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By Reuben B. Ellestad, Fremont F. Clarke

In the early days of the lithium industry most of the production was from lepidolite, zinnwaldite, and amblygonite. Nearly all the early extraction processes described in the literature involve heating the finely ground mineral with sulphuric or hydrochloric acid. On subsequent water leaching most of the bases present in the mineral (especially aluminum) are dissolved as sulphates. As a result, the leach solution required extensive chemical purification before the lithium could be precipitated as carbonate. Following the remarkable growth of the lithium industry to its present size, zinnwaldite and amblygonite ores must be considered of minor importance only. Attention is now focused on spodumene, abundant enough in North America to be a major source of supply, and there are important supplies of lepidolite and petalite in Africa. The extraction processes described below all apply to spodumene, although several will also operate on other lithium minerals, such as petalite. Base Exchange with Alkali Sulphates: A distinct advance was made with the disclosures of Wadman and von Girsewalt. In these methods the finely ground silicate ore (spodumene or lepidolite) is intimately mixed with an excess of alkali sulphate (usually K2S04) in at least a 1 to 1 proportion, and the mixture was heated to a relatively high temperature. Base exchange results, with the formation of lithium sulphate. A water leach dissolves the lithium sulphate, together with the excess potassium sulphate. Successful operation of this type of process requires very thorough grinding and mixing, as well as careful temperature control. The use of K,SO, is objectionable from cost considerations since purification of lithium carbonate re- quires the use of potassium carbonate, if the K2S04 is to be recovered and recycled. The lower solubility of K,SO, as compared with Na,SO, is also objectionable, since it limits the concentration of the Li,SO, solution to be precipitated by K,CO,. Early laboratory-scale investigation of this process by Lithium Corp. was not encouraging

Nov 1, 1955

By W. J. McConnell

OBSERVATIONS on man exposed to unusual temperatures and humidities, and studies conducted under accurately controlled environmental conditions, have supplied information regarding the physiological responses of the human body which may occur incident to such exposure. These investigations also indicate the relative importance of temperature, humidity and air motion-the three physical air factors that affect human comfort. Many and diverse were the conclusions of early investigators who associated the discomfort observed in crowded and ill-ventilated spaces with changes in the chemical constituents of the air resulting from presumably poisonous exhalations from the body. These are of interest today only because, as a recent editorial in the British Medical Journal1 states, there is still an inclination to believe in the old view that there is some injurious quality of the air in ill-ventilated and crowded rooms, quite apart from dust, microbic infection and heat stagnation. There is a tendency to fly to some mysterious unknown agent such as "deionization," which even certain American engineers are now discussing. This editorial denies the existence of the least proof of any subtle poison being exhaled by human beings or of the ionization of the air having any influence in making open-window ventilation better and more stimulating than mechanical methods which propel heated and conditioned air through ducts. Until proof is forthcoming that certain changes, with which we are not now familiar, occur in the transmission of air from the exterior to the interior of enclosures, the responsible known factors which initiate the physiological responses in human beings are limited to the combined conditions of temperature, humidity and velocity of the air. While some mention was made as far back as 1880 that high temperatures and humidities were undesirable, Hermans,2 of Amsterdam, is credited with suggesting in 1883 that the harmful effects noted in ill-ventilated rooms were due to the fact that the increased temperature and moisture of the air prevented the body from maintaining a proper thermal balance.

Jan 1, 1930

By Norman P. Goss

It is generally agreed that cold-working mechanically refines the grains into smaller fragments and with continued working these are oriented with certain crystallographic directions bearing a relation to the direction in which the metal is worked. Some of the energy expended on the metal during plastic deformation appears in the form of heat, but a very small portion remains in the metal as stored energy. The entropy, specific heat capacity, temperature at which recrystallization will just begin, density, ductility, elasticity, tensile strength, and resistance to corrosion are affected. These properties have been studied extensively and some of the changes in the physical properties due to cold-working were attributed to lattice distortion.l-8 The broadening of the Ka lines on the X-ray diffraction diagrams of plastically deformed metals is believed to indicate lattice distortion, and consequently the existence of internal stresses. The evidence supporting this theory rests solely upon the observed experimental fact that the diffraction lines are broadened and the Ka doublets are completely diffused. Elam9 has reviewed the matter of lattice distortion in relationship to the hardening of metals by plastic deformation. The X-ray diagrams of plastically deformed metals differ in general from annealed metals. The hardening of a metal was believed due to lattice distortion.9 The resolution of the doublet is lost when a metal is cold-worked and the Laue spots are elongated. At one time this elongation was thought to indicate the elastic bending of the crystal planes. However, more careful work showed that the asterism was due to new orientations developed within the fragmented grains during plastic deformation. Some theories attributed the hardening to fragmentation of the grains into smaller units. Jeffries and Archer,ll after carefully considering the problem of work-hardening from many angles, came to the conclusion that cold-working mechanically refines the grains into smaller crystal fragments, some of which at least differ in orientation from the parent grain. The increase in

