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By Richard Paul Seelig

THE following review covers published information on pressing of metal powders at room temperature. Only those operations are considered which occur between the time the powder is filled into the cavity and the compact is ejected from the die. Thus, this review does not concern hot pressing, coining or sizing feed or flow problems, commercial presses nor designs. It was also necessary to disregard to a large extent the effect of pressing on subsequent operations and on properties after sintering. The pressing operation is considered independently in its function to compact loose metal powder into useful shapes which can subsequently be handled. There are some comments by the writer in connection with a few of the findings quoted in the literature in order to stimulate thought and discussion. The selection of references quoted in the text is in some cases arbitrary although an attempt was made to favor papers containing novel ideas, techniques or results which may stimulate future research. In order to enable the reader to check further into the subjects mentioned, the original, rather extensive, bibliography is appended even though not all the references are touched on in the printed version of this review. EXPERIMENTAL APPROACH The equipment used by various workers, for example a die design created by Bridgman,22 is very interesting. The die insert has a conical external surface. The vertical pressure exerted on the punch transmits itself to the die which in turn is pushed harder into its tapered retainer. Thus, the higher the pressure exerted on the punch, the higher also the pressure exerted inwards on the die inserts. In as much as this pressure counteracts the internal pressure from the compact the two stresses balance each other so that it is possible to obtain tremendous pressures without breaking the die. The die collar was made from an oil hardening tool steel, heat treated to a tensile strength of some 300,000 psi. The die was closed at the bottom by a plug made from special tool steels. Bridgman found that there is no steel which will withstand a compressive stress of 700,000 psi without continuous slow flow or immediate fracture. Therefore, the only material suitable for use in the pressing punch was sintered carbide. In view of the ingenious design it was possible to use special tool steel as die material. Jones22 raises the question whether this method of pressing has practical application in powder metallurgy. Al- though these tremendous pressures cannot readily be utilized without many special precautions, the tapered die and retainer idea is believed to be useful even for lower pressures. Bridgman, himself,8 calls attention to the fact that the properties

Jan 1, 1947

By N. J. Grant, B. C. Giessen, U. Wolff

With the aid of the splat-cooling technique of rapid quenching, metastable alloy phases based on antimony ad bismuth have been prepared. At room temperature, simple cubic phases were found in the Sb + Au, 56 + Yd, and Sb + Ni systems. Another phase was retained in the Au-Bi system at -190°C; in this systent, a microcrystalline phase and a rhombohedrally distorted phase were also observed. The crystal chemistry of these phases is discussed in terms of their valence electron concentration range. A remarkable five-step Phase sequence was found upon heating and equilibration of certain metastable Au-Bi alloys. USING the splat- cooling technique of rapid quenching from the liquid,' a large number of metastable intermediate alloy phases have been prepared in recent years. Thus, Hume-Rothery phases of the hexagonal type based on the valence electron concentration have been produced in systems where they are missing in equilibrium, e.g., Ag-Ge 1 or AU-Sb. 3 In a comprehensive study of metastable alloys based on tin, simple hexagonal metastable y phases were found, raising the total of stable and metastable y phases from 3 to 13. 4 In the In-Bi system, five new metastable intermediate phases were retained.' In most cases, the new metastable phases have some crystal chemical characteristics in common: a) They have rather simple, elementlike structures with few atoms per unit cell, e.g., y phase,4'5 or the metastable primitive cubic phases in the Ag-Te and and Au-Te systems.= b) Their structures are often related to those of the terminal phases, or to elements that are straddled in their position in the periodic table by the constituent elements; this is the case for metastable ß (In-Bi) with the structure of white ß Sn,' or metastable a (Cd-sn). 4 c) They seem to represent the crystal structures appropriate to certain average group number (AGN) ranges in which no or few single-phase structures exist in equilibrium. These average group number ranges can probably be equated in the case of many elements of the Ba(Zn)-Bs(As) groups with the averaged valence electron concentration. In the present work, the splat-cooling technique has been applied to the alloys of antimony and bismuth. In equilibrium, neither element forms intermediate alloy phases with other B elements from groups Bl(Cu) to B4(Si) that contain more than 66.7 at. pct of Sb or Bi, respectively, e.g., AUSb 2. 7 Thus, antimony- or bismuth-rich phases, which might be closely related to antimony or bismuth, and which would reflect struc- tural changes occurring on alloying with small amounts of addition elements, do not exist. Also, the terminal solubility of antimony and bismuth for all B metals is very small. It was therefore of interest to investigate the influence of enforced, nonequilibrium solid solution of addition elements in antimony and bismuth on their crystal structures. It was found that additions of group B 2-B4 metals act distinctly differently than additions of group T 10 and B1 metals. The latter set of additives will be treated here. EXPERIMENTAL TECHNIQUES Alloy preparation and splat-quenching followed closely the procedures described in Refs. 1, 4, and 5; they consisted of the preparation of master alloys from high-purity starting materials (99.99+ pct) and blast-atomizing of 20-mg quantities onto copper sheets. The resulting approximately 1 to 5 u thick foils were investigated by X-ray diffraction. The cooling rates obtained are of the order of 107 to 10 8 C per set,'" causing solidification to proceed at a rat; of approximately 100 cm per sec.' Powder patterns of the resulting fine-crystalline materials were taken with filtered CuK, radiation. For antimony alloys the substrates were held at room temperature and for bismuth alloys at -190°C both during splat foil deposition and X-ray investigation. Annealing treatments at several

