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By Craig R. Barrett, Oleg D. Sherby

The creep characteristics of four pure metals with widely Varying stacking-fault energies (silver, copper, nickel, and aluminum) were evaluated above 0.5Tm. Creep tests were performed under conditions of constant atomic diffusivity and constant stress over the elaslic modulus. The sleady-state creep rate, Es, was found to he a funclion of the THE most common empirical representation of the steady-state creep rate, Es, at high temperatures and intermediate stresses is of the form where a is the applied stress, E is an elastic constant, A and n are constants (n is typically stacking-fault energ, y, such that Es is proportional to y3,5. In addition, it was uncovered that the primary creep strain and the strain to fracture increased with increasing y, and that the ratio of initial to steady-state creep rate decreased with increasing y. about 5), Q is the activation energy for creep (usually equal to that for self-diffusion), and kT has its usual meaning. sherbyl and McLean and ale' have used this expression to correlate creep data for a number of pure metals. An interesting aspect of Eq. [I] is the absence of any dependence on the stacking-fault energy. While most creep data seem to obey the stress and temperature dependence predicted by Eq. [I], when data for several metals are put on a master plot they do not fall on a common line but form a band. The width of this band corresponds to a variation in Es of 102 to l03. sherbyl attempted to explain this band by assuming that a grain-size effect was present which led to the observed variation. On the other hand, Felt-

Jan 1, 1965

By E. N. Aqua, C. M. Owens

The microstructure in cold-rolled Zircaloy-4 sheet has been characterized by transmission electron microscopy and X-ray diffraction line-broadening techniques. The rate of work hardening is measured in terms of microstrains, particle sizes, micro hardness, the tensile yield strength. The tensile yield strength of Prestrained (less than 10 pet) Zircaloy-4 sheet is found to be a linear function of the square root of the dislocation density, us predicted by work-hardening theories. ZIRCALOY is one of the most important structural alloys for nuclear reactor applications.''2 In order to understand the effects of the nuclear environment on Zircaloy structural members, the preirradiation microstructure must be characterized. This report will describe the substructure existing in cold-rolled Zircaloy-4 sheet as observed by electron microscopy and by X-ray diffractometry. I) EXPERIMENTAL PROCEDURE Commercial Zircaloy-4 strip was cold-rolled and annealed in argon at 760°C for 1 hr. The annealed sheet was again cold-rolled to a maximum of 50 pct reduction in thickness with segments of the strip being retained after 2.5, 5, 10, and 20 pct reductions. One-inch-square portions were chemically polished (50 parts HNO3, 50 parts H2O, 10 parts HF) and mounted onto lucite blocks using double-sided tape to prevent bending during handling. Thin foils suitable for transmission electron microscopy were prepared from each of the sheet samples. The sheets were mechanically polished through 600-grit paper to a 3 to 4 mil thickness and were chemically polished by immersion for 1 to 2 min in a solution containing: 50 parts HNO3, 50 parts H2O, and 10 parts HF, and rinsed in distilled water. The final metallographic procedure was to electropolish for less than 10 sec with an electrolyte of 10 parts perchloric acid and 90 parts glacial acetic acid, at 20 v, at room temperature using stainless-steel point cathodes and a vigorous stirring action. These foils were examined in a Philips EM 200 electron microscope using a 100-kv accelerating voltage.

Jan 1, 1968

By GEO H. DEIKE

NOT much activity has been evident during the past year in the establishment of co-operative scholarships but the interest among the coal-mining companies is more pronounced than ever. This is apparent from the replies received to a letter sent out by the Committee on the Promotion of Student Interest in Coal Mining to over 120 coalmine operating officials. With that letter was forwarded a bulletin issued by the school of mineral industries of The Pennsylvania State College entitled ?Industrial Scholarships ? a Partnership of Industry and Education.? In that circular was outlined the need for trained men in the war and postwar world, and particularly as such demands pertain to the growth of the mineral industries.

Jan 1, 1943

By Magnus Troilius

For some time I have been using with great advantage, for the purpose of determining rapidly and accurately the chemical composition of gases from Siemens producers, an apparatus arranged generally like that proposed by Prof. Eggertz; * and I now take pleasure in laying before the members of the Institute a description of the apparatus and its use, hoping that some of them may find it. of practical advantage. At the end of the paper are given some results obtained and heat calculations, with the necessary data for the same. COLLECTION OF GASES. Fig. 1. Shows the arrangement for taking a sample of gas. The funnel F, which may be made of tin plate, is made to fit the test-hole. The gas passes up through the funnel and through the rubber-tubing with the glass tube K, filled with asbestos for retaining dust,, and is drawn into the upper flask by means of water flowing from the same into the lower flask. The upper flask must be completely filled with water from the beginning, so that no air remains. When filled with gas the screw-compressors are securely fastened on, and the flask disconnected from the funnel and receiver. Quart flasks, with openings at the bottom, are very suitable, and easily obtainable. COMPOSITION OF THE GASES. The ingredients found in producer gases are: carbonic acid (CO2), oxygen (0)) ethylene (C2H4), carbonic oxide (CO), hydrogen (H), and marsh gas (CH4). The nitrogen is taken by difference. CO2,O,C2H4, and CO are determined by absorption in various liquids and by observing the resulting diminution of volume. H and CH4 are determined by combustion with oxygen. Carbonic acid.—For this gas is used a solution of 16 grams of potassium hydrate in 100 C.C. of water. 4 or 5 C.C. of this solution absorb 100 C.C. of CO2.

