Search Documents

By H. T. Clark

NO previous determinations of the deformation or recrystallization textures of titanium or of titanium-base alloys have been reported in the literature. The room-temperature structure of titanium is hexagonal close-packed with a c/a ratio less than 1.633. It would be expected, therefore, to have a rolling texture similar to that of other hexagonal close-packed metals, namely (0001) [1010]. Burgers and Jacobs1 have shown that zirconium, a metal isomorphous with titanium in its structure and similar in many of its properties, has such a texture with a scatter of the basal plane toward the transverse direction. This scatter is in the opposite direction from that found in magnesium by Bakarian2 but similar to that reported by Smigelskas and Barrett3 or beryllium. The rolling and annealing textures reported here for high-purity iodide titanium are significantly different from the . textures of any other hexagonal close-packed metal. All titanium used during this investigation was prepared by the iodode process." The annealed hardness of this material varied from 73 (material used for sample No. 2) to 97 Vickers hardness number. An estimate of the chemical composition of this grade of titanium has been reported by Finlay and Snyder.5 With one exception, shown in table I, the as-deposited titanium was cast into 10 to 20 g ingots in an electric arc furnace in purified argon before being rolled to sheet. The cast ingots were forged and ground until their cross-section was approximately rectangular, annealed 1 hr at 700°C in vacuum and cold rolled. Rolling was carried out in a two-high, 4 in. diam mill, using reductions no greater than 10 pct per pass. The direction of rolling was reversed after each pass, and, in order to avoid temperature effects, the sheet was allowed to cool after each pass. Unless the rolled sheet was sufficiently thin for X-ray penetration (about 0.004 in.), it was reduced to this thickness by pickling. Because of the possibility of introducing twinning or other deformation during grinding, no attempt was made to maintain uniform thickness of the sample during pickling by intermediate grinding or sanding operations. Those samples to be used for determining the annealed texture were recrystallized by vacuum annealing the cold-rolled sheet for 1 hr at 500°C. These thin samples were held between thick titanium sheets during annealing to prevent distortion. Table I outlines the rolling and annealing schedule of those samples for which photograms or texture patterns are shown. X-ray Techniques The usual techniques for determining textures were employed during this work. Molybdenum radiation was used for the transmission exposures and copper radiation for the glancing angle ones. Since titanium fluoresces under these conditions, it is necessary to employ a filter between the sample and the film. The Kß radiation filters are very satisfactory for this purpose. Sufficient grains having favorable orientation were present in both the cold-worked and in the cold-worked—500°C annealed samples to provide satisfactory patterns with the samples stationary. Because of the difficulties of comparing intensities of transmission photograms with those obtained

Jan 1, 1951

By G. W. Healy, N. R. Griffing

The activity coefficient of sulfur in Cr-Fe-S melts was determined by measuring the values of Ph3Rh,in equilibrium with such melts. The results showed that chromium has a pronounced negative effect on the activity coefficient of sulfur, which up to about 20 pct Cr may be represented by the equation: log f; = - 0.019 pct Cr It was also found that the influence of chromium was not altered by the presence of appreciable amounts of carbon or silicon. The influence of alloying elements on the activity of sulfur in molten iron has been the subject of many investigations; however the effect of one important alloying element, chromium, has not been reported, and the object of the present investigation was to determine its effect on the activity coefficient of sulfur in liquid Fe-Cr-S alloys both in the absence and in the presence of carbon and/or silicon. EXPERIMENTAL PROCEDURE The general method employed consisted of passing mixtures of hydrogen and hydrogen sulfide over the sulfur-containing melt of interest and analyzing the outgoing gas to determine the equilibrium value of which resulted from the reaction shown in Eq. 111. H, (gas) + S (dissolved in melt) = H,S (gas) 111 The activity coefficient of sulfur, fs, was then calculated with Eq. [2] in which K, is the known equilibrium constant of Eq. [I] for dilute solutions of sulfur in iron. Raw materials used in the preparation of the charges included commercial grades of electrolytic iron and chromium and carbon-reduced, acid-treated silicon of 99.9 pct purity. Oxygen in the former presented no problem since it was removed by hydrogen in the normal course of an experiment. Carbon was added in the form of premelted iron-carbon and chromium-carbon master alloys. Sulfur was charged as iron sulfide prepared by first heating powdered iron and sulfur in air in an alumina dish until reaction occurred, and then deoxidizing by melting in a hydrogen atmosphere. Commercially bottled hydrogen and hydrogen sulfide were used after being passed through purification systems containing palladium, "Drierite," and magnesium perchlorate in the case of hydrogen, and "Drierite" alone in the case of hydrogen sulfide. Lamp-grade cylinder argon served as a flushing agent without further purification. Charges weighing from 300 to 500 g were placed in a high-purity alumina crucible of 0250-ml capacity and heated in an argon atmosphere in the induction-heated carbon-tube furnace illustrated in Fig. 1. During heating, a dry hydrogen atmosphere was substituted for argon in order that deoxidation of the charge and flushing out of argon would be accomplished sooner. After the charge melted, a Pt-Pt 10 pct Rh thermocouple contained in an alumina protection tube was immersed in the melt, and the desired melt temperature (usually 1600°C) was established. Higher temperatures up to 1760°C were required for some chromium-rich alloys because of their higher melting points, and in these cases a Pt 6 pct Rh-Pt 30 pct Rh thermocouple was used. The thermocouple output was fed to an automatic controller which provided straight line temperature

