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By D. S. Sanders, E. W. Witcomb

FLOTATION tests, from which the flowsheet for the concentrator was determined, were made in a pilot mill at Chuquicamata and later comparative testing of full size flotation cells was done at the Andes Copper Mining Co. concentrator in Potrerillos. The principal sulphide copper mineral is chalcocite with varying amounts of covellite, enargite, and chalcopyrite. The oxidized portion is principally antlerite, a green basic copper sulphate. The gangue minerals include quartz, sericite, pyrite, feldspars and kaolin. Chuquicamata pit ores have proved to be hard grinding. The results of the flotation and metallurgical work prove that good extraction and concentrate grade can be obtained under a rather wide range of conditions. Metallurgy In general the metallurgy of the ore requires a fairly close control of the grind to the primary rougher flotation and of the regrind of the primary rougher concentrate before cleaning. Regrinding is necessary to reduce the insoluble content of the final concentrate since a large part of the middling combinations are between the copper and silica minerals. The alkalinity of the pulps can vary between wide limits and control of the percent solids gives the desired grind. Alkalinity Control Arroyo Salado water is supplied to the concentrator head tanks. It contains about 5000 ppm of salts but test work shows no deleterious effect. Actually this water permits a decrease of as much as 1 lb of lime per ton of ore as compared to San Pedro water, which is used for leaching oxide ore. About one quarter of the water flow through the concentrator will be new water from the reservoir. The remainder will be reclaimed from the thickeners. For primary grinding and rougher flotation, new and reclaimed water are combined in the head tanks. To avoid erratic results, only new water is used in the regrind system. Milk of lime is added to the rod mill feed chute to obtain the maximum benefit of mixing with the ore. This protects the equipment from corrosion due to entrained acids and soluble copper salts. Lime consumption is 3 to 5 lb per ton of ore. Grinding and Flotation The six bin gates over each belt feeder are opened in controlled combination and sequence to keep a live bed of ore in the bin to prevent arching and to obtain mixing. The milk of lime added ahead of the rod mill is regulated to suit rougher flotation requirements. The primary promoter reagent, Aerofloat 238, is added to the 10-mesh discharge of the rod mill as it is laundered to the ball mill scoop box. The classifier overflow is regulated to produce a grind of about 12 to 15 pct +65 mesh and 60 pct -200 mesh. A secondary promoter Z-4 (aml zanthate) and the pine oil frother are added in the overflow launder where a pH of 10 to 11 is maintained. Comparatively heavy beds of froth on the

Jan 1, 1952

By Norris Johnston, Carrol M. Beeson

The gravimetric-vacuum distillation method was developed to permit rapid and accurate determinations of the oil-water ratios of small samples or sands containing little oil. In addition, the samples usually are so well cleaned and so little altered by the distillation at reduced pressure that rapid estimations of other physical properties may be made with the evacuated cores. Requiring only elementary glass-blowing technique, the distilling tubes and traps used in determining oil-water ratios were easily fashioned from the usual glassware. A sketch and description are given of the necessary apparatus, including the cylindrical electrical heaters. The procedure, requiring about 40 min., consists in raising the temperature and maintaining it between 675' and 725°F. for at least 10 min. while the pressure is held between I and 2 mm. Hg. The fluids condensed in the trap (cooled by a mixture of kerosine and solid carbon dioxide) are separated in a centrifuge and the volume of water is recorded. Determination of changes in weight with an analytical balance of all parts of the apparatus permits computation of weight of oil distilled and total weight of oil recovered. Introduction In determining the oil-water ratios of core samples, distillation at atmospheric pressurel-5 has proved to be sufficiently reliable for samples containing moderate quantities of oil. Since small samples and sands with little oil are encountered, how- ever, it appeared advisable to develop a method that would be applicable under these circumstances. Thegravimetric-extraction procedure1,6-9 undoubtedly is very reliable and could be used in all tests, but the time consumed in the determination would often delay field operations. This would be especially true when dealing with tight sands or viscous oils, both of which retard the extraction process. Accordingly, the gravimetric-vacuum distillation method was developed in order to combine the good features of both of the older methods; that is, accuracy and speed. By reducing the pressure, it was found possible to perform the distillation at a temperature that permits the use of glass apparatus, all parts of which can be weighed on an analytical balance. Thus, the fluids may be removed quickly from the core, the water is readily trapped and measured, and the loss in weight of the core is easily determined. In addition, the total weight of material condensed in the distilling tube and in the trap provides a method of determining the oil-water ratio that is practically independent of the one involving the loss in weight of the sample. The use of vacuum not only permits as much accuracy as does the gravimetric-extraction process, but it actually allows an increase in speed over the atmospheric-distillation method, because of the time required to cool the metal pots from about 1200°F. between runs. More important yet, the innovation makes possible the almost immediate reporting of permeability, and saturation, which is impossible