Jan 1, 1883

By P. H. Mell

AMONG the minerals exhibited at the Atlanta Exhibition of 1881, soapstone, kaolin, and asbestos were well represented. The first two occur in large quantities, of very pure quality, throughout the South. The last is somewhat limited in amount, yet in certain localities it exists in masses sufficiently large to pay for working; in North Carolina, Georgia, and Alabama it has been mined with some profit. I would, in this paper, call special attention to the minerals soapstone and kaolin, because their many valuable qualities seem to have been al most entirely overlooked by our Southern manufacturers. Steatite, particularly, occurs in such large quantities, and generally in such close proximity to the great iron regions of Alabama and Georgia, that it is amazing that the iron companies will persist in sending abroad under. heavy expense for firebrick. It would require a much smaller sum of money to quarry this rock and place it at the various furnaces ; and the results obtained, I am sure, would prove its superiority over the majority of firebrick brought into this region. Soapstone, as well as kaolin, is found throughout the metamorphic regions of Alabama, Georgia, South Carolina, and North Carolina. Below-will be found seven analyses that I have made of this mineral, taken from various points in the four States above mentioned. I have also subjected these same specimens to severe fire-tests, and the results were very satisfactory. The tests were conducted in the following manner: Small portions of the compact variety were carefully weighed and placed in a Fletcher's new crucible furnace for gas, and subjected for half an hour to a heat that will in 12 minutes fuse iron. The only effect upon these specimens was a slight change in color .to a darker shade, a small loss in weight, due evidently to the evaporation of water, and, in one or two specimens, a slight degree of fusion on the sharp edges. The first specimen subjected to investigation was taken from a large outcropping in Tallapoosa County, Alabama. Specific gravity, 2.88 ; hardness, 1.9; color, blue gray. Composition Water, - 2.68 Silica, - 65.46 Iron oxide, - 2.10 Alumina, - 15.02 Magnesia, - 15.35 100.61

Jan 1, 1882

By H. Ries

THE stabilization of a gravel road with soil is a method of treatment developed in recent years by the United States Bureau of Public Roads for the purpose of binding the constituents together better, and maintain-ing a more durable surface. The process consists in adding to the gravel or crushed stone and sand, a soil mortar, so-called, of fine sand, silt and clay, mixed in the proper proportions. The coarse gravel and sand supply structural strength and hardness; the fine sand adds embedment support to the coarse sand; the silt acts as a filler to prevent the granular particles from rocking; while the clay serves not only as a binder but also provides pores minute enough to cause connecting moisture films which are supposed to have high cohesive properties1. It will be recognized that the clay is an important ingredient both when wet and dry, and should not show excessive expansion when wet, nor correspondingly high shrinkage in drying, as otherwise there is danger of unseating the nonplastic particles. Such a stabilized road, although an improvement on one with a floating surface, will in course of time be subject to wear, and become dusty when the clay dries out and breaks up. It has been found that if some salts are added to the road mixture they tend to maintain the soil moisture and prevent dustiness of the road or raveling of the road surface. In addition to this, it is claimed that these dissolved salts cause a thinning of the moisture films on the particles, thus permitting greater compaction of the road mixture, and thereby increasing its density. This fact can be proved by noting the increased compaction which a road mixture shows when certain salts are added to the soil water. Since certain chemical substances such as sodium chloride are electro-lytes, the question arises whether they cannot have some effect on. the qualities of the clay in the soil mortar, and perhaps improve them. In view of the fact that certain salts seem to exert a favorable effect on the road mixture it is desirable that they be held in the road soil as long a time as possible.

Jan 1, 1936

By W. R. Crane

While professiorlally engaged in the oil- and gas-fields of Kansas, in measuring the pressure and flow of gas-wells, and studying the phenomena attendant upon the production of both oil and gas, I noticed in the flow of gas a peculiar and interesting feature. That there are actual lines of flow in liquids (non-compressible fluids) discharged through an orifice, or a short section of pipe, is shown by the external shape of the discharge—the vena contracts. Such lines of flow are not observable in the discharge of gas from an orifice. It can hardly be questioned that they exist. That they are not apparent is probably due to the very small weight of the gaseous particles, which climinishes the momentum of their movement in a given direction, acquired before they issue from the orifice, and also to the expansion of the gases, which would exert a powerful influence in overcoming any such tendency in their flow. Gas flowing from an orifice, supplied by a large reservoir or blowing-engine, exhibits almost the reverse of what is noticed with liquids. Namely, the gas assumes the form of an inverted truncated cone, of large angle: with its apex-end at the orifice. (See BB, Fig. 1.) This external ahape assunled by the flow of gas shows, however, marked differences under varying conditions of volume and pressure. For instance, a large volume of gas under high pressure, flowing through a 2- or 3-in. pipe, as in the case of a natural gas-well, assumes a more definite conical form, the angle of which increases as the pressure falls. Moreover, outside of the well-defined inverted cone is a thin conical heath or zone of gas, A A, the angle of which is considerably greater than that of the main cone, and increases with +1UNIVERSITY OF KANSAS, LAWRENCE, KANSAS.