Jan 1, 1940

By Norman P. Goss

It is generally agreed that cold-working mechanically refines the grains into smaller fragments and with continued working these are oriented with certain crystallographic directions bearing a relation to the direction in which the metal is worked. Some of the energy expended on the metal during plastic deformation appears in the form of heat, but a very small portion remains in the metal as stored energy. The entropy, specific heat capacity, temperature at which recrystallization will just begin, density, ductility, elasticity, tensile strength, and resistance to corrosion are affected. These properties have been studied extensively and some of the changes in the physical properties due to cold-working were attributed to lattice distortion.l-8 The broadening of the Ka lines on the X-ray diffraction diagrams of plastically deformed metals is believed to indicate lattice distortion, and consequently the existence of internal stresses. The evidence supporting this theory rests solely upon the observed experimental fact that the diffraction lines are broadened and the Ka doublets are completely diffused. Elam9 has reviewed the matter of lattice distortion in relationship to the hardening of metals by plastic deformation. The X-ray diagrams of plastically deformed metals differ in general from annealed metals. The hardening of a metal was believed due to lattice distortion.9 The resolution of the doublet is lost when a metal is cold-worked and the Laue spots are elongated. At one time this elongation was thought to indicate the elastic bending of the crystal planes. However, more careful work showed that the asterism was due to new orientations developed within the fragmented grains during plastic deformation. Some theories attributed the hardening to fragmentation of the grains into smaller units. Jeffries and Archer,ll after carefully considering the problem of work-hardening from many angles, came to the conclusion that cold-working mechanically refines the grains into smaller crystal fragments, some of which at least differ in orientation from the parent grain. The increase in

Jan 1, 1940

By Robert C. Berggan

The hot-milling process for reconditioning rock-drill bits is not new. It has been employed by a few mines for years and in the past decade it has been widely adopted, as its advantages have become better known. Because of the extensive commercial development in England and Canada of machines to operate on this principle, general acceptance has been largely in the British possessions and until recently has been chiefly in the field of conventional steel. In the past two years there has been a definite trend toward hot-milling of detachable bits in Canada, but only in the past year has any considerable attempt been made to build special machines for this type of work. Generally a machine designed for conventional steel has been used and special holders employed to manipulate the bit. As early as 1934 at least one operator in the United States had adapted hot-milling to conventional steel with a substantial saving in resharpening costs.1 Several other operators have taken it up but there has been no widespread adoption of the method in this country by users of conventional steel. This may be partly explained by the fact that until recently no American manufacturer produced this equipment and operators have been obliged to build their own hot-millers or import them. Several years ago a few machines were built in Seattle, Washington, and operated in some mines in the northwest, but, for reasons not generally known, the effort was abandoned. The Process Hot-milling performs the function of re-dressing the bit at a forging temperature of about 1650°F., by the removal of metal from the flutes with a milling cutter, followed by a similar cut from the bit gauge. Conventional bits are thus treated following the usual forging operation in a sharpener, and usually in the same heat.

Jan 1, 1940

By Zay Jeffries

IT is well known that many properties of a given metal vary with the size of grain or cell. For most industrial purposes, where high ultimate strength and high elastic limit are desired, the manufacturer tries to produce a. fine-grained structure. For some purposes, for example in transformer iron, a coarse-grained structure is desirable. The terms fine-grained and coarse-grained are used only in a relative sense. For example, a fine-grained cast copper might have grains 100 times larger than coarse-grained high-speed steel. Similarly, a fine-grained steel rail might have grains or cells 100 times larger than coarse-grained wire, which was made of steel from the same heat. In some metals, the change in grain size is more appreciable than the changes in any of the properties determined by the tensile test. Furthermore, in metals which have been annealed or subjected to high temperatures, grain size may prove to be a better indication of the life of the metal in use than the tensile test. One of the authors was able to supplant the tensile test with grain-size determinations in the control of. metal for a specific use, the latter determination being more indicative of. the life of the metal part than the tensile test. A grain-size determination with a tensile test is, of course, more valuable than either singly. At present there is a decided dearth of data on actual grain-size determinations in metals, and consequently a corresponding lack of ability to interpret the determinations after they are made. It would be desirable to have correlation made between grain size and properties of metals, comparing thousands of determinations. In this way, grain-size determinations might be interpreted in much the same manner that tensile tests are now.

