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By R. W. Fountain, W. D. Forgeng, G. M. Faulring

Precipitation of the phase Co3Ti (Cu3Au type) from a Co-5 pct Ti a11oy has been investigated using single-crystal X-ray diffraction techniques. Oscillation and transmission Laue patterns of specimens aged for short-time periods at 600" C indicate the formation of titanium-rich and titanium-poor zones coherent with the {100} matrix planes. Longer aging times at 600° C establish that the equilibrium phase also forms on the {100} matrix planes as platelets. These observations are corroborated by electron metallography; electron diffraction studies show the phase Co3Ti to be ordered. A probable sequence of the precipitation reaction is discussed. A previous publication by two of the present authors reported on the phase relations and precipitation in Co-Ti alloys containing up to 30 pct Ti.1 The results of this investigation established the existence of a new face-centered cubic inter metallic phase, ranging in composition from about 17.0 to 21.7 pct Ti at temperatures below 1000° C The decomposition of the fcc supersaturated solid solution was studied employing hardness and electrical resistivity measurements. The changes in hardness upon precipitation in alloys containing 3, 6, and 9 pct* Ti were found to be associated with an initial increase in hardness followed by a plateau and then a second, more pronounced hardness increase. Investigation of this behavior by electrical resistivity measurements suggested that two different kinetic processes were involved, which, when interpreted in terms of the kinetic relation,2-4 indicated that initial precipitation was in the form of thin plates. On continued aging, the plates impinged during the growth process. The general features of these findings have been confirmed by Bibring and Manenc,5 while, in addition, they report the phase to be ordered. The present investigation was undertaken to provide more definite information on the structural relationships between the precipitate and the matrix. EXPERIMENTAL PROCEDURE Single crystals of a (20-5 pct Ti alloy were prepared from the melt employing the Bridgman technique. Poly crystalline rod, 1/2 in. in diam, prepared from vacuum-melted material, was machined to 3/8- in. diam to remove any surface contamination that may have resulted from hot-working. The crystals were grown under a purified hydrogen atmosphere in high-purity alumina crucibles heated by induction. Considerable difficulty was encountered in attempting to grow monocrystals because of the high melting point of the alloy and the high solute concentration. However, one crystal about 6 in. long was obtained which was essentially a single crystal except for one or two very small grains around the periphery. The as-grown crystal was solution heat-treated for 24 hr at 1200°Cin a purified argon atmosphere and water-quenched. One-quarter-in. slices were taken from each end of the solution heat-treated crystal for chemical analyses, and the remainder of the crystal was mounted and oriented by the back reflection Laue Method. The chemical analysis of the crystal was as follows: Pct Ti Pct 0 Pct C Pct N Pct H Pet CO 5.29 0.08 0.004 0.002 0.0003 Balance By proper tilting of the crystal, it was possible to obtain slices 1/32 in. thick of [loo] and [110] orientation. The solution heat-treated crystal slices were sealed in silica capsules for the aging treatments, with titanium sponge placed at one end of the capsule to act as a getter. All slices were water-quenched from the aging temperatures, the capsules being broken under the water to ensure a rapid quench. Thinning of the slices for transmission X-ray studies was accomplished by a combination of mechanical and electrolytic techniques, the final thickness being about 0.1 mm. Laue patterns of the solution heat-treated crystal indicated that no strain was introduced by the thinning technique. ELECTRON METALLOGRAPHY After X-ray examination, the structural changes attending the precipitation were followed by examination of direct carbon replicas of polished and etched surfaces of the single-crystal slices and extracted phases. The earliest indication of significant structural change was observed after aging at 600°C The structure of a heavily etched, solution-treated crystal is shown in Fig. l(a). Aside from the etch pit pattern, no regularity of background structure is observed. On the other hand, in the background of the specimen heated for 500 hr at 600°C, the etching pattern shows a directionality indicating the influence of minute precipitate particles, Fig. l(b). On electrolytic dissolution of this specimen in 10 pct HC1 in alcohol, a large volume of very small, flattened cubes

Jan 1, 1962

By M. Herman, G. J. London

A series of dilute Fe-Co alloy specimens were prepared from zone-melted iron. The iron used was given ten floating-zone passes in purified hydrogen. Alloying was accomplished by plating a gradient of metallic cobalt onto a 1/4-in.-diam bar of material from a pure plating bath. The deposit was radioac-tively tagged by a small addition of co80 to the plating bath. Alloy homogenization was accomplished by passing an additional floating-zone pass through the plated section of the bar. The final concentration gradient achieved was from residual to about 1000 ppm (0.1 pct) added Co. After homogenization, the bar was swaged to 0.057 in. wire and cut to tensile specimen blanks 1-1/16 in. long. Each specimen was counted in a well-type scintillation counter. The concentration of cobalt was computed by combining the normalized specimen counting rate with the known weight (measured to the nearest 0.01 mg) of cobalt added during plating. Fig. 1 shows the cobalt gradient obtained, exclusive of residual cobalt which was estimated by neutron-activation analysis to be approximately 50 ppm. Results of recrystallization for 1 hr at 750°, 700°, 650°, and 600°C with specimens containing 40, 170, 470, and 870 ppm added Co are shown in Figs. 2, 3, 4, and 5. Recrystallization was accomplished in a dynamic vacuum of less than 1 x 10 torr. The specimens were mounted and polished parallel to the swaging direction. The recrystallization re- sults show a radical coarsening of structure with increasing cobalt concentration. The coarsest structure obtained was at the 470-ppm level (at all recrystallization temperatures) with a slight grain refinement at the 870-ppm level shown. A more normal solid-solution effect is seen in Fig. 5 (60OoC, 1 hr) where the only specimen completely recrystallized is the one containing 47 ppm Co. Since the possibility existed that some atmosphere-contamination phenomenon might be responsible for the observed results the recrystallization series was repeated using sealed quartz capsules. These were filled with purified argon which was gettered during heat treatment on metallic titanium included in the capsules. The results obtained were essentially the same as shown. Another identical alloy was made using a 5-mm-diam bar of Westinghouse Puron. Specimen preparation and recrystallization treatment were also as described. The results obtained (see Table I) were somewhat erratic. Some coarsening in structure does appear at the highest cobalt concentrations. There is no apparent relationship between the coarse, columnar, directionally solidified structure of the as-melted bars and any of the recrystallized grain structures observed, all of which are much finer than the former structure. A recrystallization process can be most simply described as one of homogeneous nucleation of recrystallized grains in a cold-worked matrix followed by more or less uniform growth of the strain free grain into the cold-worked material.' An impurity element may influence one or both of these processes. Aust and utter' have shown that impurities strongly influence grain boundary mobility in lead. Moreover, definite recrystallization textures are produced by small concentrations of tin,3 while additions of silver or gold4 produce large boundary in-

