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By E. W. Davis

IF the tonnage of merchantable iron ore remaining in the Lake Superior district is divided by the average of the annual shipments for the past 20 years, it will be found that this ore supply will be exhausted in approximately 35 years. This computed exhaustion period would be an indication of the future activities of the iron-mining industry if it were not for the fact that merchantable ore is being manufactured from low-grade ore, of which there is an almost inexhaustible supply in the Lake Superior district. It is true that at present only the simplest of these low-grade ores are being concentrated to any considerable extent, but progress is being made with the treatment of the more complex ores, and now, in addition to 20 washing plants on the Mesabi Range, three plants are equipped with jigs for the treatment of ore that cannot be concentrated simply by washing. The latest addition to the ore-treating plants of the Mesabi Range is a magnetic roasting and concentration plant at Cooley, Minn., in which ore that cannot be concentrated either by washing or by jigging is roasted to the magnetic state and concentrated on magnetic separators. This plant is beginning its third season of operation, and while it is too soon to make definite predictions, there are strong indica-tions that this new process may make commercially possible the manu-facture of high-grade, merchantable iron ore from large quantities of low-grade ore now considered worthless. After the iron oxide contained in an ore has been converted to mag-netite, almost any desired grade of concentrate can be produced, using magnetic-concentration equipment of the types now in general use for the concentration of the natural magnetites of New York, New Jersey and Pennsylvania. The conversion of hematite (Fe2O3) to magnetite (Fe3O4) is easily accomplished by heating the ore to a dull red tempera-ture in a reducing atmosphere. The reaction is slightly endothermic, and while it requires 200 B.t.u. to heat to 900° F. one pound of hematite ore containing 45 per cent Fe, it requires only 100 B.t.u. to convert the oxide into magnetite. In the laboratory, using small quantities of ore, this conversion is very simple, but large furnaces suitable for commercial

Jan 1, 1936

SINCE it seems to me that guns are of greater importance in the art of casting than any of the other things that are made by it, and that they require more foresight and care because they need many perfections, I wish now to repeat certain useful and necessary precautions in corroboration, for though I have already spoken to you of them in some detail, the power has not been granted me to pass with one breath completely through a subject with many parts. Therefore it will not be wearisome to you to hear the same thing told again, because it will not be without amplification of some pertinent points. For this reason I have prepared the present discourse, which I have called admonitions. The first of these concerns the making of the pattern upon which the

Jan 1, 1942

By John J. Egan

THE present list of problems relating to the physical chemistry of steelmaking has been prepared by the Committee on the Physical Chemistry of Steelmaking, from answers to a questionnaire Submitted to a number of metallurgists engaged in both industrial and educational work throughout the United States. The purpose of the project is to make available to research laboratories a list of problems, all reduced to their simplest terms, the solution of which would aid in creating a better understanding of the steelmaking process. It is not intended to restrict the problems to practical steelmaking. The list also includes the study of the properties, and their correlation, as well as the physical and chemical reactions, of all Substances that occur or that may be in any way associated with steelmaking operations, Such as metallic substances, refractories, nonmetallic inclusions, and the constituents of slags. Many of the problems can be carried out in university or other research laboratories. Others may be most successfully attacked by cooperation of the research men with the operating personnel. It is the Committee's earnest wish that this cooperation be fostered. It is requested that investigators who are working on any of the problems listed and who anticipate future publication of their results, notify the Secretary of the Committee that such investigation is in progress. Suggested additions to the present list are also requested. The Committee is undertaking to act as a clearing house for information regarding the topics in this field that are being actually studied. Interested persons are invited to correspond with the Secretary. I. Data involved in the state of equilibrium for the various systems (laboratory work, almost entirely). A. SPECIFIC HEATS, HEATS OF FORMATION, ENTROPIES AND FREE ENERGIES OF VARIOUS PURE ELEMENTS OR COMPOUNDS; ALSO CERTAIN TYPICAL SLAGS AND REFRACTORIES. I . Determination of specific heats and entropies of oxides, sulphides, nitrides, etc. over a wide temperature range. 2. Determination of free energies of oxides, sulphides, nitrides, etc. over a wide temperature range. 3. Determination of the heats of formation of the oxides, sulphides, nitrides, etc. 4. Determination of the thermodynamic properties of the more important mineralogical constituents of the basic open-hearth slags such as calcium silicates, calcium phosphates, calcium ferrites, manganese silicates, FeO and Fe2O3. 5. Determination of the specific heats of open-hearth slags, including liquid silicates, if possible.

