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By B. G. Reisdorf

This paper describes the microstructural changes that occur when quenched ultrahigh-strength steels containing OA pet C and various amounts of nickel, silicon, and cobalt are tempered. The changes that occur in hardness, yield strength, and martensite diffraction-peak widths when these steels are tempered are related to the precipitation of the carbide phases. An unea$ectedly high silicon content (about 30 pct) was found in the E -carbide phase in a steel containing only 1.5 pct Si. TEMPERED martensitic steels have such wide-spread utility that they have been the subject of numerous investigations, and a sizable amount of literature has developed on this subject.M This investigation, which is a part of a larger program to correlate microstructure with mechanical properties at a variety of strength levels, is limited to the microstructural changes that occur when a quenched 0.40 pct carbon steel (USS Airsteel X-200 steel) is tempered, and to the effects of the alloying elements—nickel, cobalt, and silicon—on these microstructures. Used in this investigation were electron microscopy, electron-diffraction identification of the carbide phases, electron-probe micro-analysis of the carbides, X-ray determinations of retained austenite, and measurements of martensite X-ray diffract ion-peak widths. MATERIALS AND METHODS The chemical analyses of the eight heats examined eats No. 30 through 37) are shown in Table L Heat No. 30 has the chemical com~osition of Airsteel X-200, and the remaining seven heats contain various amounts of nickel, chromium, cobalt, and silicon. The heats were air-melted in an induction furnace and cast into 8 by 8 in. ingots that were subsequently heated to 2300 and rolled to 1-in.-thick plate. Oversize 0.505-in.-diam tensile specimens were rough-machined from the plates and austenitized in air at 1700° F for half an hour and oil-quenched. The specimens were then tempered in air at temperatures of 400° to 1000 for tempering times of 1, 4, and 16 hr, and finish-machined to 0.505-in.-diam tensile specimens. Electron micrographs were prepared from Formvar replicas of the midthickness of tensile-specimen shanks that had been electrolytically polished and etched in nital. Electron-diffraction patterns were obtained from carbon-extraction replicas. The replicas were prepared by etching the sample surface in the same manner as for microscopy, evaporating carbon on the etched surface, and re-etching the sample to free the carbon film and the precipitate particles. Electron-probe microanalysis was performed on some of the extraction replicas. To obtain adequate fluorescent X-ray intensities, several thicknesses of replica were exposed to the electron beam so that the results represent an average composition of the extracted particles rather than an analysis of single precipitate particles. The retained austenite contents of the specimens were determined by an empirical X-ray diffraction

Jan 1, 1963

By W. H. Smith

IN connection with some recent work on the effect of impurities on the ductility of chromium, it appeared desirable to know the solid solubility of carbon in chromium. A literature survey indicated that this information was not available. Although considerable work has been done on the Cr-C phase diagram,&apos;.&apos; previous investigators have been more concerned with the structure and phase boundaries of the carbide phases than with the terminal solid solution. The phase diagram shown in Fig. 1 is taken from the work of Bloom and Grant&apos; and represents the most recent determination. As indicated by the dashed line, the a solid-solubility limit was not determined. Experimental Procedure Alloys of chromium were prepared from hydrogen-treated and vacuum-degassed electrolytic chromium plus spectrographic grade carbon. The oxygen and nitrogen content of the alloys was <0.002 pct. After melting, analysis of the alloys showed them to contain 0.02, 0.08, 0.15, and 0.55 pct C. Pieces of the alloys were heated in a protective atmosphere to various temperatures and then quenched after holding for a time sufficient to insure equilibrium. Microscopic examination of the as-quenched alloys for the presence of a second phase was used as a measure of the solubility limit. The heats were made in a multiple hearth arc-furnace using a zirconium-gettered static argon atmosphere. A zirconium melt was made before each Cr-C heat. Triple melting was used to insure ingot homogeneity as shown by microscopic examination. The alloys were prepared by adding portions of a 4.5 pct C-Cr master alloy to high purity chromium. The carbon contents listed previously were those obtained by analysis. The nitrogen and oxygen contents after arc melting were both <0.002 pct. Sections 1/8X1/4X1/2 in. were cut from the 100-g ingots and a hole drilled in one end in order to suspend the sample from a molybdenum wire. After the surface was carefully cleaned, a sample of each melt was hung in a mullite tube heated externally by a platinum resistance furnace connected to a vacuum system. The lower portion of the mullite tube was sealed to Pyrex and closed off several inches below the furnace. This was filled with sili-cone oil kept cold by circulating cold water around the outside of the Pyrex. Quenching into the oil bath was achieved by melting a fuse wire supporting the sample. It required about 4 sec for the sample to cool from 1400" to 600°C. This severity of quench was considered satisfactory to freeze-in the high temperature equilibrium. For tests made at temperatures of 900" to 1200°C, heating was done in vacuum; for tests above 1200°C, an argon atmosphere was used. The holding time employed ranged from 12 hr at 900°C to 6 hr at 1400°C. Experiments were performed at temperatures of 900°, 1000°, 1100°, 1200°, 1300°, and 1400°C. Microscopic examination for evidence of a second phase was done at X1500. Experimental Result The microstructures of a 0.08 pct C-Cr alloy as-cast and after quenching from 1300°C are shown in Figs. 2 and 3. A 0.15 pct C-Cr alloy quenched from 1300°C is shown in Fig. 4. The data obtained from the quenching experiments is shown graphically in Fig. 5. If the Van&apos;t Hoff equation is obeyed, a plot on a logarithmic scale of the mol fraction of solute vs the reciprocal of the absolute temperature should give a straight line. For dilute solutions the weight percentage can be substituted for the mol fraction without introducing any appreciable error. The Van&apos;t Hoff equation can then be written as where H is the heat of solution in calories per mol. The slope of the straight line on the log pct C vs 1/T plot gives the value of AH. Assuming that the Van&apos;t Hoff equation is obeyed, which is probably justified for the dilute solution of carbon in chromium, the heavy straight line shown on Fig. 5 represents the best fit of the data. This line was obtained as follows. On Fig. 5 the results of the microscopic examination of all alloys following quenching were plotted and designated as to whether one or two phases were seen. Below 1100°C all alloys showed a second phase on quenching. The heavy vertical lines shown in Fig. 5 therefore represent the possible range of the ter-

