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ZAY JEFFRIES (communication to the Secretary*).-Having seen Mr. Ruder's micrographs of electrolytic iron, I am of the opinion that the tentative explanation offered verbally is correct. Mr. Ruder has informed me that both of the samples were cooled in the furnace. The structures as shown in Figs. Band C resulted from the last cooling through the temperature range near 900° C. Assuming that the rate of cooling through this range was the same in both cases, the differences in struc-ture of the gamma iron in the two samples must have ]:)]-ought about, in some way, the variations in grain size and grain shape shown in Mr. Ruder's micrographs. Even though there is practically no temperature gradient in muffle-furnace treatment during the "soaking" period, during both heating and cooling, there is a temperature gradient. Fig. B should normally have been fine-grained prior to the last cooling, due to the comparatively low maximum temperature to which it was heated (1,000° C.). On cooling through the allotropic change point at 900°, these small gamma grains, iii conjunction with the temperature gradient, should form an ideal condition for germination. Germinant grains should form near the surface of the sample (the-colder portions) and the small gamma grains would be progressively absorbed as they changed into non-gamma iron. The elongated grains in Fig. B, converging toward the axis of the piece of iron, indicate that germinant grains first formed near tine surface and advanced their boundaries toward the interior of the sample. The gamma grains in Fig. C, however, should have been large, prior to the last cooling, due to time high temperature treatment (1,250 to 1,300° C.). In other words, to use one of Prof. Howe's expressions, the crystalline organization should be very complete and the change from gamma to non-gamma iron on cooling would take place reluctantly. This resistance to change from gamma to non-gamma iron would probably be greater in the interior of the large grains than at their boundaries. Non-gamma iron centers or nuclei would probably form at a great many places, at the grain boundaries, thus masking the influence, to a large

Jan 6, 1917

By E. C. IBBOTSON

THIS process was reported upon by the Canadian Commission in 1904, and much detailed information was also given in a paper by Chief Engineer V. Engelhardt.1 Believing that some of the latest particulars of the process will be of interest, I submit the following data. At Gysinge in Sweden during the year ending May 31, 1906, from a fixed furnace giving 1 ton (2,240 lb.) of steel per tap, there were produced 950 tons of tool-steel and special steel ingots. . In carbon and iron tool-steels all the usual tempers were made. The bulk of this steel was made from charges composed of about 80 per cent of Swedish white pig-iron and 20 per cent. of steel-scrap. The percentage of carbon was regulated by the addition of briquettes. Other charges were made from Swedish white iron and steel-scrap. The average time taken per charge, for the year, when adding briquettes, was 7* hr., and the electric energy consumed was 1,128 units (kilowatt-hours) per ton. The average time per charge for white-iron and scrap charges was 5.5 hr., and the electric energy consumed was 886 units per ton. These consumptions include all time and energy lost from various causes, such as bad water-supply, ice, etc. It is quite ordinary practice to complete the charges with briquettes in 6.5 hr., and without briquettes in 5 hr., as shown by the following typical charges White pig-iron, 1,457; steel-scrap, 439; briquettes, 220; ferrosilicon (50 per cent. of silicon), 17 ; ferromanganese (80 per cent. of manganese), 15 lb. ; and aluminum, 1 oz.=

Nov 1, 1906

By John V. Beall

If you will be patient, we will explain how our plans to research the fishing possibilities of the Buffalo River following the SME Fall Meeting turned out, in general, to be an extension of the main theme of that meeting and, in particular, to confirm an astute observation on research made by Australian T. R. A. Davey in his Award-acceptance address at the Pb-Zn Research Luncheon. Buffalo River State Park is reached via Yellville where we tried without success to find one Odie Tollett who had been recommended as a boat liveryman. However, Mrs. Leon Dodd, in the Park, outfitted us nicely with a 17-foot aluminum canoe. Rain had dominated the recent weather of the Ozarks in northwestern Arkansas. So, under a leaden sky and intermittent showers, we stood on the bank of the turgid Buffalo demonstrating to our spouse, Sylvia, how to cast. Of course, with the water up and the sediment, the outlook for catching fish was bad. Sylvia said, however, "Oh, I get it. Let me try. Umm, like this I got one!" Sylvia reeled in a pretty ten-inch brown trout. "The poor thing, let's throw him back."

Jan 1, 1970

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

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

Jan 1, 1970

By Takao Kobayashi

Micro-crack formation zones developed near a crack tip in rocks and ceramics play a significant role in fracture behavior of these materials. In order to study micro- crack formation near a crack tip and its effects on crack behavior, a mica-epoxy composite material was developed. Multi-layer mica flakes were embedded in an epoxy matrix. Under high stress in the vicinity of a crack tip the mica delaminated, simulating the micro-cracking along grain boundaries or crystal planes in rocks and ceramics. A compact tension specimen was fabricated from mica-epoxy composite material. During the test the load and crack opening displacement were measured following the ASTM E561 (R-curve determination) procedure. Through the compliance calibration method the effective crack length and the KR were computed. The experiment clearly demonstrates the formation of micro-cracks and their effects on the overall behavior of the specimen. The paper discusses the significance of micro-crack formation on fracture toughness characterizations, and the advantages of the use of mica-epoxy composite for detailed studies of interaction between the micro-crack formation zone and the specimen geometry and size.