Jan 1, 1941

By J. T. Norton, N. J. Grant, I. S., Servi

Coarse grained high purity aluminum was tested in creep at temperatures of 400° to 1200°F to develop subgrain structures. Measurements of subgrain size, distribution, and rotation were made from X-ray diffraction patterns. Subgrain size and distribution were checked metallographically and the size was compared with average slip band spacing. The slip family was determined for several specimens. THE interest and research recently evident abroad in the role of subgrain formation and polygon-ization as a contribution to the creep of metals at elevated temperatures is deserving of greater attention in this country. Such metallic subgrains can be defined as macroblocks existing within the grains. The general observation has been that the macro-blocks which belong to the same grain have a maximum difference in orientation of a few degrees. In spite of the considerable amount of work that has been done since Jenkins and Mellorl observed the "division of existing crystals into smaller units when deformation occurs at an annealing temperature," the subject of subgrain formation is only now receiving truly active discussion and investigation. The existence of subgrains has been revealed by metallographic methods, as in the work of Jenkins and Mellor,1 and by X-ray methods, first applied to this problem by Homes.' Hirst3 and Calnan and Burns4 applied the back-reflection Laue technique to the study of coarse grained specimens. Wood et al.5 and Greenough and Smith' examined the ring obtained with a back-reflection camera for the study of fine grained specimens. In addition to the above, the transmission technique was used by Wood.6 A special technique was developed by Guinier and Tennevin8 in order to improve the resolution. Metallographically, the subgrains have been observed directly on the surface of deformed specimens by Wood et al.,3 or have been made evident on repolished surfaces by applying a suitable etching reagent. The latter technique, first suggested by Lacombe and Beaujard,9 was then improved by Wyon and Crussard.10 Subgrains can be formed in single crystals after small amounts of bending followed by heating after this cold work, or during deformation at elevated temperatures. The first phenomenon was analyzed by Cahn11 for the simple case of pure bending followed by annealing. Cahn suggested a mechanism of subgrain formation based on the dislocation theory and called this phenomenon "polygonization." He extended this mechanism to the more complex case of local bending, such as the bending which may occur when a polycrystalline specimen is deformed in tension. Cahn's suggestion was later found quite consistent with the results obtained by Dunn and Daniels." An explanation has been presented recently regarding the formation of subgrains during deformation at elevated temperatures by Chang and Grant.'" In general, there are two schools of thought on the subject. One, according to Wood et al.,5 is that subgrain formation is a mechanism of deformation which is operative under certain conditions in the same way that the slip process is the mechanism of deformation which is operative under other conditions. The boundaries between the subgrains undergo a viscous flow which contributes substantially to the deformation of the material. The second, according to Cahn,13 Wyon and Crussard,10 and Chang and Grant,18 is that subgrain formation is the effect of simultaneous deformation and annealing and is,

Jan 1, 1953

By V 7. 0 / 300 dpi

WHEN the copper smelters were built, in Montana, all of the refractory products which were used in their construction were shipped in from Eastern factories. It was apparent that if a material suitable for the manufacture of these products could be found within the State, a saving of freight could be effected and a new industry built up. Prospecting for such materials was started and experiments were made with samples from numerous deposits. Considerable effort and funds were expended in an attempt to manufacture silica brick from Dillon quartz, a light colored sandstone that is found near Dillon, Mont., on the Oregon Shortline railroad. As a brick material the Dillon quartz was a failure, but it has proved very satisfactory as a silica cement. It is now being used in laying silica brick and for reverberatory furnace bottoms. A bed of quartzite that is particularly suited to the manufacture of high-grade silica brick -was finally discovered at Browns Spur, 6 miles west of Anaconda. The material from this deposit is now being used in the manufacture of the Anaconda silica brick, which have gained a wide reputation for heat-resisting and lasting qualities. The analysis of all average sample of this quartz is: SiO2,, 96.7; Fe203, 0.3; Al203, 2.5; CaO, 0.3 per cent. The very low percentage of fluxing ingredients makes this a most refractory material. All of the Anaconda silica brick are hand molded. Various types of brick machines have been tried, but the hand-mold process proved the best suited to the manufacture of silica brick from this material. The silica is first put through a jaw crusher and is then clumped into wet pans, where 4 per cent. of lime paste is added, to produce a bond. Without the lime the. material would not be plastic enough to mold. After a few minutes' grinding in the wet pans the material is conveyed to the molder, who forces it into the molds by hand. The brick are then dumped on pallets and placed in the drier, where they are left until dry enough to be set in the kilns. Some of the brick are re-pressed before being dried. They are burned about five days, in round down-draft kilns. It is not necessary to have as much heat in the kilns as the brick will be subjected

