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By C. B. Gillson, Henry Fay

For several years past, investigations on the chemistry of tellurium have been carried on in the laboratory of this institution. The methods of preparation of pure telluriumf and the estimation of tellurium‡ have been studied, and an attempt to determine the atomic weight of tellurium is now in progress. All these problems had been investigated, however, along purely theoretical lines; and it was thought desirable to study the more practical application of the metal, which can now be had in considerable quantities as a waste product in the refining of copper-ores. In its physical and chemical properties tellurium is very similar to antimony, and it was thought

Jan 1, 1902

By A. H. Geisler, F. Keller

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947

By F. Keller, A. H. Geisler

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947

By F. Keller, A. H. Geisler

ALTHOUGH the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstätten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged alloys.1 The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will suffice to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. PREPARATION OF SPECIMENS The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously.1,2 Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen. The specimen is polished according to the usual procedure for microscopic examination.3 The specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended. Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens. The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet polishing operation are generally used, but frequently the as-rolled surface is suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1946

By Robert K. Warner

Is an accurate measurement of the efficiency of a screen under a given set of operating conditions valuable? If so, what is the efficiency of a screen and how can it be measured? Sizing, especially of the finer sizes of material, has increased in importance in the development of flow sheets as a result of the perfecting of the rapid vibrating screens. More consideration should be given screens in the preparation of ball-mill feed, where they permit the admission of a dryer feed than the classifier. Where possible, the introduction of a screen ahead of the primary ball-mill, and the diverting of ore below, say, 4 mm. to a secondary mill, might result in a greater overall economy because of the thicker feed and the better adjustment of crushing media and mill operation to the reduction demanded. With the present trend back toward a combination of gravity methods and flotation, rather than flotation alone, the accurate, economical sizing possible with the new screens makes fine jigging a method to be considered. W. o. Borcherdtl and John Bland= discuss the screening problem and also the value of close sizing in the concentration of some of the rare-metal ores. If a screen is to be used, it should be selected in competition with others; other things being equal, that screen which makes the cleanest oversize should be preferred. The quality of the screening and the tons handled per dollar together determine the choice and, therefore, both of these must be accurately measured if a correct decision is to be reached. Too frequently in mill design, the capacity has been considered almost to the exclusion of the completeness with which the undersize is separated from the oversize. It is, of course, possible to increase the aperture of the screen, and thus insure the removal of a sufficiently coarse

Jan 1, 1924

By William B. Senseman

FOR reasons well known to mining engineers, wet grinding is quite universal in plants having to do with the extraction of metallic values from crude ores. In the processing of the nonmetallic and industrial minerals, dry grinding is the more common method. The crude materials usually contain less moisture than is required for wet grinding and the products usually are marketed in dry form; most of them as powders. To grind wet, therefore, would entail the addition of water and an expense for drying the product, which is not justified. Furthermore, the material would be a dried cake that would still have to be pulverized or disintegrated before use. For producing fine products, air separators have largely replaced the earlier practice of sizing with screens and bolting reels. Mills in which the air-separating feature is an integral part of the design are now commonplace. Mill designs are many and air systems have developed along various lines, but for the purpose of this discussion, only the fundamental idea need be emphasized the idea of using air for sizing and removing pulverized material from a grinding mill. About 20 years ago, when the use of mills equipped with air separation had become common practice, heated air or gas was introduced to such a system for the removal of moisture. The purpose of this discussion is to outline the developments and trends that have followed this experiment. It is an important development, for mills equipped with air separation are now universally used for pulverizing not only nonmetallic and industrial minerals, but a great variety of other materials. All such mills are essentially the same. Dried material is pulverized, removed by an air stream, trapped in a cyclone collector, and relatively clean air from the cyclone is returned through a fan to the mill. There is no theoretical need for a vent from the system. The practical need is to vent the air that leaks into the system, and, since the cyclone is not 100 per cent efficient as a dust collector, this vented air carries some dust with it. The initial attempt. at drying was made on a system like that described, by the addition of a furnace. The minus pressure within the mill draws hot gas from the furnace. Infiltration air, along with the drying gases and evaporated moisture, is vented as before. The first application was made to a mill used for pulverizing coal. The coal contained very little moisture, so very little drying effect was needed for the success of this experiment. Actually, some calculated efficiencies of over 100 per cent were obtained before due allowance was made for the conversion of mill power into useful heat. When moisture is low,, the heat obtained from the conversion of mill power is an appreciable part of that required. That drying can be effected in the short time interval available in a grinding mill of this type is better understood by visual-

