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By M. Metzger, T. A. Read

The strengthening effects of hydroxide and synthetic plastic films in the creep of cadmium crystals were studied. The results were broadly consistent with the naive mechanical model. The dislocation-film reactions and the significance of the macroscopic stresses associated with certain films are discussed in the paper. ALTHOUGH a number of studies have been made of the strengthening of metal single crystals produced by surface films usually less than Ir in thickness, the mechanisms underlying this phenomenon are still not well established. Roscoe' first noted the critical shear stress and the stress-strain curve of cadmium-crystal wires to be raised markedly by the presence of oxide films. Subsequent investigators2-' have confirmed the effect for several metals and films including a number of plated poly-crystalline metal films. Harper and Cottrel1" with a thin film on zinc presumed to have formed as a result of etching and washing treatments) did not detect a strengthening at a rate of extension of 10 ' sec-' although at lo-' sec-' the film raised the flow stress by 7 pct at 0.0005 extension and by 22 pct at 0.01. The marked strengthening at moderate strains thus appeared to be the result of a dynamical effect dependent on the rate and amount of plastic flow. Other observations'. " are consistent with this view. The large effects of films on the tensile creep rate of single crystals were demonstrated when the observation of Andrade and Randall," that the creep rate of cadmium crystals increased on immersion in aaueous solutions of certain cadmium salts. was shown' * to hold only when a film was present initially and was explained by the attack of the solution on the film and the removal of its strengthening effect. Changes in the creep rate interpretable in terms of the removal or formation of various films have been observed by other investigators.3,8,10,31 Certain other experiments have been reported in which surface films or liquid environments have affected the plastic behavior of metals, but these are not within the scope of the present work which deals with the effect of solid films on single-crystal slip. Possible Mechanisms—The film does not significantly reduce the load on the crystal in the elastic range (the elastic moduli of film and crystal are not too greatly different and the area of the film is so small that its share of the load is negligible) so that the initial operation of internal Frank-Read sources is not affected. However, as Fisher" has pointed out, a source terminating on the crystal surface requires only half the critical stress for activation as an internal source of the same length and a relatively strong film (even a very thin one) would pin the free ends of the surface sources so that, if surface sources are responsible for plastic flow in a clean crystal. such a film would increase by roughly a factor of 2 the stress necessary for generation of dislocation loops at a given rate. The other general possibility is that the film resists the passage to the crystal surface of internally generated dislocations. If the film is adherent and if the specimen is to exhibit slip of the same general character as a film-free specimen, the film must deform or fail in shear at the active slip planes. The naive mechanical model, where shear-stress relaxation across the active slip plane in the metal transfers load to the film until it deforms and slip can

Jan 1, 1959

By J. J. Gilman

WHEN a zinc crystal is immersed in liquid N, and then plastically bent, it is observed that it bends a certain amount and then fractures. This fracture occurs at a fairly reproducible radius of curvature, and the radius varies systematically with the crystal orientation. Because this phenomenon provides an unusually well-defined set of fracture conditions, it is possible to examine various possible fracture criteria and select the best one. Zinc crystals of various orientations were bent about axes lying in their glide planes (0001) and perpendicular to their glide directions [1210]. The crystals were 0.150 in. diam and had chemically polished surfaces. They were immersed in liquid N, while they were being loaded on an Instron testing machine. A three-point bending jig was used to load them. Table I lists the beam radius at which fracture occurred for each orientation. Each value is the average of at least six measurements. The normal stresses on the cleavage planes, at the time of fracture, were calculated as follows: First, from the fracture radius, R,, the orientation angle, x,, of the (0001) plane at the outer fiber was calculated. If x, = angle between the (0001) and the rod axis prior to bending, d = rod diameter, and X, = angle between the (0001) plane and a tangent to the bent crystal, then1 sinX, _ 2R, sin xn 2R, + d Since the glide shear strain is given by' y ' cot X, — Xo the glide strain at fracture, x,, can be calculated. Next, it is necessary to know the tangential stress in the outer fiber at fracture. This depends on the plastic flow curve, so a series of tensile tests were performed at —196°C on another set of zinc crystals. A curve of the average resolved shear stress versus glide strain was prepared. From this curve, shear stresses, r,, corresponding to the glide strains in the bend tests were taken. These values are listed in Table I. Then the normal stresses in the outer fibres, u,, were calculated from the relation U, = r, tan X, This analysis assumes that the fiber stresses in a bent beam are the same as the stresses in simple