Jan 9, 1913

By William Marsh Baldwin

[Two of the most useful and important equations available to the metallurgist for the study of plastic deformation of metals are the Huber-von Mises-Hencky1-3 and the St. Venant7-10 equations. HUBER-VON MISES-HENCKY EQUATION The Huber-von Mises-Hencky equation answers the question: When does plastic flow occur in metal that is subjected to a multi-axial stress? It occurs, according to this equation, when the three principal stresses,? al, a2, and a3 satisfy the equation: (s1 - s2)2 + (s 2 - s 3)2 + (s 1 ? s3)2 = 2K2 [I] Here K is the yield strength of the material as determined in an ordinary tensile test. If the quantities a1, a2, and a3 are assigned to the coordinates of a Cartesian three-dimensional system, this expression describes a cylinder whose axis of symmetry is inclined at equal angles to the three coordinate axes4,5 (Fig. I). The radius of this cylinder is v2/3K. For the purpose of simplicity, it is sometimes advantageous to ascribe the values s 1/K = si, s 2/K = s2, s 2/K = s3 to the three coordinate axes instead of the principal stress alone. In this case, Eq. I becomes (s1 - S2)2 + (S2 - S3)2 + (Sl - S3)2 = 2 [2] and the radius of the cylinder becomes 2/3v. In the latter method of representation, a point lying inside the cylinder indicates that the metal will react elastically, whereas a point lying on the cylindrical surface indicates that the metal will behave plastically. Some of the geometric features of this cylinder are worthy of study. Let us inquire first as to what interpretation may be placed upon what we will choose to call the "circles of latitude" of the cylinder (L in Fig. I) and the "meridians" of the cylinder (M in Fig. I). Circles of Latitude Circles of latitude are formed by allowing a plane, passing perpendicular to the cylinder axis, to intersect with the cylinder. Any point, P, on this circle is presumed to have the coordinates s1, s2, and s3. The coordinates of the point resulting from the intersection of the plane and the cylinder axis will be a, a, and a (since the cylinder axis is equally inclined to the three coordi¬nate axes). Let us now pass a line through the point on the circle and the point on the axis.]

Jan 1, 1946

By R. A. Wattenbarger, H. J. Ramey

A systematic study has been made of the application of the real gas pseudo-pressure m(p) to short-time gas well testing. The m(p) function can be used in real gas flow problems to account for the variation of viscosity and z-factor with pressure. A mathematical model was solved numerically to generate solutions of various real gas flow problems. The effects of turbulence, formation damage and wellbore storage were included in the model. The analysis of simulated well tests showed that the interpretation methods normally used for liquid flow are generally accurate when the m(p) is used. For practical rates without turbulence, the solutions are not rate-sensifive, and the flow capacity.. kh and skin effect can be determined accurately from either a buildup or a drawdown test. However, the kh calculated from a drawdown test can be significantly low when turbulence is present. A case was simulated in which this error wa.s 36 percent. Turbulence does not affect the determination of kh from buildup tests. The proper determination of kh from p and pa buildup and drawdown plots is developed by analyzing their relationship to the m(p) method. A simple equation is given that can be used for long-range gas well performance forecasting. This expression is compared with a method pre-sended by Russell et al." Introduction The formation flow capacity and wellbore damage condition can be determined for liquid-producing tests by means of buildup and drawdown tests. These tests make use of short-time pressure transient data rather than stabilized flow tests that are often used for gas well testing. Tracy' presented a method of gas well testing that was based on ideal gas equations and utilized p2 buildup plots. This method was shown to be good for low pressure wells. MatthewsZ suggested plotting p and using an average slope and average gas properties. This method was more successful on high pressure wells. Al-Hussainy, Ramey and Crawfordh howed that variation in gas properties could be simplified by using the real gas pseu do-pressure m(p). Some cases showed that the use of the m(p) function Original manuscript received in Society of Petroleum Engineers office Aug. 8. 1967. Revised manuscript received June 11, 1968. Paper (SPE 1835) was presented at SPE 42nd Annual Fall Meeting held in Houston Tex., Oct. 1-4. 1967, and at SPE 4th Annual Eastern Regional ~eetin$ held in Pittsburgh. Pa., Nov. 2-3. 1967. 0 Copyright 1968 American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. 'References given at end of paper. provided an accurate method of interpreting buildup and drawdown tests. Because the work of Al-Hussainy et al. included only a few actual cases, there was a need to explore the use of the m(p) method for a greater variety of flow conditions. The occurrence of turbulent flow around the wellbore often is an important factor in gas well testing. Swift and Kiel,' and Carter et a1.' treated turbulence in gas well testing, but did not consider the variation of viscosity and z-factor with pressure. This paper presents the results of an investigation of the application of the m(p) method to buildup and drawdown testing. Vhe investigation included the effects of turbulence, formation damage and wellbore storage. Gas Flow Equations To formulate the mathematical model, many of the assumptions usually used in well testing theory are applied. The system has radial geometry with a closed outer boundary and is composed of a horizontal porous formation that has uniform and isotropic rock properties and uniform thickness. Allowance is made, however, for a radial region of reduced permeability near the wellbore. This region represents formation damage. The geometry of the system is shown in Fig. 1. Darcy's law does not always apply to gas flow. A more general expression is needed for non-Darcy, or "turbulent" REGION OF DAMAGED PERMEABILITY SEALED BOUNDARIES ClRCULAR WELL BORE Fig. 1—Radial flow model. AUGUST, BT7