Jan 12, 1915

By Robert C. Berggan

The hot-milling process for reconditioning rock-drill bits is not new. It has been employed by a few mines for years and in the past decade it has been widely adopted, as its advantages have become better known. Because of the extensive commercial development in England and Canada of machines to operate on this principle, general acceptance has been largely in the British possessions and until recently has been chiefly in the field of conventional steel. In the past two years there has been a definite trend toward hot-milling of detachable bits in Canada, but only in the past year has any considerable attempt been made to build special machines for this type of work. Generally a machine designed for conventional steel has been used and special holders employed to manipulate the bit. As early as 1934 at least one operator in the United States had adapted hot-milling to conventional steel with a substantial saving in resharpening costs.1 Several other operators have taken it up but there has been no widespread adoption of the method in this country by users of conventional steel. This may be partly explained by the fact that until recently no American manufacturer produced this equipment and operators have been obliged to build their own hot-millers or import them. Several years ago a few machines were built in Seattle, Washington, and operated in some mines in the northwest, but, for reasons not generally known, the effort was abandoned. The Process Hot-milling performs the function of re-dressing the bit at a forging temperature of about 1650°F., by the removal of metal from the flutes with a milling cutter, followed by a similar cut from the bit gauge. Conventional bits are thus treated following the usual forging operation in a sharpener, and usually in the same heat.

Jan 1, 1940

By D. K. Deardorff, H. Kato

THE transformation temperature of hafnium from hcp to bcc is 1750° + 20 °C in contrast to previously published values by Duwez and fast2 which are believed inaccurate. The Bureau of Mines determined this value by measuring the temperatures at which a sudden decrease was observed in the electrical resistance of hafnium alloys containing up to 18 at. pct Zr, and then extrapolating the temperatures to 0 pct Zr. Duwez1 previously reported a transformation temperature of 1310°C, obtained by use of a rapid-cooling thermal-analysis technique. Later, Fast2 published a much higher value of 1950° 100°C based upon: a) his own determination of 1690°C for the beginning of the transformation range for hafnium containing 5.7 at. pct Zr, and b) his belief that lattice parameters reported3 for Duwez' hafnium indicated i contained 19 at. pct Zr and that the 1310°C value should be associated with that composition. Russell4 subsequently stated that Duwez and Fast probably were reporting their lattice parameters in different units and reassigned a value of 6.0 at. pct Zr to Duwez' hafnium. If this assumption were true, Duwez' hafnium was of approximately the same purity as Fast's, but his transformation value was considerably lower. The reason for this divergence is not known. Fast's value for hafnium containing 5.7 at. pct Zr agrees well with our data. McGeary5 determined a transformation value of 1660°C by metallographic examination of heat-treated specimens, but the zirconium content of his hafnium was not definitely established. The specimens used in this investigation were 1/8-in.-diam rods 6 1/2 in. long, fabricated by hot-swaging bars cut from arc-melted buttons. These buttons were melted from crystal bar hafnium and crystal bar zirconium. The chief impurity in the hafnium

Jan 1, 1960

By Robert B. Fulton, Gill Montgomery

Fluorspar is the commercial name for fluorite, a mineral that is calcium fluoride, CaF2. The name, derived from the Latin word fluere (to flow), refers to its low melting point and its early use in metallurgy as a flux. It is the principal industrial source of the element fluorine. Cryolite, sodium aluminum fluoride, Na3AlF6, is a rare mineral which has been found in commercial quantities only in Greenland. The natural material has been supplanted by synthetic cryolite for its principal industrial use in the manufacture of aluminum. History Fluorspar was used by the early Greeks and Romans for ornamental purposes as vases, drinking cups, and table tops. Various peoples, including the Chinese and the American Indians, carved ornaments and figurines from large crystals. Its usefulness as a flux was known to Agricola in sixteenth century Europe. Fluorspar mining began in England about 1775 and at various places in the United States between 1820 and 1840. Production grew substantially following the development of basic open-hearth steelmaking, wherein it is used as a flux. Use was stimulated by growth of the steel, aluminum, chemical, and ceramic industries, particularly during World Wars I and II. Fluorocarbons entered the picture in 1931. The use of anhydrous hydrogen fluoride (HF) as a catalyst in the manufacture of alkylate for high octane fuel began in 1942. Differential flotation for separating fluorspar from galena, sphalerite, and common gangue minerals in the 1930s, and the application of heavy-media concentrating methods to the treatment of low-grade ores in the 1940s were outstanding technological advances that facilitated increased production. Recently, pelletizing and briquetting of flotation concentrates for use in steel furnaces and the development of flotation schemes for beneficiating ores containing abundant dolomite and barite have been major improvements in the industry. Uses of Fluorspar Fluorspar is used to make hydrogen fluoride, also called hydrofluoric acid, an intermediate for fluorocarbons, aluminum fluoride, and synthetic cryolite. It is used as a flux in the steel and ceramic industries, in iron foundry and ferroalloy practice, and has many minor specialized uses. Hydrogen fluoride (HF) is produced by reacting acid grade (97% CaF2) fluorspar with sulfuric acid in a heated kiln or retort to produce HF gas and calcium sulfate. After purification by scrubbing, condensing, and distillation, the HF is marketed as anhydrous HF, a colorless fuming liquid, or it may be absorbed in water to form the aqueous acid, usually 70% HF. Synthetic cryolite, organic and inorganic fluoride chemicals, and elemental fluorine are made from hydrofluoric acid. The acid itself is important in catalysis in the manufacture of alkylate, which is an ingredient in high-octane fuel for aircraft and automobiles, in steel pickling, enamel stripping, glass etching and polishing, and in various electroplating operations. The manufacture of one ton of virgin aluminum requires about 50 to 60 lb of fluorine content in synthetic cryolite and alumnium fluoride. This quantity, through improved technology and recovery practices, is being lowered significantly.