Jan 1, 1945

By William B. Senseman

For reasons well known to mining engineers, wet grinding is quite universal in plants having to do with the extraction of metallic values from crude ores. In the processing of the nonmetallic and industrial minerals, dry grinding is the more common method. The crude materials usually contain less moisture than is required for wet grinding and the products usually are marketed in dry form; most of them as powders. To grind wet, therefore, would entail the addition of water and an expense for drying the product, which is not justified. Furthermore, the material would be a dried cake that would still have to be pulverized or disintegrated before use. For producing fine products, air separators have largely replaced the earlier practice of sizing with screens and bolting reels. Mills in which the air-separating feature is an integral part of the design are now commonplace. Mill designs are many and air systems have developed along various lines, but for the purpose of this discussion, only the fundamental idea need be emphasized— the idea of using air for sizing and removing pulverized material from a grinding mill. About 20 years ago, when the use of mills equipped with air separation had become common practice, heated air or gas was introduced to such a system for the removal of moisture. The purpose of this discussion is to outline the developments and trends that have followed this experiment. It is an important development, for mills equipped with air separation are now universally used for pulverizing not only nonmetallic and industrial minerals, but a great variety of other materials. All such mills are essentially the same. Dried material is pulverized, removed by an air stream, trapped in a cyclone collector, and relatively clean air from the cyclone is returned through a fan to the mill. There is no theoretical need for a vent from the system. The practical need is to vent the air that leaks into the system, and, since the cyclone is not 100 per cent efficient as a dust collector, this vented air carries some dust with it. The initial attempt at drying was made on a system like that described, by the addition of a furnace. The minus pressure within the mill draws hot gas from the furnace. Infiltration air, along with the drying gases and evaporated moisture, is vented as before. The first application was made to a mill used for pulverizing coal. The coal contained very little moisture, so very little drying effect was needed for the success of this experiment. Actually, some calculated efficiencies of over 100 per cent were obtained before due allowance was made for the conversion of mill power into useful heat. When moisture is low, the heat obtained from the conversion of mill power is an appreciable part of that required. That drying can be effected in the short time interval available in a grinding mill of this type is better understood by visual-

Jan 1, 1947

By William B. Senseman

For reasons well known to mining engineers, wet grinding is quite universal in plants having to do with the extraction of metallic values from crude ores. In the processing of the nonmetallic and industrial minerals, dry grinding is the more common method. The crude materials usually contain less moisture than is required for wet grinding and the products usually are marketed in dry form; most of them as powders. To grind wet, therefore, would entail the addition of water and an expense for drying the product, which is not justified. Furthermore, the material would be a dried cake that would still have to be pulverized or disintegrated before use. For producing fine products, air separators have largely replaced the earlier practice of sizing with screens and bolting reels. Mills in which the air-separating feature is an integral part of the design are now commonplace. Mill designs are many and air systems have developed along various lines, but for the purpose of this discussion, only the fundamental idea need be emphasized— the idea of using air for sizing and removing pulverized material from a grinding mill. About 20 years ago, when the use of mills equipped with air separation had become common practice, heated air or gas was introduced to such a system for the removal of moisture. The purpose of this discussion is to outline the developments and trends that have followed this experiment. It is an important development, for mills equipped with air separation are now universally used for pulverizing not only nonmetallic and industrial minerals, but a great variety of other materials. All such mills are essentially the same. Dried material is pulverized, removed by an air stream, trapped in a cyclone collector, and relatively clean air from the cyclone is returned through a fan to the mill. There is no theoretical need for a vent from the system. The practical need is to vent the air that leaks into the system, and, since the cyclone is not 100 per cent efficient as a dust collector, this vented air carries some dust with it. The initial attempt at drying was made on a system like that described, by the addition of a furnace. The minus pressure within the mill draws hot gas from the furnace. Infiltration air, along with the drying gases and evaporated moisture, is vented as before. The first application was made to a mill used for pulverizing coal. The coal contained very little moisture, so very little drying effect was needed for the success of this experiment. Actually, some calculated efficiencies of over 100 per cent were obtained before due allowance was made for the conversion of mill power into useful heat. When moisture is low, the heat obtained from the conversion of mill power is an appreciable part of that required. That drying can be effected in the short time interval available in a grinding mill of this type is better understood by visual-

Jan 1, 1947

By Arthur B. Yates

Diamond drilling has advanced and expanded during the past few yean. Along with this increase there has been a marked trend to rely more and more upon drilling for the outlining of ore for reserve purposes. This is especially true underground, where men have not been available for opening up ore by crosscuts, drifts and raises. During the recent heavy call upon known ore reserves, more drilling has been done for exploration and it has become expedient to drill longer lateral holes from underground and deeper holes both from surface and from exploration headings in the mines. Furthermore, these deeper holes have to be drilled closely enough to warrant calculation of "probable" if not "proven" ore, from the results obtained therefrom. Interpretation of diamond-drill results has become more precise and reliable with the growing knowledge and understanding of the geologic structures that control the geometry of ore distribution, and this has broadened the field of usefulness of the drill. All of this has created a necessity and a demand for more accurate control of the hole as to direction, a more precise and reliable method of surveying for position, and a need for better and more complete core recovery, as well as larger cores, to provide an adequate sample. At depth the control becomes more difficult and, at the same time, more important. Control A close study of drilling in various parts of the world for a period of more than 20 years has brought to light one definite rule, practically invariable; namely, that diamond-drill holes tend to deviate into a position normal to any structure existing in the rocks, such as bedding, schistosity, gneissosity, or even parting or jointing— even if the hole is started at almost any angle other than parallel with the structure. It also appears that the better developed the structure is, the more quickly will the hole get into a position perpendicular to it. It has often been said that there is a tendency for holes to "drift" in the direction of rotation. This is obviously untrue, for in a vertical hole the measure of deviation would depend upon the azimuth chosen as zero, and there is an infinite number of choices. It has been proved. however, that in homogeneous rocks there is a tendency for the hole to corkscrew, and that the direction of the spiral is the same as the direction of rotation. This may account for the belief that holes drift in that direction. Some tests have been made using right-hand and left-hand rods, and these show that no matter what the direction of rotation the hole will swing into a position perpendicular to the structure. Methods of Control The foregoing empirical rule may be used as an indirect method of control. If the prevailing structure is known, it may be advantageous to start the hole as nearly normal to it as possible, for the