Jan 1, 1969

By M. F. Comerford

M. F. Comerford (Smithsonian Astrophysical Observatovy)- The authors' concern about the effects of preferred orientation is justified and emphasizes a phenomenon that can be a source of serious error, but the cogency of their concluding statement bears close examination. They contend that comparison of intensities from parallel planes of the two phases, as proposed by Averbach, Comerford, and Bever,13 leads to incorrect results. The state- ment is based on the fact that, in Fig. 3, intensity measurements at extreme angles of tilt, (2, lead to different values than those given by the average of all the data. The proposed explanation is that unsuspected superpositions of (110), reflections spuriously enhance the martensite intensity. However, it can be shown on appropriate stereographic projections that no superpositions occur which can affect the reflections in question. Hence, the ex-

Jan 1, 1965

By L. Webster Wickes

The bad effects of arsenic in commercial copper are well-known to metallurgists. The refining of copper by electrolysis eliminates practically all of the arsenic, provided certain requirements are fulfilled. The first, and most important, of these requirements is, that the voltage of the depositing current shall not be too high. It has been known for some time that the percentage of arsenic in the deposited copper increases with the voltage. To investigate the relation between the electro-motive force (e.m.f.) and the freedom of the precipitated copper from arsenic, the experiments were made, of which a brief summary is here given: I made three copper-arsenic alloys, containing respectively 3.56, 2.24 and 0.96 per cent. of arsenic. From these alloys I cast several anodes. For cathodes I used sheets of thin copper,

Jan 1, 1905

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

Energy conservation has been the keyword in many plant expansions. Far many years, most of the phosphate industry has been dry grinding their phosphate rock. Agrico Chemical in Florida has recently been evaluating the wet grinding of phosphate rock, a process which eliminates a pre-dry stage for mill feed while allowing higher through- puts. This same company also plans to open a new phosphate facility in Louisiana that will use wet grinding in both ball mills. The Eveleth Expansion Co.'s Fairlane concentrator will have the largest rod and ball mills in the US mining industry. The plant will consist of three lines, each with one rod mill and one ball mill, and will process 464 ltph. The rod mills will be 15 x 20% ft, drawing 2035 hp. The ball mills will be 17 x 41½ ft, drawing 6900 hp and driven by dual 3000- hp motors. The plant is scheduled for startup in the fall of 1976.

