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By G. R. M. Del Giudice, A. F. Taggart, Othon A. Ziehl

In a previous paper1 in which one of the authors collaborated, it was postulated that All dissolved reagents which, in flotation pulps, either by action on the to-be-floated or on the not-to-be-floated particles affect their floatability, junction by reason of chemical reactions of well recognized types between the reagent and the particle affected. This generalization, apparently, like many pioneer structures, had for certain observers a flimsy appearance, and these, judging its stability rather by the number than by the character of its foundation posts, have attempted variously to overthrow it, either by the frontal attack of general denial, or by the flanking movement involved in assuming that those cases in which the facts were unknown or unproved were, therefore, discordant. But as time has passed and further evidence on the question has accumulated, it has become apparent that the results of verifiable experiments add stone by stone to the substructure of the hypothesis, and that the super-tructure has lost nothing in weathering. The present paper constitutes an examination of the opposing positions in the light of the more recent evidence developed. It will clarify the discussion if, at this point, we state more fully the implications of the disputed hypothesis. In the first place, it is explicitly limited to reagents that are dissolved in the water of the flotation pulp. Next, it refers only to such of these dissolved reagents as act on the solid particles in the pulp to affect their floatability. This includes the collectors, activators, and certain depressors and gangue-control reagrnts, but not the pure frothers, and not, necessarily, conditioners whose function seems to be merely that of pH control, although in certain cases it has been demonstrated that such control has the effect of regulating the primary reaction of the collector, depressor, or the like. Finally, there is no limitation as to the nature of the chemical reaction postulated.

Jan 1, 1935

By L. D. Fetterolf, G. T. Mahler, W. M. Peirce, R. K. Waring

UNTIL recently, the only commercial method of producing magnesium has been fused salt electrolysis, despite a considerable amount of experimental work on the direct reduction of magnesium oxide. In this early work, a number of investigators demonstrated that magnesium oxide would react with any one of several reducing agents to produce magnesium vapor, but that the mixture of magnesium oxide and reducing agent must be heated to a high temperature even in a vacuum. In particular, it was demonstrated that silicon and aluminum are effective reducing agents and that when either of these is used the magnesium vapor can be condensed to massive metal. In spite of this knowledge, no successful commercial reduction process was developed, at least in this country, because of the operational difficulties imposed by the requirement of high temperature and vacuum and because of the high cost of the reducing agent. The outstanding experimental work done by Pidgeon, who carefully reviewed all of the known methods of making magnesium and then selected ferrosilicon reduction, overcame some of the operational difficulties. The process developed by Pidgeon comprises briquetting a mixture of calcined dolomite and reducing agent, pre-heating the briquets to about 600°C. in an externally heated alloy retort, reducing the MgO with silicon in an evacuated horizontal alloy retort heated externally to about 1150°C., and condensing the magnesium vapor to a solid in a cold extension of the retort projecting beyond the fr6nt of the furnace. A major advantage of Pidgeon's process is that the retort is not cooled down between charges. Earlier investigators had used apparatus that necessitated cooling and reheating of the retort between charges. Early in January 1942, when the War Production Board was considering the Pidgeon process for quickly increasing the production of magnesium, The New Jersey Zinc Co. offered to have a research investigation of the process carried on, with the hope of assisting in its further development. This offer was accepted, and a two-retort pilot plant was built at Palmerton and put in operation on Jan. 29, 1942. An intensive investigation of certain phases of the process was carried out in the ensuing four months. This investigation was completed in the last part of May 1942, and the pilot plant was then shut down. Subsequently, The New Jersey Zinc Co. was requested to have further development work done on the process, and a more extensive investigation was undertaken in August I942 under contract with the War production Board and under the super- vision of the War Metallurgy Committee. This paper describes the phases of the investigation that are thought to .be

Jan 1, 1944

By J. S. Kirkaldy, D. G. Fedak

The extra degree of freedonz introduced by a second independetzt concentration in a tenzary system gives rise to the possibility of unstable planar phase interfaces in semi-infinite diffision layer couples. Diffusion paths which pass continuously in and out of too-phase regions of the phase diagram but which are not coincident with tie-lines give rise to super saturated zones which may be either adjacent to or isolated from planar phase interfaces, with corresponding nonisolated or isolated precipitates. Nonisolated precipitates are equivalent to morphological development of the interface. Selected couples in the ternary systems Fe-Ni-Cr and Cu-Zn-Sn have been examined nzetallographically and ifz the latter case both isolated and uo~zisolated precipitates have been observed. The diffusion path in one of the couples showing interface morphological developtnent has been examitled using electron probe microanalysis. IGNORING the spurious effects of preferential grain boundary diffusion and anisotropic crystal growth7 it can be unequivocally stated that it is impossible for a binary isothermal diffusion couple constructed of two unsaturated phases to sustain a nonplanar phase interface. Consider for demonstrative purposes the schematic phase diagram of Fig. l(a). Given an initial flat phase interface, semi-infinite boundary conditions and the internal boundary condition fixed by the constitution diagram, xB = xB(T), the unique solution of the diffusion equation requires a persistent flat interface. No other solution is possible. If, however, we anticipate the involvement of surface tension, then the internal boundary condition must be written xB = xB (T,Y) where r is the radius of curvature of a hypothetical nonplanar interface. The introduction of a new parameter such as r can be equivalent to the release of an internal constraint, so that a stable nonplanar interface may be possible after all. Consider a perturbation to the interface as indicated in Fig. 1(b). According to the Ostwald-Freundlich equation: which is applicable to a system of this constitution, the solubility of A in the matrix ß ,xB (Y), at a point of curvature r is given by where Va is the molar volume of the a-phase, R is the gas constant, and a is the interfacial tension. Since the right hand side is positive, xB(r) >xB cm, as indicated in Figs. 1(a) and 1(c). Accordingly, the perturbation will carry the interface concentration in a direction which is opposite to that which would sustain local equilibrium. Such a perturbation is necessarily moderated and the system is returned to its initial condition. This result is general for all binary couples since we can regard an interfacial perturbation as an attempt to precipitate within un-

