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By R. A. Wagstaff

The method of charging a reverberatory furnace has changed many times since smelting was introduced in this country from the old smelters of Swansea, England. The cause of the latest change at the Garfield plant has been the excessive fineness of the charge due to fine grinding in the concentration of the crude copper ores. The many desirable features of deep-bath smelting as now used at Garfield have been proved. The old method of dropping the charge through holes in the arch (known as center-feed method) causes excessive dusting which makes heavy slag and flue-dust losses, also rapid deterioration of the silica brickwork of the furnace through fusion with the iron oxides from the dust. The purpose of this paper is to describe a gun feeder that was designed to overcome the disadvantages of the older methods of center feeding and still maintain the good features of deep-bath smelting with the hot finer charge. A gun feeder was designed to introduce the finely divided hot calcines under the moving gas stream of the combustion zone and still have them spread in a uniform blanket over the highly heated matte bath. The temperature of the furnace was so great that it was impossible to maintain a stationary feeder, so a movable feeder was designed that could be introduced into the highly heated zone and be withdrawn after the charge had been dropped. It was necessary to protect the nozzle of the gun with a water-cooled coil. Many different types of protected nozzles were tried, such as air jackets, water jackets and heat-resisting steel alloys, but none proved satisfactory. The angle of inclination of the feeder was found to be an important factor in spreading the charge evenly over the surface of the bath. An angle of 34" to 37" was found to be the most advantageous. To allow a continuous flow of ore from the charge car to the point of discharge inside the furnace, the feeder was made with telescopic connections. The pipe leading from the car is stationary and forms the inside part of the telescope. The outside section of the telescope is movable, and is

Jan 1, 1934

By Harold Markus, Gerhard Derge

THE first paper1 of this series described a technique of careful surface preparation by means of which reproducible results may be obtained from potential measurements of the behavior of tin in carbonate solutions with a pH range from 8.4 to 11.2. It then went on to establish the behavior of pure tin electrodes under these conditions and showed that the metal remains active at all times, though the steady potential attained after several hours decreases from I.I2[t] volts at a pH of 12.6 to 0.6 volts at a pH of 8.4. This behavior may serve as a norm with which all other data can be compared. In the second paper,2 small amounts of other anions were added to the carbonate solutions and the conclusion was reached that the common impurities encountered in alkaline materials packaged in tin do not increase corrosion. In fact, in some cases these anions may actually promote the formation of protective films. The present paper rounds out this survey by presenting data on the influence of cations added to the carbonate solutions, as well as the effect of alloy additions to the tin. In many cases the potential data are supplemented with weight-loss measurements. Information is also presented on the effects of some additional anions, the influence of gases above the electrolyte, the behavior of high-purity tin, and the effect of atmospheric oxidation on the corrosion resistance of the above-named alloys. Analysis of the entire body of data discloses some general rules applicable to corrosion in carbonate solutions. The experimental methods used are the same as those previously described. EXPERIMENTAL DATA Cations.-The carbonates of the cations K+, Li+, NH4+, which are soluble, were studied in the same way as the anions, by adding 0.01 mol of the metal carbonate to one liter of 0.2 M sodium carbonate solution, pH 11.2, or to 0.1 M sodium bicarbonate, pH 8.4. The other metallic carbonates are only slightly soluble, of the order of 0 7-3 mols per liter or less, and the sodium carbonate solutions were saturated by adding excess reagent several days before the experiment, shaking frequently, and filtering just before use. The chemicals were c.p. grade in each case except the indium salt. This salt was prepared by solution of the metal in hydrochloric acid and precipitation by addition of Na2CO3. These cations may be divided into two classes, according to their effect on the potential behavior of the tin: (I) normal, (2) passive. To offer a basis of comparison, curves I of Figs. I and 2 are given to illustrate the behavior of tin in carbonate solutions saturated with CaCO3. These curves are the