Jan 1, 1982

By B. J. Reid, J. N. Greenwood

It has been shown1 that cavities are formed in the grain-boundaries of copper and 70:30 brass (as well as in magnesium) by the application of tensile stresses at elevated temperatures. For a given rate of strain, cavities are formed in brass at a lower temperature than in copper, and they are larger; it was thought that this earlier onset of cavitation in the alloy might be caused by the distortion produced in the metal lattice by the alloying element. If the cavitation is caused by the vacancy-migration mechanism, ' the distortion of the lattice would reduce the energy required for vacancy formation, and thus provide vacancies more readily to assist in the cavitation process. It was decided to study a range of alloys to find out whether increasing amounts of an alloying element would cause any progressive increase in, or modification of, the cavitation in copper. Nickel was chosen for this purpose, since it is soluble in copper throughout the whole range of alloys. A further advantage was its low vapor pressure, which enabled the preparation of the alloys in vacuum and the consequent reduction of their hydrogen content. It has been suggested that cavities may be nucleated by the migration of hydrogen atoms to the less regular atomic spacing at the boundary, and their combination to form molecules. The latter being too large to diffuse back into the lattice, form stable cavities into which vacancies could condense. PREPARATION OF ALLOYS All alloys, ranging from pure OFHC copper to 43.7 at. pct of nickel (carbonyl), were prepared in a vacuum furnace employing high-frequency induction heating. When a charge was melted, vigorous gas evolution occurred initially, after which the pressure was reduced to 10-4 mm Hg, using an oil-diffusion pump. After remaining molten for a further 1/2 to 1 hr to aid degassing, the melt was allowed to solidify in the crucible. In this way contamination by gases evolved from the surface of a separate mold was avoided. The list of alloys prepared is shown in Table I. The percentage of hydrogen present in the OFHC copper was reduced from 0.0054 at. pct to 0.0012 at. pct, as measured by a vacuum-fusion method. The alloys were cold-rolled to 0.03-in.-thick strip, and were homogenized in vacuum for 1 hr at 900°C after every 30 pct reduction. At a thickness of 0.05 in., the strip was held at 450°C for 24 hr under high vacuum (10-5 mm Hg) in an attempt to reduce the hydrogen content still further. Tensile specimens were prepared with a gage length of 1 in., and were finally annealed for 2 hr at 800°C to give an average grain diameter of 0.1 mm. TENSILE DEFORMATION The specimens were deformed in a tensile straining machine operated by a synchronous motor at a constant rate, equivalent to 1.7 pct per hr on a 1-in. gage length. The specimen and grips were contained in a vacuum jacket. A pressure of 10-2 mm Hg was maintained, which was sufficient to prevent surface tarnishing of a specimen held at 650°C for 24 hr. Tests were made between 20. and 650°C and the temperature was controlled to within ±3° over the gage length. The load was measured by the deflection of a cantilever spring. a) Mechanical Properties-The ductility curves shown in Fig. 1 fall into two groups. Figs. 1(a) and (b) for copper and the 5 pct nickel alloy, respectively, show a continuous fall in ductility with a steep fall between 200° and 400°C. Figs. l(c) to (f) show the same sudden loss of ductility between 200° and 400°C. With higher temperatures, however, there is a recovery in ductility values to a maxi-

