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By Louise Barton Freeman, Coleman D. Hunter

The total production of oil in Kentucky during the year 1943 reached 7,010,776 bbl., which is more than at any time since 1930. Of this total, 5,287,659 bbl. was produced from the counties west of the Cincinnati arch, 692,359 bbl. from the 18 new pools opened during the year, and 3,260,765 from the Smith Mills pool, which was discovered in August of 1942. This is an important increase in western Kentucky in spite of the low price of crude, and demonstrates effectively the desire of the industry to cooperate in meeting the increased demands made by the war. Western Kentucky Two deep tests were drilled in the Kentucky portion of the Mississippi Embayment this year. Both were drilled to test the St. Peter. One well, drilled in Marshall County by the Adams Oil and Gas Co., did not encounter any St. Peter sandstone but drilled 650 ft. of formation below the position of the St. Peter and above the true Knox dolomite. The other well, in Ballard County, was reported to have tested the St. Peter and to have been temporarily abandoned at 3069 ft. At this depth the well probably was stopped in about the same formation as the Marshall County well. No accurate information is available on the Ballard County well. Several new producing areas were added to the list of fields in the western Kentucky coal basin, in Daviess, Henderson, McLean, Ohio, Union and Webster Counties. The Smith Mills pool was enlarged and production was found in the McClosky (Ste. Genevieve) in addition to the Cypress sandstone from which much of the earlier production had been obtained. There was some interest during the year in testing the Devonian and Silurian formations in the area south and east of the western Kentucky coal basin. In the fall of 1943, a 15 to 20-bbl. well was drilled in Allen County and two more wells are now being drilled. The production was obtained from within a few feet of the base of the Chattanooga black shale, probably in the upper Silurian. One well in Simpson County was drilled completely through the Silurian section before it was abandoned. Several wells were drilled in Logan, Todd and Christian Counties to test the Devonian where it is thinned by removal of the upper formations before deposition of the Chattanooga shale. None of these wells was successful but several other locations are now being tested. The Silurian thins in like manner on the eastern flank of the coal basin as the crest of the Cincinnati arch is approached, and it is along this thinning edge that such fields as the LeGrande, Logsdon Valley, Magnolia, Bowling Green and the Barren County pools were developed. A number of wells were drilled around these old pools in an effort to extend them, some of which were successful. The wells listed this year in Larue, Hardin, Barren, Hart and Warren Counties were drilled in the search for other such fields.

Jan 1, 1944

By Fred D. Gustafson

With the postwar emergency for new housing and for new industrial buildings, much research has been done on lightweight aggregates for use in concrete and plaster. The trend toward lighter weight aggregates to relieve the dead load on the higher, steel framework buildings started toward the end of the last century. Progressively the requirements became more stringent, crushed bank slag, weighing 80 lb per cu ft as compared to 100 lb for crushed rock, was supplemented in some sections by foamed slags and expanded shales weighing from 40 to 60 lb per cu ft. In other sections cinders were used weighing from 40 to 50 lb, including sand. Sections favored with more recent vulcanism turned to pumice weighing from 30 to 60 lb, whereas other localities made use of diatomite, from 28 to 40 lb. Exfoliated vermiculite weighing from only 6 to 10 lb per cu ft came into use. As the search for lighter weights in aggregates continued so did the search for other desirable properties such as nailability, ease of cutting or channeling, and good insulation to both sound and heat. This search eventually led to a widespread interest in the expansion of perlite, or similar volcanic glasses, with the result that in 1946, the Office of the Housing Expediter' listed eleven firms reporting the operation of processing plants either on pilot or commercial scale producing aggregates weighing from 2 to 16 lb per cu ft. Geology Perlite is one of the large family of rocks originating from a granitic or acidic magma and generally has a "rhyolitic composition with a marked perlitic structure."² The name "perlite" is a derivation from "perlstein" originally given "to certain glassy rocks (hyaloliparites, hyalo-rhyolites) with numerous concentric cracks, from the fancied resemblance of broken out fragments to pearls."3 The cause of the perlitic texture is somewhat controversial. Johannsen attributes the texture to strain set up in the glass by cooling and describes the finding of peculiar, glassy balls, called marekanite, more or less rounded and showing concave indentations, which may be left when perlite is broken. Frank Rutley, on the other hand, in 1881, while working on vitreous rocks from Montana, observed that there was incipient or partially started crystallization with segregation of water toward the un-crystallized portion in all specimens of perlite examined. Further he observed evidence of strain around focii of crystallization to which he ascribed the development of the spherical cracking which gives the rock its perlitic texture.4 Widespread over the western and southwestern United States where Tertiary vulcanism is exposed, perlite commonly is associated with andesitic, basaltic, and rhyolitic lavas with inter-bedded tuffs and ash of Eocene age although some deposits are associated with rocks assigned to the Pliocene age.5, 6 n nearly all cases the perlite overlies water laid tuff beds or agglomerates or breccias of explosive nature, an outstanding exception being the occurrence of perlite as the chilled selvage of andesite intrusions.7'8 Available chemical analyses of per-lites from the western and southwestern United States indicate that they are varieties of leucorhyolites rather than of normal rhyolites, leucorhyolites having less than 5 pct of dark minerals, normal rhyolites having more than 5 pct. This conforms with Johannsen's observation that leucorhyolites are the prevailing kind in North America.9 Tables 1 and 2 give