Jan 1, 1964

By John W. Cabot

In the manufacture by the Bessemer process of soft steel suitable for rolling into fine sheets, tubes and 60 forth, a difficulty is sometimes met with, in the tendency of this kind of metal to rise violently and boil in the moulds while being cast; this results in hollow-topped ingots, and consequently in an undue amount of scrap in the subsequent rolling. It has been noticed that this peculiarity does not pertain to all pig-irons, some grades producing a blown metal which pours quietly, while others, in whatever way the blow may have been conducted, give a metal which rises in the moulds, accompanied by the evolution of large quantities of hydrogen and carbonic oxide gases, and requiring a long time to solidify. This difference in behavior has been some-

Jan 1, 1891

By T. M. Chatard, Cabell Whitehead

The Republic mine, situated forty miles from Marcus, a station on the Spokane Falls and Northern Railroad, in the northeastern part of the State of Washington, was located in 1896, but no development-work was dolie until the spring of 1897. While much of the ore mined since then has been rich enough for shipment to smelters, a method of locally treating the lower-grade ores soon became a matter of prime importance, because only about 40 per cent. of the values could be recovered by plain amalgamation, even with ores assaying 4 to 5 ounces of gold per ton. Experiments with cyanidation, in various ways, led to the adoption of the Pelatan-Clerici process and the erection on this system of a 10-ton experimental plant, which was later increased to a capacity of 35 tons per day. The extractions by this process showed much improvement over previous work, especially when the ore was crushed to

Jan 1, 1901

By J. L. Gillson

Historically, rock deposits and sand deposits of titanium minerals came into production about the same time, although there may be some argument as to what is meant by production. Beach deposits of heavy minerals in India (Figs. 1-4) and Brazil (Figs. 5) were worked for monazite about the turn of century, but as there was then no market for titanium minerals, these were thrown away. The rock rutile deposits at Roseland, Va., Fig. 6, were worked to supply rutile for titanium chemicals and for coloring ceramics long before there was a titanium pigment business. The pigment industry started about the middle twenties, both in Europe and the U. S., and almost simultaneously the rock deposits at Ponte Vedra Beach near Jacksonville, Fla., were worked for titanium content. Since those days, production from both types of deposits has continued to grow at a rapid rate; many deposits of both types have been found, and reserves have grown to very large figures. In total tonnage of reserves, there is no doubt that the rock deposits are far ahead of the sand deposits; nevertheless there is a very large tonnage of commercial sands available. It is the quality of titanium mineral in the sand and the relatively lower costs of operating sand deposits that have kept them abreast, at least in annual tonnage produced, with the rock deposits. The principal titanium mineral used is ilmenite, but as soon as that mineral began to be sought as a titanium ore, it was obvious that there are ilmenites and ilmenites. Textbook ilmenite should have the composition FeOTiO2 and should analyze 52.6 pct TiO2 and 36.8 pct iron as Fe. The Indian ilmenite, for almost a generation the standard ore for manufacturing pigment in the U. S., was found to analyze about 60 pct TiO, and only 24 pct. Fe, and most of the iron is in the ferric condition. The whole process of pigment manufacture in the U. S. was built up on the use of a raw material of that grade, and the American chemical engineers who operate the pigment plants shuddered at the thought of using a rock ilmenite with 45 pct or so of TiO, and nearly 40 pct Fe. Intensive search was made around the world to find other deposits of rich black sand, like the Indian beaches, but although a few were found, there was some objectionable feature about each. A deposit in Senegal, south of Dakar (Fig. 7), was worked for a while, but an organic coating on the grains made attack by acid difficult. Modern practice would have included a scrubbing operation, in a caustic soda bath, to eliminate the organic coating. Brazilian deposits were numerous, but individually small, and shipping from them difficult. Deposits on the east coast of Ceylon had many attractive features, but the ilmenite analyzed only 54 pct TiO2 and could have been used only with a penalty. Sand deposits with 2 pct ilmenite, like those now worked in Florida, would not have been considered commercial ore, even if they had been known at that time. Most rock ilmenites are associated or mixed with hematite or magnetite, which accounts for the lower titanium and higher iron values than in the sand ilmenites. The Norwegians, English, and Germans, with cheap Norwegian rock ore at hand, learned to install in their pigment plants adequate capacity on the black side, as it is calltd, and counterbalanced the extra cost of plant, and larger amount of acid used, by the lower cost of ore. When World War II arrived, two of the largest pigment manufacturers in the U. S. had to learn how to use the Adirondack ilmenite, but one of them very gladly went back to sand ores when the Florida deposits came into large-scale production after the war. The other continues to use Adirondack ilmenite and finds it commercially attractive to do so. Rutile is not a raw material for titanium pigment manufacture by the sulfate process, since it is insoluble in sulfuric acid. In addition to its small consumption in chemicals and ceramics it began to be used in quantity in welding rod coatings. With the outbreak of World War 11, and the tremendous need for welding rods in shipbuilding and other structural steel construction, rutile suddenly became in heavy demand. The sand deposits on the eastern shore of Australia (Fig. 8A) which had been worked in a small way since 1934 were brought into production, and some stream placers in Brazil were worked and rutile concentrates shipped to American

