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By W. A. Tiller, S. O’Hara

Grain refinement in stirred melts has previously been shown to arise from dendrite segmentation. The present work discusses experiments capable of distinguishing between remelting and mechanical effects which result from fluid motion. Nucleation of still un-dercooled Sn-1 pct Pb melts with a single-crystal seed shows that the grain size of the resulting ingots decreases as the undercooling at nucleation increases up to about 1Z0C, then increases again for larger undercoolings. Pure melts exhibit little refinement as a result of nucleation at any undercooling up to 12°C. The presence of fluid motion gives rise to grain multiplication in pure melts, but the magnitude of this effect is partly obscured by solid-state pain growth. The results indicate that two grain-multiplication pvocesses can operate, one which involves dendrite remelt ing, and another associated with fluid motion. Small ingot experiments indicated that an equiaxed transition can be caused by fluid motion. THE presence of forced convection during recales-cence of undercooled Sn-1.3 pct Pb melts has been shown to give rise to extensive grain refinement during solidification of small ingots of this alloy.''2 In Ref. 2, this refining was shown to result entirely from dendrite fragmentation and not from any nucleation mechanism. The purpose of the present work is to establish what processes lead to dendrite segmentation. Experiments were therefore carried out to determine the resulting structure of both pure tin and Sn-1 pct Pb melts, nucleated at various undercoolings by single-crystal seeds in the absence of forced or natural convection. By comparing the information obtained from these experiments with the results of Refs. 1 and 2, the effects of fluid motion on the ingot structure, and the details of the segmentation mechanisms, should become clear. The results of these experiments should also be helpful in understanding the solidification structures of larger ingots since natural convection, which is known to play an important role in determining ingot structure13 differs only in degree from the fluid-motion effects studied here. I) EXPERIMENTAL PROCEDURE The apparatus shown in Fig. 1 was constructed to permit controlled nucleation of stirred or unstirred supercooled melts using a seed oriented in the tin dendrite growth direction. Because the melts, in all cases, were capable of larger supercoolings than the one used in each experiment, the structure observed always resulted from a single nucleation event at the surface. The sequential procedure was as follows: Tin was melted under purified hydrogen and the oxide removed at a temperature of 450°C . Electromagnetic stirring was then used to clear the surface completely and during this time the guide tube was lowered underneath the melt surface. A pointed Czochralski-like crystal was then propagated from a specially prepared tin dendrite seed4 inside the guide tube while the temperature of the bulk melt was held just above the melting point, ensuring a perfectly clean seed which was epitaxial with the original dendrite. The dendrite and epitaxial seed, still in the guide tube, were withdrawn from the melt which, in turn, was undercooled to 2C° below the temperature at which the nucleation experiment was to be performed. The melt was held there for several minutes, both in stirred and in still-melt experiments. The temperature was next raised to the required value and the melt nucleated by the carrot seed inside the guide tube, the heater power being shut off just after nucleation. In experiments where quenching after nucleation was required, a high-density graphite crucible was used, but otherwise the procedure was as described above. The temperature gradient in the melt before nucleation was kept below 1C° per cm by carrying the experiment out just below the center of the heater shown in Fig. 1.

Jan 1, 1968

By C. H. Herty

Almost every metallurgist who has given the Howe Memorial Lecture has had a personal contact with the distinguished gentleman to whose honor this hour is devoted. Unfortunately for me, such personal contacts were not possible. However, in the preparation of a thesis on the open-hearth process, one of my earliest tasks was to make a survey of the literature, and it was from Professor Howe's Metallurgy of Iron and Steel that I drew a number of references to previous work which formed the foundation for my reading. In his volume there is such a complete exposition of the then current thought on the subject of slags and on their role in the elimination of phosphorus from steel that I feel no hesitation in discussing in this Howe Lecture the subject of "Slag Control." In the present era of close specification, the drive for uniformity of product, and the close inspection of the product and of the cost sheet, the utmost efforts must be made to control the steelmaking variables to the best advantage of the steel producer. One of the major variables is the slag in the furnace and its effect upon the composition and quality of the metal. What advantages are to be gained from slag control? In the broad sense the advantages must be tremendous, because the very foundations of good steel melting are based on "shaping up" the slag to a point where, with proper temperature, the heat is ready for the final additions. Every melter works toward these ends through his experience with innumerable heats of steel. The elimination of undesirable constituents such as phosphorus and sulphur is entirely a matter of slag composition and physical nature, a point well known for over half a century. The role played by the slag in assisting in proper heat transfer from roof and flame to the steel has been equally well known. In more recent years there has come the problem of oxygen control in the more accurate gauging of additions for making high-grade rimmed steel for the new strip mills, and in the deoxidizing additions for grain-size control and cleanliness of forging steels, both carbon and alloy. In this problem the oxidizing characteristics of the slag are of prime importance.

Jan 1, 1940

By J. B. Austin

In considering so complex a process as the smelting of iron in the blast furnace, there is obviously no single method of calculating efficiency that gives a complete appraisal of the performance of the furnace in all its several functions; such a comprehensive view as is required to evaluate producing ability and manufacturing costs for a given furnace is obtained only by considering a group of efficiencies, each of which measures the performance of the furnace from a specific point of view. For instance, there is the rate of consumption of coke per ton of iron produced, which is probably the most frequently considered, and is certainly one of the most important of the group; there is the efficiency of recovery of iron charged; and there is the efficiency of utilization of energy, both chemical and thermal, in some respects related to the former two yet in other ways independent of either. In each of these cases, the calculation can be made on the basis of the actual input of material or energy, or it may be based upon a comparison with the minimum amount of material or energy that would be required by a "perfect" furnace; that is, an imaginary ideal furnace analogous to the perfect steam engine used in thermodynamic calculations, when this furnace is operating under optimum conditions. Moreover, the furnace itself can be considered either as an apparatus for smelting iron or, taking a somewhat less common point of view, as a gas producer yielding iron and slag as by-products. Some of these efficiencies are more useful than others, yet all are instructive; for a knowledge of them not only leads to good engineering practice from the standpoint of control but also discloses limits to possible improvement in performance and indicates the lines along which improvement is most likely to be profitable. Estimates of some of these efficiencies have appeared from time to time in the literature, but many of them are open to objection because they are based on data of uncertain accuracy or because they have been calculated without due regard to the thermodynamic principles involved. Moreover, so far as the author is aware, no general survey of the blast furnace comparing its performance in all the aspects mentioned has been made.