Jan 1, 1946

By H. Brandhorst, C. G. Dunn

THE main purpose of the present note is to provide further information on the effect of orientation on strain-induced grain boundary migration in sheet material. A secondary purpose is to draw attention to the presence of a possible (hkl) dependent surface energy driving force, when the two grains of a bicrystal specimen have different (hk2) planes at the gas-metal interface, and to suggest means of eliminating this effect from the strain effect. If two grains A and B of a bicrystal have specific surface energies ? A and ? B respectively, there exists a driving force for grain boundary migration equal to 2(? B - ? A)/t, where t is the thickness of the specimen.' When t is quite small and the residual strain energy densities €A and €B of grains A and B, respectively, adjacent to the boundary are nearly equal, it is possible that the surface effect may be larger than the strain effect. he difference € B - € A gives a driving force per unit area of grain boundary due to an applied strain.)2 However, with increasing t the surface effect decreases while the strain effect presumably remains constant. Therefore, at some sufficiently large value of t, it is possible to ignore surface energy driving forces.* On the other hand, the surface effect is eliminated for all value of t when both grains have the same (hkl) orientation or have identical values of surface energy. Although the previous study provided information on the effect of orientation on strain-induced erain boundary migration,' no orientations with the (100) plane in the plane of the sheet were included. The present paper provides information of this kind. A seed crystal reorientation technique4 was used to prepare a large bicrystal of silicon iron (3 1/4 pct Si) consisting of two (100) grains in the (100) [001] and (100) [Oil] orientations. After a cold rolling strain (7 pct reduction to 3/4 mm final thickness), small specimens were prepared as before2 and then annealed in hydrogen. The boundary migration was such that the grain in the (100) [011] orientation always grew. After overnight anneals at 1100° or 1000°C, none of the initial (100) [001] grain remained. An anneal of 30 min at 950°c, however, provided information on the start of boundary migration. Fig. 1 shows both the initial position (lower line) and the final position (upper curved line) of part of the boundary, as revealed by thermal grooves. In a different area, part of the final boundary was not revealed by thermal grooves; the rate of boundary migration presumably was too high for the growth front to be defined by the time dependent thermal grooving process. In another area there was a vacated intermediate position connected to the initial position of the grain boundary. This indicates that only part of the boundary

Jan 1, 1962

By B. H. Cody

THE Morenci concentrator of the Phelps Dodge Corporation is a part of the project that was completed after five years had been spent in development of the open-pit mine, equipment and process testing in the former No. 6 concentrator, and construction of the reduction works. The reduction works, of which the concentrator is a part, is about a mile and a quarter southeast of Morenci, on the highway that leads up Morenci Canyon. The concentrator has a nominal capacity for the treatment of 45,000 tons of ore daily. The original plant, which has a rated capacity of 25,000 tons of ore daily and is now in its fifth year of operation, began production on Jan. 30, 1942. The addition, to increase the capacity 8o pct, began operation on Dec. 1, 1943. The equipment of the original plant has been described in MINING AND METALLURGY (May 1942). No changes in equipment were recommended for installation in the concentrator extension and only one major change, forced by a shortage of maintenance labor, has since been made. Metallurgical treatment has been altered in some ways as experiments progressed and as labor and economic conditions dictated. No complete description of the operation of the concentrator has been published, so this paper will record such operating and equipment changes as have been necessary, the operating methods that have been developed and the metallurgical results that have been obtained. Descriptions are given in the order of the processes with a flowsheet and an equipment list of each process for convenient reference. The questions asked by engineer visitors have guided the detail in which operation and maintenance are described. During the period Jan. 30, 1942 to Sept. 1, 1946, ore milled has totaled 43,595,253 dry tons, from which 1,643,885 tons of concentrate have been made, containing an indicated production of 783,164,809 lb of copper. The principal results obtained in operation of the concentrator during the years 1942 to 1945, inclusive, and to Sept. 1, 1946 are shown in Table 1. A graphic general flowsheet of the plant is given in Fig I. ORE The Morenci ore that is now being treated is a medium-hard monzonite porphyry in which the principal sulphide minerals are chalcocite and pyrite. A minor amount of covellite is present. Chalcopyrite and bornite have been observed under the microscope. The chalcocite occurs mainly as a coating on pyrite. Some of the coatings are so thick that the pyrite presents the appearance of being an inclusion in chalcocite. Some are less than one micron thick and are barely visible at 500 diameters magnification of a polished cross section. Some chalcocite is present as a dissemination in the gangue. Various oxidized copper minerals are present as a result of oxidation in place but they represent a minor proportion of the copper minerals of the ore body. Oxidation