Jan 1, 1958

By C. H. Li, R. J. Stokes

This paper compares the fracture behavior of tungsten rods in three conditions: recrystallized. recovered, and wrought. Notched specimens suhjected to a 50 in.-lb impact load showed ductile-brittle transitions at 700, 4.90°, and 440°C, respectinely. The recrystallized material had an equiaxed pain structure and jracbred by simple cleavage from a grain boundary source at all temperatures up to 700°C. The wrought and recovered material had an elongated fibrous structure and at low temperatures fractured by cleavage originating from the notch. As the transition temperature was approached cleavage was preceeded by more and more intergvanular splitting which deflected the crack front into planes parallel to the tensile axis. The enhanced toughness of wrought and recovered tungsten was attributed both to its inability to initiate cleavage because no pain boundaries were suitably oriented perpendicular to the tensile stress and to its inability to maintain cleavage because of intergranular splitting ahead of the crack. It has been appreciated for a long time in a qualitative manner that the room-temperature brittleness of fully recrystallized tungsten may be alleviated by working the material at relatively low temperatures.&apos; More recently this difference in mechanical behavior between wrought and recrystallized tungsten has been examined quantitatively by measurement of the tensile properties as a function of temperature. In these experiments brittleness has been expressed in terms of ductility or reduction in cross-sectional area upon tensile fracture or in terms of the bend radius before fracture under bending.&apos; This work has shown the existence of a fairly sharp transition from brittle to ductile behavior with an increase in temperature. The ductile-brittle transition temperature for recrystallized material is approximately 200°C higher than for wrought material. An increase in strain rate, small additions of impurity,&apos; or an increase in grain size4 shift the respective transition temperatures to higher values, but the difference between them remains approximately the same at 200°C. A number of explanations for this embrittlement by recrystallization have been given. It has been blamed either on the concentration of impurity at the grain boundaries, the increase in grain size, or the change in texture which occurs upon recrystallization. The present paper examines the effect of different heat treatments on the notch-impact behavior of commercial powder-metallurgy tungsten rods. The change in the ductile-brittle transition temperature for this method of loading and the fracture mode has been related to the different mi-crostructures produced by heat treatment. EXPERIMENTAL PROCEDURE Commercial swaged powder-metallurgy tungsten rods 1-3/8 in. in length and 1/8 in. in diameter were machined to introduce a sharp V notch 0.030 in. deep. To change the microstructure from that of the as-received wrought material some of the specimens were subjected to an anneal in nitrogen either at 1300° or 1400°C for 8 hr or at 1600° or 2000°C for 1/2 hr. The notched rods were then placed in a miniature Charpy-type impact machine and struck at their midpoint (opposite the notch) with a hammer designed to deliver 50 in.-lbs of energy. The strain rate at the base of the notch was estimated to be approximately 100 sec-1 at the instant of impact. The specimens were heated in situ to the desired impact temperature. The microstructures produced by the various anneals were studied by both X-ray diffraction and metallographic techniques. Fig. 1 reproduces the microstructures observed metallographically following a 10-sec electroetch in a 10 pct KOH solution. Fig. l(a) shows the elongated fibrous grain structure of the as-received material. Following the anneal at 1300" or 1400°C the grain structure was still elongated as shown in Fig. l(b) but the etch pits delineated dense polygonized dislocation arrays within many of the grains. Occasionally a relatively dislocation-free recrystallized grain was found growing into the matrix. The anneals at 1600° and 2000°C resulted in complete recrystallization and some grain growth. The grains produced at 1600°C were still slightly elongated as shown in Fig. l(c) whereas the anneal at 2000°C produced equiaxed grains. The changes in grain size produced the expected changes in the X-ray back-reflection patterns; there was no indication either in the as-received material or the annealed material of any preferred orientation. RESULTS a) Impact Behavior. Fig. 2 reproduces the ductile-brittle transition curves measured in the manner described in the previous section. It can be seen that under these testing conditions the as-received

Jan 1, 1964

By M. C. Leverett, M. E. True, W. B. Lewis

This paper states the theory underlying the design of two kinds of dimensionally scaled models of parts of idealized oil fields. One of these simulates an oil well and its surrounding sand for a distance of 16 ft. radially from the well. The other model simulates linear flow through layered sands. Construction and operation of the models are described and typical data are given. The unique features in the design of the models are: (I) the treatment of the permeability-viscosity quotient as a single variable and (2) the use of previously reported experimentally developed relations between relative permeability and saturation and capillary pressure, saturation, porosity, permeability and interfacial tension. The models at present simulate flow of oil and water only, through unconsolidated sands. They are superior to unscaled models, which may give rise to erroneous conclusions. The models are designed to study the desirability of various methods of well completion and the effects of various factors on recovery of oil from layered sands. Introduction Recent work on the fundamental behavior of flowing mixtures of fluids in sands has resulted in the development of some new theory in this field, much of which has been presented in previous papers.l-4 However, the application of this theory to the behavior of oil wells or oil fields has proved too complicated for ordinary mathematical techniques, except in very highly simplified cases. A practical solution to this problem appears therefore, to lie in the use of dimensionally scaled models of elements of oil fields. The object of this paper is, first, to present the theoretical and experimental basis of the design of such models, and, second, to describe their construction and operation. Experiments now under way on the models already built will yield material for other reports, which will be devoted to interpretation of the results in terms of oil-field behavior. So far, simple dimensional models of two kinds have been built and are being operated. These models represent different parts of an idealized oil field but obey the same underlying theory. The only fluids represented are oil and water, since certain questionable approximations are necessary for gas-liquid systems. General Theory Dimensional models have been used in other fields for a long time, and their theory is adequately given in the literature. 5 Here, it suffices to state that each physical element entering into a dynamic relation may be given a definite description in terms of three fundamental, but arbitrarily chosen, dimensions. These usually are mass, length, and time, symbolized here by the small letters m, I, and t. Two systems are said to be dimensionally similar or dimensionally scaled if for each element in one system there is a corresponding element in the second system and the ratios of the numerical magnitudes of corresponding elements are constant for all elements of the same dimensional type.