Jan 1, 1950

By D. R. Parrish, W. E. Lamoreaux, W. W. Owens

Several methods are now being used by the industry for determining the gas-oil flow characteristics of reservoir rock samples. Most of the laboratory experirnerltal rlzethods can be classified either as steady-state, unsteady-state, or Hassler-type tests. Although the validity of the results obtained by any specific method is not questiorzed, in general, the complexity of these methods leaves much to be desired. This investigation dealt primarily with the development of a simplified unsteady-state (gas drive) laboratory test method for measuring kg/ko re1ationships of small core samples. A procedure for selecting uniform and representative sandstone rock samples was developetl since it was observed that the reliability of the test resu1ts was dependent upon having a sample which was uniform in porosity and permeability. The importance of factors known to influence the results of this type test, such as oil viscosity, gas expansion, and pressure differential were eva/uated. The method of calculating the test results was found to give valid data over a wide range of gas expansion. The limits of pressure differential and oil viscosity which would insure reliable results were defined. In cornparisorz with other presently used testing methods, the gar drive method requires considerably less apparatus, is less time consuming, and is more readily adaptable to a routine type core test. INTRODUCTION The detcrmination of the gas-oil flow characteristics of reservoir rocks has been given concentrated study by the oil industry for the past decade. Both analytical and experimental methods have been considered. The analytical methods have generally relied on a simplified characterization of porous materials in order that the fundamental laws of fluid flow and capillarity could be utilized. More direct experimental methods have been proposed by numerous production research laboratories with the primary goal being a simple and inexpensive, yet reliable method for measuring the gas-oil flow characteristics of reservoir rock samples. The experimental methods which have been reported in the literature generally can be grouped into one of the following classifications: 1. Steady state1,2,3,4 in which a fixed ratio of flowing fluids is forced through the test sample until equilibrium conditions of saturation and pressure gradient are established. 2. Hassler or stationary liquid method5,6,7 in which a uniform liquid saturation is attained, usually through capillary desaturation, then gas or oil is flowed through the sample at a pressure drop insufficient to disturb the pre-established saturation. :. Non-steady state method1,8,9,10 In which only the gas phase is injected into the sample, causing displacement of the oil phase and resulting in a system of continually changing average saturation and saturation gradient. The steady-state and Hassler methods have been most popular because, no doubt, of the simplicity of the actual relative permeability calculations. The problems involved in these methods were limited to apparatus design and measurement techniques. In the steady-state method, for instance, a constant flowing fluid ratio is established which, at equilibrium, results in an essentially uniform saturation over the entire length of the test sample. Therefore, the basic flow characteristics could be obtained by correlating the average saturation of the test sample with the kg/ko determined at various flowing gas-oil ratios.

Jan 1, 1957

By A. B. Parsons

DOWN in Washington an army of individuals constituting the government of a so-called "'democratic" nation is trying to manage the conduct, in its rnultifold phases, of the greatest war in history for the country that is potentially, at least, the strongest in the world and on which, consequently, the major responsibility rests. The enterprise is one of unprecedented magnitude and complexity. That individuals and groups have made and are making serious blunders, both as to the establishment and execution of policy, is to be expected.

Jan 1, 1942

By Y. L. Yao

A scale based on existing data for the mutual solid solubilities of metals in binary systems has been compiled. This scale is useful for estimating the relative magnitude of two solubilities, provided that these two metals do not form a continuous series of solid solutions. In his classic work on the theory of metallic solid solutions, Hume-Rothery proposed that, other things being equal, a metal of lower valency should be regarded as more likely to dissolve one of higher valency than vice versa. He called this the "relative valency effect". Later he found that the application of this general principle was limited to the three univalent metals: copper, silver, and gold. In dealing with alloys of these metals with metals of higher valency, Hume-Rothery stated, it is usually found that the solid solution of the univalent metal is of the greater extent.&apos; The question of whether there is a systematic trend in comparing the relative magnitude of mutual solubilities, if valency is not considered a criterion, naturally arises. The present paper proposes a "mutual solid solubility" scale on an empirical basis. The order of its arrangement is determined by the relative magnitude of mutual solid solubilities. Some applications of and inferences from this scale are given. ORIGIN AND SCOPE OF THE SCALE An extensive survey of over 400 binary phase diagrams shows that, with certain exceptions and within certain limitations, metals can be arranged in the following order: Na Zn Cd Ga Bi Ge Sb As Hg Sn Si Mg Li Ba In Tl Pb Al Ca Be Mn Cr Re W Mo Cu V Ta Fe Ru Cb Co Ti Hf Ni Os Zr Ir Pt Au U Rh Ce Pd Ag Th so that a metal higher on the scale tends to have a higher solubility in a metal lower on the scale than vice versa. some experimental solubility data are given in Table I. These data, unless otherwise specified, are taken from Hansen and Anderko.6 Throughout this paper, the term "solubility of A in B" is taken to mean the maximum solid solubility of A in B in atomic percent, while the maximum solid solubility of B in A in atomic percent is called "reciprocal solubility". The exceptions found in the above-mentioned survey are: Al-Ag system, 20.34 at. pct Al in Ag, 23.8 Ag in Al; Mg-Pb system, 5.9 Mg in Pb, 7.75 Pb in Mg; As-Sn system, vanishingly small amount of As in Sn, a large As primary solid solution; Cd-Hg system, Cd in Hg <Hg in Cd; Mg-T1 system, 5(?) Mg in ßT1, 15.4 T1 in Mg; W-Ti system, -21 W in ßTi, -25 Ti in W; Zr-Ag system, probably small amount of Zr in Ag, 20 Ag in ßZr.7 Considering the large number of examples, the exceptions are few. It is remarkable that metals may be so arranged without considering other factors such as size, crystal structure, electronic structure, and so forth. A limitation to the use of the scale is the fact that it cannot be tested for two metals forming a continuous series of solid solutions. It is interesting to point out that when the continuous solid solutions have a miscibility gap the critical composition is