Jan 1, 1960

By R. B. Hoy, Stanley J. LeFond, K. Reckling

Reported world production of natural diamonds approximates 40,000,000 carats a year (1980). The Republic of Zaire is the leading producer, with an output which is primarily industrial rather than gem grade. The USSR ranks second, the Republic of South Africa third, and Botswana, fourth. Diamonds are also mined in South-West Africa (Namibia), Angola, Ghana, Sierra Leone, and other African countries. In the western hemisphere, Brazil and Venezuela are the principal producers (Fig. 1). A very small output of diamonds is mined today it India, which was the first source of commercial production. In the US, efforts at commercial diamond mining have been confined to a small area near Murfreesboro, AR. The first diamond was found in a kimberlite pipe there in 1906. Small-scale trial mining has not, however, proved economical. Since diamonds were first discovered over 2,000 years ago, only about 260 tons have been mined. In order to obtain I g (5 carats) of diamonds, it is necessary to remove and process approximately 25 tons of rock. Recovering this small percentage involves a combination of highly developed techniques in mining, quarrying, and earth-moving, and extremely sophisticated recovery processes. End Uses Diamonds are used for two unrelated end uses; gem diamonds are jewels of great beauty while industrial diamonds are essential materials of modern industry. Although imitation stones are substituted for the gem diamond, none of these matches its properties sufficiently well to offer real competition. Synthetic industrial diamonds are now of a quality and size that permit them to be substituted for natural diamond in numerous industrial applications. For example, synthetic diamonds are available today in sizes up to 100 stones per carat (14/16 US mesh size). In addition, polycrystalline synthetic diamond inserts, such as De Beers Syndite®, General Electric's Compax® and Stratapax® and Megadiamond's Megapax® have replaced natural diamond in turning tools, mining and oil drilling bits and dressing tool applications. Gem Diamonds A diamond is a natural prism. It has the ability to bounce light rays (reflection), to bend them (refraction), and to break them into all colors of the rainbow (dispersion). This ability to modify light gives the diamond three characteristics for providing beauty. First is brilliance, the reflection of light back to the eye. Second is fire, dispersion of light into the colors of the spectrum. Third is scintillation, the "twinkling" that occurs when the diamond is moved (Bauer, 1969). The skill of the diamond cutter is required to unlock the brilliant, fiery beauty of a gem diamond (Fisher, 1966). Diamond-cutting skills have gradually developed over the centuries. The first cutters, in India, learned how to grind one rough diamond against another to remove their "skins" and to give them various shapes. This revealed some fire and beauty, but little compared to that of the diamonds that are cut today.

Jan 1, 1983

By A. W. Gauger

It is with some trepidation that I approach my subject, for I know that I shall at once incur the suspicion of the mechanical engineer, with his concern for boiler tests and efficiencies; of the mining engineer, with his mechanization problems; and of the chemical engineer with his unit processes. Nevertheless, it must be recognized that the technology of fuels, the systematic body of knowledge relating to the production, processing and utilization of mineral fuels, has grown to such proportions and involves so many widely diverse applications of fundamental science and engineering that it behooves us to stop and consider just what its status is in relation to other technologies, as well as in relation to the present and future needs of the social order. The time has come when technologists, applied scientists and engineers must consider the possible effects that their achievements may have on Society. The development of a machine to - -replace -several hundred men is a fine achievement when considered solely from the point of view of creative endeavor. But what of the men who are displaced by the machine! Does not the responsibility for the development of this machine embrace as well the consequences of obsolescence and technological unemployment resulting from such development? I believe that it does and that we must recognize this fact in our practice of engineering and tech- nology as well as in the training of future engineers and technologists. Magnitude of the Fuels Industry Fuel technology is the body of knowledge that relates to the mineral fuels. The fuels industry is by far the most important of all Our mineral industries. The chart in Fig. I, reprinted from U. S. Bureau of Mines Information Circular No. 6643, indicates the compartive values of metals, fuels and other nonmetallic minerals for the year 1929. Of the grand total of 13¼ billions of dollars in value of minerals at the mines, the mineral fuels contributed 48 per cent. Coal, with 34.4 Per cent, exceeded the value of any other single mineral. In fact, the value of the production of the Pennsylvania anthracite mines alone anand exceeds the value of the gold production of the entire world. Petroleum and natural gas in 1929 contributed 14.3 per cent and 3.3 per cent, respectively, of the total value of world mineral production. So much for the world picture; let us now look at the situation in the United States. Over the 60-year period 1880 to '939, $46,409,727,000 of metal1ic products, $80,788,852,000 of fuels (coal, petroleum, natural gas, natural gasoline) and $27,871,-ooo,ooo of nonmetallic minerals other than fuels were produced. The mineral fuels have contributed 52.7 per cent of the entire mineral wealth produced over this period that has seen such tremendous industrial development in our Our As a matter of fact, our present industrial civilization has been made possible through the use of the