Jan 1, 1959

By J. Chipman, N. J. Grant, H. L. Bishop

Lime and dicalcium-silicate crucibles were equilibrated with molten iron and liquid slags containing iron oxide and small amounts of sulfur. The oxygen content of metal, iron oxide activities, and desulfurization values of the slags were determined in the temperature range 1530 to 1700°C. The influence of magnesia in the slag and the temperature dependence of the solubility of lime in liquid iron oxide and the ferric oxide content were established. The temperature contour of the liquidus surface of iron-silicate slags saturated with lime and dicalcium silicate was also established at 1600°C. THE importance of the role that slag composition plays in the refining of steel has been known for many years. Numerous studies have been made using actual plant data in order to establish the relationship between the composition of the slag and metal during the refining of a heat of liquid steel. These results rarely represent equilibrium conditions since completion of the various chemical reactions involved in steelmaking is seldom realized. In order to establish quantitatively the equilibrium conditions existing between the slag and metal, several laboratory studies have been conducted in the past 20 years to determine the reactions important in slag control. These investigations have included studies of simple liquid basic and acid slags as well as more complex slag systems which approach those commonly found during the refining of a heat of steel. Since most of the previous studies of simple basic iron-oxide slags equilibriated with molten iron were made in magnesia crucibles, it was not possible to establish the distribution of sulfur and oxygen between molten iron and slags consisting only of the three essential components, lime, silica, and iron oxide. This investigation was undertaken to establish the equilibrium conditions for simple lime-iron oxide and lime-silica-iron oxide slags. Accordingly, it was expedient to prepare crucibles both of lime and dicalcium silicate to establish the equilibrium conditions between molten iron and iron-oxide slags saturated with the refractory materials and free from other components. The only other studies of the equilibrium between molten iron and lime-saturated slags are those of Fischer and vom Ende, 1, 2 in which the solubility of oxygen was determined in an air atmosphere. The

Jan 1, 1959

By R. N. Edmondson, L. Mair, M. Tenenbaum

It is the policy of The Metallurgical Society to provide, in the TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AIME, a prompt and accurate medium for publication of reports of significant new research in both the scientific and engineering aspects of metallurgy. Papers submitted to the Society are judged by competent reviewers according to established criteria for technical merit, accuracy, originality, and presentation. STAFF: Editor, Dr. Gerhord Derge; Editorial Assistant, M. A. Redmyrski; Staff Coordinator, James J. Burke. THE METALLURGICAL SOCIETY: W. R. Hibbard, Jr., President; J. C. Kinnear, Jr., Past-President; John Chipmon, Vice President; T. D. Jones, Treosurer; R. W. Shearman, Secretary. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: A. w. Thornton, Chairman; Dennis Carney, John Chipman, J. C. Fulton I. H. Hollomon H. H. Kellogg, A. E. Lee, R. Maddin, J. D. Sullivan, and D. Swan. Review and selection of manuscripts is under the supenision of the following Publications Committees: Extractive Metallurgy Division: T. 0. King Chairman; S. J. Dickenson, R. P. Hermsdorf R. Schuhmann. Jr.. and P. T. Stroup. Institute of Metals Division: Robert Maddin, Chairman F. Lincoln Vogel Jr., Vice-chairman, W. A. Baikofen, R. W. Boliuffi J. H. Bechtold M. B. Beyer. R S. Busk, C. G. Gaetzel, Paul Gordon C. D. Groham, Jr., Robert F. Hehe-mann,' R. I. Joffee, F. c. Joumot Jr lrving R. Kramer A. J. Lena Harold Morglin, C. J. McHargue, Russell A: Meussner, J. B. Newkirk H. W. Paxton, G. E. Pellissier, I. S, Servi, Alon U. Seybolt, A. J. Shaler, and Jack Washburn. Iron and Steel Division: J. C. Fulton, Chairman; T. B King, F. C. Langenberg, W. 0.. Philbrook, and T. 0. Winkler. Published bimonthly by the American Institute of Mining Metallurgical and Petroleum Engineers Inc., 29 West 39th Street, New York 18, N. Y. Telephon: pEnnsvlvanio 6-9220. Subscription 522 Per year for non-AIME members in United States and North South and Central America; $25 foreign;, $5 for AIME members. Single copies, 54.00, single copies foreign, $5.00. The AIME is not responsible for any statement made or opinion expressed In its publications . . . Copyright 1958 by the American lnstltute of Mining Metallurgical and Petroleum Engineers Inc. . . . Registered cable address AIME New York , . . lndexed in Engineering Index Industrial Arts Index and Chemical Abstrats . . . Application for second class mail privileges ii pending at New York, N. Y. Volume 212, Number 4.