Jan 1, 1983

By George Hallerman, R. J. Gray

In the customary method of studying age hardening, the process of aging is interrupted by cooling the specimen and measuring its room-temperature hardness. However, the aging process may be conveniently measured while it is occurring at an elevated temperature by a series of hardness measurements at suitable time intervals. The latter method gives data void of complications that might result from processes occurring during the quench, and the data may be more indicative of the alloy's properties at elevated temperatures. The elevated-temperature hardness tester1 used in the present study employed a dead-weight loading system with a synthetic sapphire Vickers-type in-denter mounted in a molybdenum holder. The tests were performed in a vacuum of l0 to 10 torr. Hardness impressions were made by applying a 2-kg load for 15 sec. Although the hardness impressions made in the tester at elevated temperatures were measured at room temperature, the correction for thermal contraction during cooling was insignificant and therefore neglected. The two methods of obtaining age-hardening data were compared using eighteen samples of Haynes alloy No. 25* which had been annealed for 2 hr at 2250°F (1232°C). The test surfaces of the 1 by 1 by 1/4-in. samples were ground and then polished on vibratory polishers2 prior to testing. Three groups of five samples were aged at 1400°, 1650°, and 1800°F (760°, 899", and 982°C) for 4, 16, 32, 64, and 100 hr and then water-quenched. Room-temperature hardness as a function of aging time for these samples is shown in the broken lines of Fig. 1. Only one sample for each of the three temperatures was necessary to determine the hardness of the alloy at the aging temperatures with the elevated hardness tester. The specimens were heated isothermally and hardness impressions were made after various time intervals up to 100 hr. The results of these determinations were represented by solid lines in Fig. 1. Comparison of the two sets of curves shows, as expected, the hardness values determined at the aging temperatures are lower than the room-temperature hardness of the quenched specimens and the hot-hardness values reflect a strong tempera-

Jan 1, 1964

By J. E. Spruiell, F. H. Patterson, B. F. Shuler

The microstructures and textures developed by the working of high-purzly thermochemically deposited tungstem sheet have been inuesligated. Greater than 60 pct reduction was required to deslroy the columnar grain structure which existed in the as-deposited sheet. With increasing reductions the texture gradu-ally charged from the initial as-deposited orientation with (100) parallel to the sheet normal to a (100}(011) ideal ovienlation with some spread about the rolling direction. This texture was retained after recrystalli-zation a1 2000°C. THE processes for depositing tungsten by hydrogen reduction of tungsten hexafluoride have been under development for the past several years.1,2 The nature of the deposition process is such that the as-deposited material contains a highly oriented columnar grain structure perpendicular to the deposition substrate. This well-defined columnar structure may be useful in certain applications293 but a wrought or equiaxed structure may be desired for some components such as tubing. Knowledge of the effects of working ther-mochemically deposited (TCD) tungsten is therefore necessary in order to establish the feasibility of obtaining worked and recrystallized microstructures and textures. The details of a recently developed technique for thermochemically depositing flat, uniformly thick tungsten sheet are presented with emphasis on the effects of deformation by rolling on the microstructure and texture. Although no work has been previously reported on the rolling and the annealing textures of TCD tungsten, there have been some determinations of textures for cold-rolled tungsten foil prepared from powder-metal -lurgy billets.4-8 The general description is that of a predominantly lurgy{100}(011) texture, with some spread about the rolling direction as an axis. pugh5 reports data both for cold-rolled and for annealed foil having about 96 pct initial cold work. He observed no change in texture, except for a decrease in the spread, for annealing treatments of 30 min at temperatures up to 1800°C. On annealing at 1900°C, both the low-temperature components plus new components which were described alternately as {001}(320) plus {001)(230) or as {100}(011) ± 12 deg about the sheet normal were observed. Above 1900°C, the new orientation existed alone, and it was stable up to 2500°C, the highest temperature that Pugh investigated. THERMOCHEMICAL DEPOSITION OF TUNGSTEN SHEET High-purity tungsten sheet was reproducibly deposited on the inner walls of a molybdenum mandrel by the thermochemical reaction WFs(g) + 3H2(g) - W(s) + 6HF(g). The mandrel was heated by a five-zone tube furnace which afforded a controllable fixed-temperature profile. Sheets measuring 1+ by 12 in. have been deposited with uniform thicknesses of up to 0.145 m. As shown schematically in Fig. 1, the purified reaction gases were metered into a mixing chamber at a Hz-to-WF6 ratio of 15 and preheated to 350°C. The flow rate of the WF6 was 300 cu cm per min at stp. These gases were directed through a conical injector into the deposition chamber. Inside this chamber hydrogen reduction of the WF6 to pure tungsten metal occurred on the hot walls of the molybdenum mandrel at a total pressure of 5 Torr. Typical temperatures for the five zones in the chamber were, respectively, 565", 540", 550°, 570°, and 590°C. The hydrogen fluorlde generated from the reaction, the excess hydrogen, and some un-reacted WF6 were pumped on through the scavenger