Jan 1, 1938

By C. H. Herty

Almost every metallurgist who has given the Howe Memorial Lecture has had a personal contact with the distinguished gentleman to whose honor this hour is devoted. Unfortunately for me, such personal contacts were not possible. However, in the preparation of a thesis on the open-hearth process, one of my earliest tasks was to make a survey of the literature, and it was from Professor Howe's Metallurgy of Iron and Steel that I drew a number of references to previous work which formed the foundation for my reading. In his volume there is such a complete exposition of the then current thought on the subject of slags and on their role in the elimination of phosphorus from steel that I feel no hesitation in discussing in this Howe Lecture the subject of "Slag Control." In the present era of close specification, the drive for uniformity of product, and the close inspection of the product and of the cost sheet, the utmost efforts must be made to control the steelmaking variables to the best advantage of the steel producer. One of the major variables is the slag in the furnace and its effect upon the composition and quality of the metal. What advantages are to be gained from slag control? In the broad sense the advantages must be tremendous, because the very foundations of good steel melting are based on "shaping up" the slag to a point where, with proper temperature, the heat is ready for the final additions. Every melter works toward these ends through his experience with innumerable heats of steel. The elimination of undesirable constituents such as phosphorus and sulphur is entirely a matter of slag composition and physical nature, a point well known for over half a century. The role played by the slag in assisting in proper heat transfer from roof and flame to the steel has been equally well known. In more recent years there has come the problem of oxygen control in the more accurate gauging of additions for making high-grade rimmed steel for the new strip mills, and in the deoxidizing additions for grain-size control and cleanliness of forging steels, both carbon and alloy. In this problem the oxidizing characteristics of the slag are of prime importance.

Jan 1, 1940

By C. Kremer Bain

UNDER present economic conditions the necessity of mechanizing the mines of our country has become a very important problem. More and more mines are looking toward increased or complete mechanization of their operations, so in the writer's opinion it is quite pertinent that some of the associated problems that accompany such a program be pointed out. The following generalization on attempting a comparatively slight change in mining methods at the Southeast Missouri properties of the St. Joseph Lead Co. is an attempt to point out to anyone faced with a mechanization program that much time and C. KREMER BAIN, Member AIME, is Assistant to General Manager, St. Joseph Lead Co., Bonne Terre, Mo. AIME Sun Francisco Meeting, February 1949. TP 2743 A. Discussion (2 copies) may be sent to Transactions AIME before March 31, 1950. Manuscript received Dec. 27, 1948; revision received Oct. 13, 1949. effort can be saved, and many headaches avoided, if company policy can be established whereby everyone in the organization from the top down is desirous of improvement and is working towards the common objective. Any changes in mining methods, machinery, and so on, must entah coordination of all the other phases of mining as they all have to mesh as accurately as a smooth running chain of gears if satisfactory results are to be obtained. The purpose of this paper is to point out some of the problems which :have to be surmounted when any mechanization program is attempted, rather than to go into the mechanical details and actual operating data of the equipment employed. After all, machines have to be adapted to best suit the local conditions, so no general formula can be given that would apply to other properties. Although St. Josepll Lead Co. has been mechani-cally-minded for a number of years, as shown by the fact that over 110 million tons have been loaded mechanically since 1922, any further mechanization or changes always present a problem. When our ore bodies were of great height and area the breaking and loading were developed to a high degree of efficiency according to known standards. But in recent years, when our ore bodies became smaller and more scattered, the amount of tonnage we were able to break was not sufficient to supply our shovels with enough rock to keep them working to capacity. Our first step in attempting to rectify this situation was to develop a technique of moving the shovels to the broken ore in various stopes, which sometimes entailed a move each shift. A shovel is not producing when being moved, so within the last two years we have been endeavoring to devise some means of getting more rock broken in these smaller stopes and it was then that we became interested in jumbo drilling. To illustrate the fact that mechanization is a process of a chain of developments rather than a stroke of genius can best be shown by a general summary of conditions and obstacles which were encountered in our present attempt to establish template drilling of a standardized round. Our first jumbo was more or less the conventional type with two machines mounted on a crossbar. This arrangement proved to be impractical to duplicate satisfactorily the regular routine of slabbing in a more or less radial pattern as carried out by column drilling. One machine was either too close to or too far from the face and there was another disadvantage in that one drillman was frequently delayed while waiting for his partner to bottom a hole. Our next step was to eliminate the crossbar so the machines could operate independently of each other, but we still encountered the same objections mentioned above except that one drillman was free to drill three holes instead of one in a vertical plane independently of his partner. Time studies while trying to adapt the jumbo to the regular slabbing practice as accomplished by column drilling, revealed that twice as much time was spent in maneuvering the jumbo into position and aligning the holes as was consumed in drilling.

Jan 1, 1951

By C. Kremer Bain

UNDER present economic conditions the necessity of mechanizing the mines of our country has become a very important problem. More and more mines are looking toward increased or complete mechanization of their operations, so in the writer's opinion it is quite pertinent that some of the associated problems that accompany such a program be pointed out. The following generalization on attempting a comparatively slight change in mining methods at the Southeast Missouri properties of the St. Joseph Lead Co. is an attempt to point out to anyone faced with a mechanization program that much time and C. KREMER BAIN, Member AIME, is Assistant to General Manager, St. Joseph Lead Co., Bonne Terre, Mo. AIME Sun Francisco Meeting, February 1949. TP 2743 A. Discussion (2 copies) may be sent to Transactions AIME before March 31, 1950. Manuscript received Dec. 27, 1948; revision received Oct. 13, 1949. effort can be saved, and many headaches avoided, if company policy can be established whereby everyone in the organization from the top down is desirous of improvement and is working towards the common objective. Any changes in mining methods, machinery, and so on, must entah coordination of all the other phases of mining as they all have to mesh as accurately as a smooth running chain of gears if satisfactory results are to be obtained. The purpose of this paper is to point out some of the problems which :have to be surmounted when any mechanization program is attempted, rather than to go into the mechanical details and actual operating data of the equipment employed. After all, machines have to be adapted to best suit the local conditions, so no general formula can be given that would apply to other properties. Although St. Josepll Lead Co. has been mechani-cally-minded for a number of years, as shown by the fact that over 110 million tons have been loaded mechanically since 1922, any further mechanization or changes always present a problem. When our ore bodies were of great height and area the breaking and loading were developed to a high degree of efficiency according to known standards. But in recent years, when our ore bodies became smaller and more scattered, the amount of tonnage we were able to break was not sufficient to supply our shovels with enough rock to keep them working to capacity. Our first step in attempting to rectify this situation was to develop a technique of moving the shovels to the broken ore in various stopes, which sometimes entailed a move each shift. A shovel is not producing when being moved, so within the last two years we have been endeavoring to devise some means of getting more rock broken in these smaller stopes and it was then that we became interested in jumbo drilling. To illustrate the fact that mechanization is a process of a chain of developments rather than a stroke of genius can best be shown by a general summary of conditions and obstacles which were encountered in our present attempt to establish template drilling of a standardized round. Our first jumbo was more or less the conventional type with two machines mounted on a crossbar. This arrangement proved to be impractical to duplicate satisfactorily the regular routine of slabbing in a more or less radial pattern as carried out by column drilling. One machine was either too close to or too far from the face and there was another disadvantage in that one drillman was frequently delayed while waiting for his partner to bottom a hole. Our next step was to eliminate the crossbar so the machines could operate independently of each other, but we still encountered the same objections mentioned above except that one drillman was free to drill three holes instead of one in a vertical plane independently of his partner. Time studies while trying to adapt the jumbo to the regular slabbing practice as accomplished by column drilling, revealed that twice as much time was spent in maneuvering the jumbo into position and aligning the holes as was consumed in drilling.