Jan 1, 1947

By B. H. Cody

The Morenci concentrator of the Phelps Dodge Corporation is a part of the project that was completed after five years had been spent in development of the open-pit mine, equipment and process testing in the former No. 6 concentrator, and construction of the reduction works. The reduction works, of which the concentrator is a part, is about a mile and a quarter southeast of Morenci, on the highway that leads up Morenci Canyon. The concentrator has a nominal capacity for the treatment of 45,000 tons of ore daily. The original plant, which has a rated capacity of 25,000 tons of ore daily and is now in its fifth year of operation, began production on Jan. 30, 1942. The addition, to increase the capacity 80 pct, began operation on Dec. I, 1943. The equipment of the original plant has been described in Mining and Metallurgy (May 1942). NO changes in equipment were recommended for installation in the concentrator extension and only one major change, forced by a shortage of maintenance labor, has since been made. Metallurgical treatment has been altered in some ways as experiments progressed and as labor and economic conditions dictated. No complete description of the operation of the concentrator has been published, so this paper will record such operating and equipment changes as have been necessary, the operating methods that have been developed and the metallurgical results that have been obtained. Descriptions are given in the order of the processes with a flowsheet and an equipment list of each process for convenient reference. The questions asked by engineer visitors have guided the detail in which operation and maintenance are described. During the period Jan. 30, 1942 to Sept. I, 1946, ore milled has totaled 43,595,253 dry tons, from which 1,643,885 tons of concentrate have been made, containing an indicated production of 783,164,-809 lb of copper. The principal results obtained in operation of the concentrator during the years 1942 to 1945, inclusive, and to Sept. I, 1946 are shown in Table I. A graphic general flowsheet of the plant is given in Fig I. Ore The Morenci ore that is now being treated is a medium-hard monzonite porphyry in which the principal sulphide minerals are chalcocite and pyrite. A minor amount of covellite is present. Chalcopyrite and bornite have been observed under the microscope. The chalcocite occurs mainly as a coating on pyrite. Some of the coatings are so thick that the pyrite presents the appearance of being an inclusion in chalcocite. Some are less than one micron thick and are barely visible at 500 diameters magnification of a polished cross section. Some chalcocite is present as a in in the gangue. Various oxidized copper minerals are present as a result of oxidation in place but they represent a minor proportion of the copper minerals of the ore body. Oxidation

Jan 1, 1949

By R. C. Buehl, J. P. Morris

ACTIVITY values for sulphur dissolved in liquid iron and slags as functions of composition and temperature are needed in applying thermodynamics to sulphur-control problems in iron- and ' steel-making. The purpose of this investigation was to determine the effect of carbon on the activity of sulphur in the metal phase. The method employed was the same as that used in an earlier investigation' concerning the effect of silicon on sulphur activity in liquid iron. A study was made of the conditions of equilibrium in the reaction between hydrogen gas and sulphur dissolved in iron-carbon alloys. The chemical equation for this reaction can be written as follows: S (in liquid Fe-C alloy) + H2 (gas) = H2S (gas). It was found that the activity coefficient of sulphur in liquid iron increases as the carbon content increases. At 2.3 pct carbon and 1600 °C, the activity coefficient of sulphur is twice its value in carbon-free iron, and at carbon saturation it is more than six times as great. The effect of temperature on sulphur activity was found to be small. Previous work on the reaction between hydrogen gas and sulphur dissolved in liquid iron has been reported by several investigators2,³,4 but only recently have studies been made of the effect of alloying elements. Silicon1 is known to have a pronounced influence on the activity of sulphur in iron, its effect being similar to that shown by carbon as described in the present report. Kitchener, Bockris, and Liber-man5 recently have published a preliminary report of their work on the effect of carbon on sulphur activity in iron. Their experiments were made at 1570°C and carbon saturation in the melt. Under these conditions they found that the activity coefficient of sulphur was approximately doubled by the presence of carbon. This is a much smaller effect than that found in the present work. Experimental Method: The apparatus and procedure were essentially the same as those used in the earlier investigation of the effect of silicon on sulphur activity.' Briefly, the method was as follows: A molten iron-carbon alloy was brought to equilibrium at constant temperature with a mixture of H2 and H2S of constant composition by bubbling the gas through the metal. Samples of the melt were

