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Report of Secretary TO THE BOARD OF DIRECTORS OF AMERICAN INSTITUTE OF MINING AND METALLURGICAL ENGINEERS Gentlemen -I have the honor to present the following report for the calendar year 1920 The activities which-seem to call for special com¬ment are THE NEW FORM OF MAGAZINE MINING AND METALLURGY appeared every month during the calendar year and has been developed until it contains some ten departments It has brought forth more commendatory letters than have been received at headquarters on any other subject throughout the year Less than a dozen letters unfavorable to the change have been received, and the indications are that the magazine has met a want deeply felt, especially by members distant from headquarters The technical papers printed by the Institute are published in abstract in the magazine and opportunity is given to members who desire them to receive full copies of any or all papers published The Bound Volumes, as usual, contain all the papers in full and discussions thereof FINANCES The greatly increased cost of paper and printing has put a tremendous burden on the Institute's finances, since the dues of $12 per year are only 20 per cent greater than the members paid when the Institute was founded forty-nine years ago This has resulted in a temporary deficit, similar to that encountered by many of our sister engineering societies The fact that our Institute has lower dues and gives more in the way of publications to its members than any other of\the national engineering societies has rendered the situation more difficult for us MEETINGS The Annual Meeting in New York, the Field Meeting in the Lake Superior District, the meeting of the Petroleum and Gas members at St Lours, and of the Institute of Metals Division in Columbus, Ohio, have all been described in full in the magazine

Jan 1, 1923

By B. W. Gonser

SOFT solders are used principally in the automotive, can-making, building construction and electrical industries, but their field of usefulness extends well beyond these principal users to a vast list of miscellaneous applications where metal joints are required. The most common soft solders and the only ones considered in this discussion are those com-posed of lead and tin, with or without various relatively small percentages of impurities or additions. A small amount of antimony is often pur-posely added. As an indication of the importance of these lead-tin solders, 8620 long tons were consumed in 1934 in the U.S., and during most of 1935 from 900 to 1000 long tons were used each month. A great many factors influence the properties of joints made with soft solders. Fluxes and the fluxing procedure used to prepare the surfaces to be joined in order to give a true metal-to-metal contact are among the most important of these factors. The temperatures used, cleanliness of the work and general soldering technique have their effect, but when results are unsatisfactory they are usually attributed to the metallic solder itself and the raw materials from which it is made. Some-times criticism of the solder is justified. The wrong composition may be chosen for a given job, impurities may be present that ruin certain desired qualities, or uniformity may be lacking. A solder may even be looked upon with suspicion because of its ancestry, regardless of its true composition and behavior. To clarify the effect of slight differences in composition as found in commercially refined solders, a comparison of properties of solders grouped according to their origin has been undertaken. This investigation seeks to give practical information on the proper-ties of tin-lead solders produced from virgin metals, from commercially

Jan 1, 1936

By M. H. Sommer

MANY attempts have been made to develop a relation between the tensile properties and the deep-stamping qualities of metals com-monly used in deep drawing. These operations are generally performed cold and the metal is always stressed beyond the elastic limit. However, the problem cannot be readily solved without a proper investigation of (1) the relation between actual stress and actual strain in the plastic range and (2) the stresses that are set up in the metal during the process of deep stamping. Much work has been done in recent years to add to our knowledge on plastic deformation of metals and the shortcomings of the ordinary tensile test, particularly in the plastic range, have been sufficiently recognized. It has been widely acknowledged that the local contraction, which appears in a tensile test after the maximum load is reached, is not a general characteristic of the material but is peculiar to this form of testing. The plastic deformation of materials is explained by the slip of their crystals along certain planes and this rearrangement should be similar whether observed in a tensile, compression or torsion test, and if the results of any of these forms of testing show deviations, it must be due to other influences, as for example the local contraction in a tensile test. For this reason the tensile-test curve as obtained from the measurements taken on a tensile-test machine or registered by an autographic device has been supplemented by the so-called "actual stress-strain curve," which is constructed from the observed tensile-test data by eliminating the effect of local contraction and is in complete alignment with the stress-strain values obtained in a compression or torsion test. The actual stress-strain curve shows the increase of actual unit stress in relation to unit elongation beyond the yield point and