Jan 1, 1959

By S. Jana, C. M. Wayman

The reverse transformation of bcc martensite to the fcc phase was studied in an Fe-33.95 wl pct Ni alloy by nzeans oj dilatometry, melallography, and electron microscopy. Upon "slozc" heating (-1°C per min) length cJmnge us temperature plots showed u gradual contracLion over the temperature range 200" to 280"C ,followed by a more abrupt contraction beginning a1 -280°C. Howet,ev, zchen the heating rate was increased -4°C per tnin, no gradual contraction was observed and only the abrupt contraction starting at -2BO"C was found. Thus on slower heating- the AS "temperature" for the subject alloy, unlike the MS temperature, is better defined as a range of temperatures. Both optical and transmissiorl electron microscope observations showed that some of the martensite plates exizibited a partial loss of transformation twins during reversal. The midvib region of the martensite plates disappeaved relatively early duirng the reversal. Metallographic observations slowed that the earliest detectable stage of the rezlerse tvansforrvration begins (axd Moues inulardly) at The Martensens i te - parent interface. At higher temperatirres, the. formation of martensitically reversed jcc plates within the bcc martensite plales was observed. It is concluded that the reverse transformation consists of a diffusion less process (martensitic); but this is ps-obably aided by a prior or simultaneous dijjusiorz-comltvolled process, at leasl in the case of slower heat-ing' experiments. ALTHOUGH numerous investigations have dealt with the parent-to-martensite ("forward") transformation (fcc — bcc) in Fe-Ni alloys, comparatively little is reported on the ("reverse7') martensite-to-parent transformation.'-4 Even though such reverse transformations have been studied in detail in some nonferrous systems, one of the difficulties of studying the reverse transformation in most ferrous mar-tensites is that the martensite decomposes by tempering during heating. However, carbonless Fe-Ni alloys do not exhibit this difficulty since the transformation in these alloys is completely reversible. The present investigation represents an attempt to shed more light on the nature and mechanism of the martensite-to-parent transformation. 1) EXPERIMENTAL PROCEDURE 1.1) Alloy Prepatation. Fe-Ni alloys of compositions near 34 wt pct Ni were prepared from zone-refined iron (99.994 wt pct Fe) and high-purity nickel (99.999 wt pct Ni) by induction melting in recrystallized alumina crucibles in an argon atmosphere, with prior vacuum evacuation to 10"3 mm Hg. The alloys were homogenized by induction stirring in the molten state for 5 min. After solidification, the alloys were further homogenized in evacuated quartz capsules for 96 hr at 1230°C. 1.2) Dilatometry. Slices of the ingot were hot-forged (750°C in air) into approximate rod form and these specimens were then hot-swaged (750°C in air) into long cylindrical rods 0.55 mm diam. From the rods, specimens about 1 in. long were cut. These were then vacuum-annealed for 24 hr at 1200°C, cooled to room temperature, and subsequently transformed to martensite in liquid nitrogen (whereby about 40 pct transformation was obtained). Dilatation measurements were made by observing length changes in a vacuum dilatometer with an externally mounted LVDT sensing element. 1. 3) Preparation of Electron Microscope Specimens. Slices of the ingots were cold-rolled (with intermediate vacuum anneals) to -0.020 in. Out of these rolled sheets, specimens (about 1 by 1 in.) were cut. These were then vacuum-annealed, transformed to martensite by cooling in liquid nitrogen, and subsequently heated from room temperature to various temperatures to effect either partial or complete reverse transformation. These specimens were then chemically polished to 0.002 in. in l:l HsOz (30 pct) and &PO4 (85 pct) solution, and thinned to electron transparency in an electrolyte consisting of 150 g CraOs, 750 ml glacial acetic acid, and 30 ml ~~0.~ Observations were made with a 100-kv Hitachi HU-11 electron microscope equipped with an HK-2A tilting device. 1.4) Optical Microscopy. Metallographic observations were made with a Leitz MM5 metallograph on the same 0.020-in. sheet specimens as were used for electron microscopy and on bulk specimens which were 0.2 in. or more on a side. The chemical thinning solution when cooled below 20°C also served as an etchant for this alloy. Observations of surface relief were made with a Zeiss interference microscope employing a Thallium light source of wavelength 0.54 p. Specimens for interference studies were prepared by two-stage polishing on Buehler vibromet polishers using 0.3 and 0.05 p alumina abrasives. 2) EXPERIMENTAL RESULTS 2.1) Comparison of the MS,AS, and Af Tempera-tures wTth Previous Re sults. The AS aLd Af tempera -tures of several Fe-Ni alloys were determined dila-tometrically. The MS temperatures of the same alloys were determined by continuously lowering the temperature using a mixture of isopentane and liquid nitrogen and observing the highest temperature at which a prepolished specimen showed surface upheavals. For the present the As temperature is defined as the temperature at which an abrupt decrease in length occurs in the dilatation plot. The Ms,As7 and A determinations in the present investigation and those of Kaufman