Jan 1, 1941

By P. M. Robinson, M. B. Bever

THE heats of formation at 273°K of the compounds InBi, In2Bi, and TIBi2 have been determined by metal solution calorimetry with bismuth as solvent. The published information on the thermody-namic properties of these compounds is limited. The structure of the compound InBi (mp, 383°K) is tetragonal of the PbO (B10) type.1 The compounds In2Bi (mp, 362°K) and TIBi2 (mp of highest-melting composition, 486°K) are now believed to have structures of the NizIn (B8) type273 and not the A1B2 (C32) structures reported earlier.4, 5 The compounds In2Bi and TIBi2 have limited homogeneity ranges at room temperature, while the compound InBi has no detectable homogeneity range.' Samples of the compounds were prepared from 99.99 pet Bi (Mallinckrodt Chemical Works), 99.999 pet in (American Smelting and Refining Co.), and 99.99 pet Tl (Amend Drug and Chemical Co.) by melting the components in sealed, evacuated Vycor tubes. The compounds InBi and in2Bi were of the stoichiometric compositions. The compound TIBi2 contained 40 pet T1; this composition was chosen because at room temperature the alloy of stoichiometric composition does not lie within the homogeneity range.' The melts were held approximately 50°C above the liquidus for 8 hr and then quenched into iced brine. The samples were homogenized for 48 hr at temperatures 20°C below the temperature of complete solidification. Metallographic examination of sections taken from the center and the ends of the ingots did not reveal second phases or segregation . The heats of formation were determined as the difference in the heat effects on solution of a compound and of a mechanical mixture of its components added from the reference temperature of 273°K to liquid bismuth at 623°K. The details of the calori-metric procedure and method of calculation have been described elsewhere? The calorimeter was calibrated by adding bismuth at 273°K to the bismuth bath at 623°K. The calculated values of the heats of formation of the compounds, listed in Table I, are based on a value of 4.96 keal per g-atom for the difference between the heat contents of bismuth at 273" and 623oK7 No published values are available for the heats of formation of the compounds InBi and In2Bi. Hultgren et a1.7 have calculated a value of -0.50 i 0.10 keal per g-atom for the heat of formation at 423°K of the compound TIBi2 containing 40 at. pet T1 from heat-content measurements in the range from 398" to 700°K and the heats of formation of the liquid alloy. The difference between this value and the value of -0.66 * 0.01 keal per g-atom at 273°K is too large to be attributed to a difference between the heat capacities of the compound and the components over the temperature range 273o to 423oK7 However, the direct determination of the heat of formation by a calorimetric method should give a more accurate value. The heats of formation at 273°K of the compounds InBi and In2Bi lie on a straight line when plotted as a function of composition, Fig. 1. The compound In2Bi, therefore, appears to be barely stable with respect to its neighboring phases. In order for the free energy vs composition curve to be concave towards the composition axis, the entropy change on formation of In2Bi must be more positive than that on formation of InBi. As the compounds are ordered,2, 3, 8 there is no configurational entropy change on formation. The difference between the entropy changes on formation of the two compounds, therefore, is probably associated with the vibrational entropies. In view of the low heats of formation, the changes in vibrational entropy, due to changes in bond strength on formation of the two compounds, are likely to be small. Owing to the volume contractions on formation of the two compounds,5 the vibrational entropies probably decrease slightly but the decrease of the vibrational entropy of InBi is expected to be larger than that of In2Bi.

Jan 1, 1965

By Richard Hodgson

FMC Corporation, at their mine and soda ash refinery near Green River, Wyoming, currently mines in excess of 3 million tons per year of trona. Upon completion of the current expansion, the mine will be producing in excess of 4.0 million tons per year. The single level mine, approximately 1,500 feet in depth, is currently serviced by five (5) concrete lined circular shafts varying in diameter from 12 ft. to 24 ft. A sixth shaft is complete, but not yet operational and the seventh is currently being sunk. Two of the shafts are equipped with single drum hoists. The original production shaft is equipped with a double drum hoist. The newest production shaft and the main service shaft are both equipped with ground mounted friction hoists. These friction hoists have given excellent service and another will soon be installed as a man and material hoist at No. 7 Shaft. There are a number of advantages that the ground mounted hoist has over a tower mounted hoist. There are also operating problems common to both. FMC's original experience with ground mounted friction hoists began in 1962 with the conversion of a single drum hoist to a friction hoist. The converted hoist was an Ottumwa with a 5 ft. diameter drum and a 4 ft. face. This hoist had been installed at the No. 3 Shaft for some years prior to its conversion to a friction hoist. At the time the conversion of this hoist was made, there were no friction hoists in service in Wyoming. Wyoming mining laws required that all conveyances carrying men be equipped with safety dogs. Since it was desired that wire rope guides be used, safety dogs were impractical. Agreement was reached with the State Mine Inspectors that safety dogs would not be necessary provided that recommended rope safety factors for hoisting men would still be maintained if one hoisting rope was broken. Since-the shaft is approximately 1,500 ft. deep, the recommended safety factor is 6.0 so that this installation has a safety factor in excess of 8.0 for hoisting men when new ropes have been installed. The hoist conversion was engineered by Lake Shore, Incorporated. The friction ring was made in halves and bolted over the original drum face which had been machined to remove the grooves. The ring provided for four 3/4 in. diameter ropes on 8 inch center to center spacing. The pitch diameter of the modified drum was 72 inches. The grove liners are hald in place by hard-wood wedges bolted to the drum. The other modification required by the conversion was an increase in size of bearing caps and the hold-down bolts because of the increased force tending to lift the drum.

Jan 1, 1975

By J. L. Rodda, M. L. Fuller

In connection with an investigation in this laboratory on the high-zinc side of the copper-zinc system, it was observed that well developed segregate structures of the Widmansttten type were formed when a secondary phase precipitated from the solid solution of copper in zinc. This paper presents an analysis of the crystallographic relationship between the segregate and the solid solution matrix. The data to be presented are an interesting addition to the literature on segregate structures in that the plane of segregation is one of the less densely populated planes. In agreement with the generalization of C. H. Mathewson and D. W. Smith' the plane of segregation in the matrix contains the direction of closest atomic packing of the lattice. Furthermore, the matrix and the segregate are both hexagonal close-packed, which has not been reported hitherto in the 1iternture.l The increasing commercial importance of zinc alloys containing copper makes this fundamental study of value to the metallography of zinc alloys. Zinoeich Copper-zinc Alloys Copper enters into solid solution with zinc to at least 1.8 per cent at 400" C., according to W. M. Peirce.3 The solubility is less at lower temperatures. Thus a solid solution of copper in zinc, saturated at an elevated temperature, will precipitate the excess copper in a separate phase at a lower temperature, conditions of concentration, time, and temperature being suitable. The nature of these two phases has been established by the X-ray method of crystal analysis. Westgren and Phmgmén4 and also Owen and Preston5 have shown that the solid solution eta (7) is of the substitu-tional type with copper atoms replacing zinc atoms on the hexagonal