Jan 1, 1942

By W. B. Lewis, M. E. True, M. C. Leverett

This paper states the theory underlying the design of two kinds of dimensionally scaled models of parts of idealized oil fields. One of these simulates an oil well and its surrounding sand for a distance of 16 ft. radially from the well. The other model simulates linear flow through layered sands. Construction and operation of the models are described and typical data are given. The unique features in the design of the models are: (I) the treatment of the permeability-viscosity quotient as a single variable and (2) the use of previously reported experimentally developed relations between relative permeability and saturation and capillary pressure, saturation, porosity, permeability and interfacial tension. The models at present simulate flow of oil and water only, through unconsolidated sands. They are superior to unscaled models, which may give rise to erroneous conclusions. The models are designed to study the desirability of various methods of well completion and the effects of various factors on recovery of oil from layered sands. Introduction Recent work on the fundamental behavior of flowing mixtures of fluids in sands has resulted in the development of some new theory in this field, much of which has been presented in previous papers.l-4 However, the application of this theory to the behavior of oil wells or oil fields has proved too complicated for ordinary mathematical techniques, except in very highly simplified cases. A practical solution to this problem appears therefore, to lie in the use of dimensionally scaled models of elements of oil fields. The object of this paper is, first, to present the theoretical and experimental basis of the design of such models, and, second, to describe their construction and operation. Experiments now under way on the models already built will yield material for other reports, which will be devoted to interpretation of the results in terms of oil-field behavior. So far, simple dimensional models of two kinds have been built and are being operated. These models represent different parts of an idealized oil field but obey the same underlying theory. The only fluids represented are oil and water, since certain questionable approximations are necessary for gas-liquid systems. General Theory Dimensional models have been used in other fields for a long time, and their theory is adequately given in the literature. 5 Here, it suffices to state that each physical element entering into a dynamic relation may be given a definite description in terms of three fundamental, but arbitrarily chosen, dimensions. These usually are mass, length, and time, symbolized here by the small letters m, I, and t. Two systems are said to be dimensionally similar or dimensionally scaled if for each element in one system there is a corresponding element in the second system and the ratios of the numerical magnitudes of corresponding elements are constant for all elements of the same dimensional type.

Jan 1, 1942

By Frank L. Nason

In the year 1904 an eminent Swedish geologist prepared a report on the iron-ore reserves of the world. His estimates follow: Countries. Tons. United States,.1,100,000,000 Great Britain,.1,000,000,000 Germany,.2,200,000,000 Spain,.. 500,000,000 Russia and Finland,...... 1,500,000,000 France,..1,500,000,000 Sweden,..1,000,000,000 Austria-Hungary,....... 1,000,000,000 Other countries,1,200,000,000 Total,.10,000,000,000 The iron-ore allotted to the United States by the Swedish geologist is barely sufficient to last 20 years at. the present rate of consumption. On the other hand (according to Edwin C. Eckel,&apos; from whom the above and following statistics are quoted), there is hardly need for worry on the part of our iron industries for the next two centuries or more. Upon the basis of careful work by the U. S. Geological Survey, in which Mr. Eckel has taken an important part, the following estimates are definitely, but by no means finally, given for the United States: District. Tons. Lake Superior District,... 1,500,000,000 to 2,000,000,000 f red hematite,.. 1,000,000,000 Alabama, brown hematite, hematite, . 725,000,000 red hematite,.. 200,000,000 Georgia, { brown hematite, . 125,000,000 Tennessee, { red hematite,.. 600,000,000 Tennessee, { brown hematite,hematite, . 225,000,000 f red hematite,.. 50,000,000 Virginia, } brown hematite, . 300,000,000 Total,..4,725,000,000 to 5,225,000,000

Jan 1, 1913

By Richard Hodgson

FMC Corporation, at their mine and soda ash refinery near Green River, Wyoming, currently mines in excess of 3 million tons per year of trona. Upon completion of the current expansion, the mine will be producing in excess of 4.0 million tons per year. The single level mine, approximately 1,500 feet in depth, is currently serviced by five (5) concrete lined circular shafts varying in diameter from 12 ft. to 24 ft. A sixth shaft is complete, but not yet operational and the seventh is currently being sunk. Two of the shafts are equipped with single drum hoists. The original production shaft is equipped with a double drum hoist. The newest production shaft and the main service shaft are both equipped with ground mounted friction hoists. These friction hoists have given excellent service and another will soon be installed as a man and material hoist at No. 7 Shaft. There are a number of advantages that the ground mounted hoist has over a tower mounted hoist. There are also operating problems common to both. FMC&apos;s original experience with ground mounted friction hoists began in 1962 with the conversion of a single drum hoist to a friction hoist. The converted hoist was an Ottumwa with a 5 ft. diameter drum and a 4 ft. face. This hoist had been installed at the No. 3 Shaft for some years prior to its conversion to a friction hoist. At the time the conversion of this hoist was made, there were no friction hoists in service in Wyoming. Wyoming mining laws required that all conveyances carrying men be equipped with safety dogs. Since it was desired that wire rope guides be used, safety dogs were impractical. Agreement was reached with the State Mine Inspectors that safety dogs would not be necessary provided that recommended rope safety factors for hoisting men would still be maintained if one hoisting rope was broken. Since-the shaft is approximately 1,500 ft. deep, the recommended safety factor is 6.0 so that this installation has a safety factor in excess of 8.0 for hoisting men when new ropes have been installed. The hoist conversion was engineered by Lake Shore, Incorporated. The friction ring was made in halves and bolted over the original drum face which had been machined to remove the grooves. The ring provided for four 3/4 in. diameter ropes on 8 inch center to center spacing. The pitch diameter of the modified drum was 72 inches. The grove liners are hald in place by hard-wood wedges bolted to the drum. The other modification required by the conversion was an increase in size of bearing caps and the hold-down bolts because of the increased force tending to lift the drum.

