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By Arthur Knapp

NEARLY every technical man is called upon at some time in his life to deliver a paper before a technical audience or to write a technical paper for publication. It is not necessary to be an accomplished public speaker to deliver a technical paper successfully; it is only necessary to bear in mind a few obvious points. Poorly presented papers are nearly always the result of a few errors of deportment, but they are vital and at the same time so obvious that they are often overlooked. Experience is a good teacher but a little study and careful preparation will moderate the suffering of both an amateur speaker and his audience. An author's paper suffers, through poor delivery, in direct proportion to the suffering of his audience. The best test of a paper is to have it read aloud to the author. This will bring out faults not apparent when read silently by the author. Some of the things which will probably need correcting are improper phrasing, noneuphonic sequences, and long or involved sentences. Frequently authors write their papers in short crisp sentences for oral presentation, then rewrite them for publication.

Jan 1, 1942

By H. Foster Bain

AFTER all, mineral sanctions are not a measure of peace, they are a measure of war, and we must regard them as such. We have had two examples now in the world-first, Italy, and secondly, Japan-where we have applied sanctions. When we got ready to apply sanctions to Italy that would hurt, they went to war. In the Far East, when we applied sanctions against Japan, in the latter part of 1941, there was a quick reaction, and the Japanese bombed Pearl Harbor.

Jan 1, 1944

By C. H. Herty

AN earlier paper on absorption of sulfur by the slag in the basic open-hearth furnace included a brief discussion of the absorption of sulfur during the melting period. The data available at that time showed that the amount of sulfur absorbed by the melting scrap was proportional to the sulfur content of the furnace gases, and the following statement was made: "The conclusion may be drawn from these results that if a gas entirely free from sulfur were used during the melting, any iron in direct contact with the gases would be completely, or nearly completely, desulfurized before it reached the bath proper." The experimental work discussed herein deals with absorption of sulfur by the melting scrap when fuels with both high and low-sulfur content were used. Before taking up the experimental work let us consider the process as a whole as to the "flow" of sulfur. The input of sulfur occurs in: 1, the hot metal charged; 2, the scrap; 3, the stone or lime charged; 4, the ores charged; and 5, the gas. Sulfur goes out of the furnace in the steel, the slag and the gas. The distribution of sulfur in the furnace depends on the sulfur concentration in each of these materials and on the equilibrium conditions between them.

Jan 1, 1926

By Paul D. Merica

DURING the Dark Ages, when metallurgy was practiced by the alchemists, any unusual or disturbing variation in metallurgical operations was ascribed to the, presence, in the metals or ores, of an evil spirit, and it was necessary to exorcise and drive it out "by suitable incantations. In this day of science and of engineering, things still incomprehensibly go wrong in the metallurgist's work shop. The metallurgist is even now not unwilling to lay the blame for many such experiences at the door of something which intellectually- much resembles an evil spirit, "gas in the metal." The presence of gases in his metal, he knows, occasions him many very definite troubles which he can clearly distinguish and diagnose-why may it not be also responsible for those which he cannot so well understand?

Jan 1, 1931

By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at '5 to 40 tons per sq' in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at '5 to 40 tons per sq' in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By W. N. Lacey, R. H. Olds, B. H. Sage

The volumetric behavior of five mixtures of black oil and natural gas and of two mixtures of condensate and natural gas from a field in the San Joaquin Valley was experimentally established. This work was carried out at roo°, I9o° and 250°F in the pressure interval between 400 and 5000 psi. The viscosity of the liquid phase of four mixtures of black oil and natural gas was experimentally measured in the above-indicated temperature and pressure intervals. The effect of methane upon the precipitation of bitumen from the black oil was studied at 230°F. Introduction The solution of a number of the economical and technological problems which arise in connection with petroleum production is dependent upon the availability of the necessary quantitative information covering the materials involved. This requires data concerning physical properties of naturally occurring hydrocarbon mixtures at the pressures and temperatures characteristic of underground petroleum reservoirs. The experimental determination of the desired data for each situation encountered is relatively time-consuming. However, it is considered to yield results sufficiently more reliable than those obtained from correlations to justify the effort. For these reasons there was undertaken a laboratory investigation of the viscosity of the liquid phase and the volu- metric and phase behavior of mixtures of oil and gas samples obtained from wells in a field located in the San Joaquin Valley. Terminology The nomenclature of petroleum engineering is not at present entirely standardized. Many commonly used technical terms are not everywhere given the same meanings. For the purposes of this paper the following definitions will be adopted: Black oil refers to the dark-colored, hydrocarbon liquid obtained when the producing horizon of the well lies partly in the condensed hydrocarbon phase of the reservoir. Condensate is the term applied to the relatively volatile, pale yellow or amber-colored hydrocarbon liquid that is often obtained from the surface separator system when the producing horizon of the well lies in the gas cap of the reservoir. The gas obtained from the surface separator system is called natural gas regardless of whether the well is producing black oil or condensate. As might be expected from the multi-component character of naturally occurring hydrocarbon materials, the compositions of black oil, condensate and natural gas are subject to considerable variation depending upon the temperatures and pressures prevailing in the surface separator system as well as upon the overall composition of the material produced from the reservoir. In order to obtain samples capable of reproducing the total hydrocarbon material produced by the well, all oil and gas mixtures used in this investigation were com-

