Search Documents

ASIDE from the John Fritz Medal, in which the Institute participates through its representation on the John Fritz Medal Board, the Institute itself has four awards it may make annually, as follows : the Robert W. Hunt Medal and Prize, the J. E. Johnson, Jr., Award, the James Douglas Medal, and the William Lawrence Saunders Medal. ROBERT W. HUNT MEDAL AND PRIZE The partners of Robert W. Hunt established a fund which was presented to the Institute at a fitting ceremony on May 27, 1920, to establish an annual medal and a sum of money to be awarded under the following rules 1. The award shall consist of two prizes: first of a gold medal, second of a sum of money; a certificate to accompany each prize, The money prize shall not be awarded to a member over 40 years of age, but under unusual circumstances, both prizes may be allotted to one person provided that he is not over 40 years of age. In general it will be understood that the Committee shall award the money prize to the younger men, rather than the medal. 2. The awards shall be made not oftener than once a year to that person or persons contributing to the Institute the best original paper or papers on iron and steel. The scope of the term "iron and steel" shall be determined by the sub-committee considering the awards. In general, papers dealing with the practical side of the subject have preference over those dealing with the theoretical side in recognition of the fact that Captain Hunt's main contributions to the industry have been in the improvement of production and quality of material. 3. A sub-committee of three to five, including the Chairman of the Iron and Steel Committee, shall be appointed by the Iron and Steel Committee annually to adjudge the award subject to approval. 4, The awarding committee shall submit its report to the Iron and Steel Committee at its October meeting, and the award shall be certified to the Secretary of the Institute in time to permit the presentation to be made at the Annual Meeting of the Institute, 5. The recipient of the award shall be designated "The Hunt Medallist," This prize is administered by the Iron and Steel Committee. Awards of the medal have been made as follows 1920-Robert Woolston Hunt. 1926-Charles Lewis Kinney, Jr. J. E. JOHNSON, JR., AWARD This award is made from the income of a fund of $3000 donated by Mrs. Margaret Hilles Johnson in memory of her husband, J. E. Johnson, Jr., who was a prominent engineer, author of two valuable volumes on iron blast-furnace construction and practice, vice-

Jan 1, 1928

By M. D. Hassiallis

The claim is made in a number of patents1'2'3'4 that some compounds of the class known as aryl sulphides have collector properties. One of these patents generalizes the claim to include all aryl sulphides, whose generic formula is R-S2-R' (where x = 1,2, . . . ), with the restriction that if the aromatic radicals R, R' contain substituent groups these groups may not contain nitrogen or oxygen. Moses, Hess, and Perkins cite as evidence for their claims the results of flotation tests on Anaconda and Miami copper ores using diphenyl sulphide, ditolyl disulphide and dinapthyl disul-phide as collectors. The use of alkyl sulphides as collectors has also been reported5 with the conclusion that the alkyl sulphides are better collectors than the corresponding aryl sulphides. The experimental work cited appears to confirm this contention. In order to test these claims with respect to diphenyl sulphide, a sample, purchased from the Eastman Kodak Co., was tested against Anaconda ore. The procedure followed. was that of Moses, Hess, and Perkins. A sample of ore weighing 500 • grams was placed in a laboratory ball mill. To this was added 220 grams of water, 0.06 grams of commercial diphenyl sulphide (1/4 lb. per ton of ore), and 0.8 grams of lime (3 lb. per ton of ore). The material was ground until 93 per cent passed a 65-mesh screen. This pulp was diluted to 16 per cent solids. A sample of the diluted pulp was placed in a Minerals Separation type of laboratory flotation cell. After a a-min. agitation period, pine oil was added and the froth collected for a period of 15 min. This test recovered 68 per cent of the copper, with a ratio of concentration of 6.8:I. The tailing assay was 0.3 per cent Cu. Moses, Hess and Perkins attained a recovery of 75 per cent, with a ratio concentration of I2:I. Although these results do not compare too well with those of Moses, Hess and Perkins, subsequent tests showed an improvement, as judged by vanning of the tails. It is concluded, therefore, that the patent results are confirmed. Contact-angle Tests In order to study the response of the various minerals, found in Anaconda ore, to commercial diphenyl sulphide, some contact-angle tests were made. Polished particles of bornite, chalcodte, chalco-pyrite, pyrite and quartz were conditioned for 15 min. in a suspension of diphenyl sulphide in water. The concentration of this suspension was 0.284 grams per liter, this being the concentration of this reagent in the ball mill. The conditioned particles were rinsed with water (not rubbed with filter paper or boiled linen) and then tested against an air bubble in the bubble machine, with the following results: born-

Jan 1, 1943

By Suresh P. Babu, Joseph W. Leonard

The ultimate objectives of comminution should be to reduce material to some specified size while producing a minimum of undersize or fines, with less power, higher throughputs, and with more compact machinery. Attempts to achieve these objectives have been only partially successful, since gains in some areas are achieved at the cost of concessions in other areas. An example of some of these trade-offs can be found in the closed circuit crushing operations of the anthracite and crushed stone industry where, in order to produce a minimum of unprofitable fines, unfavorable concessions must be made in the size of the crushing facility where 2 or more crushing stages are interphased by 2 or more screening operations. This paper discusses experiments with a new process which attempts to achieve some, if not all, of the comminution objectives in a single pass operation without undesirable concessions; or, at the very least, to achieve more than is possible with systems in use today. These objectives are sought by use of water-flushing to enhance comminution. The crushing of coal and other minerals is a mature technology that is long overdue for a careful re-examination. Crushing of coal is generally achieved through the use of rotary breakers and roll crushers. Water-flushing, as envisioned here, appears to have potential application in the following areas: 1) For primary raw coal crushing or for secondary crushing of rotary breaker products. 2) For use as a size reduction and/or concentrating step for crushing coal mine refuse from present production or from existing refuse dumps. 3) For possible future application in underground preparation interphased with continuous mining machinery. Size reduction with conventional methods is known to be an inefficient operation when the increase in surface energy of the material crushed is compared with the input energy. A simple breakdown of the energy consumption in size reduction, given by Orr, is shown in [Fig. 1]. It is believed that most of the energy supplied is lost in the form of interparticle friction.2 Hence, the removal of fines immediately after their formation or the implementation of steps to prevent their formation, based on reduced friction, will reduce the energy requirements of the communition operation.3 A detailed discussion of the mechanism of size reduction is available in other literature.3-5 Even though the closed circuit crushing operation is designed to carry the fines away from the crushing zone, it is still inadequate for instantaneous removal of fines. The present investigation advocates the use of a flowing liquid medium to remove the crushed product immediately after size reduction. Unlike the wet-grinding methods, no constraints are required for the liquid flow rate, and, also, the liquid medium can be used in primary crushers like jaw crushers, hammer mills,