Jan 1, 1962

By A. D. Dorenfeld

Factorial design is a mathematical method of drawing valid conclusions from a series of tests made in a predetermined pattern. It is applied to flotation ore testing using, in this case, five variables, each varied twice, requiring a total of 32 tests. Representative conclusions are checked by repeat testing. THE factorial design method of testing is particu-J- larly applicable to mill-scale plant tests because 1—the conclusions take into consideration all variabilities of the plant, 2—there are no subjective guesses as to the conclusions, 3—the number of tests necessary to check large numbers of variables are at a minimum, and 4—interactions between variables can be discerned. It is equally applicable to laboratory testing because once the variables to be investigated have been decided upon, as well as the number of levels for each variable, a well-trained assistant can run the tests, since the test work follows a predetermined mathematical pattern, leaving the conclusions to be found by the person in charge. The conclusion takes into consideration all errors of the tests. To illustrate the use of factorial design, a sample of copper porphyry ore was tested, the copper content of the batches not being uniform. Five variables were investigated, each at two levels, requiring only 32 tests. After suitable arithmetical analysis, conclusions for copper recovery and concentrate grade are arrived at. Four cases of these conclusions are checked by repeat testing. Testing Methods Reproducibility of flotation tests varies widely, depending on the experimenter, the process, the equipment, and probably a host of unknown and perhaps interacting variables. If the reproducibility of tests is good, let us say to 0.2 pct recovery of a certain metal, and the minimum difference between tests upon the variation of the interested variables is, say 1 pct, then simple averaging and inspection is ample in interpreting results. However, often such a happy situation is not the case. This is particularly true in mill-scale operations where the ores are variable, and a host of minor operating fluctuations common to most milling, and familiar to all mill operators, is the normal state of affairs. Yet, mill scale tests are run, the results averaged, and conclusions drawn therefrom. The trustworthiness of such results should be measured by comparison to the experimental error—the measure of the degree of reproducibility of the results. This comparison is a test of significance. Thus, if daily results of recoveries average 80.0 pct, and a spread of 78.0 pct to 82.0 pct, is recorded, then, clearly, on changing mill operations, an 81 pct recovery cannot be construed as significant by using averages, since it is well within the previous test limits. By using rigorous statistical tests of significance, conclusions arrived at by inspection or simple averaging may be shown to be based on inadequate evidence or even wrong. In any event, a plant super-

Jan 1, 1952

By J. K. Edgar

FOR a number of years the production and use of super-purity aluminum (better than 99.99 pct) has been steadily increasing. High-grade lots of such aluminum show certain outstanding characteristics not found in lower grades containing principally silicon, iron and copper as impurities. One such characteristic is the so-called "self annealing," that is, the recrystallization of the heavily cold worked metal at room temperature.' Interest therefore is aroused as to the effects of the impurities. It is well known that the amounts of silicon and copper which occur in aluminum of better than 99.95 pct are completely soluble, at least at elevated temperatures (above 200°C). Iron, on the other hand, is known to be fairly insoluble in solid aluminum. Thus, a knowledge of the limits of this solubility would be of considerable use in studying the characteristics of the high purity metal. All investigators have agreed that iron has very low solubility in solid aluminum. Rosenhain, Archbutt and Hanson2 reported traces of an aluminum-iron phase in the "purest samples of aluminum obtainable." Gwyer and Phillips3 reported that an iron constituent was visible under the microscope in metal containing ".0088 per cent iron." Roth1 found that in the solid state the solubility of iron in high purity aluminum was 0.01, 0.01, 0.017 and 0.022 pct at 225, 320, 500 and 600°C respectively. Dix5 working with alloys containing less than 0.03 pct impurities, concluded from microscopic and chemical analyses of eutectic areas that the eutectic composition was close to 1.7 pct iron. Dix placed the eutectic temperature at 655°C'. Archer and Fink,6 using high purity aluminum-iron alloys, found that the hypoeutectic liquidus intersects the eutectic horizontal at 1.7 pct. This is in fair agreement with the investigation of the aluminum-iron system by Gwyer and Phillips who placed the eutectic at 1.89 pct iron with a freezing point of 653° PREPARATION AND CHEMICAL ANALYSIS OF ALLOYS Electrolytically refined aluminum (99.991 pct aluminum) and a high purity aluminum-iron alloy (11.45 pct iron) were used in the preparation of the alloys for this investigation. To aid in controlling the iron content of the experimental alloys, an alloy of lower iron content was prepared first from these materials. The high purity aluminum was melted and heated to about 700°C in a plumbago crucible coated with alundum cement and the aluminum-iron alloy was then added. The alloy was thoroughly stirred, fluxed and skimmed and then chill-cast into notch bars. The analyses of the three materials are given in Table I. The alloys for the determination of the solid solubility of iron in aluminum were prepared by melting 600 g total of the aluminum plus the required quantity of the aluminum-iron alloy (No. 92531). These