Jan 1, 1951

By A. H. Bell

The results of repressuring (or gas-drive) have been very encouraging to the several companies doing experimental work along these lines in California. The most notable examples are the Shell and the Union Oil companies at Dominguez, the Marland Oil Co. at Seal Beach, and the California Petroleum Corpn. at South Mountain. The results of the Marland test at Seal Beach are interesting in that re pressuring was started while several wells were still flowing; also, on account of the high pressures required to overcome the hydrostatic pressure exerted by high-head edge water. The well first chosen for repressuring is about halfway up the flank of the structure and had been on the beam making about 250 bbl. of fluid daily, cutting about 60 per cent. emulsion. The fluid lcvel was 230 ft. from the surface and the top of the sand was 4393 ft. Tubing was run to 4000 ft. with a packer and the space above the packer was filled with water to balance the high pressures. Gas was started in slowly to allow the fluid to be pushed back into the sand, and required three days at a pressure of 1500 Ib. per sq. in. before starting into formation. The pressure was once built up to 1800 Ib. and the compressor was shut down for a few hours. When again started, the well took gas at 1500 Ib., and after about three weeks the pressure was dropped to 1450 Ib. The present pressures required range between 1400 and 1450 lb. Volumes as high as 1,500,000 cu. ft. per 24 hr. were put into the well. Increases as high as 50 per cent. in production were obtained in wells up-structure with very little increase in wells down-structure. Also, the water cut on one edge well materially decreased. After about 40 days the repressuring was moved to two wells farther down-structure and the well originally repressured was put on production. The result of this was a great increase in the production of wells one location farther down-structure, a rapid increase in one well one location up-structure, and a decrease in production of the wells farthest up-structure. Later the gas started to short-cut to the nearest well down-structure, nullifying to a certain extent the effects of the repressuring work. The increased production that could be definitely attributed to the repressuring work

Jan 1, 1928

By Alexander B. Morris

In a recent paper on the intermittent injection of gas in gas-lift operations as opposed to continuous injection, Morgan Walker presented a comparative table showing the effect on oil and gas production from the same wells under the two methods of operation.' This table carried a column showing the formational gas-oil ratios under each method, computed by deducting the volume of input gas from the volume of trap gas. During the entire spring and summer of 1928, the present writer had been engaged on some extensive test car tests of rich gas in Glenpool, seeking, primarily, for an explanation of the apparent loss of gasoline during the summer season between the field meters and the plant master meter. Tests at several of the field meters where the richest gas was obtained regularly failed to check with other tests on the same gas made farther along the line, and the difference was not made up by the quantity of drip gasoline collected between the points. In the course of these tests, the final outcome of which is immaterial to the present purpose, an attempt was made to construct a curve representing the relationship between gasoline content of the gas in gallons per thousand cubic feet and the shrinkage in the volume of gas treated as a result of removing the condensible fractions. Such a curve was made, expressed in units of gallons per thousand cubic feet on the abcissa and the ratio vapor volume to liquid volume on the ordinate. This curve is a rectangular hyperbola and shows that 3 gal. of gasoline taken from 1000 cu. ft. of raw gas as a vapor occupied much less space, per gallon, than did 1 gal. of gasoline taken from 1000 cu. ft. of another sample of gas. This is, in general, corroborated by converting to the same units the residue settlement curves prepared by the Tidal Oil Co. and by the Natural Gasoline Manufacturers Assn., though the three curves, when plotted together, occupy entirely different positions on the paper, as shown in Fig. 1. The bearing of all this on Mr. Walker's discussion of gas-lift is this: if the formational gas is to be computed by deducting the input gas from the trap gas, some correction must be made for the vapor volume

Jan 1, 1930

By D. H. Davis

HAND picking was the earliest form of coal preparation, first practiced to improve the outward appearance of the coal being loaded and to remove any pieces that might appear objection- able to the buyer. It is still extensively practiced on the plus 1-in. sizes and particularly on the plus 4-in. and larger sizes. The percentage of ash reduction that can be obtained by hand picking depends entirely upon the amount of free impurity occurring in the coal. In a particularly dirty seam, where a considerable quantity of rock occurs with the coal as mined, hand picking produces sizable reductions in ash. If the coal is prepared clean at the working face hand picking is a final check; in some cases, on the smaller sizes, it is practiced only to show that an effort is being made to prepare a clean product. Because of the variety and different methods of handling coal, the early plants were not always adapted for efficient hand picking. At most mines an attempt is made to remove the visual impurities at one or more of the following places in the surface plant? (1) in the tipple during screening; (a) on picking band, belt, or shaking conveyors;*(3) during the loading of the coal as it goes into the railroad car. Whatever the physical arrangements of the plant may be, the usual practice is to run the coal over the screen, picking table or boom at such a rate that each piece of impurity is exposed to the view of the picker. Coal should be uniformly sized and spread out on the table so as not to exceed one particle in depth. The flow should be even in tonnage and the speed of travel should be from 30 to 60 ft. per minute and not exceed 80 ft. per minute. The dirtier the coal, the slower the speed required for a fixed number of pickers. Actually, picking capacity depends on the number of particles per minute that can be picked out and rejected. The percentage of impurity removed is determined by this and the average weight of piece rejected. Handling a mixture of sizes from nut to the largest lump over the same picking table or conveyor is not conducive to efficient separation by hand picking because the lump hides the smaller