Jan 1, 1969

By R. M. Goldhoff, J. W. Spretnak

IN connection with establishing the mechanism by which boron enhances the hardenability of heat treatable steels, this research work has been undertaken. Spretnak and Speiser1,2 indicated the need for studying high temperature effects in boron steels and, chief among these, the possible nonhomogeneous distribution of boron in iron grains. The occurrence of this effect may be of significance in explaining the mechanism of enhancement of hardenability by boron as well as in explaining some of the observed characteristics of boron steel behavior. Primarily, then, this work was undertaken a) to establish whether or not boron is adsorbed in ? solid solutions, b) to determine the nature of any such adsorption effects, i.e., whether it is positive or negative as well as its temperature coefficient, and c) to establish the magnitude of any such effect. While past literature on this specific subject is rather sparse, a number of authors have postulated that the observed temporary loss of hardenability as well as the occurrence of the characteristic boron constituent in these steels is due to the nonuniform distribution of boron in austenite.3-0 Experimental Techniques Attempts to obtain direct evidence of grain boundary effects in boron steels have been unsuccessful, both by using the technique of Chalmers' in which small concentrations of solute made radioactive by irradiation are detected by autoradiographic means, and by means of studying cleavage fractures with the electron microscope.8 The present study attempts the design of experiments to measure the effect of boron on properties which might be subject to variation because of grain boundary effects. A study of the theoretical aspects of grain growth indicates that such studies may be pertinent. Another valid type of experiment involves the measurement in polycrystalline materials of properties whose values depend on the bulk of the grain, being negligibly influenced by grain boundaries. One such property is the lattice parameter measured by X-ray diffraction. The value of the lattice parameter reflects the average conditions which obtain over a relatively large number of atoms in a fixed crystalline lattice, and is therefore mainly dependent on bulk grain material. Measurement of lattice parameter variation over the austenite range of temperature in iron with and without boron should give evidence of concentration variations in the bulk grain material if adsorption effects are significant. Finally, use is made of the Grange and Garvey3 metallographic test for boron in which a characteristic boron constituent can be developed in austenite grain boundaries. The very occurrence of this phenomenon suggests grain boundary enrichment of boron and a study of the occurrence of this constituent and its varation with austenitizing temperature should help to detect grain boundary effects. Materials One lb ingots of pure iron, an Fe-B alloy, an Fe-C alloy, and an Fe-C-B alloy were prepared. The melting technique included an initial melting of electrolytic iron under vacuum followed by remelting under hydrogen and, finally, by melting under argon with the addition of alloying elements. Each ingot was surface machined between meltings. A quantitative spectrographic analysis was obtained on the pure ingot and, in addition, oxygen, nitrogen, and carbon were determined by the vacuum fusion method. The results of these analyses are given in Table I. Semiquantitative spectrographic analyses were performed on the alloy ingots, while quantitative determinations of the alloy additions were obtained. These analyses are shown in Table 11. The cast ingots were subjected to the following sequence of fabrication treatments: forging to 5/8 in. bars, swaging to 0.300 in. rounds, drawing to 0.025 and 0.010 in. wire. Portions of each ingot were retained in the swaged condition for experimental use. For certain portions of the work typical commercial steels were used. These materials were supplied by the Republic Steel Corp., Canton, Ohio, and correspond to AISI 8640 and AISI 86B40 compositions.