Jan 1, 1946

By Norris Johnston, Carrol M. Beeson

The gravimetric-vacuum distillation method was developed to permit rapid and accurate determinations of the oil-water ratios of small samples or sands containing little oil. In addition, the samples usually are so well cleaned and so little altered by the distillation at reduced pressure that rapid estimations of other physical properties may be made with the evacuated cores. Requiring only elementary glass-blowing technique, the distilling tubes and traps used in determining oil-water ratios were easily fashioned from the usual glassware. A sketch and description are given of the necessary apparatus, including the cylindrical electrical heaters. The procedure, requiring about 40 min., consists in raising the temperature and maintaining it between 675' and 725°F. for at least 10 min. while the pressure is held between I and 2 mm. Hg. The fluids condensed in the trap (cooled by a mixture of kerosine and solid carbon dioxide) are separated in a centrifuge and the volume of water is recorded. Determination of changes in weight with an analytical balance of all parts of the apparatus permits computation of weight of oil distilled and total weight of oil recovered. Introduction In determining the oil-water ratios of core samples, distillation at atmospheric pressurel-5 has proved to be sufficiently reliable for samples containing moderate quantities of oil. Since small samples and sands with little oil are encountered, how- ever, it appeared advisable to develop a method that would be applicable under these circumstances. Thegravimetric-extraction procedure1,6-9 undoubtedly is very reliable and could be used in all tests, but the time consumed in the determination would often delay field operations. This would be especially true when dealing with tight sands or viscous oils, both of which retard the extraction process. Accordingly, the gravimetric-vacuum distillation method was developed in order to combine the good features of both of the older methods; that is, accuracy and speed. By reducing the pressure, it was found possible to perform the distillation at a temperature that permits the use of glass apparatus, all parts of which can be weighed on an analytical balance. Thus, the fluids may be removed quickly from the core, the water is readily trapped and measured, and the loss in weight of the core is easily determined. In addition, the total weight of material condensed in the distilling tube and in the trap provides a method of determining the oil-water ratio that is practically independent of the one involving the loss in weight of the sample. The use of vacuum not only permits as much accuracy as does the gravimetric-extraction process, but it actually allows an increase in speed over the atmospheric-distillation method, because of the time required to cool the metal pots from about 1200°F. between runs. More important yet, the innovation makes possible the almost immediate reporting of permeability, and saturation, which is impossible

Jan 1, 1946

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

The results of an extensive experimental program relating to the effectiveness of gravel screens have been correlated. The factors considered in some detail include gravel size and condition of packing, sand size and size distribution, fluid velocity, fluid viscosity, and thickness and arrangement of grave! screens. Good agreement between calculated values based upon probability considerations and experimental results relating to the influence of the thickness of the gravel screen was obtained. All of these factors are treated in the correlation in order that their influence may be taken into account in ascertaining the characteristics of an effective gravel screen for a particular set of conditions. The details of the experimental program are not given in the present paper but a description of generalized behavior and typical experimental results are recorded in graphic form. Introduction Gravel screens have been placed in water and oil wells for a number of yearsl,2,3 with the dual objective of increasing the productivity and decreasing the entrance of sand into the well bore. An understanding of the factors controlling the effectiveness of gravel screens in this connection is of industrial interest because it will lead to the proper selection of gravel. Some of the fundamental considerations involved in the migration of sand through a coarser body of porous materials were investigated by Coberly and Wagner4 and further experimental work has been carried out by Gumpertz.5 Apparently the pertinent phenomena are somewhat complex and are influenced by many variables. The present paper deals with the prediction of the behavior of gravel screens under the conditions encountered in practice but does not attempt to discuss the experimental methods or results that were obtained as a background and upon which the prediction is based. Influence OF Gravel Screens upon Productivity The use of a gravel screen may increase the productivity of a well by increasing its effective diameter, and this constitutes one of the objectives of its use. The permeability of most gravels and coarse sands that are employed in practice is so large compared to that of the sand in place that relatively little loss in production rate will arise from the use of material fine enough to cause the desired resistance to sand migration. For example, in Fig. I is depicted the approximate variation in the permeability of closely sized spherical gravels under the conditions of packing likely to be encountered in screens. The dotted lines indicate the variation that might be found because of differences in packing. It should be realized that the permeability is not a single-valued function of the average grain diameter but is related to a large number of factors, including the size, the size distribution and the shapes of the particles. However, Fig. I does permit a rough estimation of the permeability of closely sized spherical gravels and shows that the permeability with even the smaller particles is very large compared to that of most petroleum production horizons.

Jan 1, 1942

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

The results of an extensive experimental program relating to the effectiveness of gravel screens have been correlated. The factors considered in some detail include gravel size and condition of packing, sand size and size distribution, fluid velocity, fluid viscosity, and thickness and arrangement of grave! screens. Good agreement between calculated values based upon probability considerations and experimental results relating to the influence of the thickness of the gravel screen was obtained. All of these factors are treated in the correlation in order that their influence may be taken into account in ascertaining the characteristics of an effective gravel screen for a particular set of conditions. The details of the experimental program are not given in the present paper but a description of generalized behavior and typical experimental results are recorded in graphic form. Introduction Gravel screens have been placed in water and oil wells for a number of yearsl,2,3 with the dual objective of increasing the productivity and decreasing the entrance of sand into the well bore. An understanding of the factors controlling the effectiveness of gravel screens in this connection is of industrial interest because it will lead to the proper selection of gravel. Some of the fundamental considerations involved in the migration of sand through a coarser body of porous materials were investigated by Coberly and Wagner4 and further experimental work has been carried out by Gumpertz.5 Apparently the pertinent phenomena are somewhat complex and are influenced by many variables. The present paper deals with the prediction of the behavior of gravel screens under the conditions encountered in practice but does not attempt to discuss the experimental methods or results that were obtained as a background and upon which the prediction is based. Influence OF Gravel Screens upon Productivity The use of a gravel screen may increase the productivity of a well by increasing its effective diameter, and this constitutes one of the objectives of its use. The permeability of most gravels and coarse sands that are employed in practice is so large compared to that of the sand in place that relatively little loss in production rate will arise from the use of material fine enough to cause the desired resistance to sand migration. For example, in Fig. I is depicted the approximate variation in the permeability of closely sized spherical gravels under the conditions of packing likely to be encountered in screens. The dotted lines indicate the variation that might be found because of differences in packing. It should be realized that the permeability is not a single-valued function of the average grain diameter but is related to a large number of factors, including the size, the size distribution and the shapes of the particles. However, Fig. I does permit a rough estimation of the permeability of closely sized spherical gravels and shows that the permeability with even the smaller particles is very large compared to that of most petroleum production horizons.