Jan 1, 1961

By A. T. Churchman

The deformation modes of rhenium have been identified as those typical of the hexagonal metals, titanium, zirconium, and beryllium whose c/a ratios, in common with rhenium, are less than ideal for close packing. Slip is observed on (1010), (1011), and (0001) planes and twinning on (1121), (1122), and (1012) planes. The very high rate of work hardening is believed to be associated with intersecting partial dislocations on two (1010) systems which can combine to form sessile barriers. If the stacking fault energy is low, as postulated by Seeger, these barriers should be strong and not easily bypassed by cross slipping. Such an explanation could also account for the very small temperature dependence of the yield stress which was observed. RHENIUM is interesting scientifically as a member of the group of high melting point hexagonal metals: titanium, beryllium, and zirconium with a c/a ratio less than that for ideal close packing. Unlike them, however, it work hardens at a very high rate. This rate is greater and continues to a much higher degree of deformation than for nickel, normally considered to have a high rate of work hardening. This paper presents experimental observations on the modes of deformation of rhenium and, by comparison with other hexagonal metals, some speculation on the cause of the high work hardening. MATERIALS Johnson, Matthey rhenium powder of both 99.9 pct and 99.5 pct purity, see Table I, was compacted at 10 tons per sq in., part sintered at 1350°C in vacuo, and finally arc melted in a "gettered" argon atmosphere arc furnace to produce small buttons. Little difference was observed in the as-cast hardness or working down behavior of the two purities suggesting that either silicon and potassium do not have a significant effect on the working properties of rhenium or they were lost during arc melting. SPECIMEN PREPARATION The cast structure was broken up by cold-rolling with inter-stage annealing at 1600o or 1800°C in a vacuum high-frequency furnace using a tungsten susceptor. Strip for tensile testing was taken from two thicknesses of material 0.011 and 0.064 in. The former with intermediate anneals at 1800°C had a grain size of 900 grains per sq mm, while the latter with inter-stage annealing at 1600°C had a grain size of 3600 grains per sq mm. A coarse grain size was obtained by secondary recrystallization in a half button cold-worked by 30 pct reduction. Annealing times of from half an hour to several hours at 2200° to 2600°C in a "gettered" argon atmosphere arc furnace1 resulted in grains of up to 2 mm diam.

Jan 1, 1961

By W. A. Stickney, J. W. Town

Tests demonstrated that aqueous solutions of sodiu~n sulfide would dissolve over 95 pct of the cinnabal- in 5 pct Hg flrotation concentrates and 60 to 90 pct of the cinnabav in low-grade ol-es. Double-leach tests showed that potassiutn sulfide would dissolve 90 pct of the avsenic sulfide in Hg-As satnples and only 1 to 10 pct of the Hg; the sodium sulfide would then dissolve 80 to 90 pct of the rernaining Hg and 30 to 70 pct of the vemaining As. 1 HIS paper describes the extraction, by alkaline sulfide solutions, of mercury from cinnabar-bear ing ores and flotation concentrates. Leaching time and solution temperature had minor effects on mercury extraction when compared to the effects of reagent quantity and ore type and grade. Cinnabar, although readily soluble in sodium sulfide, was only partially soluble in potassium sulfide and essentially insoluble in ammonium sulfide. A double leach process was developed to extract selectively the arsenic from Hg-As products with K2S and to treat the residue with sodium sulfide-hydroxide solutions to extract the mercury.&apos; Mercury was then recovered from the pregnant solutions either by precipitation with metallic aluminum or by electrodeposition. The solubility of HgS in alkaline sulfide solutions was first reported by Volhard in 1878.&apos; The first reported commercial application was made in 1915 when Thornhill applied the method to the treatment of an amalgamation tailing.3 Mullhollen, in 1911. described the chemical reaction of HgS with Na,S and alkaline hydrate to be:4 Most investigators have reported using a 4-pct sodium sulfide and a 1-pct sodium hydroxide soluti~n.3-4 An increase in temperature or excessive dilution of the solution causes the reaction to be reversed. Church Holmes described a similar process used for the extraction of antimony from silver concentrates at the Sunshine Mining Company&apos;s mill at Kellogg. Idaho.5 More recently. Erspamer and Wells reported the results of leaching studies on a Hg-Sb ore from Alaska.6 EXPERIMENTAL PROCEDURE Leaching tests were made on samples of mercury ore from eight deposits in Oregon, Washington, and Idaho. In addition. tests were made on flotation concentrates from seven of the samples as well as a flotation concentrate from an operating mill. Since previous investigators reported reagent requirements greatly in excess of that required by the equation HgS + Na2S = HgS . Na2S, initial studies were made on chemically pure HgS. Results showed that the reaction actually required about 1 g of Na,S per g of HgS in an aqueous solution rather than 0.338 g of Na,S as indicated by the equation. To check further the matter of reagent requirements, Na2S and HgS were mixed together in equal mole ratios. Water was then added, a drop at a time, until the components reacted; X-ray diffraction analyses showed no HgS nor Na,S present. The yellow hydrate compound which formed would not redissolve until about three additional mole equivalents of Na,S were added to the solution. This indicated that a stable solution would require at least 4 moles of Na2S for each mole of HgS. While these implications may be valid for pure HgS, the possibility of entirely different results caused by the existence of other elements present in ores and concentrates was recognized. Consequently, experiments of the same order were made on samples of a flotation concentrate from a producing mill. The concentrate, containing about 18 pct

Jan 1, 1962

By AIME AIME

AMONG the industrial motion pic¬tures released in the last year of possible interest to people in the mining industry are the following: "A New World Through Chemistry," made by the public relations department of E. I. du Pont de Nemours & Co., Wilmington, Del. This film, which is in sound and color, interprets in twenty minutes of narration and ingenious photography many of chemistry&apos;s newest developments. It may be borrowed either in 16-mm. size on an 800-ft. reel, or 35-mm. size on a 2000¬ft. reel, the only charge being the cost of returning the film. Douglas D. Rothacker, 729 Seventh Ave., New York City, is prepared to loan free of charge except for transportation each way several films prepared in the plants of the International Nickel Co., 16 mm. with sound. These include: "Nickel High Lights," 35 minutes; "Nickel Mining," 18 minutes; "Nickel Smelting," 18 minutes; "Nickel Refining," 9 minutes; and "Copper Refining," 6 minutes.