Jan 1, 1961

By C. W. Spencer, Che-Yu Li, R. J. Knight

The usual reaction product for the monotectic reaction in the Bi-Se system consists of rod -shaped particles of selenium-rich liquid embedded in a single crystal matrix of At certain crystallo-graphic orientations of the matrix with respect to the reaction interface, more complex shapes are as -sumed by the liquid particles. This reaction has been examined at different growth rates and relative crystallographic orientations of the matrix with respect to the reaction interface. The uhriation in auerage particle size of the liquid phase with reaction rate has been determined at one crystallograpIzic orientation of the matrix. On a plot of logarithm of average particle diameter vs logarithm of reaction rate, data points for crystals grown at rates of 10- to 1.0 cm per hr fall near a curve of slobe -0.4. MONOTECTIC reactions in binary alloy systems are reactions of the eutectic class in which, as the system is cooled through the three-phase reaction isotherm, one liquid phase (L) decomposes to a solid phase and another liquid phase (LII).' A partial phase diagram, as taken from Hansen, showing the monotectic reaction in the Bi-Se system is given in Fig. 1. This diagram specifies the monotectic point at 618°C and 72 at. pct Se, and the monotectic reaction products as the intermetallic Bi Se3 and a liquid (LII) which contains approximately 98 at. pct Se. At a lower temperature, 217°C, this liquid may undergo a eutectic reaction in which the reaction products are BizSe3 and crystalline selenium. However, under conditions of rapid cooling, or quenching, from above 217°C, this selenium-rich liquid may be partially retained to room temperature in an amorphous or glassy state. The intermetallic BizSe3 is rhombohedral, of the space group jm;' however, for convenience it is usually represented by a hexagonal struture. A pronounced plane of cleavage, which lies perpendicular to the main axis of the rhombohedral unit cell or parallel to the basal plane of the hexagonal cell, exists in the structure. The usual monotectic reaction product consists of rod-like particles of LII embedded in a single-crystal matrix of BizSe3, although at certain crystallographic orientations of the matrix BizSe3 other more complex shapes are assumed by LII. A similar rod-like, or cylindrical, morphology for the carbide phase has been reported by westbrook7 in the a Cr-Crz3Ce eutectic structure. In this paper the morphological characteristics of the LII particles, as retained to room temperature, have been examined under conditions of varying growth rate and crystallographic orientation of the matrix BizSe3 with respect to the growth direction. EXPERIMENTAL PROCEDURE Alloy specimens corresponding to the monotectic composition, 72 at. pct, or 50 w pct Se, were prepared from 99.999 pct pure bismuth and selenium obtained from the American Smelting and Refining Co. The two elements, corresponding to a total specimen weight of approximately 30 g, were encapsulated in 13 mm OD Vycor tubing under a vacuum of 5 x X mm of Hg. The capsules were suspended on a fine platinum wire in a Bridgman-type furnace which exhibited a temperature gradient of

Jan 1, 1963

On Friday, Jan. 17, the thirteenth impression of the Perkin Medal was presented to Dr. Frederick Gardner Cottrell, at a meeting of the New York Section of the Society of Chemical Industry, held at the Chemists' Club, in New York City. The presentation address was delivered by Dr. C. F. Chandler, Senior Past President of the Society. The medal was awarded for the recipient's work in the electrical precipitation of suspended particles in gases. Dr. Cottrell's career, which is so familiar to members of the Institute, was sketched by Dr. Chandler. He told at some length of the experiments leading up to the final solution of electrostatic precipitation, which has done so much to solve the problem of smelter smoke. The principal interest in Dr. Cottrell's speech of acceptance lay in his remarks about helium, the production of which has been so reduced in cost that it has practically supplanted the use of hydrogen for inflation purposes in war balloons. He said: "Two or three weeks after war was declared in 1917, Dr. R. B. Moore attended a meeting of the American Chemical Society in Kansas City. At the general session, Mr. Seibel of the University of Kansas, gave a paper on krypton and xenon in some of the natural gases of Kansas. At the end of his paper, he expressed regret that at such a time, when everyone was thinking of war problems, his paper was of a purely scientific nature and had no practical bearing on the war. Dr. Moore immediately got up and said that he did not agree with Mr. Seibel. The presence of helium in those wells could, and should, have a very practical bearing on the war, as this gas could be extracted in quantity from the natural gas and used for balloons and Zeppelins. He pointed out some of the natural advantages of helium over hydrogen, and quoted Sir William Ramsey's letter advocating the use of helium for airships. The general attitude of those present was one of scepticism, so he finally asked Dr. Cady for his opinion who stated that he believed-the thing could be done, but was very doubtful whether it could ever be made practical on account of the cost." Dr. Moore in a letter wrote: "That same day I talked to Dr. Parsons, who was present at the meeting and was returning to Washington almost immediately. I told him what had happened, and that I believed the matter should be taken up by the Bureau at once and presented to the War Department. He promised to do this as soon as he got to Washington; and I know that he did take the matter up with other Bureau officials." Dr. Cottrell continued in part: News of Ramsey's suggestions also reached this .country through other channels and eventually came to our attention. Professors Satterly and Patterson of the University of Toronto commenced experimentation of the subject Jan. 1, 1916. Col. G. A. Burrell, who headed the research department of the Gas Warfare Service at the American University, tells me that Cady's experiments had also suggested similar possibilities to him.

Jan 3, 1919

By Morris Muskat

It is pointed out that the application of capillary pressure curves obtained by drainage or desaturation processes to the calculation of the fluid distribution in interphase transition zones involves a number of difficulties; namely: (I) the development of very low nonwetting phase saturations appears to be in contradiction with the lack of mobility of such distributions indicated by permeability-saturation curves, (2) dispersed nonwetting phases are thermodynamically unstable, and (3) discontinuous phases should not be subject to hydrostatic equilibrium requirements. While these difficulties could be obviated by assuming that the capillary pressure drainage curve has an initial horizontal segment, they are automatically circumvented by application of the imbibition capillary pressure curve to the lower part of the water-oil transition zone. These generally show zero displacement pressure at only partial wetting-phase saturations. The countercurrent upward flow of oil into the main oil-saturated pay and downward drainage of water also suggests that wetting phase imbibition processes will control the saturation distribution immediately above the water-saturated section. Similar considerations, with a generalized interpretation of the apparent wetting-phase behavior of the oil and gas phases, provides a basis for constructing the curve for fluid distribution in the oil-gas transition zone. In the transition zones so derived, the oil begins with a nonvanishing saturation at the water-oil contact and terminates with a similar saturation at the top of the gas-oil contact. The gas-oil transition zone begins with an equivalent nonvanishing gas saturation. Introduction It has been a common assumption for some years that the nature of the fluid dis- tribution in virgin reservoirs, and in particular that in the transition zones between the oil and water and between the oil and gas sections, can be computed by a simple application of capillary pressure data. The results of such calculations appear to have been first reported by Leverett.' The latter, however, indicated only the numerical values of the parameters used in the computations, without explicitly describing the procedure. Leverett's illustrative calculated transition zones are reproduced in Fig I. Although no critical study of the apparently obvious method of calculation has been published, one cannot proceed very far in the computation without encountering some rather fundamental questions not yet answered in the literature. This paper is not written under the pretense that the whole transition-zone problem has been fully and satisfactorily solved. Its purpose, rather, is to discuss suggestions for its treatment, much of it admittedly hypothetical, and emphasize the nature of the uncertainties arising therein; for the literature, as now available, gives little indication that there are any problems still outstanding. The Transition-zone Equation The basic equation, which presumably gives directly the fluid distribution without recourse to any further consideration, is: Ap = (r1 - r2)gh [1] where r1, y2 are the densities of the two contiguous fluids, h is the height above the "capillary-free" zone of complete saturation with fluid I, g the acceleration of gravity, and Ap is the capillary pressure across the average interface at the height