Jan 1, 1975

By Arthur La Motte

I NDUSTRIAL explosives, as distinguished from military explosives, include high explosives and blasting powder. The high explosives which are best known are straight dynamite, gelatin dynamite, ammonia dynamite and permissibles. There are two kinds of blasting powder, saltpetre blasting powder and nitrate of soda blasting powder. Blasting powders are mechanical mixtures of nitrate of potash or nitrate of soda with sulfur and charcoal, highly compressed, granulated and glazed. They ignite from a spark and burn with relative slowness, the rate of burning and hence the rate of conversion into gases depending upon the size of the granulation and upon the degree of. confinement under which the powder is placed. High explosives, on the other hand, are chemical compounds which detonate; that is, when the explosive is subjected to a violent shock, provided in practice by a blasting cap or an electric blasting cap, the molecule of the essential ingredient, usually nitroglycerin, is disrupted and the energy and heat released cause any other explosive ingredients which may be present, such as ammoniuin nitrate or T.N.T., to decompose with a resultant evolution of gases at an extremely rapid rate varying from 6000 to 20,000 ft. per second.

Jan 1, 1924

By Parviz Montazer, Robert King, William Ubbes, Gideon Chitombo

This paper describes the results of a detailed study that was undertaken to define the spatial distribution of permeability within a five meter thick envelope around the CSM/ONWI room. Detailed fracture orientations and distribution were determined through mapping of the walls of the opening, logging of oriented core, and visual examination of borehole walls with a borescope and a T.V. camera. Over 3,500 measurements were made from which the three dimensional distribution of fractures was determined. Two principally different testing equipment designs and various methods of air injection tests were used in all boreholes to identify and characterize conductive fractures. Through analizing the distribution of permeability and fracture index around the room a zone of blast damage of approximately .5 m thickness was delineated. The effect of stress modification seems to extend farther into the host rock to approximately 3.5 m depth.

Jan 1, 1982

By R. J. Mechin

TOP-SLICING was introduced in the Pachuca district in 1917 by T. C. Baker, at that time mine superintendent, of the Santa Gertrudis mine. There then existed 1200 ft. (365.7 m.) below the surface, lying between the fourteenth and eighteenth levels (a vertical distance of 108 meters) a block of ore having a length of 295 ft. (90 m.), and an average width of 82 ft. (25 m.) and dipping at an angle of 65°. This block lay in the hanging wall of the vein and consisted of highly altered and fractured andesite, cut through with mineralized quartz stringers. On the foot-wall side, 26 ft. (8 m.) of old filling, left by former operators, was of payable grade. Stoping therein was first undertaken by the square-set filling system, but because of the extremely heavy hanging wall and loose dry filling in the foot wall, all square setting had to be accompanied by spiling, which made the operation exceedingly slow and costly. A system of mining was sought that would eliminate the difficulties inherent to the square-set system in heavy ground and that at the same time would effect the desired economies in mining. After several years, top-slicing has met all the conditions most satisfactorily, so that when similar conditions presented themselves in El Bordo mine, this method was adopted with necessary modifications. El Bordo mine is operated by the Santa Gertrudis company, and is situated about two miles north of Pachuca. Because of the diversity of the orebodies, a number of different mining methods are in use, among them top-slicing.

Jan 10, 1925

By D. L. Albright, R. W. Kraft

Solidification experiments were conducted with the objective of testing the theory of eutectic colony formation. Appropriate control of variables in tests on a series of high-purity aluminum-copper specimens of eutectic composition resulted in the observation of three types of eutectic microstructures, these being a unique structure consisting of lamellae essentially parallel to one another, a banded structure, and the colony structure. Lamellar faults, which are morphologically similar in many respects to edge dislocation models in crystals, produced a complex substructure in these specimens. SOLUTE rejection at the advancing solid-liquid interface of a unidirectionally solidified single-phase metal can cause the liquid immediately in front of the interface to become constitutionally super-cooled below the equilibrium liquidus temperature. Constitutional super-cooling occurs if the solidification rate, R, is too rapid, or if the thermal gradient in the liquid at the interface, G, is too low. 1 This constitutionally supercooled layer in turn stabilizes a cellular rather than a planar interface.&apos; A similar cellular interface has been observed when lamellar and other types of eutectics were unidirectionally solidified, and it has been shown that the cellular interface led to the formation of eutectic colonies.&apos; The lamellar structure is fan-shaped at the edges of colonies (which correspond to valleys or grooves in the cellular interface) because the lamellae grow normal to the local interface. One of the possible mechanisms which might cause the formation of the cellular interface, in the case of solidifying eutectic alloys, is constitutional supercooling of the liquid with respect to a third component rejected by both phases of the eutectic.3,4 On the basis of the analogy between the solidification of single-phase metals and binary eutectics, a eutectic alloy should solidify with a planar interface if the ratio of G/R is sufficiently high to compensate for any impurity which might be present and causing constitutional supercooling. The fan-like microstruc-ture of eutectic colonies should not occur under these conditions and the lamellae should be parallel to one another and to the solidification direction for extended distances. The experiments conducted in this investigation were designed to test these ideas. Following a resume of the experimental procedure, the various microstructures observed during the study are described, and their relationship to the growth conditions which produced them is discussed. EXPERIMENTAL PROCEDURE The eutectic between an aluminum solid solution and 0 phase (approximate composition CuA12) was chosen for this work for the following reasons: it was known that a lamellar structure forms, the eutectic temperature is low enough to facilitate experimental work, and the components can be procured commercially in a very pure form. High-purity copper (est. 99.999 pct Cu, obtained from National Research Corp.) and spectrographic aluminum rods, having impurities other than copper estimated to be Zn-15 ppm, Mg-10 ppm, Fe-3 ppm, Na-2 ppm, Cd-1 ppm, and Mn < 1 ppm, were melted in a stabilized zirconia crucible in a vacuum induction furnace at a pressure of 10 pof Hg. The melt was superheated to about 1000°C to assure mixing, cooled to 780°C and cast into an investment mold which yielded sixteen cylindrical specimen blanks 1/2 in. in diam and 5 1/2 in. long. The casting was allowed to solidify under vacuum. This master heat had an analysis of 32.6 wt pct Cu and 67.4 wt pct A1 by difference. The cylindrical specimen blanks were remelted and solidified unidirectionally in an apparatus illustrated schematically in Fig. 1. An RF induction coil heated