Jan 1, 1933

By J. T. Michalak, H. W. Paxton

The recovery of the initial flow stress of poly-crystalline iron is characterized by a) a logarithmic time dependence; b) an increasing activation energy with increasing recovery; c) an increased ?,ate and fraction of recovery with decreased temperature of deformation; and d) an increased rate with increased deformation. Isochro)ml studies of the recovery of single crystals revealed more sluggish recovery. The original flou3 stress of single crystals could be regained by recovery anneals at 800"or 900°C. ThE great majority of the theoretical treatments and experimental studies of strain-hardening have been concerned with the close-packed lattices.' Very little effort has been expended on the bcc structure so that the theory of work-hardening of this lattice is essentially nonexistent. The limited amount of experimental data resulting from the direct studies on silicon-iron,2 low-carbon steel,3 and purified irons4"7 does not as yet permit a detailed analysis of the strain-hardening. Studies concerned with the effects of annealing following deformation have been few in number," have been somewhat limited in extent, and have had the disadvantage of using irons containing a substantial impurity content. The present research was undertaken to augment the limited knowledge we have of the characteristics of a bcc metal as regards strain-hardening and recovery from the strain-hardened state. The recovery of the flow stress has been employed since it was felt that the stress associated with the hardened state gives at least a fair qualitative description of the state of the imperfections causing the hardening. The study was concerned primarily with the recovery of flow stress following strain-hardening of polycrys-talline, zone-melted iron as a function of the amount of deformation, the temperature of deformation, and the time and temperature of the recovery anneal. A limited investigation of the recovery of the initial flow stress of single crystals of this same material as a function of the recovery temperature was also conducted in conjunction with the Lambot X-ray technique." MATERIAL The zone-melted iron used in this investigation was obtained through the courtesy of the American Iron and Steel Institute and Battelle Memorial Institute. The analysis, as given by the supplier indicated a maximum impurity content of 0.02 wt pct excluding those impurities listed in Table I. (The actual impurity content is very probably less than this since detection limits were considered as the amount of a particular impurity level.) Also listed in Table I are the interstitial impurity contents of the iron at various stages of experimental work indicating that these im-

Jan 1, 1962

By D. Mills, G. B. Craig

ZIRCONIUM has been float-zone-refined in an electron-beam furnace and the redistribution of oxygen, iron, and tungsten has been measured. The iodide zirconium used in the present experiments initially contained both oxygen and iron in the range 100 to 200 ppm by weight, and tungsten in amounts less than 10 ppm. Float-zone refining of zirconium, using induction heating, has previously been attempted by Kneip and Betterton1 and Langeron.2 Kneip and Betterton were primarily interested in the removal of iron and nickel. They achieved some purification, with respect to both these elements, in material given up to six passes at 150 mm per hr under an argon atmosphere. Langeron reported purification for a large number of elements after four completed passes in a static vacuum system operating at pressures less than 10-6 mm of Hg and with rates of zone travel between 30 and 40 mm per hr. He did not report oxygen concentrations, but stated that there was inverse segregation of this element. westlake5 has also used a minimum of four zone passes to remove iron from zirconium. No rates or conditions were given. Belk6 has shown that tungsten contamination can occur during electron-beam melting. He reported an increase from 0.01 to 0.05 pct by weight tungsten in molybdenum after four complete zone passes. The vacuum system for the electron-beam unit used in the present investigation consisted of a single-stage rotary pump backing a liquid-air-trapped oil-diffusion pump. A pressure of less than 10-8 mm of Hg was obtained with Dow-Corning 705 fluid in the diffusion pump. In order to avoid contamination of the zirconium by evaporation from the tungsten filament, a special focusing cage4 was employed. Three rates of zone travel, 114, 38, and 4 mm per hr, were investigated, with the liquid zone moving from the bottom to the top of the bar. The bars used were 3 mm diam and the total melted length was 130 mm. Oxygen was analyzed by neutron-activation analysis using a neutron flux of 10' neutrons per sq cm per sec to form the isotope N16 by the 016 (n,p) N16 reaction. The standard deviation is quoted for each oxygen determination. The iron and tungsten analyses were performed spectrographically, and the precision is estimated to be ±6 pct. Analyses for tungsten were all below the detectable limit of 10 ppm, confirming the protection given by the focusing cage. No significant redistribution of oxygen was found at the two higher rates of zone travel. The redistribution of oxygen and iron obtained after five passes at a rate of zone travel of 4 mm per hr (1.1 x 10-4 cm per sec) is recorded in Tables I and 11. Burris, Stockman, and Dillon3 have estimated the distribution of solutes during multipass zone refining. Using their curves for an effective distribution coefficient of Keff = 1.5 and 2 for oxygen and Keff = 0.3 for iron, the expected concentrations were estimated for the present material. These are shown in Tables I and 11, along with the experimentally measured values. The calculated concentrations are based on a molten-zone length of 10 pct of the total melted length, whereas in the present experiments the molten zone was approximately 5 pct of the total melted length. The effect of zone length on solute redistribution is most pronounced after a large number of zone passes. Comparison with Pfann's published data8 for solute redistribution for various Keff's and zone lengths indicates only small differences at low numbers of completed zone passes. It is evident that the expected distribution has not been realized in the case of iron. Scrapings of material deposited on the inner surfaces of the electron-focusing cage were found to be magnetic. It is, therefore, concluded that redistribution of iron is masked by evaporation. Deposition of iron inside the focusing cage was observed at all rates of zone travel. The results of the investigation may be summarized as follows: 1) Segregation of oxygen is typical for a solute with a distribution coefficient, Keff > 1. 2) No redistribution of oxygen takes place at high rates of zone travel. 3) The distribution coefficient for oxygen lies between 1.5 and 2.0. 4) Purification with respect to iron occurs mainly by evaporation. 5) The focusing cage is effective in preventing tungsten contamination.