Jan 1, 1943

By R. G. Ward, John Henderson. R. G. Hudson, G. Derge

Densities of melts of the iron oxide-silica system in contact with solid iron have been measured by the maximum hubble pressure method in the composition range O to 37 wt pct SiOz and the temperature range 1255 to 1410C. The constitution of the melts is discussed and it is postulated that the structure changes from a dislribution of iron ions in an oxygen ion network at pure "FeO" to a distribution. of iron ions in a network of silicate tetrahedra at the orthosilicate composition. JOHN HENDERSON, Junior Member AIME, was formerly with the Metals Research Loborotory, Carnegie Institute of Technology, Pittsburgh, Pa., on leave from Broken Hill Proprietary Co., Ltd., Research Division, Shortland, Australia. R. G. HUDSON, formerly with Metals Research Laboratory, is now with the John Jay Hopkins Loborotory for Pure and Applied Science, General Atomic Division, General Dynamics Corp., LaJolla, Calif. R. G. WARD, was formerly with the Department of Metal lurgical Engineering, Carnegie lnstitute of Technology, while on leave from the Department of Metallurgy, University of Sheffield, England. G. DERGE, Member AIME, is Jones and Laughlin Professor of Metallurgical Engineering, Carnegie lnstitute of Technology. Manuscript submitted January 19, 1961. ISD The system iron oxide-silica is an important one metallurgically because it forms the basis of several complex slag systems in use for industrial smelting and refining processes. In recent years considerable work has been done on liquids of this system but there are still many points of difference among workers using different experimental techniques and theoretical approaches. Phase equilibria/"3 activity,4-6 electrical conductivity,' current efficiency,' transference number,8 viscosity,9 surface tension,'' and density" measurements have all contributed to an understanding of the problem. Measurement of density is one procedure which is directly indicative of liquid structure since any deviation from ideality must be a result of structural interactions. Liquids of the iron oxide-silica system are of special interest because this is one of the few metal oxide-silica systems on which measurements can be carried out conveniently over the entire composition range from pure oxide to silica saturation. This includes the range of high basicity which has received relatively little attention in other systems. Although one investigation of density in this system has previously been undertaken," the results seem of sufficient importance to warrant the independent redeter-mination reported here.

Jan 1, 1962

By George V. Smith, Daniel E. Sonon

Various mechanical properties of the Ni-Co-C alloy system were investigated to delineate the strengthening effect of carbon. Carbon concentration, cobalt concentration, vain size, temperature, and strain rate were varied so that thermal activation analysis and the Hall-Petch analysis could be used to evaluate the strengthening effect of carbon. Increasing carbon increased the strength of nickel and a Ni-60 pct Co alloy , with the effect becoming more pronounced at lower temperatures. Yield stress depended linearly on carbon concentration in nickel, but it depended on the square root of carbon concentration in the Ni-60 pct Co alloy. The Hall-Petch slope of nickel increased with carbon concentration; however, that of the Ni-60 pct Co alloy did not. The yielding behavior of these alloys was sensitive to composition, grain size, and temperature. Cobalt eliminated serrations in the flow curve of carbon-containing nickel at 300' and weakened them severely at higher temperatures. Pairs, or clusters, of carbon atoms appear to be responsible for the observed strengthening behavior. FLINN' conducted several experiments with carbon in nickel in an effort to provide information on the strengthening effect of interstitial impurities in solid solution in fcc metals and alloys. Strengthening which increased with decreasing temperature led him to conclude that carbon causes Cottrell locking in nickel. Fleischer2 analyzed Flinn's data and calculated that the strengthening effect of carbon in nickel was smaller by a factor of fifty than the strengthening effect of carbon in a! iron. Fleischer2 termed the magnitude of strengthening of carbon in nickel "gradual" and that of carbon in a! iron "rapid". He attributed "gradual" hardening to hydrostatic strains and localized changes in modulus of elasticity around solute atoms, whereas he attributed "rapid" hardening to tetragonal strains around solute atoms. Sukhovarov et a1.3-7 reported strain aging and serrated plastic flow in nickel, both of which they attributed to the presence of carbon. Serrated plastic flow has been rationalized by a process involving a series of dislocation pinning and multiplication steps.8, This process is more probable when screw dislocations are strongly pinned. Screw dislocations cannot be pinned by pure hydrostatic forces from the symmetrical strains of an interstitial impurity in an fcc lattice, except for small, second-order effects. However, they might be pinned by localized changes in modulus of elasticity around solute atoms,' by the pinning of the edge components of the partial dislocations of an extended screw dislo~ation,'~ or by clustered groups of solute atoms whose net elastic stress field is unsymmetric. The purpose of the present work was to investigate various mechanical properties of the Ni-Co-C a1loy system which are sensitive to pinning effects in order to delineate the specific pinning mechanism of carbon. Carbon concentration, grain size, temperature, and strain rate were varied so that thermal-activation analysis and the Hall-Petch analysis could be used to evaluate the pinning mechanism. Cobalt was added to lower stacking fault energy so that the number and extension of split, screw dislocations would be increased in order to test the possibility of pinning by carbon at extended screw dislocations. EXPERIMENTAL PROCEDURE Nickel and cobalt (both 99.98 pct-. pure) were melted with graphite in stabilized zirconia crucibles and cast at lo-' Torr to form Ni-C and Ni-60 pctCo-C alloys. Two ingots were heated to 1250°C and were forged to 1-in.-sq bars. These bars were machined to 4-in.-round bars, and then swaged cold to 0.144-in. -diam rods. Reductions in area of approximately 75pct were used with intermediate anneals at 900°C for 1 hr. The carbon content of batches of 0.144-in.-diam rods from each ingot was reduced to two levels by annealing 5-in. lengths in palladium-purified, dry hydrogen at 1100°C for 25 and 100 hr. The remaining material from each ingot was annealed at 10"5 Torr for 1 hr at 1100"~. These treatments gave a total of three carbon levels for both the nickel and the Ni-60 pct Co alloy. The 0.144-in.-diam rods were swaged to 70-mil wire, cut into test specimens, and then re crystallized at lom5 Torr in capsules for 1 hr at temperatures ranging from 760" to 1050" ~. The capsules were broken and the specimens were immediately quenched into water. Average grain size was measured using Hilliard's method of circular intercepts." Annealing twin boundary intercepts were counted in addition to grain boundary intercepts to establish an average grain size. Average grain sizes ranged from 5 to 140 p depending on the cobalt concentration and re-crystallization temperature. Tension tests were made in duplicate at various temperatures at a crosshead speed of 8.34 x 10"4 in. per sec with an Instron Universal Testing Machine. Specimens of 1-in. gage length with soldered ball ends were used at atmospheric and cryogenic temperatures. Pinch grips were used on specimens at elevated tem-