Jan 1, 1962

By Tracy C. Jarrett

In 14-karat gold alloys, as in 10-karat gold alloys,3 the addition of such metals as zinc, nickel, copper and silver produces a wide range of physical and chemical properties such as color, hardness, corrosion resistance and melting points. These important factors made gold alloys desirable in the optical work and for jewelry. In 14-karat gold alloys, as well as in 10-karat or 12-karat, it is possible to have two golds of the same color, one of which will corrode more than the other, although it may be harder. Some of these alloys have been investigated by F. E. Carter,&apos; E. M. Wise,= and L. Sterner Rainer.4 In this group of alloys the gold content of 58.3 per cent (14-karat) was held constant, while the copper varied from 36 to 24 per cent. The balance of the alloy consisted of one, two, or three of the metals silver, zinc, and nickel. All the alloys were melted in an induction furnace and cast into an ingot that measured 3 by 1/4 by 3/4 in. The method of determining the melting points, color determinations and acid test have been discussed in previous papers by the author.2, 3 It is necessary to use small test bars (Fig. I). The tensile bars were annealed at 1300oF. for 20 min. and then air-cooled. There being a very marked drop when the yield point was reached, "the drop of the beam" method was used in determining the yield point. Alloys Gold-copper.zilzc A~loys.—Gold-copper-zinc alloys melt, cast, and labricate easily. The low melting points, however, limit their use to some extent. The physical properties of these alloys are not entirely satisfactory. When the ultimate strength is satisfactory, the elongation and reduction of area are too low (Table I). Gold-copper-sinr-nickel A lloys.—In this group of alloys, in which zinc and nickel replace copper in approximately equal parts (Table I), the yield point, hardness, and ultimate strength increase with the increase of zinc and nickel content, while the reduction of area and elongation decrease. The physical properties are desirable, particularly of the white gold alloys. The alloys of this group are not difficult to cast and fabricate, and most of these colors could be used commercially. Gold-copper-nickel A lloys.—Gold-copper-nickel alloys are similar to the gold-copper-zinc and the gold-copper-zinc-nickel alloys. They do, however, possess high yield point, ultimate strength and hardness, somewhat higher than those of the other two groups mentioned (Table I). The difficulty with these alloys is that they fire-crack readily and heavy rolling is necessary between annealings. Being hard to fabricate, many

Jan 1, 1941

By Tracy C. Jarrett

In 14-karat gold alloys, as in 10-karat gold alloys,3 the addition of such metals as zinc, nickel, copper and silver produces a wide range of physical and chemical properties such as color, hardness, corrosion resistance and melting points. These important factors made gold alloys desirable in the optical work and for jewelry. In 14-karat gold alloys, as well as in 10-karat or 12-karat, it is possible to have two golds of the same color, one of which will corrode more than the other, although it may be harder. Some of these alloys have been investigated by F. E. Carter,&apos; E. M. Wise,= and L. Sterner Rainer.4 In this group of alloys the gold content of 58.3 per cent (14-karat) was held constant, while the copper varied from 36 to 24 per cent. The balance of the alloy consisted of one, two, or three of the metals silver, zinc, and nickel. All the alloys were melted in an induction furnace and cast into an ingot that measured 3 by 1/4 by 3/4 in. The method of determining the melting points, color determinations and acid test have been discussed in previous papers by the author.2, 3 It is necessary to use small test bars (Fig. I). The tensile bars were annealed at 1300oF. for 20 min. and then air-cooled. There being a very marked drop when the yield point was reached, "the drop of the beam" method was used in determining the yield point. Alloys Gold-copper.zilzc A~loys.—Gold-copper-zinc alloys melt, cast, and labricate easily. The low melting points, however, limit their use to some extent. The physical properties of these alloys are not entirely satisfactory. When the ultimate strength is satisfactory, the elongation and reduction of area are too low (Table I). Gold-copper-sinr-nickel A lloys.—In this group of alloys, in which zinc and nickel replace copper in approximately equal parts (Table I), the yield point, hardness, and ultimate strength increase with the increase of zinc and nickel content, while the reduction of area and elongation decrease. The physical properties are desirable, particularly of the white gold alloys. The alloys of this group are not difficult to cast and fabricate, and most of these colors could be used commercially. Gold-copper-nickel A lloys.—Gold-copper-nickel alloys are similar to the gold-copper-zinc and the gold-copper-zinc-nickel alloys. They do, however, possess high yield point, ultimate strength and hardness, somewhat higher than those of the other two groups mentioned (Table I). The difficulty with these alloys is that they fire-crack readily and heavy rolling is necessary between annealings. Being hard to fabricate, many