Jan 1, 1958

By M. R. J. Wyllie, Michael A. Torcaso

With the continued deep drilling of today, increasing numbers of high pressure and high temperature gas-condensate reservoirs are being discovered. Correspondingly, the ranges of properties of gas-condensate reservoir fluids are also being increased. The literature1*'." contains several excellent reviews of the property ranges in presently known condensate reservoirs. When one examines these property ranges, it becomes apparent that the need for reliable data is great if the engineer is to evaluate properly or appraise a gas-condensate reservoir. It is the purpose of this paper to present phase-behavior data that will point out some of the important variables that influence recovery from gas-condensate reservoirs produced by pressure depletion. All these variables may be resolved into two major categories: the hydroc:arbon composition of the reservoir fluid and the physical properties of the reservoir. But the variables which we will consider are those which are usually determined from well tests shortly after discovery and are, consequently, readily available to the engineer. They are as follows: (1) the producing separator gas-stock-tank liquid ratio, (2) stock-tank liquid gravity, and (3) reservoir temperature. Laboratory depletion studies have been performed on several reservoir fluids to illustrate the effect of changes in the cronsidered variables upon ultimate recoveries. The deviation factors, Z, of a series of reservoir fluids were determined experimentally to illustrate their order of magnitude and their effect upon the calculation of in-place reserves existing at high pressurcs and temperatures. The procedures followed in conjunction with the performance of these studies and their associated calculations are illustrated in Fig. 1. For the purpose of this paper, the depletion recoveries are expressed only in terms of pcr cent of initial stock-tank liquid, with the abandonment pressure assumed to be 500 psig. VARIATION OF RECOVERY WITH INITIAL PRODUCING SEPARATOR GAS-STOCK-TANK LIQUID RATIO The producing separator gas-stock-tank liquid ratio has long been one of the principal criteria in assumptions and generalized correlations' used for the estimation of ultimate recovery from gas-condensate reservoirs. Fig. 2 presents a plot of the cumulative recovery of stock-tank liquid at abandonment as a function of the initial producing separator gas-stock-tank liquid ratio. The graphical illustration represents the results of 44 laboratory depletion studies performed on actual gas-condensate fluids. These data are presented not only to illustrate the general trend of ultimate recovery increase with initial producing ratio increase but to emphasize the considerable variation in possible recovery at any given producing ratio. Table 1 presents the properties of two actual reservoir fluids chosen to illustrate the approximate extremities of producing ratios for gas-condensate systems. The fluids designated as A and B exhibited initial producing ratios of 3,400 and 114,000 scf/bbl, respectively. Fig. 3 presents a graphical comparison of the cumulative stock-tank liquid recoveries, calculated from the well-stream compositions and produced volumes for each fluid during depletion. It is to be noted that Fluid A exhibited a recovery of only 16.5 per cent when produced to an assumed abandonment pressure of 500 psig while the corresponding recovery for Fluid B was calculated to be 62.2 per cent. This difference in recovery, which exemplifies the general trend of recovery increase with initial producing ratio increase, is readily explained by consid-

By F. Clerf

Blast-furnace practice in France is determined more or less by the character of the ores used. Some French ores are siliceous and others are calcareous, therefore by proper burdening a self-fluxing mix can be used. This is not always done, as, for instance, at the Caen furnaces of the Société Métallurgique de Normandie, where the Soumont ore of Normandy is used, which is a carbonate. This ore is crushed and calcined at the mines, yielding a product that is porous and well sized for blast-furnace consumption. The lines of the Caen furnaces are given in Fig. 1. Originally these furnaces had 16 tuyeres; six are plucked and these tuyeres are set in the lower part of the bosh. Operating data on these furnaces are given in Table 1. Table 1.—Operating Data, Caen Furnaces Kg. Lb. Blast-furnace burden per ton of iron: Soumont ore....................................... 200&2100 (44004650) Limestone...................................... 900-1000 (2000-2200) Basic Bessemer slag (bearing phosphorus).............. 100 (220) Scale.............................................. 35 (77) Manganese ores.................................... Coke.............................................. 1100-1200 (2420-2640) Coke analysis: Ash, per cent............. 9.5 H2O, per cent............. 4.0-10.0 Flue dust (approx.), kg. per metric ton.... 200 (440 lb.) Blast volume, cu. m. per hr.............. 83,000 (49,000 cu. ft. per min.) Preesure, lb............................ 12 Blast heat, deg. C....................... 650 (1200" F.) Top temperature, deg. C................ 250 (445O F.) Top-gas analysis, per cent............... CO2 9.3 CO 30.3 O2 0.3 H2 3.0 Production per 24 hr. about 510 tons. MINETTE ORES The most important ore deposits in France are in the west of Lorraine. They are called the "minette" ores and are of two classes-—siliceous and

Jan 1, 1937

By Michael Tenenbaum

The importance of semikilled steel as a high tonnage grade has long been recognized. The increasing severity of the applications for which semikilled steel is used makes it desirable to obtain further information regarding the features of open hearth practice and ingot structure that can affect steel performance in subsequent rolling and fabricating operations. Accordingly, an investigation is being carried out studying the structure of various types of semikilled steel ingots. This paper reviews some of the observations made and information gathered in this investigation. By definition, semikilled steel may be considered to include all nonrimming steels in which the natural shrinkage occurring during ingot solidification is offset to an appreciable degree by gas formation. Accordingly, this type of steel includes the entire range intermediate between rimmed and fully killed steel. The resultant ingot structures range from those of steels that have been capped to suppress a weak rimming action to those steels that have been killed in the furnace or ladle to the extent that no mold deoxidizer is required. A survey reported to the 1946 -AIME Open Hearth Conference' reviewed the practices being used at 28 major plants for the deoxidation of semikilled steel. It was found that most plants divide the deoxidizing additions between the ladle and the mold—many of the plants adding only minor amounts of deoxidizer to the bath or none at all. Silicon, aluminum and titanium were the only elements used for ladle and mold deoxidation. Mold deoxidizers were added as capping additions or as uniformly fed additions. Several practices were reported in which the steel was deoxidized in the ladle to the extent that little or no mold deoxidation was needed. No reference was made to grades capped by using special mold designs or special closures over the top of molds. .Accordingly, specific examples of this type of practice will not be considered in this paper. It appeared from this survey of deoxidation practice that semikilled steel can be divided into three types, namely, capped semikilled, in which aluminum is added near the end of pour or after shut-off, intermediate semikilled steels, in which aluminum is fed uniformly throughout the pour, and semikilled steels requiring no mold deoxidation. In an attempt to cover the ingot structures obtained by the range of practices reported in the preceding survey, three series of experimental heats were made using increasing amounts of aluminum, silicon and titanium for ladle deoxidizers. The ladle deoxidizers were added as stick aluminum, 50 pct ferrosilicon and 20 pct ferrotitanium (4 pct carbon), respectively. Two methods of studying ingot structures were used. Ingots were removed from production, burned longitudinally and machined to allow observation of the central pipe and coarse blowholes. During the machining operation much of the finely porous subsurface structure was obliterated. Accordingly, observations were also made