Jan 1, 1949

By Charles Trotter

AN instrument has recently been developed for determining the inclination and azimuthal direction of boreholes. This instrument is known as the Tro-Pari Instrument and is the invention of C. Trotter and G. Pajari of Sudbury, Ontario. DESCRIPTION The instrument is characterized by a unit mounted in gimbals and provided with a clockwork mechanism to clamp a compass to indicate azimuthal direction and simultaneously to clamp the unit in its plumb position to indicate inclination (Fig I). By means of a timing ring suitably calibrated in 5-min divisions, the unit may be set to lock after a lapse of time sufficient to allow the placing of the instrument at the desired point in the drill hole where readings are to be taken. The maximum time lapse obtainable with the instrument designed for use in EX or AX size holes is 1 hr 30 min which is considered to be ample time to lower to the greatest depths that may be drilled with this size of equipment. Larger sizes could be developed for larger diameter holes such as BX and NX sizes or the larger oil-well sizes and a correspondingly greater time lapse could be provided for. Up to the present time only the EX-AX size has been built. OPERATION Assuming a borehole is to be surveyed at 1000-ft depth and assuming it will take 30 min to lower the instrument to this depth, the timing ring is rotated through seven divisions which represent a time lapse of 35 min (5-min leeway) and is then returned to its zero position. This operation imparts energy to a spring which drives the clockwork mechanism. Simultaneously the compass needle is freed to swing to its magnetic north-south position and the encased mechanism is freed to hang plumb within a semicircular portion of the frame which is graduated in degrees after the fashion of a protractor. This semicircular protractor portion has a V-shaped notch at each degree division of its inner periphery. The instrument, now in its free position, is inserted in a bronze container made to suit the size of hole to be surveyed (Fig 2). Soft rubber washers are provided within the container to prevent undue shock. The container is connected to the drill rods with three 5-ft lengths of brass or aluminum alloy rods separating it from the steel rods in order to prevent distortion of the magnetic field. The assembly is then lowered to the desired point where readings are to be taken and is allowed to remain at rest until a period of time has elapsed slightly in excess of the time for which the timing ring was set. In the example cited above, when the 35 min has elapsed the compass needle is locked in its north-south position and the protractor locking pin is extruded and locks in the V notch opposite its plumb position. The device may now be removed from the borehole and it will remain in this locked position in spite of jarring or shak-

Jan 1, 1947

By J. H. Scaff, H. C. Theuerer

Germanium may be reversibly converted from n to p type by heat treatment. Data for the conversion and the associated changes in resistreatment.tivity are given and the results are interpreted in terms of changes in the donor-acceptor balance. MEANS for controlling the electrical properties of germanium in a predictable manner are of interest because of the increasing utilization of this element as the semiconducting material in electrical devices. Since both the mechanism and the magnitude of the electrical conductivity depend upon the kind and quantity of impurities present, the conductivity usually is adjusted by first carefully purifying the germanium, and then, by standard alloying procedures, adding the elements desired. The elements usually added are from the third or fifth periodic groups depending upon whether p- or n-type germanium is desired. However, in the development of germanium rectifiers during the war, it was found that it was possible also to modify reversibly the conductivity of germanium and even to produce conversion from n to p type by heat treatment.1,5 Since then a detailed study of this effect has been made. The data are presented in this paper and an explanation is offered for the effects observed. Preparation and Experimental Procedure The method used in preparing the germanium ingots for this investigation has been previously described.' The method consists essentially of (1) reduction of GeO2* and (2) preparation of a 50-g ingot from the reduced material. Graphite containers are used in both steps. In the first step the GeO2 is reduced in hydrogen at 650 °C to form a sponge germanium which, to assure complete reduction and to obtain massive materials, is fused subsequently in the reduction furnace by gradually raising the temperature to 1000°C. The button of germanium thus obtained corresponds to a yield of 99.8 pct. The final ingot is prepared by fusion of the germanium button in a helium atmosphere. A cylindrical crucible in a vertical silica tube furnace is employed and the crucible is heated by an external induction coil. The ingot is solidified from the bottom upward by raising the induction coil at a constant rate with power to the coil kept at a fixed value. In such ingots, segregation is normal and most of the impurities are concentrated in the last region of the ingot to freeze. It follows then that the major portion of the ingot is purer than it would have been if freezing had occurred in a random fashion. Moreover the orderly advance of the freezing surface during solidification establishes in the ingot a succession of surfaces of constant composition, if it is assumed that the liquid is homogeneous and that diffusion in the solid is negligible. Therefore, some information on the distribution of impurities in the ingot may be acquired by determining the shape of the solid-liquid interface at different stages of solidification. This is of importance because the concentration of impurities will be seen to affect the response of germanium to heat treatment. Such information is difficult to acquire by direct means, for the impurities responsible for the electrical properties of germanium prepared in this way are present

Jan 1, 1952

By J. H. Smith, H. W. Paxton

ALTHOUGH many structural and kinetic investigations have been made for alloys of iron and nickel, only meager data exist from thermodynamic investigations. The purpose of this note is to estimate the free energy of the Fe-Ni solid solutions from thermodynamic data available for ternary alloys containing iron and nickel. The lack of a description of the thermodynamic behavior for the Fe-Ni system has required the structural and kinetic analyses of the system to assume some form of solution behavior, usually regular, e.g., the mar-tensite transformation analysis of Kaufman and Cohen, 1 consistent with the limited thermodynamic data. Indications that this system could exhibit ideal solution departures might have been suggested by the large deviations from additivity rules observed in the density and lattice-parameter measurements of Jette and Foote2 who interpreted this in terms of possible solute-solvent interactions. Later Turkdogan et al. 3 and more recently Ward and wright 4 found a minimum in the graphite solubility in liquid Fe-Ni solutions near the concentration of FeNi3 with deviations from linearity persisting at all concentrations. This was interpreted by Ward and wright4 to indicate negative heats of solution and was suggestive of short-range ordering. The infinitely dilute activity coefficient of carbon (?oC) was also observed by smith5 to pass through a maximum near the FeNi3 concentration in Fe-Ni solid solutions. Recent investigations of the liquid solutions over the entire concentration range by Zellars et a1.' and Speiser et a1.," using vapor-pressure determinations, revealed both negative departures from Raoult's law and a nonregular solution behavior. The solid alloys have been studied by Oriani 8 and Kubaschew-ski and von Goldbeck6 employing gaseous H2/H2O equilibria with Fe and FeO. Both investigations were in substantial agreement, indicating very small departures from ideality. However, Oriani observed the formation of Fe3O4 (instead of FeO) at XFe= 0.441 which severed the equilibrium and precluded experimental investigation of the nickel-rich alloys. Heat-capacity and heat-content measurements have been evaluated by Montgomery10 and found generally unsatisfactory for gleaning thermodynamic information. This is due to the unknown final states of the alloys caused by the interference of the martensite transformation on cooling iron-rich concentrations and superlattice formation, magnetic transformation, and the varied heat treatments used by investigators of nickel-rich concentrations. As an alternative to the experimental difficulties, indirect estimates of the solid-solution behavior have been made by Fleischer and Elliott11 and Smith et a1.12 From their measurements of the solubility of Fe-Ni alloys in liquid lead, Fleischer and Elliott calculated the nickel activity (aNi) (and integrated for aFe) by assuming: 1) liquid lead has no solubility in solid Fe-Ni alloys, 2) Henry's law is obeyed throughout the liquid lead-rich phase (0— 12 at. pct Nil, and 3) Henry's law constant is independent of relative iron and nickel concentrations. The estimate of Smith et a1.12 was obtained