Jan 1, 1968

By H. Herman, M. E. Fine

Kinetics of reversion and reformation of GP I were studied resistometrically in Al-1.7 at. pct Cu. The reversion process is over in roughly 1/2 minute at 205 "C irrespective of the amount of primary aging. After reversion the occurrence of an incubation time before reaging begins has been substantiated. The reaging kinetics is drastically accelerated by plastic deformation to the specimen. An incubation time is observed only if the specimen is aged before reversion. The incubation time and the effect of plastic deformation indicate that nucleation of GP I is heterogeneous. Simple clusters of copper atoms apparently do not act as nuclei for GP I. AFTER quenching aluminum-rich copper from the solid solution range, Guinier-Preston zones of the first kind, GP I, form very rapidly at room temperature. The rate, largely controlled by the concentration of vacancies, is initially most rapid1 (that is, at the time of the first measurement: 1/2 min) and decreases with time. The nucleation is thought to be athermal. If after aging for several days the GP I is dissolved by reversion at 205°C, according to measurement of Young's modulus an incubation period is observed before GP I begins to form on subsequent aging.2 Yet if the reversion is carried out immediately after quenching, both resistivity3 and modulus changes2 show no incubation effect. The zones which form after reversion have the same structure as those which form after the quench.4 Because of entropy considerations and also the short diffusion time, the solid solution after reversion, 2 min at 205°C, is probably more highly clustered than at the original solution treating temperature, 520" to 550°C. It appears most reasonable to associate with nucleation the incubation time observed on reaging after reversion. A simple cluster of copper atoms, many of which are presumed to be present after reversion, is then not a sufficient nucleus for GP I; a GP I nucleus must contain something in addition to a cluster of copper atoms. The purpose of the present note is to give some additional experimental information concerning the incubation time and rates of reaging after reversion. The existence of the incubation time has been verified by measurement of another property, the electrical resistivity. Acceleration of reaging after reversion by plastic deformation has also been investigated. In acl.dition, the kinetics of the reversion process itself was studied. EXPERIMENTAL Electrical resistance was measured by the poten-tiometric four probe method. The 1.7 at. pct Cu alloy was furnished by the Aluminum Co. of America in the form of 1/2 in. rod. The major impurities reported by Alcoa were Fe (0.002 wt pct), Si (0.003 wt pct), and Mg (0.001 wt pct). Specimens for measuremenl of resistance were prepared by rolling to 0.010 in., cutting 2 by 0.2 in. pieces, rolling the middle pclrtions of these to 0.005 in., and splitting the 0.010 in. sections up to the reduced central section to form current and potential leads. Aluminum extension wires insulated with ceramic tubes were spot welded to the leads. The specimen was supported by the lead wires. The whole specimen assembly was annealed at 500" C in an air furnace for more than 12 hr and then aged at room temperature. This was done to assure quick and complete resolution during subsequent solution treatments. These were carried out in Houghton's "430 Temper Salt" at 520'C for 1 hr. Unless otherwise specified, quenching was accomplished by quickly transferring the specimen from a salt pot to 25°C water. Aging was carried out in a 3 liter dewar of distilled water, rotated and stirred. The temperature was controlled to +0.01°C with a thermomercurial regulator in conjunction with a transistorized relay

Jan 1, 1962

By O. E. Kiessling

THE Committee-on Production Control, at its meeting held during the last annual session in February, 1930, evidenced great interest in problems of stabilization affecting all mineral industries. . No immediate program of activity for the Committee as a- unit was decided on, however,, and efforts during the past pear have consisted lirgely of further stressing the economic aspects of mineral production and of the action by committee members, :.serving in their individual capacities, in sponsoring constructive changes, in specific, industries. Of greatest interest to the general subject of production control in 1930 was the very definite advance toward better coordination of demand and supply in the petroleum industry. Furthermore, since opinion both within and without the oil industry now favors a constructive program, and with a gradual change in legal precedents, it seems not unreasonable to expect greater progress in the near future.

Jan 1, 1931

INTRODUCTION The first installation of large, commercial, high gradient-high field cannister and matrix magnetic separators for removal of impurities from kaolin was made in 1973 (1). Since then the technology and equipment have been widely adopted for clay processing with about 12 units in commercial use. These new separators have filled a need, caught the imagination of many and become a technology worth fighting for. A fight has occurred, and a resolution on royalties for kaolin processing, at least, has been achieved. LIMITATIONS TO APPLICATIONS OF MAGNETIC SEPARATORS Other than the use of these magnets on kaolin clay, no other application has yet achieved widespread adoption. Dr. Iannicelli blames inertia, and1 would agree that it is a factor. There are other reasons too, and if they are examined, they may isolate problems that R&D can significantly assist in solving. I'd like to break the problems into two areas. Machine limitations - the mineral properties are there but performance is insufficient or uneconomic. Separation limitations - the mineral properties aren’t there, but the magnetic separation would perform well if the properties were there (size is right; concentration is right, etc).

Jan 1, 1979

By Paul L. Cloke, S. R. Titley

Paul L. Cloke (Assistant Professor, Dept. of Geology and Mineralogy, The University of Michigan, Ann Arbor, Mich.) - On examination of the paper by S. R. Titley it appears that several errors have been made, many of them of a fundamental nature. It is the intent of this discussion to point out these mistakes, and, insofar as possible with the data at hand, to correct them. EXPERIMENTAL WORK Ferrimolybdite-Limonite-Water: The results of the experiments described are very difficult to interpret; nevertheless, a correct interpretation is essential as is pointed out subsequently. The difficulties become apparent when reasons are sought for the continuing change of pH after conversion of ferrimolybdite to ferric hydroxide and for the change of pH when -stirring is stopped after a steady value has been reached. In seeking an explanation of this experiment it seemed to this writer that the (temporarily) steady pH values might be due to kinetic rather than equilibrium effects. In this view the steady pH on stirring might be explained as a balance of several reactions proceeding simultaneously. The first of these would be the slow solution of ferrimolybdite,