Jan 1, 1949

By R. H. Oliver

The purposes, types, preparation, and testing of flocculants are discussed. A flocculation compendium is included, indicating choice of flocculant for a given set of conditions. An economic evaluation of the process is presented. Solid-liquid separation is a major expense in most mineral processing flowsheets today. Proper use of flocculation can often lower the overall cost of a solid-liquid separation by reducing the size of sedimentation or filtration equipment. PURPOSE OF FLOCCULATION When is use of a flocculant justified in terms of overall process economy? 1) when it results in process improvement, such as producing a clear liquor for electrolysis, precipitation, ion exchange, or solvent extraction; 2) when it results in satisfying requirements of pollution abatement ordinances; 3) when it results in increased recovery of values that would otherwise be lost; or 4) when it results in considerable savings in capital expenditure due to use of smaller equipment. When can the use of a flocculant adversely effect overall process economy? 1) when it results in increased filter cake moisture, 2) when it results in decreased filtration rates, 3) when it results in considerable bulking of sedimentation underflow, 4) when it contaminates either the supernatant or sludge, or 5) when the cost of using the flocculant is greater than the savings due to its use. First step in consideration of flocculants for a given application is establishment of desired goals in terms of increased clarity of effluent, increased recovery of solids, or decreased size of equipment. The most economical solution to a solid-liquid separation problem is that combination of equipment and flocculant costs which meets the established goals at the lowest total annual expenditure. This economic decision can be made only after technical data has been obtained as outlined in next four sections. TYPES OF FLOCCULATION Flocculation is a process wherein individual particles are united into more or less tightly bound agglomerates or flocs, thereby increasing effective particle size of solids suspended in a liquid. Degree of flocculation of a suspension of finely divided solids in a liquid is controlled by a combination of probability of collision between particles and probability of adhesion after the collision has occurred.' Probability of collision can be increased commercially through use of a paddle-type flocculator, combination flocculator, and clarifier or flocculating-type feedwell. Probability of adhesion usually can be increased by addition of a reagent known as a flocculant. Reagents act as flocculants through one or a combination of three possible mechanisms. The first is electrolytic neutralization of inter molecular repulsive force due to Zeta potential. This neutralization enables Van der Waal's cohesive force to hold the particles together after they collide.' The second is the precipitation, within a definite pH range, of voluminous metallic hydroxide flocs which entrap fine particles. This process is known as coagulation.14 Third is the bridging of two or more particles by either natural or synthetic long-chain, high-molecular-weight organic polymers. This bridging is accomplished by adsorption of two particles at different sites on the same molecule or by bonding of two molecules, each adsorbed to a different particle. Considerable effort has been expended in explaining the action of these polyelec-trolytes and detailed accounts are available in the literature. CHOICE OF FLOCCULANTS It is impossible, at the present time, to specify the optimum type or amount of flocculant for a given application from a knowledge of the material to be treated. The standard procedure is to choose reagents or combination of reagents most likely to be effective on the slurry; then test them.' The accompanying Flocculation Compendium (Table I) contains details of all currently available reagents sold as flocculants and it should be used when selecting the group of reagents for tests. This selection can be based on information listed in columns 4 and 5. Column 4 presents industries in which each floc-

Jan 1, 1961

By J. B. Cheatham, C. E. Murphey

Presently, computer control of Borobolic direction cannot be obtained during drilling, and most straight-holc drilling methods attempt to resist hole deviation rather than control direction. Many of the theories advanced as possible explanations of the cause of hole deviation are Summarized berein. A new correlation of physical partables is introduced to indicate bow factors such iis drill collar stiffness clearance and hit weight influence borehole deviation, .A methord is proposed for predicting the rate of change of hole angle when drilling conditions are changed. INTRODUCTION Control of borehole direction during drilling can be difficult and costly. Unintentional crooked holes are often lrilleti in dipping formations and many times directional drilling is required when the surface location is not directly above the target area —- for example, at offshore and mountainous locations. Prilllng progress can be greatly hindered in either air or liquid drilling when it be comes necessary to use low bit weight to prevent excessive hole angle build-up. If hole inclination becomes too great, drill pipe drag becomes excessive and fishing risks are increased, logging is more difficult and problems of differential sticking, key seating and fatigue failures may be encountered. Dog-legs and key seats are more serious problems than steep inclination angles: therefore, reducing rate of direction change is preferred to attempting to maintain absolutely vertical holes. Consequently, a straight inclineti hole is preferable to a nearly vertical crooked hole containing numerous dog-legs. In this paper, theories of the cause of hole deviation and analyses of drill string behavior under down-hole conclitions are summarized. Methods for computing hole deviation are presented und systems for resisting deviation as well as neans for provic!ing control of holt- direction are iliscusseI. A new correlation of physical variables is introduced tu indicate how factors such as drill collar stiffness, clearance and bit weight influence borehole deviation. A method is oroposeti for predicting the rate of change of hole anFrle when drilling conditions are clianged. IIEVIEU' OF PREVIOUS WORK ON HOIaE DEVIATION Significant progress in the theoretical analysis of hole deviation problems has been made in the past 1 5 years. The pioneering work has been primarily a result of the efforts of Lubinski and Woods.l-5 In 1950, Lubinski 1 considered the buckling of a drill string in a straig:rt vertical hole, a problem also considered by Willers6 in 1941. It wns concluded that very low bit weights must be used to prevent hole deviation resulting from drill collar buckling. The use of conventional stabilizers was proposed2 in 1951 by Mac Donald and Lubinski as a method for permitting greater Sit weights to he carried without drill collar buckling. These authors pointed out that a 2° nearly vertical spiral hole can cause severe key seatinp, and drill pine near, wilereas n 3 straight inclined hole with deviation all in one direction, while not vertical, will not result in serious drillirig or producing problems. Studies were continued with an investigation of straight inclined holes by Lubinski and Woods3 in 1953. In this paper they concluded that perfectlv vertical holes cannot be drilled even in isotropic forriations unless extremely low bit P-eights are used. .l'l~ey postulated that constant drilling conditions produce holes of constant inclination angle and varying conditions cause the hole to drill at a neiv equilibrium angle. This analysis was not concerned with drill string buckling since it was based on an equilibrium solution in which the ~irill string Was presumed to lie along the lower side of the hole abcrve the point of tangency. Weight of the drill collars below the point of tangency tends to force the hole toyard the vertical, whereas the weight on hit tends to force the hole aurav from the vertica l. The concept of an anisotropic formation Lvas introduced as an empirical method for explaining actual drilling data and as a means for extrapolating known deviation data to otiier conditions of hit