Jan 1, 1978

By H. S. Rankin, E. C. Houston

OLIVINE is considered a valuable potential source of metallic magnesium in the chloride electrolytic process. Treatment of olivine with hydrochloric acid can be carried out under conditions that prevent the formation of gelatinous silicic acid, which would inhibit the reaction by forming a covering around the ore particles. It is our hypothesis that the formation of gelatinous silicic acid is avoided by the dehydrating action of the magnesium chloride, which takes up water to form a series of hydrates and leaves the silicic acid in granular condition. Leaching serves to separate the magnesium chloride from the silicic acid and unattacked ore, which can be treated with fresh acid in successive steps until extraction is essentially complete. The leach solution can be purified by the addition of caustic magnesia and the precipitated impurities removed by decantation or filtration. The resulting magnesium chloride contains: Fe, less than 0.001 per cent; Mn, 0.012 per cent; Ni, none. Chlorination[f] of olivine has two major defects: (1) a large part of the chlorine goes to form silicon and iron chlorides, (2) the anhydrous magnesium chloride is held by absorption in the finely divided silica. SUPPLY It is well known that olivine, a silicate of magnesium and iron, is present in large amounts in several localities in the United States. The largest deposits occur in the southeast and on the Pacific Coast.1 The southeastern deposits were surveyed by Lewis2 in 1896 and by Hunter3 in the period 1933-1940. It is estimated that high-grade olivine, conveniently located with regard to transportation and power, is present in excess of 230 million tons above local drainage level in western North Carolina and north Georgia. PREVIOUS TECHNICAL WORK In the past few years, olivine has attracted considerable attention in the refractory field. In the chemical processing industry, however, it has long been thought axiomatic that the cost of processing silicates is an economic barrier to their utilization, especially where more reactive minerals, such as carbonates, oxides or salts, are available. This attitude is not entirely justified in connection with olivine. Unlike most silicates, olivine is readily attacked by acids, chlorine and other reagents without resorting to fusion to break down the silicate structure. Olivine has been suggested as a raw material for making epsom salt by roasting with pyrites.4 Other processes include acid treatment5 and digestion with calcium chloride.6 Recently a small plant was built near Webster, N. C., for making epsom salt from olivine by treatment with sulphuric acid. This plant is now in commercial operation, producing approximately two tons per day. Olivine is also receiving attention from the fertilizer industry as an inexpensive source of soluble magnesium.

Jan 1, 1942

By R. Scot Clark

The reactively sputtered silicon dioxide capacitor -was developed for use in the monolithic integrated circuit, thereby requiring the capacitor to be fabricated on an oxidized silicon slice. The silicon dioxide film is formed by reactively sputtering silicon in a 50 pct Ar-50 pct 0, atmosphere and the physical properties are indistinguishable from silica. A practical upper limit of capacitance per unit area of 0.25 pf per sq mil is reached with the capacitors fabricated from the Si0, film. Methods shown to enhance this value are double stacking the thin-film capacitors and addition of aluminum to the silicon cathode during sputtering to form an aluminosilicate dielectric. A major contribution to the field of diffused integrated circuits would be the addition of auxiliary passive devices for replacement of diffused passive devices which are currently being fabricated for many integrated circuits. This accomplishment would increase the flexibility of the diffusion process in order to concentrate more on transistor parameters rather than on fabricating diffused resistors and capacitors. To pursue this technique, a thin-film SiOz capacitor was developed which has _ proven applicable to many integrated circuits. Although the SiOl capacitor has an application, the major deterrent from extending the integrated circuit into many useful areas such as low-frequency linear application is the low dielectric constant of SiO, and the low usable capacitance in an integrated circuit. This paper will cover the sputtering techniques used for forming the SiO, film, the physical and electrical properties of sputtered SiO,, and yield information concerning the application of these capacitors to integrated circuits. REACTIVE SPUTTERING Reactive sputtering is simply the sputtering of a metal or semiconductor in glow discharge in the presence of a reactive gas. The material to be sputtered is seen in Fig. 1 as the cathode of the system and is bombarded with positively charged ions of the ambient gas. In this investigation, the ambient gas is composed of 50 pct Ar and 50 pct O2 at a pressure of approximately 2.5 X l0-' Torr. The ions are accelerated toward the cathode in the cathode dark space by the electric field and upon striking the cathode effect a momentum energy transfer to the surface atoms. The transferred energy is sufficient to dislodge a surface atom or atoms and these particles diffuse through the glow discharge to the collector or anode. Several mechanisms of oxidation in the reaction chamber can be considered during reactive sputtering. 1) The surface of the cathode is oxidized and the oxide is subsequently sputtered. 2) Oxidation and sputtering occur simultaneously. 3) Sputtering of the cathode material is followed