Jan 1, 1964

By C. F. Jr. Park

HOG MOUNTAIN is in the north central part of Tallapoosa County, Alabama, about 13 miles northeast from Alexander City. The Hog Mountain Mining and Milling Co. controls 1658 acres of land and is the only company operating in the district. The principal mine workings are in sections 10 and 15, T.24N., R.22E. The region has been visited by geologists many times, has been briefly described in several papers,1 and mentioned in many others. No detailed map of the mine or vicinity has been published. The field work for this report was started in March, 1934, as part of the Public Works reemployment program. About a month and a half was spent mapping both the surface and underground geology. The mine owners and operators have cooperated in every way possible to facilitate the work. N. 0. Johnson, the mine engineer, E. W. Ells-worth, J. E. McCoy and J. G. Englebert have acted as assistants for part of the work. The University of Alabama and the State Geologist's office have aided materially by permitting free use of their libraries and laboratory equipment.

Jan 1, 1935

Albert R. LEdoux, New York, N. Y.—I can add a little to the information which has been given, by saying that it has been our business for some years, among other things, to inspect outgoing copper from some of the works here in the East, and to find out why there are variations not only in the conductivity of the wire-bars, but also in the character of the cathode-copper shipped; and we have found two things: These impurities which have been mentioned are largely upon the surface of the cathode. Samples taken of the inside, even of the nodules or " berries " which grow on the outside of the cathode, show that they do not contain more impurities than the denser material in the interior. In other words, it is a superficial deposit or contamination. There is still another reason for impurity in some of the copper which finds its- way to the manufacturers, namely, carelessness in the handling of molds or in casting. We have found copper which was comparatively pure, as far as the copper itself was concerned, but contained, mechanically intruded in the interior of the ingots,

Jan 1, 1913

By E. H. Sellards

ON Oct. 9, 1929, a sink formed in the Sour Lake salt dome oil field in Texas, and on Oct. 12 a second smaller sink formed at the north margin of the first. The purpose of this paper is to give such observations as it has been possible to make on the earth movement incident to this subsidence. Sour Lake salt dome is typical of the salt domes of the Gulf Coastal Plain of Texas. Structurally the dome is a plug of salt which rises to within 900 ft. or less of the surface. Above the salt is a cap rock consisting of anhydrite with more or less calcium carbonate. The salt plug, as contoured on the cap rock, is circular in outline with, however, some appreciable irregularities. Overlying the cap rock are relatively uncompacted sediments consisting of sand, clay and gumbo.. At the crest of the dome these deposits are no more than 700 or 800 ft. thick. However, the sides of the dome are steep, and the sediments thicken rapidly away from the crest. The sink formed about 1500 ft. northeast of the crest of the dome where the sediments overlying the cap rock are from 1000 to 1200 ft. thick. The cavity permitting the subsidence was quite certainly either in the cap rock or in the salt below the cap rock, so that the sink was formed by the caving of as much as 1000 or 1200 ft. of earth.

