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By Martin C. Kuhn, Lawrence G. Stevens, J. Mark Richardson

The majority of the world's known and anticipated reserves of nickel ores are lateritic deposits At present, there are several different process alternatives for recovering nickel and other desired metal values from laterite ores An overview is given of the selective reduction roast/ammoniacal leach process, one of the processes in commercial operation.

Jan 1, 1981

By G. S. Phipps, E. E. Schumacher, G. M. Bouton

THE seriousness of the present tin scarcity has stimulated large consumers of this vital metal to develop drastic conservation measures in order to extend the available supplies to cover the emergency period. By devising new soldering methods and alloys the Bell System has contributed a substantial share in the tin conservation effort, Fortunately, the changes, as far as can be determined now, have not introduced weakness into the soldered joints. Some of the new procedures were already in the process of development at the onset of the emergency, while others were devised under its stress. In some instances, the newly developed solders were found to be more difficult to use than the alloys previously available, and would not have been introduced under normal conditions. One major change made that previously had been under consideration will result in large savings of tin. Unless service difficulties are encountered, this modification gives promise of remaining after the emergency has passed. The change involves a reduction in the amount of solder placed on a wiped joint between the cable sheath and the sleeve. Instead of the customary full sized wiped joint, a wipe of fillet proportions is formed. Through this change, a solder saving of more than 60 per cent per joint can be realized. Plumbers and cable splicers for many years have joined lead pipes and cable sheath by a soldering process called "wiping." The name is an apt description of the operation. For a wiped joint, the sections to be united' are heated by molten solder poured over their surfaces, and the resulting semiliquid mass is manipulated by wiping with cloth pads to a well rounded symmetrical form like the one shown in Fig. I, The operation requires considerable skill on the part of the splicer and close control of the composition of the solder. At first consideration, the problem of tightness in such joints seems simple but experience shows that even under the best conditions the fissures frequently found in the solder occasionally link and form a path that allows leakage to occur. In telephone cables not maintained under gas pressure, such leaks permit the entrance of water, which wets the paper-covered conductors and thereby impairs the insulation value and causes service interruptions. By going to an extreme and wiping off all the solder in excess. of a fillet, it has been found that many causes of porosity are eliminated. Figs. 2 and 3 show cross sections of joints wiped in the old and the new ways. The saving in solder, and consequently in strategic tin, is evident. The field splicing forces find that joints are easier to make by the new method and are less likely to be porous. The metallurgical considerations that are responsible for the success of the fillet wipe are of interest. Much has been written about the wiping process of soldering cable joints and the many requirements of a good wiping solder have frequently been listed. The success of the procedure described

Jan 1, 1943

By Russell C., Fleming

FOK, many years the officials of the Magma Copper Co. mine at Superior, Ariz., have had to contend with adverse conditions underground in the form of high rock temperatures, hot water, and high relative humidity. These conditions in the mine have been such that working the mine would have been impossible were it not for the constantly expanding and improved sys- tem of ventilation to produce bearable conditions in the working places. Results that have already been achieved make an interesting study of what can be done along those lines. From the time the mine was first opened in 1910 it has been hot. An idea of the conditions that have persistently been encountered can be obtained from parts of the mine that are not being worked at present or that do not yet have sufficient ventilation. Virgin rock temperatures as determined in drill holes at the faces range from 104° to 116°*. An observation made at the face of No. 5 West footwall drift on the 2800-ft. level.

Jan 1, 1930

By Wayne L. Worrell

Thermodynamic data for the stable carbides and oxides of chromium, molybdenum, and tungsten have been critically eualuuted and are used to determine the stable condensed phases at 1 atm total pressure in each metal-carbon-oxygen system. Pourbaix-Ellingham diagrams have been constructed and are used to estimate the minimum temperatures neces.see)*y to oblain these metals by corbolhermic redlrction under reduced pressures. USING recently reported data for the carbides and oxides of chromium, molybdenum, and tungsten, the stable phases in the Group VI metal-carbon-oxygen systems at specific temperatures and pressures can be determined. The thermodynamically stable regions in each metal-carbon-oxygen system can be completely pictured using a Pourbaix-Ellingham diagram in which the two coordinates are oxygen potential (-RT In Po2) and temperature. Worrell and chipman' have described and constructed such diagrams for the metal-carbon-oxygen systems of vanadium, columbium, and tantalum. Downing2 has used similar diagrams to provide a description of the reactions in submerged arc furnaces. One of the examples which he cited was the Cr-C-O system; however, an improved diagram is presented in this paper using recently obtained data for the carbides of chromium. Although some of the oxides and carbides of the Group VI metals exist over slight ranges of composition,3 all solid phases are represented as stoi-chiometric compounds in the subsequent diagrams. Any error introduced into the calculated equilibria by neglecting the compositional variation of these phases is less than the uncertainty in the thermodynamic data. In a Pourbaix-Ellingham diagram for a three-component system, the phase rule requires that at equilibrium four condensed phases specify a point, three condensed phases determine a line, and two condensed phases define an area. To obtain a well-defined area at high oxygen potentials and teniperatures, the initial carbon to oxygen mole ratio is specified to be more than sufficient to reduce the oxide but not enough to convert all the metal to carbide. Thus, the lowest regions in the subse- quent Pourbaix-Ellingham diagrams represent areas in which the metal and its carbide are the stable condensed phases. Cr-C-O SYSTEM A) Thermodynamic Data. To simplify the subsequent calculations, all thermodynamic data are presented in the form of linear Gibbs-energy-of-formation* equations which were derived for the temperature range 505° to 2000°K and are reasonably accurate over the entire temperature ranges of the diagrams. The thermodynamic data for the compounds occurring in the Cr-C-O system are summarized in Table I. Several volatile chromium oxides have been reported,4 but their influence is negligible in the Cr-C-O system. Thermodynamic data for CO and CO2 were taken from the compilation of Coughlin.5 The only solid chromium oxide sufficiently stable to exist below 1800°K in the Cr-C-O system is Cr2Os.11 The Gibbs-energy-of-formation equation for Cr2O3 was obtained by revising the data tabulated in Coughlin,5 using the heat of formation of ah' and the high-temperature thermal data for chromium.7 In 1953 Richardson8 re-evaluated the original work of Kelley and coworkers,9 who measured the thermodynamic properties of the chromium carbides. However, the high-temperature equilibrium results of Boericke9 yield values for ?G°f of Cr2O3 which are 2 kcal more positive than the accepted data. His results for the chromium carbides are based on the same questionable equilibria. Gleiser10 recently determined the Gibbs energy of formation of Cr3C2 and the equation in Table I was calculated from her data and the thermal data of Kelley and coworkers.9 Thermodynamic data for the Cr7C3 and Cr23C6 carbides were obtained by combining the Cr3C2 data