Jan 1, 1948

By E. C. W. Perryman

The recovery of X-ray line broadening, hardness, and electrical resistivity from cold worked AI-Mg alloys has been investigated. The results, together with those from density measurements, suggest that magnesium atoms freeze in the excess vacancies formed by cold working, and that this affects the climb of dislocations during the recovery process. PREVIOUS work1, " has shown that while 1 pct Mg increases the activation energy for recrystalliza-tion, it decreases the activation energy for the recovery of mechanical properties and decreases the subgrain size both after cold working and annealing. A similar result has been reported by Varley2 for an A1-2 pct Mg alloy. With plastic deformation at high temperatures, McLean and Farmer' and Rachinger have found that magnesium appears to retard the motion of dislocations and, furthermore, they find little or no effect of magnesium on the size of subgrains formed during high temperature deformation. In view of the apparent contradictions as to the effect of magnesium on subgrain size, the recovery process in Al-Mg alloys has been investigated more thoroughly by studying the annealing out of X-ray line broadening, hardness, and electrical resistivity from alloys cold worked at room temperature. Material Used—The chemical analyses of the alloys are given in Table I. Fabrication—The material used was cold rolled 20 pct at room temperature, the grain size prior to the last cold rolling operation being similar to that used in previous work; i.e., 230. The experimental procedure for annealing, determination of X-rav half-veak breadth. hardness measurement, electEica1 resistivity, and density and metallographic examination was exactly the same as previously described." Variation of X-Ray Half-Peak Breadth with Annealing Time—Isothermal annealing curves at 100°, 200°, and 250°C were obtained for material cold worked 20 pct. The half-peak breadth of the (333) Ka, line directly after cold working is shown as a function of magnesium content in Fig. 1. Only with the 2.87 pct Mg alloy was overlapping of the a, and n.. reflections observed to any appreciable extent. To separate these, Rachinger's method' was used. Typical isothermal annealing curves are shown in Figs. 2 and 3 for 100" and 200°C, respectively. These curves are similar to those obtained previously for super-purity aluminum except that the

Jan 1, 1957

By T. A. Rickard

Freeman, the English historian, said that he had learned from Macaulay "never to be afraid of using the same word or name over and over again if by that means anything could be added to clearness or force. Macaulay never goes on, like some writers, talking about `the former' and `the latter', `he', `she', `it', and `they', through !clause after clause, while his reader has to look back to see which of several persons it is that is so darkly referred to". He might have learned also from Macaulay that a preposition makes a' feeble ending for a serious statement. How often do you hear `the former' and `the latter' in conversation? Good conversation is a guide not to be dis¬dained. When you must use `the latter', do not confuse it with `the last'. Cheap labor, cheap fuel, and cheap transport are essential, the latter [last] being particularly important in base-metal mining. The apparatus may be used to determine such gases as hydrogen sulphide, chlorine, oxides of nitrogen and some others, as well as sulphur dioxide. In the case of the latter two, etc. The two last mentioned are "sulphur dioxide" and "some others". He should have stated which two, and he should have avoided that wretched phrase "in the case of ". Pinning may be partly prevented by use of chalk, oil, or turpentine. The latter [last] is best. I "Partly prevented" is a poor phrase. `Prevented! is a word that does not lend itself readily to modification. He means `checked' or `corrected'.

Jan 1, 1931

By John H. Hollomon

In a recent paper,' a very early suggestion by Ludwik2 concerning the nature of the mechanical behavior of metals has becn reexamined and extended. In essence it was suggested that there exists, at least under certain conditions, a mechanical equation of state; that the stress required for flow depends upon the instantaneous values of the strain, strain rate, and temperature, and not upon their past values. It is proposed that under these circumstances thc stress does not depend upon past history of these variables, but is like the temperature of a gas that depends only upon the instantaneous values of the pressure and volume. This notion has not been applied to present-day studies of metals, though it is especially applicable to the study of creep. It is the purpose of this paper to analyze the significance and possible range of applicability of this idea and to determine how it influences the accepted ideas concerning creep. Stress-strain Relations It is wcll known that the stress-strain curves of metals are influenced by both train rate and temperature. For a fixed strain rate and temperature there is associated with each metal a stress-strain curve. If either the strain rate or temperature is changed a new stress-strain curve will be characteristic (Fig. I). A much more genera1 relation between the effects of these variables is possible, however. Consider the stress-strain curves of Fig. I determined at

Jan 1, 1947

By John H. Hollomon

In a recent paper,' a very early suggestion by Ludwik2 concerning the nature of the mechanical behavior of metals has becn reexamined and extended. In essence it was suggested that there exists, at least under certain conditions, a mechanical equation of state; that the stress required for flow depends upon the instantaneous values of the strain, strain rate, and temperature, and not upon their past values. It is proposed that under these circumstances thc stress does not depend upon past history of these variables, but is like the temperature of a gas that depends only upon the instantaneous values of the pressure and volume. This notion has not been applied to present-day studies of metals, though it is especially applicable to the study of creep. It is the purpose of this paper to analyze the significance and possible range of applicability of this idea and to determine how it influences the accepted ideas concerning creep. Stress-strain Relations It is wcll known that the stress-strain curves of metals are influenced by both train rate and temperature. For a fixed strain rate and temperature there is associated with each metal a stress-strain curve. If either the strain rate or temperature is changed a new stress-strain curve will be characteristic (Fig. I). A much more genera1 relation between the effects of these variables is possible, however. Consider the stress-strain curves of Fig. I determined at