Jan 1, 1965

The great Bingham Canyon mine and mill complex of Magna, Arthur, and Bonneville had their beginning in a 300 ton per day operation which was commenced by Daniel C. Jackling and his associates in 1904 as the Utah Copper Company. This small plant was quickly expanded to 500 tons per day and eventually Kennecott, the Utah Copper successor, was processing about 45,000 tons per day of ore in each of its mills, Magna and Arthur. Finally, in 1966, the Bonneville crushing and grinding plant was added to produce a slurry of ground ore for flotation concentration at the expanded Magna and Arthur mills. Bonneville is one of the few railroad dump primary gyratory crushing plants constructed in recent years; another which is described in this Monograph is Cuajone in Peru, started in 1976. Two others are the Climax Henderson unit and the Phelps Dodge Tyrone crusher, which has been fed by trucks since it commenced operation. The Bonneville, Henderson, and Cuajone crushers are all located considerable distances from their mines, hence the use of rail haulage. Shovels in the Bingham pit are 8 to 15 yd capacity; and ore is sent to the Bonneville crusher in 100 ton rail cars, where they are dumped, two at a time, by a hydraulically driven rotary dumper. Ahead of the 54 in. by 74 in. Allis-Chalmers gyratory are two grizzlies, each 27 ft 9 in. (8.46 m) long with bar spacings of 4 ½ in. (114 mm) at the feed end and 6 in. (152 mm) at the discharge end. Grizzlies are sloped at 38. Oversize rocks are re- moved from the crusher pocket by an overhead crane, and the crusher produces a nominal 6 in. (152 mm) product. Rail cars are dumped in the direction away from the crusher, and water sprays at the dumper level and in the rock boxes are used for dust suppression. There are two 72 in. by 19 ft (1.83 m by 5. 8 m) apron feeders under the 500 st cr'ushed ore pocket and two more under the grizzly undersize pocket. Feeder speeds are variable up to 72 fpm. Grizzly undersize is dropped to the feeder pocket by three shelves forming a rock ladder attached to the pocket walls. Each pair of apron feeders, one for crushed ore and one for grizzly undersize, discharge to a 72 in. (1. 83 m) picking belt for tramp removal; this belt feeds one of two 54 in. (1.37 m) feeder conveyors which in turn discharge to a 60 in. (1. 52 m) takeaway belt operating at 175-300 fpm (53.3 - 97.4 mpm). Both picking belts are equipped with metal detectors and tramp iron magnets, and a separate 30 in. (760 mm) conveyor is used to remove tramp material.

Jan 1, 1978

By M. R. Hatfield, F. J. Vosburgh

In a recent article, it was shown that in the blast furnaces in Germany that are lined with carbon blocks no cooling plates are used, and that shower cooling is employed on the hearth and bosh sections. While one of the authors was in Germany he was told that one furnace was being operated without even the shower cooling on the bosh section, though the hearth section was shower-cooled. In discussion of this interesting situation with a number of blast-furnace operators in this country, it was made clearly and promptly evident that shower cooling was very unpopular, probably because of its messiness and its ineffectiveness. Both of the causes for the dislike of shower coolings are reasonable ones. Shower cooling can be and frequently is messy, but the present cooling of blast furnaces leaves much to be desired on that score. Shower cooling is ineffective as compared with plate cooling, so far as its usefulness in keeping the bricks cool enough not to melt or fall to pieces is concerned. However, the introduction of carbon linings changes the situation. No one is concerned with keeping a carbon lining cool, for no temperature in the blast furnace has any effect on carbon, which is just as stable at 3000°F. as it is at 70°F. The only concern is for the shell—to keep it cool enough for safety and comfort— and for that shower cooling is sufficient. Of course, with only the shell to cool, instead of the shell plus all the refractory material, much less water would be required, and the necessity for constant attention to the flow would be lessened, as the hundreds of inlets and outlets would be eliminated. Probably half of the water used in cooling a blast furnace is used for cooling the shaft and tuyeres and the remainder for the bosh and hearth sections. However, in view of the dislike of shower cooling in the United States, and particularly because at least one German blast furnace is operated with no cooling of the bosh section, thought was given to the possibility that a carbon-lined blast furnace might be operated without any cooling of the entire carbon-lined portion. For that reason a series of experiments was performed to determine what might be the temperature of the shell of a blast furnace protected by a carbon lining and operated under varying conditions up to a maximum inside temperature of 3000°F. Experimental Procedure A schematic diagram of the experimental setup is shown in Fig. I and a photograph of the entire assembly in Fig. 2. The heating element was a a tubc nominally 25/8 in. 0.d. by 2 in. i.d. by 30 in., used as a resistor. Power was furnished by a I5-kva. transformer operating

Jan 1, 1942

By M. R. Hatfield, F. J. Vosburgh

In a recent article, it was shown that in the blast furnaces in Germany that are lined with carbon blocks no cooling plates are used, and that shower cooling is employed on the hearth and bosh sections. While one of the authors was in Germany he was told that one furnace was being operated without even the shower cooling on the bosh section, though the hearth section was shower-cooled. In discussion of this interesting situation with a number of blast-furnace operators in this country, it was made clearly and promptly evident that shower cooling was very unpopular, probably because of its messiness and its ineffectiveness. Both of the causes for the dislike of shower coolings are reasonable ones. Shower cooling can be and frequently is messy, but the present cooling of blast furnaces leaves much to be desired on that score. Shower cooling is ineffective as compared with plate cooling, so far as its usefulness in keeping the bricks cool enough not to melt or fall to pieces is concerned. However, the introduction of carbon linings changes the situation. No one is concerned with keeping a carbon lining cool, for no temperature in the blast furnace has any effect on carbon, which is just as stable at 3000°F. as it is at 70°F. The only concern is for the shell—to keep it cool enough for safety and comfort— and for that shower cooling is sufficient. Of course, with only the shell to cool, instead of the shell plus all the refractory material, much less water would be required, and the necessity for constant attention to the flow would be lessened, as the hundreds of inlets and outlets would be eliminated. Probably half of the water used in cooling a blast furnace is used for cooling the shaft and tuyeres and the remainder for the bosh and hearth sections. However, in view of the dislike of shower cooling in the United States, and particularly because at least one German blast furnace is operated with no cooling of the bosh section, thought was given to the possibility that a carbon-lined blast furnace might be operated without any cooling of the entire carbon-lined portion. For that reason a series of experiments was performed to determine what might be the temperature of the shell of a blast furnace protected by a carbon lining and operated under varying conditions up to a maximum inside temperature of 3000°F. Experimental Procedure A schematic diagram of the experimental setup is shown in Fig. I and a photograph of the entire assembly in Fig. 2. The heating element was a a tubc nominally 25/8 in. 0.d. by 2 in. i.d. by 30 in., used as a resistor. Power was furnished by a I5-kva. transformer operating