Jan 1, 1905

By P. H. Mell

AMONG the minerals exhibited at the Atlanta Exhibition of 1881, soapstone, kaolin, and asbestos were well represented. The first two occur in large quantities, of very pure quality, throughout the South. The last is somewhat limited in amount, get in certain localities it exists in masses sufficiently large to pay for working; in North Carolina, Georgia, and Alabama it has ken mined with some profit. I would, in this paper, call special attention to the minerals soapstone and kaolin, because their many valuable qualities seem to have been almost entirely overlooked by our Southern manufacturers. Steatite, particularly, occurs in such large quantities, and generally in such close proximity to the great iron regions of Alabama and Georgia, that it is anlazing that the iron companies will persist in sending abroad under heavy expense for firebrick. It would require a much smaller sum of money to quarry this rock and place it at the various furnaces ; and the results obtained, I am sure, would prove its superiority over the majority of firebrick brought into this region. Soapstone, as well as kaolin, is found throughout the metamorphic regions of Alabama, Georgia, South Carolina, and North Carolina. Below will be found seven analyses that I have made of this mineral, taken from various points in the four States above mentioned. I have also subjected these same specimens to severe fire-tests, and the results were very satisfactory. The tests mere canducted in the following manner: Small portions of the compact variety were carefully weighed and placed in a Fletcher's new crucible furnace for gas, and subjected for half an hour to a heat that will in 12 minutes fuse iron. The only effect upon these specimens was a slight change in color to a darker shade, a small loss in weight, due evidently to the evaporation of water, and, in one or two specimens, a slight degree of fusion on the sharp edges. The first specimen subjected to investigation was taken from a large outcropping in Tallapoosa County, Alabama. Specific gravity, 2.88 ; hardness, 1.9; color, blue gray. Composition: Water,....2.68 Silica,..........65.48 Iron oxide,.........2.10 Alumina,.........15.02 Magnesia,... 15.35 10061

Jan 1, 1882

If problems are opportunities in disguise, the mining industry certainly had plenty of "opportunities" in 1975. Considering the industry's generally lackluster 1975 profit record, and in view of the slowdown in inflation, there's some hope that 1976 might be a better year in spite of the increasing risks and uncertainties that plague the mining industry.

Jan 2, 1976

By Huey-Lin Luo, T. R. Anantharaman, William Klement

Two new metastable phases have been obtained in Au-Ge alloys by rapid cooling from the melt. One is of the hep structure with near-ideal axial ratio and may be considered a Hume-Rothery phase. The other has a complex tetragonal structure (a = 11.627Å and c = 22.191Å for the Au60Ge40 alloy) and may be looked upon as a superlattice made up of forty-four fee unit cells. Alloys with the tetragonal phase are charactevized by marked preferred orientation. The metastable constitution of the Au-Ge alloys is discussed with reference to the rate of cooling from the melt. THE Au-Ge equilibrium diagram features a rather deep eutectic near 27 at. pet Ge with a maximum solid solubility of 3.2 at. pet Ge in gold and is similar to the Ag-Ge, Ag-Si, and Au-Si diagrams.' The present study of the effects of rapid cooling from the melt on the structure of Au-Ge alloys constitutes an extension of similar investigations2-8 in this laboratory on alloys of noble metals with germanium and silicon. Nonequilibrium hep structures have so far been obtained by quenching Ag-Ge2, 3 and Ag-Si4, 5 alloys from the melt; an Au-Si alloy of approximately eutectic composition has been found6 to solidify in a noncrystalline state. EXPERIMENTAL PROCEDURES Twenty-nine alloys prepared from gold of 99.9+ pet and germaium of 99.999 + pet purity were investigated. The method of alloy preparation, the technique of rapid quenching from the melt, and the X-ray diffraction procedures were similar to those described previously.3, 4 Essentially, small sections (-20 mg) of thin alloy rods (-1 mm diam) were rapidly heated up to 1200°C in a graphite crucible under argon and the liquid alloy ejected by a helium blast onto a polished copper strip held on the inner periphery of a rotating wheel. The resulting thin foils were examined with or without the copper substrate in a G.E. X-ray Diffractometer or in a 114.6-cm-diam Debye-Scherrer camera. RESULTS Table I gives the constitution of liquid-quenched Au-Ge alloys, as estimated from intensities of X-ray reflections from the corresponding phases, viz., a (fee solid solution), ß (hep phase), ? (tetragonal phase), and diamond-cubic (dc) germanium. Despite unavoidable variations in the quenching rates, the proportions of the phases in different alloys were generally reproducible and stable at room temperature. There was no evidence of quenching strain, since the a doublets were well-resolved in high-angle Debye-Scherrer reflections in all cases except where stacking faults in the a fee and ß hep structures contributed to X-ray line broadening. The ß and ? metastable phases showed signs of decomposition to the equilibrium a phase and germanium only after a few hours annealing above 100°C. A few alloys around the eutectic composi-