Jan 1, 1967

By S. H. McFarlane, K. H. Zaininger, G. W. Cullen, C. C. Wang, G. E. Gottlieb

Heteroepitaxy of silicon on stoichiometric spinel has been studied. Both boron-doped (p-type) and arsenic-doped (n-type) single-crystal silicon films have been grown by the pyrolysis of silane on sioichiometric spinel (MgAl2O4) substrates prepared by a flux technique. The spinel crystals are free from strain and subgrains, and exhibit no thermal instability at temperatures employed for silicon deposition. The growth parameters of epitaxial silicon have been studied. Effects of substrate orientation, surface preparation, and growth conditions on the silicon Properties have been determined. The silicon-spinel composite was characterized by X-ray diffraction, electron diffraction, electron microscopy, and optical techniques. Information on epitaxial orientation relationship, defect structures and film-substrate interface has been obtained. A parallel orientation relationship was found between silicon and spinel. The silicon films exhibit no subgrain structures. However, growth pyramids, microtwins, stacking faults, and dislocations are the prevalent defects. The deformation of epitaxial silicon was measured by an X-ray technique. It was found that the epitaxial silicon is strained under compres-sive stress due to the thermal expansion difference between the film and substrate. The stress was estimated using the classical plate theory and beam equation. Electrical properties of the epitaxial silicon have been measured, including resistivity, carrier concentration, and Hall mobility. MIS and vertical through diffused junction structures have been fabricated wing silicon-spinel composite. Information on MIS characteristics, minority carrier life time, and junction properties has been obtained. THE achievement of single-crystal growth of large area silicon semiconductor films on oxide insulating substrates is of technical importance to many solid state electronic devices. The semiconductor-insulator composite structure is also of scientific interest because the heteroepitaxy is determined by the spatial relationship between the atomic arrangement in the substrate and that of the atoms in the appropriate crystallographic plane of silicon. The degree of crystalline perfection of the silicon deposits depends also on the physical condition of substrate surface. Epitaxial growth of silicon on commercial flame fusion Al-rich spinel (MgO:3.3A12O3) has been reported by several investigators.'-4 The lattice of spinel of this composition is distorted. The material cracks and exsolves the excess alumina in the lattice at temperatures (-1200°C) used in fabricating silicon devices. Stoichiometric MgA12O4 spinel exhibits neither lattice distortion nor thermal instability. Results are given on the epitaxial growth and characterization of silicon on stoichiometric spinel. EXPERIMENTAL Fabrication of Silicon-Spinel Composite Structures. The MgA12O4 spinel substrate wafers were prepared from bulk single crystals grown at about 1200°C by a flux technique5 using a PbF2 flux. The crystals are free from strain and subgrains, and exhibit a typical dislocation density of less than 50 lines per sq cm. The crystals are thermally stable without cracking and exsolution of alumina to at least 1500°C. The spinel crystals were oriented for cutting by the Laue X-ray back-reflection method.6 Substrate wafers (about 25 mil thick) of (Ill), (loo), and (110) orientations have been obtained bu cutting the X-ray oriented crystals using a standard type diamond wheel. An accuracy of better than 1/2 deg is maintained throughout the operation. The spinel substrate wafers were mechanically lapped and polished to produce the flat and smooth surface which is required for silicon epitaxy. Lapping was carried out with about 30-µ boron carbide abrasives to obtain a flat coplanar surface. The lapped surface was further polished using successively finer grades of alumina, ending with the 0.3-µ grade. After polishing the wafers generally have a flatness of ±0.4 µ per cm, as revealed by interferometry. Fig. 1 shows (111) oriented MgA12O4 spinel wafers of various shapes.

Jan 1, 1970

By A. Vifian, I. lwasaki

Several samples of copper-nickel ore from the Duluth Gabbro were studied to relate their mineral-ogical characteristics with their amenability to concentration by flotation. The most common rocks in the samples were norites, gabbros, and troctolites. The texture of the rocks varied from coarse pegma-titic to very fine. The copper contents ranged from 0.2-0.7% and the nickel contents from 0.07-0.15%. The ore minerals were chalcopyrite, cubanite, pyrrhotite, and pentlandite. Most of the ore minerals occurred in interstices between laths of plagioclase, but some were included in the gangue grains. The samples responded readily to xanthate flotation. After a 65 to 100-mesh grind about 95% of the copper and 85% of the nickel were recovered in a bulk sulfide concentrate. Such recoveries remained constant even with grinds as fine as 270 mesh due to the extremely fine inclusions of sulfides in the silicate gangue. A finer grind than 270 mesh was necessary to free the copper-iron sulfides from the nickel-iron sulfides. A combination of time and British gum* was quite effective in producing concentrates analyzing 25-30% copper. The nickel concentrate averaged 1.5% nickel. Most of the nickel lost in the tailing was present as un-liberated sulfides and not as nickel in the olivine structure. The nickel content of the olivine was only about 0.05 or 0.08%. Western world nickel usage in 1967 is expected to be the second highest on record, amounting to 825 million lb. Despite a rise in mine production, however, demand is expected to exceed supply in 1968. ' Hence, exploration, development, and production expansion projects are being accelerated on a world scale. In Minnesota the copper-nickel bearing Duluth Gabbro is receiving much attention. During the past year 11 companies have been granted leases in the region, and the 1967 Minnesota legislature enacted a tax law designed to encourage the development of a copper-nickel industry. Although it is only during the past few years that mining companies have shown an active interest in the Minnesota copper-nickel deposit, copper-nickel minerals have been known to exist in northeastern Minnesota since 1899.3 At the 28th Mining Symposium, Dr. P. K. Sims, from the Geological Survey of Minnesota, gave a review of copper-nickel exploration in northeastern Minnesota,4 in which he emphasized that the potential of the Duluth Gabbro complex is large. Tests on samples from the Kawishiwi River area were reported by the United States Bureau of Mines in 1955.' In 1964, the Mines Experiment Station described tests on samples from the Gunflint Trail: and in 1966 the Minnesota Geological Survey published a geological map of the Gabbro Lake Quadrangle. The Mines Experiment Station published a study of the concentration of a Minnesota copper-nickel ore in 1967.7 The present paper is divided into three parts. The first describes the mineralogy of some rock samples from the Kawishiwi River area of northeastern Minnesota; the second summarizes the results of numerous flotation tests that were made on the samples, and the third explains the loss of nickel in the flotation tailing. MINERALOGY OF KAWlSHlWl ROCKS Recently five samples of mineralized gabbro from the Kawishiwi River area, a few miles east of Ely, were received at the Mines Experiment Station. One of the samples was a 175-lb composite, which was designated Ore 1556. The other four samples were 7-lb grab samples that had been obtained from four different exploration pits. They were designated Ore 1626, Lots 1 through 4. Basic Mineralogy: Many authors have reported that the rocks of the so-called gabbro of the Duluth Intrusion vary widely in composition.8-9 The samples on which our studies were based also contained a wide range of rocks. A gabbro, olivine-gabbro, anorthosite-gabbro, norite, and a troctolite were represented. The essential minerals in the samples were plagio-clase, pyroxene, and olivine, in variable proportions.