Jan 1, 1947

By L. R. Jackson

It is convenient to have a consistent system of notation that will allow the representation of the entire range of complex stresses from hydrostatic compression to hydrostatic tension on plastic flow in a single diagram. Such a system is provided by making use of the fact that any complex stress system can be resolved into a hydrostatic tension or compression and a pure shear. Consider a stress system having the principal stresses This system can be resolved into a new system consisting of the three components and three pure shears. If Sm is positive, the net stress effect is hydrostatic tension; if it is negative, the effect is hydrostatic compression. In order to produce a systematic notation, a quantity that will be referred to as the "triaxial ratio" will be defined by the equation _ Sm Tr = Sm - Sm is given by Eq. I and Sl is the absolute magnitude of the largest principal stress without regard to sign. Table I lists the triaxial ratios for various common systems. Table i.—Triaxid Ratios for Various CommonSyslems Triaxial Ratio Stress System Tr Hydrostatic compression — SI - —St - -S³............................... -1 Torsion or shear -SI - S². S² = O..... O Simple tension SI. SI = SI = 0......... +0.33 Biaxial tension SI = S² S³ - 0......... +0.66 Hydrostatic tension +SI - +S³ = +S³. +1.00 Representation of Strains Strains will be plotted as "true" strains according to the system proposed by Ludwik.1

Jan 1, 1945

ASIDE from the John Fritz Medal, in which the Institute participates through its representation on the John Fritz Medal Board, the Institute itself has five major awards to make annually for excellence in technical papers, as follows: The Robert W. Hunt Medal, The Hadfield Prize, The J. E. Johnson Jr., Award, The Lewisohn Platinum Prize to senior members, and the President's Prize to junior members. ROBERT W. HUNT MEDAL The partners of Robert W. Hunt established a fund which was presented to the Institute at a fitting ceremony on May 27, 1920, to establish an annual medal and a sum of money to be awarded under the following rules: 1. The award shall consist of two prizes; first of a gold medal, second of a sum of money; a certificate to accompany each prize. The money prize shall not be awarded to. a member over 40 years of age, but under unusual circumstances, both prizes may be allotted to one person provided that he is not over 40 years of age. In general it will be understood that the Committee shall award the money prize to the younger men, rather than the medal. 2. The awards shall be made not oftener than once a year to that person or persons contributing to the Institute the best original paper or papers on iron and steel. The scope of the term "iron and steel" shall be determined by the sub-committee considering the awards. In general, papers dealing with the practical side of the subject have preference over those dealing with the theoretical side in recognition of the fact that Captain Hunt's main contributions to the industry have been in the improvement of production and quality of material. 3. A sub-committee of three to five including the Chairman of the Iron and Steel Committee, shall be appointed by the iron and Steel Committee annually to adjudge the award subject to approval. 4. The awarding committee shall submit its report to the Iron and Steel Committee at its October Meeting, and the. award be certified to the Secretary of the Institute in time to permit the presentation to be made at the Annual Meeting of the Institute. 5. The recipient of the award shall be designated "The Hunt Medallist." SIR ROBERT HADFIELD PRIZE Sir Robert Hadfield has offered an Institute prize of $1000 for researches with regard to the different forms of combination of carbon in iron and steel. Until within a few weeks no paper has been submitted which could compete for this prize. If the paper in hand should not meet the requirements, the donor has suggested that the prize be transferred and offered for: (a) the determination of the hardness in metals in connection. with super-hardness, (b) in consideration of questions of fuel economy, (c) in consideration of questions of industrial development and labor. J. E. JOHNSON, JR. AWARD This award is made from the income of a fund of $3000 donated by Mrs. Margaret Hilles Johnson in memory of her husband, J. E. Johnson, Jr., who was a prominent engineer, author of two valuable volumes on iron blast-furnace construction and practise, vice-chairman of the Institute's Iron and Steel Committee, and a frequent contributor of papers to the Institute's TRANSACTIONS.

Jan 1, 1925

By Robert G. Johnson, Richard J. Prosen

THE present work was done in connection with a program for investigating metal-to-ceramic braze techniques using the well-known reactivity of titanium with certain ceramic oxides. The investigation extended over the range of 0 to 30 pct Ti. The indium was obtained from the Indium Corp. of America and was specified to be 99.97 pct pure. The titanium was supplied by Metals Disintegrating Co. and was stated to be 99.5 pct pure. Each 2 to 4 g quantity of the alloy compositions studied was prepared using a mixture of 300 mesh powders pressed into pellet form. The pellets were heated in thin-walled molybdenum crucibles using a resistance-wound furnace in a vacuum less than 10-4 mm of Hg. Little reaction occurred between the molten alloy and the crucibles at the temperatures and short time intervals used. Only slight spectroscopic traces of molybdenum were found in the melt after a typical period of heating. The points shown on the phase diagram of Fig. 1 represent thermal arrest measurements. The phase boundaries shown are consistent with the thermal arrest and X-ray data obtained. The temperatures were determined using a Pt-Pt 10 pct Rh thermocouple with the junction spot-welded to a short molybdenum rod. The rod was almost completely immersed in the liquid metal, so that good thermal contact with the melt was achieved. The small mass of the crucible and its contents made it possible to obtain many heating and cooling curves in a few minutes time, an advantage which helped to minimize the effects of indium evaporation at the higher temperatures. A Brown strip chart recorder was used to display the thermal arrest curves. To check the technique, the melting point of 99.999 pure Al was measured and found to be within 1 of 660.2c, the accepted melting point. The upper limit of temperature with this technique was about 900°C beyond which the evaporation rate of indium became great enough to alter appreciably the alloy composition during the runs. A peritectic transition was found at 796°+ 5°C from 1.5 to 30 wt pct Ti. It was not found at 0.5 or 1.0 pct. A small super-cooling effect was observed. The melting-point transition to the B + L phase was found up to 20 pct Ti but not at 25 pct. Within the 1 deg accuracy of the measurement, the transition temperature was that of pure indium, 156°C. The liquidus line to the left of the 1.5 titanium point was located only approximately. The two crossed circle points at 1.0 and 0.5 pct Ti place a lower limit on the liquidus line and were determined by observing visually the cessation of vibrations in the melt caused by the damping effect as B-phase crystals were formed during cooling. The B-phase boundary was found at 23.8 pct Ti by X-ray analyses of small single crystals of the B phase isolated from 2 pct Ti melts. The compound was found to be Jetragonal with lattice dimensions of c = 3.052A and a = 10.094W. From the unit cell dimensions and the measured density of 6.42 i 0.05 g per cc, the compound was determined to be In4Ti3 which has 23.8 pct Ti. The calculated density of 6.44 g per cc is obtained assuming 2 mol