Jan 1, 1951

By R. J. Tailleur, M. Rosenberg

Oil well drilling muds prepared with lubricating aids such as oil, graphite or mica will not produce a sufficiently strong protective lubricant film for the bit bearing surfaces under high load conditions encountered in drilling operations. Consequently, the damage to the bearing surfaces resulting from the absence of such a film frequently results in a shortening of the drill bit life. Several different types of extreme pressure lubricating additives for use in muds have been developed. These arlrlitives are capable of providing a protective lubricating film for bearing surfaces subjected to high load pressures. A modified version of the Timken lubricant tester, an instrument commonly used for testing the extreme pressure lubricating properties of oils, is used for measuring and controlling the lubricating qualities of the mud. Comparison tests made in the laboratory with 55/8-in. tricone bits drilling on steel plates immersed in extreme pressure lubricating muds and conventional muds showed that the bearing life of those bits tested in the lrrbricating mud was three to four times greater than obtained with conventional muds. Drilling tests made with extreme pressure lubricating muds in West Texas increased over-all bit life three to fourfold, reduced drilling torque and wear on drill pipe and drill collars. INTRODUCTION Roller bit cones contain roller, ball and journal-type bearings that are subjected to very heavy loading during drilling operations in which the only lubricant available for these bearings is either water or drilling mud. These bearings must be able to operate satisfac- torily in order for the cutting structures on the surface of the cones to be fully utilized. Frequently, the bearings wear to the point that the cones freeze and the bit must be pulled before the cutting structures on the cones become worn. In some instances the bearings continue to turn with severe wear but the cones, which are held on the bit by the bearings, drop off; and this causes an expensive fishing job. In other instances the bearings wear to the point that the cones pinch in causing an undergauge hole and delays to ream the hole. The advantage of increasing bit bearing life is self-evident. Because of inability to control the internal wear of bits while drilling, it was felt that improvement of the lubricating qualities of the circulating mud would be helpful. However, the often-discussed lubricating property attributed to muds has been a rather vague and intangible one. The literature has implied that the oil-emulsion muds are more effective lubricants than non-emulsion muds. Actually, there has been no direct method of measuring the lubricating property of muds which would indicate that one mud was better than another; there has been no way to determine whether the lubricating property of any mud was adequate. Furthermore, in comparing lubricating properties of muds, two qualities should be considered—the coefficient of friction and the extreme pressure lubricating qualities. For example, graphite can reduce the coefficient of friction, but does not provide a strong enough lubricating film to protect bit bearings subjected to high loads. The primary object of the investigation reported herein was to find a method for prolonging the bearing life of drill bits; and considering the heavy loads used in drilling, it was felt necessary to find both a method of measuring lubricating properties under high load conditions and methods of establishing effective lubrication under these conditions. Extreme pressure lubrication deals with that realm of lubrication where metal surfaces are in rubbing contact with each other under very high pressures. These pressures may be quite high, as for example,

By R. T. Hukki, P. Voutilainen

This paper describes a new apparatus for continuous wet fine-screening. Its preferred size range seems to be from 0.1 to 1 mm. The supercritical trommel screen is a short cylindrical trommel of wedge-bar type construction operated at a speed greater than the calculated theoretical critical speed and at a speed lower than the speed at which particles introduced into it will centrifuge. The paper describes results obtained with the prototype supercritical trommel screen in pilot plant scale. The results point to a high capacity and simultaneously to a high sharpness of screening. Finally, an analysis is presented of the forces acting in screening on a supercritical trommel screen. In the era of high speed, high capacity processing of raw materials the conventional slowly rotating trommel screen is often considered a relic from the times passed. A typical trommel screen is the cylindrical trommel rotated about a horizontal or slanting axis at a relatively low speed. Its screening characteristics are well known. Trommel screens of various types of construction, methods of operation, performances and other characteristics have been described in detail by Taggart.1 The theoretical critical speed of a trommel screen is defined by the same well known equation as that applied for grinding mills: where ncritical = the numerical value of the theoretical critical speed in rpm, D 1 = the inside diameter of the trommel in feet, and D2 = the inside diameter of the trommel in meters. ncritical corresponds also to the centrifuging speed provided that the coefficient of friction f between the trommel surface and the outer layer of the charge is = 1.0. In a general case: From Eq. 2 it is seen that in all cases where f < 1.0 the centrifuging speed of the trommel is greater than the theoretical critical speed. The supercritical trommel screen concerns screening operations within that speed range which is between the theoretical critical speed defined by Eq. 1 and the centrifuging speed defined by Eq. 2, under conditions such that the coefficient of friction f<1.0. It is reported by Taggartl that the optimum speed of a conventional cylindrical trommel screen 36 in. in diam was experimentally found to be about 16 rpm. From Eq. 1, the critical speed of this trommel is 44.2 tpm. The indicated optimum speed corresponds to (16/44.2) x 100% = 36.2% of the theoretical critical speed. The optimum speed range based on information available seems to vary from 33% up to 45% of the theoretical critical value. The trommel screen operated at a supercritical speed: operates at a speed greater than the calculated theoretical critical speed; operates at a speed lower than the speed at which the charge introduced into it will centrifuge; operates within the supercritical speed range in such a way that the coarse fraction of the charge must slide in respect to the inside surface of the trommel; the outer layer of the said fraction next to the screen tends to proceed in the same direction as any selected point on the trommel surface, but now at a lower speed, and indeed at a subcritical speed; allows to a certain degree adjustment of the maximum determining particle size x of the fine product simply by a variation of the speed of the trommel within the supercritical speed range. With increasing trommel speed, finer and finer material only will get the opportunity to find its way into the fine product while the screen opening remains constant. In conventional practice, the low speed trommel is generally used for sizing of coarse and medium coarse material, but seldom for fine screening. The characteristic feature of the product passed through the conventional trommel is that the determining size x of the biggest particle is barely smaller than the nominal size of screen opening. The supercritical trommel screen, on the other hand, is best suited for sizing of relatively fine material. Furthermore, the characteristic determining size x of the biggest particle in the fine product can be substantially smaller than the nominal width of the screen opening or slot. In the trommel screen best suited for the applications