Jan 1, 1964

By M. C. Flemings, P. J. Ahearn

Dendvite morphology of unidirectionally solidified Sn-12 pct Bi alloy was determined with the aid of X-ray and macroetch techniques. Columnar growth direction (growth direction of primary arms) in this alloy is [110]; secondary arms grow in the [lii], [111), and [112] directions. Interstices between [112] dendrite arms fill in during early stages of solidification so that well-defined (110) planes are seen in the final structure (parallel to the heat-flozo direction). Similarly, interslices betweex the [111] secondary arrlls fill in to form (112) planes, and interstices between [1111 ] arms fill in to form (112) planes. DENDRITE morphology in alloys is conveniently studied in unidirectionally solidified castings. In this type of solidification, heat is extracted from a single chill surface of the casting while other surfaces are insulated. Solidification progresses from the chill and results in cast grains that are columnar with the long axis of the grain perpendicular to the chill. Dendrite morphology is conveniently studied by examination of etched surfaces parallel and perpendicular to the chill, as previously described.'" Experimental studies on the growth direction for tin are in general agreement. The major growth direction is [110]:-' although this is altered somewhat by supercooling. In one study, tin dendrites pulled from a supercooled melt had a growth orientation 12 deg away from the [110] direction toward the [002] direction.' This orientation could be changed back to the [110] or close to the [110] direction by changing the tempera- ture gradient in the melt. In a study using autoradio-graphic techniques, (111) directions were shown to be directions of preferred growth in addition to the [110) direction.7 PROCEDURE The samples employed in this study were cut from 12 pct Bi-88 pct Sn castings, 1.5 in. in diam and 3.5 in. tall. The casting procedure consisted of heating the charge to 390°C and then pouring the molten alloy directly into a gypsum sleeve mounted on a massive copper chill. Specimens were cut from the ingot, mounted, polished, and etched with Taffs reagent [FeC13 .6H2O, 2 g; HC1, 5 cu cm;H20, 30 cu cm; CzHaOH (95 pct), 60 cu cm].' The dendritic pattern was clearly visible after etching. Photomicrographs at about 8 and 35 times were taken on surfaces parallel and perpendicular to the chill. Laue back-reflection patterns were obtained from three different columnar grains in a singIe polished face 2 in. from the chill. The cut face was polished and positioned in the beam of a Laue camera, so that diffraction occurred from a single dendritic grain. The resulting diffraction pattern was interpreted to determine crystal log raphic orientation in relation to the heat-flow direction and in relation to microstruc-ture of the given grain. RESULTS Fig. 1 shows a horizontal and vertical section of the columnar structure, at low magnification. Light regions are rich in tin, and darker regions tin-poor; the primary phase is tin-rich a phase. The two sections shown were taken orthogonally from the same metallographic specimen. It is readily seen from Fig. 1 that the dendrites have

Jan 1, 1968

By C. A. Bruch, J. F. Duffey

On the basis of metallographic and cooling-rate studies of 15 U-Zr alloys, a new version of the 6 phase region of the U-Zr phase diagram is proposed. IN several published diagrams of U-Zr alloy system:' there is good agreement that at elevated temperatures complete solid solubility exists between y uranium and ß zirconium. Similarly, there is reasonably good agreement concerning the uranium-rich and zirconium-rich ends of the diagram. However, there is no agreement concerning the nature of the diagram at intermediate compositions and at temperatures below about 650°C. The early work of Saller et al.8 hows an intermediate phase, 6. In a later diagram by Saller and Rough' shown in Fig. 1, the d phase field is drawn with dotted lines, indicating doubt that this phase exists. The diagram of Summers-Smith2 does not show the d phase. More recently Holden and Seymour' have shown that in the composition range 40 to 60 wt pet Zr, the high-temperature ? phase, which is body-cen-tered-cubic, transforms to an ordered structure, 8. They found that the order-disorder transformation occurs between 595° and 610°C, and presented a diagram based on the study of four different alloy compositions. Most recently Saller et a1.5 presented a new diagram which differs with respect to the composition limits of the 8 field from the others proposed by these authors. The purpose of the present investigation was to determine the boundaries of the d phase field. Experimental Procedures and Results Alloys—Buttons, weighing 80 g of 15 different alloy compositions were prepared by arc melting Mal-linckrodt uranium and iodide-process zirconium in a water-cooled crucible. A controlled atmosphere of argon and helium was maintained in the furnace. Prior to making each button, a sacrificial button of zirconium was melted to increase the purity of the furnace atmosphere. Each alloy was then melted six times to improve its homogeneity. Subsequently the alloy buttons were jacketed in copper and hot rolled to slabs at 775°C. From these slabs, specimens were machined for chemical, thermal, and metallographic analyses, Table I gives both the estimated chemical composition of the alloys, and the values which were obtained by analysis. The oxygen contents varied from 0.013 to 0.032 pet, nitrogen from 0.0014 to 0.014 pet, and carbon from 0.0013 to 0.011 pet. The purity of the alloys ranged from 99.947 to 99.975 pet. Thermal Analysis—The specimens for thermal analysis were blocks 11/4 x 1/4 x % in. The bead of a calibrated thermocouple was placed between two of these blocks and molybdenum wire was wrapped around the assembly. Each assembly was sealed in a quartz capsule having an argon atmosphere. The capsule was placed inside a refractory crucible which was heated in a furnace. Using a method described by Smith,' the emf of a differential thermocouple, with junctions inside and outside of the refractory crucible, was used to activate the