Jan 1, 1968

By C. D. Thompson, D. C. Violetta, C. A. Czako

The mechanics of the continuous sintering process are briefly reviewed and the application of this process for the beneficiation of principal minerals used in making cement is shown. Pilot plant tests using pyrobeneficiation techniques were conducted with mixtures of limestone and shale in various ratios. Results are illustrated and show the percentage removal of carbon, carbonates, sulfur, alkalies, and volatiles as a function of the limestone-shale ratio. Tests with varying quantities of solid fwls, added to mixtures containing limestone and shale in a 4 to 1 ratio, were made to attain optimum elimination of the volatile constituents. Experimental results show that 90 pct of these constituents were removed during the calcination sintem'ng process. The advantages of using the beneficiated material for making cement are discussed with regard to prepam'ng, handling, and clinkering operations. A sintering process for treating raw materials or kiln waste products which contain high amounts of alkaline materials is described. Tests were performed with a high alkaline waste dust mixed in a 1 to 1 ratio with raw cement meal. The data from these tests and others using different halides for aiding alkali removal are evaluated by the alkali content of the cement clinker. Test results showed that the Dwight-Lloyd process could be applied with facility in beneficiating raw materials for cement making. Substantial quantities of deleterious volutile constituents were removed by calcining and sintering techniques. The continuous sintering process has been applied for a number of years as a means of beneficiating minerals for subsequent conversion to merchantable products. The process was developed and first used for nonferrous metallurgical applicatfons. However, it has risen to prominence for ferrous metallurgical applications where last year in the U.S. and Canada nearly 40 million tons of iron ore were treated by grate firing processes. Through the years of process development many investigators have realized the versatility of the sintering process and have directed experiments toward the use of it for applications with nonmetallic minerals. These have included calcining limestone, carbonizing coal, expanding shale, and burning cement raw meal. Today commercial sintering plants produce cement clinker from mixtures of limestone and shale, lightweight aggregate from shale or clay, and calcined products from phosphate shale. The mechanics of the downdraft sintering process have been presented by many authors. In general practice the materials to be agglomated are mixed as moistened fines with a solid fuel and this mixture is spread uniformly on the grates of the sintering machine. The charge is then momentarily directed under an ignition furnace. After ignition a continuous downdraft of air promotes combustion of the fuel and through heat transfer particles become partially fused into a coherent mass. This is cooled from continued draft induced after combustion. Many investigators have shown that distinct zones are formed during the process of sintering iron ores. At the midway point of the sintering process these are prominent and are, respectively, from the top of the bed to the bottom, comprised of a cooling zone of sintered material, a combustion zone of sinter formation, a calcination zone, a drying zone, and a zone of unreacted materials. Completion of sintering occurs near the discharge end of the machine where the firing zone approaches either the grates or grate dressing material called hearth layer. Here the peak draft temperature usually can be noted in the windboxes. The zonal pattern has been illustrated with the use of graphs which show thermal gradients as they progress through the bed of materials during sintering. Fig. 1 shows, in simplified form, thermal gradients existing when clinkering cement on a sintering machine. The thermal gradients illustrated are for periods of initiation, midway and completion of the clinkering process. The occurrence of these zones has importance for the beneficiation of cement raw materials. A research program was performed at the Dwight-