Jan 1, 1949

By Michael Tenenbaum

The importance of semikilled steel as a high tonnage grade has long been recognized. The increasing severity of the applications for which semikilled steel is used makes it desirable to obtain further information regarding the features of open hearth practice and ingot structure that can affect steel performance in subsequent rolling and fabricating operations. Accordingly, an investigation is being carried out studying the structure of various types of semikilled steel ingots. This paper reviews some of the observations made and information gathered in this investigation. By definition, semikilled steel may be considered to include all nonrimming steels in which the natural shrinkage occurring during ingot solidification is offset to an appreciable degree by gas formation. Accordingly, this type of steel includes the entire range intermediate between rimmed and fully killed steel. The resultant ingot structures range from those of steels that have been capped to suppress a weak rimming action to those steels that have been killed in the furnace or ladle to the extent that no mold deoxidizer is required. A survey reported to the 1946 -AIME Open Hearth Conference' reviewed the practices being used at 28 major plants for the deoxidation of semikilled steel. It was found that most plants divide the deoxidizing additions between the ladle and the mold—many of the plants adding only minor amounts of deoxidizer to the bath or none at all. Silicon, aluminum and titanium were the only elements used for ladle and mold deoxidation. Mold deoxidizers were added as capping additions or as uniformly fed additions. Several practices were reported in which the steel was deoxidized in the ladle to the extent that little or no mold deoxidation was needed. No reference was made to grades capped by using special mold designs or special closures over the top of molds. .Accordingly, specific examples of this type of practice will not be considered in this paper. It appeared from this survey of deoxidation practice that semikilled steel can be divided into three types, namely, capped semikilled, in which aluminum is added near the end of pour or after shut-off, intermediate semikilled steels, in which aluminum is fed uniformly throughout the pour, and semikilled steels requiring no mold deoxidation. In an attempt to cover the ingot structures obtained by the range of practices reported in the preceding survey, three series of experimental heats were made using increasing amounts of aluminum, silicon and titanium for ladle deoxidizers. The ladle deoxidizers were added as stick aluminum, 50 pct ferrosilicon and 20 pct ferrotitanium (4 pct carbon), respectively. Two methods of studying ingot structures were used. Ingots were removed from production, burned longitudinally and machined to allow observation of the central pipe and coarse blowholes. During the machining operation much of the finely porous subsurface structure was obliterated. Accordingly, observations were also made

Jan 1, 1949

By Nathan C. Rockwood

LIME is a very general term applied to products of limestone, in popular treatises often incorrectly, including ground or pulverized limestone used in agriculture. When used without qualifying adjective, the term usually means burned or calcined limestone, or quicklime, or calcia. The corresponding calcined product of magnesite is magnesia. If the calcined rock is relatively pure calcium carbonate, the resulting lime is a "high-calcium" lime; if the rock is dolomite, or a combination of calcium and magnesium carbonates, the lime is a "dolomitic" or a "high- magnesium" lime. There are various grades in between, depending on the percentage of magnesium carbonate and other ingredients in the raw rock. For some industrial purposes only high-calcium limes are suitable; in other processing-as, for example, neutralizing acid wastes -the relative percentages of magnesium and calcium carbonates in the raw material are not important. Limestone is burned (roasted or calcined) in furnaces known as lime kilns by direct exposure to the hot gases and flames. When heated to incandescence, the carbon dioxide content of the rock is expelled, leaving calcium and magnesium oxides, according to the formula usually written: [ ] This thermal reaction is reversible, which requires that the lime be withdrawn from the "calcining zone" of the kiln about as fast as made. Pure calcium carbonate would lose 44 pct of its weight in the calcining process; dolomite, 48 pct. Generally, the lime will retain the approximate size and shape of the piece of rock from which it is made but some few limestones tend to break down into granules or dust. Hence lime (quicklime) comes from the kilns in lumps or granules and normally is packed in water- tight containers in these forms, or is pulverized after calcination.