Jan 1, 1941

By G. S. Cole, G. F. Bolling

Recent experitnents on crystal growth have indicated that thermal convection in the liquid influences the conditions of solidification and subsequent crystal characteristics. However, the important columnar-equiaxed transition in castings has not been examined as a function of this free convection. An experiment is presented here to demonstrate a change in the transition as convection is suppressed. Lead- and tin-based alloys were cast in stainless-steel molds either without special procedures or with thin grids placed horizontally across the tnold diameter in portions of the castings. While the grids allowed some diffusion of heat and mass transport to occur during solidification, massive fluid flow was hindered in the vegiotz of the grids. A larger percentage of columnar grains appeared in the grid region than in other parts of the special castings or than in all regions of normal castings. This structural difference can be explained in terms of thermal convection. THERE is little information about the possible effects of natural convection which may occur during the solidification of a casting. Ruddlel-3 has stated that the movement of liquid metal produced by convection might assist in the transfer of heat, but in the absence of confirmatory evidence he suggested that this idea be treated with caution. chalmers4 considers, but does not assess, the importance of fluid motion in casting, while Tiller5 suggests that, in liquid metals which have extremely high thermal diffusivities, the effects of thermal convection may be negligible. In addition, throughout the literature, there are statements indicating the possible presence of thermal convection but without proofs or evaluations of its influence. Natural convection may be divided into two categories: thermal convection, where liquid flow is due to density differences caused by temperature gradients in the liquid (e.g., liquid near a cold wall falling with respect to hotter liquid further away from the wall); and solute convection, where flow is due to density differences as a result of concentration gradients, see Wagner.6 In most instances thermal convection predominates over solute convection. Nevertheless, even thermal convection has not been studied in any detail and is difficult to handle, since it can vary quantitatively from one experiment to another depending upon the exact positions of heat sources and sinks or the attitude of the container with respect to gravity. In spite of these difficulties it is possible to realize that a higher rate of heat transfer must result with convection than in any situation where conduction acts alone. Thus, the degree of increased heat transfer is the important undecided question in considerations of casting. It will be demonstrated here that a reduction in convective flow leads to a suppression of the columnar-equiaxed transition in a casting and that this suppression is related to a decrease in the degree of heat transfer. Fortunately it is possible to do this by comparative rather than quantitative measures. The insertion of horizontal plates or grids into a simple mold does not appreciably influence heat transfer per se, but in reducing the allowable height through which colder liquid may fall freely it reduces natural thermal convection. This leads to a reduced fluid velocity, a different flow pattern, and an altered heat transfer which can be measured. EXPERIMENTS The alloys were prepared from elements of 99.9 pct nominal purity and cast into an uncoated 2-in.-diameter stainless-steel mold insulated at the bottom with a suitable refractory so as to ensure predominantly radial heat flow during freezing. Casting was performed either in empty molds or in molds containing grids or plates in various configurations . The grids were constructed of aluminum screen (1/32 in. thick) which was cut to the desired shape, cleaned in aqua regia, and coated with a mixture of 2 parts aqua dag graphite -1 part Sauereisen cement mixture, thus supplying a hard, protective, and insulating layer approximately 0.006 in. thick. The

Jan 1, 1965

By Paul A. Farrar, Harold Margolin

The system Ti-Cr has been re investigated From 40 to 100 pct Cr. The high-temperature modification of TiCr, was found to exist in the temperature range from 1365 where it terminates in the eutectoid reaction TiCr,(TI)* — HE chromium-rich region of the Ti-Cr system was investigated by Vogel and Wenderott,&apos; Mc Quillan,&apos; Van Thyne et dl.,&apos; and Cuff Duwez and Taylor determined the crystal structure of the low-temeperature modification of TiCr, to be fcc a = 6.943A and Levinger&apos; discovered the existence of a second (high-temperature) modification of TiCr, and determited its crystal structure to be hexagonal a = 4.932A, c/a = 1.617i. No information was obtained as to the temperature range over which each modification of TiCr? existed; therefore the present investigation was initiated. I) Experimental Techniques Alloys employed for the delination of this system were prepared from iodide titanium and high-purity chromium. The purity of these materials is as follows: Iodide titanium: purity 99.99 pct; major impurities—carbon 0.0001 pct; oxygen 0 to 0.002 pct; nitrogen 0 to 0.002 pct; silicon 0 to 0.005 pct; manganese 0.001 pct; copper 0.001 pct (Foote Mineral Co., Lot 609-29). Chromium #1: metallic purity 99.997 min.; interstitial content—oxygen 0.27 to 0.46 pct; hydrogen 0.028 to 0.038 pct; nitrogen 0.0002 pct (Ave-quipo Inc.). Chromium #2: purity 99.9 pct; major impurities—carbon 0.01 pct; oxygen 0.013 pct; nitrogen 0.02 pct; silicon 0.01 pct; sulfur 0.03 pct; iron 0.01 pct (Fulmer Research Institute Ltd.). A total of sixteen alloys of thirteen different compositions was prepared in the range from 40 to 95&apos; *All percentages are given in weight percent. pct Cr. The compositions of the alloys prepared were as follows: Ti-40, 45, 50, 60, 62, 64, 66, 68, 70, 80, 85, 90, and 95 pct Cr. Two buttons were prepared of the 66, 90, and 95 pct Cr alloys. The 40 pct Cr and one of the 66 pct Cr alloys were prepared from the chromium # 2. All the other alloys were prepared from chromium #1. The alloys were arc-melted as 25-g buttons in a copper-hearth glass-walled furnace7 under an inert atmosphere of high-purity helium. The alloys were sintered at 250 amp and melted twice at 350 amp for 30 sec with the buttons being turned over between melts. Weight losses during melting were determined and in the range 45 to 68 pct Cr they were found, in all cases, to be less than 1.25 pct of the total alloy weight. A number of the high-chromium alloys shattered during cooling from either the first or second melt, which made the weight loss considerably larger than usual. The 70 and 80 pct alloys lost approximately 5.7 pct of their total weight, the 85 pct alloys 1.5 pct, the 90 pct alloy 2 pct, and the 95 pct alloy 3 pct. However, it is felt that the actual composition of the alloys in this region is probably within approximately 1 pct of the intended composition, as a large portion of the material lost was that due to shattering after melting. Nominal compositions were therefore used in plotting data and referring to the alloys. The alloys were cut into specimens, wrapped in molybdenum sheet, and encapsuled in argon-filled quartz or Vycor tubes for heat treatment. The heat-treatment times and temperatures are given in Table I. The specimens were quenched in iced brine (I.B.Q.) following heat treatment. The standard techniques of grinding, polishing., and etching were used in preparing the specimens for metallo-graphic examination. For alloys below 68 pct Cr