Jan 1, 1967

By J. Gurland

The strength variation ofWC-Co alloys with composition and particle spacing falls into two ranges. 1) Above a critical value of the mean free path, the strength follows a dispersion hardening relation; it is proportional to the volume fraction of WC and in-versely proportional to the particle size. 2) Below a critical value of the mean free path, the strength variation is based upon the Griffith criterion of fracture and is controlled by the case of crack propagation. The maximum strength is attained when the structure and load just satisfy the critical conditions for spontaneous crack propagation. THE relation between the strength and the structure of cemented carbides is of interest not only for its own sake but also for its contribution to the understanding of composite materials in general. The cemented carbides are essentially aggregates of a brittle carbide constituent and a ductile binder phase and, at certain structures of intermediate composition, the composite alloys attain strengths far higher than those of the separate constituents in bulk. It is this variation of strength with structure which will be discussed. The experimental procedures of sample preparation, mechanical testing, and quantitative metallo-graphic analysis have been described in Ref. 1. The reported strengths are the maximum fiber-stresses in bending calculated on the basis of completely elastic behavior. The plastic contribution to the over-all deformation is small and was neglected in the calculations (the elongation at fracture of the most ductile alloy, 50 pct WC-50 pct Co, is less than 0.5 pct).2 The pertinent structural parameters are: f, the volume fraction of tungsten carbide; p, the mean free path through the binder phase; the contiguity C, defined as the average fraction of surface area shared by a particle of wc with all neighboring particles of the same phase; and d, the average equivalent spherical diameter of the WC particles. The strength variation of WC-Co alloys with composition and particle spacing is shown in Fig. 1 and Table I, which are based partly on previously published data' and partly on new experimental work which extends the range to higher values of the mean free path. Each data point represents the average of five samples. For a given composition, the transverse rupture strength reaches a maximum

Jan 1, 1963

By L. W. McKeehan, W. C. Elmore

The magnetic powder method, long used for roughly mapping magnetic fields, has recently been refined1, "or investigating the microscopic variations in the surface magnetization of ferromagnetic crystals. Bitter2 first discovered regular powder patterns connected with the crystal structure of such specimens. Several other investigators:' have used Bitter's original technique, with slight modifications, to study the variation of the patterns with variations in the magnetizing field applied parallel to the surface, and their dependence upon the state of strain, of polish and of crystal cut. All of the explanations of these patterns on metallic ferromagnetics have been couched in general terms. In a preliminary report we have described an improvement ill the powder technique which led us to the discovery of a new effect throwing considerable light on the magnetic secondary structure of alpha iron4 and of nickel5 single crystals. We now report additional evidence confirming the existence and stability of a magnetic block secondary structure. Specimens The following list describes the specimens used in the present investigation. Designation Description A1 Silicon ferrite furnished to us by Dr. W. E. Ruder, of the General Electric Co., for which lie gave the following typical analysis: C, 0.05; P, 0.038; S, 0.026; Mn, 0.15; Si, 3.24. Disk, 0.60 cm. diameter, about 0.05 cm. thick. By X-ray analysis angles between disk normal and [100] 75o, [0101 76" [00l] 21o. A2 Same as A1 except: diameter 0.75 cm. A, Same as A1 except: diameter 0.68 cm.

Jan 1, 1936

By L. W. McKeehan, W. C. Elmore

The magnetic powder method, long used for roughly mapping magnetic fields, has recently been refined1, "or investigating the microscopic variations in the surface magnetization of ferromagnetic crystals. Bitter2 first discovered regular powder patterns connected with the crystal structure of such specimens. Several other investigators:' have used Bitter's original technique, with slight modifications, to study the variation of the patterns with variations in the magnetizing field applied parallel to the surface, and their dependence upon the state of strain, of polish and of crystal cut. All of the explanations of these patterns on metallic ferromagnetics have been couched in general terms. In a preliminary report we have described an improvement ill the powder technique which led us to the discovery of a new effect throwing considerable light on the magnetic secondary structure of alpha iron4 and of nickel5 single crystals. We now report additional evidence confirming the existence and stability of a magnetic block secondary structure. Specimens The following list describes the specimens used in the present investigation. Designation Description A1 Silicon ferrite furnished to us by Dr. W. E. Ruder, of the General Electric Co., for which lie gave the following typical analysis: C, 0.05; P, 0.038; S, 0.026; Mn, 0.15; Si, 3.24. Disk, 0.60 cm. diameter, about 0.05 cm. thick. By X-ray analysis angles between disk normal and [100] 75o, [0101 76" [00l] 21o. A2 Same as A1 except: diameter 0.75 cm. A, Same as A1 except: diameter 0.68 cm.