Jan 1, 1949

By Joseph S. Malesky

The discovery and development of explosives mark one of the most important findings in the history of civilization. Without explosives our vast economic enterprise concerning the mining of coal, copper, iron, aluminum, and various other ores could not function. Explosives are used in all kinds of construction works, in the razing of old buildings, blasting of trenches, driving of tunnels, and in many other instances common to our everyday life. For these reasons explosives are rightfully referred to as the forerunner of progress. An explosive may be defined as a substance (usually a mixture) that, when flame or shock is applied, yields readily to rapid combustion or oxidation, accompanied by the formation of such relatively large quantities of gases as to produce much violence and pressure which, in turn, react against their surroundings and cause what is termed an explosion. By their very nature the action of explosives is destructive and disruptive of adjacent materials. Decomposition of explosives can occur through deflagration, which is rapid burning or combustion, as in the case of black powder, or through detonation, which is an almost instantaneous disruption, as in the case of dynamites and blasting agents. HISTORY OF BLASTING WITH EXPLOSIVES At one time workmen obtained stone blocks for building by grooving the rock with crude picks, driving wooden wedges into niches in the rock, and pouring water on the wedges; the swelling of the wood forced out the blocks. As late as the 17th century, fires were placed against the face of rock to crack it, and water was sometimes dashed on the heated rock to shatter it by sudden cooling. The progress of our country is synonymous with advancement of the improved manufacture and extended use of explosives. Coal had been

Jan 1, 1981

By Charles T. Holland

This discussion is concerned with those comparatively infrequent bumps that eject material from the failed mass with enough energy to wreck heavy machinery and seriously injure or kill people. In such cases there is a loud report, and the pressure waves set up in the mine atmosphere wreck ventilation controls several hundred feet from the site of the failure. Vibrations are induced in the earth's crust which may be detected several miles from the point of origin, and explosive gases may be released in large quantities.* Usually a dense suspension of dust is produced from the failed mass, together with dust placed in suspension by the resulting air blast. These rock bursts or bumps have also been called mountain shots, bounces, pillar bursts, and crumps. Such occurrences, when extensive, are serious catastrophes, and may force abandonment of the mine.1

Jan 9, 1958

By Roy C. Kirkman

Dear Editor: It is with great pleasure that I read Mr. Howard M. Wells article in the December 1978 issue of MINING ENGINEERING entitled: "Optimization of Mining Engineering Design in Mineral Valuation." Mr. Wells very adequately presents the case and point that there are a great number of variables which must be analyzed during an economic evaluation of an FUND RESOURCE, such as copper or uranium. I wish to take this opportunity to suggest that, given today's economic climate, decision making takes place under conditions of uncertainty and that this uncertainty justifies our need to examine each one of the parameters entered into the evaluation model. It is my contention that the influence of the tonnages and grades as well as their distributions, have the most profound effect upon the results of an evaluation. Everyone concerned with the evaluation of FUND RESOURCES realizes that as metal prices decline or stagnate with sharply rising direct operating costs, cutoff grades (Gc) must increase according to the equation below which Mr. Wells uses: Gc = Total Operating Cost/(Market Price X 20 X Recovery) However, historically, we have seen cutoffs move dramatically lower in both the copper and uranium industries for the past decade. Henceforth, this established the metals industry most important argument for processing greater tonnages of lower grade materials from disseminated deposits (refer to paper by Kirkman, Roy C.). These disseminated deposits, created by either concentration processes (uranium) or dispersion processes (copper, gold, molybdenum), have log-normal grade distributions (Fig 1). Gross profits are rising, but unit profits are falling. The industry has created longevity through economy of scale, i.e., mining vast tonnages of low grade. In order to develop the great tonnages necessary to prove economic viability, we must examine alternatives at the low-end of the tonnage grade relationship. Notice from [Fig. 2] that as we move further to the right away from line A-B drawn tangential to the average grade curve at 45°, total profits will increase (given fixed annual production capacity) and unit profits decrease. The theoretical optimum operating point is where: [ ] At this point my observation is that slight shifts in production capacity bring about greater changes in profitability due to greater grade changes. Therefore, the best financial risk evaluation is obtained by totally revising the mining engineers methods and fixing the financial parameters such as discount and interest rates. A 10% shift in either of these two parameters will not cause near the same variance in economic viability as will a change on the GRADE-TONNAGE curve [(Fig. 2)].

Jan 1, 1980

By William M. Huang, T. Carl Shelton

There are undoubtedly many factors that affect the emission of gas from coal but the permeability of coal to gas flow would seem to be fundamental. However, there is very little information on coal permeability to gas flow available in the U.S. at the present time, despite the fact that such knowledge would appear to be significant in any degasification effort. Studies made recently in the mining engineering laboratories at Virginia Polytechnic Institute have determined values of permeability on one-inch cubes of selected coals. COAL PERMEABILITY The permeability values given in this paper are based on adaptations of Darcy's Law formulated by Henry Darcy in 1856 from experiments with fluid flow in porous media.' Using air as the gaseous fiuid, they were obtained by employing similar methods as are used to determine the permeability of petroleum and gas reservoir rock specimens.