Jan 1, 1963

By Nicholas J. Grant, Robert H. Kane, Bill C. Geissen

The platinum-rich section of the Ta-Pt Phase diagram was worked out by metallographic and X-ray techniques, using twenty alloys; solidus temperatures and solid solubilities were determined. Besides s phase, four intermediate stoi-chiometric phases were found: TaPt (high-temperatzrre phase, structure unknown); TaPt2 (ortho-rhomhic, new type); a TaPt3 (orthorhombic, TiCu3 type); ß TaPf3 (monoclinic, new type). TaPt2 and TaPt3 melt congmentlv; two eutectic, two beritec-tic, and one eutectoid reactions occur in the inuestigated range. THE Ta-Pt system was examined as part of a study of the phase diagrams and the intermediate phases of niobium and tantalum with Group VIII transition metals. Since the main scope of this work was the relation among the ordered close-packed phases occurring in the concentration range from AB to AB3 (A = Nb, Ta; B = Pd, Pt, and so forth), only the platinum-rich side of the diagram was worked out thoroughly, while spot checks were made to determine the approximate outline of the tantalum-rich portion. The system has not been thoroughly treated in the literature; Greenfield and Beck1 in their survey of refractory metal intermediate phases found a o phase between -18 and 37 at. pct Pt which coexists at higher platinum concentrations with an unidentified intermediate phase. Browning2 worked on the range between 55 and 100 at. pct Pt; however, this preliminary study did not cover temperatures >1500°C, and included no conclusive crystallo-graphic data. More recently, a study of the platinum-rich section of the Ta-Pt system has been carried out by Ray,3 while Hartley, Parsons, and steedly4 have studied the tantalum-rich section. The crystal structures of TaPt2, a TaPt3, ß TaPt3, and others have been reported in abstracted form by Giessen and Grant.5 EXPERIMENTAL METHODS The methods of alloy preparation and processing and of the metallographic and X-ray procedures follow very closely those described by Ritter, Giessen, and rant&apos; for other refractory metal-noble metal systems, and will not be repeated except where significant differences exist. Starting materials were: tantalum rod of 99.95 pct purity, supplied by National Research Corp., and platinum sponge 99.9 pct, supplied by The International Nickel Co. An oxygen analysis of the tantalum rod showed 30 ppm O; other impurities were C, N, Si, Nb, Mo, none of these exceeding 50 ppm, and 100 ppm W. Homogeneous buttons were readily prepared as follows: ingots of 5 g were weighed and arc-melted under welding grade argon, followed by two remelts after inverting the button. Between 40 and 100 at. pct Pt, weight losses during the first melt rarely exceeded 0.1 pct, in which case the alloy was rejected, and were nil on subsequent remelts. Since the vapor pressure of platinum far exceeds that of tantalum, the small evaporation loss could be assumed to consist of platinum; therefore, a corresponding amount of platinum was added on the second melt. Since it was confirmed on pure tantalum samples that no weight gain through oxygen or impurity pickup occurs (see Ref. 71, it could be assumed that the uncertainty in the composition did not exceed ±0.1 at. pct for the range 40 to 100 at. pct Pt. For the four control melts from 0 to 40 at. pct Pt, an error of ±0.5 at. pct was calculated. Microscopic examination of the whole buttons after melting showed no inhomogeneity other than local coring. This was eliminated by a homogenization heat treatment. A total of twenty-three alloys were prepared. Heat treatments were carried out in a tantalum

Jan 1, 1965

By E. S. Bumps, H. D. Kessler, M. Hansen

The titanium-rich end of the Ti-AI phase diagram has been determined to the compound TiAI3 (62.7 pct Al), thus joining the aluminum-rich portion previously investigated by others and completing the diagram. Micrographic analysis and X-ray diffraction were the chief methods used to determine the phase relationships. THE Ti-Al phase diagram has been investigated as part of a program on titanium phase diagrams for the Wright Air Development Center. Included in the available information concerning the phase relationships in titanium-rich Ti-A1 alloys is a brief statement by Brown&apos; that: "aluminum raises the transformation temperature to 1000°C (183Z°F)." This observation is interesting in that it is the first example of a metallic alloying component raising the transformation temperature of titanium, and consequently widening the field of the a solid solution. Busch and Freyer&apos; presented resistivity data which indicated the formation of titanium-rich solid solutions of 1 and 3 pct A1 alloys prepared by powder metallurgy methods. Duweza found that there is only one other intermediate phase other than the known compound TiA1, (62.7 pct Al). This phase, designated as y, is of variable composition; its crystal structure is of the AuCu type and is therefore based on the composition TiAl (36.02 pct Al). Earlier work on the constitution of the aluminum-rich alloys has been reviewed by Hansen, and need not be discussed here. The tetragonal crystal lattice of TiAl,, as found by Fink, Van Horn, and Budge," was confirmed by Brauer." Recently, Schubert7 has reported that TiA1, is homogeneous within a limited composition range; however, the solubility limits were not given. The Ti-A1 phase diagram as presented in. this paper was determined by micrographic analysis of alloys containing from 1 to 62 pct Al, annealed at and quenched from temperatures between 700" and 1400°C. The phases and phase ranges investigated extend to the compound TiA1, (62.7 pct Al) to join the aluminum-rich end of the system determined by other investigators, thus completing the diagram. Methods of Investigation Preparation of Alloys: Iodide titanium, 99.9+ pct pure, obtained from the New Jersey Zinc Co., and high-purity (99.99+ pct) aluminum sheet from the Aluminum Co. of America were used to make up alloy ingots weighing 10 to 20 g. Detailed descriptions of melting techniques have been presented previously for work on the Ti-Mo and Ti-Cb> nd Ti-Si" phase diagrams. Briefly, the melting practice consisted of arc melting an accurately weighed charge in a copper block crucible insert in a non-consumable tungsten electrode furnace, under helium at atmospheric pressure. All ingots were carefully weighed after melting to detect possible losses. Comparison of weight before and after melting showed no appreciable weight changes. Also, chemical analyses were in close agreement with nominal compositions, Table I. The diagram as presented is, therefore, based on nominal compositions. Alloys were prepared having the following nominal aluminum contents: 1 ... 36 (1 pct increments), 38, 40, 41, 42.5, 44, 45, 46, 47.5, 49 . . . 64 (1 pct increments), 67, 70, 80, and 90. Ingots with up to 14 pct A1 were cold-pressed various amounts in order to increase the rate of attaining equilibrium structures on heat treatment. The amount of cold deformation that could be applied decreased with increasing aluminum content, until alloys containing 12 pct A1 or more cracked after only a few percent deformation. Annealing Treatments: Samples annealed at temperatures of 700" to 1000°C were sealed in