Jan 1, 1942

By Don M. Jackson

The techniques for the growth and controlled, graded doping of silicon epitaxial overgrowth layers were established. Grading of- impurities such as arsenic or boron in arbitrarily chosen profiles oiler four orders of magnitude (from I X 10Lg to 1 X 10L5 cm) was accomplished. The graded structures were grown in a stepwise manner where in the profiles were approximated by growing many separate layers with small doping-level changes between layers. Masked-area growth of silicon through windows in a SiO2 masking film was acconiplished through the simultaneous injection of HCl gas 102th Sic14 in the epitaxial reactor. The HCl served to inhihit the growth of silicon on the Sz02 surface, and also to control the cross-sectional profile of the silicon mesas. silicon from the substrate was etched out through the windows, and then epitaxial material was used to fill the holes hack in to form planar diodes. Simullaneous HCl injection was adapted to control the cross-section profile of the hack-filled regions. Arsenic-huried regions beneath in te- In recent months, the epitaxial growth process in semiconductor materials technology has evolved into a complex system directed at both material improvement for better monolithic integrated-circuit characteristics and the development of new silicon structures for future integrated-circuit needs. The advent of high-temperature HC1 gas etching1 grated-circuit transistors reduced V(SAT) by slightly more than one third, bringing this parame-ter to that of an isolated component transistor. When arsenic was diffused into the starting sub-stvate, it was necessary to remove any excess arsenic in order to avoid excessive audodoping of the subsequent epitaxial layer. Oxide isolation of single-crystal regions in a substrate provided complete electrical isolation of integrated-circuit components, thereby eliminating parasitic capacitance which is inherent in standard integrated-circuit processing. The process involved the etching of deep mesas on silicon Wafers, the formation of an oxide over the mesa surface, and then the deposition of several mils of polycrystalline silicon over the oxide. The original substrate was lapped and polished allay until the mesas were left isolated in the polycrys-talline matrix. The Final components were fabri-cated in the single-crystal islands. Speed and power-handling capabilities of standard circuits were improved through the process. wherein work-damaged material is removed from the surface of the silicon wafer just prior to the silicon deposition step has made it possible to grow silicon films with structural quality that approaches that of the substrate. HBr used in the same volume ratio as HC1 etches silicon at the same rate and with the same results as HC1. Recent developments in epitaxial materials technology have occurred in the areas of precise doping control, buried prediffused regions between over-

Jan 1, 1965

By H. L. Luo

SYSTEMATIC investigations of the Fe-Ga system have been reported only very recently."' The maximum solid solubility of gallium in a-Fe is nearly 50 at. pet at 900°C. However, from Ref. 1, it was not evident that the a-Fe solid solution could be retained successfully beyond 17.38 at. pet Ga by solid-state quenching. The present investigation reports the retention of a-Fe solid solution at 50 at. pet Ga by quenching from the liquid. An ordered phase of CsC1-type B2) structure was observed between 34 - 50 at. pet Ga. Since it was considered very probable that the CsCl structure would occur at high temperatures, alloy filings were also quenched by the conventional quenching technique. In addition to the CsCl phase, a second ordered phase of BiF3-type (DO3) structure was found in the range 25 - 30 at. pet Ga. Alloys were prepared from elements of 99.99 pet purity or better, induction-melted in alumina crucibles under hydrogen. After reweighing, the alloy ingots were cast into wires under argon. From the weight losses and the reproducibility of the lattice parameters, compositions were estimated to be within ± 0.3 at. pet. The techniques of quenching from the liquid state were reported before.3-5 Prior to quenching, a small section of cast alloy wire (30 - 50 mg) was melted in an alumina insert under an argon flow. The quenched specimens were in the form of flakes, typically 1 sq mm in area. For solid-state quenching, alloy filings passing 200 mesh were sealed under a reduced helium atmosphere in a thin-bottom silica tube. After heating for -30 min at the desired temperature in a vertical furnace, the sealed tube was rapidly dropped into ice water so that the thin bottom of the tube broke on impact. The quenched alloy filings were always ferromagnetic and could be collected by a magnet. X-ray diffraction patterns were taken with iron-filtered cobalt radiation in a 114.6-mm-diam Debye-Scherrer camera. High-angle lines were always resolved and spacings were computed relative to ? (CoKa1) = 1.78890Å. Lattice parameters were obtained from extrapolation against the Nelson-Riley function. The variation of lattice parameter with composition is shown in Fig. 1, together with the data of Dasarathy and Hume-Rothery.1 Uncertainties in the present measurements are within the dimensions of the symbols or indicated by error bars. X-ray diffraction lines indicative of CsC1-type ordering could be clearly identified for alloys of 34 - 50 at. pet Ga quenched from the liquid and alloys of 35 - 41 at. pet Ga quenched from -975°C. Within experimental error, no difference in