Jan 1, 1941

RUSSIA was the United States Number One source of manganese ore in 1948 when 34 pet of imports were received from that source, stated Norwood B. Melcher, assistant chief, ferrous metals and alloys branch, Bureau of Mines. In 1949, this country received only 20 pet of 1948 shipments from Russia, and only token amounts are now being received. Aggressive programming by industry and government resulted in prompt increases in shipments from major, producing sources; India, Gold Coast, and the Union of South Africa all increased exports to fill the vacuum left by Russia and provided an excess adequate to increase total imports approximately 290,000 short tons in 1949. Again in 1950, and with, even less ore from Russia, imports increased another 290,000 short tons. Since the shift from Russia as a source of manganese, the United States has received in total about 85 pet of its imports from India, Union of South Africa, Gold Coast, and Brazil in that order of importance. Producers of both home consumed and merchant ferromanganese have been able to adjust downward the manganese content of the home-consumed product and so obtain partial relief. Millions of tons of steel were produced in 1951 with a relatively low grade ferromanganese. This adjustment has been made without decreasing the quality of the steel, although with some increase in cost through introduction of new problems, including increased hand- . ding of material and additional removal of carbon. Forced into a pattern of price and grade structure such as exists today, the producer of ferromanganese must adopt one of three possible courses as a short-range program: 1-He may continue to deplete his stocks by producing standard (78 pet) ferromanganese and hope that the future will bring some form of relief; 2-he may attempt to produce 78 pet ferromanganese by paying higher prices for premium ores; or 3-he may drop the grade of ferromanganese and stretch stocks and future supplies of ore as far as possible. The present rundown condition of Indian railroads is attributed to the fact that the service has had no opportunity to recuperate since the beginning of World War II, while the demand for the movement of commodities has probably increased. The Union of South Africa has expanded its exports to the United States greatly since 1948, but, the showing of that country in 1951 was disappointing. Efforts have been made for some time by firms in the United States, at the urging of the manganese miners in the Union, to prevail on the railroad authority to grant and make available larger allocations of cars for manganese ore movement. As a whole, such efforts have been unsuccessful. Although the allocation of rail shipping has been the obvious factor in the decreased movement of ore, many other less determinate factors appear to be involved. Brazil, long an important supplier of manganese to the United States, has important manganese deposits in three areas, all of which are significant to this country. The Gold Coast is an important source of supply. Its metallurgical ore is particularly of significance because of its unusually high grade which permits considerable latitude in blending with the lower grade materials of South Africa and India. The Belgian Congo should have an output of 100,000 tons or more annually beginning this year. R. S. Dean presented two papers. One with K. M. Leute on hydrometallurgical methods for recovery of manganese from domestic ores and one as sole author on the so-called carbamate or Dean process. The two papers tied into each other. In the first mentioned he reviewed the various processes applicable to oxidized, and nonoxidized and reduced ores. The advantages of each .were pointed out. So far the only process tried on a substantial scale on oxidized ores was the SO2 process used at Las Vegas, Nev., on Three Kids ore during World War II. Many problems were encountered. Some of them were whipped while some of those remaining perhaps would have been whipped had time permitted. Since then work has been done elsewhere to avoid the formation of the troublesome thionates encountered at the Three Kids plant. Dean discussed the thionate and NO, processes as applied to oxidized ores. The only commercially used process on reduced ores is that of making electrolytic manganese. Among others that have been considered are the nitric acid process, the Bradley-Fitch ammonium sulphate process, and Dean&apos;s ammonium carbamate process. Dean&apos;s thesis was that extremely large tonnages of so-called low grade manganese ores are available, and that these should not be depleted in attempting to simulate a foreign metallurgical grade ore. He pointed out that the grade of the domestic manganese ores would be considered high if the same grade were found in copper ores. The selling price of electrolytic manganese and electrolytic copper are roughly the same. In addition to electrolytic manganese, he believes that domestic ores should be used to make exceptionally high grade products. These might be battery grade oxide or substantially pure oxide sinter, which might be used for high manganese alloys or for upgrading metallurgical grade manganese to produce a high manganese ferroalloy. The carbamate process is based on the fact that manganous oxide is readily soluble in concentrated ammonia solutions containing ammonium salts. In solutions of sufficiently high concentration the manganese exists as an anion. Lixiviants of ammonia and ammonium carbonate permit extraction of the manganese from reduced ores and the manganese can be recovered as carbonate by heating or by driving off ammonia. R. V. Lundquist presented a paper on upgrading high-silica ores or concentrates with sodium hydroxide to extract silica and to yield a product with a more favorable manganese: silica ratio. The NaOH is, regenerated in part by CaO.

Jan 1, 1952

By G. O. Prickett, P. Somasundaran

An experimental progmm based on statistical principles is used for optimizing a flotation operation for the separation of minerals. In this case, flotation of sylvite from sylvinite ore with amine and starch as the flotation reagents was studied to find the optimum reagent levels at various slime levels. The experiments were first done on a two-level three-factor design. Analysis of the results showed that the interactions between various factors were significant. Hence, a first-order linear model of the flotation response would not be accurate. The two-level three-factor design was expanded into a composite design in order to test the fit of a higher-order model. Data were treated to obtain an expression for flotation response as a function of the different variables, to predict the optimum reaaent levels at various slime levels, and also to determine the path of steepest ascent. Tests around the predicted optimum and along the path of the steepest ascent were done until a near-optimum region was obtained. Exploration of the nature of the response surface in that region established the actual location of the maximum response. The optimum amine level was found to be 0.20 lb of amine per ten of ore at all slime levels, while the optimum starch level varied as a function of the slime present. Computer access at the laboratory by means of a teletype terminal on a commercial time-sharing system enabled efficient and accurate treatment of experimental data. The efficiency of experimental investigations can be improved significantly by the use of experimental design and data analysis based on statistical principles. The common approach used in experimental research is to study a property of a system as a function of "one-variable-at-a-time". Several authors&apos;-4 have pointed out the inadequacy and deceptiveness of this method. Results obtained for the effects of a variable on the measured response of the system using