Jan 1, 1965

By B. W. Dyer

IN 1924, the Crescent Eagle Oil Co., while drilling the salt section of the Paradox formation in Grand County, Utah, encountered a salt that did not appear to be sodium chloride. This salt was analyzed and showed the presence of potash minerals, both sylvite (KC1) and carnallite (KMgC12.6H20). Because of the high potash content of the sample, there was considerable speculation: (I) as to whether the hole had been salted, and (2), if not, the extent, richness, and the depth at which the deposit occurred. The discovery caused a large amount of activity in the area. During the next few years, 68 potash prospecting permits were issued by the Government, 24 under the Act of 1917 and 44 under the Act of Feb. 7, 1927, each including about four sections of land. Several holes, all shallow, were drilled for potash. A number of holes were drilled for oil into the salt horizon and the cuttings collected at the oil wells were examined petrographically and chemically. The shallow test holes were not sufficiently deep to reach the potash horizon and revealed nothing of value, but several of the oil test holes gave some indication of where potash might be found. LOCATION AND GEOLOGY OF DEPOSITS The potassium and magnesium salts have been found in various places from the Denver and Rio Grande Western Railroad tracks about seven miles west of Thompsons, in eastern Utah, to Cane Creek, a tributary of the Colorado Rivera distance north and south of about 35 miles. In this locality, there appear to be five separate deposits: the Crescent Eagle area, which is in T. 22 S., R. 19 E.; the Salt Valley area, in the vicinity of the north-south line of T. 23 S., between R. 20 E. and R. 21 E.; the Seven Mile area, in the eastern part of T. 25 S., R. 2o E.; the Cane Creek area, on the Colorado River, in T. 26 S. and T. 27 S., R. 2o E. and R. 21 E.; and the Salt Wash area, in T. 22 S. and T. 23 S., R. 16 E. and R. 17 E. (Fig. I.) The Crescent Eagle and Salt Valley areas are in the Salt Valley anticline, some of the wells being in the fault graben and others outside. Structurally, the Salt Valley anticline is very complex, and can be described in general terms as a northwesterly plunging collapsed anticline about 15 miles long. In the Crescent Eagle area, the valley graben is about 1 mile wide and the salt probably forms a plug, the apex of which is in the vicinity of the Crescent Eagle well. Owing to the complex structure, there has been every opportunity for flowage in the salt to cause local thinning or thickening of beds. The regular succession of formations in the general area* is: [Cretaceous Mancos Dakota Jurassic Morrison Summerville Entrada Carmel]

Jan 1, 1945

By Frank S. McKenna, Myron A. Pugacz, Clarence E. Jackson

THE notched-bar impact test has proved worth while in certain applications as a test for control of the quality or the heat- . treatment of steel. In view of the serious thought that even so simple a test as the tensile test, has evoked during the past years, it is not surprising that the notched- bar impact test should have inspired much experimental work. The correlation of the great number of data has not been successful, although steady progress has been made toward a better understanding of this test. Progress has been made, especially, in the isolation of the effects of the many variables that control the results. The stress system imposed on a specimen with a notch is so complicated and un- predictable that no simple evaluation of the test has been possible. Because of this uncertainty, many engineers hesitate to use the notched-bar impact test, and this attitude may well continue until a better understanding of the effects of the variables in the test are available. Without doubt, any additional data that may be presented should be accompanied by as complete a description of the details of test as possible, so that it may be added to the general fund of information that is to serve as the basis for the theory of the notched-bar impact test. The many factors that may control the test results have been pointed out repeatedly. The importance of the effect of the type and dimensions of the specimen has been recognized. Most of the work reported by American investigators has been limited to small- size (Charpy) specimens tested as a simple beam; two types of notches (Fig. I) have been commonly used. Considerable data have also been presented by many investigators using a small specimen tested as a cantilever beam; this commonly being called the Izod test. Here, however, a shear component of stress makes the stress system even mare complex than that present in the simple beam type of test, hence a critical analysis is difficult. Much work has also been reported by investigators using the tension type of specimen. A second variable that must be con- trolled is the testing temperature. An indication that the tests were performed at room temperature is not sufficient, since in many steels a variation of a few degrees in the actual testing temperature may be sufficient to give an entirely different range of results. Other factors. such as the com- position and condition of the material being tested and the speed of test, should also be considered. Many investigators have contributed data and theoretical discussions on the problems encountered in notched-bar test-