Jan 1, 1936

By W. F. Flanagan, D. H. Polonis, S. D. Dahlgren

Rotation diffraction patterns of Cu-4.84 wt pct Si polymystalline samples were taken during the course of isothel-ma1 affing of the suPersaturated a phase, a diffraction spots were obserzled to streak during the initial stages of aging, and this streaking was similar to the streaking of a spots observed earlier by Barvett with deformed super saturated samples of the same composition. Although it was suggested that stacking faults were the sole cause of styeaking in the deformed samples, the present study has shown that plates with one small crystallite dimension can also contribute to the streaking when there is lattice coherency across close-packed planes. THE decomposition of the supersaturated a phase in Cu-Si alloys has been reported to occur by means of both thermal and stress activation.1-4 According to the Cu-Si phase diagram,3 Fig. 1, the supersaturated a phase (fcc) is expected to transform during aging by the precipitation of the y phase. The results of earlier studies2,4 have indicated that metastable k phase (hcp with nearly ideal close packing) forms initially at temperatures below the eutectoid temperature, after which the k transforms to the a and y phases. Hof-mann et al.4 have proposed a metastable version of the phase diagram, showing the approximate boundaries for k formation below the eutectoid temperature. In view of the close-packed nature of both the a and k phases, it is essential to consider the role assumed by stacking faults in the transformation. Streaking effects have been reported by Barrett 1 in the rotating crystal X-ray patterns of strained Cu-Si alloys and were attributed to stacking faults rather than particle size effects. This deduction was based on the observation that streaks in the diffraction patterns did not occur tangent to the 220fee Debye ring. It is known that the atom movements involved in faulting leave some X-ray reflections unaffected while others are broadened,' and, in particular, it has been shown that faulting will not cause streaking of 220fee reflections tangent to the 220fee Debye ring as would be expected if all the reflections were broadened.' The formation

Jan 1, 1967

By AIME AIME

PETROLEUM technology was the sole subject of discussion at the meeting of the Petroleum Division at the Baker Hotel, Dallas, Texas, Oct. 6-7, except for the brief talks by President Becket and Secretary Parsons at the dinner on Friday evening. Even on this occasion, following the scheduled official features, it was in order to talk "shop." W. E. Wrather and E. A. Stephenson, respectively Chairman and Secretary of the Division, had planned for a meeting of this nature and by preference, apparently, the 122 who registered fell in with the scheme wholeheartedly. Not because the competent local committee had not provided for it, but by choice, the members just did not sign up for entertainment or field trips, but did attend largely the three technical sessions and engage in earnest discussion of the approximately dozen excellent papers. In this connection, and without question, the high lights of the meeting were the papers by Morris Muskat and R. D. Wyckoff, and Prof. W. K. Lewis. The former, entitled, "A Theoretical Analysis of Waterflooding Networks," had been entirely demathematized by the authors for presentation at this and the Los Angeles meetings; the author of the latter, which was on the "Physical-chemical Relationships of Hydrocarbon Gas-liquid Mixtures at High Pres¬sures," had airplaned to Dallas in the company of Dr. H. D. Wilde from Chicago in order to present his paper at the final session on Saturday morning.

Jan 1, 1933

The annual report f the Secretary of the Navy for the fiscal year, ending June 30, 1917, but including operations and recommendations up to Dec. 1 of that year, contains the following remark about the activities of the Naval Consulting Board. The members of the Institute who are members f this Board are William L. Saunders, Benjamin B. Thayer, Thomas A. Edison, Thomas Robins, Lawrence Addicks, Joseph W. Richards, W. R. Whitney, assisted by 47 other members f the Institute, in the capacity of associate members of the Naval Consulting Board. During the year, the work of this board, organized and approved by Congress in 1915, has increased very materially in importance and volume, its meetings have been frequent and the work of its individual members has been such in some cases as to occupy almost their entire time in the service of the Government. Some time before the active entry of this country into war the board called a special meeting to which were invited some 50 of the leading scientists and industrial managers, whose special study fitted them to advise on the methods of meeting the

Jan 2, 1918

By R. J. Evans, A. G. Revesz

Silicon films have been grown by chemical reaction on (111) silicon substrates. The surfaces were examined by various microscopic and interfero-metric methods. Surface structures are classified into two groups depending on whether the angles between the bounding planes and the (111) surface are small (<3 deg) or large (> I0 deg). A layer-gvowth mechanism is postulated to explain the topography and the influence of growth parameters. Growth proceeds by lateral expansion of the (111) layers in (211) directions, thereby forming steps. The step edges are perpendicular to the direction of expansion and are thus along (110) directions. Step bunching md surface nucleation both play an important role in modifying the flow pattern and in the step regeneration. These are influenced ver?) much by impurities, especially oxygen. Although the growth is a result of a surface-controlled ga: reaction, it is very similar to growth from an impure solution. OVERGROWTH ("epitaxial growth") of silicon is important and widely used. During the past years several investigators have observed various topographical features or so-called faults on the grown films. A study of the surface morphology gives some insight into the growth mechanism. I) EXPERIMENTAL Silicon films have been grown on silicon substrates by a method described by Theuerer.&apos; Silicon is formed by reduction of SiCl, in hydrogen. The rate of incidence of SiC1, was varied between 5 x 10"6 and 2 x 10&apos;4 moles min-&apos; cm-&apos;. The mole fraction of Sic4 in the Hz-SiCL mixture was about 5 x X Both the rate of incidence and the mole fraction were calculated on the assumption that the Hz bubbling through the SiC1, reached equilibrium saturation. Assuming uniform velocity distribution, the linear velocity of the gas in the reactor tube was estimated to be 2 cm sec-l. The temperature of deposition was varied between 1070" and 1260°C. Chemically polished p-type silicon wafers of 20 to 100 ohm cm resistivity were used as substrates. These were within 1/2 deg of a (111) orientation. The thickness of the grown n-type film was determined by two methods: a) measurement of the depth of the p-n junction taking into account the junction shift due to diffusion, b) measurement of the traces of stacking-fault tetrahedra on the (111) plane.&apos; The agreement between the two methods was better than 20 pct. The rate of growth varied between 0.2 and 4.0 pmin-&apos;. The formed films were examined by reflection and light-section microscopy, and by multiple-beam interferometry. Phase-contrast illumination revealed height differences of about 30A. For measuring heights greater than 1 p a light-section microscope3 was used. The resolution by multipke-beam interferometry4 was between 50 and 100A. Crystallographic directions on the surface were determined by X-ray and from the orientation of etch pits and stacking faults as revealed by Dash etch (I part HI?, 3 parts HNOJ, and 12 parts CH3COOH). Some specimens have been investigated by electron microscopy. Platinum-shadowing and carbon-replica techniques were used to show the fine topography and reflection diffraction to determine the structure of the grown layers. 11) RESULTS The topographical features can be classified into three groups. he first group is comprised of fine ridges (striations). The second group consists of structures, which are bounded by planes making angles of less than 3 deg with the (111) surface. They are, therefore, vicinal planes. Structures which closely resemble growth or etch pyramids from the third group would normally be bounded by perfect low-index crystallographic planes. In this case they are deformed. The angles between the bounding planes and the (111) surface are generally larger than 10 deg. The fine ridges are present, even on the smoothest surfaces, as shown in Fig. 1. They are along a (110) direction. The height differences could not be resolved with interferometric techniques. The basic characteristic structures of the second group are depressions and hillocks. These are bounded by three planes, two of them with larger slopes than the third one. The edges between the planes, as projected to the (111) surface, point in (211) directions. Various habits of these structures are shown