Jan 1, 1970

By H. C. Chang, N. J. Grant

REEP studies and measurements in most in-V> stances are based on a relatively gross gage length. Even in some recent theoretical studies on the mechanism of creep, changes were followed by means of X-rays and metallography without regard for the behavior of the individual grains and grain boundaries.&apos;" Analytical studies of creep have frequently indicated that more than one competing process is operative and that the ultimate creep performance depends on the effects of temperature, time, and strain rate as well as grain size.&apos;-" he grains and grain boundaries are known to respond differently to these variables but the extent of the response is still little known, especially in poly-crystalline materials where the relative orientations of grains and grain boundaries are important. This paper reports some experimental observations of the behavior of the grain boundaries and their effect on the deformation in the grains. High purity aluminum was used to avoid complications of aging reactions, second phase, inclusions, etc. Experimental Procedure A small vertical nichrome wound furnace was built to permit direct loading on the test specimen. This furnace is capable of operating up to about 1300°F with reasonable temperature distribution. A ground rectangular quartz window, 1.25x0.5 in., is imbedded in the external stainless steel tube to permit observations of the creep process with a microscope. An argon atmosphere ,was provided to prevent oxidation. The quartz window caused a temperature gradient between the back and front surfaces of the specimen of 15" at 700°F. The temperature gradient could be cut down to 3°F along the length of the specimen by adjusting shunts across the furnace windings. An ordinary metallurgical microscope with a working distance of 14 mm was rebuilt so that it could be moved in three mutual perpendicular directions. Visual examination could be made with either a 30X eyepiece or a 15X filar eyepiece. Using an objective of focal length 24.3 mm and a numerical aperture 0.20 a total magnification of 120X or 240X could be obtained. High purity aluminum rated at 99.995 pct was supplied by the Aluminum Co. of America as % in. then the gage portion was further machined to 3/16 in. diam. The ends were Y4 in. diam and threaded to fit available specimen holders. Two opposite flat surfaces of the gage portion were obtained by milling, giving final dimensions of the gage portion of 3/4x3/16x3/32 in. Machined specimens were first electropolished in Jacquet&apos;s solution.&apos; Reference marks were produced by pressing a thin sewing needle into the surface of the specimen. The specimen was then annealed at 900°F for 24 hr and at 1150°F for 12 hr. Typical macrostructures of specimens treated in this manner are shown in Fig. 1. The range of the grain size was 1 to 5.5 mm (see Fig. l), but most of the grains were of 2.5 mm and went through the whole thickness of the specimen. The specimen was re-electropolished and etched electrolytically to reveal the grain boundaries. In order to reveal the orientation difference of the grains, etch pits were produced on the surface of the grains by etching in a mixture of hydrochloric and nitric acids (HC1, 45 pct; HNO,, 10 pct; H,O, 45 , by volume). The specimens were very carefully put into the holders and furnace; yet even with this care, fine slip lines were developed on the specimen surface.

Jan 1, 1953

By Orville R. Lyons

THE Russellton preparation plant of Republic Steel Corp., located north of Pittsburgh, Pa., prepares 3 1/2x0-in. Thick-Freeport coal by means of a 13-ft 6-in. diam Chance cone and 16 No. 7 Deister tables. The plant feed ranges between 370 and 410 tons per hr, of which approximately 31 pct is ¼x0-in. size, and the plant reject ranges between 14 and 16 pct of the feed. The 3½xY4-in. washed coal, the cone product, is dewatered and desanded by a double-deck Parrish-type shaking screen 46 ft long and 7 ft wide. The 1¼x¼-in. portion is further dewatered by two 4x12-ft single-deck vibrating screens. The ¼x0-in. washed coal from the tables is distributed to three 54x70 in. Bird centrifuges. The dewatered centrifuge product is combined with the product of the de-watering screens prior to loading into railroad cars. During the early part of 1951 complaints were received from officials at Republic&apos;s coke ovens concerning the moisture content of Russellton washed coal. The records revealed that during the first half of 1951 the shipped washed coal moisture averaged

Jan 1, 1954

By James M. Hodge

The Cumberland Gap extension of the Louisville and Nashville railroad, recently completed from Cumberland Gap to Norton, 71 miles, connects at the latter point with the Norfolk and Western, making a direct through line from Louisville to Norfolk. The whole of this connecting link skirts the southern boundary of the southwest Virginia coal region, but for the first 57 miles of its course it is separated from the coal by a mountain range (Cumberland mountain and its extension, Stone mountain), which bars entrance to the field from that direction, excepting at Pennington Gap, where access may he had to a small area only, which has not yet developed any very satisfactory coal. The railroad passes through the range at Big Stone Gap, and for the last 14 miles of its course to Norton is in direct contact with that part of the coal region known as the Big Stone Gap coal-field. By this road a western and southwestern outlet from the field is secured; the Clinch valley extension of the Norfolk and Western railroad gives exit eastward from Norton, and the South Atlantic and Ohio railroad, built through Big Stone Gap simultaneously with the L. & N. R. R., delivers the coal to points south and southeast. Besides these lines already built, an early connection with the East Tennessee, Virginia and Georgia railroad, via its Rogersville branch, is probable, and connections with the railroads of eastern Kentucky are projected. The Charleston, Cincinnati and Chicago railroad has already done some grading on one of the latter, but the rugged country intervening will prevent its construction till the demand for it becomes urgent. The coal-field embraces in Virginia about 120 square miles, to which should be added some 30 square miles in Kentucky, also tributary to Big Stone Gap, the whole of it underlaid by coal, probably of workable thickness, and much of it by two or more such beds. The determination of the boundaries of the field, however (except on the south, where Stone mountain forms a natural limit beyond which only a small, isolated tract of coal is found), is involved in much