Jan 1, 1969

By P. L. Raffo, T. E. Mitchell

Single crystals of Ta-Re alloys have been deformed in tension and compression as a function of solute concentration and temperature. The temperature dependence of the yield stress is decreased by alloying. At low temperatures there is a minimum in the yield stress (at about 2 at. pct) as a function of concentration. Three-stage hardening was not observed in the alloys. Linear hardening rates, where observed, were characteristic of stage II in pure tantalum. At low temperatures and high concentrations, work softening was often prominent at high strains. Electron microscopy revealed that dislocations are mostly of screw orientation, although heavily jogged and cusped, and often occurring in dipole pairs. The alloys become more prone to cleavage with increasing rhenium content, due mostly to an increasing yield stress rather than a change in cleavage strength. Alloying apparently decreases the Peierls stress of bcc metals at low temperatures by facilitating kink nucleation at solule atoms on screw dislocations. Higher solute concentrations further increase the yield stress. Quantitative calculations and comparisons with other bcc alloy systems are made to show that the predominant hardening mechanism is due to the interaction of dislocations with misfitting solute atoms close to their slip planes. The interaction is so localized that the core dilatation of dislocations could be important. CONSIDERABLE interest has arisen in recent years concerning the mechanical properties of unalloyed bcc metal single crystals.'-7 These and similar studies on polycrystalline materials have resulted in a considerable understanding of the macroscopic yielding characteristics8, 9 and the process of work hardening.'' This latter advance is due in a large part to the increased use of transmission electron microscopy in P I RAFFO junior Membar AlMF is Metallyureist Iewis such studies and the general observance of three stages of work hardening in the shear stress-shear strain curves. The properties of substitutional alloy single crystals of bcc metals have not been determined in as much detail as in the pure metals. Insufficient systematic studies have been made on the effect of alloying on the magnitude and temperature dependence of the yield stress or the stress-strain curves. The alloy systems which have been studied to some extent have been Ta-W,11, 12 Ta-Mo," Ta-Nb,12'14 Mo-Re,15 W-Re,16 and alloys of iron with nickel,17 platinum,17 vanadium,18 and aluminum.18 A large body of data exists on Fe-Si alloys, but these have mainly been a result of the experimental convenience of using this material in place of unalloyed iron, rather than a comprehensive study of the mechanical properties of the alloy system per se. The present authors have previously reported additional data on the properties of Ta-Re, Ta-W, and Ta-Mo alloy single crystals.1g Some of the data on Ta-Re alloys will be described later in this paper. Briefly, single crystals of Ta-Re (1.2 to 10.6 pct), Ta-W (6.2 and 10.2 pct), and Ta-Mo (2.9 and 9.0 pct) were grown by the floating zone method in vacuum. Compression tests were performed in the temperature range 77" to 623°K. Slip was found to occur in Ta-Re alloys at 77' and 298°K on the (~ll)[lil] system and slip lines were coarser and straighter than in unalloyed tantalum. No three-stage hardening was observed in any of the alloy systems and the curves were nearly parabolic. At temperatures above 175°K the yield stress* increased monotonically with in- creasing composition while at 77" and 175°K the yield stress initially passed through a minimum after which it began to increase again for concentrations greater than about 2 pct Re. Similar minima were observed in Ta-Mo alloys and to a lesser extent in Ta-W alloys. The minimum was interpreted as being a result of a