Jan 1, 1942

By A. W. Gauger

It is with some trepidation that I approach my subject, for I know that I shall at once incur the suspicion of the mechanical engineer, with his concern for boiler tests and efficiencies; of the mining engineer, with his mechanization problems; and of the chemical engineer with his unit processes. Nevertheless, it must be recognized that the technology of fuels, the systematic body of knowledge relating to the production, processing and utilization of mineral fuels, has grown to such proportions and involves so many widely diverse applications of fundamental science and engineering that it behooves us to stop and consider just what its status is in relation to other technologies, as well as in relation to the present and future needs of the social order. The time has come when technologists, applied scientists and engineers must consider the possible effects that their achievements may have on Society. The development of a machine to - -replace -several hundred men is a fine achievement when considered solely from the point of view of creative endeavor. But what of the men who are displaced by the machine! Does not the responsibility for the development of this machine embrace as well the consequences of obsolescence and technological unemployment resulting from such development? I believe that it does and that we must recognize this fact in our practice of engineering and tech- nology as well as in the training of future engineers and technologists. Magnitude of the Fuels Industry Fuel technology is the body of knowledge that relates to the mineral fuels. The fuels industry is by far the most important of all Our mineral industries. The chart in Fig. I, reprinted from U. S. Bureau of Mines Information Circular No. 6643, indicates the compartive values of metals, fuels and other nonmetallic minerals for the year 1929. Of the grand total of 13¼ billions of dollars in value of minerals at the mines, the mineral fuels contributed 48 per cent. Coal, with 34.4 Per cent, exceeded the value of any other single mineral. In fact, the value of the production of the Pennsylvania anthracite mines alone anand exceeds the value of the gold production of the entire world. Petroleum and natural gas in 1929 contributed 14.3 per cent and 3.3 per cent, respectively, of the total value of world mineral production. So much for the world picture; let us now look at the situation in the United States. Over the 60-year period 1880 to '939, $46,409,727,000 of metal1ic products, $80,788,852,000 of fuels (coal, petroleum, natural gas, natural gasoline) and $27,871,-ooo,ooo of nonmetallic minerals other than fuels were produced. The mineral fuels have contributed 52.7 per cent of the entire mineral wealth produced over this period that has seen such tremendous industrial development in our Our As a matter of fact, our present industrial civilization has been made possible through the use of the

Jan 1, 1942

This issue presents the first of several articles making up the Bump Symposium, which was held at the 1958 Annual Meeting of AIME. Other Symposium papers will appear in the September issue of Mining Engineering. THE term mountain bump describes the sudden rupture of one or more coal pillars under excessive stress. These bursts occur with varying degrees of violence and sometimes include adjacent strata, especially the bottom rock. Many failures do not develop enough violence to be dangerous and are regarded as an aid to coal production, but severe occurrences are accompanied by tons of flying coal, dense clouds of dust, and excessive gas emission. Such bursts sometimes throw heavy machinery several feet. Major factors to be considered in the problem are the nature of the strata above and below the seam and the depth of cover. Bumps are classified as to their nature, extent of damage, and point of occurrence, e. g., face bump, coal bump, high side bump, low side pavement bump, and district bump. The problem is extremely complex, and it cannot be over-emphasized that preventive measures, if they are to be successful, must be based on a thorough study of conditions in the individual mine. In western Canada, for example, the McGillivray mine, operating in a 9-ft seam at 2000 ft, has experienced severe bumps, but there have been no occurrences in the International mine, which operates in the same coal seam at 2400 ft, where the coal averages 17 ft thick. Differences in conditions governing the operation of these two mines are described in one of the following articles (see page 883). Again, most bumps in coal mines take place along pillar extraction lines, but at the Sunnyside mine in Utah they also occur a long way from active workings and sometimes in virgin territory. It is usual, too, for such failures to occur under fairly deep cover. But at Sunnyside, to cite only one instance, there have been disturbances along the main fault zone under less than 500 ft of cover. All too often conditions favorable to bumps are revealed only by actual mining—at Springhill No. 2 mine, drilling in roof and pavement strata disclosed a 60-ft sandstone bed after operations had started— and where extraction has advanced too far for preventive measures to be incorporated in the mining plan, districts have had to be abandoned. But in an era when premium ores are being rapidly depleted in the face of rising demands, abandonment is not easily justified. There must be systematic planning to eliminate coal mine bumps, insofar as this is possible. As in the Gary district of West Virginia (see page 888) much has been accomplished by planned operations based on known factors in bump control. But even this is not enough. Precise instrumentation is needed to indicate where bumps are likely to occur, and in both the U. S. and Canada stress analysis studies are being carried out with this object in view. These pages reveal the progress being made.