Jan 1, 1953

By Charles C. Templeton

Any explanation of the nature of multiphase fluid flow through porous media must ultimately involve a knowledge of the mechanism of such flow through the individual pores of the medium. To provide quantitative information of the latter type, a study was made of gas-liquid and liquid-liquid displacements in single uniform Pyrex capillaries with diameters as small as 4 microns. Quantitative observation of air-liquid displacements with zero contact. angle indicates the adequacy of a model based on Poiseuille&apos;s Law and the independence of capillary pressure and interfacial velocity. Consequently, this work discounts previous claims that flow is abnormally retarded in very small capillaries. For the displacement of a very viscous oil by water in a capillary initially filled with water, flow is faster than predicted by the above model. This behavior is probably due to the existence of a thin annular film of water between the oil column and the capi1lary wall as postulated by Yuster. INTRODUCTION The need for experimental observation of the microscopic nature of multiphase fluid flow, to further the understanding of the results of macroscopic flow investigations, has been previously recognized. Chatenever and Calhoun1 in connection with the API Project 47B have extensively studied the flow of fluids through layers of glass or lucite spheres between glass or lucite plates. Lowman2 prepared an interesting film concerning flow in a single capillary, using an apparatus which made a moving interface appear stationary in the field of a microscope. The purpose of the present investigation was to deter- mine what contribution might be made to this field by comprehensive quantitative observation of gas-liquid and liquid-liquid displacements in single capillaries of uniform, very small diameter. The techniques used are similar to those of Lowman but incorporate improvements necessary for quantitative work. Quantitative observations must begin with fluids of simple chemical composition to provide a basis for analyzing the more complex behavior that may be expected with natural reservoir fluids. However, some qualitative observations on systems involving crude oils are presented. Experiments of this sort involve the observation of the velocity of the interface separating two fluids, and have been performed in horizontal or vertical capillaries by several investigators.3,4,5,6,7,8 The most general treatment of their mechanics, by Brittin,9 involves forces due to capillarity, viscous resistance, gravity, an "end-drag" effect, and the rate of change of momentum of the capillary contents. Since the range of pore diameters of interest in petroleum reservoirs is about 0.1 to 100 microns, it was desired to perform these experiments in the smallest capillaries possible, to ascertain whether capillary diameter had any effect on the existing theory based on data from larger capillaries.* It was also important to be able more systematically to vary the direction and rate of displacement than was done by previous investigators. Finally, to concentrate attention on viscous and capillary forces by eliminating gravity as a parameter, this study involves only horizontal capillaries. The work of Eley and Pepper&apos; with a "large" (0.766-mm diameter) horizontal capillary is the previous investigation which is most similar to the present method of quantitative observation. Here capillaries with diameters as small as 4 microns will be studied.

Jan 1, 1955

By H. Bartholomew, L. Bernstein

Experirmental bonds of Ag-In SLID to gold, copper, nickel, Kovar, Dumet, nickel-plated molybdenum, ALL-Pt vrzetallizing on ceramic, and nickel-plated Mo-Ti metallizing on Al2O3 ceramic have been made and exalnined. Metallographic taper sections were made of all bonds for Phase identification. In addition, failuve temperatltres were determined for bonds heated undev shear load. Sowe bonds were subjected to electvon-probe microanalysis. The ternary SLID system Ag-In-Sn was similarly evaluated. Plwtonticrogaphs and electron-probe data are discussed and related to over-all phase diagrams , diffusion effects, and wetting properties of the liquid. The rates of diffusion andor compound formation of gold, silver, and copper in indium and In-Sn liquids are found to descend in that order, as measured by the relatzve thickness of phase layers in the interfaces of bonds made at 200to 400°C. It is concluded that the SLID process enables one to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures, and meet most requirements for application in interconnection, silicon bonding, or hermetic sealing of electronic devices. In a previous publication by one of the authors, the theory and principle of SLID bonding in simple binary systems was discussed. SLID bonding can be defined as a joining process using a preform with a laminated structure: a low-melting material clad on a high-melting core. During the bonding cycle a metallurgical transformation occurs such that the resultant structure can withstand, without reliquefying, temperatures higher than those at which the bond was made. The phases present in the joint interface region are high-melting compounds or, if equilibrium is reached, solid solution. Properties will depend on the phases present, ultimately approaching those of the solid substrate core of the SLID preform. The high-temperature strength of bonds made in these systems was correlated to phase identification in the interfacial bond regions from metallographic cross sections and electron-probe X-ray microanalysis data. When complex electronic components are assembled, multiphase systems result at the interfaces of bond regions. In these ternary and higher-order systems very little diffusion and phase-diagram data is available with which to predict the nature of the interfacia1 region that will result from conventional fabrication processes and subsequent field use of the component. Clarke and Rhines did early work in the field using the Al-Mg-Zn system as a vehicle. Guy and co-workers studied a portion of the Cu-Zn-Ni system and some mathematical4 and general5 aspects of multiphase diffusion. irkald&apos; and coworkerse recently studied diffusion in the Cu-Zn-Sn system. No diffusion studies have been made on ternary systems directly applicable to this investigation but some phase diagrams are available: g-u-n, u-i-n, and CU-i-n. I) DESCRIPTION AND EXPERIMENTAL PROCEDURE The elements Au, Ag, Cu, Ni, In, and Sn are found in alloy systems commonly used in fabricating and assembling electronic components. Reference to the appropriate phase diagrams9 and the previous publication will indicate that the binary systems of any of the two low-melting elements, indium and tin, with any one of the other four higher-melting elements are capable of producing SLID bonds. It is not unreasonable to assume that any ternary or higher-order alloy system containing at least one of the elements gold, silver, copper, or nickel and one or both of the elements indium and tin could be used to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures. Indeed, the liquidus contours and isothermal sections of those phase diagrams available7 do so indicate. The parameters affecting the bond and the equipment used in evaluating the bond were described in an earlier paper.&apos; The current investigation used the