Jan 1, 1944

By H. P. Leighly

WORNER1 briefly studied the embrittlement of titanium by mercury. He found that mercury will wet the titanium surface at 400°C in vacuo, if the specimen had been heated previously to 700°C to dissolve the oxide coating. Subsequent exposure to the atmosphere causes the mercury film to recede rapidly. Bending of the titanium specimen even after the mercury film has receded results in a brittle fracture. For the study of the embrittling effect of mercury on titanium, specimens 2 by 12 by 0.051 in. were cut from RC-130-A sheet, an alloy having a nominal 8 pct Mn content and a mixed a-ß structure. The specimens were stressed horizontally at a predetermined value after which a plastic ring having a cavity 1/2 in. diam by 1/2 in. deep was placed on the specimen. The cavity was filled with mercury and a hole was drilled in the specimen through the pool of mercury. If the stress level was high enough, fracture occurred instantaneously with the drilling. By repeating the test at different stress levels, the threshold stress can be determined. Mercury embrittlement causes a drastic reduction in the ultimate tensile strength of this alloy from 132,000 psi to about 15,700 psi. The drilling of the hole, in the absence of mercury, does not change the tensile properties. Fig. 1 shows the typical fractures observed as a result of the embrittlement of this alloy by mercury. The central portion of the fracture was brittle represented by the jagged region which appears to have occurred on the shear planes at about 45 deg to the stress axis. Ductile fracture, which is perpendicular to the stress axis, occurred near the specimen edges accompanied by a reduction of the specimen thickness. Examination of the fracture reveals that only in the brittle region does mercury wet the

Jan 1, 1962

By L. C. Armstrong

Twice in the past two years and in two widely separated localities—ane near Williamsville, Mo., and the other in the Allard Lake district of Quebec— the Contract Drilling Division of the Longyear Company has experienced perplexing difficulties in drilling granitoid igneous rocks. The rocks in both places are characterized by appreciable amounts of feldspar intimately inter-grown with quartz particles of microscopic dimensions. The disappointingly slow rate of advance and the exceptionally high bortz loss, obtaining during the life of these two projects, are ascribed largely to the resistance to abrasion of these two minerals when arranged in this intergrown pattern. Whether all intergrowth-bearing igneous rocks would offer extraordinary resistance to bit progress cannot be stated with assurance on the strength of these experiences alone. More data on diamond drilling this sort of material in a number of localities are needed before any generalizations can be made safely. It should be pointed out that the lack of time and funds made it impossible for the writer, or other persons interested in correlating the details of bit histories with the kinds of rocks drilled, to be present during the performance of the contracts. However, the records kept in the normal course of drilling are deemed complete enough to be reportworthy. This information is presented here together with the findings made in studies of the rocks involved, with the thought that it may attract the comments of others who may have encountered similar refractory drilling conditions. A pooling of knowledge on the problem would be of material aid in devising more efficient cutting tools and procedures for penetrating this kind of rock. Drilling Blastholes in the Williamsville Granite Due to the unsatisfactory perform- ance of pneumatic percussion drills in boring blastholes on a construction contract near Williamsville, Mo., tests were made with a diamond drill. The poor progress achieved and the excessive loss of diamonds, however, soon led to the abandonment of these trials. The diamonds, in all of the bits tried, lost their cutting edges and acquired a polish after being in service for distances ranging from a few inches to a few feet. Coring bits containing surface-set, whole-stone bortz in a tungsten powder matrix were employed. The cost assignable to bortz wear averaged $7.17 per foot. This item of expense is several times the amount normally expended in diamond drilling in firm, unfractured, granitic rocks. Diamond-impregnated, tungsten carbide bits also were used without success. The diamond wear was at the rate of $0.98 per foot, but the diamond chips became too polished for further duty in less than a foot of drilling. The Williamsville granite is pink and medium-grained. In the hand specimen, it has a fresh, sound appearance; it is seemingly composed almost entirely of interlocking grains of feldspar and quartz and has no discernible features suggesting a greater durability than is usually found in rocks with this composition and texture. Microscopic examination, however, reveals a predominance of feldspar grains with more or less regularly distributed and sharply angular masses of quartz (see Fig 1). The pattern assumed by the two minerals in this mode of occurrence is referred to as a "graphic intergrowth," as it bears some resemblance to the cuneiform characters of ancient Persian writing. The other principal constituents are quartz-free feldspars (microcline and orthoclase) and quartz. All of these constituents are in nearly equidimensional grains, ranging up to about 3 mm in length. There are also

Jan 1, 1950

By F. W. Jessen, R. W. Durie

The dissolution of salt in the development of salt cavities is controlled by free-convection boundary layer flow along the salt surfaces. It is the purpose of this paper to expand upon results published previously, and primarily to illustrate the influence of surface features on the boundary layer and hence the dissolution process in the development of underground salt cavities. General dissolution equations are presented that apply to a surface inclined to the vertical. A salt surface inclined so as to be overlain by water is dissolved by boundary layer flow, while an inverted surface is dissolved by a combination of boundary layer and cellular flow. Detailed investigation of the boundary layer was limited to laminar free-convection flow. Truly laminar free-convection boundary layer flow may be encountered only in laboratory solution cavities, but the boundary layer will control dissolution even where cavity dimensions are such that free-convection turbulence will occur. The factors found to significantly affect the laminar boundary layer will affect dissolution with a turbulent boundary layer. INTRODUCTION Underground salt cavities have been used extensively for the storage of LPG products, and the use of these cavities is expanding each year. The increasing requirements for such cavities suggest the need for a better understanding of the mechanisms involved, for the purpose of the control of cavity geometry and the most effective use of the injected water. A previous paper outlined a quantitative approach to the determination of salt dissolution rates in the laminar free-convection dissolution of salt. It is the purpose of this paper to expand upon the results previously published and to point out significant factors in the application of these results to the dissolution of field cavities. The dissolution of salt in laboratory scale cavities is controlled by the free-convection boundary layer, which is the region of flow along the salt surface caused by the difference in buoyancy forces resulting from the salt dissolution. The transfer of salt into solution at the salt face causes an increase in salinity, and hence a greater density, in the water at the salt surface. The region of higher density tends to fall through the lighter, less saline water and a flowing boundary layer is the result. The water remains stationary at the contact with the salt surface,l so the resulting velocity profile is such that the influence of gravity is opposed by a viscous shear force at the salt surface. For salt to be transferred into solution from a solid surface to a boundary layer of fluid, it must diffuse through a stationary film of water at the salt contact. According to Fick's first law, the rate of mass transfer by diffusion is the product of the diffusion coefficient and the concentration gradient, with diffusion transfer in the direction of decreasing salinity. Once the salt has passed into the boundary layer, it will be transferred by a combination of molecular diffusion and convection. The convection transfer will in turn affect the rate of dissolution by influencing the gradient of the salt concentration at the surface. In the previous investigation by the authors to determine the basic mechanism of the salt dissolution process, an equation was developed that agreed very well with the experimental rates of free-convection salt dissolution from a smooth vertical surface. The technique was taken from the work of Eckert2 in the analogous heat transfer system and will be referred to as the integral method. The rate of salt transfer from a vertical section of height H was found to be:

Jan 1, 1965

By T. D. Tiemann

The extraction of iron oxide from several types of siliceous iron ore by digestion in sulfuric acid solutions was investigated in the temperature range from 80 to 258°F at concentrations from 10-60% H2SO4. Degree and rate of extraction were found to be critical with respect to both temperature and acid concentration, requiring temperatures in excess of 250° F and acid concentrations of 50% to effect 80-90% extraction of iron oxide in 60 min. Rate of extraction is directly related to surface area and apparently controlled by the rate of chemical reaction. The activation energy was found to be approximately 25,000 cal per g mol. Extraction characteristics of the several ores were found to be similar. The Department of Minerals and Metals Engineering at the University of Wisconsin conducts a continuing research program to develop processes for the utilization of low-grade iron ore deposits such as the nonmagnetic taconites of the Wisconsin Gogebic range. Methods under study include high-intensity magnetic and high-tension electrical concentration, flotation, direct reduction and chemical extraction. Concentration of a number of low-grade siliceous iron ores by the extraction of silica in sodium hydroxide solutions has been reported by the writer and others in the literature.1,2,3,4 Residual concentrates containing as much as 65% iron have been obtained from taconites containing less than 30%. Currently an alternative approach is under study, namely the dissolution of iron oxides from siliceous gangue by extraction in acid, with subsequent recovery of the iron from solution. Such a process for extracting iron oxide from the low-grade oclitic deposits of Alberta with hydrochloric acid was investigated and described by Gravenor, Govett and Rigg.5 The current investigation, which is entirely devoted to extraction with sulfuric acid, is the subject of this paper. In part, the objective of this research was to determine the possibility of leaching iron ores in situ with sulfuric acid. The investigation of a recovery method is left to later research. The ores investigated contained hematite (Fe2O3) as the principal iron-bearing mineral and minor amounts of goethite (Fe2O3 .H2O), magnetite (Fe3O4), and iron-bearing silicates. The gangue was essentially quartz occurring as single crystals and microcrystalline aggregates. Detailed description of the ores may be found in the literature.1,2,4,6 A comparison of the specific ores used in this investigation is shown in the partial analyses of Table I. EXPERIMENTAL METHODS All extractions were made at atmospheric pressure using beakers with a mechanical stirrer for those tests run below the boiling point, and Erlenmeyer flasks for those at the boiling point. A thermostatically controlled hot plate was used for heating, and this maintained the mean temperature within the solution to within ±3°F during extraction. The sample of ore for extraction was weighed to + 0.02 g. For tests below the boiling point, the sample was added to the beaker containing the sulfuric acid solution at the desired temperature. For the boiling-point tests, the sample was added to the Erlenmeyer flask followed by distilled water and the

Jan 1, 1968

By T. L. Fritzlen

Extrusion of aluminum alloys in this country is performed mainly by direct extrusion, therefore this paper is confined only to factors affecting the rate of extrusion by this method. Many factors affect the rate of extrusion of aluminum alloys. It is the purpose of this paper to present a discussion on the factors that are subject to technical control. Most of them are closely related, so that a clear-cut distinction between them is rather difficult. However, an attempt will be made to evaluate the effect of each factor separately, as far as possible. The most important factors only will be considered, and these will be discussed in detail under three general headings: (I) characteristics of the equipment, (2) size and structure of the ingot, and (3) temperature of ingot, cylinder, and other parts. It is a well established fact1 that the pressure and the speed of extrusion are related and are exponential functions of one another. Therefore, whenever a certain condition tends, for instance, to increase the pressure required for extrusion, it will reduce the extrusion speed if the pressure is maintained constant. For this reason, in this paper the effect of various conditions is expressed either in regard to their effect on the pressure required or the extrusion speed. Another established fact is the relation- ship between the temperature of the material being extruded and the pressure required to extrude. According to Schi-shokin,= this relationship is of the exponential type, and as the temperature is increased the pressure required is decreased. It would seem from the preceding that the greatest rates of extrusion can be obtained by the use of higher temperatures. However, as is well known, other factors intervene to limit the rate of extrusion of aluminum alloys when increasing the temperature. These factors will be discussed in detail later. Characteristics of the Equipment The capacity of the press determines * the maximum unitary pressure that can be applied for any given cylinder diameter. Pressures used for extrusion of aluminum alloys range from approximately 50,000 lb. per sq. in. to 150,000 lb. per sq. in., dependent upon the alloy and the size of the shape extruded. Higher pressures could be used to advantage, but existing steels limit pressures employed in the production of extrusions. Numerous mechanical characteristics of the extrusion press affect extrusion rate. The most important characteristics of the press itself are: (I) sensitivity of the main pressure valve and accuracy of pressure gauges, (2) accuracy of equipment to heat the cylinder uniformly and to control cylinder temperature, and (3) accuracy of means of measuring the speed of extrusion. The variables subject to control during the extrusion operation are pressure, temperature, and speed, and it is evident that the preceding characteristics