Jan 1, 1959

By T. E. Seidel, A. U. MacRae

The dependence of the electrical and crystalline properties of silicon containing ion implanted boron atoms have been studied as a function of the incident dose, substrate temperature, and annealing tempera-ture. Hall effect studies show that the compensation due to defects is negligible after annealing at and above 500°C for a dose of 1013 ions per sq cm. Steps occur in the isochronal annealing curve for the sheet resistance at 300°C and 800°C and the mechanisms responsible for these steps are discussed. The range of the ions at 150 kev is 3500 * 5001. Electron diffraction studies on samples implanted with 150 ker ions show the existence of damaged (polycrystalline) silicon closer to the surface than the range of the ions. Etching and subsequent annealing of etched and unetched specimens suggest that the poly crystalline silicon is closer to the surface than the bulk of the distribution of ions. THE purpose of this study is to investigate some electrical and crystalline properties of ion implanted boron in silicon. Sheet resistance, Hall measurement, depth distribution by chemical staining, thermal probe and electron diffraction have been used to study the properties of samples implanted in a random direction with ions having energy up to 150 kev. The boron-silicon system has been the subject of considerable study'-7 due to its possible application in the fabrication of electronic devices. The implanted ions produce considerable crystalline damage to the substrate crystal before they lose most of their primary energy and come to rest. Fortunately, most, if not all, of this damage can be removed by subsequent annealing or by holding the substrate at an elevated temperature during the implantation process. Sheet resistivity measurements of the p-type layers produced by boron implantation into room-temperature silicon, reveal that the annealing occurs in a two-step process: the first occurring at -300°C and the second at -800°C.' Electron-microscope and low-angle electron diffraction studies of this damaged material indicate that the bombarding ions produce an amorphous silicon region about the trajectory of each ion.' At high doses, these damaged regions overlap and an amorphous surface layer results. Furthermore, the 800°C annealing step, appears to be associated with the elimination of this gross damage. The depth distribution of the as-implanted and also the annealed samples have been studied by an angle lap and staining technique as well as by Hall measurements.3-7 We find the experimentally determined ranges of the boron are less than those calculated by the Lindhard-Scharff-Schiott theorys (hereafter referred to as the LSS theory). Our results are in essential agreement with pre- vious results. In addition, we have made Hall measurements on samples bombarded with a low dose (2 x 1013 ions per sq cm) to minimize impurity banding effects, and find that deep ionized levels influence the carrier concentration and room-temperature hole mobility until the sample is annealed at temperatures above 500°C. Above this temperature, the data corresponds to that obtained when silicon is doped with boron by conventional techniques. We have also made a depth distribution determination of the crystalline damage due to the implanted boron by using glancing angle electron diffraction techniques. It was found that the gross damage depth distribution of heavily implanted samples is closer to the surface than the depth distribution of the electrically active boron. By removing this gross damage, without affecting the distribution of the implanted boron, we have determined that the 800°C annealing stage is not exclusively due to the improvement in the crystalline perfection of the amorphous material but also appears to be associated with the annealing of some point defects. These results and their relation to previous results are discussed in the following sections. IMPLANTATIONS Boron ions were implanted into silicon samples using an accelerator capable of operating from 10 to 150

Jan 1, 1970

By Philip E. LaMoreaux

Fluoride, generally less than 0.5 ppm, is present in ground water from rocks of Paleozoic age and older, in northern and eastern Alabama. Some of the water-bearing formations in the Coastal Plain area of the State yield water with as much as 6.8 ppm fluoride.

Jan 1, 1950

By O. W. Ellis

IN VIEW of the extensive use of the brasses and bronzes in engineering practice it is indeed surprising that so little scientific work has been done on the oxides in these alloys. Recognition of the ill effects of these compounds is universally accorded, both in foundry procedure and in such specifications as cover the melting of these useful mixtures. In the latter, limits, for example, are placed on the proportions of scrap metal in the charge, and clauses governing the use of fluxes are included, the addition of fluxes to the charge being made with the object of avoiding oxidation during the process of melting and of subducing and separating non-metallic matter from the melt.1 In the manufacture of brass it occasionally, though rarely, occurs that the virgin metals, copper and zinc, alone are used. In the event of virgin metals being employed, that of the higher melting point is always melted first. If it is melted under suitable conditions, little or no oxidation will occur. Whether oxidation has occurred or not, however, can best be determined by microscopic examination of a sample taken from the melt.

Jan 1, 1930

By C. S. Roberts

The creep mechanism and kinetics of fine-grained magnesium have been studied over the temperature range 200&apos; to 600°F. As a result of a photographic study of microstructural changes, transient and steady-state creep components have been correlated with slip, subgrain formation, and cyclic deformation at the grain boundaries. THE approach of this research has been the blend of a quantitative study of the creep strain of polycrystalline magnesium as a function of time, stress, and temperature with direct microstructural observations of the operative deformation processes. The validity of the conclusions is dependent on the condition that the microstructural changes seen on the polished surface qualitatively represent those occurring in the bulk of the metal. The work was intended as much to lay a background to a study of highly creep-resistant magnesium alloys as to provide a description of the behavior of the base metal itself. The spectroscopic analysis of the electrolytic magnesium used in this study is as follows: Al, 0.009 pct; Ca, <0.01; Cu, 0.0011; Fe, 0.021; Mn, 0.012; Ni, 0.0004; Pb, 0.0012; Si, <0.001; Sn, <0.001; and Zn, <0.01. The impurity level is approximately that of commercial magnesium alloys. The original ingot was melted under Dow type 310 flux and cast as a 3 in. diam billet. It was extruded into 1 in. flat stock under the conditions: billet preheat 800°F (1 hr), container and die temperature 800°F, speed 3 ft per min, and area reduction ratio 45:1. The extrusion process was chosen in preference to rolling and recrystallization because it allowed easier grain size control from specimen to specimen. The grains of the extruded metal were fairly equi-axial and uniform in the size range of 4 to 6 thousandths of an inch. The preferred orientation of basal planes about the transverse direction was determined by an X-ray diffraction surface reflection method. A beam of filtered copper radiation was directed at an angle of 17" to both the transverse direction and the surface yet perpendicular to the extrusion axis. Analysis of the (002) diffraction arcs in the resulting photographic patterns gave an approximate intensity distribution along the great circle which extends through the center of the basal plane pole figure and to the extrusion axis poles. Successive layers of metal were removed by macro-etching between exposures. The extruded texture is relatively sharp, but the most significant point is the position of the maximum basal plane pole density and its variation with depth below the surface. Fig. 1 shows that this maximum is rotated 15" from the normal at the surface toward the extrusion direction. Such an inclination has been reported for extruded 1 pct Mn and 8 pct A1-0.5 pct Zn alloys.&apos; The inclination decreases until the maximum splits at about 0.025 in. depth into two elements of equal and opposite rotations from the ideal. The double texture persists to as great a depth as was experimentally convenient to examine. It probably continues to the very center of the extrusion. There is no great change in the sharpness of the individual elements of the texture with depth. A plate of metal about 0.015 in. thick at the surface of the extruded stock was produced by etching. A transmission diffraction pattern was made for the purpose of determining any preferred orientation of a direction in the basal planes. Relatively uniform {loo) and {101) rings were produced. There is little tendency for parallelism of a given direction in the plane with the projection of the extrusion axis on it. The creep specimens were machined from 6¼ in. lengths of the extruded stock. Creep was measured on the reduced section, ½x1/8X2¼ in. long. This section was electropolished on one side for the studies of microstructural changes during creep. An orthophosphoric acid-ethyl alcohol electrolyte was used under the conditions recommended by Jacquet.² Hand polishing was used for previous mechanical preparation. Electropolishing was continued until all mechanical twins had been removed. The electro-polished surface was protected from oxidation during creep testing by a thin layer of silicone oil. All micrographs were taken at room temperature on conventional metallographic equipment and after removal of the oil film. The creep tests were performed with machines which have been described in detail by Moore and McDonald." Five testing temperatures, 200°, 300°, 400°, 500°, and 600° ±3°F were used. Difference in temperature between the two ends of the specimen reduced section was 2°F or less. The testing was done at constant load. Strain readings were taken as frequently as necessary to develop usable creep curves. Tensile Creep vs Time, Stress, and Temperature A definition of terms is necessary. Whenever successive sections of a creep strain-time curve show decreasing, constant, and increasing slope with time they will be termed primary, secondary, and tertiary