Jan 1, 1959

By David B. Reger

The substantial expansion of previously discovered gas pools was the principal feature of petroleum activity in West Virginia during 1940. At least one new gas pool was discovered and various other successful wildcat completions may prove to be gas-pool openers. Some slight extensions of oil pools were also made. The new productive territory, principally gas, added by these extensions was approximately 33,800 acres. ' In general, oil activity was slight because of unfavorable crude prices. Gas activity, on the contrary, increased considerably, although the price of gas did not materially change. The account of operations, as gathered from trade journals and other reporting services, shows that 709 new wells were drilled, resulting in 102 new oil wells with I055 bbl. of daily new produc-tion; 468 new gas wells with 633>g47,000 cu. it. of daily open flow; and 139 dry holes. Also, 91 old wells were drilled to deeper sands, with 143 bbl. and 44,833,000 cu. ft. of added production. On the new wells the oil average was 10.34 bbl, per well per day; and the gas average was 1,354,000 cu. ft. per well per day. On new wells the ratio of dry holes to completions was 19.61 per cent. On deeper drilling to other sands the ratio of failures was 12.I per cent. From an exploratory standpoint, one strictly new gas pool (Lorentz) was opened in Upshur County. Little forecast of its extent or reserve can now be made. The new extensions of various other previously discovered pools, however, give assurance of a new gas reserve that will equal approximately a year of gas demand. In addition to these definite supplies two widely separated Oriskany sand (L. Dev.) wildcats in Jackson County, one of which was completed late in 1940 and the other early in 194.1, may indicate two separate pools or may greatly extend known pools. In south-ern Kanawha County, also, an old Oris-kany-sand well deepened to the White Clinton sand (Sil.) showed a volume of 733,000 cu. ft. and rock pressure of 1800 Ib., giving rather clear assurance that this deep sand, in which only slight quantities of gas had previously been found, should eventually supply much new gas. On the other hand, various deep tests to the Oriskany sand in Harrison, Putnam, Randolph and Wood Counties were totally dry or gave only small volumes of gas, The principal oil wells completed, by counties, were: Calhoun, 15; Clay, Ir; Pleasants, 14; Ritchie, 15; and Roane, 7. Production for the year was estimated by the U. S. Bureau of Mines as 3,444,000 bbl., as compared to 3,684,000 bbl. in 1939. The leading counties in gas-well completions were: Boone, 36; Braxton, 17; Cabell, 25; Calhoun, 16; Clay, 22; Gilm.er, 47; Jackson, 38; Kanatvha, 77; Lincoln, 18; Putnam, 32; IGtchie, 40; and Wayne, 31, Production for the year is estimated by me as I70,000,000,000 cu. ft. as compared to I59,226,000,000 cu. ft.* in 1939. No long pipe lines were built but various gas-line extensions and cross connections,

Jan 1, 1941

By N. J. Themelis, A. W. Last

Autogenous grinding, broadly defined as the self-comminution of ore in a cylindrical tumbling mill without using auxiliary grinding media, was first applied in the early 1930s in the so-called Hadsel mills (Hardinge, 1955) as seen in [Fig. 1], mainly used in gold mines on the US West Coast. A number of these mills were built in sizes of 6.1 to 7.3 m (20 to 24 ft) in diameter and 1.5 to 1.8 m (5 to 6 ft) in length but were later abandoned because of operating and maintenance problems. Further development of autogenous grinding led to the Hardinge wet grinding mill, the Aerofall dry grinding mill, and others. A tabulation of all known autogenous and semiautogenous installations around the world was sent recently to the authors by G. J. Kushner of Koppers Metal Processing Division. In the size range of 7.3 to 9.8 m (24 to 32 ft) in diameter, it lists a total of thirty mills used in the processing of copper ores. An additional 120 units are listed in the same size range for the processing of iron ores and other minerals. The largest mills in existence are 11.1-m-diam X 4.6-m-long (36-ft-diam X 15-ft-long) mills in Minnesota, powered by 8950 kW (12,000 hp) motors and used in taconite beneficiation. It is indicative of the phenomenal growth of this technology that none of the above 150 mills was in operation prior to 1964. Grinding rates in autogenous mills are very sensitive to variations in ore breakage characteristics and even with fairly constant ore type can exhibit large fluctuations in throughput. Autogenous grinding also depends on availability of a fraction of the ore to be ground in the form of "competent" rock which can withstand to a certain degree the tumbling and impact action within the mill. If the ore is uniformly "soft", it will soon be crushed into small size particles and further grinding, which depends on the existence of large size rocks in the mill, becomes impossible. This apparently is the case with most copper ores, as discussed by Bachman, Last and Nabbs (1970) who described pilot testing of a large number of ore samples from Kennecott 's Chino Mines. Under circumstances where autogenous grinding is impractical, it is possible to realize most of its benefits by utilizing large grinding balls in place of the "competent" rock and practice what has become known in the mining industry as semiautogenous grinding. In semiautogenous grinding (SAG), a grate discharge tumbling mill is fed the product of a primary crusher or run-of-mine rock. Forged steel or alloy grinding balls, in proportions ranging from 3.10% of the total volume in the mill, are used to complement the self-grinding ability of the ore. Semiautogenous circuits can be either designed for single-stage closed-circuit grinding which produces a final product for recovery processes, or for two-stage operation in which the SAG mill product is fed to a second stage of grinding in a conventional ball mill.

Jan 1, 1981

By David B. Reger

The substantial expansion of previously discovered gas pools was the principal feature of petroleum activity in West Virginia during 1940. At least one new gas pool was discovered and various other successful wildcat completions may prove to be gas-pool openers. Some slight extensions of oil pools were also made. The new productive territory, principally gas, added by these extensions was approximately 33,800 acres. ' In general, oil activity was slight because of unfavorable crude prices. Gas activity, on the contrary, increased considerably, although the price of gas did not materially change. The account of operations, as gathered from trade journals and other reporting services, shows that 709 new wells were drilled, resulting in 102 new oil wells with I055 bbl. of daily new produc-tion; 468 new gas wells with 633>g47,000 cu. it. of daily open flow; and 139 dry holes. Also, 91 old wells were drilled to deeper sands, with 143 bbl. and 44,833,000 cu. ft. of added production. On the new wells the oil average was 10.34 bbl, per well per day; and the gas average was 1,354,000 cu. ft. per well per day. On new wells the ratio of dry holes to completions was 19.61 per cent. On deeper drilling to other sands the ratio of failures was 12.I per cent. From an exploratory standpoint, one strictly new gas pool (Lorentz) was opened in Upshur County. Little forecast of its extent or reserve can now be made. The new extensions of various other previously discovered pools, however, give assurance of a new gas reserve that will equal approximately a year of gas demand. In addition to these definite supplies two widely separated Oriskany sand (L. Dev.) wildcats in Jackson County, one of which was completed late in 1940 and the other early in 194.1, may indicate two separate pools or may greatly extend known pools. In south-ern Kanawha County, also, an old Oris-kany-sand well deepened to the White Clinton sand (Sil.) showed a volume of 733,000 cu. ft. and rock pressure of 1800 Ib., giving rather clear assurance that this deep sand, in which only slight quantities of gas had previously been found, should eventually supply much new gas. On the other hand, various deep tests to the Oriskany sand in Harrison, Putnam, Randolph and Wood Counties were totally dry or gave only small volumes of gas, The principal oil wells completed, by counties, were: Calhoun, 15; Clay, Ir; Pleasants, 14; Ritchie, 15; and Roane, 7. Production for the year was estimated by the U. S. Bureau of Mines as 3,444,000 bbl., as compared to 3,684,000 bbl. in 1939. The leading counties in gas-well completions were: Boone, 36; Braxton, 17; Cabell, 25; Calhoun, 16; Clay, 22; Gilm.er, 47; Jackson, 38; Kanatvha, 77; Lincoln, 18; Putnam, 32; IGtchie, 40; and Wayne, 31, Production for the year is estimated by me as I70,000,000,000 cu. ft. as compared to I59,226,000,000 cu. ft.* in 1939. No long pipe lines were built but various gas-line extensions and cross connections,