Jan 1, 1946

By T. L. Fritzlen

Extrusion of aluminum alloys in this country is performed mainly by direct extrusion, therefore this paper is confined only to factors affecting the rate of extrusion by this method. Many factors affect the rate of extrusion of aluminum alloys. It is the purpose of this paper to present a discussion on the factors that are subject to technical control. Most of them are closely related, so that a clear-cut distinction between them is rather difficult. However, an attempt will be made to evaluate the effect of each factor separately, as far as possible. The most important factors only will be considered, and these will be discussed in detail under three general headings: (I) characteristics of the equipment, (2) size and structure of the ingot, and (3) temperature of ingot, cylinder, and other parts. It is a well established fact1 that the pressure and the speed of extrusion are related and are exponential functions of one another. Therefore, whenever a certain condition tends, for instance, to increase the pressure required for extrusion, it will reduce the extrusion speed if the pressure is maintained constant. For this reason, in this paper the effect of various conditions is expressed either in regard to their effect on the pressure required or the extrusion speed. Another established fact is the relation- ship between the temperature of the material being extruded and the pressure required to extrude. According to Schi-shokin,= this relationship is of the exponential type, and as the temperature is increased the pressure required is decreased. It would seem from the preceding that the greatest rates of extrusion can be obtained by the use of higher temperatures. However, as is well known, other factors intervene to limit the rate of extrusion of aluminum alloys when increasing the temperature. These factors will be discussed in detail later. Characteristics of the Equipment The capacity of the press determines * the maximum unitary pressure that can be applied for any given cylinder diameter. Pressures used for extrusion of aluminum alloys range from approximately 50,000 lb. per sq. in. to 150,000 lb. per sq. in., dependent upon the alloy and the size of the shape extruded. Higher pressures could be used to advantage, but existing steels limit pressures employed in the production of extrusions. Numerous mechanical characteristics of the extrusion press affect extrusion rate. The most important characteristics of the press itself are: (I) sensitivity of the main pressure valve and accuracy of pressure gauges, (2) accuracy of equipment to heat the cylinder uniformly and to control cylinder temperature, and (3) accuracy of means of measuring the speed of extrusion. The variables subject to control during the extrusion operation are pressure, temperature, and speed, and it is evident that the preceding characteristics

Jan 1, 1946

By Winston A. Wong, John J. Jonas

Commercial purity aluminum was deformed by extrusion over the temperature range 320° to 616°C and the strain rate range 0.1 to 10 per sec. Flow stresses and strain rates were calculated from the experimenLa1 ram pressures and speeds. The stress-strain rate-lemperature relationship in extrusion was found to be similar to that in creep. Extrusion, torsion, compression, and creep data extending over ten orders of magnitude of strain rate and over two orders of magnitude of stress were correlated by a single creep equation. It was concluded that hot-working is a thermally activated process, in which the rate-controlling mechanism is either the climb of edge dislocations or [he motion of jogged screw dislocations. The microstructural changes observed during extrusion were consistent with the proposed deformation mechanisms. ALTHOUGH great progress has been made in understanding the technology of extrusion, very little is known about the actual deformation mechanisms operating during flow. Previous accounts describing extrusion have indicated that the relationship between ram speed (V), pressure (P), and temperature (T) can be given as follows:1 V = apb and P = A' exp(-AT). In these equations, a and b are constants which depend on temperature, A' is a constant which depends on ram speed, and A is a "coefficient" with a different value for each metal. Although these equations have fairly wide application, they do not contribute much to a fundamental understanding of the deformation. Furthermore, extrusion has not hitherto been considered as a thermally activated rate process. This lacuna is surprising because hot-working is similar to high-temperature creep in several respects. There is, in fact, a fair body of experimental evidence suggesting that the material response under hot-working conditions is similar to that occurring under creep conditions, in spite of the many orders of magnitude difference in strain rate.2"4 Since creep has been extensively analyzed in terms of dislocation mechanisms, the comparison of hot-working to creep is useful, for it can suggest the possible deformation mechanisms operating during hot-working. In this paper, the hot extrusion of aluminum will be examined from the point of view of thermally activated deformation mechanisms, such as operate during creep. EXPERIMENTAL PROCEDURE The experimental procedure consisted of extruding commercial purity aluminum* over a range of ram velocities and temperatures at constant die reduction by the direct method. Details of the experimental equipment have been published elsewhere.5 Extrusion was carried out at each of the following billet temperatures: 320°, 376°, 445°, 490°, 555°, and 616°C at the following constant ram speeds: 0.002, 0.008, 0.02, 0.1, and 0.2 in. per sec.* All results were obtained using a square-shouldered die with an extrusion ratio of 40:1, giving a reduction in area of 97.5 pct. The ram force was the dependent variable, and was measured by means of strain gages on the ram and was plotted as a function of ram travel. The sequence of events before making an extrusion was duplicated before each run so as to minimize as much as possible variations in experimental conditions. For example, after the equipment had been assembled, the billet was allowed to heat up to temperature inside the insulated container. Once the container attained the desired temperature, a period of 1/2 hr was allowed to elapse before the extrusion was made. This time was found to be required to allow the billet to reach a steady-state temperature, as determined from previous tests. When all was ready, extrusion was carried out without interruption; that is, the billet was upset and extruded in one operation. EXPERIMENTAL RESULTS AND DISCUSSION The two usual experimental approaches for investigating high-temperature deformation exhibit an important common feature. In the first approach, which corresponds to creep, a constant stress (or load) is applied to the material at constant temperature and the resultant strain is recorded against time. After an initial transient stage, a state of constant strain rate exists (secondary creep), in which a steady-state condition is established which is sensitive to variation in either applied stress or temperature. In the second approach, a constant strain rate is applied and the resultant flow stress is recorded. This corresponds to the situation in hot torsion or hot compression, where it is observed that, for a constant test temperature, there is an initial rise in stress to a steady value which is maintained up to very high strains. In tests of this type, a steady-state region is also established in which the stress is sensitive to variation in either the strain rate or the temperature.3,4,6-16 In both types of tests, therefore, a steady-state region is established after an initial transient. In the case of hot-working this region may be called steady-state hot-working, and it is analogous to steady-state creep with which it has many common features. Stress Dependence of the strain Rate in Extrusion. In order to assess the stress dependence of the strain rate under extrusion conditions, and to compare it to that of creep, as well as of hot torsion and hot compression, the extrusion data were analyzed according to power, exponential and hyperbolic sine creep equations.