Jan 1, 1965

By G. Wakefield, A. H. Daane, D. H. Dennison, F. H. Spedding

Preparation of pure scandium metal was accomplished by calcium reduction of the fluoride by two methods; a low-temperatzdre alloy process and direct reduction with subsequent distillation of the product. The following properties were determined: melting point: 1181OK; boiling point (calculated): 3000°K; lattice constants at 298°K (hexagonal lattice): a = 3.308 * 0.001 A, c = 5.267 * 0.003A; calculated density at 298°K, g per cm3: 2,990 + 0.007; electrical resistivity, ohm-cm: 299°K, 66.6 ± 0.2 x 10 -6; 373oK, 77.4 * 0.2 x 10 -6; thermal coefficient at 299°K, ohm-cm per deg: 5.4 X x; heat of sublimation at 298°K, kcal pel- mole: 80.79. The vapor pressure was determined as a function of temperature between 1505o and 1748°K, with the data fitted to a straight line shielding the equation: Log Pmm = -1.718 X 104/ToK + 8.298. SCANDIUM, element number 21, was first discovered by Nilson in 1879 and was recognized as the Ekaboron as predicted by Mendeleff. As it is in group III of the periodic table, the general properties are a little like aluminum and also resemble quite closely the properties of yttrium and the rare-earth metals, in both the metallic and ionic form. Although the earth&apos;s crust contains approximately 5 ppm of scandium (the element is as abundant as arsenic and twice as abundant as boron) it generally occurs so widely distributed that it has earned the reputation of being very rare. The one exception to this is the mineral thortveitite, which has been found in Madagascar (20 pct Sc2O3) and in Norway (35 pct Sc2O3). Scandium also occurs in small but distinct amounts in uranium and rare-earth ores; the recent larger scale processing of these materials has made some scandium available from these sources. As with other naturally-occurring monoisotopic elements (except Be), scandium contains an odd number of protons and an even number of neutrons. Scandium metal was first prepared by Fischer and coworkers1 in 1937 by electrolysis of scandium chloride in a molten eutectic mixture of lithium and potassium chlorides, using molten zinc as a cathode and collector of the scandium metal produced. The zinc was removed from the Zn-2 pct Sc alloy by vacuum distillation, leaving a product reported to be 94 to 98 pct Sc, with the main impurities being iron and silicon. They reported a melting point of 1400° C for this material. Scandium has also been prepared by the reduction of scandium chloride with potassium metal in a glass apparatus by Bommer and Hohmann in 1941,&apos; resulting in a mixture of metal and potassium chloride; these workers did not isolate the metal proper, but the X-ray diffraction of the slag-metal mixture showed it to be hexagonal with a = 3.30A, c = 5.45A. petru3, 4 and coworkers have recently reported the preparation of the metal in a compact form by the reduction of either ScF3 or ScC13 with calcium metal and subsequent distillation of the product. This process probably yielded a metal of high purity, but they list no chemical analysis nor do they list any of the properties of their product. Previous related work in this Laboratory has been concerned with the production of yttrium and the rare-earth metals and the determination of their physical properties. Because of its similarity to these metals, scandium is being included in this study. PREPARATION OF SCANDIUM METAL The preparation of yttrium and the rare-earth metals may be accomplished by reduction of their fluorides with calcium metal in tantalum crucibles.5 This process leads to the introduction of tantalum (up to 0.5 pct) as an impurity in the higher melting rare earths, but since the tantalum occurs as dendrites, uncombined with the rare-earth metals, its presence is not objectionable in some cases. The preparation of scandium metal in this manner, however, was found to yield a product containing 2 to 5 pct Ta. To obtain a purer product, the following two methods were developed for the reduction of scandium fluoride with calcium metal: i) a low-temperature process utilizing zinc to form a low

Jan 1, 1961

By F. N. Rhines

STUDIES upon the sintering of metal powders, in the solid state, have led to the proposal that the surface energy of the powder particles provides the driving force that causes points of contact between pairs of particles to grow into broad welds which isolate the residual vacant space into pores that tend to spheroidize and gradually to diminish in total volume.&apos; Investigators differ with regard to the mechanism of the movement of the metal, under the influence of surface energy, to accomplish these changes. One school asserts that there is a mass movement of the metal, referred to as a "viscous flow," while the other school prefers to view the movement as a self diffusion process, wherein individual atoms are, transferred without disturbance of the basic pattern of the crystal lattice. Extensive experimental studies upon the sintering of copper, conducted recently by A. J. Shaler,2 have been in- terpreted by their author as support for the viscous flow mechanism of transport, the theory of which was developed originally by J. Frenkel.3 Duplicating a portion of this work with minor changes, G. C. Kuczynski4 is led to the alternate view, namely, that the initial stages of sintering, at least, proceed as a self-diffusion process. Both of these investigations were designed to deal with an isolated unit of sintering, i.e., with the shrinkage of a single pore, or with the growth of a single point weld. It remains to ascertain the behavior of a typical metal powder compact composed of a large number of particles of varying size and sintering to a body with a multiplicity of pores. The observation of density changes alone during sintering is not sufficient in such a case; it is essential to know how the internal geometry of the compact changes. This has been the object of the present investigation, the results of which are used to support the self-diffusion mechanism of sintering. The present studies consist in the measurement of the number of pores as a function of size and time at temperature during the sintering of a copper compact made from a commercial copper powder lightly pressed and sintered in several different atmospheres. A brief survey was made also of the change in shape of the pores, under the influence of the same variables. All of this was done by direct observation with the microscope. Densities were measured on the same sample. It is found that, while the compact is exhibiting an overall shrink-