Jan 1, 1942

By R. L. Wiegel

The two questions considered in this study are: (1) what similarity is there in the liberation of magnetite from various iron formations, and (2) how is this liberation affected by the size reduction technique employed. Twelve sample suites were obtained from commercial concentrators processing magnetite iron formation in the United States, Canada, and Australia. These samples have grades in the range 15 to 45% magnetite iron and approximate mineral grain sizes o f 50 to 2000 microns. Efforts were directed at measuring the liberation characteristics of the samples obtained from the concentrators primary grinding mills. The Davis tube, a laboratory magnetic separator, was used to concentrate individual size fractions of the size reduction product to determine liberation data. These liberation data were compared with relationships calculated from a highly idealized mathematical model of liberation in a binary mineral system. The results of these comparisons have been encouraging for nine or ten of the twelve samples tested. This leads to the conclusion that for most commercial iron formations, at least with conventional rod mill size reduction, it is possible to quantitatively characterize liberation with two parameters: an effective mineral grain size and ore grade. Limited laboratory size reduction tests as well as one of two sets of liberation data from commercial primary autogenous grinding lend some support to the contention that autogenous grinding can affect mineral liberation.

Jan 1, 1976

By William E. Ford, Edward Salisbury Dana

Twin crystals are those in which one or more parts regularly arranged are in reverse position with reference to the other part or parts. They often appear externally to consist of two or more crystals symmetrically united, and sometimes have the form of a cross or star. They also exhibit the composition in the reversed arrangement of part of the feces, in the striae of the surface, and in re-entering angles; in certain cases the compound structure can only be surely detected by an examination in polarized light. The above figures (Figs. 384-386) are examples of typical kinds of twin crystals, and many others are given on the pages following.

Jan 1, 1922

By J. E. Gould, H. J. Hand

Many independent studies are being made on slag-metal relationships in the open-hearth furnace, and these studies cannot help but result in an ultimate improvement in the quality of open-hearth steel of both the open and killed types. In maintaining quality control at the National Tube Company's plant, emphasis has been placed on an evaluation of the iron oxide content of the steel in as quantitative a manner as possible, in order that the most desirable level of oxidation might be obtained for a given type of steel, and to secure a more precise basis for final de-oxidation. In the past, various methods were used for estimating FeO content of the metal at tap to ensure uniform and thorough deoxidation of killed steel, avoiding overdeoxidation to minimize the amount of inclusions present and to make as sound a steel as possible. For the open-type steels, such control involves obtaining the necessary level of oxidation for the most suitable action of the steel in the molds to provide good surface quality and cross section for the specific grade involved. While rapid analytical methods are available for determination of FeO in the liquid metal, such methods are still not sufficiently rapid for routine control on the open-hearth floor, nor do such analyses provide information as to what causes high or low FeO values. The method of sampling can still be considered a problem in view of the variability encountered in taking simultaneous duplicate tests. With the accurate rapid methods now available for determining carbon in the metal, estimating slag basicity and obtaining temperatures of liquid metal, it was believed possible to determine the influence of the various furnace reactions in establishiug the state of oxidation at a given time. Simultaneous slag and metal tests were used in this analysis, aided by statistical methods, to determine the factors that affect the metal FeO, and also to make a quantitative evaluation of these factors. Data obtained are from actual iurnace operations, the metal test being of the I spoon, Herty type, and taken in duplicate. Metal temperatures were taken with the open-tube bath pyrometer developed by the Research Laboratory of the United States I Steel Corporation. This method of taking open-hearth metal temperature was invented by Collins and Oseland,l and was developed into its present form by L. 0. Sordahl,2 of the Research Laboratory. The instrument and its mode of operation have been fully described by Sordahl and Sosman in three publications.3,4,5 lag components were obtained by chemical analysis. Data were taken from four 165-net-ton furnaces during the working period of the heat. Recognizing that additions of ore affect the metal FeO. no tests were included within 30 min. after ore additions. In all, 65 tests (48 heats) were used in this study.