Jan 1, 1965

By K. O. Stamm, B. A. Rogers

Because it is the basis of the economically important operation of hardening steel by quenching, the A3 transformation in iron has been the subject of numerous investigations. Although the contributions to this subject are interesting, no general review will be given here. Readers who care to follow the matter further are referred to the comprehensive summary by Cleaves and Thompson,l which covers the literature to about 1935. Their references to 53 papers on the subject suggest that further investigation is hardly justifiable. However, considerable interest has devel oped recently concerning the reversibility of the transformation. From thermo-dynamic considerations, the transition ought to occur at the same point on heating or cooling, if the change of temperature is sufficiently slow. Yet all of the earlier investigators found a difference of several degrees. Burgess and Crowe,2 who used thermal methods, obtained average temperatures of 912" for Ac3 and 900°C. for Ar3 on electrolytic iron. Their data indicate a considerable range of temperature over which the change occurs, both on heating and on cooling. Terry3 measured the susceptibility in the critical range and estimated from the steepest parts of his curves that Ac3 came at 9I8° and Ar3 at 903°C. Ishiwara4 was one of the first investigators to report a shorter interval between the temperature of the change in the two directions. He measured the change of susceptibility of kaolin-coated samples of steel, in a hydrogen atmosphere, at rater of heating and cooling so low that about 3 or 4 hr. were required for the transformation to complete itself. His results show some variability between samples, but indicate that the difference between Ac3 and Ar3 is in the vicinity of 6°C. Roberts and Davey5 measured the space lattice in pure iron in the vicinity of 900°C. and concluded that a change occurs reversibly between 907' 3" and 910" 3°C., probably between 907" and 910°C. Wells, Ackley, and Meh16 made dilatometric determinations of the Ac3 and Ar3 points in samples of hydrogen-treated carbonyl iron maintained under a vacuum. They used three rates of heating and cooling: 2°, ½°, and .?°C. per min. and found the spread between the two points decreased with low rates. At the slowest rate, the Ac3 transition occurred at 909° to 909. 5°C. and the Ar3 change at 907°C. in three of the samples believed to contain the lowest percentages of alien elements. They concluded that if the rate of temperature change and the content of alien eiements were low enough, the A3 transformation would be completely reversible at 909.50 + 1°C. The question of reversibility is an interesting one and when some iron with especially small percentages of alien elements became available the opportunity to conduct an investigation was welcomed. This iron was prepared by the Division of

Jan 1, 1942

By B. A. Rogers, K. O. Stamm

Because it is the basis of the economically important operation of hardening steel by quenching, the A3 transformation in iron has been the subject of numerous investigations. Although the contributions to this subject are interesting, no general review will be given here. Readers who care to follow the matter further are referred to the comprehensive summary by Cleaves and Thompson,l which covers the literature to about 1935. Their references to 53 papers on the subject suggest that further investigation is hardly justifiable. However, considerable interest has devel oped recently concerning the reversibility of the transformation. From thermo-dynamic considerations, the transition ought to occur at the same point on heating or cooling, if the change of temperature is sufficiently slow. Yet all of the earlier investigators found a difference of several degrees. Burgess and Crowe,2 who used thermal methods, obtained average temperatures of 912" for Ac3 and 900°C. for Ar3 on electrolytic iron. Their data indicate a considerable range of temperature over which the change occurs, both on heating and on cooling. Terry3 measured the susceptibility in the critical range and estimated from the steepest parts of his curves that Ac3 came at 9I8° and Ar3 at 903°C. Ishiwara4 was one of the first investigators to report a shorter interval between the temperature of the change in the two directions. He measured the change of susceptibility of kaolin-coated samples of steel, in a hydrogen atmosphere, at rater of heating and cooling so low that about 3 or 4 hr. were required for the transformation to complete itself. His results show some variability between samples, but indicate that the difference between Ac3 and Ar3 is in the vicinity of 6°C. Roberts and Davey5 measured the space lattice in pure iron in the vicinity of 900°C. and concluded that a change occurs reversibly between 907' 3" and 910" 3°C., probably between 907" and 910°C. Wells, Ackley, and Meh16 made dilatometric determinations of the Ac3 and Ar3 points in samples of hydrogen-treated carbonyl iron maintained under a vacuum. They used three rates of heating and cooling: 2°, ½°, and .?°C. per min. and found the spread between the two points decreased with low rates. At the slowest rate, the Ac3 transition occurred at 909° to 909. 5°C. and the Ar3 change at 907°C. in three of the samples believed to contain the lowest percentages of alien elements. They concluded that if the rate of temperature change and the content of alien eiements were low enough, the A3 transformation would be completely reversible at 909.50 + 1°C. The question of reversibility is an interesting one and when some iron with especially small percentages of alien elements became available the opportunity to conduct an investigation was welcomed. This iron was prepared by the Division of