Jan 1, 1954

Jan 1, 1884

By R. J. Reynik

A semiempirial small flunctation theory of diff- sion in liquids is presented, which employs a fluctuation energy assumed quadratic for a small atomic or molecular displacement and Einstein&apos;s random-iralh model. The resulting diffusion equation is given by In these equations. D is the diffusivity, is the average liquid shite coordination number (at interatomic distance d. cm. T is the absolute temperature, xu. em, is (the diffusive displacement. K, is the quadratic fluctuation energy force constant, and rg, cm, are the radii oj diffusing atoms A and B, respectively. The quantities Xn and K are calculated from the computer-filled values of the slope and intercept. respectively. The radius of self-diffusing atom or radii and of diffusing atoms A and B are eta United and compared with values reported in the literature.. The predicted linear variation of diffusivity with. It tempera lure htm been observed in approximately thirty-iire metallic liquid systems, and in over seventy-fiee other liquid systems, including the organic .alcohols, liquified inert gases, and the molten salts, ALTHOUGH the average density within a macroscopic volume element of liquid is constant for fixed total number of atoms. pressure. and temperature, there exist microscopic: density fluctuations within the respective volume element. As such the microscopic volume available to an atom and its Z first nearest neighbors at any instant of time fluctuates above and below the average volume available to these atoms. If one assumes that liquid state atoms vibrate as in a solid. and further postulates that the mean position of any atom in the liquid state is not stationary. but shifts during every .vibration a distance 0 5 j 5 xo. then every atom in the liquid state continuously undergoes diffusive displacements which vary in the range 0 5 j 5 ro. Mathematically. for a binary liquid system consisting of atcrms A and B. the maximum diffusive displacement. .YO, is defined by the equation: where d is the average liquid state interatomic distance at specified liquid state coordination number Z. and v~ \ and vg are the effective radii of diffusing atoms A and B: respectively. For self-diffusion. r^ equals rg , and Eq. [I.] reduces to: It is interesting to note that Eq. [l] or [2] can be used to compute the radii of the diffusing atoms, provided one had an experimental evaluation of xo. As such. the computed radii could be compared with metallic or crystallographic ionic radii to ascerlain the electronic character of the diffusing atoms. Thus it is proposed that in the liquid state the n~otion of an atom relative to its original equilibrium position of oscillation represents the thermal vibration of any atom and its Z first nearest neighbors. while the small and variable displacements. 0 5 1 5 xc,. of the centers of oscillation represent the complex diffusive motions of the atoms at constant temperature and pressure. This is consistent with data obtained from slow neutron scattering by liquids1 &apos; and resembles an itinerant oscillator model of the liquid state.&apos;" It is further postulated that the atomic displacements characterizing the liquid state diffusion process are essentially a random-walk process. As such. it nlay be described by Einstein&apos;s equation:&apos; where D is the diffusivity. sq cm sec-&apos;. j2 is the mean square value of the diffusive displacement. and i> is the frequency of density fluctuations giving rise to diffusion. FORMULATION OF DIFFUSION EQUATION The effective spherical volume occupied by an atom, as a consequence of a microscopic density fluctuation which enlarges the volume available to any atom, exceeds its average liquid state atomic volume by an amount: where AV is the enlarged spherical volume, v is the radius of the diffusing atom. and j is the elementary displacement distance from the original center of oscillation of the vibrating atom to a new center of oscillation position. For small atomic displacements. where c is a constant whose value depends upon the assumed geometry of the enlarged volume. For a spherical increase in volume, c equals 4nr2. Following the treatment of Furthl&apos; and ~walin." assuming the enlarged volu~nes AL7 for the diffusing atoms are distributed in a continuunl. the probability of finding a fluctuation in the size range 0 5 j 5 xo defined by Where c includes the geometric constant cl and Eij) is the fluctuation energy causing the volume change. But the proposed model assumes all the Z first nearest-neighbor atoms are centers of oscillation. and hence the probability that any of these atoms is adjacent to a fluctuation of magnitude 05j5xo is unity. Thus:

Jan 1, 1970

By J. A. Solomon, H. E. Shafer

As a result of the great demand for metallic aluminum and the scarcity of domestic bauxite, numerous processes have been proposed and developed to extract the oxide of this metal (Al2o3) from clays, shales, and other low-grade raw materials.1-4 An exploratory study was made to extract alumina with sulfuric acid from relatively impure coal-associated draw-slate and to establish an optimum calcination temperature for maximum recovery. Draw-slate is the term used to describe the hard, slaty material directly overlying many coal seams and may range from a few inches to a few feet in thickness. Alumina content of these draw-slates may range from as low as 15% to over 35%. Although the following results are limited in scope, some of the data should prove beneficial for further work. Coal-associated clay, shale, and gob heretofore have been considered nuisance products; any successful alumina extraction process would greatly enhance the worth of these almost limitless resources. This research demonstrated that an optimum calcination temperature for alumina extraction could be established for a coal-associated draw-slate and that this temperature was lower than those suggested in previous work with unspecified clay types. It should be noted that slightly higher acid concentrations and somewhat finer particle sizes were used in this series of tests as compared to previous work. EXPERIMENTAL WORK Essentially, alumina extraction proceeded in four steps: 1) grinding, 2) calcining, 3) acid leaching, and 4) precipitating of aluminum sulfate. An initial series of reference tests to determine the optimum temperature of solubility for alumina was run using relatively pure kaolin. Kaolin forming clays are hydrous aluminum silicates of the approximate composition 2H2O A12O3 2SiO and kaolinite is the mineral that predominates in most kaolins. 5 The kaolin was ground to -30 mesh and subsequently calcined at temperatures ranging from 100°C to 700°C. Each sample was calcined for 1 hr in a muffle furnace and in turn subjected to sulfuric-acid leaching (H2SO4, 9 molar) for a 2-hr period. The filtrates were analyzed for the amount of dissolved alumina recovered.637 Also, each sample of leached or barren residue was

Jan 1, 1968

By W. M. Parris, P. D. Frost, H. A. Robinson

The effects of hydrogen content and strain rate on the static tensile and notch-rupture properties of the Ti-3Mn-complex alloy heat-treated to differed strength levels were investigated. The extent of embriulement was found to be proportional to the amount of hydrogen present and the strength to which the specimens were heat-treated. The research suggests the possible necessity of specifying lower hydrogen limits than are now allowed when titanium alloys are heat-treated to higher strengths than are presently used. The research also supports a hypothesis advanced earlier for a mechanism of hydrogen embrittlement. MUCH attention has been focused on the effects of hydrogen in in Most of the published in- formation has dealt with the effects of hydrogen on alloys in the annealed or lowest-strength condition. The work of Kotfila and Erbin3 is one of the few exceptions. In view of the fact that heat-treatments are now being used to produce high strength in titanium alloys,&apos; it is necessary that more attention be given to the effects of hydrogen on these alloys in the heat-treated condition. Research was initiated to establish the effects of hydrogen on the properties of the Ti-3Mn-complex alloy at various strength levels. This research, which supplemented that of Kotfila and Erbin, was started because it was found that high-strength tensile specimens of this alloy were strain-rate sensitive. The essential results of the research are summarized in this paper. MATERIALS AND EXPERIMENTAL PROCEDURES Material for this investigation was a 41/2-in.-diam bar forged from a single commercial heat of the Ti-3Mn-complex alloy having the composition given in Table I. The as-received forging was reduced further by forging at 1750°F to 3/4-in. square bars. About one fourth of this material was vacuum annealed at 1400°F for 24 hr to obtain a base hydrogen content of 25 ppm. The remaining bars were hydrogenated to levels of 90, 140, and 260 ppm in a large Sievert&apos;s apparatus in the following manner: Four 3/4-in. square bars, 5 in. long, were placed in the reaction chambzr. The chamber was evacuated, heated to 1400°F, and a measured amount of hydrogen was introduced. When absorbtion was complete, as indicated by the drop in pressure, the reaction tube was cooled and the bars removed. Each batch of bars was then sealed in individual evacuated Vycor containers and heated for 24 hr at 1400°F in order to distribute the hydrogen homogeneously. After vacuum-annealing or hydroge nation, the bars were rolled at a temperature (1400°F) below the ß-transus to 1/2 - in. - diam rounds. Groups of the rolled specimens representing each of the hydrogen levels were given the following heat-treatments: 1) One hr at 1300°F, water-quenched. 2) One hr at 1300°F, water-quenched, and aged 8 hr at 1100°F. 3) One hr at 1300°F, water-quenched, and aged 4 hr at 1000°F. 4) One hr at 1300°F, water-quenched, and aged 48hr at 800°F. Heat-treated bars were machined into standard 0.250-in.-diam tensile specimens having 1-in. gage lengths. Throughout the processing and testing of this material, hydrogen analyses were made by vacuum-fusion methods to check for accuracy of hydrogen additions, homogeneity, and possible losses during processing. A summary of these analyses is given in Table II It may be seen that the actual hydrogen contents were reasonably close to the desired levels. In addition, it was noted that the variation in hydrogen content within any one bar did not exceed