Jan 1, 1967

By Lawrence Adler

For openings in bedded rocks, analyzed by simple beam theory, it has been shown that roof loads can be shifted from one support to another.&apos; This transfer is effected by controlling the relative deflection of adjacent supports. If this action is used to reduce loads in the props or bolts and increase them in the ribs or pillars, it could be productive of economies averaging 30 pct. Such savings can be realized by: 1) using smaller artifical supports such as props and bolts, and 2) increasing loads in the rib to induce eventual failure for longwall caving. Since the rib is relatively load-insensitive, it provides a natural load sink. However, caution must be used in applying such permissive deflections, for while the supports are being handled properly, the stresses in the roof itself are very sensitive to such manipulations.&apos;

Jan 5, 1960

By Simon D. Strauss

The world appetite for minerals in the, third quarter of this century grew at a higher rate than had been anticipated. To illustrate, consider the experience of four, commodities. Excluding the Communist bloc, sometimes referred to as the centrally planned economies, demand for aluminum increased at a compound rate of 8.6% between 1950 and 1975,; copper rose by 4.4%; iron ore by 5.5%; and tin, the laggard in the group, by 2%. Except for tin, the figures are substantially greater than growth rates anticipated in 1950 in the Paley Commission report and other studies. The growth rate was not evenly distributed in geographical areas. Professor Wilfred Malenbaum of the University of Pennsylvania did an interesting study breaking these figures down as among three principal sources of demand -- the United States, other industrialized nations (which he referred to as the "rich lands"), and the developing world (which he referred to as the "poor lands").

Jan 1, 1982

By A. P. Anderson, J. H. Jensen, W. E. Breckoff

Bromine is the intermediate member of the halogen family of elements between iodine, a solid, and chlorine, a gas. The name is derived from the Greek "bromos," meaning stench. Bromine is the only nonmetallic element that is liquid at room temperatures with a melting point of -7.2° C and a boiling point of 58.78º C. Reddish brown in color, it dissolves easily in water to yield a red solution. Bromine volatilizes at ordinary temperatures to a red vapor that is very irritating to the eyes, nose, and throat. Density of the liquid is 3.12 and gas weighs 7.59 gpl at standard conditions. As the element is highly active, it exists in nature only as bromide compounds. Bromine was discovered by Antoine Jerome Balard in seawater bitterns in 1826 and first prepared in quantity in 1860. Distribution Bromine is widely distributed in nature and compounds occur in solution in natural brines, in seawater, saline lakes, oil and gas well brines, and in evaporite chloride minerals. The concentration of bromine salts ranges from 60-65 ppm in seawater to several thousand ppm in oil well brines and saline lakes. The distribution of bromine in marine evaporite minerals and in the solutions from which they crystallized was determined many years ago by H. E. Boeke (1908). Theoretical aspects regarding the geochemistry of bromine have been published in numerous papers (Raup and Mite, 1969). Bromine occurs in solid solution in carnallite and sylvite associated in potash deposits; in halite in salt beds; salt in oil shales; and in trona deposits. Its presence is useful as a guide in geochemical exploration. The analysis of small amounts of bromides in the presence of large amounts of chlorides is discussed by W. Schwerdtner (1963). Manganese, iron, and iodine may interfere with the determination. Other analytical methods are discussed at length in the literature (Stenger and Atchison, 1964). Sources and Reserves The sources and reserves of bromine, given in Table 1, appear ample to meet present and foreseeable requirements in all producing countries. With the occurrence of bromine salts in seawater and other brines, the potential for bromine production is worldwide. It has been estimated that 99% of all commercially recoverable bromine is in the ocean. However, actual subterranean brines having a higher bromine content than seawater will continue to be the preferred sources of bromine for the foreseeable future. [ ]

Jan 1, 1983

By Sidney G. Parker, Jack E. Pinnell

Cubic ZnSe crystals have been grown with HCl, HBr, and I, as chemical transport reagents. The growth of large, well faceted crystals is in the order HCl < HBr < I, with some produced by I, transport being 1 cm on an edge. ZnSe:I crystals showed no strain in cross polarized light and were homogeneous as determined by electron microprobe. These ZnSe:I crystals had a mobility at 25°C of about 300 sq cm per v-sec and contained 103 dislocations per sq cm; further, these crystals were pure cubic and showed both photolumi-nescence and photo conductance. Doping was attempted during crystal growth. ZnS and Zn (S,Se) crystals were also grown by I, transport. ZnSe crystals have been grown by most of the common techniques.1"6 Of these, chemical vapor transport as developed by Kaldis2 showed promise of producing high perfection, cubic ZnSe. With chemical transport, crystals can be grown far below the transition temperature for conversion of cubic to hexagonal structure. A small temperature gradient between source and growth region tends to allow near equilibrium growth, which should lead to good crystalline perfection. Because it is necessary to form volatile compounds, halogens or their compounds are extensively used as transport agents. HCl, HBr, and I, were compared as transport agents for growth of ZnSe crystals. Doping during crystal growth was attempted. ZnS and ZnSxSe1-x crystals were also grown by chemical transport. Electrical and optical properties of the crystals were examined. EXPERIMENTAL Fig. 1 is a sketch of the growth apparatus, which was a modification of Kaldis&apos;. A quartz rod which butted against the seed crystal served as a heat sink to promote growth only on the seed. Initially, crystal growth was attempted with ZnSe prepared by wet chemical methods. Because such a material contained oxides and selenates, HC1 reacted with these oxygen compounds to form H2O and no ZnSe transport occurred. Further, this ZnSe contained about 10 ppm Cu plus other impurities. High purity ZnSe, containing small amounts or no oxygen compounds, was prepared by reaction of H2Se with zinc vapors at 600° to 800°C in an atmosphere of palladium diffused H2.7 The ZnSe thus produced was usually copper free and contained only 1 ppm by weight of magnesium as determined by emission spectrographic analysis. G.E.&apos;s electronic grade ZnS, which had about 10 ppm metallic impurities, was used without further treatment. ZnS-ZnSe charges were prepared by mixing the two compounds together, then sintering 24 hr at 1100°C in an H2S ambient. The gases, HBr and HC1, were commercial grade, of 99.9 pct purity, while the I2 was 99.999 pct pure. The single crystal seeds with (111) faces for growth were mechanically held in place by sealing the outer quartz tube to the growth tube. After the charge was introduced, the system was outgassed at l0-5 torr while heated to 500°C. The desired quantities of transport reagents were then sealed off in the system, which had been cooled to 25°C. The growth tubes were inserted into a furnace with the desired temperature and thermal gradient. The system was allowed to cool for 1 to 12 hr from growth temperatures of about 850" to 25°C. The tubes remained stationary during crystal growth. HCl CHEMICAL TRANSPORT GROWTH Preliminary runs with HC1 had a temperature gradient of 100° to 200°C and no seed or heat sink. Only small crystals were obtained in these experiments as