Jan 1, 1961

By H. Conrad, V. V. Damiano, G. J. London

A method is described for producing single crystals of high-purity beryllium, Be-4.37pct Cu, and Be-5.24 pct Ni. These crystals were prepared for testing in compression parallel to the [0001] by orienting and lapping to within ±3' of arc of the (0001). Microstrain testing apparatus is described along with c axis compression results for ingot purity beryllium, twelve-zone-pass material, and the above-mentioned alloys. Results show no measurable plasticity for the ingot purity material from -196" to 400°C, although some surface traces of (1122) slip was observed at 200°C and above. The twelve-zone-pass material shows substantial microstrain plasticity at 220°C with slip on (1122). Both alloys show significant plasticity at room temperature and above with slip also on (1122) planes. THE two slip systems which normally operate during the plastic deformation of beryllium in the vicinity of room temperature are:' basal slip (0001)(1120) and prism slip . Pyramidal slip with a vector inclined to the basal plane has been reported for elevated temperatures,'-a but occurs near room temperature only at very high stresses.~ A summary of the available data on the effect of temperature on the critical resolved shear stress for slip on these systems has been compiled by Conrad and Perlmutter.~ It has been postulated6'7 that one of the principal factors contributing to the brittleness of poly crystalline beryllium at temperatures below about 200°C is the difficulty of operating pyramidal slip with a vector inclined to the basal plane. Hence, detailed information on the operation of such a slip system is important to understanding the brittleness of beryllium. The operation of pyramidal slip with a vector inclined to the basal plane is best accomplished in beryllium by compressing single crystals in a direction parallel to the c axis. In such a test the resolved macroscopic shear strzss on the basal and prism planes is zero and (1012) twinning which is favored by tension along the c axis does not occur. Hence, in c axis compression of beryllium the normal deformation modes are inhibited and the operation of pyramidal slip with a vector inclined to the basal plane is favored. In the present investigation, c axis compression tests were performed on beryllium single crystal as a function of temperature (77" to 700°K), purity (commercial and twelve zone pass), and alloy content (4.37 wt pct Cu and 5.24 wt pct Ni). Presented here is a description of the test techniques employed and the gross mechanical behavior observed. A detailed analysis of the slip traces developed on the surfaces of the deformed specimens during these tests and the results of electron transmission studies of the deformed crystals are given in a separate paper.B PROCEDURE 1) Materials and Preparation. Single crystals about 1 in. diam were prepared of the following materials: commercial-purity beryllium, high-purity beryllium, and two beryllium alloys, one with 4.37 wt pct Cu and the other with 5.24 wt pct Ni. The commercial-purity single crystals were obtained by cutting specimens from large-grained ingot of Pechiney SR material, which is approximately 99.98 pct pure. The high-purity crystals were prepared by floating-zone refining (twelve passes) a rod (7 in. by 1 in, diam) of Pechiney SR grade cast and extruded beryllium. Although an absolute chemical analysis of the zone-refined material was not established, mass spectro-graphic analysis, emission spectrographic analysis, and y activation analysis indicated that it contained in atomic fractions about 5 to 10 ppm each of carbon and oxygen, 1 to 5 ppm each of nickel and iron, and about 1 to 2 ppm of copper, with the remaining residual impurities being less than 1 ppm. Further indication of the purity of this material is provided by the critical resolved shear stress for basal slip, which was approximately 300 psi. The starting material for the alloy single crystals was 1-in.-diam floating-zone-refined (six passes) rod of Pechiney SR grade beryllium. Two such rods were wrapped respectively with sufficient weight of wire of high-purity copper (99.999 pct) or nickel (99.999 pct) to yield a 5 wt pct alloy. A seventh floating-zone pass was then applied to each of the rods to accomplish the initial alloying and an eighth pass for homogenization. Analytical samples were taken from regions of the rod immediately adjacent to where the mechanical test specimens were cut; these indicated 4.37 wt pct Cu and 5.24 wt pct Ni. 2) Crystal Orientation. To avoid the occurrence of basal slip during c axis compression testing, it is necessary to load the crystals as nearly parallel to the c axis as possible. Preliminary c axis compression tests indicated that plastic flow and/or fracture occurred at stresses of the order of 300,000 psi; hence on the basis of a critical resolved shear stress for basal slip of 300 to 400 psi, the maximum crystal misorientation permitted is about 4 to 5' of arc. Since this accuracy cannot be obtained using the usual back-

Jan 1, 1969

By J. C. Danko, R. D. Stout, A. H. Holtzman

The deformation characteristics of pearlite have been studied by light and electron microscopy.1,2 In the electron-microscopic work, deformation was found to take place by 1) ferrite slip which is parallel to the lamellae, 2) slip transverse to the lamellae with both cementite and ferrite deforming, and 3) ferrite-cementite interfacial slip. The transverse slip gives a step-like appearance to the lamellae in light microscopic work. It was thought that spheroidization of deformed pearlite would commence at the regions of maximum cementite deformation, the "stepped" areas. Although there is no possibility for seeing slip in the microstructure if the specimen is polished after deformation, the step-like appearance of the lamellae clearly indicates the transverse deformation. Thus, the areas of cementite deformation are apparent after polishing and the effect of deformed areas on spheroidization may be studied by the usual metallographic techniques. This note reports the result of a metallographic investigation which substantiates that spheroidization begins in the "stepped" areas. An AISI 1080 steel was normalized, re-austeni-tized at 1040°C, and isothermally transformed at 700 ± 4°C for 4 hr. Cubes, 5 mm to a side, were compressed between parallel plates to strains of 20, 40, and 50 pct. After deformation, specimens were heated to 600, 650, and 700°C; withdrawn at increasing time intervals and examined metallo-graphically for the percentage and distribution of spheroidite. The percentage of spheroidite was determined by lineal analysis. A micro structural region considered as spheroidized was one in which a lamellar skeleton was not distinguishable. Table I gives the times necessary for 95 pct spheroidization for each condition of strain and annealing temperature. Fig. 1 shows the microstructure of coarse pearlite compressed 20 pct, then polished and etched. Here the lamellae form a step by bending at two