Jan 1, 1969

By C. W. Sherman, John Chipman

IN the mathematical statement of the law of mass action, the activity of each substance consumed or produced in a reaction is used to obtain a numerical constant which is characteristic of the equilibrium of that reaction at the given temperature. The activity in many cases is equal to, or proportional to, the concentration. If this is the case, any units denoting concentrations, such as weight percentage or mol fraction, may be substituted in the equilibrium expression. It is even permissible to use mixed units provided only that each unit is that used in defining the activity of the corresponding substance. The indiscriminate use of concentration units in writing equilibrium constants sometimes leads to very erroneous results. On the other hand, what appear to be contradictory results from similar investigations often might be resolved if the activity is the quantity that is used to determine the equilibrium constant for the reaction in question. De-sulphurization serves as an important illustration. Sulphur in lron and Steel The control of the sulphur content of the finished product is one of the oldest and broadest problems in the metallurgy of iron and steel. In general, this control must be exercised through the action of a slag, and for this reason experimental studies of the distribution of sulphur between slag and metal have assumed considerable importance. Under slags of the type found in the basic open-hearth furnace the ratio (% S)/[% S] does not in general exceed about 8. Under blast-furnace conditions, however, de-sulphurization ratios of 50 to 100 are readily obtained, and under laboratory conditions using similar slags, the ratio may be as high as 400. The fact that blast-furnace metal is much more readily desulphurized than is molten steel rests upon two distinct phenomena. The first of these is connected with the slag reaction. In the open-hearth furnace, the equilibrium in the following reaction places a definite limit on the sulphur content of the slag: S + 0-- = 0 + S- - where the symbols underlined indicate elements dissolved in the liquid metal, while slag constituents are represented as ions. The high oxygen content of the open-hearth bath prevents this reaction from proceeding far enough to effect good desul-phurization. In the blast-furnace process, however, the oxygen activity is limited by the presence of carbon in the metal and in the coke bed and the controlling reaction becomes: S_+O- + C_=S- + CO(gas) [2] The second phenomenon which contributes to the easier desulphurization of blast-furnace metal is the effect of high concentrations of other elements. These elements, notably carbon, silicon, and phosphorus, increase the thermodynamic activity of sulphur several fold. As a result of this increase, the escaping tendency of sulphur from the metal phase is increased and its removal facilitated. Previous Studies It becomes, therefore, a matter of importance to determine the effects of various elements upon the activity of sulphur in the melt. The experimental approach to this problem has been made through the equilibrium between sulphur in the melt and gaseous atmospheres containing hydrogen and hydrogen sulphide. The reaction and its equilibrium constant are written as follows: S + H2(gas) =H2S(gas);K1 = -- [3] Pn2 • as where the symbol a, represents the activity of the sulphur in solution in the metal. The understanding of the chemical behavior of sulphur in steel and pig iron rests on a firm knowledge of the binary system Fe-S. A number of studies of the equilibrium have given closely agreeing results from which the activity and free energy of the dissolved sulphur may be found. The recent paper by Sherman, Elvander, and Chipman1 includes a discussion and quantitative comparison of the results of several of the significant researchesr-" on dilute solutions of sulphur in iron. The results of this study indicate that the relationship between the ratio Ph,s/p+ and the percentage of sulphur in solution is not a linear one. This

Jan 1, 1953

By A. W. Schlechten, C. M. Hsiao

The apparent vapor pressures of a number of metal sulphides were determined by measuring their rate of weight loss when they were heated under vacuum. The calculated pressures are due in some instances to the volatility of the sulphide and in others to the decomposition pressure. FIE direct reduction of metallic sulphides, as in the precipitation method for lead or antimony, is not a widely used process today. However, it might be employed for the production of a number of metals if the operation were carried out under reduced pressures. Two general procedures are possible; the reducing agent could form a stable nonvolatile sulphide from which the valuable metal could be removed by volatilization or liquation. The other approach would be to choose a reducing agent which would form a sulphide that could be volatilized away from the valuable metal. A vacuum operation would serve to protect the sulphides and metals from oxidation and would increase the evaporation rates. A related process is the separation of metallic sulphides by selective volatilization either at atmospheric pressure or under vacuum. This procedure is already used commercially for the elimination of lead and cadmium as PbS and CdS from zinc calcines; it might well have other applications. To predict such processes it is necessary to know the relative volatilities of the metallic sulphides and to know whether they volatilize as sulphides or whether the predominant weight loss is due to decomposition. Such data would also be of value in studying problems such as the use of sulphides for refractories, as described by Brewer,] or in the evaluation of the theory of ore deposition from the vapor state, as proposed by Brown.' Qualitative statements concerning the volatility of metallic sulphides can be found frequently in the literature and are well summarized by Mellor, but accurate determinations of rates of evaporation or vapor pressures are very scarce. Kelly" lists vapor pressure data only for PbS; his reference being to the work of Schenck and Albers,4 who measured the vapor pressure of PbS by a dynamic method between 850" and 995°C. More recently Veselovskii5 has determined the vapor pressures of the sulphides of antimony, lead, cadmium, and zinc at temperatures ranging from 360" to 1000°C using Knudsen's method. A second Russian worker, Pogorelyi,6 determined the vapor pressures of CdS and ZnS at temperatures from 900" to 1250°C. The results obtained by these workers are shown in subsequent graphs in comparison with the data of this paper. Brewer and coworkers1 have studied some of the metallic sulphides to determine their suitability as refractories in vacuum. Veselovskii's determinations on PbS checked well with those of Schenck and Albers, and his determinations of CdS check almost exactly with Pogo-relyi. For the vapor pressure of ZnS the data of Veselovskii and that of Pogorelyi are in fair agreement, as shown in Fig. 1, but it should be pointed out that Lumsden7 has discovered that the equation given by Veselovskii for the vapor pressure of ZnS: - 14,200 log P9.495 is in error by a factor of ten when compared to the experimental data. In contrast with the scarcity of data on vapor pressures, the decomposition pressures of many metal sulphides have been determined and are summarized by Smithells.8 Theoretical Considerations The experiments described in this paper consisted of determinations of the rate of weight loss of certain metallic sulphides under very low pressures at different temperatures. These data plus observation and analyses of the products reveal the mechanism of the weight loss and also provide a basis for the calculation of the vapor pressure or apparent vapor pressures of the sulphides.