Jan 2, 1975

By J. R. Szedon, T. L. Chu, G. A. Gruber

Amorphous adherent filnzs of silicon dioxide have been deposited on silicon substrates by the oxidation of silane at temperatures ranging from 650 to 1050C. Various diluents (argon, nitrogen, hydrogen) were used to suppress the formation of SiO2 in the gas phase. Deposition rates of the oxide were determined over the temperature range in question as functions of' re-actant flow rates. Etch rate studies were used for a cursory comparison of structural properties of deposited and thermally grown oxides. From electrical evaluation of metal-insulator-silicon capacitors it was determined that the interface charge density of deposited films is similar go that of dry-oxygen-grown films in the 850° to 1050 C temperature range. Deposited films exhibit several ionic instability effects which differ in detail from those reported for thermal oxides. Stable passivating films of silicon nitride over deposited oxides appear to be practical for use in silicon planar device fabrication. Such films can be prepared under temperature conditions which have less effect on substrate impurity distributions than in the case of grown oxides. AMORPHOUS silicon dioxide (silica) is compatible with silicon in electrical properties and is the most widely used dielectric in silicon devices at present. Silica films can be prepared by the oxidation of silicon or deposited on silicon or other substrate surfaces by chemical reactions or vacuum techniques. The ability of thermally grown silicon dioxide films to passivate silicon surfaces forms one of the practical bases of the planar device technology. Properly produced and treated films of grown SiO 2 can have low densities of interface charge (-1 X 10" charges per sq cm) and can be stable as regards fast migrating ionic sgecies. 1 To maintain these properties, even with an otherwise hermetically sealed ambient, the Sia layers must be at least l000 A thick. Such thicknesses require oxidation in dry oxygen for periods of 7.8 hr at 900°C or 2 hr at 1000°C. Although oxidation in steam or wet oxygen can reduce these times to 17 and 5 min, the resulting oxides must be annealed to produce acceptable levels of interface charge., Oxidation or annealing involving moderate to high temperatures for extended periods of time can be undesirable. Under some conditions, there can be changes in the distribution of impurities within the underlying substrate. A chemical deposition technique using gaseous am-bients is particularly attractive and flexible for preparing oxide films. With a wide range of deposition rates available, films can be produced under condi- tions of time and temperature less detrimental to impurity distributions in the silicon than in the case of thermal oxidation. The pyrolysis of alkoxysilanes, the hydrolysis of silicon halides, and various modifications of these reactions are most commonly used for the deposition of silica films.3 Silica films obtained in this manner are likely to be contaminated by the by-products of the reaction, organic impurities, or hydrogen halides. The use of the oxidation of silane for the deposition process has been reported recently.4 The deposition of silica films on single-crystal silicon substrates by the oxidation of silane in a gas flow system has been studied in this work. The deposition variables studied were the crystallographic orientation of the substrate surface, the substrate temperature, and the nature of the diluent gas. The electrical charge behavior of Si-SiO2-A1 structures prepared under various conditions was investigated by capacitance-voltage (C-V) measurements of metal-insulator-semiconductor (MIS) capacitors. The experimental approaches and results are discussed in this paper. 1) DEPOSITION OF SILICA FILMS The overall reaction for the oxidation of silane is: The equilibrium constants of this reaction in the temperature range 500° to 1500°K, calculated from the JANAF thermochemical data,= are shown in Fig. 1. In addition to the large equilibrium constants, the oxidation of silane is also kinetically feasible at room temperature and above. However, the strong reactivity of silane toward oxygen tends to promote the nucleation of silica in the gas phase through homogeneous reactions, and the deposition of this silica on the substrate would yield nonadherent material. The formation of silica in the gas phase can be reduced by using low partial pressures of the reactants. Argon, hydrogen, and nitrogen were used as diluents in this work. 1.1) Experimental. The deposition of silica films by the oxidation of silane was carried out in a gas flow system using an apparatus shown schematically in Fig. 2. Appropriate flow meters and valves were used to control the flow of various reactants, i.e., argon, hydrogen, nitrogen, oxygen, and silane. Semiconductor-grade silane, argon of 99.999 pct minimum purity, oxygen of 99.95 pct minimum purity, and nitrogen of 99.997 pct minimum purity, all purchased from the Matheson Co., were used without further purification. In several instances, a silicon nitride film was deposited over the silica film. This was achieved by the nitridation of silane with ammonia using anhydrous ammonia of better than 99.99 pct purity supplied by the Matheson CO.' The reactant mixture of the desired composition was passed through a Millipore filter into a horizontal water-cooled fused silica tube of 55 mm