Jan 1, 1970

By T. L. Berger, M. C. lnman, M. F. Rose

AFTER shock loading, mechanical twinning has been observed by several authors1-4 for a variety of fcc metals and alloys. It has been shown2,3 that low stacking fault energy materials deform primarily by the formation of mechanical twins and stacking faults during dynamic loading. Further, Inman, Murr, and Rose2 have shown that a correlation exists between the average hardness and the volume percent of mechanically twinned material in stainless steel. It has been observed in nickel&apos; that mechanical twins are produced during shock deformation if the peak pressure associated with the shock wave is greater than 350kbar. It is the purpose of this work to discuss shock-hardening mechanisms in nickel and to determine to what extent the initial condition influences the final response. The "flying plate technique" was used to generate planar shock waves with peak pressures as high as 710 kbar. The details of the technique5" have been discussed elsewhere and will not be repeated here. The material used in this study was polycrystalline nickel of 99.98 pct purity and had an initial grain size of 0.18 mm. Prior to any deformation, all samples were given a stress-relief anneal of 6 hr at 600°C in a vacuum furnace. After annealing, the initial condition of the samples was changed by cold rolling individual samples from 0 pct to a maximum of 80 pct reduction in thickness. This provided samples with controlled initial histories for shock deformation. Immediately after shock loading, the specimens were slowed and quenched by suitable arrangement of buffer material and water bath. This technique minimized specimen damage and the effects of shock heating on the samples. Since deformation twins in high stacking fault energy fcc metals are only produced at high stress levels, the initial defect configuration prior to mechanical twinning should greatly influence the number of twins formed. In fact, Zukas and Fowler7 have found that prestraining in iron and steel greatly suppresses the formation of mechanical twins during the shock deformation process. Following the methods of Warren and warekois8 and Cohen and Wagner,9 X-ray diffraction profile analysis was performed to determine the incidence of stacking faults and mechanical twins in the deformed nickel. Analysis was made on samples in the annealed, cold-rolled, shock-loaded, and cold-rolled—shock-loaded states. The estimated accuracy of the peak position measurements is *0.01 deg in 2?. Therefore the accuracy in the measurement of the relative peak shifts between the (400) and (222) diffraction line profiles is on the order of *0.04 deg in 2?. None of our measurements indicated peak shifts greater than 0.04 in 28. This would correspond to a fault density of -1 pct and sets the limit on the sensitivity of our instrument. Similarly, analysis of the shift in the center of gravity of the diffraction line profiles yields the minimum measurable value of the twin fault probabilitya to be -0.002. Fig. 1 shows mechanical twinning in nickel shock-loaded to 400 kbar. In this photograph, fault intersections are clearly visible. The thickness of the individual fault lamellae was determined from the image widths of their lines of intersections by the

Jan 1, 1968

By W. L. Falke, A. A. Cochran

A basic problem in connection with manganese is to find economical ways to utilize domestic resources. As a part of its program to conserve domestic mineral resources and to reduce dependence of foreign sources, the Bureau of Mines had conducted extensive research to broaden manganese technology and to find economical, technically-feasible processes for recovering manganese from these low-grade resources. This paper analyzes some of the major difficulties which have been encountered in previously proposed processes for treating low-grade manganese ores and discusses a process which may circumvent many of these difficulties. Vast deposits of low-grade manganese ore exist in the U.S., yet domestic production is insignificant compared to the more than 2 million tons of ore imported yearly into this country.&apos; A basic problem in connection with manganese is to find economical ways to utilize domestic resources.2 As a part of its program to conserve domestic mineral resources and to reduce dependence on foreign sources, the Bureau of Mines has conducted extensive research to broaden manganese technology and to find economical, technically feasible processes for recovering manganese from these low-grade resources. Although a great many processes have been proposed for treating domestic manganese resources, a failing of many of them is that too many steps are involved for economical operation.&apos; Some of the major processes that have been proposed were reviewed by Norman and Kirby.3,4 Chlorination processes have become increasingly useful as a means of recovering valuable metals from raw materials, because the relative cost of chlorine (Cl2) and hydrogen chloride (HC1) has decreased through the years, and because the corrosion resistance of materials of construction has been improved. The objective of these processes is to form metal chlorides that are more volatile or water-soluble than are the corresponding oxides or sulfides; these compounds then can be separated from the gangue or other minerals by volatilization or leaching. Several chlorination processes for the recovery of manganese have been investigated by the Bureau of Mines5-8 and others; the major chlorination processes were reviewed in 1963, and their main features were compared.4 In all these processes, the simultaneous leaching or volatilization of iron chlorides with manganese chloride (MnCl2) is a problem, and the more iron that is present, generally the greater the problem. The leaching step is not highly selective, and the product of this step is, at best, suitable only for the production of ferromanganese or for further processing to remove iron. The product of the volatilization step is, in all cases, a mixture of iron and manganese chlorides that contains too much iron even for ferromanganese production, and must undergo additional processing steps for iron removal. THERMODYNAMIC CONSIDERATIONS The literature indicates that the desired chlorination reactions will proceed at practical rates at temperatures near 1200°K (927°C). Free energy changes at 1200°K for the critical steps of the reduction and chlorination reactions9-11 follow: Most of the research on chlorination processes for manganese recovery has been done with HC1 rather than with C12, for the following three main reasons: 1) Recycling of the chlorinating agent, which is economically vital, appeared to be easier for HC1

Jan 1, 1968