Jan 1, 1959

Transit A light weight, totally enclosed theodolite, especially designed for mining, has been placed on the market by Askania Werke, A. G. The instrument weighs only 41/4 lb and measures 51/8 x 71/2 in. without tripod and in a waterproof aluminum hood. It may be mounted on tripod or bracket without removing the protective hood. [ ] Standard equipment includes diagonal eyepiece rotating in all directions which eliminates need to be in line with scope for sighting and makes an auxiliary scope unnecessary for steep sights. The transit reads direct to 1 minute and may be estimated to 6 seconds by means of optical micrometer on both horizontal and vertical circles. The telescope in vertical position serves as optical plummet, sighting through an opening in the base. The instrument is shown above mounted for attaching to a pin driven in timber or rock, eliminating tripod or set-up bar in cramped quarters. The chain clamp in the lower picture is used on timber or steel ground supports. Complete with carrying case and set-up brackets, ready for use in a raise, it weighs less than 6 lb, and the protective hood remains on until the instrument is securely mounted. [ ] Accessories for increasing versatility of this mining theodolite are: tripod, electric illumination for optical micrometer and reticule, close range objective lens, and objective lens prism for sighting vertically in front of the instrument. Circle No. 1

Jan 1, 1952

By Edward Wichers

THE purpose of this paper is to set forth the matters of principal interest in connection with work done in the past few years on the purification of the metals of the platinum group, including the study and modification of methods already in the literature and the development of new procedures. For the most part, the results will be given in summary form, reserving the publication of detailed data and directions for a forthcoming paper to be issued by the Bureau of Standards. In recent years increasing interest has been shown in the preparation of the pure platinum metals, both by those concerned with the manufacture of the metals and their alloys for scientific and industrial purposes and those who are engaged in the study of the chemical or physical properties of the elements. The purification of the metals usually has been regarded as a matter so involved and difficult as to require the attention of specialists. It is hoped that this paper will show that any of the metals can be prepared in any desired degree of purity by relatively simple straightforward chemical methods. For the most part, it is thought that the methods given are suitable for small-scale refineries as well as for the laboratory; also, that they will bring the time required for the purification of any of the metals within reasonable limits. The new procedure suggested for purifying platinum should prove to be much shorter than any methods described in the literature.

Jan 1, 1928

By Edward Wichers

THE purpose of this paper is to set forth the matters of principal interest in connection with work done in the past few years on the purification of the metals of the platinum group, including the study and modification of methods already in the literature and the development of new procedures. For the most part, the results will be given in summary form, reserving the publication of detailed data and directions for a forthcoming paper to be issued by the Bureau of Standards. In recent years increasing interest has been shown in the preparation of the pure platinum metals, both by those concerned with the manufacture of the metals and their alloys for scientific and industrial purposes and those who are engaged in the study of the chemical or physical properties of the elements. The purification of the metals usually has been regarded as a matter so involved and difficult as to require the attention of specialists. It is hoped that this paper will show that any of the metals can be prepared in any desired degree of purity by relatively simple straightforward chemical methods. For the most part, it is thought that the methods given are suitable for small-scale refineries as well as for the laboratory; also, that they will bring the time required for the purification of any of the metals within reasonable limits. The new procedure suggested for purifying platinum should prove to be much shorter than any methods described in the literature.