Jan 1, 1964

By S. R. Goodman, Hsun Hu

A study has hem made of the formation of annealing textures in an 18-8 austenitic stainless steel (Type 304L) from various deformation textures obtained by rolling at different temperatures. When the deformation texture is a mixture of the ferritic type and the brass type owing to the pres -ence of both martensitic ferrite and retained aus-tenite in the specimen, recrystallization takes place by the growth of the existing austenite phase. In a previous report,&apos; it was shown that the rolling texture of austenitic stainless steel (Type 304L) changed gradually from the brass type to the copper type with increasing temperature of deformation above 200°C. These changes are similar to those in high-purity silver2,3 and electrolytic copper;4 a brass-type texture is favored at low rolling temperatures, whereas a copper-type texture is favored During the course of rolling -texture transition from the brass type to the copper type, the subsequent recrystallization textures change accordingly. The orientation relationship between the annealing textures and the various rolling textures, being consistent with previous observations on various fcc metals, can be described as [Ill] rotations of approximately 25 to 40 deg. Carhide precipitation may influence the annealing textures. at high rolling temperatures. Furthermore, the annealing textures in high-purity silver5 and electrolytic copper4 were found to depend entirely on the prior deformation texture. From a copper-type rolling texture a strong cube texture will form upon recrystallization, whereas from a brass-type rolling texture the annealing texture will be quite different from the cube orientation. In an earlier comm~nication,6 the formation of a strong cube texture in 18-8 austenite stainless steels (Types 304 and 304L) was reported briefly by the authors. The present paper constitutes the results of a complete study of the annealing textures obtained from a

Jan 1, 1965

A tentative plan for the Colorado Meeting has been formulated as follows: One day will be spent at Denver, one day at Colorado Springs, one day at Cripple Creek, a trip by automobile to the top of Pike&apos;s Peak, one day at Pueblo, one day at Leadville. All the principal mines and mills of the districts mentioned will be visited, including the gold mines in Cripple Creek, the lead, zinc, and steel works. of Pueblo, the production of ferro-molybdenum by electric furnace at Leadville, etc. Special arrangements are being made for the social entertainment of ladies at all points; one evening at Colorado Springs will be devoted to a reception and dance, and the usual dinner will he given on another evening. The following papers have already been accepted for the Colorado Meeting, and some have already been published: Fireproofing Mine Shafts by the Anaconda Copper Mining Co. By E. M. Norris. (March Bulletin.) Air Blasts in the Kolar Gold Field, India. By E. S. Moore. (March Bulletin.) The Use of Coal in Pulverized Form. By H. R. Collins. (April Bulletin.) Coal Mining in Washington. By F. A. Hill. (April Bulletin.) Carbocoal. By C. T. Malcolmson. (May Bulletin.) Gaging and Storage of Oil in the Mid-continent Field. By O. U. Bradley. (March Bulletin.) An Interpretation of the So-called Paraffin Dirt of the Gulf Coast Oil Fields. By A. D. Brokaw. (April Bulletin.) The Theory of Volcanic Origin of Salt Domes. By. E. DeGolyer. (May Bulletin.)

Jan 5, 1918

By Charles B. Henderson

DESPITE the loss, by enemy conquest, of a high percentage of our normal sources of supply for tin, the position of this important metal is easier today than that of rubber and a long list of other strategic materials, many of which are produced in this country. Actually, there is no shortage of tin for essential war purposes, owing to a strict control of its use, to increasing considerably the amount of secondary tin available, and to the foresight of the Government in authorizing the Reconstruction Finance Corp., as early as June, 1940, to acquire and produce certain critical and strategic materials of which tin was one of the most important. The construction of the Longhorn Smelter on the Gulf Coast in Texas is an important part of this program.