Jan 1, 1930

By P. E. Rider, K. A. Gschneidner, O. D. McMasters

The solid solubilities for thirteen rare-earth metals in gold were determined by using the X-ray parametric method. Solubilities ranged from 0.1 at. pct for lanthanum in gold up to 8.8 at. pct for scandium in gold. The solubilities from lanthanum to gadolinium were very small and essentially constant, but a sharp increase occurred from gadolinium to scandium. The large solubilities for the heavy rare-earth metals were not expected because of the large size and electrochemical differences between rare-earth atoms and the gold atom. Contributions from first- and second-order elasticity theory plus an electronic contribution were found to reasonably account for a more favorable size factor. Electron transfer from the rare-earth metal to the gold Is thought to occur such that the resultant rare-earth and gold electronegativities are favorable for solid-solution formation. It was also found that this mutual adjustment of size and electronegutivity does not occur if the pure-metal size factors are greater than a critical value of 25 pet. The eutectic temperatures for ten systems were determined and these remained fairly constant at approximately 809 "C for the lighter lanthanide metal-gold systems until the Er-Au system was reached, at which Point the eutectic temperature successively increased reaching a maximum of 1040°C in the Sc-Au system. This rise was correlated to the size factor becoming more favorable for solid-solution formation at erbium. The valence state of ytterbium was found to change from two in the pure metal to three when ytterbium is dissolved in the gold matrix. RECENT results1 reported concerning the solubility of holmium in copper, silver, and gold, showed that the solubility of holmium in gold was quite large, 4.0 at. pct, compared with 1.6 in silver and 0.02 in copper. The small solubilities of holmium in silver and copper are quite reasonable in view of the large size difference (22.2 and 38.2 pct, respectively), large electronegativity difference (0.59 for both systems), and possible unfavorable valency factor (assuming one for silver and copper and three for holmium). The large solubility in gold, however, is unexpected because these same factors are also unfavorable for holmium and gold (22.5 pct size difference and 0.69 electronegativity difference), and because the light rare-earth metals, lanthanum, cerium, and praseodymium, have negligible solid solubilities in gold.2 In view of this unexpected behavior, it was felt that a study of the solid solubilities of most of the rare-earth metals in gold would be desirable to better understand the factors involved in the formation of solid solutions. Of the rare-earth metals added to gold in this study, only ytterbium is divalent in the pure metallic state (the other rare-earth metals are all trivalent) and many of its physical properties (such as the metallic radius, electronegativity, and so forth) are much different from those of the normal trivalent rare-earth metals.' The properties of ytterbium are such that one would expect solid-solution formation to be less favorable for ytterbium in gold than for any of the normal trivalent rare-earth metals. But chemically ytterbium is known to possess a stable trivalent state, and it is quite possible that ytterbium may alloy as a trivalent metal under certain conditions rather than as a divalent metal. Because of the dual valency nature and because so little is known about the alloying behavior of ytterbium, the gold-rich ytterbium-gold alloys are of special interest. EXPERIMENTAL PROCEDURE Materials. The gold used in this investigation had a purity of 99.99 pct with respect to nongaseous impurities. In general the rare-earth metals were prepared by reduction of the corresponding fluoride by calcium metal.3 The impurity contents of the metals used in this study are given in Table I. Preparation of Alloys. Two- or 3-g alloy samples were prepared by arc melting. The samples, with the exception of some of the Er-Au alloys, had weight losses of 0.5 pct or less. All alloy concentrations noted in this paper are nominal compositions. After arc melting, the alloys were wrapped in tantalum foil, sealed off in quartz tubing under a partial atmosphere of argon, homogenized for approximately 200 hr at 780°C, and then quenched in cold water. X-Ray Methods. The X-ray parametric method was used in determining the solubility of the rare-earth metals in gold. filings were sealed in small tantalum tubes by welding under a helium atmosphere. The tantalum tubes were then sealed in quartz tubing under a partial argon atmosphere, and annealed for times ranging from 1/2 to 3 hr (the length of time was inversely proportional to the an-

Jan 1, 1965

By C. H. Mathewson, Robert Maddin, W. R. Hibbard

A SATISFACTORY mathematical relationship between shear, elongation and change of orientation in the axial straining of a single crystalline rod or wire may be based on a simple model in which blocks, representing glide lamellae, glide over one another and rotate so as to maintain the original fixed position of the axis as the wire elongates.1 Obviously such a model gives no information concerning strain-hardening or the atomic adjustments at the sliding surfaces and their influence on the internal structure of the blocks. Moreover such an operation could be conducted with rigid blocks only by using self-aligning grips or a flexible attachment which would permit the adjacent blocks to freely assume their changing orientations. There are many unsolved problems (see Andrade2) concerning the manner in which nature departs from the simple model in permitting the essentials of slip, rotation and elongation to occur along with strain-hardening and the appearance of glide lamellae of various dimensions and special characteristics, not fully appreciated at the present time. This paper describes part of an extensive investigation on the development and characteristics of glide ellipses in single crystalline alpha brass rods and is especially concerned with the observation of cross-slip in crystals oriented wholly within the range of slip on a single system according to the generalizations first presented by Taylor and Elam in 1923.3 EXPERIMENTAL PROCEDURE Half inch rods of alpha brass (nominally 70 pct Cu, 30 pct Zn) * were converted into single crystals by melting and gradual solidification in a graphite mold according to the Bridgman method.' In order to remove any coring, the crystals were homogenized at 800°C for 16 hr and tested by etching with a 50 pct nitric acid solution. The back-reflection Laue technique as described by Greninger5 was used for determining the orientations of the crystals. Standard stereographic operations were employed to locate the specimen axis in a triangle of the Taylor and Elam3 projection so that the slip plane and direction could be predicted. The lineage structure reported by Buerger6 was present in the crystals used in this investigation. However, only crystals were used in which the internal differences in orientation did not exceed two degrees. Very little is known concerning the effect of the presence of a lineage structure on the detailed mechanism of plastic deformation.