Jan 1, 1959

By S. R. Seagle, R. Schuhmann, N. A. Parlee

Rates of CO evolution and CO absorption were measured for liquid-iron alloys containing from 0.15 to 4.4 pet C, using a modified Sieverts apparatus. The alloys were held in alumina crucibles, so that both crucible-metal and gas-metal reactions occurred simultaneously. The data are interpreted on the hypothesis that the C-O reaction rate is controlled by oxygen diffusion across the boundary layers at the gas-metal and crucible-metal surfaces. CARBON-monoxide evolution from liquid Fe-C-0 alloys is a key reaction in steelmaking processes, both in the steelmaking furnace and in the ingot mold. Also, this reaction probably is an essential step in the desulfurization of iron under blast-furnace conditions, for which carbon is the principal reducing agent or deoxidizer present in the iron. The thermodynamic properties of the solutions of C and 0 in Fe and the equilibria of these solutions with gaseous CO and CO, have been investigated in some detail and are reasonably well understood. However, while these equilibrium data have accumulated in the laboratory, other data have accumulated to show that equilibrium conditions are often not achieved under plant operating conditions. Thus, an understanding of the rate and mechanism of the carbon-oxygen reaction not only has theoretical interest, but ultimately may assume considerable practical importance. Reaction Mechanisms and Rate Equations The over-all reaction under consideration is C (in liquid Fe) + 0 (in liquid Fe) + CO (gas) [I] Although this appears to be a straightforward heterogeneous reaction, involving just two phases (liquid metal and gas), a wide variety of reaction mechanisms has been proposed. Different authors have expressed divergent views as to the nature of the rate-controlling steps. Accordingly, a brief discussion of the possible reaction steps will be given. 1) Homogeneous Reaction Within Liquid Iron— Feild' and Jette2 have applied chemical reaction-rate theory as if the C-0 reaction were a homogeneous, second-order reaction occurring within the liquid-metal phase. This mechanism necessarily produces CO "molecules" dissolved in liquid iron. In order to yield CO gas, the dissolved CO must nucleate CO gas bubbles, and the dissolved CO also must be transported to the bubble surface where it enters the gas phase. However, this mechanism is inconsistent with present concepts of the structure of liquid-metal solutions. 2) Reaction at Gas-Metal Interface—At the surface of contact between gas and metal, a second-order reaction between dissolved C and 0 may occur to produce a CO molecule which enters the gas phase. This reaction presumably involves an "activated complex" structure in the interface. Some such surface mechanism appears essential because the carbon and oxygen do not occur in the same species in the two phases and therefore must react in some way at the surface. At liquid-iron temperatures, calculations based on reaction-rate theory indicate that the surface reaction must proceed extremely rapidly and thus cannot be a rate-determining step in the C-O reaction under ordinary conditions.3 ccordingly when the over-all reaction is measurably slow, the surface reaction may be considered at equilibrium; that is Cc* Co* = m'Pco [2] in which Co* and Co* are the concentrations of carbon and oxygen (weight per unit volume of metal), respectively, in the liquid-metal phase at the interface, Poo* is partial pressure of CO in the gas phase at the surface (atmospheres), and m' is the mass-action constant for Reaction [I]. Since activities of C and 0 are not strictly proportional to concentrations, m' is not a true thermodynamic equilibrium constant but varies with carbon content.' 3) Mass Transport—If the reaction is to proceed at the gas-metal surface, as described above, dissolved carbon and oxygen in the liquid iron must come to the surface and gaseous carbon monoxide must move away from the surface. Details of the mass-transport mechanisms depend on the kind of system under consideration. For a stirred metal bath in contact with a CO gas phase, the transport of C and 0 to the surface can be described by 1 Do Mols CO evolved per sec = — 1/16— Do/do Agm (CO-Co*) = 1/12 Do/do Agm *(Co-Co*) [3] In this equation, Do and D, are the diffusion constants for oxygen and carbon in liquid iron, 6, and 6,. are the boundary-layer thicknesses, A,,,, is the