Jan 1, 1959

By Kim C. Harden

INTRODUCTION The purpose of the following discussion is to present the state of the art of solution mining. Since the economics of a mining method ultimately determines its applicability and viability this presentation shall revolve around the costs of in- situ solution mining. First the assumed physical characteristics of the hypothetical ore body are described, followed by the appropriate operating assumptions. Then after a brief discussion on the type of surface plant to be used, the assumed project time tables and costs for Texas and Wyoming are presented. Finally, the economics of in-situ uranium leaching are analyzed through the use of discounted cash flow rate of return analysis. ORE BODY CHARACTERISTICS The assumption of the ore body characteristics is probably the most variable portion of this discussion. The characteristics that have been used are based mainly on state of the art technology, however, consideration of the most common depths of ore, ore thicknesses, and permeabilities also influenced these assumptions. In addition, it is assumed that these assumptions are equally applicable to Texas and Wyoming. The average grade of the ore is assumed to be .09% U308 with no apparent disequilibrium. The average thickness of ore is 2.29 m (7.5 ft) which results in an average grade-thickness (GT) of .675. The assumed depth to the top of the ore is 121.92 m (400 ft), the ore density is placed at 1.78 gm/cc (18 cu ft/ton), the porosity is estimated to be 28% and the permeability 1 darcy. These assumed ore body characteristics are shown in Table I. In addition, it is specified that the costs to be later discussed are based on a minimum GT cut-off of 0.15. It is more common to use GT cut-offs of 0.30 to 0.50 but GT cut-offs as low as 0.15 in conjunction with a minimum grade of 0.05% U308 have been used in the past with success and is considered state of the art. The ultimate percentage of uranium recovered from the ore is left to the discretion of the reader since the costs and economics are based on pounds recovered by the surface plant. OPERATING AS.SUMPTIONS An annual production rate of 200,000 lbs U308!yr was chosen for this example. In order to maintain this production rate, based on the ore body characterized above, a flow of 4731 liter/min (1250 GPM) with a recovery solution grade averaging .039 gm U308/liter is assumed. A regular 5 spot well field pattern is used with a well spacing of 21.5 m (70.7 ft) between like wells and 15.24 m (50 ft) between unlike wells. This well spacing gives each well an area of influence equal to 232.25 sq m (2500 sq ftl. An excess wells factor of 1.17 is used to estimate additional monitor wells and well field boundary wells. Each production well is expected to yield an average flow rate of 37.85 liter/min (10 GPM). In addition it is assumed that the ore body has a good shape in that it is not tenuous and narrow but has at least an average width of 200 ft. The process chemistry required for this ore body is assumed to be based on the sodium carbonate System- Oxygen is the chosen oxidant. Sodium chloride elution followed by precipitation with hydrogen peroxide makes up the remaining portion of the process. A fluidized up-flow ion exchange system is specified. The operating assumptions are listed in Table II. Restoration of the ore body shall be assumed to be accomplished through the use of ground water flush. Other methods may be considered as having to fall within the costs estimated for a ground water flush in order to be economic. In Texas it is assumed that a high capacity disposal well (200 GPM +I is required and in Wyoming evaporation ponds covering approximately 35 acres are to be used. No specific cost has been given to restoration. Instead only the additional capital investment for restoration equipment is given. Then, one year of restoration operating expense is estimated and included as the operating expense for one year beyond the last pound of U308 produced. It is also assumed that restoration will be pursued in the mined out areas of the ore body contiguous with ongoing production.

Jan 1, 1980

Jan 1, 1925

By W. C. Knoblaugh

Rotary kilns are adaptable to many fuels, but this paper deals principally with the use of powdered coal. The observations and conclusions presented are based on rotary kilns used in the manufacture of basic refractories for steel furnaces. Solid fuels are pulverized for two principal reasons: (I) ease of control, and (2) rapidity of combustion. By the use of pulverized coal, the operator can increase or decrease the fuel supply by small increments and with very little time lag between the change of control and the resultant change in the flame. This is extremely important in this type of furnace, as the temperature range for maturing the clinker is very narrow. By fine grinding, it is possible to increase the rate of burning of the coal, thereby liberating great quantities of heat within a small space in a short time. Under given conditions, temperature is a measure of the heat liberated per unit of time. To attain the temperatures of 2950° to 3150ºF., which are encountered in the manufacture of various steel-furnace refractories, it is estimated that it is necessary to liberate 125,000 to 175,000 B.t.u. per cubic foot of the burning zone per hour. The manufacture of dolomitic refractories is a ceramic process and, as is true in most such processes, the material must be subjected to a certain critical temperature for a certain length of time in order to complete the reaction. If the time of reaction is reduced, the temperature must be increased; in other words, if the rate at which the material flows through the hot zone of the kiln is increased, the temperature of the hot zone must be increased to compensate for this shorter exposure to the flame. Firing with Pulverized Coal Fig. I is a line drawing of a rotary kiln with the attendant equipment indicated in their relative positions. The kiln proper consists of a sloping, refractory-lined steel tube rotating slowly about its longitudinal axis (0.75 r.p.m.), and is countercurrent in operation in that the raw feed is introduced at the stack end and gradually approaches the zone of highest temperature at the lower end, where the fuel is introduced. Before 1930, the usual method of firing a rotary kiln was to store the coal in the pulverized form and then feed from this storage to the kiln as needed. This proved unsatisfactory and dangerous because of dust explosions and the inability to obtain an even feed to the kiln caused by arching of the coal in storage and flooding of the coal feeders. In later years the practice has been to store the raw coal and grind it as it is needed. Such a layout is indicated in Fig. I. The coal is stored in bins, charged from the top and drawn from the bottom into recording scales and then into some type of unit pulverizer. There are a number of good pulverizers .on the market, each incorporating features that the manufacturer considers outstanding.

Jan 1, 1948