Jan 5, 1962

By F. B. Plummer

PETROLEUM ENGINEERING deals with the production, transportation, and refining of crude oil. Refining is chiefly the work of the chemical engineer; production, that of the petroleum engineer. Production engineering only is discussed in this paper. Petroleum production engineering is closest related to and, in fact, is a branch of mining engineering. Formerly, many petroleum engineers were trained as mining engineers or mining geologists. The profession is related also to mechanical and civil engineering to about the same extent that mining engineering is. Petroleum production draws upon the mechanical branch for drilling and pumping machinery and upon civil engineering for the construction of transportation lines, water supplies, and water-disposal plants. Fundamentally, petroleum production engineering deals with the removal of the oil from the reservoir rocks, just as mining is concerned with the removal of ore. The process of oil production demands a specialized knowledge just as distinct from mechanical and civil engineering as mining is distinct from operating a Diesel engine. Even though the chief tools of the petroleum engineer are the drill and the pump, these may be of little avail, and certainly not efficient, if their selection and use is not based on a knowledge of the physical chemistry of oil, the geology of the formations, the structure of the oil sand, the hydrodynamics of the reservoir, and the interrelation of all these many factors.

Jan 1, 1936

By Robert S. Shoemaker

Receiving the Richards Award is undoubtedly the most memorable event in my entire life. There should, however, be more names engraved on it. These are the names of men who were my teachers (but not all of the academic variety) and my friends, each of whom had a part in my ever continuing education and thus have a part of this award. There was Bill Caldwell who made me into a chemist, and Will Shorey who added a lot of ore dressing. There was Rush Spedden who put me to work in his minerals research lab, Joe Brennan who made me turn my research into plant practice, and Tom Meek who sent me all over the world on metallurgical jobs. Bob Cheatham and Abe Dor taught me to try to give the client what he needs rather than what he wants, while Ed Malouf and Casey Davis always gave their particular brand of advice at exactly the right time. And, lastly, there was Leo Abell and Frank McQuiston, both fine metallurgists and the best friends a man could have. In addition to those I have mentioned, there are literally scores of others I would like to acknowledge with my sincere appreciation.

Jan 6, 1974

By Bernard G. Carbajal

The dielectric properties and thermal stability of glow-discharge polytnerized films of styrene, chloro-benzene, and other organics and photoresist filrns are presented. Variations in the glow-discharge polymerization procedure are related to thermal stability. Thermal treatwzents to improve the dielectric properties of both positive (A2 340) and negative (KMER) photoresists are given. THIS study of the dielectric properties of thin organic polymer films is part of a program to investigate the electronic applications of organic materials. Thin organic polymer films have been produced in an ac glow discharge,13 with a low-energy electron-beam process,4 and in an rf dicharge. A process has been developed during the course of this program for forming thin organic polymer films in a dc glow discharge. These glow-discharge polymerized (GDP) films exhibit some useful dielectric and insulative properties. Variations in the properties of the GDP films can be induced by changes in the source material (monomer) andor in the conditions of the glow discharge. Thin organic polymer films can also be produced from typical positive and negative photoresists. Some variations in the properties of the photoresist films can be induced by suitable post-application treatments such as thermal crosslinking. The properties of interest in this study are dielectric constant, dielectric strength, resistivity, and thermal stability. POLYMER FILM PREPARATION I) GDP Films. The GDP films were prepared in a dc glow discharge in an atmosphere of organic monomer vapor. The details of the glow-discharge procedure have been presented previously.6 Briefly, under the influence of a dc glow discharge organic vapors can be polymerized in the vapor phase and the resultant polymer (GDP film) deposits on and in the vicinity of the cathode. Substrates placed behind a screen cathode can be uniformly coated over all exposed areas. Pattern definition can be achieved using normal mask stencil techniques. Table I presents the pertinent parameters in the preparation of GDP styrene. Conditions of Forrrzation of GDP Styrene. The rate of deposition for GDP films was monitored using a current-time integrator. The thickness of the deposited film for a given set of experimental conditions was a function of the current-time integral. The fifth row in Table I is a compilation of the deposition rate of GDP styrene films. Other organic monomers behave in a similar fashion. With the exception of the highly halogenated saturated hydrocarbons, all organics subjected to the conditions of the glow discharge form GDP films. 11) Photoresist Films. Photoresists are normally recognized to exist in two forms, a low molecular weight, soluble polymer form (A) and a high molecular weight, crosslinked insoluble form (B). Typical negative photoresists are applied in the low molecular weight form A and converted to the high molecular weight form B by the action of light. (Positive photoresists are applied in form B and converted to form A by the action of light.) Eastman Kodak Metal Etch Resist (KMER) has been chosen as a typical negative photoresist. Polymer film samples were prepared in the same configuration used for GDP films. The KMER was applied in the usual fashion using a 120°C drying step (infrared-lamp heating) and a 180°C post-bake. Care must be taken to completely remove the solvent in the drying step and to properly develop and postbake to exposed photoresist. If the photoresist film is not properly dried and postbaked, severe blistering and peeling will occur during subsequent elevated-temperature exposure. Thickness can be controlled by varying the viscosity of the form A photoresist and the spin rate at application. AZ 340 was chosen as a typical positive photore-