Jan 1, 1968

By Jack A. Kanz, Samuel R. Shortes, E. C. Wurst

Zinc diffusion into GaAs from the vapor phase through reactively sputtered SiO, films Izas been inrestigated for various zinc pressures at 1000"C. Diffusions were carried out in evacuated quartz ampules with elemental zinc and with various Zn-Ga alloys. Sputtered films have proved effective in lowering surface concentrations and preventing surface deterioration during diffusion. Approxin.ate complenzentary error-function impurity distributions were found when surface concentrations were reduced to approximately 3 -—4 x 10" atoms cm'3 or less with dilute zinc sources or by diffusion through SiO, films. Zinc difhsions in GaAs tlzrough SiO, films produced more planar diffusion fronts than were observed with uncoated zuafers under identical conditions. A) Surface Deterioration During Diffusion. Device technolorn-- in compound semiconductors has been hampered by several difficult problems not normally encountered with silicon and germanium. 111-V and 11-VI compound semiconductors generally have volatile constituents at temperatures used for diffusion. To achieve specific junction depths in reasonable lengths of time, or to obtain particular impurity distributions and doping levels, it is often necessary to use temperatures which cause surface deterioration and erosion of the wafer. The resultant surfaces are generally unsuitable for devices. The type and extent of surface damage depends to varying degrees on the particular environment of diffusion and on the particular impurity in question. The most common type of deterioration results from simple dissociation of the gallium and the arsenic during diffusin.' The deterioration process is significantly enhanced by thermal gradients in the diffusion zone, usually resulting in vapor transport and condensation at the cooler portion of the system. The resulting damage sometimes appears as a general haziness over the surface or an array of pyramidal etch pits characteristic of the particular orientation. Occasionally, erosion of the surface occurs uniformly over the wafer so that surface loss is not readily apparent. Workers in GaAs usually resort to the sealed-ampule type of diffusion system3"5 rather than the more conventional open system used for silicon and germanium. Another type of deterioration results from direct interaction of the impurity with the surface. The form of deterioration may vary from surface alloying, as in the case of zinc, to direct chemical attack and vapor transport of the reaction products, as in the case of sulfur. Surface alloying with zinc occurs at higher temperatures and source vapor pressures.4 The process is largely controlled by the amount of free gallium on the surface of the wafer in equilibrium with the arsenic lost to the system. The group-VI elements, sulfur, selenium, and tellurium, are commonly used donor impurities for gallium arsenide. These elements are characterized by high vapor pressures and high chemical

Jan 1, 1964

By J. W. Spretnak, V. Kandarpa, G. W. Powell, R. A. Erickson

Neutron-diffraction pattens were obtained at room temperature from two austenitic manganese steels, oxc wth n carbon content of 1.23 zct PC/ and the olher 0.63 wt pct. Analysis of the data showed that the curOan atols (ions) occupy tile octaheadral site. any of the cavbon is in the tetahedral site, tile concentration is too strzall lo be detecled by tzeulr-on d$facton. AS part of a long-range investigation of eutectoid decomposition, a study of the structure of austenite has been undertaken in order to characterize as best as possible the parent phase in the Fe-C system. Austenite is a solid solution of carbon atoms in fcc iron, the carbon atoms being located in interstitial positions. Of the two kinds of interstitial sites, octahedral (0, +, +) and tetrahedral (4, a, $), in this lattice, the larger octahedral sites are usually considered as the probable position of carbon. The strain energy involved in pytting a neutral carbon atom (covalent di; ameter 1.54)' into a tetrahedral site (diameter 0.56A) is considerably greater than that associated with p2tting carbon into the octahedral site (diameter 1.08A). Dayal and arkeen' observed the migration of carbon in iron under the influence of an electric field indicating tha tye carbon is ionized. pe ionic radius of C'4 is 0.15A and that of C" is 0.29. Consequently, it is conceivable that carbon ions could occupy the tetrahedral sites if one considers only the strain energy. Size considerations alone do not provide a complete explanation for the formation of the interstitial solid solutions, however. because metals such as copper, zinc, and cadmium do not appear to form interstitial solid solutions in spite of their large interstitial sites. Evidence which suggests partial ioni-zation of the carbon in austenite has also been obtained by Speiser, Spretnak, and alor who derived formu- lae relating the observed change in lattice parameter to the effective diameter of the solute atom. Assuming the carbon occupies the octahedral site. they computed the effective diameter of carbon to be 1.33A whereas the covalent diameter is 1.54A. petch5 concluded from powder X-ray diffraction experiments that carbon atoms occupy the octahedral sites. His conclusion was based on the general trend observed in the intensity of the diffraction lines as the carbon content of the austenite was increased. However, the major difficulty associated with application of X-ray diffraction to this particular problem is the relatively poor scattering power of carbon. Williamson and smallman' utilized X-ray diffraction to study the line broadening caused by the strain field about carbon atoms inferrite: these investigators concluded that at least 85 pct of the carbon in ferrite occupies the octahedral (0: 3, B) site rather than the larger

Jan 1, 1967

By M. R. Goldick

The Roan Antelope concentrator was originally designed with a nominal milling capacity of 6000 tons of copper ore per day but this was subsequently considerably exceeded. In broad outline the plant consisted of two No. 30 McCully gyratory crushers for coarse crushing, five 5½-ft Standard Symons crushers in open circuit for secondary crushing, ten No. 98 Marcy ball mills arranged in five sections, each two-mill section with primary and secondary Dorr classifiers for two-stage grinding. One stage of flotation roughing was followed by two stages of cleaning, all in airlift type pneumatic flotation machines, with the final concentrates filtered on Oliver drum filters. Tailing was thickened in a 250-ft Dorr traction type thickener before pumping to the tailing dam. Concentrating operations commenced in June 1931, on the completion of the first two ball-milling sections and output was increased during the next few months as the remaining sections were finished. From the start, very few technical difficulties were experienced but a number of evolutionary changes have been made as a result of operating experience and the availability of improved equipment. These have resulted in plant and ore-flow alterations although the general scheme of ore treatment remains substantially as before. The main changes to date were the installation of a new crushing plant at Storke shaft, some 7000 ft west of the original Beatty shaft; the completion of a two-stage secondary crushing plant; an increase of 20 pct in ball-milling capacity; a change-over from pneumatic to a mcchanical type of flotation machine for flotation roughing; the reduction of flotation cleaning from two stages to one stage. Ore Treated Typically the ore treated consists of metamorphosed shales and sandstones with shales as the principal mineral-bearing rock carrying chalcocite, bornite and chalcopy-rite as the main copper minerals. Chalcocite predominated in the original eastern end of the ore body but there is a pronounced trend to an increased proportion of the copper-iron sulphides as mining proceeds westward. Although the ore can be described as soft, this advantage is offset by the extremely fine dissemination of the copper minerals which calls for a high degree of comminution of the ore (go pct minus-zoo mesh Tyler standard) to give a reasonably satisfactory separation of mineral from gangue. Latterly, there has been a tendency for the ore to become harder as shown by a reduction in the ball-milling rate from a previous figure of over goo tons per ball-mill day to the present output of some 800 tons. Chalcopyrite is not so finely disseminated and has also proved more amenable to flotation than chalcocite. Nonsulphide minerals are mainly the so-called oxides such as malachite, cuprite and melaconite with some chrysocolla and