Jan 1, 1959

By C. T. Holland

This discussion is concerned with those com-J- paratively infrequent bumps that eject material from the failed mass with enough energy to wreck heavy machinery and seriously injure or kill people. In such cases there is a loud report, and the pressure waves set up in the mine atmosphere wreck ventilation controls several hundred feet from the site of the failure. Vibrations are induced in the earth's crust which may be detected several miles from the point of origin, and explosive gases may be released in large quantities." Usually a dense suspension of dust is produced from the failed mass, together with dust placed in suspension by the resulting air blast. These rock bursts or bumps have also been called mountain shots, bounces, pillar bursts, and crumps. Such occurrences, when extensive, are serious catastrophes, and may force abandonment of the mine.' CAUSES OF ROCK BURSTS Rock bursts in coal mines have occurred in sev-eral places under diverse geological conditions, mining methods, and/or practices. A study of many such occurrences indicates that they depend on the following conditions: 1) cover thickness of 500 ft or more, 2) cover composed of strong members and having a strong member lying close to or on the coal bed, and 3) a floor that does not readily heave. The minimum thickness of cover under which coal mine rock bursts occur is based on observation. Under unusual circumstances involving very strong roof members and/or mining systems, and/or practices especially likely to induce bursts, a burst conceivably could occur under less roof. Under special circumstances rock bursts have occurred in marble quarries almost at the surface.' Furthermore, under very heavy cover it is likely that controlling roof members need not be as strong and as close to the coal bed to cause bumps. Just what constitutes a strong roof or roof member is open to question. Obviously the strength of a roof member is determined by its thickness, the distance between bedding planes across which little or no bond exists, the spacing and development of joints, and the inherent strength of the rock material. Strata sections showing roofs under which rock bursts in coal mines have developed are illustrated in Fig. 2. In several instances the strength of rocks composing the roof of mines developing bumps has been tested. The tests (Table I) show that these rocks develop considerable strength in compression, bending, and shear and that in some cases the strengths are very high. No quantitative data are available concerning joints in roof members over coal beds where rock bursts have occurred, but the author has examined many mines subject to bursts and has received the impression that joints in the shales immediately over the coal beds are always present and well developed. In the main sandstone or conglomerate members themselves, however, where observed, he has yet to see a fracture system indicating well developed joints. Undoubtedly joints are present, but the evidence indicates that they are few, poorly developed, and widely spaced. In a mine subject to bumps, moreover, actual measurements of roof spans up to 225 ft between supports under a cover of about 800 ft have been made before roof failure occurred. Such spans signify strong roof. In coal beds subject to rock bursts, the bottom rock is usually a sandy shale. A few tests (Table I) have been made on the floor rock of coal beds. Observations in mines indicate that they are usually weaker than roof rocks and that under load they show more plastic effects. Observation in ground subject to bursts invariably indicates a relatively strong floor highly resistant to heaving, although some heaving may occur. Other factors listed as favorable to rock bursts are: 1) mountainous surface; 2) steeply dipping beds; 3) proximity of faults, folds, and other similar geologic structures. Many bursts have occurred in mines under mountainous country, although many bursts in mines under a surface with little relief indicate that thickness of cover, not relief, is the essential factor. In steeply dipping beds, many bursts occur in mines that are essentially flat, and rock bursts have been recorded in beds dipping as much as 35o Most rock bursts in the U. S. occur in beds that dip less than 10 pct. It is also true that most U. S. coal is produced from beds dipping less than 10 pct. Geologically, faults are regarded as providing stress relief, but in the vicinity of faults, as well as sharp folds, it would seem that residual stresses could be present. The fact that rock bursts occur in areas remote from faults and sharp folds suggests that their presence is not necessary for this phenomenon to take place. There have been many bursts close to faults and folds, and it may be assumed that occasionally such structures accentuate their occurrence3 The conditions and circumstances under which they occur, coupled with the effects produced, leave In the Crowsnest Pass coalfield, British Columbia, a rock burst is estimated to have released 1.8 million cu ft of methane.

Jan 1, 1959

By J. H. Keeler

QUESTIONS raised during earlier investigations of the preferred orientation in titanium1 and zirco-nium sheet led to the examination of the rolling and annealing textures of beryllium and hafnium sheet. Since the c/a ratios are 1.568 and 1.584, less than that of ideal close packing, 1.633, it would be expected that the preferred orientations would be similar to those exhibited by zirconium and titanium. This was found to be true. However, in several regards the orientations observed for beryllium differed from those reported by Smigels-kas and Barrett4 and so are given here. The okientations for hafnium are presented since only the cold-rolling texture has been reported in the unclassified literature. The pole figures were determined by transmission using an X-ray spectrogoniometer with copper Ka radiation and the automatic pole-figure recorder designed by Geisler described previously.6 The intensity units in the pole figures in this case are only arbitrary since calibration against a random sample of the same material was not considered necessary for the original purpose of the examination. The beryllium sheet, cold-rolled from 0.036 in. to 0.006 in., a reduction of about 84 pct, exhibited a split texture with the [1010] direction in the rolling direction as shown in Fig. 1. The same specimen annealed in vacuo for 1 hr at 1000°C showed no change in orientation. These textures

Jan 1, 1959

Univ of Alabama-University, Alabama-Mining and Metallurgical Society William L Mason, Faculty Sponsor, E C Wright, Dept Head Univ of Alaska-College, Alaska-Mining Society of the Univ of Alaska Douglas W Huber, Faculty Sponsor, E H Beistline, Mining & Metallurgy Dept Head, Troy L Pewe, Geology Dept Head, James Crawford, Chapter Counselor Univ of Arizona-Tucson, Arizona-Miners Society Willard C Lacy, Faculty Sponsor, J D Forrester, Mining & Metallurgy Dept Head, F W Galbraith, Geology Dept Head Univ of California-Berkeley, California-Mineral Technology Association H E Hawkes, Faculty Sponsor, Joseph A Pask, Dept Head