Jan 1, 1941

• As part of $850,000 granted by the House Appropriations Committee for development of manganese in the U.S., the Bureau of Mines will build a pilot plant at Artillery Peak, Ariz., for development of low grade manganese ores. • The historic Argo tunnel and mill in Idaho Springs, Colo., will reopen shortly for the mining of uranium. The Uranium Co. of America has acquired control of the tunnel and mill and 12 nearby mining properties. J. H. Rodgers and G. C. Ridland will manage the operation. •The opening of a new 4000-ton per day coal mine in Washington Co., Pa., and the reopening of another mine of the same capacity in Fayette Co. has been announced by the H. C. Frick Coke Co. They'll help meet added war demands. •A 7000 bbl per day commercial synthetic liquid fuel plant, making gasoline from natural gas at Brownsville, Texas is being operated by the Carthage Hydro-col Corp., a Texaco subsidiary. The gasoline is produced by the Hydrocol process, chemically similar to the Fischer Tropsch process, but differing mechanically in several ways. To operate the process it has been necessary to build an oxygen plant producing 95 pct pure oxygen in quantities equal to U. S. production of commercial oxygen in 1946. •Over 96 pct of the class of 1950 at Montana School of Mines are now employed,, in industry, and they're scattered from MIT to the island of Cuba., • Cobalt, heretofore almost entirely imported, will soon be produced in Idaho. The Calera Mining Co. is building a 600-ton mill in which a cobalt and copper concentrate will be obtained from Idaho ores. •Plans for mining iron ore on the Conarky Peninsula in French Guinea, (an ECA project) call for equipment purchases as follows: 8 wagon drills, electric shovel for mining, conveyor for the port, 8 trucks, wrecker, 2 tractors, as well as miscellaneous accessories and spare parts. •A low-grade lead-zinc mineralization, located east of any known ore bodies in Utah's East Tintic district, has been located by a 2000-ft wildcat USGS drill hole. * Higher-than-going rates have been authorized by the Munitions Board for its stockpile program, where domestic production of scarce materials is low or uneconomical. Payment in excess of 25 pct over the foreign price is now permitted. •A new self-centering conveyor roll, developed by Carnegie-Illinois Steel, is expected to revolutionize materials handling. It completely eliminates the necessity for sideguides to keep materials on a conveyor. See P. 1028. •Great Britain's socialized coal industry employs twice as many miners, but produces less than half as much coal as America's coal industry. last year, British mines produced 28 million fewer tons of coal than the output of the same ,mines in 1939. Absenteeism amounted to a big 12 pot of working time. • Labor market conditions have tightened on almost a country-wide scale. Only 4 out of 143 major labor market areas have a substantial surplus -- less than half the total for May. Growing scarcities of skilled labor are in evidence.

Jan 10, 1950

By H. T. Clark

Within the last twenty years at least three sets of lattice constants for the room temperature (alpha, hexagonal close packed) phase of titanium have been reported in the literature. These values, summarized in Table 1, differ one from another by amounts far greater than can be explained on the basis of inaccuracies in parameter measurements. This paper presents new values determined for high purity titanium. It also details the effect of two elements, oxygen and nitrogen, on these parameters and shows that two of the previously reported values are probably in error because of the presence of one or both of these elements in the material used for examination. Preparation of Samples The titanium+ used for this study was prepared by the thermal decomposition of titanium tetraiodide7 on a hot titanium filament. This titanium rod was prepared for X ray examination by melting about 10 g in purified argon in an electric arc furnace on a cold hearth. This cast button was cold rolled to 0.040 in. thick sheet, cleaned, annealed in vacuum at 1000°C and cold rolled to 0.020 in. thickness. About 0.003 in. of surface material was then removed by hand grinding on papers to remove any contamination caused by the rolls and the sample was bent to the radius of the focusing camera. The sample was then vacuum annealed at 600°C, a temperature just high enough to cause recrystallization, producing a fine grained structure. Such a structure is essential in sheet specimens prepared for focusing cameras in order to have a sufficient quantity of grains to develop continuous diffraction lines. The use of sheet specimens rather than powder samples appears to be essential for the X ray examination of titanium. This is because of titanium's exceptionally high gettering power and its rapid absorption of adsorbed gases, water -vapor, and the like at annealing temperatures. While the effect of this contamination may be neglected for sheet specimens, its effect on 200-300 mesh powder is appreciable. Titanium alloys of oxygen and nitrogen were prepared by a technique simi- lar to that described above except that the required amount of the highest purity titanium oxide or nitride available was added prior to melting in the arc furnace. These materials were added by placing them in holes drilled in the titanium. A small weight loss invariably occurs during the melting of these oxygen and nitrogen alloys. This is believed to be due entirely to the loss of some of the powdered compound in the blast of the electric arc, an assumption which is justified on the basis that there is no weight loss during the melting of titanium metal and that wet analyses for nitrogen on representative samples have checked with the calculated analyses when it was assumed that the entire loss during melting was due to the loss of titanium nitride powder. These alloy buttons were reduced to sheet in the same manner as used for the unalloyed titanium. Experimental Procedure A North American Phillips 12 cm diam symmetrical precision focusing vacuum camera and copper radiation