Jan 1, 1951

By F. H. Wilson, E. W. Palmer

G. L. Bailey (British Non-Ferrous Metals Research Association, London, England)—I was glad to see this further work on the structure and properties of the Cu-Ni-Fe alloys of low nickel content in which we have been so interested in the United Kingdom since before the war." The authors&apos; data on the variation in solubility of iron in both 5 and 10 pct Ni alloys with temperature is based on more detailed observations than we have made but is generally in line with our own work. The difficulty in these matters is in the identification of the structures obtained. The precipitation of the second phase which we presume to be the a&apos; solid solution, richer in nickel and iron, from the a solution with which it is in equilibrium occurs in such a fine state of division that its resolution by ordinary micro-graphic methods is impossible in the early stages. We have published some electron micrographs which illustrate the effects observed more clearly but we agree with the authors when they say that dark staining characteristics when the alloys are subjected to sea-water corrosion are more sensitive in detecting the presence of the a&apos; phase than is the microscope. After taking this point into consideration, however, I confess to some difficulty in understanding Fig. 4. I can only assume that the precipitates visible at such a low magnification as 150 diam in these relatively coarse forms are produced from iron-rich areas of the initial solid solution due to inadequate homogenization. If this is so I find it difficult to accept the authors&apos; contention that such local variations in iron concentration as are capable of giving the heavy precipitates shown in Fig. 4 do not in fact materially affect the solvus surfaces of their equilibrium diagrams. I share the authors&apos; enthusiasm about the resistance to corrosion of these alloys by seawater but I am not fully in agreement with them on the vexing question of the best iron content for these alloys. In Fig. 3 of ref. 8, we give many results showing that the resistance of these alloys to impingement attack in the Jet Test increases as the iron content rises to 2 pct. With higher iron contents pitting at shielded areas is likely to occur. Admittedly the addition of 0.75 pct Fe produces a large improvement in corrosion resistance compared with a pure 90/10 Cu-Ni alloy, but the further improvement on raising the iron to 2 pct is substantial. We recommend from 1.5 to 2 pct Fe as the desirable range from the point of view of corrosion resistance. While it is true that British practice generally uses a hard tube, the corrosion resistance of the 10 pct Ni alloys has in our work been little affected by the structural condition. Although the annealed alloys blacken in seawater, this effect seems to be superficial and not to be accompanied by any real decrease in

Jan 1, 1953

By H. l. Burghoff, C. H. Mathewson

THE study of the creep of metals under conditions of prolonged loading has received the attention of many investigators for several years and almost innumerable papers have been published on the various aspects of the subject. As it appeared that much could still be learned from a study of single crystals, the present work was carried out to study the effects of temperature and conditions of loading upon the properties and deformation in tension of single crystals of alpha brass containing about 70 per cent copper and 30 per cent zinc. In particular, it was hoped to obtain information from tests below and above the recrystallization temperature of the material, so that properties such as elastic limit, yield point or critical stress, and manner of deformation might be compared for tensile tests at an ordinary loading rate and for prolonged. loading. Accordingly, short-time tensile tests and creep tests were made at room temperature, 300º, 500° and 700°F. The two latter temperatures are above the lowest possible recrystallization temperature of polycrystalline 70-30 brass. PREVIOUS WORK Clarke and White1 have made creep tests of some copper-zinc alloys, including 70-30 brass, and copper-zinc-tin alloys at temperatures both below and above the recrystallization temperature of the materials considered. Hanson and Wheeler have studied the flow and fracture of single crystals of aluminum for short-time and prolonged tensile loading over a range of temperature extending from room temperature to 400°F., their experiments being made without consideration of the orientations of the test specimens. Extensive creep and fracture tests on single crystals of lead at room temperature have been made by Betty3 and by Baker, Betty & Moore.4 Results of the last-named investigation were published while the present work was in progress. Millers examined the elastic limit of zinc single crystals at and above room temperature by means of creep tests, while Miller and Milligan6 reported the results of tests designed to show the influence of temperature on elastic limit of single crystals of aluminum, silver and zinc. The behavior, of iron crystals under static tensile loading at room temperature was reported by Gensamer and Mehl7 while the present investigation was in progress. Their specimens exhibited a well-defined yield point, below which no appreciable creep could be detected. The manner of yielding proved interesting, as the shape of the creep-time curve for the iron crystals differed from the common type of creep curves. Elongation did not begin immediately, or at least was initially very slow. The rate of elongation then increased continuously and finally decreased to zero. This S-shaped type of elongation-time

Jan 1, 1941

By F. H. Callaway, W. O. Keller

The various theories as to the well spacing-recovery relationship are reviewed in considerable detail and these theories analyzed in terms of their consistency with modern reservoir engineering concepts. It is concluded that the well spacing problem must be analyzed in terms of recovery efficiency and that a positive answer to the relation between well density and recovery efficiency is not available from direct comparisons of the production histories of wells and fields. The results of an engineering analysis designed to permit approximate calculation of recovery efficiencies as a function of well spacing in a depletion type reservoir from basic reservoir data is presented. Results of this type analysis indicate that the effect of well spacing on recovery efficiency in depletion type reservoirs can be expected to be very small. Limitations of this approach are pointed out, particularly with respect to its application in lenticular reservoirs. Testing techniques are outlined which should indicate whether or not a reservoir is continuous between wells and whether or not satisfactory drainage is being obtained with present spacings. A mass of data of this type indicates continuity to exist in most fields. INTRODUCTION The purpose of this paper is to review critically the engineering aspects of the well spacing problem, both from the standpoint of certain concepts and from the standpoint of reservoir mechanics. The well spacing problem is primarily an economic problem in which the optimum well density for a particular field is that density which will yield the greatest oil recovery consistent with justifiable development costs. The well spacing answer in terms of economic conditions, however, is extremely sensitive to the variation in recovery efficiency with well density. The variation in recovery efficiency with &apos;References given at end of paper. Manuscript received at the office of the Petroleum Branch October 2, 1949. Paper presented at the Petroleum Branch Meeting in San Antonio. Texas, October 5-7. 1949. well density is properly an engineering problem. Different opinions as to the correct answer to this engineering problem is the basis for most of the wide difference in opinion among various members of the industry as to optimum well spacing. This paper will be confined to the engineering problem of the relation between well density and ultimate oil recovery; economic considerations necessary for the evaluation of optimum well density for any particular field will not be discussed. The paper can be logically divided into two parts. The first part deals with a critical examination of the background and logic of the Cutler Rule and of similar studies by other authors and of related well spacing concepts. It is indicated that the variations in recoveries with well density* observed by Cutler and. others can be logically attributed to regional migration. Theoretical justification of the Cutler type relation wherein observed variations in recovery with well density in the same field is attributed to variations in recovery effiiency, in terms of energy relations, is refuted. The second part consists of a review of concepts of reservoir mechanics with regard to the well density-recovery relation. It is indicated that little variation of recovery efficiency with well density can be expected in a depletion type reservoir, unless lenticular conditions prevent communication between wells. The significance of field test data with regard to the existence or non-existence of lenticular conditions is pointed out. THE CUTLER RULE The first published article concerning the engineering aspects of the well spacing problem to receive wide attention was the work of W. W. Cutler&apos; of the U. S. Bureau of Mines, published in 1924. In a study of decline curves from a large *The expression "well density" as utilized herein refers to the number of acres attributed to each well in a uniform well pattern, and is expressed in acres per well. The term "well spacing" Is utilized to denote the average distance between adjacent wells in a uniform well pattern. †Although the Cutler rule is treated critically in this discussion the authors intend no personal criticism of W. W. Cutler or of his hark The currently accepted concepts of reservoir mechanics were no": existent at the time of Cutler&apos;s work, as were even the moat basic tools (such as the bottom hole pressure bomb) for observing reservoir behavior.