Jan 1, 1942

By B. A. Rogers, K. O. Stamm

BECAUSE it is the basis of the economically important operation of hardening steel by quenching, the A3 transformation in iron has been the subject of numerous investigations. Although the contributions to this subject are interesting, no general review will be given here. Readers who care to follow the matter further are referred to the comprehensive summary by Cleaves and Thompson,1 which covers the literature to about 1935. Their references to 53 papers on the subject suggest that further investigation is hardly justifiable. However, considerable interest has developed recently concerning the reversibility of the transformation. From thermodynamic considerations, the transition ought to occur at the same point on heating or cooling, if the change of temperature is sufficiently slow. Yet all of the earlier investigators found a difference of several degrees. Burgess and Crowe,2 who used thermal methods, obtained average temperatures of 912° for Ac3 and 900°C. for Ar3 on electrolytic iron. Their data indicate a considerable range of temperature over which the change occurs, both on heating and on cooling. Terry3 measured the susceptibility in the critical range and estimated from the steepest parts of his curves that Ac3 came at 9180 and Ar3 at 903°C. Ishiwara4 was one of the first investigators to report a shorter interval between the temperature of the change in the two directions. He measured the change of susceptibility of kaolin-coated samples of steel, in a hydrogen atmosphere, at rates of heating and cooling so low that about 3 or 4 hr. were required for the transformation to complete itself. His results show some variability between samples, but indicate that the difference between Ac3 and Ar3 is in the vicinity of 6°C. Roberts and Davey5 measured the space lattice in pure iron in the vicinity of 900°°C. and concluded that a change occurs reversibly between 907° ± 3° and 9100 ± 3°C., probably between 907° and 910°C. Wells, Ackley, and Mehl6 made dilatometric determinations of the Ac3 and Ar3 points in samples of hydrogen-treated carbonyl iron maintained under a vacuum. They used three rates of heating and cooling: 2°, '1/2°, and 1/8°C. per min. and found the spread between the two points decreased with low rates. At the slowest rate, the Ac3 transition occurred at 909° to 909.5°C. and the Ar3 change at 907°C. in three of the samples believed to contain the lowest percentages of alien elements. They concluded that if the rate of temperature change and the content of alien elements were low enough, the A3 transformation would be completely reversible at 909.5° ± I°C. The question of reversibility is an interesting one and when some iron with especially small percentages of alien elements became available the opportunity to conduct an investigation was welcomed. This iron was prepared by the Division of

Jan 1, 1941

By Robert B. Fulton

The objective of this chapter is to discuss the interrelationship between industrial minerals and chemical manufacturing. It is intended to supplement rather than duplicate the commodity chapters. Particular emphasis is given to the pertinent chemical element and to market factors. Condensing this broad subject into a few pages of this handbook permits treating only the most important elements derived from industrial minerals. Hydrocarbons, which quantitatively dominate as raw materials for the chemical industry, are omitted, as are the metallic elements and the minerals covered in other "use" chapters such as phosphorous, potassium and nitrogen for fertilizers, and titanium dioxide for pigments. The remaining six elements of major importance are: boron, bromine, chlorine, fluorine, sodium, and sulfur. These elements are treated individually under separate headings. Table I (Jones, 1973) affords an overview of the main industrial minerals, the chemical products derived from them, and end uses of the products. Salt brines have particular importance as raw material sources for the chemical industry. Table 2 (Anon., 1967) is a chart of the chemical compounds derived from four types of brines: (1) Owens Lake-type brines, which are sources of boron and sodium compounds; (2) Midland-type brines, from which bromine, iodine, and chlorides of calcium, magnesium, potassium and sodium are derived; (3) Searles Lake-type brines, yielding boron, bromine, lithium, magnesium, potassium, and sodium compounds; and (4) Silver Peak-type brines, produced mainly for lithium. Market Attributes Some of the important market traits common to industrial minerals used by the chemical industry are listed below. 1. They are international commodities, such as fluorspar and sulfur, which largely move to foreign consumers. 2. Grade, and freedom from deleterious elements are important factors affecting their usability in chemical processes. An example is salt (NaCl) used in electrolysis where ultrapure evaporated salt is required to meet rigid specifications. 3. Purified products take on the characteristics of specialty items and command a distinctly higher price than the basic commodity from which they are derived. 4. In practically all cases, chemical users require some sort of cleaning or beneficiation of the naturally-occurring mineral to bring it to specification, and individual specifications may vary from user to user for essentially the same use. 5. In some instances it is necessary to strike a balance between what the vendor can supply and what the buyer requires, with the result that specifications have to be eased to afford the needed materials in marginal cases. 6. Because they tend to be bulk commodities, low cost for handling and transportation are important and such costs may limit the area from which a chemical user can draw his supply. For example, fluorspar from China and Thailand normally goes to Japan, while South African fluorspar can go either to Japan or to the US. 7. Shipments are usually in bulk and frequently in multiple-car, full-trainload or full-shipload lots to reduce transport costs, which in turn may require large terminal investment facilities.

