originally as a gravity concentrator, in 1889. Prior to 1925 the Corporation's milling operations were confined to the beneficiation of silver-bearing copper ores, and treatment of these ore: by flotation was started in 1918. Although fairly large deposits of complex, fine-grained lead-zinc ores existed, little progress had been made in the treatment of such ores--in Peru or elsewhere-until the early 'twentics. The Casapalca concentrator began the selettive concentration of complex leadzinc ores by all-flotation methods in 1925, or contemporaneously with the commercial development of selective lead-zinc flotation in the United State:.

Jan 1, 1945

By G. R. Wilms

A study has been made of the structural changes in polycrystalline high purity aluminum during the tertiary stage of creep under conditions of constant tensile load. It appears that there is no basic modification in the particular mechanism of deformation that characterized the preceding secondary stage of creep, but that the changes in crystalline structure produced during the tertiary stage are only a consequence and not a cause of the accelerated strain. Intercrystalline fissures were observed on entry into the tertiary stage, and these might supplement the accelerated rate of strain owing to local stress concentrations. There is evidence that the formation of these fissures may be associated with the presence of surface imperfections, and it is suggested that a more generalized treatment of the results may explain certain creep characteristics of commercial alloys. IN previous work'-4 a study was made of the changes produced when specimens of annealed aluminum were deformed at various temperatures and rates of strain, especially under conditions leading to creep under constant tensile load. It was shown that, as the temperature was increased or as the rate of strain was decreased, elements of the substructure produced within the grains became coarser, and with the strain rate constant at a given temperature, their size tended to an equilibrium value. The preliminary process of the breaking down of the grains into a substructure was identified with primary creep.' The subsequent equilibrium, condition was associated with secondary creep. The question then arose whether the tertiary stage corresponded to any further significant change in the substructure. The question is also of interest in view of the opinion, expressed for instance by Andrade,5 that the tertiary stage is merely an accelerated rate of strain due to the reduced area of section of a specimen under continuous tensile load, and the other opinion, as suggested by the observation by Sully, Cale, and Willoughby6 of a tertiary stage in com-pressive loading, that this third stage is a real effect in its own right. The object of this paper is to record some observations on the tertiary stage of high purity aluminum. Experimental Procedure The material was aluminum of 99.98 pct purity as previously used. The specimens had a rectangular section of l/8 x l/2 in., and extensions were measured over a 1 in. gage length. After machining to shape, the specimens were annealed to give a standard grain size of 0.2 mm and then electropolished. The general procedure involved metallographic and X-ray diffraction examination at progressive stages of elongation (marked by arrows on the curves shown in Figs. 1 and 2), the specimen being extended to fracture under constant load at a given temperature. The X-ray tests were made by the back-reflection method from a stationary specimen, using CoK radiation. The longer edge of the micrographs in the paper corresponds to the direction of applied stress. Results The previous work showed that, in the secondary stage of creep in aluminum, three basic types of structure could be developed according to the temperature and rate of strain. These were: 1—slip, which predominated at the lower temperatures and higher rates of strain and produced the finest and least perfect substructure; 2—cell structure, which superseded slip as the temperature was raised and the rate of strain decreased and which was characterized by a coarser and more perfect structure and an absence of slip lines; and 3—a stage termed "boundary microflow," which predominated at still higher temperatures and lower rates of strain when the cell size had increased and become comparable

Jan 1, 1955

By Roger Holmberg, Kenneth Mäki

This paper describe; open pit studies where blasting damage introduced in the remaining rock has been investigated. Results from two open pit mines are described and discussed. Parallel performed laboratory experiments, where simulated blasting damage has been introduced into samples before shear strength testing took place, are also reviewed. These studies are tied together in order to throw some light upon how the blasting damage influences the slope stability. A mathematical model is also described which will make it possible to optimize the blast design for a specified damage zone in the rock mass.