Jan 1, 1950

By C. M. Wayman, R. Bullough

The rediffraction of Bragg diffracted beams by differently oriented regions (such as twins) of a crystal may give rise to "extra" reflections or reciprocal lattice points. These two papers are concerned with predicting these additional reflections which result from twin related regions of a lattice. Analysis is made for {111}fcc twins, (112)bcc twins, and {hkil}hcp twins. It is first required, knowing the specific variant of the twinning plane in each case, to predict the positions of the twin reflections relative to the matrix reciprocal lattice. Once this is done, the positions of the "extra" multiply diffracted reflections may be deduced. Part I is devoted to establishing "selection ru1es" for twinning, i.e., the necessary and sufficient conditions for the existence of twinned reciprocal lattice points. 1. INTRODUCTION. Transmission electron diffraction patterns are frequently complicated by multiply diffracted beams. Pashley and stowell1 have recently demonstrated that certain extra reflections in evapo- rated films of gold result from the rediffraction of matrix Bragg diffracted beams by (111) microtwins in the gold. It was previously (and erroneously) suggested 2,3 that observed "irrational" reflections in fine-grained gold were due to the presence of some hcp gold. A similar situation exists, apparently, for some bcc materials; fine (112) twins in bcc martensite in Fe-Ni alloys4 give rise to extra reflections. There are many other examples. The number of transmission electron microscopic investigations is continually increasing, and because of the importance of double (and multiple) diffraction in the interpretation of diffraction patterns, it was judged that a detailed elaboration of the principles involved is desirable, as well as the extension of these principles in reasonably closed form to other crystal structures, particularly bcc and hcp. The present analysis considers double diffraction caused by (111) twins in fcc metals, (112) twins in bcc metals, and {hkil} = {hkl) twins in hcp metals. For each case of twinning, the various possible (variants of) twins give rise to a set of interpenetrating reciprocal lattices. The relative spatial arrangements of these reciprocal lattices can be deduced (Part I) and are expressed in terms of simple "selection rules". The resulting sets of interpenetrating reciprocal lattices are then analyzed for possible doubly diffracted reflections (Part II). The notation used, and some important formulas are given in Appendices I and 11.

Jan 1, 1967

By Robin O. Williams

The increase in internal energy as the result of deformation has been measured for lead, aluminum, silver, nickel, iron, and zirconium by using rapid, adiabatic compression. The stored energy increase is roughly Proportional to the strain; the propor-tionality constant increases rapidly with increasing melting point. The fraction of the mechanical energy which is stored increases more slowly, since the strength of the metals also increases with melting point. The values of the stored energy are considered accurate to about 10 pet. The present values appear about 50 pet larger than the more reliable published results where comparisons are possible. It is possible that this difference is due to the high strain rate used in this investigation. Immediately after deformation all these metals release energy at a rate roughly proportional to (time)-&apos;. This release is considered to be associated with dislocation motion but in aluminum (and copper) some additional process seems to be present. This release can represent 20 pet or more of the stored energy. WHEN pure metals are plastically deformed, most of the mechanical energy is converted into heat. The energy remaining within the metal is significant in that it is the energy of the disorder produced and thus detailed knowledge of this energy is a powerful tool in understanding the nature of deformational disorder. While much effort has been expended on this problem, the amount of information available is limited. The situation as of 1958 has been carefully reviewed by Titchener and ever.&apos; The present results have been obtained by a new experimental approach to this problem. The method necessitates high-strain rates which make comparisons with published results less certain, but a high-strain rate is an advantage in that the energy release immediately after deformation can be followed. EXPERIMENTAL PROCEDURE In the experimental method used, the internal (stored) energy is given as the difference between the mechanical work used in deforming the sample and the heat which is released (the first law of thermodynamics). The work is supplied by two identical hammers swinging freely from a fixed height, the available energy being the product of the mass, the gravitational constant, and the distance through which the center of gravity moves. The initial temperature rise of the sample represents the heat produced by the deformation. The sample temperature is determined by a small thermocouple embedded in and supporting the sample. This process can be repeated over and over to produce increased strains. Most samples are run through about five cycles to a total strain of around 0.7. Further details are covered elsewhere. The determination of the heat is dependent upon the sample weight, its specific heat, the rise in temperature, and any gains or losses to the surroundings. One is dependent on published results for specific heals (the values were taken from a collection).3 The values must be accurate to about 0.1 pet in order that they not affect the results. The best values thus do not contribute to the uncertainty, but this is probably not always the case. The accuracy of the temperature rise is limited primarily by knowledge of the thermocouple characteristics over short temperature intervals, but careful calibration eliminates this as an important factor. One can calculate readily the heat flow between the sample and hammers if the time of contact and the sample temperature are known and if there were no oil at the interface. Assuming the maximum temperature difference, upper values for this interchange have been calculated (the time of contact is determined from the decrease in sample length) and it may or may not be significant. However, no correction is colnsidered necessary because of the presence of a thin oil film which has a thermal conductivity much less than the metals. Except for the possible uncertainty in specific heat, the heat is considered to be adequately known. The mechitnical losses which are recognized as important are: 1) friction between the sample and the hammer:;, 2) the kinetic energy in the hammer suspension system which may not be entirely usable, 3) the rebound energy of the hammers, and 4) the vibration of the hammer heads. All these have been covered in detail elsewhere2 and only the more significant points are made here. The friction turns out to be small except for soft materials (lead)