Jan 1, 1934

By E. A. G. Colls

IN all branches of the chemical industry, corrosion plays a very costly part unless it is suitably com-batted, and as a result it is probably correct that chemical and design engineers are more corrosion conscious in the field of chemical industry than in others. Most metals occur in nature in combination with other elements. The refined or reduced state to which man converts them for his use, by removing the combining elements, leaves them in an unstable condition. Therefore in most of the media to which the metals are exposed they are constantly combining with the constituents of their environment, or in other words they are continually being corroded. Similarly, nonmetallic materials are corroded by undergoing chemical change. The rate at which corrosion takes place varies widely from metal to metal and medium to medium. In practically all cases the corrosion of metals in solutions (electrolytes) is electrolytic in nature and the rate of corrosion is dependent on many factors such as temperature, pressure, internal stresses, galvanic action, metal-ion concentration, and so on. In the chemical industry substances must be handled which are particularly corrosive to materials of construction. At the chemical plants of The Consolidated Mining and Smelting Co. of Canada, Ltd. (otherwise known as Cominco), situated at Trail, B. C., Canada, the following are some of the materials that have to be handled: Gases. Sulphur dioxide, sulphur trioxide, carbon dioxide, carbon monoxide, oxygen, hydrogen fluoride, ammonia, hydrogen sulphide, and oxides of nitrogen. Liquids. Solutions of ammonium sulphate, ammonium sulphite, ammonium nitrate, caustic soda and potash, sulphuric acid, nitric acid, hydrofluo-silicic acid, hydrofluoric acid, phosphoric acid, aqua ammonia, and formic acid. Solids. Gypsum (containing phosphoric acid), ammonium sulphate, ammonium nitrate, phosphate rock, caustic soda, potash, and phosphate fertilizers.

Jan 1, 1951

By E. A. G. Colls

IN all branches of the chemical industry, corrosion plays a very costly part unless it is suitably com-batted, and as a result it is probably correct that chemical and design engineers are more corrosion conscious in the field of chemical industry than in others. Most metals occur in nature in combination with other elements. The refined or reduced state to which man converts them for his use, by removing the combining elements, leaves them in an unstable condition. Therefore in most of the media to which the metals are exposed they are constantly combining with the constituents of their environment, or in other words they are continually being corroded. Similarly, nonmetallic materials are corroded by undergoing chemical change. The rate at which corrosion takes place varies widely from metal to metal and medium to medium. In practically all cases the corrosion of metals in solutions (electrolytes) is electrolytic in nature and the rate of corrosion is dependent on many factors such as temperature, pressure, internal stresses, galvanic action, metal-ion concentration, and so on. In the chemical industry substances must be handled which are particularly corrosive to materials of construction. At the chemical plants of The Consolidated Mining and Smelting Co. of Canada, Ltd. (otherwise known as Cominco), situated at Trail, B. C., Canada, the following are some of the materials that have to be handled: Gases. Sulphur dioxide, sulphur trioxide, carbon dioxide, carbon monoxide, oxygen, hydrogen fluoride, ammonia, hydrogen sulphide, and oxides of nitrogen. Liquids. Solutions of ammonium sulphate, ammonium sulphite, ammonium nitrate, caustic soda and potash, sulphuric acid, nitric acid, hydrofluo-silicic acid, hydrofluoric acid, phosphoric acid, aqua ammonia, and formic acid. Solids. Gypsum (containing phosphoric acid), ammonium sulphate, ammonium nitrate, phosphate rock, caustic soda, potash, and phosphate fertilizers.

Jan 1, 1951

By H. W. Highriter

THE method developed and used in this laboratory for the production of metallic uranium of such purity that it is ductile and can be cold-worked to fine wire or thin sheet by rolling has already been described1. It consists, briefly, in the electrolysis of potassium uranous fluoride (KUF5) in a molten bath composed of equal parts of sodium and calcium chlorides. The bath is contained in a graphite crucible, electrically heated to about 775° C., the crucible serving as the anode for electrolysis. The uranium deposits in finely divided form mixed with salts upon a molybdenum cathode suspended axially in the crucible. Upon com-pletion of the electrolysis the cathode is removed and cooled, the deposit broken and leached to remove salts. The metal powder is washed with water and dilute acetic acid and dried in vacuo to reduce oxidation. Suitable amounts are then pressed into pellets and heated in vacuo by high-frequency induction, using a thoria crucible. The uranium melts and flows away from the pellet, leaving a shell, which is largely oxide. In general, this method produced a satisfactory metal, although at times the uranium was not ductile. The investigations recorded here were made to find the cause of this embrittlement. It was known that the metal generally contained carbon, derived from disintegration of the graphite crucible in which electrolysis is conducted, in amounts dependent upon the thoroughness of washing the metal powder. Accordingly, analyses of several samples, both ductile and brittle, were made by combustion and absorption of C02 in Ascarite, using air instead of oxygen to reduce the temperature and rate of oxida-tion. Several of these metals were made with special precautions to reduce carbon content. The results show no relationship between ductility and carbon content in the range investigated (Table 1).