Jan 1, 1962

By Peter J. Szabo

INTRODUCTION The time period from the detailed feasibility study to the post investment audity usually ranges from three to eight years depending upon the nature of the mining project considered. It is the only after the post investment audit that we know the adequacy of the assumptions made concerning operational risk assessment in the detailed feasibility or acquisition economics. The post investment audit results from numerous mining projects can best be described by a verse by John Greenleaf Whittier's Maaud Muller. It reads "For all sad words of tongue or pen the saddest are these 'It might have been!"' Dissecting the negative results of numerous mining projects we find faulty assumptions concerning markets, geology, capital investment and operational risk assessment. Although in hindsight many of these assumptions could have been considered impossible or impracticle to have forecast with any degree of certainty, we find that refined assumptions concerning operational risk assessment could have been made with only a modicum of additional "Due Diligence". Anyone who invests in a mining property should employ a much higher discount rate of future cash flow, (usually in the minimum range of 25%-30%), than he would expect from such safe investments as Treasury Bills or high grade Utility Bonds. The nature of this steep discount translates to a large uncertainty concerning the timing and actualization of assumptions contained in the detailed feasibility study. We must remember that when a project gets beyond 20 years, any contribution to the value of the project of cash flow is minimal due to the nature of the discounting process. Thus for each full or partial day lost in the development or early operation stage of a project, the financial impact will be greater than similar lost days later on in the project. Adequate operational risk assissment is particularly critical when bidding on competitive tenders for coal deposists in remote locations such as the Bowen Basin in Queensland, Australia. Because of the market attractiveness of these coal deposits for supplying end users in the Far East, Middle East and Europe, state governments require competitive tender biddings via the Authority to Prospect process. Front end bonuses and super royalty payments must be commited before the actual mining conditions are known. Time to submit firm offers from the actual request for proposal vary from 90 to 120 days. Thus any operational risk assessment must be detailed, realistic and reflective of the actual project. When one searches the literature, one finds limited qualitative data on operational risk assessment in valuation papers. Usually this facet of valuation takes a secondary role to such areas as reserves, markets, and environmental considerations. When one comes to the question of operational risk assessment more often than not one finds the use of "rules-of-thumb", such as tons per man shift, average production, average seam height, etc., are used to forecast results on which banks and other financial institutions are required to make investment decisions. Because of the extremely competitive environment of the 1970's and 1980's numerous financial institutions approved loans without adequate "Due Diligence", and are currently paying a steep price in terms of non performing loans and charge offs. One must always remember that each operation is unique with its own characteristic