Jan 1, 1969

By A. J. Shaler, H. Udin, J. Wulff

In the study of the sintering of meta powders, we have come to the conclusion in this laboratory that further progress requires a more basic understanding of the operating mechanisms. This is emphasized in detail by Shaler. He has shown that a knowledge of the exact value of the surface tension is imperative for a solution of the kinetics of sintering. This force plays a principal role in causing the density of compacts to increase.2 Furthermore, a knowledge of the surface tension of solids is also applicable to other aspects of physical metallurgy. C. S. Smith3 points out the relation between surface and interfacial tension and their function in determining the microstructure and resulting properties of polycrystal-line and polyphase alloys. This paper describes one group of results of an experimental program designed for the study of the surface tension in solid metals. As a by-product of this work, considerable information has been obtained on the rate and nature of the flow of a metal at temperatures approaching the melting point and under extremely low stresses, a field of mechanical behavior heretofore scarcely touched by metallurgists. The importance of this additional information to students of powder metallurgy need not be stressed. Theoretical Considerations Interfacial tension arises from the condition that an excess of energy exists at the interface between two phases. Gibbs proves that this energy is a partial function of the interfacial area; thus: ?F/?s = ? where ?F/?s is the rate of change of free energy of the system with changing surface area, at constant temperature, pressure and composition, and ? is the interfacial tension, or interfacial free energy per unit area. If one of the phases is the pure liquid or solid, and the other the vapor of the substance, ? may properly be termed "surface tension," and is a characteristic of the solid or liquid. The attempt of a body to lower its free energy by decreasing its surface gives rise to a force in the surface which is numerically equal in terms of unit length to the free energy per unit area of the surface. Thus ? may be expressed either in erg-cm-² or in dyne-cm-1. Similarly, surface tension may be determined either by a thermo-dynamic measurement of the surface energy or by a mechanical measurement of the surface force. We have chosen the latter approach. Tammann and Boehme4 determined the surface tension of gold by measuring the amount of shrinkage or extension of thin weighted foil at various temperatures and interpolating to zero strain. The method is of questionable accuracy because of the tendency of foil to form minute tears when heated under tension. Their assumption of F = 2W?, where W is the width of the foil, is unsound, as the foil can decrease its surface area by transverse as well as by longitudinal shrinkage. Although their experimentation was meticulous, the paper does not include details of the sample configuration required for recalculating ? on a correct basis, even if such a calculation were possible. In the experimental procedure chosen here, a series of small weights of increasing magnitude are suspended from a series of line copper wires of uniform cross-section. This array is brought to a temperature at which creep is appreciable under extremely small stress. If the weight overbalances the contracting force of surface tension, the wire stretches; otherwise, it shrinks. The magnitude of the strain is determined by the amount of unbalance, so a plot of strain vs. load should cross the zero strain axis at w = F?. If balance is visualized as a thermodynamic equilibrium, the critical load is readily calculated. At constant temperature, an infinitesimal change in surface energy should be equal to the work done on or by the weight: ds = wdl [A] For a cylinder, s = 2pr2 + 2prl [2] If the volume remains constant, r = vV/pl [31 s = 2vpl+2V/l [4] ds = vpv/l - 2V/l²) dl [5] Substituting [5] into [I] gives for the equilibrium load, w = ?(z/rV- 2V/12) [6] and, again expressing V in terms of r and l, w = pr?(1 - 2r/l [7] Here the end-effect term, 2r/l, is neglected for thin wires in subsequent work. Eq 7 can be confirmed by means of a stress analysis. If the x-axis is chosen along the wire, then the stress is 2pr? - w pr² pr2 [8] A cylinder of diameter dis equivalent to a sphere of radius r, insofar as radial surface tension effects are concerned.³ Thus xv = 2?/d = ?/r = sz [9] For the case of zero strain in the x direction, the strain will also be zero in the y and z directions. Since the wire is under hydrostatic stress, Eq 8 and 9 are