Jan 1, 1959

By O. D. Sherby

In 1938, Kanter' revealed that the steady-state creep rate of low-carbon iron alloys could be correlated by an activation energy expression, where the activation energy for creep, Qc, was found equal to about 90.0 kcal per mole for most of the alloys investigated. He suggested that creep at high temperatures might be controlled by some sort of solid self-diffusion process since the value of Qc was about equal to the known value for self-diffusion, Qd. Correlations were not further attempted along these lines until many years later, when new evidence2-8 was presented suggesting that Qc = Qd for many metals. This equality now appears to be established for ten metals (Al, Pb, Ni, Mg, Cd, In, a Fe, y Fe, Cu, and Au). This experimental fact prompted several investigators to postulate various mechanisms of dislocation motion which would yield an activation energy for creep equal to that for self-diffusion.7-9 Possibly the most accepted theory is that based on dislocation climb7 where a dislocation is envisioned to surmount a barrier by an atom-vacancy exchange process, thereby "climbing" from one slip plane to another. Such a model would suggest that the steady-state creep rate, i, should be directly proportional to the rate of self-diffusion, D, for a given creep stress. In order to more clearly reveal the relationship between creep and diffusion, and to eventually determine the correct model, it would be desirable to obtain data showing correlations between i and D, rather than with a comparison of the temperature coefficients, Q. It has been known for some time that the self-diffusivity of iron atoms is greatly decreased when body-centered-cubic (a) iron transforms to face-centered-cubic (y) iron. This has been ascribed to the more close-packed structure of y iron. The diffusivity ratio at the transition temperature is Da/Dy =350. Correlations of creep data for a and y iron5 reveal that the creep rates under a given stress at the transition temperature differ by about the same ratio (ea/ey 2 200). It would be difficult to reconcile these results on any other basis than that the diffusivity of atoms probably controls creep of iron in some very direct way. No other published data on other allotropic metals appear currently available for further checking such a possible correlation between i and D. Thallium transforms from a hexagonal close-packed (a) structure to a body-centered-cubic (ß) structure at 230°C (503°K) and the self-diffusivities of the two structures have been determined by shirn.10 His results are plotted in Fig. 1 where it will be noted that Dß/Da = 25 at the transition temperature. It would appear desirable, therefore, to determine the creep rates of polycrystalline a and ß thallium at the transition temperature, as well as determine

Jan 1, 1959

By W. E. Horst

Flotation feed was hell constant for batch laboratory tests and continuous pilot and commercial plant tests on a spodumene ore to determine the relation.ship between flotation behavior and the size and type of flotation machine. Results. showed that additional retention time would be needed in the plant flotation circuit to duplicate laboratory or pilot plant performance when operating Dariables of the. plant flotation machines remained unchanged. During the past few years of operation at Kings Mountain, N. C., full-scale flotation has generally yielded poorer metallurgical results than those obtained in the laboratory or pilot plant. After 2 min in each size of Denver flotation machine in the spodumene rougher circuit, pilot recovery (41.7 pct) was almost three times that of the plant (13.6 pct) and about twice that of the laboratory (21.0 pct). Pilot and commercial plant data are based on continuous operation, and laboratory results on batch testing of rougher performance. The ore is a pegmatite containing spodumene, feldspar, quartz, mica, and amphibolite. Data were accumulated to evaluate the scale-up relationships between laboratory, pilot plant, and plant flotation cells. Flotation rate constants and dimensional analysis were used to define the relationship existing between flotation behavior and scale of operation. Measuring Flotation Rates: Efficiency of the rougher stage was measured by flotation rate, defined as the recovery that can be attained within a given time." • The problem of measuring flotation rates has been studied by many investigators, whose methods have varied. Published studies an flotation kinetics have been summarized recently by Gaudin.l When comparing flotation rates, it is more satisfactory to compare straight line relationships between recovery and flotation time than exponential curves resulting from plotting cumulative recovery vs cumulative flotation time. To convert the exponential curves into straight line relationships, rate equations were applied similar to those used in chemical kinetics to study the velocity of chemical reactions. Two rate equations have been used in this investigation to measure efficiency of the various cells: 1.5 order Rate Equation dR/dt=k (A-R)1.0 [Eq.1] Second Order Rate Equation dR ---- - K(A - R)2 [Eq. 2] dt Upon integration Eq. 1 becomes 1/(A-R)1/2=k/2 t+1/A1/2 [Eq. 3] and Eq 2 becomes: or fEq. 4] t/R=1/A2K+t/A [Eq. 4] where R = cumulative recovery [percent recovery of total value (spodumene) in flotation feed]. A = initial concentration, pct (100 pct of mineral to be separated). t = flotation time (minutes). k = flotation rate constant for 1.5 order rate equation [units: 1/(percent) 0.5 (min)1. K = flotation rate constant for second order rate equation [units: 1/(percent) (min) 1.