Jan 1, 1942

By J. E. Gould, H. J. Hand

Many independent studies are being made on slag-metal relationships in the open-hearth furnace, and these studies cannot help but result in an ultimate improvement in the quality of open-hearth steel of both the open and killed types. In maintaining quality control at the National Tube Company's plant, emphasis has been placed on an evaluation of the iron oxide content of the steel in as quantitative a manner as possible, in order that the most desirable level of oxidation might be obtained for a given type of steel, and to secure a more precise basis for final de-oxidation. In the past, various methods were used for estimating FeO content of the metal at tap to ensure uniform and thorough deoxidation of killed steel, avoiding overdeoxidation to minimize the amount of inclusions present and to make as sound a steel as possible. For the open-type steels, such control involves obtaining the necessary level of oxidation for the most suitable action of the steel in the molds to provide good surface quality and cross section for the specific grade involved. While rapid analytical methods are available for determination of FeO in the liquid metal, such methods are still not sufficiently rapid for routine control on the open-hearth floor, nor do such analyses provide information as to what causes high or low FeO values. The method of sampling can still be considered a problem in view of the variability encountered in taking simultaneous duplicate tests. With the accurate rapid methods now available for determining carbon in the metal, estimating slag basicity and obtaining temperatures of liquid metal, it was believed possible to determine the influence of the various furnace reactions in establishiug the state of oxidation at a given time. Simultaneous slag and metal tests were used in this analysis, aided by statistical methods, to determine the factors that affect the metal FeO, and also to make a quantitative evaluation of these factors. Data obtained are from actual iurnace operations, the metal test being of the I spoon, Herty type, and taken in duplicate. Metal temperatures were taken with the open-tube bath pyrometer developed by the Research Laboratory of the United States I Steel Corporation. This method of taking open-hearth metal temperature was invented by Collins and Oseland,l and was developed into its present form by L. 0. Sordahl,2 of the Research Laboratory. The instrument and its mode of operation have been fully described by Sordahl and Sosman in three publications.3,4,5 lag components were obtained by chemical analysis. Data were taken from four 165-net-ton furnaces during the working period of the heat. Recognizing that additions of ore affect the metal FeO. no tests were included within 30 min. after ore additions. In all, 65 tests (48 heats) were used in this study.

Jan 1, 1942

By G. R. Wilms

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

Jan 1, 1955

By Martin S. Maier, H. R. Nelson

THE diffusion of metals plays an important role in many metallurgical processes, 1,2 as, for example, the formation of alloys by the annealing of mixed powders, the homogenization of segregated alloys, and the carburization of steel. Other equally important phenomena, such as recrystallization and creep, are based on the movement of like atoms. Although much is known concerning the effects of diffusion in metals, very little is known concerning the details of the physical processes involved.1,3-5 The data that should give most information concerning the processes involved in diffusion are those on the diffusion of like atoms-self-diffusion. Very little is known concerning the rates of self-diffusion of metals because before the discovery of artificial radio-activity in 1934 there was no means of detecting the movement of the diffusing atoms through the solvent metal except in the elements possessing natural radioactive isotopes-lead, thallium and bismuth. Using the induced radioactivity of the element as an indicator, atoms can now be "tagged" so that the rate of diffusion of the radioactive isotopes of an element (tagged atoms) into the stable isotopes of the same element can be measured. As the radioactive and stable isotopes of an element differ only in nuclear structure, it is quite certain that all isotopes of an element diffuse at the same rate. Two techniques have been used to measure self-diffusion. In one, a thin layer of radioactive metal is deposited on the face of the solvent metal, and the decrease in the surface activity as the radioactive atoms diffuse into the solvent metal is measured. This method has been used to determine the coefficients of self-diffusion of lead6-10 and bismuth10 using natural radioactive isotopes, and of gold11 and copper12 using artificial radioactive isotopes. In the other technique a thin layer of the radioactive metal is deposited on one face of the solvent metal, and after diffusion has occurred the specimen is cut in thin sections to obtain the concentration-penetration curve. This method has been used to determine the coefficients of self-diffusion of gold,13 zinc, 14-16 silver,17 and copper.18 The second method was used for the work described in this paper. MATERIALS The coefficients of self-diffusion were determined in two grades of polycrystalline copper and in single crystals of copper. Commercial OFHC copper was used in the form of disks I in. in diameter by 1/8 in. thick. Samples of high-purity copper described by Phillips and Skinner19 were supplied through the courtesy of the American Smelting and Refining Co. The high-purity copper rod was used without remelting by cross-rolling to a thickness of 0.075 in., from which disks 7/8 in. in diameter were cut. A good grade of bus-bar copper was used to make the single crystals.