Jan 1, 1969

By H. A. Wilhelm, P. Chiotti, G. A. Tracy

A summary of analytical, X-ray, thermal, and metallographic data obtained in the study of the Mg-U system is presented. No intermetallic compounds are formed by these two elements, and their mutual solubility is limited at temperatures up to 1255°C. The compositions of the liquids which coexist at 1135°C under a pressure of 3 atm are 0.14*0.05 wt pet U in magnesium, and 0.004 wt pet Mg in uranium. The solubility of uranium in magnesium decreases to 0.0510.03 wt pet at 675OC, and to about 0.0005 wt pet at 650°C. Due to the reactivity of both uranium and magnesium toward crucible materials, the choice of a suitable crucible presented a problem. Crucibles made from high purity magnesia to which 10 wt pet MgF2 was added to reduce porosity proved to be satisfactory. Some observations made with the use of other crucibles are given. THIS investigation was made to establish the phase diagram for the Mg-U system. Ahmann,' formerly of the Ames Laboratory, did some work on the system. He used several methods in an attempt to prepare Mg-U alloys. One of the methods involved the reduction of UF, with a large excess of magnesium. In these experiments, the magnesium wet the surface of the uranium, but there was no evidence for compound formation. The maximum solubility of magnesium in uranium was indicated to be 0.01 wt pet. In another set of experiments, uranium chips as well as uranium powder were heated in contact with molten magnesium in a graphite crucible for periods of time up to 48 hr. A reaction layer was found at the Mg-U interface in several instances. X-ray analysis of the layer material showed the presence of UC and some additional unidentified lines which were interpreted as indicating the possibility of an intermetallic compound of uranium and magnesium. These studies indicated the maximum content of magnesium in uranium to be 0.043 wt pet. One sample of magnesium which had been heated at 1025°C in contact with excess uranium was found by chemical analysis to contain 0.275 wt pet U. Rules, based on empirical or semi theoretical considerations, which attempt to predict the alloying behavior of metals have been presented in the literature. Although these rules are not infallible, they nevertheless serve as useful guides. Using them, several generalizations can be made concerning the Mg-U system. According to Hume-Rothery's' atomic

Jan 1, 1957

By Harry L. Brown, James M. Dickinson, Philip E. Armstrong

The elastic stiffness coefficients of niobium have been rneaslrred from -150°C to over 650 C and ave in accord with the anomalous temperature dependence previously observed for Young's modulus. This unusual behavior has been shown to be the result of changes in the relative values of the shear elastic coefficients. The bulk modulus remained essentially constant over the temperature range studied, while changes in the shear coefficients produced a more nearly isotropic behavior as the temperature increased. A number of investigators have reported data on the temperature dependence of Young's modulus of polycrystalline niobium. The values cited for the room-temperature modulus ranged from 0.71 to 1.17 x 10" dynes-cm-' (10.3 to 17.0 x lo6 psi) and in each case the modulus was observed to decrease with increasing temperature. In our recent study,8 both polycrystalline and single-crystal samples of essentially strain-free high-purity niobium showed a Young's modulus whose temperature dependence as well as magnitude was strongly dependent on specimen orientation. This was shown to be the result of changes in the relative magnitude of the two shear moduli, C and C'. Young's modulus of polycrystalline samples with strong [110] textures and Young's modulus of single crystals whose orientations were away from the [loo] actually increased as much as 12 pct between room temperature and 1000°C. While studies on the residual effects of previous fabrication, thermal treatments, and impurity contents will probably resolve the problem of the widely differing Young's modulus values observed in polycrystalline niobium, a more complete description of the elastic properties requires an evaluation of the single-crystal elastic constants. A knowledge of these constants can provide a clearer picture of the nature of the temperature dependence, as well as establish a basis for predicting the modulus behavior of polycrystalline niobium, both in the randomly oriented condition and with various fabrication textures. The effects of residual strains on the elastic behavior then can be separated from orientation effects. EXPERIMENTAL METHOD Thin rod-resonance techniques were used to obtain both the Young's modulus and shear modulus of single-crystal specimens. The determination of these moduli as functions of the crystallographic orientation of the specimen axis provided sufficient information to permit calculation of the single-crystal elastic constants. The necessity for torsional as well as longitudinal measurements led to the design and assembly of a vertical-tube vacuum furnace incorporating probes for the simultaneous determination of both longitudinal

Jan 1, 1967

By A. H. Daane, J. J. Hanak, F. H. Spedding

IN the study of the rare earths at the authors' laboratory, methods have been devised for preparing pure rare earths and many of their properties'- have been determined. Very little information is found in the literature on the properties of europium metal, which is the scarcest of the naturally occurring rare earths. Since we have recently prepared europium in appreciable quantities, we are in a position to describe the method of preparation and some of the properties of this metal. Metallic europium was first prepared by Klemm and Bommera who heated a mixture of potassium and EuC1, in vacuo, and obtained a mixture of europium metal and KC1. Trombe4 electrolyzed a molten salt bath containing NaC1, KC1 and EuC1, and collected the europium in a molten cadmium electrode as a cadmium alloy. The cadmium was subsequently removed by distillation but the properties of the residue indicate that pure europium was not obtained. McCoy attempted to prepare europium by distilling mercury from europium amalgam, but the stability of the Eu-Hg intermetallic compounds prevented a complete separation of the two elements. The preparation of very pure europium was suggested by previous work in this laboratory1,4 in which ytterbium and samarium were prepared by heating the respective sesquioxides with lanthanum metal turnings to 1450°C in vacuo and distilling ytterbium and samarium from the mixtures. Subsequently, small test experiments showed that europium also could be prepared by this method. A more detailed version of this method was used in the work described in this paper. Klemm and Bommer3 found by X-ray analysis that the metal had a body-centered cubic (bcc) structure with a lattice constant a, = 4.582 ± 0.00A (converted from kX units), with a bulk density of 5.30 g per cu cm. They found europium to be weakly ferromagnetic. Spedding, et al,7 found a,, to be 4.606 ± 0.001A. Barrett' showed that the bcc structure persists throughout the temperature range 5 to 3000K with a, at 5, 78, and 300°K being 4.551 ± 0.003, 4.551 ± 0.004 and 4.577 ± 0.001A, respectively. Trombe1 described europium as being iron gray, malleable, about as hard as neodymium and not attacked by cold water. He estimated the melting point to be between 1100 and 1200°C. Previous work in this laboratory indicated that the pure metal corrodes rapidly in air and reacts with cold