Jan 1, 1969

By J. H. Swisher

In measuvements of the solubility of nitrogen in fer-rilic Fe-P alloys, tile nitrogen solubility is found to be Less in pIrospliorus-bearing alloys than in pure iron. The reduction in solubility is about 20 pct in a 1.0 wt pct P alloy at 1300°C and about 30 pct in a 0.23 wt pct P alloy at 440°C. Diffusion coefficient measurements at 1150 and 585°C show that phosphorus also decreases the nitrogen diffusivity in iron. In previous work on the Fe-P-N system, phosphorus was found to reduce the nitrogen solubility in liquid iron slightly.&apos; Indirect evidence for similar behavior in a Fe at low temperature was obtained by Dickenscheid and Brauner.&apos; These authors found that phosphorus reduces the height of the internal-friction peak due to dissolved nitrogen. The results of Dickenscheid and Brauner were confirmed by J. C. Swartz of this Laboratory in a single internal-friction experiment using the same specimen stock as in the solubility measurements described below. In the present investigation, the solubility of nitrogen in a fer rite-stabilized Fe-1.0 wt pct P alloy was measured in the temperature range from 800" to 1300°C. Additional experiments were performed in the temperature range from 440° to 585°C, using an Fe-0.23 wt pct P alloy and NH3-H2 gas mixtures. EXPERIMENTAL The experiments were performed in a vertical tube furnace wound with platinum wire. For experimental temperatures of 800°C and above, a mixture of 5 pct Hz in N2 was used as the reacting gas. The gas mixture was prepurified from oxygen by passage over platinized asbestos at 450°C, and subsequently over anhydrone to remove water. Flow rates of the gases were measured with capillary flow meters. The temperature was measured before and after each experiment with a Pt/Pt-10 pct Rh thermocouple. The specimens used for the high-temperature solubility measurements were in the form of rectangular plates, 0.534 by 1.6 by 3.8 cm. The specimens were cleaned in trichloroethylene and annealed for 2 hr in hydrogen at the beginning of each experiment. In measuring the nitrogen solubility, the specimens were held in the reacting gas until equilibrated, then cooled in a water-cooled copper block at the bottom of the furnace. The time needed for equilibration at 1150°C was determined by measuring the average nitrogen content of the 1.0 pct P alloy as a function of reaction time. As will be described, the nitrogen diffusivity in the alloy at 1150°C is only slightly less than its calculated diffusivity in pure iron. At temperatures other than 1150°C, the reaction time used in measuring the nitrogen solubility was about twice the calculated equilibration time for pure iron at the same temperature. With a few exceptions, the procedure for the low-temperature solubility measurements was the same as that described above. The compositions of the NH3-H2 gas mixtures were determined by collecting gas samples from the gas train and analyzing them for NH3 by titration with HC1. The specimen thicknesses were less than those used for the high-temperature experiments, eg., 0.124 and 0.051 cm for measurements at 585° and 440°C, respectively. Nitrogen concentrations were obtained by chemical analysis, using the Kjeldahl method. The Fe-P alloys were made by adding ferrophos-phorus to electrolytic Plastiron (Type 104 A). Commercial ferrophosphorus, containing 3 pct Mn and 0.35 pct Si as the major impurities, was first purified by melting under an FeO slag. In a separate heat, the electrolytic iron was melted and vacuum-carbon-deoxidized prior to making the ferrophosphorus addition. The principal impurities and their concentrations in weight percent in the 1.0 pct P alloy are as follows: Mn, 0.01; Si, <0.01; C, 0.01; 0, 0.003; and N, 0.0012. The impurity levels in the 0.23 pct P alloy are con-