Jan 1, 1893

By John E. Conley

THE slate industry of the United States has shown a marked decline in value of products made annually since the peak year 1925, although there has been moderate improvement over the lean years 1932 to 1934. In 1940, the value of all slate products sold was approximately 5 3/4 million dollars for a total output of 473,450 short tons. The quantity sold was a little less and the value a great deal lower than the annual averages for the past two decades. Enormous quantities of waste materials result from the quarrying, splitting and milling of slate. Obviously, utilization of such waste material is desirable, not only from the viewpoint of economical operation but also for the purpose of conserving natural resources. One possible use is to produce expanded or puffed lightweight aggregate for use in concretes. Such concretes are strong enough for specific uses, and the advantage of lightness could be obtained in such structures as the walls and roofs of buildings, suspension-bridge roadways and various other applications where weight is a factor. Conceivably, these uses could consume an appreciable annual tonnage. USE OF WASTE SLATES FOR MAKING AGGREGATES The lightweight-aggregate industry has been discussed elsewhere4.5 and need not be covered in detail in this paper. The materials commonly utilized are naturally occurring aggregates such as volcanic cinder, tuff and pumice; by-product materials, such as ordinary cinders and air-cooled slags; and the specially manufactured products, including Haydite, Pottsco, Gravelite, Cel-seal, Superock and Waylite. Slates, however, have not been given the consideration they merit, especially in the United States. In the British Isles, some work has been done&apos; on certain Welsh slates by the Building Research Station to stimulate the use of these wastes. REQUIREMENTS FOR RAW MATERIALS As pointed out by Hughes,4 the lightweight-aggregate industry is segregated in regions adjacent to large cities in order to localize the market and avoid the necessity of long freight haulage. Waste slate from the deposits of eastern Pennsylvania, northern Maryland, and Virginia would meet the basic requirement of any low-priced structural raw material. One apparent advantage is attained when slate waste, normally discarded, is utilized in the manufacture of a by-product. Mining or quarrying costs usually have been assessed against the main product. Some additional grinding might be desirable, but this operation would be relatively cheap, as most slates grind easily. It is believed that virtually all slates, when properly heated, will expand to some degree. However, types that will expand from 3 to 7 times their original volume are preferred. Fig. I illustrates the expansion of a Pennsylvania slate. The cube originally

Jan 1, 1942

By W. G. Oldham

By monitoring the capacitance of abrupt p-n junctions it is possible to follow the motion of substitu-tional impurities. A p-n junction is formed by growth of silicon from an Al-Si alloy on an n-type silicon sutstrate at a temperature in the range 650" to 750°C. The diodes are etched and sorted for consistent V-I and capacitance behavior and separated into groups. After irradiation, each set with an unirradiated control set is annealed to various temperatltres for 10 mm and the capacitance remeasnred. For very heavily doped diodes (-1019 per cm3) observable capacitance changes occur at neutron fluences of >1015 per cm 3. The results may be interpreted in seceral ways, the simplest of which is to assume simple vacancy diffiision with small impurity -racancy interaction (at the diffiision, i.e. annealing temperature of 700°C). In this interpretation it is found that a typical vacancy makes about 1024 jumps and travels about 10-5 cm before disappearing. The required effective annihilation center density is about 1016per cm3 . Estimates of the vacancy-impurity interaction can be made and the above numbers correctecl, but for arty reasonable assumptions the number of vacancy sinks connot be much reduced. ThE complete annealing of radiation induced defects requires that the vacancies and interstitials either recombine, travel to the surface of the crystal, or travel to an annihilation center, e.g., a dislocation or a precipitate. If the interstitial is ignored except as a possible vacancy annihilation center at low temperatures,* the motion of vacancies may be followed by monitoring the corresponding motion of substitutional impurities. pfister2 has measured the enhanced diffusion of impurities in an asymmetric shallow diffused silicon structure by optically monitoring the junction movement. In these experiments we monitor instead the capacitance of a heavily-doped deep symmetric p-n junction. The sensitivity for this method is several orders of magnitude higher than in Pfister&apos;s technique, mainly for two reasons: 1) the junction capacitance of a heavily-doped junction is sensitive to impurity movements in the Angstrom range* com- and 2) the junction may be far from the surface which is a major annihilation center for vacancies. THE EXPERIMENT A p-n junction is formed by the epitaxial growth of silicon from an A1-Si alloy on a silicon substrate at a temperature in the range 650° to 750°C. The technique used is the transport of an aluminum melt through a temperature gradient.4 A 10-mil thick aluminum disc is sandwiched between two silicon wafers and the assembly raised to about 650° C with a temperature gradient normal to the sandwich. After about 8 hr the upper (hotter) wafer has been entirely transported and deposited epitaxially on the substrate wafer. The substrate and overgrowth resistivity are measured with a 4-point probe. The as-grown structure is lapped until the wafer is about 1/2 mm thick with the junction in the center. Contacts consisting of electroless nickel covered by electroplated rhodium are applied to both the p and n sides. The wafer is diced into square dice 1/2 to 1 mm on a side and the dice are etched sufficiently to remove approximately 1 mil of silicon. The following results are all for aluminum (p-side) and antimony (n-side) doped specimens with NA =3x 1018 per cm3, ND = 2-8 x 101A per cm3. The diodes are sorted for consistent V-I and capacitance behavior and separated into groups. After irradiation, each set with an unirradiated control set is annealed and the capacitance remeasured. A special capacitance measurement method is used to insure a low sensitivity to shunt resistance. The diode is voltage driven and the current monitored by a phase lock amplifier. It is possible to adjust the detector phase to a point where shunt resistances as low as 100 O have no effect on the reading. The diodes in this study have a capacitance in the range 1000 to 5000 picofarads and a shunt resistance in the range 100 to l06 O depending on the stage of the anneal. THEORY The theoretical problem is twofold: 1) The computation of the amount of impurity diffusion and hence the impurity profile resulting from a given amount of vacancy motion, and 2) the computation of the capacitance from the impurity profile. A comparison of the theoretical and experimental capacitance (in particular the changes) yields the amount of vacancy motion. Vacancy Motion. A convenient parameter to measure the total amount of vacancy motion is Jv the total number of vacancy jumps per unit volume. Although this parameter varies with position in the crystal, owing to vacancy annihilation at the surfaces, it is approximately independent of position far from the surfaces, i.e. in the junction region. In terms of the number of vacancies per unit volume Nv and the vacancy diffusivity given by

Jan 1, 1970