Jan 1, 1962

CONTENTS PAGE ZAPFFE, CARL.-Manganiferous Iron Ores of the Cuyuna District, Minnesota. Discussed by A. K. Knickerbocker 1 MCCORMACK, C. P.-Economics of the Cuyuna Manganiferous Iron Ores. Dis-cussed by T. L. Joseph, J. Wilbur Van Evera, C. P. Perin, T. T. Read, L. E. Ives 4 READ, T. T.-Probable Error in Blast-furnace Records and Calculations Therefrom. Discussed by C. H. Herty, Jr., T. T. Read, T. L. Joseph, Ralph H. Sweetser 8 SCHWARTZ, H. A. and HIRD, (Mrs.) ANNA NICHOLSON.-Chemical Equilibria During Solidification and Cooling of White Cast Iron. Discussed by N. B. Pilling, Ralph H. Sweetser, H. M. Boylston, Albert Sauveur 10 HERTY, C. H., JR., BELYEA, A. R., BURKHART, E. H., and MILLER, C. C.-Some Factors Affecting the Elimination of Sulfur in the Basic Open-hearth Process. Discussed by Henry D. Hibbard, L. F. Reinartz,. C. H. Herty, Jr., Ancel St. John, A. L. Feild, C. R. Hayward, Ralph H. Sweetser, C. D. King, Haakon Styri, George A. Orrok 12 HIBBARD, HENRY D.-Finishing Melting Temperatures of Simple Ingot Steels. Discussed by Haakon Styri, George V. Luerssen, A. G. Zimermann, A. L. Feild, George A. Orrok, Albert Sauveur, R. F. Harrington, Henry D. Hibbard, I. A. Billiar, William J. Priestley, H. W. Gillett, W. P. Barba, Jerome Strauss, Harry H. Smith, H. LeChatelier, L. F. Reinartz 19 HERTY, C. H., JR., and TRUE, O. S.-The Reaction between Manganese and Iron Sulfide. Discussed by A. L. Field, H. S. Rawdon, C. H. Herty, Jr., T. L. Joseph, Haakon Styri 37 KAMURA, HEIHACHi.-Reduction of Iron Ores by Carbon Monoxide. Discussed by T. L. Joseph, R. Franchot, Ralph H. Sweetser, C. H. Herty, Jr 43 JOSEPH, T. L.-Effect of Sulfur on Blast-furnace Process. Discussed by R. Franchot, C. A. Meissner, T. L. Joseph, C. H. Herty, Jr., Ralph H. Sweetser, I. E. Waechter, F. N. Speller, T. T. Read 45 GOOSTRAY, JOB, HARRINGTON, R. F., and HOSMER, M. A.-Brief History of Metallurgical Practice in Cannon-making with Particular Reference to the Cast-iron Gun. Discussed by A. G. Zimermann, Geo. A. Orrok, Chas. Me-Knight, Jr., F. Brauer 51 Manganiferous Iron Ores of the Cuyuna District, Minnesota Discussion of the paper of CARL ZAPFFE, presented at the New York Meeting, February, 1925, and issued, as Paper No. 1390-I, with MINING AND METALLURGY, December, 1924. A. K. KNICKERBOCKER,* Virginia, Minn. (written discussion).¬The author makes a broad distinction between the "black" ores (the

Jan 6, 1925

By H. I. Meyer, D. F. Searcy

INTRODUCTION The analysls of our previous paper&apos; on the behavior at two immiscible fluids separated by gravity into two dlstinct saturated zones in the porous medium was shown to be theoretically valid only if one of the two fluids was immobile. The practical problems associated with flow of both phases have so far been impossible of solution by these analytic methods. We, therefore, decided to resort to a simulator study to answer the following pertinent questions: 1. If the lighter fluid is produced from a point above the fluid-fluid interface, how long will it take for the heavier fluid to come up to the point where production of both fluids is taking place? 2. After steady-state two-phase production is established, what is the relative production rate of each phase, on what physical variables does this depend, and what are the boundary conditions at the outflow face? 3. A third question was at least partially answered in the course of this investigation: that of the shape of the interface under flow conditions. These questions are of fundamental importance in the fields of hydrology and the reservoir mechanics of oil and gas production. In order to simplify equipment used and still retain a fair physical representation of these phenomena, it was decided to use a Hele-Shaw type of analogy in which the flow took place between two vertically mounted pieces of plate glass. The advantage of this system is that it eliminates any surface effects between the matrix of the porous medium (e.g. packed sand) and also allows equilibrium conditions to be established more quickly. The principle disadvantage (apart from the obvious one of being one more step removed from the prototype) is that our equipment limited us to two dimensional flow studies. In spite of these limitations answers to the questions were obtained which seem adequate for our purposes. We would like to see more work of this nature done to verify and to improve our conclusions. DESCRIPTION OF EQUIPMENT AND PROCEDURE A drawing of the equipment used in this study is shown in Fig. 1. Fluid flow takes place between the two 36 in. x 12 in. pieces of plate glass held apart at the long edges by two spacers of cellulose acetate sheet (Kodapac IV) which is available in several thicknesses. This sandwich was clamped together by small c-clamps whose stress was distributed by long pieces of 3/8-in. keystock. Accurate spacing was obtained by tightening these clamps as indicated by micrometer measurements on the outside of the glass. At the upstream end of the plates a piece of 6-in. diameter pipe simulated an infinite reservoir, while at the downstream end a 2-in. Lucite cylinder with a small hole near the top of the flow region served to drain the fluid. Sealing was achieved by O-rings, the whole system being tightened by pressure on the Lucite tube provided by set screws (not shown in the drawing). The total head