Jan 1, 1935

By E. P. Chartkoff, W. P. Sykes

In 1926 one of the authors published researches on the determination and description of the iron-tungsten and iron-molybdenum systems,' including the equilibrium diagrams. In 1929, further work was carried on, including the examination by X-rays, which is recorded here. Meas-urements were made of changes in lattice parameters in the solid solutions. Precipitation from the solid solution and the accompanying changes in hardness were studied as well as the formation of the intermetallic com-pound phases upon sintering a mixture of metal powders. Materials All the specimens were prepared from the same quality of metals and by the same methods as were described in the determination of the constitutional diagrams. The metal powders as mixed and pressed were sintered or fused in a hydrogen atmosphere and subsequently treated as indicated in the titles of the figures. The formation of the iron-rich solutlon in the solid was accomplished by sintering in hydrogen for a period of 20 to 30 hr. at a temperature 25' to 50' C. below the melting point of the eutectic. The tungsten-rich and molybdenum-rich solid solutions of iron were prepared by adding the iron as a solution of iron ammonium oxalate to the oxide of tungsten or molybdenum, followed by a hydrogen reduction. This method results in a homogeneous alloy after sintering the pressed metal powder for 20 to 30 hr. at a temperature slightly below that of the peritectic reaction in the system involved. For X-ray examination the specimens were variously prepared, depending on the nature of the sample and what it was desired to show. For example, the iron containing tungsten or molybdenum in solid solution was cut with a file, the chips were put through bolting cloth, and this powder of filings formed the specimens for comparative study. The

Jan 1, 1930

By A. U. Seybolt

Since the time this topic was originally treated in 1954, more recent French3,1 work has been published making it advisable to repeat the earlier oxygen solubility experiments, but using iron of a higher purity. Upon repeating oxygen saturation experiments with zone-refined iron, it was found that the oxygen solid solubility was at least an order of magnitude less than previously observed. SINCE the publication of an earlier paper1 (1954) on this subject by the present author, several contributions on this topic have appeared. Meijering2 in 1955 attempted to reconcile recent conflicting solubility data, without reaching any definite conclusion. sifferlen3 (1955) found that iron of high purity appeared to absorb a quantity of oxygen (0.005 to 0.025 pct) approximately proportional to the structural imperfections present, such as polygonization and grain boundary area. However, he also indicated that purity itself was a significant factor. He concluded that very pure iron nearly free of lattice imperfections would have essentially zero oxygen solubility. His second paper4 (1957) supported this contention since a zone-melted iron containing initially 0.0007 pct O analyzed only 0.0006 pct 0 after prolonged soaking at 850°C with an FeO layer on the surface. Because of the discrepancy between the results of Ref. 1 and those of Sifferlen, it seemed desirable to attempt to resolve this disagreement. EXPERIMENTAL PROCEDURE AND MATERIALS The experimental method used by sifferlen3,1 was essentially the same as that of Ref. 1. In this technique thin iron strip with a surface layer of FeO is soaked for prolonged periods at an elevated temperature in order to saturate the iron with oxygen. After two days at temperatures near 800° to 900° C, one would expect that the iron would be in equilibrium with the surface FeO. In the work reported in Ref. 1 there was evidence that two days holding at 8000to 900°C was more than sufficiently long for saturation. Sifferlen used 48 hr at 850°C. Because of the evidence presented by Sifferlen that the apparent oxygen solubility is a function of iron purity, three grades of iron were used as indicated in Table 1. The Bureau of Standards wire was used only for resistivity tests, while the other two irons were used for saturation-analysis tests of the type described above.