Jan 1, 1959

By Merrill F. McCarty, Robert S. Olson

New organic flocculants of high-molecular weight are replacing lime, glue, and starch in liquid- solid separation. Of these synthetic materials, polyacrylamides are outstanding. Polyacrylamides form a class of compounds varying widely in composition and activity. Separan 2610H, one of the first of these flocculants' released to the mining industry in 1954, is described' as a high- molecular weight polymer of acrylamide with or without a copolymer material and with some replacement of amide by carboxylic groups.

Jan 1, 1959

By H. Bernstein

WHILE the beryllium -copper (2 pct Be) alloy is nominally nonmagnetic, the presence of iron impurity causes variations in the magnetic proper- ties which, at times, attain excessive proportions. This investigation was carried out to establish the effect of small amounts of iron on the susceptibility of the material and to determine if the effect could be minimized. Beryllium-copper is an age-hardening alloy which

Jan 1, 1959

By W. Rostoker, S. A. Spachner

FOLLOWING the discovery of the w transition phase in certain titanium-chromium alloys by Frost, Parris, Doig, and Schwartz, much interest has centered on the alloys in which this phase is found and its mode of precipitation. The w phase has been found in alloys of Ti-Cr, Ti-Fe, Ti-Mn, Ti-MO,2 and Ti-v.3 The temperature-time-transformation characteristics have, as yet, not been determined for most of these. In this study, such transformation characteristics have been investigated for two heat-treatable titanium alloys known to exhibit transition phase phenomena. The alloys chosen, Ti-8Cr and Ti-13M0, are representative of two classes of binary equilibrium systems. In the

Jan 1, 1959

By J. Peperakis

Coal mine bumps are normally associated with pillar mining under moderate or deep cover. Severe bumps at Sunnyside, however, have not been confined to pillar lines. Many have occurred in virgin development and in localities a long way from active pillar workings. As early as 1918 bumps in virgin territory were attributed to the faulted structure in the Sunnyside area.' Sunnyside is an old property, mined for more than 60 years. Both man-made and natural conditions contribute greatly to bump occurrences, and loss of life and great destruction of workings have resulted from some unusual bumps in recent years. Before Kaiser Steel acquired the Sunnyside Mines in 1950, about 21 million tons of coal had been extracted. Large areas had been worked out and equally large areas first-mined. As demand for coking coal gradually diminished, extensive blocks were shut down, and during the low production period of the 1930's mining on a very limited scale was confined to a section of the property close to the coal tipple. Following purchase of the property Kaiser Steel developed the mines into a fully modernized operation. The worked out and first mined areas covered about four square miles extending five miles along the strike and up to one and a half miles down dip from the outcrop. The sections with favorable mining conditions and clean coal had been largely extracted under the selective mining system imposed by economic conditions and the lack of cleaning plant facilities. Large reserves remained on the fringes of the worked out sections and in areas under deep cover and difficult roof. There were also considerable reserves in first-mined areas. In recent years much of Sunnyside's daily output of 7000 to 8000 tons has been derived from the partially mined localities. Many bumps have occurred when pillars have been pulled within the first-mined areas and on the fringes. The bumps have been associated with retreating pillar lines backing up against old workings and pillar lines in old first-mined areas backing up against highly stressed oversized barrier pillars surrounded by smaller pillars. In some parts of the property the upper Sunnyside seam was extensively worked in the past, and sizable areas of old works overlie the present lower seam workings. Abutment pressures from barrier pillars and pillar remnants are transmitted to the lower seam, contributing to bumps and squeeze conditions. Cover: The terrain is exceedingly rough, and cover varies considerably over relatively short horizontal distances. For example, at No. 1 mine the 2000-ft cover line is ony 2700 ft from the coal outcrop, and at No. 2 mine the cover over the main hoisting slope increases from 1000 to 2000 ft in a horizontal span of 1200 ft. Cover over the present mining sections ranges from several hundred feet in the valleys to 2500 ft under the crest of the divides. A short distance ahead of Sunnyside's deepest development down dip the cover reaches 3000 ft or more.