Jan 1, 1953

By R. H. Frazier, C. H. Lorig, F. W. Boulger

This investigation establishes the effect of ferrite grain size resulting from various heat treatments on the transition temperature of a semikilled steel plate. Different austenitizing temperatures and various cooling rates were used. The ductile-brittle transition temperatures were determined by the Navy tear test and the keyhole Charpy test. THE data presented in this paper deal with quality characteristics of ship-plate material which were investigated in a research project sponsored at Battelle by the Bureau of Ships, Dept. of the Navy. Specifically, the object of this investigation was to establish the effect of ferritic grain size (resulting from various heat treatments) on the so-called transition temperature of ship-plate steel. Transition temperature is not a fixed property of steel. It is derived from a series of static or dynamic tests made at various temperatures and is qualified by specifying the type of test employed as well as the testing criteria. Because in earlier investigations of ship-plate quality1,2 the so-called Navy tear test and standard notched-bar tests (keyhole Charpy) proved to be useful in interpreting instances of brittle behavior of ship plate in service, these tests were used in the investigation reported in this paper. By definition,' in the Navy tear tests the highest temperature at which one or more of four specimens breaks with a brittle fracture (that is, when less than 50 pct of the fracture area has a dull fibrous texture) is termed "transition" temperature. In the Charpy tests, the 12 ft-lb level of energy absorption was used as a criterion indicating the "transition" temperature, although other levels of energy absorption were also used for comparison. Earlier work" on ship-plate steels indicated that the temperature at which ship plate is finished has a very significant effect on its notched-bar properties. Plates rolled in the laboratory, where the finishing temperature can be carefully controlled, showed a 16°F decrease in tear test transition temperature when the finishing temperature was lowered 200°F (from X" to Y°F). The same plates showed a drop of 10°F in the keyhole Charpy transition temperature from the same decrease in finishing temperature. Commercially finished plates' exhibit a similar trend. When the ferrite grain size of the hot-rolled laboratory plates was determined, a close relationship was found between the ferrite grain size and the notched-bar transition temperature." " he indicated relationship between grain size and transition temperature was in agreement with the findings on low carbon steels of Hodge, Manning, and Reichhold' despite the differences in composition of the steels. The cooling rate after rolling varies from one steel plant to another. This variation changes the micro-structure" and appears very likely to affect the notched-bar properties of the steel plates. In the investigation summarized in the present paper, heat treatments simulating finishing practices in the hot rolling of ship plate were used in order to vary the ferritic grain size. It is believed that the indicated relationship between grain size and transition temperatures of the ship-plate material will prove useful in estimating the effect of rolling temperature and of cooling rates from rolling temperatures on the notched-bar properties of semikilled steel plate. Material The semikilled steel plate used in this investigation was a ¾ in. hot-rolled plate from an open hearth heat. Other plates from this heat have been used on many other studies performed for the Ship Structure Committee," "," and the heat has been identified as project steel "A". The chemical composition of the plate1 was 0.25 pct C, 0.49 pct Mn, 0.011 pct P, 0.045 pct S, 0.04 pct Si, and 0.004 pct N.

Jan 1, 1956

By P. R. Sahm, T. V. Pruss, D. A. Gandolfo

Cb 3 Sn powders were hot-pressed to estahlish densi-fication conditions and assess the possible use of such compacts in multiphase structures with ceramic or magnetic inclusions. Superconducting transition temperatures, Tc, were measured as a function of powder particle size, pressing temperature, and second-phase admixtures. The highest transition temperatures were found in coarse powder (5 to 500 u) compacts and were only weakly depended on pressing temperatures up to 1200°C. Fine powders (below 5 p), however, both single-phase CbsSn and Cb3 Sn-composites, showed a stronger dependence on hot-pressing temperatures. While Al2 O3 phase admixtures did not affect T, much more, a Pronounced T, degradation was observed upon the addition of ferrimagnetic Fe2 Mno. 5 Zno.5 O4 powders. Likewise, critical current densities, Jc, at 4.2° K were lowered appreciably in the ferrite doped samples, whereas the neutral A1203 inclusiow gave slightly improved Jc values. MULTIPHASE structures in electronically active materials have recently gained in interest as pointed out by Galasso in a review article.' In superconductors the most widely reported group are eutectic alloys which have been mostly investigated with respect to the proximity effect.2"4 In addition, "artificial eu-tectics", for example in the form of mercury-vycor glass sponge5 or fine niobium wires imbedded in a copper matrix,= have been prepared to attain higher critical fields and critical current densities. The idea was to enhance flux pinning phenomena by second-phase inclusions or ho1es. 7 Flux pinning should also be possible by the introduction of insulator inclusions into a superconducting matrix. Ceramic-metal combinations are most easily produced by hot pressing (= pressure sintering), as it permits an almost unlimited selection of material combinations. Cb 3 Sn has been prepared by vapor phase growths or in the form of thin films. Large compacts must be sintered,1° however, and normally present difficulties. At temperatures below 1350°C insufficient densities are obtained and at higher temperatures the loss of tin due to dissociation upsets the stoichiometry. Hot pressing is a natural approach to circumvent the problems, since one can obtain satisfactory densities despite low sintering temperatures. This work was mostly concerned with establishing conditions to hot press Cb3 Sn and Cb3 Sn multiphase structures (= composites), because no data are presently available, and to evaluate these with respect to their transition temperatures. However, a few measurements on critical current densities were also carried out, in particular to assess the value of ferrimagnetic inclusions. I) EXPERIMENTAL PROCEDURE The experimental procedure involved the preparation of feed material and powders, hot pressing, and evaluation of the resulting ingots. As no attempts were made to synthesize Cb3Sn from the elements during hot pressing, feed material had to be produced. For this purpose, a stoichiometric Cb-Sn powder mixture was compacted into a 3-cm-diam ingot (80,000 psi) and then inserted into a quartz tube and evacuated. Rf heating was employed. Above the tin melting point (230°C) liquid tin was forced out of the ingot, but was pulled back by capillary action after approximately 0.5 hr of continuous pumping at 700°C. Thus, it appears that evacuation at this temperature caused desorption of impurity gas creating wetting surfaces which, later on, favored alloying at relatively low temperatures. After a presintering period of 17 hr at 800°C, the quartz tube was tipped off and sealed into another such larger-diameter tube which, in turn, was connected to a pump system. This configuration permitted a temperature treatment at 1400°C, carried out for 65 hr, without collapsing of the glass walls or unfavorable chemical interaction of Cb3Sn with the quartz. The resulting material was