Jan 1, 1928

By R. G. Knickerbocker

THE copper smelter and refinery of The Messina (Transvaal) Development Co. Ltd., at Messina, South Africa, was erected in 1920 and 1921, but initial operations were deferred until late in 1922 on account of the collapse of the copper market in the interim. Because the anticipated production was to be only 20 tons of copper per day from a high-grade matte containing 60 per cent copper, and because the ore did not contain gold or silver in quantities sufficient to pay for separation from the copper bullion, it was decided to design the plant along lines quite different from the modern smelteries treating large quantities of sulfide ores carrying appreciable amounts of gold and silver. The plant was built, therefore, for the production of copper by the Nicholls-James process. By this method two-thirds of the copper matte produced was roasted in a Merton calciner and charged into a bath of the remaining one-third portion of unroasted matte in a reaction furnace. The original design was not only novel in providing for the Nicholls-James process, but also in comparison with new plants built elsewhere, because of factors inherent in the locality. Sources of supply for machinery were very remote; it takes three months after the placing of an order to accomplish delivery of machinery into Messina from the United States. Native labor was available at 30 to 40¢ per 8-hr. shift. These factors permitted plant design which provided no overhead cranes, no matte ladles, no slag pots or other usual mechanical means of transportation between departments. The design resulted in a compact simple plant with furnaces arranged close together and. terraced so as to provide for gravity transfer of molten material from one furnace to another and for manual disposal of products. Fig. 1 shows the relative location of furnaces. The three furnaces are parallel on successively decreasing elevations. A superimposed feed floor was provided above the furnaces. All three furnaces were provided with coal-dust burners served from a Bonnot system of coal-dust transportation, and the waste gases were discharged into waste-heat boilers.

Jan 1, 1932

By Edward Pesout

THE McGill smelter started operations in the year 1907. The smelter furnaces were fired with run-of-mine coal on grates until April 1911, when oil firing was introduced. Oil firing continued until April 1918, when the initial coal-pulverizing plant was started.1 EARLY PULVERIZING PLANT Various alterations were made to that plant during its operation, one of the more important being in connection with the system for delivering pulverized coal. In order to minimize coal-dust explosions and fires, the return portion of the main delivery line was eliminated in the year 1928. Thereafter coal-dust explosions and fires were greatly reduced. Pulverized coal was prepared at this plant primarily for the reverberatory furnaces, but for several years it was also delivered to the converting plant, roasters and power-plant boilers by a system of auxiliary fans and delivery lines. During the period March 29 to April 8, 1929, one reverberatory furnace was fired with pulverized coal produced by an Aero, type J, unit coal pulverizer with a rated capacity of 5 tons per hour. This machine actually pulverized its rated capacity but the product was too coarse. After certain regulations, a finer product was obtained but the pulverizer capacity decreased and this resulted in insufficient coal for efficient furnace operation. Table I gives a comparison of the average screen analyses of the pulverized-coal products from the impact-type unit pulverizer and the regular coal-plant installation. [ ] It was definitely proved that this size and type of unit pulverizer could not furnish sufficient coal of proper fineness to give smelting results comparable to that obtained with the regular coal-pulverizing plant. The coal from this unit pulverizer was so coarse that it did not ignite or burn properly and thus did not produce the proper heat for efficient smelting. During the latter part of 1929 and the early part of 1930, experimental work was conducted with a 7-ft. 0-in. by 48-in. Hardinge conical ball-mill coal-grinding unit, which was installed alongside a furnace in the reverberatory building. Results obtained from the test run indicated that this unit would furnish sufficient coal of proper fineness for good smelting.

Jan 1, 1945

By Nicholas J. Grant, Noboru Komatsu

Metallographic and X-ray studies were made of oxide dispersion strengthened Cu-12 vol pet SiO2 and Cu-3.5 vol pet Al2O3 alloys following time exposures at temperatures approaching the melting. point of the matrix metal. Changes in hardness, oxide particle size and crystal structure were studied to determine the time-temperature stability of these alloys. An interpretation of the mechanism of oxide agglomeration is proposed. One of the most striking features of dispersion strengthened metal-metal oxide alloys is their stability at elevated temperatures, both with respect to recrystallization and maintenance of mechanical properties after exposure at high temperatures. A small amount of work has been done on the re-crystallization phenomenon in dispersion hardened metal-metal oxide alloys'l and several theoretical treatments have been advanced regarding the stability of these alloys by Lenel and Ansell,8 and by Grant and his co-workers.9, 10 This paper reports on metallographic and X-ray studies following various heat treatments of Cu-AI2D3 and Cu-SiO2 alloys at elevated temperatures and the effect of subsequent cold work on the recrystallizalion temperature. An interpretation of the recrystallization behavior of this type of alloy, based on the decomposition and agglomeration of oxides, is proposed. EXPERIMENTAL PROCEDURE Cast ingot bars of copper-1.59 pet Si and Cu-0.77 pet Al, 7/8 in in diam, were annealed in argon for 80 hr at 1000CC for homogenization. The homogenized rods were machined into fine chips and ball milled. Milled particles in the range minus 20 to plus 60 mesh were separated for internal oxidation. The internal oxidation was accomplished by the same method used by Preston and Grant,9 except that the oxidalion temperature for the Cu-Si alloy was 750°C, and for the Cu-A1 alloy was 800°C. These powders were then hydrogen-reduced at 450°C, compacted in a copper container, evacuated at room temperature to 0.04 µ, and sealed for extrusion. They were extruded at 1400°F (760°C) with a ram speed of 55 in. per min for an extrusion ratio of 15.6 to 1 to give a rod 0.38 in. diam by about 3 ft long.

Jan 1, 1962