Jan 1, 1949

By Bruce F. Grant, Stefan F. Szasz

During 1947, a Sinclair research team was assigned to investigate thermal methods of oil recovery. The assignment was recommended by a survey of possible research approaches to increase the amount of oil that ultimately can be recovered from oil producing reservoirs. The use of heat to stimulate oil production rates by the melting of paraffin deposited in well bores can be traced back to within one or two decades of the drilling of the Drake well. The application of heat on a larger scale has been discussed by generations of oil producers. Shortly after the turn of the century, one intrepid operator is reported to have injected steam into a Pennsylvania property. After a few weeks, he apparently became discouraged and terminated his experiment. Subsequently, the literature contains references to several well-developed techniques for supplying heat to a producing well bore to melt paraffin or to reduce the viscosity of oil contained in the formation immediately around the well bore.1.?.3.4 Some early references discuss procedures to furnish heat to the reservoir,5,6 with the injection well as the heat source, thus obligating the process to maintain the entire rock mass at a temperature above that at which the desired improvement in oil recovery would occur. Another approach to reservoir heating was reported by a group of Russian technologists in 1935.7,8,9 They definitely demonstrated that combustion can occur within the porous structure of an oil-bearing sandstone. Their field experiments, however, relied less on combustion within the rock than on heat furnished by combustion of oil supplied to the injection well bore. Ignition of the air-oil mixtures in the well bore was found very difficult, and the field tests were carried on for only short periods of time. Publication of the Russian work spurred at least one independent operator in this country to try firing an air-gas injection well, on for only short periods of time. Publication of the Russian work spurred at least one independent operator in this country to try firing an air-gas injection well. The Brundred Oil Corp. reportedly obtained combustion in the sand immediately around the injection well bore, but the experiment was abandoned because of interference with normal production schedules. Injection capacity of the experimental well was greatly reduced by firing. The well was reshot and pieces of sand showing partial fusing of the quartz matrix were recovered. To the authors' knowledge no other field experiments utilizing combustion techniques for formation heating were undertaken prior to 1948, although the patent literature evidences continued interest in formation heating."'," CONCEPT OF COMBUSTION-SUPPORTED HEAT WAVE The references cited were in agreement that heat applied to a reservoir would increase recovery, but there

Jan 1, 1955

By T. J. Bosworth

The effect of hydrogen pretreatment of alumina, magnesia, and zirconia crucibles on reduced oxygen levels in iron charges has been studied. Hydrogen treatment of commercial high-purity magnesia crucibles was observed to produce as high as 70 pct reduction in oxygen content in iron melts. Hydrogen treatment of the commercial high-purity grade zirconia crucibles produced a 25 pct reduction in oxygen levels in iron melts. An average reduction of Knoop hardness of 47 pct was recorded on the iron charges melted in hydrogen-treated crucibles. On the basis of the experiments and the free-energy diagram, it appears that the major source of reducible oxygen to the iron charge is the suboxides and impurity oxides rather than the major oxide of the crucible. Suitable pretreatment of the crucibles to reduce and remove these oxides yields low oxygen levels in iron melted in the crucibles. DURING the last decade, attempts to produce more pure and uniform alloyed metals have brought about the development of many new melting techniques. Notable among these are vacuum-induction melting, inert and consumable-electrode melting, the cold-mold technique, and numerous techniques for removal of impurities by chemical reaction. However great the achievements in this field, metals must still be melted in contact with media of varying reactivity; i.e., gas, ceramic, and slag. Studies have been made to attain an understanding of the reactions that take place during melting, including slag-metal reactions and equilibria, equilibrium of hydrogen and water vapor, and carbon dioxide and carbon monoxide with oxygen in molten iron. These reactions have been treated quite thoroughly. There is one condition, however, that has been widely overlooked, and, to the author's knowledge, only cursive investigation has been made of it. This is the reaction between the ceramic crucible material and the iron charge. In recent years, Hadley and Bianchi' made a series of studies on hydrogen deoxidation of iron in magnesia crucibles. Bianchi2 studied crucible-FeO equilibria in the temperature range 1525°to 1650°C in high vacuum with, however, inconsistent results. Richardson and Jeffes3 in their series of articles on thermodynamic reactions in the making of iron and steel refer to Wentrup and Hieber's4 work on iron and aluminum deoxidation. Their pork included melting iron in alumina crucibles and measuring the aluminum and oxygen content in the iron. Because of the low values obtained, question has arisen of their analytical accuracy.3 Dastur and chipman5 obtained values on hydrogen-oxygen equilibrium in molten iron contained in alumina crucibles similar to those obtained in experiments in the present program. Hochmann6 studied removal of impurities in chromium irons in high vacuum. His results with respect to oxygen level in chromium-iron melted in magnesia crucibles are consistent with results we have obtained.