Jan 1, 1969

By F. J. Fayers, J. W. Sheldon

A theoretical discussion is presented of the behavior of the interface between two fluids of different physical properties when displacement is occurring along a thin tilted bed. An approximate equation of motion is deduced for the motion of the interface, suitable boundary conditions are derived and the conditions necessary for the approximation to be valid are determined. Steady-state behavior and the circumstances under which a steady-state interface can develop are discussed. Finite-difference solutions of the equation of motion for two characteristic water-drive problems are presenled. The theory of displacement in a thin bed may be regarded as being the porous-medium-equivalent of the classical "shallow-water wave" theory of hydrodynamics. INTRODUCTION The solution of moving interface problems are important in predicting the behavior of oil reservoirs under various conditions of production. Kidder4,5 has obtained analytic solutions for the fingering problem and for another particular case of the motion of the interface between two immiscible fluids of unequal density in a porous medium. In the present analysis, we analyze the problem of the motion of an interface along a slightly dipping bed whose length is long compared with its thickness. The requirement of a thin bed is necessary in order to give a simple differential equation for the motion. The two fluids are of unequal density and mobility. In the derivation of the equation of motion, it is assumed that the lighter fluid is being injected at constant rate at the high end of the porous layer, while heavy fluid is produced at the low end of the layer. The analysis applies equally well, however, to the reverse procedure in which the heavier fluid is injected at the low end of the tilted layer. It will be shown that the behavior of the system is critically dependent on which fluid has the higher mobility and that the interface can in certain circumstances achieve a simple progressive steady-state shape. The fluids may be considered to be immiscible or miscible. It is assumed, however, that the thickness of the interface region is negligible in comparison with other dimensions of the system, and that the strength of the saturation or concentration discontinuity remains constant during the motion. In conjunction with Buckley-Leverett theory and areal sweep-out calculations, the tilted interface problem is one of the fundamental problems of reservoir engineering; it defines the very important underpassing and overpassing phenomena associated with water-drives, gas-drives and secondary recovery operations. The tilted interface problem has been dealt with previously by Dietz.2 In the present paper, we endeavor to derive the pertinent mathematical results more rigorously, and in doing so we obtain modifications in both the differential equation and boundary conditions for those given by Dietz. We also attempt to show the connection between these results and some of the recent work on the stability of interfaces. Finally, we attempt to demonstrate the practical importance of the thin bed theory by showing the difference in behavior of two characteristic waterflood problems. In the favorable mobility case recovery is improved by increasing production rate, while in the unfavorable case undercutting or overcutting is minimized by reducing the displacement rate. PROPERTIES OF THE EQUATION OF MOTION Fig. 1 illustrates a porous layer of constant thickness H and tilt 8 with Fluid 1 of mobility ?l and density pl below Fluid 2 of mobility ?2 and density p2. The fluids are incompressible and flowing with volumetric flux q along the layer. Both the slope a of the interface with respect to the bed and the curvature of the interface are assumed to be small. What is meant by "small" is indicated in the derivation given in Appendix A of an approximate equation of motion for the interface. Other symbols are defined in the "Nomen-

By Donald L. Katz

The compressing of gas into a partially depleted gas drive oil reservoir to bring the contents to a single phase miscible with gas is proposed as a process worthy of serious study. The compressed gas and vaporized oil would be recovered by cycling. This paper explores the Possibility of recovering oil from reservoirs of 6,000 ft or more by this method. INTRODUCTION Many new methods for increasing the recovery of oil from reservoirs are under consideration in the various research laboratories. One method which should be considered for recovering oil From partially depleted gas drive fields is to compress gas into the reservoir until the contents become a single phase miscible with more gas. Natural gas then may be cycled through the reservoir to recover the oil. This procedure ideally will eliminate the capillary effects of the liquid ill the porous media and should permit recoveries similar to those obtained in cycling operations, probably of the order of 80 per cent. This paper explores the information now available for the prediction of the performance of such a project and discusses the problems likely to be encountered in recovering oil by cycling. For many years dry natural gas has been passed through oil reservoirs to recover natural gasoline which would vaporize from the oil. Recently a process of recovering more of the high boiling hydrocarbons has been described by employing high pressures at which the heavier hydrocarbons have a higher volatility. Nevertheless. this reported method does not eliminate the differential nature of the vaporization process and capillary forces are still present in the reservoir. The process under discussion in this paper would minimize differential vaporization and would remove capillary forces which are responsible for low oil recoveries. Higher gas pressures are required to accomplish this removal of the miniscus, but it does not follow that more gas is required for oil recovery. The process is limited to reservoirs deep enough to permit the use of the required pressure — Probabably 6,000 it and deeper. DESCRIPTION OF THE PROCESS Briefly, the process is to compress natural gas into an oil reservoir which is partially depleted so that it has an oil saturation in the range of 40 to 60 per cent of the hydrocarbon pore space. The injected gas will pass through the channels formerly carrying gas to the wells to build up the pressure and dissolve in the oil phase. This injection will continue without production from the field until the reservoir reaches a single phase. If one were to select unique conditions such that the gas composition, the reservoir oil composition and the Per cent saturation would bring the mixture in the reservoir to the critical temperature and pressure simultaneously the phase behavior accompanying injection is shown by Fig. 1. The oil-gas mixture in the depleted reservoir has a critical temperature at C,. Addition of natural gas to the mixture will give a new critical temperature for each addition. Mixture No. 3 is shown to have its critical temperature at the reservoir temperature and reservoir pressure at P: the critical pressure. Under ideal behavior, the entire reservoir would be at iti critical temperature and pressure and the entire hydrocarbon content would be at a single phase. If the reservoir content were a binary system of methane and a heavy constituent. it would be miscible with more methane. However, for complex mixtures the critical locus does not confine the two phase region, and the dew point curves of Fig. 1 occur above the critical locus. If fluid which was injected into the rezervoir at the critical point were of the