Jan 1, 1950

By W. M. Lehrer

RECENT development of high-temperature brazing alloys has required information regarding the eutec-tic temperature and composition of the Pd-rich section of the Pd-B system.. Literature on this subject was found to be scanty with no complete system yet determined. Buddery and welch1 report an inter-metallic compound occurring in the Pd-B system at 6.33 wt pct B (PdsBz). Another source, Sieverts and Bruning,2 indicates that after annealing at 700°C, a 1.6 and a 2.0 wt pct B alloy were two phase whereas a 0.75 pct B alloy was single phase. Recent work3 using a hot-stage microscope has proposed a eutectic temperature of 743OC. This method utilized the observation of the onset of incipient melting at grain boundaries. The eutectic composition, however, was not determined. METHODS AND PR0CEDURES Five alloys were prepared by triple inert arc-melting high-purity palladium (95.98 pct) with additions of 2 to 6 pct purified amorphous boron. The alloys were crushed within a hardened steel mortar with a steel pestle. The 2 pct alloy, however, was too tough to be crushed in the above manner so was crushed by successive reductions through a rolling mill. Approximately 17 to 18 g of the crushed alloy was used in the thermal analysis. The alloys were melted in pure quartz crucibles. The thermocouple protection tubes were also of quartz and fused along the inside wall of crucibles to prevent floating of the thermocouple. This was an expediency as centering of the thermocouple in the melt would have been preferable. Melting was done in a tube furnace with a slow flow of tank helium maintained as a protective atmosphere. Heating and cooling rates were maintained at 3.5OC per min through the critical temperature ranges by means of a synchronous motor hook-up to a furnace controller. All specimens were heated to 100°C over the indicated liquidus on heating prior to reversing to the cooling cycle. Specimens emerged from the furnace with mirrorlike brightness attesting to the protective quality of the helium atmosphere. Thermal arrests were detected by the differential thermocouple technique using chrome l-alumel couples and nickel as the reference specimen. Arrests were recorded on a Leeds-Northrup automatic X-Y recorder. The specimen temperature and temperature difference were read to + 7.5OC and ± 1.5OC, respectively. These readings were well within the sensitivity of the instrument amplifier. Chromel-alumel couples were used in lieu of Pt-Rh as very few arrests were contemplated in excess of 1200" to 1300°C, the approach of instability. No standardization was performed on these thermocouples subsequent to their use. RESULTS The thermal arrest temperatures obtained are plotted in Fig. 1 as a function of wt pct B. The composition function was obtained by chemical analysis of portions of the specimens after the thermal analysis was completed. The 2 to 6 pct nominal alloys were found to have 1.80, 2.35, 3.65, 4.18 and 5.90

Jan 1, 1960

By T. D. Teimann, R. L. Stone

The rate of extraction of silica from certain Wisconsin and Minnesota taconites was investigated by autoclave digestion in sodium hydroxide solutions over the temperature range from 296° to 416°F. Rates obtained were from 7 to 254 g mol per cm2 per sec giving activation energies from 15,000 to 19.000 cal per mol. Activation energy was found to increase with increase of sodium hydroxide concentration. Digestion of different forms of quartz indicated the rate of extraction to be solely a function of surface area under similar conditions of digestion. The results of an experimental investigation on the caustic extraction of silica from certain Wisconsin and Minnesota taconites were presented in a recent publication.' It was shown that residual concentrates containing as much as 65% iron can be produced by this method. The occurrence of silica as a micro-crystalline variety of quartz with high specific surface area gave correspondingly high mean rates of extraction in solutions of sodium hydroxide. The present paper extends this previous work by presenting the results of a study of the specific rates of extraction of silica from these ores as related to temperature, sodium hydroxide concentration and variety of quartz. Calculated activation energies for the dissolution of silica are presented and some possible mechanisms are discussed. TACONITES The low-grade siliceous iron ores investigated included taconite from the Wisconsin Gogebic range and a semi-taconite2 from the Minnesota Mesabi range. These are adequately described in the former paper1 and by the U. S. Bureau of Mines. The principal iron minerals are hematite (Fe2O3) and goethite (Fe2O3 . H2O), while the gangue is essentially a microcrystalline variety of quartz. Minor amounts of other minerals are present. Typical analyses show the Wisconsin taconite to contain approximately 28% Fe and 54% SiO2 and the Minnesota semi-taconite 39% Fe and 39% SiO2. Analyses of the actual samples used are given in Table I. The taconite samples were prepared for digestion by reducing the original ore to minus 200 mesh in a Braun pulverizer. QUARTZ Three varieties of quartz were studied in the investigation: Ottawa sand, chert and chalcedony. The Ottawa sand was obtained from the Ottawa Silica Co. The chert and chalcedony came from Wards Natural Science Establishment. A minus 200 plus 400 mesh fraction of the Ottawa sand, used as a surface area standard, was repeatedly washed in hot concentrated hydrochloric acid followed by distilled water before autoclaving. The other two varieties were used directly after grinding through 200 mesh in a laboratory hammer mill. Analyses of these samples appear in Table 11. Microscopic examination of the silica samples by the oil immersion method showed that the Ottawa sand consisted of clean, uniform spheres of quartz with little deviation in size from a mean diameter of 82µ determined by a distribution count. The other two varieties consisted almost entirely of microcrystalline aggregates of quartz crystals; the aggregates ranged from 10 to 70µ. The individual crystals in the chert aggregates were estimated to be of the order of

Jan 1, 1964

By John T. Galey

A combination of two factors in addition to the current Federal drilling and price regulations reduced by 120 from I942 the number of new wells completed in southwestern Pennsylvania during the year. No new prospective area was found comparable to the Armbrust gas pool, Westmoreland Co., which accounted for a seventh of the last year's drilling, and it is considered doubtful whether, even if such a field had been discovered, the drilling contractors, who have been seriously affected by the manpower shortage, could have drilled many more wells than they did during the year. New wells totaling 445 were completed for a combined footage of over 1,250,000 Dry holes numbered 131 and had a footage of nearly 400,000. Old wells drilled deeper total 55, of which 17 were found nonproductive. Shallow Development Oil Oil completions yielded an initial of only slightly over one hundred barrels from 21 wells for about the same per well average as that of a year ago. However, 65 bbl. of this total came from two wells in two new strikes. The footage drilled of nearly 33,000 gives an average of nearly I00 ft. less per well than a year ago. Two old wells drilled deeper had a combined initial of only 4 bbl. The largest oil well of the year, 40 bbl., was found in the Speechley (U. Dev.) sand at a depth of 3492 ft. in German township, Fayette County. The location is several miles east of the nearest oil production hut as the area that could be occupied by a pool is fairly well delimited by drilling, the extent of this production would not appear to be large. The other notable oil production was found in the Dunkard (Penna.) sand, Cumberland township, Greene County, at a depth of 1065 ft. Here the first well had an initial of g bbl. and the second 25 bbl. However, a third proved dry, and as this area is also delimited by drilling, the pool doubtless will be of small area. Gas Gas completions yielded an initial of slightly over one hundred million cubic feet per day and new wells, totaling 303, account for all but four million of this volume. Old wells drilled deeper, numbering 35, found gas. The per well average in new drilling of approximately 320 M cu. ft. is nearly 165 M cu. ft. less than a year ago and the total footage is slightly over 830,000, which is about a quarter of a million feet less than in 1942. Average rock pressure of new completions is approximately 365 lb. per sq. in. The entire volume of new production is from the Upper Devonian or higher stratigraphic horizons. In Allegheny County, the grestest activity was in Forward and Plum townships. Wells there account for more than one half the completions. One large well was drilled in Forward township and an open flow of 3.623 million cubic feet was found in an old Gantz (U. Dev.) sand area. The top of the sand was encountered