Jan 1, 1959

By C. S. Roberts

Four binary alloys in this system were creep tested at 300°' to 600°F. A photographic study of microstructural changes showed that the outstanding creep resistance results primarily from a potent precipitation hardening locally at grain boundaries. Twinning was correlated with the primary stage and nonbasal slip with the tertiary stage of creep. THE utility of the rare earth metals as ingredients of magnesium alloys destined for elevated temperature application has been recognized for about 15 years. A review of the early development of these alloys has been given by Leontis. 1,2 It has been only recently that a desire has arisen to understand basically their remarkable creep resistance. The present research had that object. The work of Leontis showed that the differences between the behavior of the individual magnesium-rare earth element binaries was of commercial significance. However, the variations were small compared to the overall difference in creep resistance between the group as a whole and the magnesium alloys of the Al-Zn type. It was decided to conduct this investigation with one binary system which would be representative of the magnesium-rare earth element alloy group. Cerium was chosen as the solute because of its near-middle position in the series and because of its availability in the commercially pure form. A previously published description of the creep behavior of electrolytic magnesium" serves as the background to this research. The experimental approach used in that investigation has been partially repeated here. A series of binary alloys was planned to include the following: 1—A dilute alloy which would contain the cerium almost entirely in solid solution. This would assess the solid solution effect. 2—An alloy which is nearly saturated at the selected solution heat treatment temperature, 1070°F. Here the effect of nearly maximum precip- itation would be obtained without the influence of undissolved Mg-Ce intermetallic. 3—An alloy containing slightly more cerium than is soluble at 1070°F. This would allow the investigation of the effect of a small amount of excess intermetallic. 4—A high cerium alloy in which the influence of a large volume of undissolved intermetallic may be examined. Experimental Details In order to specify compositions of the binary alloy series a knowledge of the solubility of commercially pure cerium in solid electrolytic magnesium and also of the composition of the terminal intermetallic phase was necessary. The latter has been proven to be approximately Mg,Ce by Voge14 and Haughton and Schofield.5 A series of both cast and extruded alloys were solution heat treated 24 hr at 1070°F for a solubility determination. Lineal analyses of the polished and etched microstructures were accomplished with the aid of a Hurlbut

Jan 1, 1955

By Mark J. Klein

The behavior of nitrogen in Cr-0.12 at. pct Y was studied in specimens of varying interstitial concentration and thermal history. It was found that soluble nitrogen can be introduced into this alloy by increasing the concentrations of either oxygen or nitrogen. For low nitrogen concentrations the nitrogen in solution is low relative to that in unalloyed chromium. However, the nitrogen in solution increases with increasing nitrogen concentration, approaching that in unalloyed chromium. When the alloy is supersaturated with nitrogen, the nitrogen precipitates readily from solution as a chromium nitride. The stress -induced relaxation of nitrogen is influenced by internal oxidation or internal nitrification of this alloy. THE addition of small concentrations of reactive elements such as yttrium have been found to enhance the low-temperature ductility of chromium.&apos; However, the mechanism by which the ductility is increased is not known. It has been suggested that this effect is caused by a drastic reduction in the concentration of nitrogen retained in solution and therefore a decrease in the number of dislocations locked by nitrogen, a factor that has been associated with an increase in ductility.1,2 However, a change in the type of interstitial precipitate induced by yttrium could also contribute to enhanced ductility of the alloy, since chromium nitride precipitates appear to be embrittling.&apos; In this regard, it has been shown that yttrium scavenges nitrogen in chromium to form YN,4 thus reducing the embrittling chromium nitride phase. However, the change in nitrogen solubility induced by yttrium and the partition of nitrogen between chromium and yttrium nitrides are not known. The object of this investigation is to study the effect of yttrium on the behavior of nitrogen in chromium to obtain information relevant to the mechanism by which scavengers enhance the ductility of chromium. EXPERIMENTAL PROCEDURES The experimental procedures used in this investigation have been described in detail elsewhere.5,6 Wires of Cr-0.12 at. pct Y, 15 cm in length and 1 mm in diam, were drawn from rods 0.6 cm in diam supplied by the General Electric Co. The grain size of the wires after recrystallization at 1150°C was somewhat nonuniform, varying from 0.006 to 0.06 mm in diam. The interstitial analysis for the wires in ppm by weight was about 160 0, 80 N, 12 C, and <2 H. Heat treatments were carried out after encapsulation of the specimens in quartz tubes containing argon. Changes in interstitial concentrations, or interstitial "loading" as it is termed in this study, were generally accomplished by annealing in oxygen, ammonia or methane at 1150°C. The internal friction was measured using a conventional torsional pendulum enclosed in an evacuated chamber. Electrical-resistivity measurements were made at liquid-nitrogen temperature.

Jan 1, 1967

By H. Eyring, J. W. Fredrickson

Many theories have been advanced to explain the phenomena of elastic and plastic deformation. The object of this report is to present a mechanism for deformation, not radically differing from existing theories, but embodying.certain principles and concepts of these theories. This proposed theory cannot be the complete answer to the age-old problem of deformation but it is believed that it will be a step further in the proper direction. The plastic properties of solids have recently been reviewed by Seitz and Read.&apos; ZenerZ has reviewed and correlated the existing work on the anelasticity of metals. With these and others3&apos;4&apos;5 resent theories of deformation are well-known. Of the many theories now extant, those receiving most attention have been proffered by Griffith,6 Becker,l Smekal,8 Polanyilg Orowanlo and Taylor.&apos;&apos; Although differing quite widely in details, these theories are based more or less on a common principle of flaws or dislocations that exist in the crystal lattice. The effect of stress concentrations surrounding a flaw or crack has been treated most recently by Fisher and Hollomon.12 The various authors differ as to the exact nature of the flaws or dislocations, the causes of their appearance, or the manner in which they initiate slip. All of the theories agree that the number of dislocations increases with progressing deformation. It is universally agreed that the shearing process is not a simple gliding of ideally perfect atomic lattice planes. It is also agreed that the "macroscopic" process of gliding, or slip, is brought about by the spreading of a large number of locally initiated "glide steps" through the whole crystal. The occurrence of these "glide steps" is closely related to the presence of some kind of deviations from the "ideal" lattice structure, even in the undeformed crystal. These deviations are overcome &apos;&apos;one at a time," in a manner of speaking, due to some stress-concentrating effect.13 Proposed Theory Many solids show a continuously increasing deformation if subjected to a constant load of suitable magnitude in an extended range of temperature for a sufficient time. This deformation, or flow, may be said to be due, in general, to the tendency of the atoms or molecules in an elastically stressed body to readjust themselves in such a way that if the deformation were kept constant, a release of stress would take place. If rupture does not occur, this process of relaxation causes the rate of flow to obtain a final constant value, as shown in the curve (Fig I) obtained by Taylor and Quinney.14 In this state the release of stress by relaxation exactly counterbalances the increase due to the elastic strain on the test pieces.