Jan 1, 1943

By John P. Hager, Igor A. Wilkomirsky

The thermodynamic properties of the Pb-Ag system have been determined between 775° and 950°C by the cell: Electrotransport measurements on silica-saturated PbO-SiO2 melts established that the conduction was entirely ionic and that lead is present only in the divalent state. The activities of lead and silver exhibit Positive deviations from ideal behavior. In dilute solutions the activities of lead and silver follow Henry&apos;s law. The values obtained for yhb and yig at 1200°K are 1.49 and 1.69, respectively. Determination of a portion of the liquidus curve agrees well with the established phase diagram. provides an accurate means for the thermodynamic study of liquid alloy systems. However, Wagner and wernerl have shown that cells of type I are limited to alloy systems for which the reaction at the alloy-electrolyte interface will be extremely small. The traditional electrolyte for cells of type I has been a low melting point mixture of group IA chlorides, to which a small amount of the compound ACIZa has been added. However, the choice of a chloride electrolyte may not always be practical, in that the Gibbs free energies of formation of the compounds ACIZ, and BCIZb may not be sufficiently different to minimize Reaction [I]. On the other hand, the Gibbs free energies of formation of the oxides of metals A and B may be sufficiently different to minimize Reaction [I]. In this case, the use of molten oxide electrolyte would be clearly advantageous. In the present study, the thermodynamic properties of the Pb-Ag system have been investigated using the cell: Previous galvanic cell studies on the Pb-Ag system2&apos;= are not reliable due to the displacement reaction between the alloys and the chloride electrolyte. Wagner and ~erner,&apos; using Laitinen and Liu&apos;s&apos; value at 450°C for the standard electrode potential of Reaction 111, have estimated the percent error in the activity of lead bPb) when using a chloride electrolyte. At 1000°C the error for xpb = 0.10 is 12 pct. Taking the Gibbs free energies of formation for PbClz and Ag cI,&apos; and the equations of Wagner and Werner,&apos; the error in apb at 1000°C and Xpb =0.10 was calculated to be 140 pct. However, using the Gibbs free energies of formation for Pb O&apos; and an estimated value for Ag 20, the error in apb when using a molten oxide electrolyte at 1000°C was estimated to be less than 1 pct for The virtual reaction of cell I1 for the passage of n Faradays of positive electricity from left to right in the cell is: where 5 is the Faraday equivalent (23,063 cal per v equivalent), E is the electromotive force of the cell in volts, and n is the number of Faradays of electricity required for the transfer of 1 g-atom of lead through the cell. The value of n should be equal to 2 since lead is generally divalent in oxide melts. However, the presence of either tetravalent lead ions or electronic conductivity through the molten oxide electrolyte will result in a value of n greater than 2. Bockris, Kitchener, and Davies&apos; have determined the amount of ionic conductance in a liquid PbO-SiO2 mixture (xPbO= 0.50) at 920°C by measurement of the volumes of CO and C& evolved at a carbon anode during electrolysis. From their data a value of 2.13 * 0.16 was calculated for n. Although their measurements indicate the possible presence of multivalent lead ions and/or electronic conductivity, their measurements were not at silica saturation and no definite conclusions can be drawn. However, as a result of the electrotransport measurements described in the next section the ;due of n can be taken as equal to 2.

Jan 1, 1969

By E. F. Bailey, W. J. Harris

THE temperature of the ferrite to austenite re-action is established frequently by continuous heating experiments. However, equilibrium studies of this reaction have demonstrated that austenite may form at temperatures considerably below those at which the reaction is first observed during continuous heating. Because of this discrepancy, tempering is sometimes performed above the true critical temperature and in these cases austenite forms during tempering. The lowest temperature at which austenite forms and the kinetics of the reaction have been studied by Bain,&apos; Bleakney and Gros-venor,2 and Dube and Cunningham. This austenite can affect the properties either as austenite per se, if it is retained at room temperature, or as a decomposition product if it transforms. The effect of austenite formation during tempering on low temperature impact properties of an 8 1/2 pct nickel steel was reported by Brophy and Miller4 in work published after the present investigation was initiated. They concluded that the improvement in low-temperature notch toughness which followed tempering at certain temperatures could be attributed to the austenite formed during tempering. Kramer et al.5 found anomalous hardness increases and embrittlement after tempering of a low-carbon manganese-nickel steel. They concluded that austenite formed during tempering, and that the decomposition products were responsible for the increase in hardness and the embrittlement. Quan-titative correlations of the microconstituents and mechanical properties were not made by these investigators. The present study was undertaken in order to establish the kinetics of formation of austenite at various temperatures, the characteristics of the decomposition of this austenite, and the relationship between mechanical properties and the phases present. Experimental Procedure A low-carbon manganese-nickel steel was selected because of the sluggishness of its austenite decom-position reactions. The composition of this steel in percent was: C, 0.10; Mn, 3.52; Ni, 2.34; Mo, 0.52; Cr, 0.17; Si, 0.19; V, 0.15; P, 0.019; and S, 0.020. Samples were prepared by forging sections from a large ingot to 3/4 in. bars. Formation and decomposition of austenite were investigated by dilatometric techniques which were checked by X-ray measurements. Dilatometer specimens were hollow cylinders 1 in. long, 1/2 in. diam, with a 1/8 in. central hole. All specimens were aus-tenitized for 1 hr at 1650°F and quenched in water prior to insertion in the dilatometer. Oxidation was prevented by using an inert atmosphere of purified nitrogen. Dilation was measured with a dial gauge which could be read by interpolation to 0.00005 in. Temperature was maintained within ± 3°F by a Brown Electronik Controller. Chromel-alumel thermocouple leads were welded to opposite ends of the specimen with the specimen serving as the hot junction. As a check on temperature uniformity comparison was made of the specimen temperature as measured with the chromel-alumel leads and the temperature of the center of the specimen as measured with a calibrated platinum—platinum-rhodium thermocouple embedded in asbestos in the central hole of the specimen. During heating a 5°F temperature difference was noted below 1000°F, but none above, while in cooling, a 5°F difference was observed from 1300" to 735°F, but none below. Heating rates of 35°F per min and cooling rates of 60°F per min were employed for all dilatometric studies. For transformation studies below room temperature, the dilatometer was allowed to cool to 150°F and then was quenched into liquid nitrogen.