Jan 1, 1944

By H. I. Aaronson, C. Wells

THIS is a preliminary report on a detailed metal- lographic investigation of the bainite reaction in a plain carbon hypoeutectoid steel. In view of the current interest in the bainite reaction and of the controversies which still exist about even the basic phenomenology of this mode of transformation, it was considered desirable to present a summary of the more important results obtained to date prior to the completion of this investigation. The steel used contained 0.29 pct C, 0.76 pct Mn, 0.25 pct Si, 0.005 pct P, and 0.007 pct S. The alloy was homogenized for 48 hr at 1250°C. Individual specimens were then austenitized for 30 min at 1300°C and isothermally transformed for various times at temperatures above and within the bainite region, ranging from 775" through 500°C at intervals of 25°C. These specimens were carefully examined on a research metallograph; a few specimens of especial interest were also studied electron microscopically.' Bainite may be defined as the aggregate structure resulting from the precipitation of carbides from supersaturated ferrite which formed by nucleation and diffusion-limited growth. Two groups of experimental observations made during the present study provide support for this mechanism of the bainite reaction: 1—at 625°C, partial conversion of pro-eutectoid ferrite to bainite began after more than 99 pct of the austenite had decomposed and 2—the precipitation of bainitic carbides occurred only within the ferrite phase. The proeutectoid ferrite and the bainite reactions in the steel studied were found to be morphologically continuous. Following the classification scheme of Mehl and Dube,2 three principal morphologies of proeutectoid ferrite were identified in the temperature region (625" to 550°C) in which the two reactions blend—grain boundary allotriomorphs," * Grain boundary allotriomorphs are crystals which nucleate at and grow preferentially along matrix grain boundaries. Widmanstaetten side plates, and intragranular plates. Carbide precipitation converted these morphologies into their bainitic equivalents with increasing isothermal reaction time. Conversion took place more rapidly as the reaction temperature was reduced. The replacement of supersaturated ferrite by bainite, however, did not occur uniformly even within individual austenite grains and was noticeably incomplete at higher transformation temperatures, e.g., 625° to 575°C. The ferritic and bainitic forms of a given morphology thus were frequently found to coexist, often inextricably intermixed, in a given specimen. At 625" and 600°C, the conversion of ferrite to bainite was clearly seen to have occurred entirely by the nucleation of carbides at ferrite/ferrite boundaries, as shown in Fig. 1. The nature of the loci at which carbides formed at lower temperatures was often difficult to ascertain with a light microscope, although the alignment in rows of many of the carbides, illustrated in Fig. 2, suggested that nucleation had again occurred at grain boundaries or subboundaries within the ferrite. Application of the electron microscope confirmed this deduction for bainitic structures formed at these temperatures, as shown in Fig. 3. The dense black appearance of bainite formed at very low reaction temperatures in higher carbon steels3 indicates, however, that isolated lattice defects within ferrite crystals prob-

Jan 1, 1956

By R. I. Jaffee, J. W. Roberts, D. N. Williams

DISPERSION hardening as an alloying process has aroused increasing interest in the past few years. This alloying procedure, in which an insoluble phase is dispersed randomly through a metal or alloy, is believed to be especially suited for the attainment of creep strength at elevated temperatures since the dispersed phase is metallurgically stable. Another advantage is that the physical properties of the matrix phase, such as electrical conductivity, remain relatively unaffected by alloying. These two characteristics resulted in interest in the applicability of dispersion hardening to copper and copper alloys. A study of copper alloys prepared by powder metallurgy methods has shown some strengthening from oxide dispersions.' However, powder metallurgy processing would not be economical for large scale production of dispersion hardened copper-base alloys. Therefore, the research described in this article was initiated to examine methods of forming dispersion alloys which would not require powder metallurgy processing. If powder metallurgy processing is to be avoided, a method must be found by which the dispersion material can be introduced into and dispersed through the melt before casting. When the dispersed phase is an oxide or similar nonmetallic, it is extremely difficult to form a satisfactory liquid: solid dispersion since successful mixing requires that the melt wet the dispersed phase. It is almost impossible to force a nonwetted particle beneath the melt surface. This difficulty can be avoided, however, if the oxide particles are produced in molten copper by reaction within the melt. The problem would then reduce to maintaining randomness until solidification. Four procedures were considered for producing an oxide particle within molten copper by reaction. In all cases, the intent was to react oxygen (0) with a reactive metal (X) to form an oxide (XO) within the copper melt. These reactions were as follows: 1) (Cu-X), + (O)g (Cu)1 + (XO)S [1] 2) (Cu-X)1 + (Cu2O)s (Cu)x + (XO)S [2] 3) (Cu-OK)1 + (Cu-X)1 (Cu)1+(XO)9 [3] 4) (Cu-OK)1 +(X)s (Cu)1 +(XO)s [4] The reactions were carried out in an 8-lb melt of 99.98 pct Cu maintained in the vicinity of 2200oF by induction heating. Where possible the amount of the reactants was controlled to give 1 to 5 vol pct oxide. Mechanical stirring during the reaction period was used to minimize agglomeration of the reaction product. The presence of a reaction product was determined metallographically by study of an ingot cast from the melt at the end of the reaction period. Reaction [I] was studied by dissolving aluminum in the melt followed by forcing oxygen through the melt. The melts became quite sluggish during the reaction period suggesting that A12O3 was formed. However, the reaction product rose out of the melt rapidly, possibly due to the flushing action of the oxygen stream, and little dispersed phase was formed. Reaction [2] was examined by dissolving aluminum, silicon, or nickel i; the melt and then adding Cu20 (melting point 2250F). This procedure was unsuccessful. Although Cu2O was easily stirred into cop-

Jan 1, 1961