Jan 1, 1967

By D. Weinstein, F. C. Holtz

AS a possible method of improving the elevated temperature strength properties of zirconium, an investigation was initiated on the feasibility of producing a dispersion-strengthened material. Because of the high reactivity of zirconium, its high solubility for oxygen, and the stability of the Zr-0 solid solution, the major problem in such a development is choice of a suitable dispersant. Thus, in the present investigation we were concerned primarily with the stability of various dispersants in the zirconium matrix. The experimental procedure consisted of blending powders of zirconium and a dispersant, followed by cold compaction and extrusion. The best available source of -325 mesh zirconium powder contained between 1500 and 3500 ppm Oz; to this material, powders of zirconium carbide (5 p max), vanadium carbide (5 p max), alumina (0.03 p average), lan-thana (0.8 to 2 p), ceria (0.8 to 2 p), yttria (0.8 to 2 p), calcia (44 p rnax), or thoria (0.6 to 0.8 p) were added in amounts of 7 vol pct and compacted at 65 tsi. A cylindrical compact having a density between 70 and 80 pct of theoretical and dimensions of 1 in. diam by 1-114 in. high was thus produced. After canning in copper, these billets could be extruded (5: 1) on a 54-ton capacity, slow-traverse hydraulic press with the billet temperature at 1550°F and the extrusion die at 900°F. However, lack of densifica-tion of some of the extruded billets necessitated ratios of at least 23 :1. Ultimately, all billets were successfully extruded at 1500°F to 0.190 in. diam (32 :I), fully dense rods using a 200-ton capacity press and a ram speed of 90 ipm. The microstructures of as-extruded Zr-7 vol pct LazOS and Zr-7 vol pct Y2Os are shown in Fig. l(a) and (c), respectively. These structures are similar to all the as-extruded materials and consist of an elongated, single-phase zirconium matrix dispersed with oxide or carbide particles. Very little porosity is observed, and the interface between matrix and particles appears satisfactory. The size and distribution of particles, however, are not ideally of the type desired for dispersion strengthening. Since the primary study was of particle stability with respect to zirconium, no attempt was made to overcome agglomeration during powder blending and fabrication. Some areas exhibit fine, well-distributed particles; undoubtedly, a small proportion is submicroscopic and has the

Jan 1, 1963

By F. L. Ruhlman, Max C. Eastman

The termination of the recent war marked a major changc in the oil-field operations at. Elk Hills. Production was greatly curtailed, various experimental production projects were started, and a long-range exploratory program was inaugurated. Production was reduced from the wartime peak of 65,000 bbl per day to the current rate of about 8ooo bbl per day in order to maintain an available source of crude that can be drawn upon during a national emergency. The existing production rate is deemed essential to carry on the experimental production projects. These projects are being conducted to determine the best methods and means of maintaining the Reserve, shut in, but in a state of readiness to produce the maximum quantity of oil in the most expeditious manner. Projects now being investigated include: (I) protection of surface equipmerit; (2) repair of wells that might damage the reservoir; (3) gas injection; (4) water eneroachment, (5) gravity drainage. An exploratory program is being carried on to determine the amount of recoverable oil in the unexplored portions of the Reserve. The Shallow-zone exploration is practically completed, but owing to the complexity of the Stevens structure and the magnitude of the oil discoveries in the Stevens, exploration will probably continue in that zone for another two years. Introduction Summary of Development History of Elk Hills Although a detailed history of Elk Hills oil field is presented in various publications,1,2 a summary of its unusual development and production history will be given in order that the present problems may be more readily understood. The first development that resulted in commercial production was in the central part of the Reserve. The first well, Hay No. I, in sec 36-R,* was completed in January I9I9, and was soon followed by 37 Others in the same general area. It is commonly referred to as the Hay-Carman area and was shut in in stages from 1925 to 1934 as a result of litigation regarding the title to the land. Not being highly producti,, only about 6½ million barrels of oil with a large volume of gas was produced from the area prior to the shutdown. Shortly after the start of the development of the Hay-Carman area, drilling was started 6 miles east in sec 36-S' Tupman NO. I came in for 5000 bbl per day early in I92o, It was followed by more than 200 others in the next few years, and the field became one of major importance. Produc-