Jan 1, 1942

By Dorsey Hager

North Central Texas has recently become a center of interest for the oil men of America. The bringing in of the McClosky well at Ranger, Eastland County, and the shallow pool at Brownwood, Brown County, in 1917, has stimulated interest in this area to fever pitch. Oil men from all over the United States are now investing there. The area of present interest is shown by the accompanying map (Fig. 1). The money spent in leases runs into millions of dollars. It is no exaggeration to say that a strip of country 200 miles (321 km.) long and 125 miles (201 km.) wide, comprising some 15,000,000 acres (6,070,310 ha.), has been leased practically solid at a cost for rentals and bonuses of at least $1 per acre. The test holes contracted for will certainly number 400, at a cost of at least $5,000,000. From what has been done in the past six months, $20,000,000 at least will be spent. To pay returns on this amount of money, new production to the extent of at least 12,000,000 bbl. must be obtained. At present, the production from new fields will not average over 5000 bbl. per day; three wells at Ranger are producing 3000 bbl.; 250 wells at Brownwood produce 1000 bbl.; and the Gray well, Coleman County, is as yet an unknown factor. However, at Ranger there is every indication of developing a good pool covering from 1500 to 2000 acres (607 to 809 ha.), more or less, but the wells are deep, 3400 to 3800 ft. (1036 to 1158 m.), and cost $35,000 to $40,000 to drill. Large wells are necessary to pay for such expensive holes. As new wells are drilled, the gas pressure will be lowered rapidly, and large production need not be expected. For those oil men who expect a second Cushing or an Eldorado, Ranger holds little of promise. At Brownwood, Brown County, there are some 250 shallow wells (depths from 200 to 350 ft.) averaging 4 to 7 bbl. per day. There is a chance of an extensive producing area for these shallow sands to the southwest, and the opening of several thousand acres of shallow oil territory, and also some promise of deeper oil horizons in the Ranger horizon, but probably all under 2500 ft. At present, the lease brokers and speculators, and only a handful of oil men, have made any money. More fields must be developed, and it is more particularly with these possibilities that this paper deals. Lack of water for drilling purposes has undoubtedly held back development so far this year; this part of Texas has had a drouth for two years and there is an actual scarcity of water. Geological investigations so far undertaken cover nearly all the area outlined, and while pakt of the

Jan 1, 1920

By H. R. Nelson, Martin S. Maier

The diffusion of metals plays an important role in many metallurgical processes,lJ as, for example, the formation of alloys by the annealing of mixed powders, the homogenization of segregated alloys, and the carburization of steel. Other equally important phenomena, such as recrystalli-zation and creep, are based on the movement of like atoms. Although much is known concerning the effects of diffusion in metals, very little is known concerning the details of the physical processes involved. 1,3-5 The data that should give most information concerning the processes involved in diffusion are those on the diffusion of like atoms—self-diffusion. Very little is known concerning the rates of self-diffusion of metals because before the discovery of artificial radioactivity in 1934 there was no means of detecting the movement of the diffusing atoms through the solvent metal except in the elements possessing natural radioactive isotopes—lead, thallium and bismuth. Using the induced radioactivity of the element as an indicator, atoms can now be "tagged" so that the rate of diffusion of the radioactive isotopes of an element (tagged atoms) into the stable isotopes of the same element can be measured. As the radioactive and stable isotopes of an element differ only in nuclear structure, it is quite certain that all isotopes of an element diffuse at the same rate. Two techniques have been used to measure self-diffusion. In one, a thin layer of radioactive metal is deposited on the face of the solvent metal, and the decrease in the surface activity as the radioactive atoms diffuse into the solvent metal is measured. This method has been used to determine the coefficients of self-diffusion of lead6-l0 and bismuth10 using natural radioactive isotopes, and of gold1' and copper12 using artificial radioactive isotopes. In the other technique a thin layer of the radioactive metal is deposited oil one face of the solvent metal, and after diffusion has occurred the specimen is cut in thin sections to obtain the concentration-penetration curve. This method has been used to determine the coefficients of self-diffusion of gold,13 zinc,14-l6 silver," and copper.17 The second method was used for the work described in this paper. Materials The coefficients of self-diffusion were determined in two grades of polycrystalline copper and in single crystals of copper. Commercial OFHC copper was used in the form of disks I in. in diameter by % in. thick. Samples of high-purity copper described by Phillips and Skinnerl9 were supplied through the courtesy of the American Smelting and Refining Co. The high-purity copper rod was used without remelting by cross-rolling to a thickness of 0.075 in., from which disks 7/8 in. in diameter were cut. A good grade of bus-bar copper was used to make the single crystals.

Jan 1, 1942

By Martin S. Maier, H. R. Nelson

The diffusion of metals plays an important role in many metallurgical processes,lJ as, for example, the formation of alloys by the annealing of mixed powders, the homogenization of segregated alloys, and the carburization of steel. Other equally important phenomena, such as recrystalli-zation and creep, are based on the movement of like atoms. Although much is known concerning the effects of diffusion in metals, very little is known concerning the details of the physical processes involved. 1,3-5 The data that should give most information concerning the processes involved in diffusion are those on the diffusion of like atoms—self-diffusion. Very little is known concerning the rates of self-diffusion of metals because before the discovery of artificial radioactivity in 1934 there was no means of detecting the movement of the diffusing atoms through the solvent metal except in the elements possessing natural radioactive isotopes—lead, thallium and bismuth. Using the induced radioactivity of the element as an indicator, atoms can now be "tagged" so that the rate of diffusion of the radioactive isotopes of an element (tagged atoms) into the stable isotopes of the same element can be measured. As the radioactive and stable isotopes of an element differ only in nuclear structure, it is quite certain that all isotopes of an element diffuse at the same rate. Two techniques have been used to measure self-diffusion. In one, a thin layer of radioactive metal is deposited on the face of the solvent metal, and the decrease in the surface activity as the radioactive atoms diffuse into the solvent metal is measured. This method has been used to determine the coefficients of self-diffusion of lead6-l0 and bismuth10 using natural radioactive isotopes, and of gold1' and copper12 using artificial radioactive isotopes. In the other technique a thin layer of the radioactive metal is deposited oil one face of the solvent metal, and after diffusion has occurred the specimen is cut in thin sections to obtain the concentration-penetration curve. This method has been used to determine the coefficients of self-diffusion of gold,13 zinc,14-l6 silver," and copper.17 The second method was used for the work described in this paper. Materials The coefficients of self-diffusion were determined in two grades of polycrystalline copper and in single crystals of copper. Commercial OFHC copper was used in the form of disks I in. in diameter by % in. thick. Samples of high-purity copper described by Phillips and Skinnerl9 were supplied through the courtesy of the American Smelting and Refining Co. The high-purity copper rod was used without remelting by cross-rolling to a thickness of 0.075 in., from which disks 7/8 in. in diameter were cut. A good grade of bus-bar copper was used to make the single crystals.