Jan 1, 1952

By S. C. Sun, John A. L. Campbell

Objective of the ittvestigation was to determine the electrokinetic differences, if ally, of anthracite lithotypes and thus establish the feasibility of making a coqlstituent separation by froth flotation or other surface-dependent processes. The elec-trokinetic properties were determined by streaming potential methods. In addition, chemical and physical analyses of the lithotypes were made to establish nonsubjec-tive parameters for their diflerentiation. Electrokinetic results indicate a difference in the characteristics of the lithotypes. The isoelectric points of 4 anthracites and 12 lithotypes were obtained. It was suggested that the relative flotation rates of the lithotypes were pH dependent and that the maximum flotation rate of anthracite occurs in an acidic circuit. Although there has been an increased interest in the electrokinetic properties of coal,' research on the subject is still in an early stage of development."' To the authors' knowledge, no electrokinetic studies have been made on coal lithotypes, particularly anthracite litho-types. This paper presents the results of an investigation of the double layer properties displayed at the anthracite/water interface (whole coal and lithotypes) as determined by streaming potential methods. It is hoped that this investigation and related future investigations will provide correlations from which the surface properties of any coal can be predicted and then related to surface-dependent processes such as froth flotation and flocculation. Another aspect of this research, undertaken to determine the physical and chemical parameters necessary for anthracite lithotype differentiation, was previously published.? The number of parameters involved, lithologic, organic and inorganic, and the wide divergence of these parameters within an individual coal limits the practical utilization of the results; however, the result? are of value and of interest in guiding theoretical developments. Keeping the limitations in mind, the results are analyzed in terms of their application to froth flotation processes and are used to indicate the feasibility of making a lithotype separation by flotation. Experimental Procedure Prior to discussing the experimental work per se, it would be of value to establish an understanding of anthracite lithology. Anthracite Lithology: Coal seams display two different modes of variation, rank and type. A coal's position in the continuous series ranging from peats through anthracites determines its rank. The rank of the material under consideration is anthracite. The different bands of coal which constitute a coal seam are distinctly contrasted in regard to physical properties and chemical composition. These megascopic bands are the coal types and are termed lithotypes., A megascopic examination of 11 anthracites revealed three distinct, homogeneous, lithotypes. The classic description of bituminous coal lithotypes as proposed by Stope" was found to be quite adequate for recognizing the three lithotypes in anthracite, namely vitrain, durain, and fusain. The term vitrain describes the brilliant constituent of coal; durain describes dull coal; and fusain is the term applied to fossil charcoal. The anthracites studied were generally found to contain 60-80% vitrain, 10-30% durain, and 1-10% fusain. A complete description of the physical characteristics and chemical composition of the studied lithotypes can be found in a previous publication.' Sample Preparation: Nine of the anthracites used in the investigation were from Pennsylvania, one was from Russia, and one from Wales. Table 1 shows the various designations and sources of the employed anthracites. The letter V, D, or F added to the whole coal designation indicates respectively the vitrain, durain or fusain lithotype of that coal. The samples were carefully collected to avoid contamination. To insure against oxidation, the samples were obtained as fresh as possible and stored under nitrogen or water. Generally a representative sample of the seam and samples containing high concentrations of one or another of the petrographic constituents were secured for each coal. Pure lithotypes were prepared by manual separation and selection. The pure lithotypes and representative samples were ground to —35 mesh and screened to 35 x 48 mesh. The 35 x 48-mesh fraction was then passed over a magnet to remove iron contamination, washed with doubly

Jan 1, 1971

By N. L. Carwile, G. W. Geil

A metallographic study was made of deformation twinning (Neumann lamellae) in ingot iron slowly deformed in tension at —196O and —150°C. The results showed that twinning is initiated mainly during the initial stages of plastic deformation. However, the breadth of the twins generally increases with increase in strain up to fracture of the specimen. HE results of an investigation of the effect of low I temperatures on the flow, fracture, strain hardening, and strain aging characteristics, and the true stress-strain relationship for specimens of ingot iron deformed in tension were reported recently.1,2 In that study specimens of ingot iron, in different initial conditions, were slowly deformed in tension at various temperatures between —196" and +100°C. A phenomenon observed, but only briefly reported, was the formation of deformation twins (Neumann lamellae) in the specimens deformed at the lower temperatures. Preliminary metallographic examination of these specimens indicated that there was apparently some correlation between the deformation twinning and the strain of the specimen and that this factor merited further investigation. Some recent investigations have indicated a direct association of Neumann lamellae and the fracture of the metal. Bruckner".' * postulated that the twinning immediately precedes the fracture and the latter is initiated by the stopping of the propagation of twins, either at subgrain boundaries or at other structural features. Tipper and Sullivan5 postulated that Neumann lamellae are initiated by the shock or a shock wave set up at fracture in the still highly stressed unbroken metal, and that a high rate of deformation is a necessary condition for their formation. An extensive metallographic examination, therefore, was made of many of the specimens used in the study of ingot iron at this Bureau and of additional specimens deformed to selected strains under various conditions. The present paper summarizes the effects of deformation under these conditions upon the breadth and scope of the deformation twins. Other features of twinning will be discussed in another paper. Material and Testing Procedure All of the specimens were prepared from one lot of ingot iron, as hot-rolled, of chemical composition other than iron as follows: C, 0.02 pct; Mn, 0.02; P, 0.005; S, 0.018; Si, 0.002; Cu, 0.10; 0, 0.058; and N, 0.002. Cylindrical tensile specimens with a 2 in. gage length were used. The reduced section was slightly tapered from each end; the diameter (0.438 in.) at the midsection of the gage length was about 0.003 in. less than at the ends. The specimens were finished to the final dimensions by grinding and polishing in the axial direction. The ends of the specimens were machined with 3/4 in. x 10 threads and the shoulder fillets were machined to a radius of 0.75 in. The specimens were extended slowly in tension (deformation rate less than 0.5 pct reduction in area per minute) while immersed in an appropriate cryogenic liquid maintained at the desired temperature. The minimum diameter of the specimen was measured during the test by means of a specially designed reduction of area gage accurate to 0.0001 in." A detailed description of the testing equipment and the method of maintaining the desired temperature is given in a previous paper.' Each specimen, after deformation to a specified strain at a selected temperature, was sectioned longitudinally and examined metallographically. The preparation of specimens for metallographic examination was carried out in the usual manner by mechanical polishing and etching. Results and Discussion Deformation twins in specimens of ingot iron extended slowly in tension at —196" and —150°C are shown by the representative micrographs of Figs. 1

Jan 1, 1954