Jan 1, 1950

By M. O. Abo-el Fotoh, J. B. Mitchell, J. E. Dorn

The effect of strain rate and temperature on the tensile flow stress of a polycrystalline bcc alloy of magnesium containing 14 wt pct Li and 1.5 wt pct Al was investigated for strain rates of 3.13 x lom5 to 3.13 x 10-3 per sec over the range from 20° to 300°K. From about 180° to 300°K the alloy exhibited an ather-ma1 deformation behavior where the flow stress was independent of strain rate and increased only slightly with decreasing temperature. At lower temperatures the flow stress was strongly strain-rate- and temperature-dependent, characteristic of deformations controlled by thermally activated mechmzisms. The activation volume for thermally activated plastic defornzation was between 5 and 30 cu Burgers vectors, independent of plastic strain. This low-temperature thermally activated deformation behavior was found lo be in satisfactory agreement with the theoretical dictates of the Dorn-Rajnak1 formulation of the Peierls mechanism where deformation is controlled by the rate of nucleation of pairs of dislocation kinks over the Peierls energy barriers. SEVERAL studies of the low-temperature thermally activated deformation of bcc metals and alloys (molybdenum,1 tantalum,1 Fe-2 pct Mn,2 Fe-11 pct MO,3 and AgMg4) have revealed that the strain rate is controlled by the activation of dislocations over the Peierls-Nabarro energy hills. Although there is some uncertainty as to the nature and effect of solute atom-dislocation interactions during low-temperature deformation of bcc metals, it has been concluded by Dorn and Rajnak,1 Conrad,1 and Christian and Masters6 among others that overcoming the Peierls-Nabarro stress which arises from the variations in bond energies of atoms in the dislocation core as it is displaced is the probable mechanism controlling low-temperature deformation. The purpose of this research was to investigate the low-temperature plastic deformation of the bcc alloy Mg-14 wt pct Li-1.5 wt pct A1 to determine if the behavior of this alkali metal alloy might be analogous to that for other bcc metals. This alloy was selected because of its availability and its current industrial importance as a lightweight material for aircraft and aerospace applications. I) EXPERIMENTAL PROCEDURE Polycrystalline tensile specimens having cylindrical gage sections 2 in. long by 0.2 in. in diam were machined from as-received alloy sheet stock of Mg-14 wt pct Li-1.5 wt pct Al. Specimens were annealed in an argon atmosphere at 423°K for 4 hr and maintained in a kerosene bath together with the sheet stock to prevent corrosion. The resulting specimen microstructure consisted of a coarse uniform dispersion of incoherent precipitate MgLi2Al particles7 in a bcc 0 phase matrix having an average grain size of 150 p. Prior to testing the specimens were chemically polished in dilute hydrochloric acid. Comparison of tensile properties and microstructures of specimens cut from center and edge sections of the sheet stock revealed no effects of inhomogeneities in the sheet material. Tensile tests were performed on an Instron machine at crosshead speeds corresponding to tensile strain rates of 1.56 x 10-5 and 1.56 x 10"3 per sec. Stresses were determined to ±2 x 106 dynes per sq cm and strains to within ±0.0001. Average values of shear stress t and shear strain y reported were taken as one half the tensile stress and three halves the tensile strain, respectively. Flow stresses were taken at 0.05 pct strain offset. Test temperatures down to 77°K were obtained by immersing the specimens in constant-temperature baths. Lower-temperature tests were performed in a liquid helium cryostat to within ±2°K of the reported values. Prior to testing at the various temperatures and strain rates all specimens were prestrained at 2 35°K at a shear strain rate of 3.13 x 10-5 per sec to a stress level of 0.606 x 10' dynes per sq cm to obtain a uniform initial state. Additional tests were made to determine the effect of changes in strain rate and strain on the flow stress by rapidly changing the crosshead motion during testing. Shear moduli of elasticity, needed for analyses of the data, were obtained at several temperatures by a common technique of determining the resonant frequencies of vibrations of rectangular test specimens. 11) EXPERIMENTAL RESULTS Fig. 1 shows the experimentally determined flow stress vs temperature for two strain rates. Two distinct regions of behavior are evident. Below about 180°K the strong increase in flow stress with increased strain rate and decreasing temperature indicates that deformation is controlled by a thermally activated dislocation mechanism. At higher temperatures an athermal region is evident where the flow stress is independent of strain rate and only slightly dependent on temperature. The applied stress t to cause plastic flow was separated into two components:

Jan 1, 1969