Jan 1, 1942

By L. L. Wyman

THE resultant embrittlement caused by the exposure of oxygen-bearing copper when hot and exposed to reducing gases has been the subject of many studies.1 Little attention, however, has been given to the possible embrittling effects due to atmospheres or conditions that under some circumstances might be the source of a reducing gas. At rather infrequent intervals there occur reports of copper becoming embrittled during normal annealing cycles in commercial steam-atmos-hered furnaces such as customarily are used for this operation. As might be expected, several other factors exist-such as oil, dirt on the wire, or in the furnace, or metallic surface contacts that might produce reducing gases and be the source of the trouble. However, in consider-ation of the statement made by Ruder,2 it would seem that under some conditions steam itself might prove to be the source of trouble. A consideration of the amount of the dissociation of water vapor up to temperatures of the melting point of copper shows that' the amount of hydrogen that could come from this source is far too minute to account for any embrittlement. What such information does not tell is what will happen at the surface of copper when subjected to steam at elevated temperatures, for entirely different conditions may persist, which would account for Ruder's observation. Furthermore, there are no data as to what might happen at the surfaces of other materials present, the result-ant of which might affect the condition of the copper present. For this reason, it was decided to make a series of experiments com-parable to those previously conducted by the writer,1 which would clarify the effect of the steam on copper, and in copper in the presence of steel.

Jan 1, 1940

By G. Derge, Ling Yang, G. M. Pound

The specific conductance and its temperature dependence were measured over the entire composition range of the molten Cu2S-CuCI system. At a typical temperature of 1200°C, 10 rnol pet of the ionically conducting CuCl reduced the specific conductance from about 77 ohm-lcm-l for pure Cu2S to about 32 ohm -1cm -1, and 50 mol pet CuCl reduced the conductance to that for pure CuCI—about 5 ohm 1cm1. The nature of electrical conduction in molten Cu2S, FeS, CuCI, and mixtures was studied by measuring the current efficiency of electrolysis at about 1100°C. The Cu2S, FeS, and mattes were found to conduct exclusively by electrons, but addition of 1 5 wt pet CUS to Cu2S produces a small amount of electrolysis. Addition of CuCl to Cu2S suppresses electronic conduction, and ionic conduction reaches almost 100 pet at a CuCl concentration of about 50 mol pet. These facts are interpreted in terms of electron energy level diagrams by analogy to the situation in solids. RESULTS of electrical conductivity studies on molten Cu-FeS mattes as a function of composition and temperature have been reported.' The specific conductances ranged from about 100 ohm-' cm-' for pure Cu2S to 1500 ohm-' cm-1 for pure FeS. This is in sharp contrast with the low specific conductance of molten ionic salts for which the transfer of electricity is by migration of ions in the field. In general, these ionically conducting molten salts, such as NaC1, KC1, CuC1, etc., have a specific conductance of the order of magnitude of 5 ohm-' cm-'. It was concluded on the basis of this evidence that molten FeS and Cu,S exhibit electronic conduction. Pure molten FeS has a small negative temperature coefficient of specific conductance, resembling metallic conduction, while pure molten Cu2S has a small positive temperature coefficient, resembling semi-conduction. The molten Cu2S-FeS mattes follow a roughly additive rule of mixtures, both with respect to specific conductance and temperature coefficient. Savelsberg2 has studied the electrolysis of molten Cu2S and Cu2S + FeS. He concluded that while molten Cu2S is an electronic conductor, there is some ionic conduction in molten Cu2S + FeS3 owing to the formation of the molecular compound 2Cu2S.FeS and its dissociation into Cu1 and FeS2-1 ions. The present work does not verify his results. Chipman, Inouye, and Tomlinson" have studied the specific conductance of molten FeO and report a high specific conductance, about 200 ohm-1 cm-1 of the same order of magnitude as that found for molten mattes, and a positive temperature coefficient. They interpret these results in terms of p-type semiconduction in the ionic liquid by analogy to the situation in solid FeO.1 imnad and Derne' detected appreciable ionization in molten FeO by means of electrolytic cell efficiency measurements. In order to verify the conclusion that electrical conduction in molten Cu2S and mattes is electronic, and to gain further insight into the structure of molten sulfides, the following investigations were carried out in the present work: 1) The specific conductance, s of the molten system Cu2S-CuC1 was measured as a function of temperature over the entire composition range. As discussed later, molten CuCl is an ionic substance. It was thought that if molten Cu2S were simply ionic in nature, addition of small amounts of CuCl might not have a catastrophic effect in lowering the high conductance of the Cu2S. On the other hand, if much electronic conduction occurs, addition of the ionic CuCl should have a large effect in destroying the electronic conduction. 2) The electrolytic cell efficiency of the following molten systems was measured at about 1100°C in specially designed cells: Cu3; Cu2S + FeS, 50:50 by wt; FeS; Cu2S + CuS, 15 wt pet; Cu2S + CuC1, 5.9 to 46.4 mol pet; and CuC1. This gives a direct measure of the fraction of current carried by ions in these melts. Further, the cell efficiency, extrapolated to zero ionic current, is given by cell efficiency = (s leasile + s elexstronic). [1] s lucile for molten CulS would be expected to be no greater than that for molten CuC1, whose s lonle is about 5 ohm-' cm-1, as will be seen in the following. u,.,,.,.,.......for molten Cu,S is of the order of 100 ohm-' cm-'.' Thus, a large increase in cell efficiency from 0 to values of 10 to 100 pet upon addition of CuCl to Cu2S would indicate destruction of the electronic conductance. Conductance Measurements Experimental Procedure—The apparatus and experimental method were the same as those described in detail in connection with the study of electrical conduction in molten Cu,S-FeS mattes.' A four terminal conductivity cell and an ac poten-