Jan 1, 1959

By H. M. Otte

Certain choices for the shear elements of the inhomogeneous distortion in the phenomenological theory of martensite formation are examined for their agreement with crystallographic and X-ray data of iron alloys. The assumption that the shear elements must represent slip or twinning systems characteristic of bcc metals is found to covey all observations, even when a small uniform dilatation is taken into consideration. In bct martensite, (011) becomes a possible twinning or faulting plane, in addition to {112), and qualitatively similar X-ray line broadening is to be expected from both. The basic concept inherent in the current theoriesl-4 of the formation of martensite is that the interface between the parent (austenitic) and product (martensitic) phase is an invariant strain plane (i.e., one that is undistorted and unrotated). Experimental evidence that the interface is of such a nature is available in certain transformations2'5'6 but for the transformation in iron alloys direct observation has not proved enlightening. Internal strains resulting from the formation of the small martensite platelets within the parent austenite matrix7 make it difficult to produce the desired evidence. Indirect evidence, however, such as the continuity of scratches in passing from untrans-formed to a transformed region, strongly indicates that the habit plane in iron alloys is an invariant strain interface. The scatter in habit planes in a given specimen8 would suggest that internal stresses have a slight but definite influence. On the other hand, composition changes which affect the lattice parameter can alter the habit plane appreciably, and by an amount greater than the scatter.' The success of the theories depends on the choice made for the "inhomogeneous distortion" or "complementary shear'' in the analysis and also on the choice for the parameter 6 representing a small uniform dilatation. In the approach developed by Wechsler, Lieberman, and Read'," it is implicitly assumed that 6 is unity. In the case of iron alloys, all observations cannot be explained without varying either the inhomogeneous distortion or 6 . Bowles and Mackenzie3 considered only the effect of varying d. They found it difficult to reconcile the wide scatter of habit planes with the theory and were forced to the conclusion that it may also be necessary to consider variations or different choices of the inhomogeneous distortion. Wechsler and Read" considered a limited number of possible choices for the inhomogeneous distortion, but no variation in 6, though this could easily have been introduced if so desired. It is the purpose of the

Jan 1, 1961

By C. S. Barrett, P. Coheur

AXnealing twins are common in the microstructure of copper that has been rolled and recrystallized. In such samples it follows that a twin relationship should exist between components of the re-crystallization texture,' and several examples of this have been reported. For example, twin relationships have been found in recrystallized electrolytic copper sheet, as indicated in Fig. I, from a paper by Coheur and Lejeune.2 In this pole figure the cube texture (100) [001] is indicated by the hollow squares in the lower half of the figure (the pole figure for 200 reflections) and in the upper, (III), part of the figure. The texture contains, in addition to this orientation, the first-order twins of it, shown in the figure by the filled triangles. This orientation relation has been suggested by others also, under certain annealing conditions,3'4 although pole figures have not been published to confirm it. Some orientations in recrystallized sheets are identical with their twins, because of the symmetry elements of the texture— this is true, for example, with the (113) [ZII] texture so commonly reported for brass—hence it appears impossible in such samples to decide whether the twin relationships result from twinning or merely from the symmetry of the deformation process. The present investigation of a commercial copper strip seems to yield an example in which annealing twins account unambiguously for the principal orientations present. It proves to be a case, also, for which the recrystallization texture cannot be viewed as derived from the deformation texture by a first or second-order twinning mechanism. Materials and Methods The samples investigated were of secondary copper (melted in belgium) to which 0.19 per cent iron had been added to raise the recrystallization temperature. How much the orientation characteristics of this metal can be ascribed to the iron content and how much to other impurities or to melting and pouring practice have not been investigated.* The rolling was done in one direction only, on a mill with rolls of about 20-cm diameter. A strip I. cm wide was reduced from 5 mm thickness to 0.05 mm by several cold passes at commercial speeds. The samples cut from this 99 per cent reduced strip were X-rayed throughout their entire thickness. A pole figure made soon after rolling and annealing was identical, within experimental error, with one that was made when a two-year interval occurred between rolling and annealing. X-ray patterns were made on a camera2 that traversed