Jan 1, 1983

By H. I. Aaronson

Isothermally formed plates of proeutectoid a, lengthen at approximately the rates predicted by the Zener-Hillert equation, indicating that their lengthening kinetics are controlled by the volume diffusion of chromium in the ß matrix. Solution annealing treatments in the vicinity of the transus introduce a second mode of transformation, in which the lengthening rate is at least 1.8 x 104 faster than predicted by this equation. Little or no volume diffusion appears to accompany the latter transformation. The Presence of oxygen is evidently a Prerequisite for the occurrence of this reaction. X HE effects of thermal history prior to the initiation of transformations which proceed by nucleation and diffusional growth are currently evoking considerable interest. The rate of nucleation (but not the rates of growth) of pearlitel and of bainite,2 and the over-all rates of aging reactions in Al-cu3 and Al-si4 alloys have been shown to be appreciably dependent upon thermal history in the solid-solution region"' or in the two-phase region prior to the onset of pre~ipitation.3,4 In none of these reactions, however, was the transformation mechanism changed by variations in the temperature-time path used to reach the reaction temperature. Preliminary experiments reported by M. K. McQuillan5,8 and a systematic investigation by Farrar and Margolin7 have disclosed that the transformation behavior of hypoeutectoid Ti-Cr alloys is considerably more sensitive to thermal history. Qualitative evidence strongly suggests that not only the rate of nucleation but also the rate of growth and even the mechanism of the ß — a reaction can undergo remarkable changes when a solution annealing treatment in the vicinity of the ß/a +ß, or transus temperature, is interposed between a high-temperature solution anneal (conventionallq at 1000°C) and the isothermal reaction treatment. The present investigation was undertaken in an attempt to ascertain the nature and origin of these effects. Study of the changes in the kinetics and morphology of the ß - a, reaction produced by varialtions in thermal history was the primary means employed for this purpose. EXPERIMENTAL PROCEDURE The compositions of the alloys used in this in~esti~ation are given in Table I. These alloys were homogenized for 5 days at 1050° C in evacuated (2 x 10 -5 mm of Hg), zirconium-gettered fused quartz capsules. The capsules themselves were enclosed in a porcelain chamber evacuated with a mechanical pump during the homogenization anneals. Upon completion of homogenization, the alloys were cooled to room temperature and then reheated to 550°C for 3 1/2 days in order to transform the alloys to a finely divided mixture of a and TiCr2, and thus provide an approximately constant initial mi-crostructure. Individual specimens were sealed in evacuated and internally gettered Vycor capsules and heat treated as previously described.8,9 EXPERIMENTAL RESULTS Ti-10.64 Pet Cr. This investigation was largely performed on the 0.64 pet Cr alloy. The "base"

Jan 1, 1962

By A. N. Holden, J. H. Hollomon

Inhomogeneous yielding during the early stages of plastic flow has been observed in many metals and has long been a subject of controversy. Low carbon steel, when strained at room temperature, exhibits a distinct yield point at which the metal ceases to behave elastically and begins to flow plastically without further increase in stress,† often with an actual decrease in stress from that existing at the yield point. One manifestation of this behavior is the familiar Lüders lines. The extent of the yield point elongation (the plastic strain which results without raising the stress above that at the initial yield point) may be several percent. Several explanations of this type of yielding in steels have appeared in the literature:1-3}; 1. The segregation of carbides or other constituents at the grain boundaries of ferrite forms cell-like blocks which break down at a higher stress than that at which the ferrite alone will flow. 2. The precipitation of various constituents within the ferrite itself in some way blocks initial flow until a higher stress is reached, after which a great deal of flow occurs without further increase in stress. 3. The restraining influence of neighboring, less favorably oriented grains in a polycrystal results in a storing up of energy, which on yielding is sufficient to cause the continued propagation of slip bands on the multiplicity of slip systems available in adjacent iron crystals without increase in stress. 4. Local segregation of carbon atoms increases the stress required for the initial propagation of dislocations. The stress required for further deformation is lower.3 Such an explanation would require the presence of upper and lower yield points in single crystals. Low and Gensamer2 have shown that heterogeneous yielding can be eliminated by removal of carbon and nitrogen from polycrystalline steels by wet-hydrogen treatment. They also demonstrated that the re-introduction of minute amounts of carbon or nitrogen caused a return of the yield point. Observations of the initial flow of single crystals containing small amounts of carbon and nitrogen- should provide a clue to the explanation of inhomogeneous yielding. Previous tests of iron crystals4-6 can not be considered conclusive because it is uncertain whether the carbon and nitrogen were satisfactorily removed by the decarburization technique employed. The purpose of the experiments described herein was to determine whether single iron crystals containing either carbon or nitrogen would exhibit in-homogeneous yielding. Experimental Procedures THE PREPARATION OF SINGLE CRYSTALS All crvstals were formed in the following way. Aluminum killed sheet material 80 mils thick was machined into specimens of the outer contour shown in Fig 1. These mildly tapered specimens were decarburized at 730°C for 16 hr in hydrogen that had been bubbled rapidly through water maintained at 70°. The resultant grain size after decarburizing was approximately ASTM 5. Several stress-strain curves were made of the decarburized niate-