Jan 1, 1959

By E. I. Alessandrini, A. U. Seybolt

Selective oxidation (preferential oxidation of a single alloy component) can be an important oxidation mode in the case of alloys such as Si-Fe, Al-Fe, and so on, when heat-treating in atmospheres of low oxygen potential. It was the purpose of this work to identify the oxide films formed on iron containing 31/4 pct Si at low oxygen potentials, and to make some observations on the H2O/H2 ratios required to form them. EXPERIMENTAL METHOD HYDROGEN of varying water content offers a very convenient method of establishing a wide range of oxidizing power, or oxygen potential. The method chosen to provide a desired H2O/H2 ratio was to nearly saturate hydrogen at room temperature by bubbling the gas through water at room temperature, and then to wring out the excess water by passing the wet gas through a long glass spiral immersed in a refrigerated liquid at a desired dew point. After oxidation, the samples were examined by electron diffraction in order to identify any film which might be present. PREPARATION AND TREATMENT OF SAMPLES The samples were prepared from a Si-Fe alloy made in the laboratory using electrolytic iron and 96 pct ferro-silico11, vacuum-induction melted, hot-rolled then cold-rolled to 0.015-in. thickness. After the cold-rolling the samples were annealed at 1000°C. Transmission Laue X-ray patterns showed very little evidence of preferred orientation, but it is likely that a weak texture could have escaped notice. The chemical analysis was as follows: 3.34 Si, 0.01 Al, 0.001 0, 0.006 C, 0.002 N. Before each sample was oxidized, it was polished through 4/0 emery paper, cleaned and dried using benzene, carbon tetrachloride, acetone, absolute alcohol, and ether. The method of oxidizing the samples was as follows: Samples about 1/2 by 1 by 0.015 in. were held in the upper, cool part of a vertical vacuum furnace until the desired temperature was established in the furnace, Fig. 1. The sample was then lowered into the uniform hot zone where it was heated quickly to the desired temperature, and subjected to hydrogen of controlled moisture content (dew point) as mentioned previously. Temperatures from 400" to 1000°C were used, and dew points from room temperature to —78°C were explored. In general, the runs lasted about 6 hr, but a few runs were of different duration, as will be indicated later. After the predetermined period of time had elapsed, the specimens were withdrawn by the hollow stainless steel-quartz holder to a cool zone at the top of the furnace. EXPERIMENTAL RESULTS The results are summarized in Table I. Most of the electron-diffraction patterns were obtained by glancing-angle reflection, but in a few cases it was possible to strip the oxide films from the surface by a total immersion in a 3 pct bromine-methanol solution. Some of the thinner stripped films yielded quite satisfactory transmission patterns. However, both diffraction techniques yielded the same results; the patterns while most frequently showing a (low) tridymite, also showed a (low) cristobalite in some cases. A few patterns showed evidence of both phases. Because of the known nonequilibrium behavior of silica, it is not surprising that both forms of silica could coexist on one sample. It was noted that at fairly low dew points such as —40°C, there was a tendency for diffuse diffraction rings, suggesting a very small crystallite size. Also some subsequent experiments to be reported later show that thin silica films can be amorphous.

Jan 1, 1959

By C. S. Barrett, D. B. Masson

Martensitic transformations have been found in AgCd both upon cold-working at room temperature and cooling to lower temperatures. The crystal structures of the transformation products were found to be close-packed hexagonal in the first case and or-thorhombic in the latter. The transformation characteristics also were studied. Similar treatment of AuZn alloys failed to yield any transformation. THE literature on martensitic transformations of body-centered cubic metals and alloys indicates widespread instability of this structure at low temperatures, a tendency which merits further study. The body-centered cubic ß-phase of CuZn, for example, when it contained less than 42 wt pct Zn, was found by Greninger and Mooradian' and others' to transform on cooling to subzero temperatures to a phase that was tentatively considered to be tetragonal. Further work by Massalski and Barrett" demonstrated that cold work at low temperatures causes a partial transformation of ß CuZn of higher Zn content. The structures of the strain-induced transformation products were found to be different from those induced by simple cooling. Another well-known martensitic transformation among body-centered cubic phases is that of ß AuCd, first studied with X-rays by Olander,' then very thoroughly by Chang and Read.5,6 Here again transformation was found to occur both as a result of cooling and of strain. The alkali metals Li and Na, as well as certain Li-Mg alloys, also undergo transformation from their normal body-centered cubic structure, both on cooling and on cold-working. The phase AgCd, the subject of the present report, should be expected to behave quite similarly to CuZn for a number of reasons. It is the chemical analogue of CuZn, silver being directly below copper and cadmium directly below zinc in the periodic table. The size factors (percent difference in size) of the atoms, possibly a consideration in the stability of the ß-phases, are +3.1 in AgCd and + 4.2 in CuZn. Likewise the relative electronegativities of the two pairs of metals are about the same, CuZn possessing an electronegativity difference of 1.0 and AgCd one of 0.8. These values are from a table of electronegativities given by Darken and Gurry." The phase diagrams of the two systems around 50 atomic percent are similar, both possessing a disordered body-centered cubic phase, ß, at high temperatures and an ordered bcc phase, ß, at room temperature; however, the ß and ß' phases of AgCd are separated by a hexagonal phase, [, stable in the range 220-440oC, which has no analogue in CuZn. There has been confusion in the literature as to the structures of the ß' and [-phases. The phase diagram in the ASM handbook'" has the structures of the two phases interchanged; however, Hansen" reports the correct relative positions and Muldawer" verified that ß', the low-temperature phase, is body-centered cubic. Work by the present authors also