Jan 1, 1947

By C. S. Barrett, P. Coheur

AXnealing twins are common in the microstructure of copper that has been rolled and recrystallized. In such samples it follows that a twin relationship should exist between components of the re-crystallization texture,' and several examples of this have been reported. For example, twin relationships have been found in recrystallized electrolytic copper sheet, as indicated in Fig. I, from a paper by Coheur and Lejeune.2 In this pole figure the cube texture (100) [001] is indicated by the hollow squares in the lower half of the figure (the pole figure for 200 reflections) and in the upper, (III), part of the figure. The texture contains, in addition to this orientation, the first-order twins of it, shown in the figure by the filled triangles. This orientation relation has been suggested by others also, under certain annealing conditions,3'4 although pole figures have not been published to confirm it. Some orientations in recrystallized sheets are identical with their twins, because of the symmetry elements of the texture— this is true, for example, with the (113) [ZII] texture so commonly reported for brass—hence it appears impossible in such samples to decide whether the twin relationships result from twinning or merely from the symmetry of the deformation process. The present investigation of a commercial copper strip seems to yield an example in which annealing twins account unambiguously for the principal orientations present. It proves to be a case, also, for which the recrystallization texture cannot be viewed as derived from the deformation texture by a first or second-order twinning mechanism. Materials and Methods The samples investigated were of secondary copper (melted in belgium) to which 0.19 per cent iron had been added to raise the recrystallization temperature. How much the orientation characteristics of this metal can be ascribed to the iron content and how much to other impurities or to melting and pouring practice have not been investigated.* The rolling was done in one direction only, on a mill with rolls of about 20-cm diameter. A strip I. cm wide was reduced from 5 mm thickness to 0.05 mm by several cold passes at commercial speeds. The samples cut from this 99 per cent reduced strip were X-rayed throughout their entire thickness. A pole figure made soon after rolling and annealing was identical, within experimental error, with one that was made when a two-year interval occurred between rolling and annealing. X-ray patterns were made on a camera2 that traversed

Jan 1, 1947

By C. S. Barrett, P. Coheur

ANNEALING twins are common in the microstructure of copper that has been rolled and recrystallized. In such samples it follows that a twin relationship should exist between components of the recrystallization texture,1 and several examples of this have been reported. For example, twin relationships have been found in recrystallized electrolytic copper sheet, as indicated in Fig. I, from a paper by Coheur and Lejeune.2 In this pole figure the cube texture (100) [001] is indicated by the hollow squares in the lower half of the figure (the pole figure for 200 reflections) and in the upper, (111), part of the figure. The texture contains, in addition to this orientation, the first-order twins of it, shown in the figure by the filled triangles. This orientation relation has been suggested by others also, under certain annealing conditions,3,4 although pole figures have not been published to confirm it. Some orientations in recrystallized sheets are identical with their twins, because of the symmetry elements of the texture this is true, for example, with the (113) [211] texture so commonly reported for brass-hence it appears impossible in such samples to decide whether the twin relationships result from twinning or merely from the symmetry of the deformation process. The present investigation of a commercial copper strip seems to yield an example in which annealing twins account unambiguously for the principal orientations present. It proves to be a case, also, for which the recrystallization texture cannot be viewed as derived from the deformation texture by a first or second-order twinning mechanism . MATERIALS AND METHODS The samples investigated were of secondary copper (melted in Belgium) to which 0.19 per cent iron had been added to raise the recrystallization temperature. How much the orientation characteristics of this metal can be ascribed to the iron content and how much to other impurities or to melting and pouring practice has not been investigated.* The rolling was done in one direction only, on a mill with rolls of about 20-cm diameter. A strip 10 cm wide was reduced from 5 mm thickness to 0.05 mm by several cold passes at commercial speeds. The samples cut from this 99 per cent reduced strip were X-rayed throughout their entire thickness. A pole figure made soon after rolling and annealing was identical, within experimental error, with one that was made when a two-year interval occurred between rolling and annealing. X-ray patterns were made on a cameral that traversed

Jan 1, 1946