Jan 1, 1950

By H. W. Hitzrot, R. H. Limons, L. V. Fegan

The testing of a new method for measuring pellet-bed temperatures in the traveling-grate or shaft furnace is presented in this paper. This method, using silver-palladium alloy wires as indicators, overcomes disadvantages existing in the methods based on the use of thermocouples which are costly and time-consuming. The authors have developed and tested a new method for measuring pellet-bed temperatures in the traveling-grate or shaft turnace through the use of silver-palladium alloy wires as indicators. This method overcomes the disadvantages of existing methods, which, based on the use of thermocouples, are generally costly and time-consuming. For example, in the case of the traveling-grate furnace, the installation of an instrumented pellet, together with its attached thermocouples, requires stopping the furnace, with resulting loss of production time. As for temperature measurement in the shaft furnace by the existing method, the movement of the shuttle-car feeder seriously interferes with both the actual insertion and the resulting distribution of continuously fed thermocouples. The authors have overcome these difficulties by using, as temperature indicators, a range of silver-palladium alloy wires that can be easily recovered, after firing at any desired location in a pellet furnace. Silver-palladium wires having specific melting points from 2000°F to 2500°F are enclosed in ceramic capsules. Each capsule is placed in a ni-chrome wire basket filled with a sample of green pellets, the baskets being the means for recovering the capsule after firing. After the encapsulated wires have been exposed to the firing cycle, the alloy wires are examined to determine the maximum temperatures attained by the pellet sample. This method gives accurate, rapid determinations of maximum temperatures attained during pellet induration in either the traveling-grate or shaft furnace The new method has the following advantages over existing methods: 1) it is less expensive; 2) no furnace downtime is required; 3) the testing units can, be made in quantity in advance; 4) measurements can be made in rapid succession at all desired locations; 5) measurements of maximum firing temperatures are more accurate; 6) on the basis of points 4 and 5, the new method gives a more reliable picture of the correlation of pellet quality, petrographic textures and maximum temperatures, thus providing a more effective quality-control tool. A disadvantage of the method is, of course, that the measurements are not continuous and only maximum temperatures are determined. TEST PROGRAM Preparation of Materials: CALIBRATION OF ALLOYS - In the following discussion the term "bead point" (see Fig. 1) refers to the temperature at which each alloy begins to melt and form a bead. Fig. 2 gives the bead point curve for silver-palladium alloys. Before the alloys are used in plant tests, the bead point of each alloy should be determined in the laboratory to verify the alloy compositions. Once a given alloy has been calibrated, it can be

Jan 1, 1965

By G. W. Sheary

At Bethlehem's Grace mine's 6000-tpd pelletizing plant a cascade control system is utilized to approach a constant magnetite filter cake moisture, a critical factor in obtaining quality green pellets. Variables being controlled by instrumentation are filter feed solids, filter tub level, first and second stage pump sump levels and thickener sludge level, all at varying feed rates. Startup difficulties, modifications and contemplated additions to obtain closer control of the moisture are discussed. Situated 45 miles west of Philadelphia and 50 miles southwest of Bethlehem Steel Co. 's Beth-lehem plant, the integrated Grace mine facilities produce 4000 tpd of high-quality iron ore pellets. Startup of the Grace mill was in November 1958, and iron concentrates were shipped until March 1960, when the pellet plant went into operation. The underground mine, when fully developed, will hoist about 9000 tpd, including development rock. The crude ore, which has an iron content of approximately 42%, is magnetically cobbed and crushed in closed circuit with %-in. slotted vibrating screens. The ore is washed and screened in the mill and the 1/4-in. screen product is again cobbed prior to feeding to the rod mills. Grinding is done in rod mills, and in ball mills that are in closed circuit with 30-in. cyclones, to 1% on 100 mesh and 65% -325 mesh. The ground ore is magnetically concentrated by three-drum permanent-type finisher magnets to 67% Fe. The magnetite concentrate is pumped from the mill to a 50-ft thickener in the pellet plant. The thickened magnetite concentrate is relayed to the filters through a two-stage pump arrangement. The filter cake is fed by belt from filter concentrate bins to mixer-muller belts where it is intimately mixed with bentonite and a slight amount of water for moisture control. The fluffed concentrate then drops into balling cones. The green pellets from the balling cones are fed in a prescribed feed pattern to shaft furnaces through the use of shuttle car mechanisms. The green pellets are dried, heated to 2500°F and cooled to 1200°F as they descend through the furnace and into pellet coolers where the pellets are further reduced in temperature to 250°F. Heat is recovered in the cooling process through the use of air-to-air heat exchangers. The cooled pellets discharge on a rubber conveyor belt and are transferred to 6000-ton pellet railroad loading bin. The final pellet product consists of 90% +'1/4 in. material (after tumble testing1) and contains 66% Fe plus 3% silica. It has been the usual practice to maintain constant filter tank level by pumping an excess constant volume and using a moveable fishtail splitter to divert the desired amount of slurry to the filter tank. The excess from the fishtail and from the filter overflow pipe, which maintains a constant level, is returned to the source. At the Grace mill, tremolite builds up in the pipelines when pumping heavy magnetite concentrate slurries, making it necessary to use polyvinyl