Jan 1, 1968

By Nicholas J. Grant, David S. Bloom

An investigation of the Cr-Ni system has revealed that there exists a eutectoid transformation at about 1180°C. &apos;The transformation in chromium implied by the eutectoid reaction was detected at about 100°C below its melting point. Associated with the eutectoid transformation, a metastable transition structure has been found. THE Cr-Ni phase diagram is shown in current literature to be a simple eutectic system in which the high chromium end of the diagram is incompletely determined, Fig. 1. The last investigation of this system was undertaken in 1936.&apos; Because of limitations in metal purity, especially of chromium, and temperature measuring techniques, the diagram should be accepted with some reservations, as was indicated by Hansen.V or examwle.-, the wresence of the compound Cr²Ni, with a tetragonal structure," remains unverified and incompatible with the simple eutectic diagram. The work reported here began because of discrepancies that appeared in experimental studies in the binary alloys Cr-Ni and in the ternary system Cr-Mo-Ni. The existing binary Cr-Ni diagram failed to provide a complete explanation of observations made by microscope, X-ray, and thermal analyses. Experimental Methods The materials employed were of a higher degree of purity than were available to previous investigators. The Mond nickel used had a nominal purity of 99.87 pct, while the electrolytic chromium analyzed 99.03 pct with the major impurity being 0.5 to 0.7 pct oxygen with some iron. All alloys were melted in a vacuum furnace to remove dissolved gases, sufficient carbon was added to the charge to combine with all the oxygen as CO. Final analysis determined the carbon as about 0.02 pct and the oxygen around 0.06 pct or slightly more. Stabilized zirconia crucibles and thermocouple protection tips were used throughout and contributed no detectable impurity to the melts, as long as the oxygen in the chromium was kept low. Heats averaged about 250 g, which permitted about 2 in. of the thermocouple protection tips to be submerged. The temperature drop across the thermocouple protection tip was determined to be about 3°C, a minor source of error. The alloys, after removal from the vacuum furnace, were placed in a furnace operating in a purified argon atmosphere for the thermal analyses. An- nealed wolfram-molybdenum thermocouples provided the primary means of temperature determination, though a Pt-Pt-10 pct Rh couple was employed for a check when possible. A sensitive, high-speed Leeds and Northrup Speedomax recording potentiometer indicated the thermocouple output. X-ray diffraction patterns were obtained primarily on a Norelco unit, which permitted diffraction angles only up to 45" (28 = 90"). In general, either rotated or stationary solid samples were used, because it later evolved that many samples were susceptible to transformation resulting from the cold working involved in pulverizing. It was also noted that rotating a sample sometimes suppressed weak lines, so, usually, samples were not rotated. Later a high temperature camera was adapted for use at temperatures up to 1400 °C on the Norelco unit utilizing both solid and powdered samples. Unless otherwise noted, all X-ray patterns were made with a chromium tube and a vanadium filter. Further-

Jan 1, 1952

By George B. Clark

7.1-1. Introduction. The fundamentals of blasting involve both the properties of explosives and of the rock being blasted. While the knowledge of property correlation between rocks and explosives for most effective blasting is far more complete, many quantitative evaluations have been made. Four of the most important explosive properties appear to be energy density, bulk density, rate of energy release, and the pressure-time history of the gases produced. Important rock properties are density and porosity strength, and energy absorption properties, including the effective moduli of elasticity. Rock structure also has a marked effect on its breaking properties, i.e., joints, bedding, fractures, alteration, etc. Several mechanisms enter into rock fragmentation by blasting. These include slabbing, radial fracturing, crushing, and bursting by the gas bubble. All of these factors are closely related to properties of both explosives and rock. Slabbing depends upon the character of the first generated stress wave, whose shape and magnitude are a result of the pressure generated by the explosive, its time history, and the resultant response of the rock, including its ability to sustain the stress wave. Actual slabbing, in turn, is a function of the magnitude and shape of the pressure pulse and the tensile strength of rock. Further fragmentation depends to a great extent upon the amount of gas in the bubble and its energy and pressure. Blasting rounds are best designed by taking the above factors into consideration. This is effectively accomplished by use of cratering curves which relate breakage- parameters to the explosive energy. Optimum depths from single charge cratering curves must be adjusted to changes in shot geometry and related to multiple hole blasting. Blasting damage may occur from either air blast or ground waves, and in the latter ease may be due to direct vibration or to settlement caused by vibration. Technical information indicates that blasting damage is often

Jan 1, 1968

By Gligorije Stankovic

This paper describes the fluo-solids roaster and acid plants at the new 40,000-TPY Trepca electrolytic zinc plant. The electrolytic zinc plant units were constructed to the design of Singmaster and Breyer, New York and began operation in mid-1967. The fluo-solids roaster plant, constructed according to the design of Dorr-Oliver, Paris, includes concentrate handling and storage facilities; two independent concentrate roasting circuits, each with a 110 to 155 TPD fluo-solids roaster; waste heat boilers; cyclones; electrostatic precipitators; calcine coolers; and calcine conveyors. The acid plant uses the "Petersen system" contact process. The plant has one acid circuit with a capacity of 230 tons of monohydrate per day. Gases for the acid plant are obtained from roasting zinc concentrates. When the roaster plant is operating at maximum capacity, excess SO2 is used in two other Petersen System circuits in the near vicinity.