Jan 1, 1949

By J. K. Edgar

For a number of years the production and use of super-purity aluminum (better than 99.99 pct) has been steadily increasing. High-grade lots of. such aluminum show certain outstanding characteristics not found in lower grades containing principally silicon, iron and copper as impurities. One such characteristic is the so-called "self annealing," that is, the re-crystallization of the heavily cold worked metal at room temperature.' Interest therefore is aroused as to the effects of the impurities. It is well known that the amounts of silicon and copper which occur in aluminum of better than 99.95 pct are completely soluble, at least at elevated temperatures (above 200°C). Iron, on the other hand, is known to be fairly insoluble in solid aluminum. Thus, a knowledge of the limits of this solubility would he of considerable use in studying the characteristics of the high purity metal. All investigators have agreed that iron has very low solubility in solid aluminum. Rosenhain, Archbutt and Hanson2 reported traces of an aluminum-iron phase in the "purest samples of aluminum obtainable." Gwyer and Phillips3 reported that an iron constituent was visible under the microscope in metal containing ".0088 per cent iron." Roth4 found that in the solid state the solubility of iron in high purity aluminum was 0.01, 0.01, 0.017 and 0.022 pct at 225, 320, 500 and 600°C respectively. Dix5 working with alloys containing less than 0.03 pct impurities, concluded from microscopic and chemical analyses of eutectic areas that the eutectic composition was close to 1.7 pct iron. Dix placed the eutectic temperature at 65s°C. Archer and Fink,6 using high purity aluminum-iron alloys, found that the hypoeutectic liquidus intersects the eutec-tic horizontal at 1.7 pct. This is in fair agreement with the investigation of the aluminum-iron system by Gwyer and Phillips who placed the eutectic at 1.89 pct iron with a freezing point of 653'C. Preparation and Chemical Analysis oP Alloys Electrolytically refined aluminum (99.991 pct aluminum) and a high purity alumi-num-iron alloy (11.45 Pet iron) were used in the preparation of the alloys for this investigation. To aid in controlling the iron content of the experimental alloys, an alloy of lower iron content was prepared first from these materials. The high purity aluminum was melted and heated to about 700°C in a plumbago crucible coated with alundum cement and the aluminum-iron alloy was then added. The alloy was thoroughly stirred, fluxed and skimmed and then chill-cast into notch bars. The aIlalyses of the three materials are given in Table I. The alloys for the determination of the solid solubility of iron in aluminum were prepared by melting 600 g total of the aluminum plus the required quantity of the aluminum-iron alloy (No. 92531). These

Jan 1, 1949

By K. M. Weigert

The position of the three-phase field between the alpha and the beta phases was established. The exact location differs from previous assumptions. The extremely high strength and hardness values were found near the phase boundaries of the ternary compositions. IN 1929, UenoL investigated vertical sections of the Ag-Cu-Zn diagram at constant silver and zinc values. From the evaluation of cooling curves and microscopic studies, he concluded that there was no evidence of a three-phase field in the solid state between the a and ,8 fields. The failure to find evidence for this field was due to the fact that it exists only in a very narrow range of compositions and requires special methods of heat treatment to establish phase equilibrium. In a later publication on the same subject Keinert2 rearranged Ueno's diagrams to conform with the basic phase rules. The existence of a three-phase field was postulated in the solid state between the a phases and the homogeneous ,9 phase between the Cu-Zn and the Ag-Zn binary border systems. The approximate location was based on a few microscopic observations of the structure and it was pointed out that the exact position could be determined only by a larger number of experiments. In the twenty years following these investigations alloys of Ag-Cu-Zn have become of general interest due to various technical applications, principally for brazing. In the course of an overall investigation of the physical properties of ternary Ag-Cu-Zn alloys the author found extremely high values of hardness and strength in alloys of compositions between the a and the yS fields. The exact location of the intermediate phase fields was established by the evaluation of more than a hundred cooling curves and microscopic mountings. Experimental Procedures Preparation of Test Samples: At the beginning of the investigation samples were chillcast into Vi in. diameter iron molds to determine hardness, strength, and the mechanism of primary crystallization. These

Jan 1, 1955

By William L. Fink, L. A. Willey

Since so many different curves have been published for the solid solubility of zinc in aluminum, it seems desirable to definitely establish the correct curve by two or more independent methods. The curve published in part I1t was based entirely upon X-ray measurements because the other methods employed at that time were not satisfactory. The present paper (the seventeenth of this series on high-purity aluminum alloys) describes the determination of the solid solubility of zinc in aluminum by the measurement of electrical resistivity at temperature and by microscopic examination. Since the publication of our part I in 1932, an investigation of the solubility relations in the aluminum-zinc system has been reported by Schmid and Wassermann2, who obtained their solubility results from lattice-parameter measurements on heat-treated and quenched specimens. The diagram that they published is shown in Fig. 1. In this investigation they also found by X-ray measurements that the parameter of the gamma phase changed continuously with zinc content and at such a rate that it would be identical with that of the beta phase at 60 atomic per cent zinc. It was concluded therefore that the beta and gamma phases, from the point of view of structural relationship, are one single phase. They also suggested a gap of immiscibility between 270" and 350" C. The complete boundary in this region could not be determined satisfactorily by the method employed and therefore was not shown in their diagram. Aluminum-zinc Alloys Materials Used.—Electrolytically refined aluminum3 was used in preparing the alloys for the work reported in this paper. Chemical analysis showed the following impurities: 0.004 to 0.005 per cent silicon, 0.006 to 0.008 per cent iron and 0.005 to 0.006 per cent copper. Also,

Jan 1, 1936