Jan 1, 1962

By Louis E. Toth, Alan W. Searcy

A modification of Le Claire's microscopic model for self-diffusion is developed in a form suitable for prediction of activation energies for diffusion in disordered substitutional solutions as well as in pure metals Bonding is considered as a localized interaction, and the energy of bonding between atoms of different types is taken as the arithmetic mean of the energies in the pure elements. The activation energies for vacancy formation and migration in substitutional alloys are shown to depend on the empirical constants developed for self-diffusion when the equations are adjusted for the mole fractions of the two elements. The differences in activation energies between alloys and pure metals are calculated and compared with the experimental differences. MaNY different correlations have been proposed for use in predicting activation energies for self-diffusion or diffusion in dilute alloys. Usually theories for self-diffusion cannot be applied to alloys nor can theories for dilute alloys be satisfactorily adapted to self-diffusion. We present here a correlation scheme which can approximate activation energies for diffusion, vacancy formation, and atom migration in substitutional-alloy systems of any concentration. The activation energy for self-diffusion QD has been correlated to the melting temperature Tm,1, 2 the sublimation energy L,,l the heat of fusion Lf,3 crystal structure, and valence.4 Working with mechanical parameters Le claire5 proposed that the activation energy for vacancy migration Qm could be related to appropriate shear moduli. He also proposed that the activation energy for vacancy formation 62, is proportional to Ls. THEORY We consider that Le Claire's expression for 4, is satisfactory. But an alternate expression for Qm in terms of the bulk modulus is just as satisfactory from a theoretical point of view for the prediction of the energy of vacancy migration in pure metals and can more easily be used for alloys. In order for Qm to be a minimum, not only the moving atom but also adjacent and nearby atoms must undergo distortions. These distortions are neither isotropic as is implied by a correlation with the bulk modulus nor unidirectional as implied by a correlation with a shear modulus, but are complex and multidirectional. A complete analysis in terms of the bulk modulus and all the shear moduli is not yet available. In a first approximation in which only one parameter is used, there is no obvious theoretical reason to prefer the shear modulus over the bulk modulus. The bulk modulus is a much more convenient parameter for use in predicting Qm. Shear moduli are known for less than half of the metallic elements while bulk moduli are usually available. Furthermore, because of the directional dependence of shear moduli, their estimation for alloys appears inherently more difficult than is the estimation of bulk moduli. We assume that the bulk modulus Bs reflects an average value of the shear moduli such that the strain energy at the point of maximum distortion of the lattice during vacancy migration can be expressed as

Jan 1, 1964

By G. H. Anderson

Cadmium-coppeR precipitate, a byproduct of the purification stage of the zinc plant, is composed mainly of zinc, cadmium and copper in varying amounts depending on the efficiency of precipitation and the cadmium and copper contents of the impure solution treated. The composition range is approximately: cadmium 10-12 pct, copper 6-8 pct, and zinc 3&35 pct. As received at the cadmium plant, the precipitate is a dark gray to black press cake produced by filter pressing the flocculent cadmium-copper precipitate formed when impure zinc solution is agitated with zinc dust. The details of the cadmium-copper precipitation are to be found in the paper "Electrolytic Zinc at Risdon, Tasmania," by W. C. Snow. Transactions AIME, 121, 501. The treatment, in addition to recovering cadmium as metal, yields a copper product as a residue for realization and recovers in solution for return to the zinc plant, the excess of zinc dust used during purification. The recovery of cadmium metal is approximately 200 tons† per year, but, with the amount of copper residue recovered, varies with the zinc production tonnage, composition of the original concentrates, degree of roasting and other operational factors. The operations involved in the recovery of the foregoing materials are carried out in a building adjacent to the purification section of the zinc plant and can best be described by dividing the process into the following stages: 1. Oxidation and Grinding of the cadmium-copper precipitate. 2. Leaching and Filtering. 3. Precipitation of cadmium. 4. Oxidation and Grinding of the precipitated cadmium. 5. Leaching oxidized cadmium precipitate and Purification of leach solution. 6. Electrolysis. 7. Melting, Casting and Packing. A feature of the process is the use of two distinct solution circuits. Spent electrolyte from the zinc plant circuit containing about 10 pct sulphuric acid is used as the primary solvent of the cadmium and zinc present in the oxidized precipitate. When the cadmium is later separated by precipitation and filtering, the filtrate, originally zinc plant spent electrolyte and now fortified in zinc, is returned to the zinc plant. The precipitated cadmium, after oxidation, is redissolved in spent electrolyte from cadmium electrolysis which solution is in closed circuit within the cadmium plant except for discards to the zinc plant circuit as mentioned in Section 5 hereinafter. (Fig 1.) Details of the various operations follow. I. Oxidation and Grinding of the Cadminm-copper Precipitate The precipitate having had a preliminary drying by compressed air in Dehne filter presses in the zinc plant is trucked to a storage platform of sufiicient length to store 3 to 4 days' production separately. After 48 hr exposure to atmosphere, oxidation is sufficient to enable all cadmium and zinc but only a portion of the copper to be dissolved in dilute sulphuric acid. The oxidized precipitate is shovelled into trucks and, after weighing and sampling, is broken in size by means of

Jan 1, 1950