Jan 1, 1983

By R. E. Ogilvie, J. I. Goldstein

The a and y solubility limits in the Fe-Ni phase diagram have been redetermined at temperatures above 500°C. Both a diffusion-couple and a quench and anneal technique were used. The solubility limits were measured with an electron-probe micro-analyzer. The nickel concentration at the phase boundary is increased below 700°C and the a solid-solubility range is much larger than had been previously measured. The solubility limits are also extrapolated to 300°C. It is suggested that the solubility of nickel in a FeNi reaches a maximum in the temperature interval 400o to 500°C. THE equilibrium diagram has been of great use in the field of meteoritics, where the phase relations between kamacite (a) and taenite (?) in metallic meteorites can be described by means of the Fe-Ni diagram. The study of metallic meteorites by electron-probe microanalysis has cast some doubt on the accuracy of the presently available Fe-Ni diagrams.1, 2 Recent thermodynamic studies of the Fe-Ni system also suggest that the diagram may be in error.3 For these reasons the high-temperature (800o to 500°C) part of the diagram was redetermined. INTRODUCTION The currently accepted Fe-Ni diagram is that of Owen and Liu.4 Above 910°C, there is a region of complete solid solubility, ? (fee). Below 910°C, the a (bee) phase is stable in pure iron. The effect of increasing amounts of nickel is to stabilize the y phase. The phases that form when Fe-Ni alloys are heated or cooled bear little relation to the equilibrium diagram. If an alloy is cooled from the y state and held at a temperature within the a + y field, no evidence has been found for the occurrence of the y - a transformation.5 If the alloy is cooled to low enough temperatures the y phase breaks down into a supersaturated bee phase called a2. In fact, in alloys over 27 pet Ni the y phase is retained at room temperature.6 The a, phase has the same composition as the original y. The temperature at which a2 forms, the M, temperature, has been determined experimentally.' A state of equilibrium can be approached by cooling below M, to form a2 and then reheating the alloy into the two-phase region of the diagram. The y phase will then begin to precipitate out of the a2 phase and grow. The growth of the phase, however, is quite slow. Using the interdiffusion coefficients -Da of Goldstein et al.,8 it is estimated that it takes about 1 year to grow a 10-µ-wide region of ? at 700°C in a 5 pet Ni alloy. Owen and Liu4 used the technique just described to form the equilibrium phases. The phases present were determined by means of X-ray analysis. The accuracy of their diagram depends on the number of alloys available near the phase boundary at a given temperature. In this study two different techniques were used to determine the a/a + ? and ?/a + ? solubility limits. The inherent accuracy of both techniques was greatly improved over that used by previous investigators because the phase-boundary compositions were measured with an electron-probe microanalyzer. PROCEDURE The two methods used to determine the Fe-Ni diagram are the diffusion couple (D.C.) and the quench-and-anneal (Q.+A.) techniques. In the first method, diffusion couples whose diffusion path goes through a two-phase region of the phase diagram were used. A description of the technique used for making the diffusion couples has been described in a previous paper.' After the diffusion treatment a discontinuity in the resultant concentration vs distance profile was measured. The nickel concentrations in the a and ? phases at the interface of the discontinuity are the solubility limits of the a and ? phases in the phase diagram at the diffusion temperature. If the interface com-

Jan 1, 1965

By B. R. Banerjee

MATERIAL used throughout this investigation was high-purity aluminum (99.998 pct). The 1/2-in. cubes were cut out of a cold-rolled slab and annealed at 550°C for 1 hr before deformation. The single crystal specimen was 1 in. in diam x 0.33 in. thick, cut from a cylindrical crystal produced by cooling at about 55°C per hr in a furnace which had a convenient gradient of about 10°C in every 4.5 in. vertical crucible length. Specific data on the ten specimens studied are summarized in table I. Three types of deformation were employed: (I) compression in a hand-operated hydraulic press; (2) impact with a 7-lb sledge hammer; and (3) rolling, using a wedge-shaped specimen' to obtain a gradient of deformations varying from 0 to 50 pct along the length of the wedge. Specimens were either deformed at room temperature, or first cooled in a freezing mixture of dry ice and ether at a temperature of —72°C and then deformed between steel blocks cooled with dry ice. The specimens deformed at the low temperature were ground and polished through 000 emery paper and wheels impregnated with alundum and alumina No. 1. During this entire procedure the specimens were dipped frequently in the freezing mixture of dry ice and ether in order to maintain constantly a frosty surface as insurance against overheating. All specimens were given a final electrolytic polish, using two different electrolytes* to insure that the surface effects observed were not char- acteristic of the polishing technique. With both electrolytes, the annealed specimens gave even surfaces with good polish. Several standard etchants were tried without success. The best results were obtained with an immersion etchant, developed in this connection, containing: hydrofluoric acid, 4 parts; nitric acid, 1 part; glycerine, 3 parts. Discussion of Results Typical strain markings have been observed within deformation bands, as shown in figs. 1, 2, and 4. By stereographic plotting of metallographic measurements, the strain markings within a deformation band in a single crystal of aluminum deformed by compression were found to be traces of (111) planes within a maximum scatter of 6". The edges of the deformation band were found to be traces of the (100) planes also within the maximum scatter of 6" (in agreement with previous workers). At 30 pct deformation, this scatter was considered quite normal because of the fragmentation and rotation of the crystal. This solution, based on the traces on one plane of observation is not unique, but as the planes were observed to be those normally and logically to be expected, further work in this regard was not felt to be necessary. The study of strain markings in a wedge-shaped specimen, rolled to obtain a gradient of deformation from 0 to 50 pct, revealed prominent strain markings at 25 pct reduction in thickness (fig.5). Faint and weak strain markings were visually observable up to a minimum reduction in thickness of about 12 pct. Since strain markings have been observed in other face-centered cubic metals after much smaller deformations;1, 2 and since the rate of recovery in aluminum is high, it is believed that, at lower deformations, self-recovery removes the localized strains at the slip interfaces, thus removing the source of the etching effects that give rise to strain markings. At high magnifications, strain markings sometimes seem to appear as very thin, light-banded re-gions bounded by a pair of dark edges. This so-