Jan 1, 1959

By W. C. Knopf, I. M. LeBaron

In the Carlsbad area potash is dry-mined and wet-concentrated. Wet concentration involves recircu-lation of saturated brines, with resultant difficulties of brine disposal and inherent losses in recovery through solution of the KCl. A dry beneficiation process for potash minerals would offer many advantages over present methods. International Minerals & Chemical Corp. has been working on development of a dry process for some time. This article is a progress report. Potash ores available in this country are largely mixtures of halite and sylvite contaminated with slimes and often with many sulfate and magnesium minerals. Electrostatic concentration of KCl when the contaminating minerals are in low percentage has been accomplished. Continuous production of better than 60 pct K2O concentrate from high potassium sulfate ores has not been demonstrated at the present time. Laboratory Procedure: Laboratory work on electrostatic beneficiation of potash minerals has been carried out using both pure crystals and mined ore. Electrostatic separation of the two main components of potash ore, sylvite (KCl) and halite (NaCl), is accomplished by first heat-treating the ore to allow for electric charging of the particles. Preferential exchange of' electrical charges between different mineral particles through surface contact is the principal mechanism involved. After proper conditioning of the particle surfaces, the oppositely charged minerals are dropped vertically into a horizontal electric field having a field gradient from about 5000 to 15,000 v per in. The particles are free-falling in the field. A suitable power supply is used to produce the proper total voltage for the electric field. Total required voltage is, of course, a function of electrode spacing. A typical electrode arrangement with power supply is shown in Fig. 1. In general, the total voltage on any system is 75,000 to 90,000 v. Power consumption is negligible, as leakage at insulators and corona discharge are the main losses in the system. Optimum preheat temperatures for pure material components generally are not the same as for mined minerals. Fig. 2 shows clearly that maximum recovery on a 50 pct pure KCl, 50 pct pure NaCl mixture occurs at a preheat temperature of about 600°F. In this test the preheat mixture was allowed to cool to about 225°F before dropping through the electric field. The optimum temperature for sep- aration is practically never the optimum temperature of preheat. Optimum separation for mined Carlsbad potash ores occurs when a preheat temperature closer to 900°F is used, as shown by Fig. 3, which plots percent sylvite (KCl) in the concentrate and tails as a function of preheat temperatures. Here again the ore was allowed to cool to about 225°F before separation. It should be noted that efficiency of separation increases continuously with increasing preheat temperatures until incipient fusion of the ore takes place at about 950°F. The increase in optimum preheat temperature for Carlsbad ores over the pure minerals can be traced to the effect of the clay slimes intimately associated with the mined potash. If the slimes associated with the ore are removed by washing with alcohol or other non-aqueous material, the necessity of preheating to the high temperature is removed. This temperature range has been proved critical within these limits during continuous pilot plant operation. Concentrate and tailings grade and optimum recovery also are functions of the temperature of the potash mineral particles during separation in the electric field. Fig. 4 presents data indicating that feed to the rougher pass should range between 150°F and 275°F for best results. It has been found by subsequent pilot plant work that these temperatures can be maintained in actual operation.

Jan 1, 1959

Established as a Society February 26, 1957 John S Bell, President Wayne E Glenn, President-elect Basil P Kantzer, Past President R E Howard, Vice, President M B Penn, Vice-President Everett G Trostel, Treasurer Joe B Alford, Executive Secretary 800 Fidelity Union Bldg Dallas 1, Texas

Jan 1, 1959

Jan 1, 1959

By R. C. Hall

In the present work, experiments determined the effect of the order-disorder reaction near the Fe,Al composition on the magnetic anisotropy and magnetostriction of single crystals: A material which is more difficult to magnetize in one direction than in another is anisotropic, that is, the ease with which ferromagnetic materials may be magnetized in different crystallographic directions determines the anisotropy. Two investigators have estimated the anisotropy of the aluminum iron alloys from poly-crystalline data;1,2 however, these estimates should not be considered to be reliable. Siege1 made two accurate measurements of the first anisotropy constant* from single crystals of 4.0 wt pct aluminum sotropy throughout the ferromagnetic aluminum iron system have been described. These results were obtained from single crystals which were slowly cooled and, hence, ordered near the Fe3Al composition.4 Magnetostriction is the change in length per unit length resulting from applying a magnetic field to a ferromagnetic material. For the purpose of this report, the saturation magnetostriction was measured. This is the maximum change in length per unit length resulting from an applied magnetic field large enough to saturate the material in a given direction. This magnetostriction has been determined for single crystals of the ferromagnetic aluminum-iron system.' The crystals near Fe3Al were also ordered. PREPARATION AND TREATMENT OF SINGLE CRYSTALS Single crystal bars were grown from the melt.' The raw materials for these crystals were iron and aluminum of 99.9 and 99.99 pct purity, respectively. From the bars, crystals in the shape of circular

Jan 1, 1959