Jan 1, 1948

By A. E. Blakeslee

Morphological and electrical properties of GaAs epitaxial layers are influenced not only by changes in the nominal substrate orientation but also by small amounts of misorientation from the exact crystal planes. Deviations up to 5 deg from {11IA}, {11IB}, and (100) planes were investigated. Growth rates increase progressively with angle, approximately I u per hr per deg. Size and density of growth pyramids fall off with increasing angle, but other effects that are deleterious to the surface may occur which are heightened by increased misorientation. Carrier concentration decreases and electron mobility consequently increases as the angular offset increases, except in the case of strong compensation, where the mobility trend is reversed. It has long been known that changes in the crystallo-graphic orientation of the substrate may cause pronounced effects on the morphological properties of vapor grown semiconductor films. Reports of orienta-tion-dependent growth rates and surface characteristics are as old as the literature on epitaxy itself. shawl has recently published a comprehensive study of the dependence of growth rate on substrate temperature and orientation in epitaxial GaAs. It is also well-known that misorienting the substrate surface a few degrees away from the nominal low-index crystal-lographic plane often produces a much smoother epitaxial surface. This was reported by Tung2 for silicon, Reisman and Berkenblit3 for germanium, and by Kontrimas and Blakeslee4 for GaAs, and use is commonly made of this fact in the semiconductor industry to help guarantee smooth vapor deposits. The effects of substrate orientation on the carrier concentration and mobility of vapor grown GaAs were first documented by williams5 in 1964 and have been observed by several other authors since then,6,7 but no one has yet reported a careful study of how small changes influence these properties. We have made such a study and have found that sizable differences in growth rate, morphology, carrier concentration, and mobility can indeed be observed for epitaxial films grown on substrates that are oriented by progressive small increments away from the exact crystal plane. EXPERIMENTAL Early in the investigation an arsine synthesis system of conventional design8 was employed to produce growths on {111A}-oriented GaAs substrate crystals. In that early work, pronounced effects on carrier concentration and electron mobility were observed as a function of slight misorientation from this low index plane. That observation led to the more careful study that is reported here. An AsC13 system, differing in major aspect from those commonly in use today9 only in that the reactor is vertical rather than horizontal, was used for the detailed study. The gallium source was at 900°C and the substrates were at 750°C. The flow rate of pal-ladium-diffused H2 through the AsCl3 bubbler was 200 cu cm per min, and the flow rate of bypass H2 was also 200 cu cm per min. The substrates consisted of chro-mium-doped semiinsulating GaAs to facilitate elec-trical evaluation of the overgrowth by means of Hall and conductivity measurements on conventional eight-legged Hall bridges. They were misoriented by 0 to 5 deg from the {111A}, {111B}, and (100) planes, toward the (100) from the {111A} and {111B} and randomly toward the <111A> or <111B> from the {loo). The crystals were oriented for sawing by the Laue back-re-flection technique, which is good only to about ±1/2 deg; but after polishing or sometimes after epitaxial growth the wafers were checked by a diffractometer technique which is accurate to about * 0.1 deg. After lapping, the wafers were polished with NaOCl after the technique of Reisman and Rohr,10 and just before use they were cleaned in NaOC1, thoroughly rinsed with de-ionized water, and blown dry with nitrogen. Each run employed four wafers, each misoriented by differing amounts from one of the three major faces, and at least two runs were made for each orientation. The runs were continued long enough to provide at least a 15-µ or thicker layer. SURFACE MORPHOLOGY The appearance of all the films that were grown in a given run always changed from wafer to wafer as a function of increasing misorientation, but not always in the same regular fashion. At least three different trends were observed. These are more easily seen than described, and reference to the series of photo-

Jan 1, 1970

By Ernest Klepetko

A notable amount of fossil resin exists in many of the bituminous coal beds of Utah, The upper part of these show a marked concentration of resin, which occurs primarily in the fracture seams. In general, these seams are less than 1/8 in. thick, but it is not uncommon to find coal with areas as thick as 3/8 in. The resin is of the hard kauri variety, with coloration varying from deep blood red to lemon yellow and almost colorless. There is also an almost black variety, which is not readily soluble in the same solvents as the lighter colored resins. These resins are valuable for many industrial purposes. When refined, they are suitable for uses similar to those for which lac resins are usually employed. They are particularly desirable for preparing dielectric varnishes. They are also desirable in preparing printing inks, waterproofing agents, special synthetic rubbers and rubber cements, They are especially suitable as an admixture in synthetic rubbers and cements, as they supply the essential tackiness the synthetics lack. The following chemical trade characteristics&apos; have been found by Inter-Chemical Co. research chemists in the refined resins: Specific gravity (melted)....... I. 03 -1.06 Acid number.................. 6-8 Softening point, mercury method 160°-165°C Iodine valus (Wijs)............ 140-150 Refractive index............... 1.544 Color (Hellige, 25 pct toluol)... 14 Molecular weight, average...... 732 purity, 99 + pct pure hydrocarbon "Unaffected by alkalies and resistant to one hour fusion with solid potassium hydroxide. Completely soluble in aliphatic and aromatic hydrocarbons. Insoluble in alcohols, ethyl acetate and other commonly used alcohols and esters. Compatible with natural and synthetic rubbers, chlorinated and cyclized rubbers, waxes, vegetable oils, mineral oils, rosin, ester gum, phenolic and modified phenolic resins and other natural and synthetic resins of like solvent solubility."* The recovery and refining of these fossil resins has been the subject of much research work and has intrigued many investigators. Broadly speaking, the problem involves separation of the resin from the coal into a very high-grade concentrate, and subsequent treatment of this concentrate to produce an acceptable refined resin for its various usages. Obviously it is also desirable to recover the residua] coal without excessive size degradation. The late W. D. Green, concentration engineer for Combined Metals Reduction CO., obtained U. S. Patent No. 1773997 for the recovery of resin from coal through