Jan 1, 1957

By C. C. Nathan

Data are resented on the physical properties of five waxes obtained from fields in Texas and Louisiana in which "parafin" troubles are being experienced. The crude parafin was fractionated into three components, voluble in cold acetone, soluble in boiling acetone, and insoluble in boiling acetone. The acetone insoluble fraction was found to consist essentially of straight chain parafin hydrocarbons in the molecular weight range 525 to 700. Solubilities of the purified high molecular weight parafins were determined in a number of solvents. It was found that in hydrocarbon solvents, including crude oil, solubilities could be calculated satisfactorily by use of ideal solubility relations. In chlorinated, and oxygenated solvents, large deviations from ideal behavior were observed. These deviations could be partially correlated with the internal pressure of the solvent. INTRODUCTION A problem encountered in many producing oil fields is that of "paraffin" deposition. The problem refers to the deposition of material from the crude oil onto tubing, pumping rods, flow lines, or other material contacted by the crude. This problem has been recognized for nearly a hundred years, and numerous investigations have been reported on its causes and prevention or alleviation. One of the more comprehensive of such investigations was published by Reistle1 in 1932. A few of the salient findings of his report are briefly as follows: The term "paraffin" as used to describe this problem refers to the deposit of carbonaceous material which is not soluble or dispersible by the crude oil under the conditions where deposition occurs. The "paraffin" normally consists of high molecular weight paraffin hydrocarbons, both straight chain and branched, resins and asphaltic materials of undetermined nature, occluded oil and water, and possibly sand. In consistency, the deposit may vary from a soft, sticky material, to one which is hard and brittle. Deposits are usually black, although lighter colors are sometimes observed. Under the conditions of temperature, pressure, and crude oil composition occurring in the underground reservoir, the paraffin is in suspension or solution in the crude. As the oil flows to the surface, there is generally a reduction of temperature, pressure, and the amount of dissolved gases contained in the oil. Reduction of temperature and gas break-out were shown by Reistle to be factors causing reduced solubility of the paraffin in the crude. Thus, as the crude containing paraffin rises to the surface and flows to storage tanks at atmospheric temperature, the solubility of the paraffin may be exceeded. Deposition will begin at the point in the system where the temperature of the system falls below its cloud point, and continue as long as there is a further drop in the solution power of the crude for the paraffin. The severity of the deposition as well as the location of the bulk of the deposition, i.e., in subsurface or surface equipment, will depend on the amount of paraffin originally in the crude, the manner in which pressure and temperature of the crude

Jan 1, 1956

By J. M. Seeman, R. A. Dodd

If some solution-quenched supersaturated aluminum solid solutions, e.g.., Al(Cu), are plastically deformed at room temperature and then aged at 200oC, the hardness may first decrease before increasing in the usual manner &apos; A similar transient softening is observed, even in the absence of plastic deformation, when a thin foil or small-diameter wire Al(Cu) specimen is rapidly quenched from the solution-treatment temperature and then aged.&apos; Also, some solution-quenched and neutron-irradiated alloys undergo an initial hardness decrease during subsequent aging.3 The usual explanation of the transient softening in the above examples involves the effect of vacancies introduced by plastic deformation, rapid quenching, and neutron irradiation, respectively However, the mechanism of softening is not unequivo-cably established. In the first-noted case, Gane and parkins&apos; observed that the softening was approximately proportional to the difference in the atomic diameters of solute and solvent, and it was argued that, if a large relative difference in atomic diameter promoted vacancy-assisted room-temperature solute diffusion to dislocations, dislocation climb occurring during subsequent aging at 200°C could cause transient softening. Some substantiation of this theory was offered by the additional observation that discontinuous yielding of solution-quenched polycrystalline Al(Cu) tensile specimens was suppressed by interrupting the test for a short aging treatment at 200°C. Of course, reversion (resolution of GPI) at 200°C would also cause softening, and Sil-cock4 expressed the opinion that the softening in the case of Al(Cu) must be partly associated with reversion. Also, Hirsch5 commented on the possibility that, if jogs cause hardening, an anneal at 200°C should straighten the jogged dislocations and result in softening. However, parkins&apos; has re-expressed his belief that these mechanisms are not entirely consistent with the observed serrated stress-strain curves. Experimental. New data has now been obtained for Al(Cu), Al(Ge), Al(Mg), and Al(Zn) primary solid-solution alloys. These alloys were prepared from metals exceeding 99.99 pct purity, and specimens 4 by 4 in. diam were solution-treated, quenched, deformed 10 pct in compression at room temperature, and aged at 200&apos;C in a cottonseed oil bath for various times. Generally, these operations could not be carried out in rapid succession, so the alloys were stored in a freezer between treatments to minimize aging. The variation in hardness with aging time, Figs. 1 to 4, was determined by microhardness testing with a 3.0-kg load. At least five readings were averaged to obtain each data point, and all measurements were taken about the center circumference of each cylinder (region of maximum deformation). Each specimen was used to obtain only one data point, i.e., specimens were not replaced in the aging bath after measurements were made. In

Jan 1, 1968

By R. A. Burmeister, P. E. Greene

Two methods for the synthesis and growth of single crystals of B6 P are described: a solution-growth process employing nickel as the solvent, and a vapor-growth process employing BBr3 and pH3 as the reac-tants. Relevant portions of the Ni-B-P phase diagram have been examined and liquidus data are presented for an isobaric section at an equivalent P2 pressure of 3.8 Torr, and an isothertnal section at 1300°C. Solution-growth techniques are described and the purity and crystalline perfection of the resulting material is discussed. Epitaxial growth of BeP on &P substrates has been obtained using the vapor-phase system. Evidence is presented which supports the assignment of the stoichioknetry B6P to boron sub-plwsphide. THE B-P system differs from other III-V systems in that it contains two distinct compounds. The existence of the monophosphide (BP) has been known for some time,&apos; whereas the subphosphide (B6P) was reported only recently.&apos; Both of these compounds are large bandgap semiconductors (Eg = 2.0 ev for BP~ and 3.3 ev for B6P4), and are therefore of interest for optoelectronic applications. The crystal structure of B6P is quite different from those of most semiconductors, being derived from that of a-rhombohedral boron by the incorporation of the two phosphorus atoms in the intericosahedral sites of the a-boron unit cell?76 B6P also exhibits a number of unusual characteristics, including a high degree of chemical inertness, hardness, and high-temperature stability. No information concerning other physical properties is available in the literature. The present study is part of a broader investigation of the preparation and properties of B6P. This paper considers methods of growing single crystals of B6P of suitable size and quality for physical-property measurements. A detailed discussion of the electrical and optical properties of B6P will be given elsewhere.&apos; GENERAL CONSIDERATIONS The method first used to synthesize B6P was the disproportionation of BP&apos; according to the reaction The equilibrium P2 pressures corresponding to this reaction were also determined .&apos;" It is therefore possible, in principle, to apply several of the reactions reported for the synthesis of BP to the synthesis of B6P merely by selecting lower phosphorus pressures or higher temperatures, in accordance with the equilibrium data. Other techniques for the direct synthesis of microcry stalline B8P have also been reported.1°

Jan 1, 1968