Jan 1, 1957

By B. B. Rath, Hsun Hu

In wedge-shaped bicrystals of zone-refined aluminum it is observed that (111) pure tilt boundaries migrate under the driving force of their own inter-facial free energy. The boundary velocity is a power function of the driving force. The driving force exponent decreases with decreasing angle of misorien-tation. For example, at 64O°C, the exponent decreased from 4.0 for a 40 deg to 3.2 for a 16 deg tilt boundary. An evaluation of the driving force acting on the boundaries during their motion indicates that for low driv-forces, up to about 2 x l03 ergs per cu cm, the velocity is relatively independent of misorientation, whereas at higher driving forces a 40 deg tilt boundary exhibits the highest velocity. The measured activation energy for boundary migration approaches that for bulk self-diffusion at low driving forces, decreasing from 33 to 27 kcal per mole as the driving force is increased from 1 x l0 to 5 x l03 ergs per cu cm. These results are compared with current theories of grain-boundary migration. In previous experimental studies of grain boundary migration the driving force has been limited to a difference in stored energy across the boundary. This stored energy has been introduced into the crystal either by prior deformation1-3 or by grown-in lineage structure. A part of the energy stored in the deformed crystal is released by recovery either prior to or concurrently with grain boundary migration, thus introducing an uncertainty as to the magnitude of the driving force responsible for grain boundary migration. The grown-in lineage structure, though thermally stable during annealing, neither provides conditions under which different levels of energy may be stored in the imperfect crystal nor provides a control of orientation difference across the migrating boundary of a growing grain. Furthermore, because of variation in the lineage structure, it is difficult to determine accurately the energy stored in the imperfect crystal. Several investigations of grain boundary migration during normal grain growth have also suffered from difficulties in estimating the driving force because of uncertainties in the principal radii of curvature.~ In the present investigation the velocity of pure tilt boundaries in zone-refined aluminum bicrystals of selected orientation (40, 30, and 16 deg around the [Ill] tilt axis) has been measured in the absence of a dislocation density difference across the moving boundary, thus eliminating the previous experimental difficulties. The driving force for boundary migration is derived from a gradient of the total interfacial free energy of the migrating boundary in wedge-shaped bicrystals. A similar method was attempted by Bron and Machlin in a study of grain boundary migration in silver. However, they found that one of the crystals was deformed and consequently the motion of the boundary was partly due to a difference of stored energy across the boundary. The observed behavior of boundary velocities as affected by the driving force is examined in the light of the predictions of the current theories of grain boundary migration.7"10 The effect of boundary misorientation on velocity is compared with the theory of " which is based on a dislocation core model for high-angle boundaries. EXPERIMENTAL METHOD Seed-oriented bicrystals of zone-refined aluminum, 2.5 cm wide, 0.5 cm thick, and 12 cm long, containing tilt boundaries with a common (111) axis, were grown from the melt in the direction of this axis. Spectro-graphic analysis, reported earlier,'' indicated the purity of the crystals to be 99.999+pct. Three such bicrystals containing 16, 30, and 40 deg tilt boundaries were used. Wedge-shaped specimens were prepared from these bicrystals by spark cutting followed by electrolytic polishing. The angle of the wedge was usually 40 deg and the specimens were usually 0.25 cm thick. The intercrystalline boundary was located within 0.2 to 0.5 cm from the tip of the wedge. Fig. 1 shows a section of an oriented bicrystal containing an outline of a wedge-shaped specimen. The crystallographic directions shown in Fig. 1 represent the orientation of one of the crystals (the larger section of the bicrys-tal); the orientation of the other crystal differs only by rotation around the common [lil] axis. The parallel faces of the wedge always corresponded to the common (171) planes in both crystals, whereas the orientation of the side faces varied, depending on the misorientation angle. The bicrystal orientations were determined