Jan 1, 1949

By S. S. Nosseir

INTRODUCTION General Quebec Cartier Mining Co. (QCM) , Canadian subsidiary of U . S. Steel Corporation, operates two iron ore concentrators at the North Shore of Quebec, Canada. In its own operation at Mount-Wright, over 45 million tons per year of crude ore are ground, fully autogenous in six 32&apos; x 11-1/2 Dominion Engineering mills. At Fire Lake/Lac Jeannine operation, property of Sidbec Normines Incorporated (SNI), over 11 million tons per year of crude ore are now ground, fully autogenous, in twelve 18&apos; x 5&apos; Hardinge mills. The Lac Jeannine concentrator was originally constructed by Q.C.M. in 1960 and. was since operated, in beneficiating the Lac Jeannine ore deposit until fully depleted in 1977, at an annual capacity of 18 million tons of crude per year. In 1976, the new company, Sidbec Normines, was incorporated by Sidbec Corporation, British Steel Corporation and Quebec Cartier Mining Co., in proportional holding of approximately 51 to 41 to 8 percent respectively. Since the acquisition of the Fire Lake ore deposit and Jeannine concentrator by the new company, QCM has continued managing the mine and concentrator operaions for S idbec Normines Inc . Flow-Sheet Design Jeannine concentrator comprises twelve identical mill lines grinding the ROM from 8" top size to 14 mesh nominal size range. Driven by 600 H.P. motor at 13.4 RPM corresponding to 73% critical speed, each mill is operated in a closed circuit with two 5&apos; x 12&apos; vibrating screens dressed with 2.5 x 25 mm slot opening cloth. The ground product or screen undersize at an average grade of 33.4% Fe is beneficiated by gravity separation to produce 66.5% Fe concentrate grade at 42.7% weight recovery. At the rougher stage, each mill line con-tains 128 Humphrey 13- 1/2" pitch spirals which produce a final tailing, middling and concentrate products. The rougher concentrate - so produced - is classified by 64 Humphrey pocket sizers into an underflow, which is a final concentrate product and an overflow which is further upgraded by 64 cleaner spirals. The cleaner concentrate together with the pocket sizer &apos;s underflow are dewatered on a 13&apos;[6] horizontal filter. The rougher middling together with the cleaner tailing are recycled in a closed circuit with the spirals. The rougher tailing after dewatering by hydrocyclones is disposed of by a

Jan 1, 1982

By N. A. Gjostein

The self-diffusion coefficient D, for a surface near the (100) plane in copper was determined by means of the Mullins theory of thermal grooving, and was found to obey the Arrhenius relationship, and Do = 6.5 x 10&apos; sq cm per sec. Suppression of surface diffusion by chemisorbed impurities encounters difliculties as a satisfactory explanation for the large Q, and Do. Instead, a model is presented which indicates that Q,, as determined by a mass-transport technique, may involve both the energy needed to form an adsorbed atom from a ledge in the surface as well as that for the movement of the adsorbed atom.; LITERATURE reviews1-3 indicate that the mechanism of self-diffusion on metal surfaces is not clearly understood. The lack of experimental data on the temperature variation of the surface self-diffusion coefficient DJ has contributed greatly to this situation. Radioactive tracer techniques4-rn have been used to measure Ds, but for many years only Nicker-son and Parker8 had determined (for polycrystalline silver) an activation energy B, and a frequency factor Do for the surface self-diffusion process. Even in this case, a mechanism could not be clearly inferred because it was suspeted7 that a contribution from volume diffusion was not taken into account by the investigators. Some later work by Li and parkere on polycrystalline gold, in which they obtained essentially the same results as for silver and in which volume diffusion could be accounted for, seems to invalidate this criticism. In 1957, Mullins10&apos;11 developed the theory for the thermal grooving process. This advance has opened a new and promising technique for measuring the surface self-diffusion coefficient Ds. Recognizing that a thermal groove may form by several different mass transport processes, Mullins first consideredlo the cases where a) the groove forms by evaporation and condensation or b) by diffusion along the groove surface, in either case, in a system where a metal surface is in contact with only its dilute vapor phase. In a later paper," he extended the treatment to cases where the groove forms by volume diffusion into c) the solid phase or d) by mass transport through a passive gaseous phase at 1 atm pressure. The time dependence of the groove dimensions and the shape of the groove profiles predicted by Mullins&apos; treat-

Jan 1, 1962