Jan 1, 1951

By R. C. Gifkins, K. U. Snowden

The value of the index n in power ktivs for the stress sensitivity of minimum creep rale at lead is derived front results drawn from lite literature and from previously unpublished nork on commercial (99.99 pel) and high-purity (99.999 pel) lead polycryslalline and hi crystal specimens. In tests al 0.5Tm (22 to 50&apos;C) for slvesses below 250 psi, n fulls to mily for poly-cr,yslullirle specimens, single crystals, and bicrystals, and toy grain boundary sliding in bicrystals. Between 250 and 500 psi there is a tyansilion range and, for the polycrystalline specimens al least, u high-stress regime for 500 to 1500 psi where n is 5 or 6. These results are such that none of the suggested stress taws can he used to extrapolate to very loir stresses. Meclianisms for deformation in Ike grains and toy grain boundary sliding in the low-strcss regime are outlined. In particular, the mechanism for grain boundary sliding involves sliding controlled by diffusion from tensile to compressire Ledges. predictions based on this model give promising numerical agree-nicul with experiment. II is suggested that the mechanism for grain boundary sliding may he important in other circumstances, e.g., in creep of ceramic materials or superplaslicity, because it can operate with lille or no dislocation aclirity. WhEN the stress dependence of secondary creep rate is represented by a power law the values taken by the stress exponent n are found to vary between 1 and 7, see, c.g., Garofalo.&apos; In Eq. 1 11 u is the applied stress and A a constant. The case for accepting values of v = 1 rests principally upon tests at high temperatures (>0.9Tm) and there have only been isolated tests at lower temperatures (rather than plots of creep rate against stress) for which the creep rates are such that some form of Nabarro-Herring creep with n = 1 is applicable. Hanson5 and Greenwood and cole6 plotted creep rate against stress for tests made in the vicinity of 0.5Tw, and found a "creep yield", so that below a certain low stress the creep rate was linearly related to stress: these observations appear to have been subsequently ignored. Various models have been proposed which agree with a large body of experimental results in which n equals -5 at high stresses (e.g., weertman7 and McLean8). Various alternatives to Eq. [1] have been proposed principally as a means of unifying creep data, but sometimes, it seems, in order to obviate the necessity for assuming a series of regimes of deformation associated with the various values of n; further refer- ence to these will be made in the section on stress laws. This paper calls attention to extensive results which show n = 1 for the creep of lead at room temperature (0.5 T,). RESULTS Fig. 1 is a composite diagram based on figures in the literature6,9,10 with additional results obtained by the present authors and their colleagues11,12 in the course of a number of investigations not directly concerned with stress sensitivity. In Fig. 1 In creep rate is plotted against In stress. The curves show results for two kinds of material. Lead I is of commercial purity (99.99 pct Pb) and lead IT a specially refined material, hydrogen-purified to remove oxygen; it contains 99.999 pct Pb. Curve A is for lead I in polycrystalline form (grain diameter 0.02 to 0.05 cm) at room temperature (22&apos; to 26°C). Curve B1 is for lead I, polycrystalline, tested at 50C. Curve B2 is for lead 11, polycrystalline (grain diameter 0.02 cm), tested at room temperature (22 O- Curves C to F relate to tests made of bicrystals of lead 11: all of the same nominal orientation ("Y" in Ref. 12). Curves C and V are for creep within the component crystals of the bi crystals at 22°C (AB and CD in Fig. 2). Curve E is for creep measured in a gage straddling the boundary, approximately 0.15 mm either side (BC in Fig. 2). Curve F shows rates of grain boundary sliding (as distinct from strain rates in the other curves), obtained by averaging the offsets of six marker lines on the bi-crystal boundaries. The principal feature of the results is that the stress sensitivity falls into two distinct regimes, according to whether the stress is below approximately 250 or above 500 psi (there is a transitional range between 250 and 500 psi). The new result is that below -250 psi two of the curves (A and BI) give a value of n 1, and the other curves also drop below n - 2 to -1.5 but do not extend to low enough stresses to show clear evidence of n 1. At very high stresses the curves tend to give values of n - 6, as previously determined in other investigations. Curve R2 for the high-purity lead in polycrystalline form at room tenlperature almost merges with B, and thus gives new significance to the values for stresses of 150 and 200 psi; previously&apos;3 these points had seemed to fall away from the curve of slope -3, but they now can be seen as almost completing a transition to n = 1. It should be noted that there was originally considerable apparent scatter in the results for the high-purity lead. However, this was found to be associated with annealing conditions or variations in residual content of oxygen and curve B2 was constructed using the highest rate (i .e., the rate for the purest lead) determined for each stress during the course of various investigations over the years: altogether, some forty tests were used in constructing curve R2.

Jan 1, 1968