Jan 1, 1960

By M. E. Straumanis, R. P. Shodhan

LATTICE parameters of molybdenum of various purities are summarized in Table I. The latter shows that the parameter fluctuates between 3.1467 and 3.1475A. The room-temperature expansion coefficient a is also not well-known as values from 4.90 to 5.20 x 10-6 can be found in the literature.=-' It, therefore, seemed appropriate to repeat the measurements under exactly controlled conditions, using high-purity Hilger molybdenum powder (containing 0.0015 wt pct of Fe, 0.005 of Si and traces of other elements) and a 99.95 pct pure Sylvania Electric preparation (containing Cr, Fe, Ni, Si, Sn, and C in amounts of 50 ppm of each and in still smaller amounts Cu, Pb, Mg, and Mn). Of course, both samples could have contained at least 0.01 pct of oxygen in form of a surface oxide. However, oxygen, because of its small solubility in molybdenum, does not influence its lattice constant.g The determinations were made in a cylindrical precision X-ray camera, 64 mm in diam, the temperature of which was controlled within *0.05"C, by inserting it into a special thermostat." To exclude the film shrinkage effect (after the development of the film), the asymmetric film placement method was used." Absorption corrections (e.g., by extrapolation)" were unnecessary because of the use of a thin Li-B-glass fiber (about 0.08 mm in diam) which was fastened to the sample holder of the camera and dusted with the fine molybdenum powder. Cum radiation of the wavelength 1.389350 kX was applied because it produced in 30 min the line (420) having a high Bragg angle of about 81.6 deg. The conversion factor of 1.00202 gave the results in angstroms. To obtain the expansion coefficient a, exposures were made at various temperatures t, see Fig. 1, on at least two films at each temperature. The films were measured with a componator and the lattice constants a were calculated. The expansion coefficient was found from: where a2s is the constant at 25°C and A is the change in a and t. The same equation (knowing a) was used to reduce all the constants obtained at various temperatures to that of 25"C, Table 11. The probable error S507p (at a 50 pct confidence limit) was calculated from the reduced constants:

Jan 1, 1969

By W. H. Smith

IN the course of an investigation on chromium containing minor amounts of alloying elements, the information herein has been obtained on the crys-tallographic orientations resulting from arc melting, rolling, and annealing. The chromium used in this investigation was electrolytic flake obtained from the Electro Metallurgical Co. This material was heated for 20 hr at 1600°C in hydrogen with a dew point of about — 100°C. The oxygen and nitrogen content of the chromium after this treatment was 0.0003 pct 0 and 0.005 pct N. Five pounds of this chromium were arc melted in a water-cooled copper crucible. After arc melting, the oxygen and nitrogen contents were 0.002 and 0.025 pet, respectively. A section of this ingot is shown in Fig. 1. By means of a back-reflection Laue technique, the crystal habit of the cast ingot was determined. As expected, it was found that the [loo] was approximately the axis of the columnar grains. In this respect, chromium behaves like other body-centered-cubic metals in that a cubic axis is normal to the cold surface of the mold. A slab cut from this ingot was rolled at 600°C as follows: four 30 pct reductions were made with intermediate anneals at 1200°C for 15 min. Rolling was done with the [loo] of the columnar grains in the rolling direction. Following the final anneal, an 80 pct reduction was taken at 600 °C. The final sheet thickness was ten mils. By polishing and etching, the thickness was reduced to four mils and the grain orientation determined by the transmission Laue method using molybdenum radiation with a zirconium filter. Fig. 2 is the (110) pole figure for this material with the ideal (100) [011] and (111) [112] orientations indicated. The orientation is typical of most cold rolled body-centered-cubic metals having the [llO] of the grains approximately in the rolling direction and the (100) planes approximately in the plane of the rolled sheet. There is also evidence of some 10) [1 orientation. The grain orientation of sheet rolled 40 and 80 pct in the same direction as before at 600°C followed by recrystallization at 12000 C for 15 min was determined by a back-reflection Laue technique. A random texture was found in both cases. This 1200°C 15 min anneal was found to give complete recrystallization and some grain growth.