Jan 1, 1985

By W. Bonfield

The temperature dependence of the microscopic yield stress (the stress to produce a plastic strain of 2 x 10-6 in. per in.) and the stress-plastic strain curve of polycrystalline Cu 1.9 wt pct Be have been measured for the solution treated condition, an intermediate condition containing G.P. zones and ?' precipitate and the overaged ? precipitate condition, in the range from -58° to 200° C. A transition in micro -yield behavior and a large temperature dependence were noted for the intermediate condition, which are interpreted in terms of the interaction of glide dislocations with two differently sized zones. In comparison the microscopic yield stresses of the solution treated and overaged conditions were less sensitive to temperature variations and are satisfied by the Mott-Nabarro and dislocation bowing theories, respectively. A determination of the temperature dependence of the yield stress of a precipitation hardening alloy has provided a powerful tool for evaluation of the operative deformation mechanism. There is a marked contrast between the effect of temperature on the yield behavior of a metal containing coherent zones or intermediate precipitates, which can be "cut through" by mobile dislocations, and a metal containing a dispersion of noncoherent particles, through which dislocation "bowing out" is the dominant role of deformation.' These studies have in general been confined to single crystals, as it was considered that similar experiments on polycrystalline material did not produce good data because of the lack of sensitivity with which the yield stress could be determined. However, this objection has been removed by the introduction of mi-crostrain techniques, with which the yield stress in polycrystalline materials can be measured to a strain sensitivity of 10-6. Such measurements have not only shown that the deformation of polycrystalline precipitation hardening alloys can be examined with the same detail as single crystals, but also that some unexpected results are obtained.' In this paper the results obtained from a study of the temperature dependence of the microscopic yield stress (the stress to produce a plastic strain of 2 x 10-6 in. per in.) and the stress-plastic strain curve of a polycrystalline Cu 1.9 wt pct Be precipitation hardening alloy (Berylco 25) are discussed. The temperature dependence of the alloy was measured for three different conditions: 1) The solution treated condition (a supersaturated solid solution of a containing ~12 at. pct Be3) which is obtained by water quenching the alloy from 800° C. 2) The condition of y' intermediate precipitate, to- gether with some G.P. zones,' which is produced after an aging treatment of 2 hr at 315°C from the solution treated condition. (The alloy was cold rolled to 40 pct reduction prior to aging to minimize grain boundary precipitation effects.)4 3) The condition with equilibrium ? precipitate structure2 which is developed after an aging treatment of 24 hr at 425° C. EXPERIMENTAL PROCEDURE Tensile specimens of gage length 1 in. and with rectangular cross section of 0.18 by 0.06 in. were prepared from the solution treated, cold rolled alloy and were either resolution treated for 1 hr at 800°C, followed by water quenching, or aged for 2 hr at 315°C and 24 hr at 425° C to produce the desired precipitate structures. The microstrain characteristics of the aged specimens were determined at temperatures from —58" to 200° C and those of the solution treated specimens from -58° to 30° C. Each temperature was controlled to ± 0.2°C, which was a level of stability sufficient to eliminate thermal expansion effects from the measurements (~1.2°C temperature increase produced an extension of 2 x 10-6 in.). The microplastic behavior of the specimens in the temperature range below 82" C was measured with a standard Tuckerman strain gage,5 while at temperatures above 82°C a modified Tuckerman gage with a reduced strain sensitivity (4 x10-6 in. per- in.) was used. A load-unload technique was used to establish values of the microscopic yield stress. The specimen was strained at a constant cross head speed of 2 x 10-2 in. per min to a given stress level, at which the total strain was measured. Then the specimen was immediately unloaded at the same rate and any residual plastic strain determined. This procedure was repeated for an increasing series of stress levels until the microscopic yield stress was established by a direct measure of the stress to produce a residual plastic strain of 2 x 10-6 in. per in. (It should be noted that, as reversible dislocation motion occurs at stresses less than the microscopic yield stress,2 the plastic strain rate at this level was not constant.) In an ideal test, the microscopic yield stress would be determined from a continuous stress-strain measurement, rather than from a load-unload sequence, in order to eliminate mechanical recovery effects.6 However, it was found experimentally that mechanical recovery was negligible in Cu 1.9 wt pct Be at small plastic strains for all the temperatures investigated, as the microscopic yield stress was independent of the number of load-unload cycles employed (i.e., the values measured for specimens subjected to different numbers of cycles was within the experimental scatter determined for specimens tested in an identical manner). Therefore, it is reasonable to consider the microscopic yield stress determined in the load-unload

Jan 1, 1969

By D. T. Peters, C. R. Cupp

Aging of commercial 18 pct Ni maraging steel and of related binary, ternary, and quaternary alloys has been studied by electrical resistivity, X-ray diffrac-tion, and hardness measurements. The aging process is in three stages: 1) recovery of martensite; 2) two precipitation reactions; 3) formation of nickel- rich austenite. The main objective of this work was to discover the nature of the Co-Mu interaction. Addition of cobalt to the Fe-18 pct Ni-5pct Mo alloy results in acceleration of the pvecipitation reaction by increasing the super-sat~lration 0f molybdenum. The cobalt-containing al- loys show no incubation period for the precipitation reaction, but the alloy without cobalt shows an initial slow reaction. These results are interpreted in terms of precipitation on dislocations. At low aging temperatures, the presence of cobalt leads to the appearance of a second type of precipitate which is a particularly effective hardener. Cobalt was found to retard the formation of austenite. Overaging is a combination of classical overaging and the formation of austenite in the structure. he- activation energy for the precipitation reaction determined from resistivity ,measurements is 42.8 kcal per mole and the growth of the precipitate is found to obey at law at high tenzperatures and a tU3 law at low temperatures. HE mechanism of strengthening of the 18 pct Ni maraging steels has been studied extensively since 1962.'-? The strengthening is due to precipitation hardening of the martensitic matrix. The main precipitate is an inter metallic compound involving molybdenum, but there is disagreement about its identity.

Jan 1, 1967

By Kenneth M. Ritchie

Mineral wool is a term applied to man-made fibers of silicate glass with useful properties resulting from their fibrous nature. In contrast with crystalline fibrous minerals such as asbestos, mineral wool fibers are amorphous, solid filaments produced by drawing from molten liquid and subsequent cooling. Chemically they are silicate glass with varying percentages of metallic oxides, especially those of aluminum, calcium, magnesium, iron, and in glass wool, sodium, potassium and boron. Other elements such as manganese, titanium, sulfur, etc., result from their presence in the raw materials used and are not purposely added. In the United States, mineral wool is a generic term and may be applied to rock, slag or glass wool. In Europe, glass silk and silicate cotton are products in the same category, but the term mineral wool is less commonly used. Current usage is to ignore the actual source and to differentiate products on a composition basis; thus rock and slag wools have about 35-45 pct of silica, while glass wool has 54 to 60 pct. Much mineral wool of slag origin is called "rock wool," and this practice is increasing, although wool made of slag from lead or copper refining is often referred to as "lead slag wool." Its greenish-gray to greenish-black dark color, due to 5-25 pct Fe (reported as FeO), distinguishes it from "white" wools made from iron, blast furnace slag containing only 1-2 pct FeO or Fe203. Most mineral wool is used for thermal insulation against heat and cold; sound absorption and isolation are probably the next most important uses. Both its thermal and acoustic values result primarily from the physical structure of the heterogeneous mixture of fibers and air which is the form in which the fibers are first obtained and handled. For this reason, within fairly wide limits, differences in chemical composition are relatively unimportant, and for most conventional applications all types are competitive in properties and value. Mineral wool intended for extreme conditions of high temperature, acid resistance and special purposes must have a chemical composition which will insure the desired properties. This may differ greatly from that of ordinary wools; for example one product approximately 98 pct Si02 and another consisting of 50 pct A1203 and 50 pct Si02 are produced and sold for high temperature service up to 2000°F or more. These are considerably more expensive to manufacture and their cost limits their use. Historical The manufacture of mineral wool consists fundamentally of a process which subjects molten material to shear and/or tensile forces that draw them into fibers. The liquids are cooled at a rate which solidifies them quickly. As a solid glass they are technically super-cooled liquids since they have no true melting point. The drawing out of glass into thin rods, filaments and tubes was known from very early times, and present day continuous production of glass filament for textiles was evolved gradually by adapting hand methods to automatic machinery. Rock and slag wool manufacture had a somewhat different development. Early explorers reported finding filamentous material