Jan 1, 1949

By J. H. Keeler

The tensile characteristics of Zr-Fe binary alloys containing up to 5 atomic pet Fe are reported for the temperature range —195o to 500°C. A linear relation between stress at constant strain and volume fraction ZrFe2 was found. The coincidence of data from unalloyed zirconium with zero volume fraction ZrFe2 indicated little or no solid solution in IL-zirconium, in agreement with Hayes, Roberson, and O&apos;Brien.&apos; The absolute increase in strength due to particle strengthening, although decreasing with increasing temperature, was a greater percentage at high temperature. ZIRCONIUM is of interest for use in nuclear reactors because of its low neutron absorption, good corrosion resistance, and high melting temperature. The alloying of zirconium with iron has been considered as a means of increasing the mechanical strength of zirconium without seriously increasing the neutron absorption " over that of unalloyed zirconium. The Zr-Fe system has a eutectic at 934°C and 23.7 atomic pet Fe and a eutectoid at 800°C and 4.0 atomic pet Fe. The zirconium-rich end of this system determined by Hayes, Roberson, and O&apos;Brien&apos; is shown in Fig. 1. The intermetallic phase coexisting with a and ß-zirconium has been reported as Zr2Fe3,1 with a,, - 7.04A, and as ZrFe2,2 face-centered-cubic, the phase being of the MgCu, type (C-15). It was more recently agreed to be ZrFe33 and face-centered-cubic. This intermetallic phase is essentially insoluble in a-zirconium, the hexagonal-close-packed modification; and the lack of solubility makes the system particularly interesting metallurgically. The system is strengthened almost exclusively by particles of in-termetallic phase, and there is very little solid solution strengthening to complicate the analysis. The Bureau of Mines, in its survey of zirconium-base alloys,&apos; reported the tensile properties of Zr-Fe alloys made from chloride process zirconium, induction melted in graphite crucibles, and swaged at 850°C in iron sheaths. Additional data on these ZrFe alloys were given by Hayes, Roberson, and O&apos;Brien.&apos; Chubb and Muehlenkamp% have recently reported the strength of Zr-Fe alloys containing up to about 1.25 atomic pet Fe. These alloys were made from crystal bar zirconium, hot worked at 820°C, annealed at 700°C, and tested both at room temperature and at 316°C. Experimental Procedure The materials used in this investigation were high purity zirconium made by the iodide process and electrolytic iron. The composition of the zirconium as obtained by spectrographic analysis and the nominal composition of the iron are given in Table I. Alloy ingots weighing 100 g were made by are-melting under argon in water-cooled copper crucibles in a multihearth furnace."

Jan 1, 1957

By C. L. Magee, H. W. Paxton

PREVIOUS workersl&apos;% ave found that as-quenched ferrous martensites can be plastically deformed at low stresses. They have also found that the stress to obtain small strains can be significantly increased by aging at temperatures up to 150°C. This behavior has been interpreted in two ways: 1) that the deformation at low applied stress is due to internal stresses and thus the aging phenomenon is due to relaxation of the internal stresses;&apos; 2) that the microdeformation arises through the motion of unpinned dislocations and the aging process is the diffusion of carbon to the dislocations to pin them.293 In a recent paper,4 we have shown that under certain conditions the dominant microdeformation mechanism of as-quenched Fe-31Ni marten-site-austenite aggregates is the transformation of retained austenite. Our results on resistance changes during deformation and temperature dependence of the deformation also established that, at temperatures above 300° K, the microdeformation was not due to this transformation. The purpose of this note is to report results of experiments which indicate that explanation 1 is appropriate for this deformation. All results presented here are from conditions where transformation does not make a measurable contribution to the microplastic deformation, in Fe-31Ni-0.002C, or in Fe-29Ni-0.02C-0.25Ti. The experimental techniques that were used for measurement of the plastic deformation are described4 and analyzed5 elsewhere. Fig. 1 shows the microplastic response of 100 pct austenite at 300" and 350° K. The microplastic response of an austenite-martensite aggregate is also given in Fig. 1 and it is seen that, after formation of martensite, the initial plastic deformation occurs at lower stresses. Thus, the softness is not entirely due to retained austenite—the quenched structure can be deformed at lower stresses despite the fact that the macroscopic strength is significantly higher. A result which allows a distinction to be drawn between the alternative explanations for this behavior is derived from aging experiments on the low-carbon alloy containing titanium. We have previously shown4 that the presence of titanium in this alloy reduced the free carbon to a sufficiently low level that thermal stabilization of the austenite-martensite transformation was not detected. Despite this, Fig. 2 shows that the microplastic response is decreased by aging treatments. A similar aging effect in Fe-ZONi, with some titanium, has previously been reported by . Thus, carbon is not necessary for the aging process and explanation 2 is at best incomplete. Since internal stress relief can occur independently of carbon (any temperature dependence of the flow stress can result in decreased internal

Jan 1, 1969