Jan 1, 1970

By James C. Word, R. M. McLouski

This paper will describe the development and application of large-scale integration techniques employed in the fabrication of a germanium multielement array. The array consists of 100 by 228 PNP bipolar transistors fabricated on 5 mi1 centers. Back-biased p-n junction techniques are used for electrical isolation of the individual elements. The end use of the array is a high resolution, large area IR sensor. The monolithic array is fabricated in 1 ohm-cm p-type germanium epitaxially deposited on 6 ohm-cm n-type substrate. Epitaxy was accomplished through the hydrogen reduction of germanium te trachloride. Di-borane was used as the dopant. Base regions are achieved by the diffusion of arsenic from doped oxide or arsine sources. Oxide-masking of the arsenic im-pzlvity was achieved by the chemical deposition of a boron doped glass. The emitter is formed by an aluminum alloy diffusion technique. Vacuum deposited aluminum is used for the emitter, interconnections, and for the contact and bonding pads. ALTHOUGH a great volume of literature pertaining to the development of large scale integration techniques (LSI) has been published for silicon and in particular silicon imaging applications,&apos; to date only a small number of similar devices have been constructed using germanium technology.&apos; Since the physical and chemical properties of germanium are vastly different from those of silicon, the fabrication technology for integrated structures in germanium is also different from that of silicon. In particular germanium does not possess a stable oxide as can be grown on silicon by heating in an oxidizing ambient for masking of dopants and passivation. This paper describes the application of germanium LSI techniques employed in the fabrication of a multielement infrared sensor array. The array is used in a high resolution, large area infrared sensor for operation in the 0.8- to 1.5-u spectral range. Back biased p-n junction techniques are used for electrical isolation of individual elements. Discrete germanium devices have been fabricated routinely for some time. However, mainly due to the lack of a suitable mask for selective doping and the high current leakages inherent in germanium p-n isolation, few monolithic germanium structures have been constructed. THE INFRARED MOSAIC A cross-sectional view of the array is shown in Fig. 1. The monolithic structure consists of 12,800 PNP transistor elements in a 100 by 128 matrix fab- ricated on 5 mil centers. The emitters of each line of transistors are connected together using aluminum interconnects while the strip collectors are connected together in series at right angles to the emitter lines. The selection of this structure is dictated by the readout technique involved. Access to each element transistor is obtained by applying a bias voltage to a particular collector strip and separately interrogating each emitter row. A charge storage, i.e., an integration mode is used for reading out this particular array Construction techniques available for use with germanium do not include a selective p-type diffusion capability for surface concentrations greater than 10" per cu cm and junction depths greater than about 10 u. This fact limits the type of structure that may be used. Therefore, an array of PNP transistors that did not employ p-type diffusions was chosen. The structure was fabricated by growing a 1 ohm-cm p-type epitaxial layer on a carefully prepared 6 ohm-cm n-type substrate. N-type dopants were used for the isolation and base diffusions and alloyed aluminum was used to form the emitter junctions. The array was then completed by evaporation of aluminum interconnections and contact pads. SUBSTRATE AND SUBSTRATE PREPARATION Germanium substrates of (111) orientation grown by both Czochralski and zone leveling techniques were utilized for mosaic fabrication. Czochralski substrates were preferred because of the lower dislocation densities available in this type of material. Dislocation densities for the Czochralski material were typically less than 3000 per sq cm, while those for the zone leveled material were typically less than 5000 per sq cm. All substrates were uncompensated to minimize thermal conversion problems in subsequent epitaxial and diffusion processing. Both in-house and vendor polished wafers were used. The in-house polishing technique employed consisted of an initial gross chemical etch in CP4 to remove saw damage from both surfaces. This was followed by a chemical-mechanical polishing operation of one side of the wafer. The chemical-mechanical polishing solution used was Lustrox 1000 (Tizon Chemical Co.), and consists of zirconium dioxide, sodium hypochlorite, water and a surfactant. The wafer thickness before and after polishing was typically 0.020 and 0.010 in, respectively. THERMAL CONVERSION The problem of thermal conversion of both the substrate and epitaxial layer was particularly acute because of the relatively low carrier concentrations employed in both regions. This problem has been encountered by other workers in the past.3 Without special treatment before epitaxial growth substrate conversion (n-type to p-type) and changes in the re-

Jan 1, 1970

By L. L. Wyman

Previous studies1 by the writer dealing with the embrittlement of copper have been concerned with the behavior of various pure and deoxidized coppers when exposed to an oxidation-reduction cycle, and the consequent evaluation of these materials on the basis of their resistance to this action. No attention was devoted to the variations in penetration of embrittlement with time, when these copper materials are exposed to a strong reducing gas, such as hydrogen, nor to the variations in oxygen penetration, with time and temperature, into the "pure" coppers. The cause of the embrittlement is the reduction of the oxygen in the copper by the hot reducing gas, so that a consideration of time, temperature, the occurrence of hydrogen and oxygen must be given. For the purpose of differentiating some of the involved factors, the present work may be divided into two separate series of experiments. The first of these deals with the oxidation of purified coppers under various conditions and then the subjection of these to a standard hydrogen treatment. The second series concerns the reduction, under different conditions, of tough-pitch coppers of several oxygen contents. The resulting data will give the rates of oxidation, and of reduction, for the materials involved. The first series of experiments will reveal how rapidly copper may become oxidized, while the second series will indicate how rapidly embrittlement will penetrate into an oxygen-containing copper when it is exposed to hydrogen at different temperatures. Materials For the purpose of determining these variables, three types of material were selected, to cover the extremes in the ranges of materials commercially obtainable. The first class of materials is represented by an oxygen-free copper, as well as the high-purity vacuum-melted copper2 used in previous work. These materials were selected to determine the variation of oxidation with time and temperature, by oxidizing these coppers under various combinations of these factors, and noting the effect as indicated by a

Jan 1, 1934

By Thomas M. Price

Sand production for use in hydraulic concrete is probably the most important element affecting the physical characteristics of the resulting concrete in the opinion of most engineers, aggregate producers and contractors of today, who are engaged in the effort to produce stronger concrete per unit of cement used. Their opinion is based on both laboratory and field results. In the past, proper cement production has been the object of most of the study given this subject and while it is still studied by the extensive and well equipped laboratories that are a part of every cement mill, as well as by all governmental laboratories, at the present time the object of most of these studies has been in the field of low heat and quick setting qualities rather than the effect on the strength of the concrete. It is recognized that concrete must have two important qualities; namely, workability with the least water possible, and uniformity. These qualities have been accepted as axiomatic and possible to obtain if the foreman in charge knew his business. Now, however, with concrete produced by plants that mechanically weigh and chart all the ingredients, including water, of a batch of concrete, the foreman cannot cut and fit his aggregates, cement and water to fit his own desires and the secret of the important qualities of workability and uniformity are found to lie largely in the sand, hence the attention given its production at the present time. With this condition in mind the engineers of the United States Bureau of Reclamation and the Six Companies Incorporated in designing the plant for producing the aggregates for the Boulder Canyon Project included every possible means for the production of a sand of a constant and acceptable fineness modulus as well as a constant moisture content, and for attaining these results with as few detrimental ingredients, like silt and vegetable matter, as possible. This aggregate plant (Figs. 1 and 2) is in Hemenway Wash, 7 miles north of Boulder City. It is 4 miles upstream from the low-level mixing plant. At this screening plant 8,234,000 tons of raw aggregate are being

Jan 1, 1934