Jan 1, 1960

By R. C. Ernrnons, Ray Wilcox

RECENTLY completed experimental work, carried out in the department of geology at the University of Wisconsin, aiming at a prevention of silicosis in industry has been reported in the American Mineralogist. A vast amount of work on silicosis has been reported in the literature, the clinical aspects having been especially well covered. A host of critical observations have been made on the variations in the nature of the silicosis problem in different environments, and a great deal of valuable experimental work has helped to clarify these observations. At present a greater amount of information of a critical sort is available than ever before, which affords a more sound basis for interpretive thought. It has been observed in industry that essentially pure silica dust gives rise to silicosis. Jones would modify this conclusion to place the responsibility on sericite, a silicate mineral present in the siliceous dust. Material such as granite dust, which carries a high free silica (quartz) content, is also a silicosis hazard. But sericite, too, is usually present in granite. In general it is widely believed that silicosis is caused by the presence in the lung of silicic acid regardless of the source. This view is adopted here.

Jan 1, 1937

By B. C. Craft, Murray F. Hawkins, John R. Rayne

A reservoir mechanism of sulfur recovery by the Frasch process is presented. Improving the economic, of recovery appears to be largely a well, rather than a reservoir problem. A most important factor is the limitation of the lateral extraction of .sulfur about the wells due to the almost vertical .flow of the injected hot water. Model studies are described which confirin the mechanism of sulfur recovery by presently used methods. Studies on a five-spot system indicate improved econo171ics regarding recovery, recovery rate, therinal efficiency, and well spacing. INTRODUCTION Sulfur mining by the Frasch process is one of the most important methods of sulfur production. Developed by Herman Frasch in 1894, it enjoyed a rapid growth and presently supplies 40 per cent of the world's sulfur and about 80 per cent of the U. S. sulfur." The Frasch process of mining the underground native sulfur deposits involves melting the sulfur in place by introducing super-heated water into the sulfur bearing formations, and producing the sulfur as a liquid. Many problems are encountered in mining these native sulfur deposits, and sulfur production depends chiefly upon the nature of the sulfur deposit and the underground thermal efficiency of the heat transfer system. THE RECOVERY MECHANISM Sulfur is typically found in salt dome cap rock as crystal aggregates occurring within the cavities, seams, and pores of limestone and gypsum formations.' Sulfur-bearing limestone is typically cavernous, vugular, and fractured. Porosity averages about 20 per cent and sulfur saturation averages approximately 25 per cent by weight.1,15 Vhe sulfur bearing formations are very heterogeneous in nature and physical characteristics vary widely within small distances. Total cap rock thickness may vary from 50 to more than 1,000 ft, and net productive thicknesses from a few feet to a few hundred feet. In most cases the upper portion of the limestone formation is barren of sulfur, varying from 5 to 200 ft in thickness.1,15,33 The immediately overlying sediments and the underlying dense anhydrite formation provide permeability barriers to the flow of water from the cap rock section.'" Sulfur wells are drilled with conventional oilfield drilling rigs. Fig. 1 illustrates the casing program of a completed sulfur well. The cap rock sections are drilled with core bits and continuous core logs are recorded. After coring, the cap rock section is underreamed to a diameter of 9 7/8 in. The bottom of the 8-in. casing is welded closed and rests on the bottom of the drill hole, which extends through the cap rock to a few feet above the bottom of the sulfur-bearing formation. The 8-in. pipe contains 5 ft of 3/4-in. perforations on 6-in. centers and 15 ft of 1-in. perforations on 1-ft centers. The 20-ft perforated section is set opposite the lower 20 ft of the sulfur-bearing formation. The 4-in. sulfur pipe is set inside the 8-in. water line on a seat ring at the top of the 5-ft section of 3/4-in. perforations. The mining water, heated to about 330°F under a pressure of 250 psi, is forced down the annulus between the 8-in. and 441-1. pipes and through the 1-in. perforations to the sulfur-bearing formation. Compressed air, at 400 psi pressure, is supplied through a 1-in. air line near the bottom of the well to provide air-lift of the liquid