Jan 1, 1951

By F. N. Rhines, B. H. Alexander

MUCH attention has been directed to the effects of grain size upon the properties of alloys, but there has been scant study either of the conditions that determine the pattern and dimensions of den-drites in metal systems, or of the influence of their shape and size upon the overall properties of cast-ings. The aim of the research that is about to be described has been to investigate the effect of vari-ous factors upon the mode of formation of dendrites in alloys by measurements of the distance between adjacent dendrite arms (dendrite spacing). Early investigators, including Grignonl and Tschernoff,2 showed that a metal dendrite is com-posed of a tree-like system of stalks and branches arranged in a simple geometrical pattern. North-cott and Thomas3 demonstrated that, in the face-centered cubic solid solutions of copper-base, these stalks and side arms all lie in (100) directions in the crystal. Several investigators, including Sauveur and Chou,0 Sauveur and Reed,' and Martin and Mar-tina have reported that the addition to steel of alloy-ing elements, such as nickel, chromium, and molybdenum, not only makes the dendrites easier to reveal by etching, but makes them coarser. The latter authors8 proposed that the coarsening of the dendrites is roughly proportional to the increase in the temperature range of freezing, caused by adding the alloying elements. Sauveur and Chou6 showed, in addition, that the dendrites are coarsened by a decreased rate of cooling of the casting. Measurement of Dendrite Arm Spacing Among the physical conditions that could be ex-pected to have an influence upon the dendrite arm spacing, that appears in a cast metal, are: composi-tion, rate of freezing, crystal structure, and type of constitution. The relationships obtaining between these variables and the dendrite dimensions have been examined, in the present research, by measur- ing the arm spacing in a wide variety of alloys, listed in tables II through VI. Alloy compositions are recorded in the tables by showing the symbol of the major metal followed by the percentage and symbol of the alloying agent; thus, "Al-10Ag" is an aluminum-base alloy containing 10 pct of silver. Although none of the alloys were analyzed, an im-pression of their degree of purity may be obtained from that of their component metals given in table I. Five hundred grams of each alloy was made by melting in small clay-graphite crucibles in an elec-tric muffle furnace. After alloying the temperature was adjusted to 50" to 75°C above the liquidus and the melts were poured into cast iron molds, at room temperature, the molds having a wall thickness of 1 in. and a cavity 11/2 in. sq in cross-section. Each ingot, thus cast, was sectioned at mid-height and the sectioned surface was polished and etched for metallographic examination. Dendrite spacing meas-urements were made at three positions, namely, ad-jacent to the mold wall, midway between the wall and the center of the ingot, and at the center (desig-nated e, m, and c respectively, in the tables). A typical series of microstructures is presented in fig. 1. For each measurement, the average was taken of the dendrite spacing of several grains covering a zone about 2 mm wide. Only those grains which had a major dendrite axis nearly in the plane of polish were selected in order to eliminate corrections for orientation differences from grain to grain. Although the dendrite spacings were measured to the nearest thousandth of a millimeter, the values listed in the tables are thought to be significant only to the nearest hundredth of a millimeter. The larg-est difference in readings found, when various ob-servers rated the same specimens, was 0.012 mm; the largest difference between corresponding meas-urements upon duplicate specimens was 0.027 mm.

Jan 1, 1951