Jan 1, 1970

By Patrick H. O’Neill

FUNDAMENTALLY a dredge designed for operating under arctic conditions and particularly when the temperature is below freezing is not greatly different than one for use in more moderate climates. Because of the accumulation of ice it is necessary to design suspension units to carry an increased weight when ice forms on the digging ladder or stacker. Winch room and house must be made with double walls and insulated. The dredge must be heated either by steam or by circulating warm air electrically heated. The stacker must be covered and heated to avoid having the drive units frozen tight. Actually the worst trouble that might develop in a stacker, because of cold weather, is the freezing of spilled material and ice accumulation on the head pulley and the underside of the belt. For this reason, stackers are completely enclosed and the pan kept open to get rid of any spilled material and to prevent overloading. Since the stacker is the most vulnerable place on a dredge in cold weather, heat is turned on there long before it is necessary any other place on the dredge. The principal points of interest in' connection with dredging, under subfreezing conditions, concern the preparation of the ground being dredged and the frozen ponds. In the interior of Alaska, and also in the Yukon territory of Canada, most of the gold bearing gravel deposits are permanently frozen and they are also covered by variable thicknesses of fine grained sediment, locally called muck. The better pay areas in this frozen ground have generally been worked by the earlier miners who sank shafts to bedrock in the frozen ground, then drifted in four directions and dug out the areas between the drifts as they re- treated toward the shaft. They thawed only the area they were excavating, doing so with steam from wood-fired boilers, and hoisted pay gravel to the surface for subsequent washing.

Jan 11, 1954

R. F. WOOD,* Sandusky, Ohio.-I made a few tests of gun-metal specimens, after I noticed the results on quenching -reported by the Bureau of Standards. The data of one such test are given herewith. The bars were heat treated and quenched before they were machined, and in all cases they were brought up to 700° or 800°. They became extremely brittle,, showed almost no elongation, except such as was caused by the failure of the pieces to fit together after they were pulled, and the tensile stength was reduced from around 35,000 to about 13,000 lb. per sq. in. In addition, the weakening effect of the quenching seemed to be almost as marked when the bar was allowed to slowly air-cool from red to black, and then quenched, as it was by quenching directly from the red heat. Test Bars.-Rough size, 9/16 in. diam. over test section, grips 13/16 in. diam. Cast two in a flask, one on each side of a block 8 by 4 by 1 in. and fin-gated thereto from the grips but not from the test section. Poured with flask in inclined position, with gate to lower end of block and riser from upper end of each test bar. Bars were machined to ½ in. over the test section, after heat treatment. Casting the Bars.-Charge of 1500 lb. consisting of 400 lb. of new metals and 1100 lb. of G turnings and scrap was melted in open-flame oil furnaces and then poured into a 1-ton ladle. From the ladle 150 lb. was poured into a preheated No. 50 crucible, land from this the flasks of test bars were poured. The six flasks are indicated below by the numbers 1 to 6 and the bars in each flask by the letters a and b, thus 4a and 4h, for instance, were the two bars in flask No. 4.

Jan 12, 1919

By H. A. Saller, F. A. Rough

Studies of the V-U system have been made to determine the constitutional diagram. The diagram is fairly simple, since no intermediate phases are formed. Additions of vanadium lower the uranium melting point and allotropic transformation temperatures. The maximum solid solubility of vanadium in uranium is 12 atomic pct and the maximum solid solubility of uranium in vanadium is about 4 atomic pct. WITH the advent of high purity iodide vanadium,' it became of interest to study the alloying characteristics of vanadium and uranium. Alloys were prepared covering the entire system and were studied using a combination of metallographic examination and thermal and X-ray analyses. As a consequence of this work, the V-U constitutional diagram was evolved. In order to prepare suitable alloys for equilibrium-phase studies, it is desirable to have the purest possible starting materials. For this investigation, calcium-reduced vanadium, de Boer process crystal-bar vanadium, and good Mallinkrodt Chemical Co. uranium were used. The first work was done using the best vanadium then available, that being calcium-reduced vanadium produced at Knolls Atomic Power Laboratory. Subsequently, the important features of the diagram were checked using alloys made with crystal-bar vanadium produced at Battelle. These checks are in agreement with the earlier work. Analyses of the starting materials are contained in Table I. Only minor amounts of any impurities were present in either the vanadium crystal bar or uranium. Nevertheless, care was exercised in selecting the uranium for the alloys. The procedure followed was to section the stock into suitable pieces for melting, and macroetch each piece. Only those pieces which appeared to be clean by macroetch examination were used for alloying. Experimental Procedure Melting: Alloys with 0 to 50 atomic pct V were induction melted in beryllia (BeO) crucibles under vacuum of 10 microns pressure or better. A number of remelts was frequently required to insure uniformity of the individual ingots. Although no visible reaction between the alloy and crucible was found in any of these operations, the alloys were checked by spectroscopic analysis. Only trace amounts of beryllium were detected in the alloys. Alloys containing 50 to 100 atomic pct V were arc melted in a water-cooled copper crucible under an atmosphere of helium. A tungsten electrode was used. Ingots of 10 to 15 g were produced readily by turning and remelting a few times. Such small ingots were necessary because high purity vanadium was not available in appreciable quantities at this time. After melting, the ingots were examined metal-lographically for segregation and were consolidated by remelting before fabrication was attempted. Spectroscopic analyses showed that only small amounts of tungsten were picked up during the arc-melting process. Fabrication of Alloys: Alloys containing up to 20 atomic pct V could be fabricated by rolling in air at 600°C with 5 min between passes. After each pass through the rolling mill the alloys were returned to

Jan 1, 1954