Jan 1, 1957

By Hermann Schmalzried, Carl Wagner

UPON heating a metal oxide or sulfide in H2, first only oxygen or sulfur is removed from the surface. Thus the metal/nonmetal ratio in the oxide or sulfide increases and the thermodynamic activity of the metal increases accordingly. For the formation of metallic nuclei, a certain super saturation is necessary, i.e., the activity of the metal must become greater than unity. Once nuclei of the metal have been formed, the supersaturation is supposed to decrease. Even under steady-state conditions of a reduction process, however, the activity of the metal inside an oxide or sulfide phase must be greater than unity in order to have a driving force for the individual steps of the reduction process. As an example, consider the reduction of Ag2S with a high mobility of cations and electrons. As shown schematically in Fig. 1, the reduction process involves the following steps:' 1) sulfur removal along the entire Ag2S surface in form of H2S, 2) migration of Ag' ions and electrons from the Ag2S surface to nuclei of metallic silver, 3) transfer of Ag+ ions and electrons from the Ag2S phase to the metal. For a finite rate of step 3, the activity of silver in Ag2S next to the Ag2S-Ag interface must be greater than unity. Moreover, for a finite rate of step 2, the activity of silver at the gas-Ag2S interface must be still somewhat greater. Theoretical considerations lead to the tentative conclusion that at least under steady-state conditions the supersaturation will be rather low.' To test this conclusion, the average activity aAg of silver in a Ag2S tablet about 2 mm thick with a diameter of 5 mm was followed as a function of time by measuring the electromotive force E of the cell Pt I Ag | Agl I Ag2S I Pt where AgI is used as a solid electrolyte in which only Ag+ ions are mobile. The activity aAg is calculated as aAg=exp(-EF/RT) Since the diffusion coefficient for transport of silver in Ag2S is very high (- 3 . l0-2 sq cm per sec),3 the average activity aAg is representative for both the bulk and the surface of the Ag2S tablet. Experiments were conducted at about 400°C. The cell was surrounded by an aluminum block in order to secure a uniform temperature and to eliminate thermoelectric effects. With the help of a potentiometer, first a potential of 0.16 v was applied to the above cell in argon in order to obtain a well defined initial state with a Ag/S ratio close to 2.000.~ Then the cell was disconnected from the potentiometer and a gentle stream of H2 was passed along the Ag2S surface. In view of the removal of sulfur in form of H2S, the electromotive force E decreased within 20 to 30 min to zero corresponding to a Ag/S ratio of 2.003 and became negative, indicating a value of aAg> 1. A representative plot electromotive force E vs time is shown in Fig. 2. The minimum of the electromotive force characteristic of the onset of

Jan 1, 1963

By C. F. Floe, M. Cohen, M. B. Bever, V. G. Paranjpe

NITROGEN is becoming recognized as one of the important elements in ferrous physical metallurgy. Several investigations indicate that nitrogen plays a significant part in such phenomena as strain aging and temper brittleness. Nitrogen is known to be a powerful austenite stabilizer and may be a useful alloying element in stainless steels. The hard-enability of steels has been found to be increased by nitrogen. The nitriding and carbonitriding pro- cesses are examples of successful industrial application of nitrogen in ferrous materials. For a complete understanding of the various roles played by nitrogen in ferrous metallurgy a knowledge of the phase relations in the binary iron-nitrogen system is essential. The literature contains a variety of iron-nitrogen phase diagrams. Those suggested by Fry, Sawyer,² Epstein and his coworkers,³,4 Lehrer,5 Eisenhut and Kaupp, and Hägg7,8 differ significantly from one another. Moreover, the most recent of these investigations dates back about twenty years. A re-determination of the entire diagram, therefore, appeared desirable. In addition to the published phase diagrams, investigations have been carried out on portions of the iron-nitrogen system. Bramley and Haywood determined the composition and temperature of the iron-iron nitride eutectoid. The maximum solubility of nitrogen in a iron was investigated by Portevin and Seferian10 and by Diikstra. 11 Several investigators have determined the crystal structure of the various iron-nitrogen phases. In fact, Eisenhut and Kaupp6 and Hägg7 based their entire phase diagrams on the results of such studies. Epstein' and Emmett12 reported lattice-parameter measurements on the E (hexagonal close-packed) phase. Osawa and Iwaisumi13 also studied the change in lattice parameters of the a, ? and E phases with nitrogen content. Brill" and Hägg7 showed that the y' phase has an ordered structure, and Hendricks and Kostingsl5 suggested a structural relation between the E and phases. In a recent investigation Jackl6 arefully studied the super-lattice reflections from the y' and phases. Experimental Procedure A large variety of experimental methods has been used by previous investigators in studying the iron-nitrogen system. These methods include thermal analysis, microscopic examination, X ray diffraction, magnetic measurements, dilatometric analysis and anelastic experiments. Thermal analysis is of low accuracy in determining changes in the solid state. This accuracy is further decreased for iron-nitrogen alloys since composition changes will occur during heating or cooling unless extreme care is taken to use a proper atmosphere. Metallographic methods are of small value . because homogeneous iron-nitrogen alloys of sufficient size can be produced only with great difficulty. The dilatometric method is open to the same objections as thermal analysis in that changes in composition may occur during heating and cooling. Lattice parameter measurements by X ray diffraction can be used satisfactorily for determining phase boundaries if cooling is fast enough to prevent structural changes. In view of the limitations of the various other techniques two methods only were adopted in this investigation, (1) X ray diffraction measurements, and (2) a controlled nitrogenizing method. The second method is an innovation for investigating the iron-nitrogen system, and will be described at length. Materials: All iron-nitrogen alloys were prepared from carbonyl iron powder of the analysis shown in table I. The average particle size was about 20

Jan 1, 1951