Jan 1, 1956

By Perry G. Harrison

The increased use of sintering for the beneficiation of iron ores and the reclaiming of flue dust creates a lively interest in sintering costs and economics. The character of material sintered and geographical location of plants so radically alter sintering costs and economics that it is well.to understand at least the basic elements which control such changes. The following cost factors are believed to be roughly approximated for large-scale Dwight-Lloyd continuously operated sinter-machine installations located anywhere. Per Crude Ton Labor, supplies and repairs 0.15 Power 6.5¢ X kw-hr. rate ? Plant overhead and administration 0.05 Depreciation per ton annual capacity 0.05 Fuel: 6 per cent coke breeze or equivalent minimum ? 1 per cent coke breeze additional for each 5 per cent free and combined water in ore or dust ? Ignition distillate at 0.6 gal. per ton ? Per Sinter Ton Royalty on ore 0.10 Royalty on flue dust 0.15 Per Crude Ton "Winter expense"; i. e., the cost of the five months enforced idle . period for plants tied in to Great Lakes transportation season 0.03 Using the foregoing data, it is possible to roughly approximate the cost of efficient sintering at any location for any ore, viz: Per Crude Ton Per Ton Handled Sinter 1. Flue Dust—Steel Plant Locations Sinter recovery, 15 per cent moisture and carbon 85 per cent Labor, supplies and repairs 0.15 0.18 Power 6.5¢ X 1¢ kw-hr. 0.065 0.08 Plant overhead and administration 0.05 0.06 Depreciation per ton 0.05 0.06 Dust handling and preparation 0.10 0.12 Fuel: free, contained in dust Ignition: blast-furnace gas free Royalty 0.15 Total $0.65 Note:—Cost increased by either deficiency or considerable excess of carbon in dust.

Jan 1, 1932

By M. Gell, G. R. Leveran

The high- and low-cycle fatigue properties of the nickel-base superalloy, Mar-MBOO, in columnar-grained and single-crystal forms were determined at room temperature. It was found that the fatigue lives of these materials were greatly affected by the size of preexisting cracks in MC-type carbides contained in the micro structure. Most of the data falls on two curves given by: (zN)'/A€= K, where Nf is the number of cycles to failure, Af is the total strain range, and K is a function of carbide size. No difference was observed in the fatigue behavior of the columnar-grained and single-crystal materials for the same MC carbide size. Matrix slip and crack initiation occurred at precracked MC carbides and, to a lesser extent, at micropores. Fatigue crack propagation was mainly in the Stage I mode, i.e., on cry stallo graPhic slip planes. The Stage I fracture in these materials was unusual in that distinct features were observed on the fracture surfaces. In high-cycle fatigue, these features resembled those commonly observed on the cleavage fracture surfaces of bcc and hcp materials. Yet, in this study, the cracks propagated slowly in a cyclic manner. In low-cycle fatigue, the Stage I facets contained equiaxed dimples, similar to those observed on the tensile fracture surfaces of ductile materials. These observations indicate that both local normal and shear stresses are involved in these Stage I fractures. A model is proposed to explain these results based on the weakening of the cohesive energy of the active slip planes by reversed shear deformation and the fracture of the bonds across the weakened planes by the local normal stress. RECENT developments in casting technology have produced cast nickel-base superalloys in columnar -grained and single-crystal forms.1'2 The tensile and creep properties of the nickel-base superalloy, Mar-M200, cast in these forms have been shown to be superior to the corresponding properties of the conventionally cast polycrystalline material.lp2 This improvement in properties results, in part, from the elimination of grain boundaries in the single crystals and the alignment of the grain boundaries parallel to the stress axis in the columnar-grained castings. As part of a program to evaluate the fatigue properties of nickel-base superalloys cast in single-crystal and columnar-grained forms, a study has been made of the cyclic deformation and fracture of Mar-M2OO at room temperature. M. fiFl I .hininr Mpmher AIMF ic ^pninr Rocoarrh Accn^iata anH I) EXPERIMENTAL PROCEDURE The composition range of Mar-Ma00 in weight percent is: 8 to 10 Cr, 9 to 11 Co, 11.5 to 13.5 W, 0.75 to 1.25 Cb, 1.75 to 2.25 Ti, 4.75 to 5.25 Al, 0.01 to 0.02 B, 0.03 to 0.08 Zr, 0.07 to 0.12 C, bal. Ni. All of the castings met the above specifications. The castings were solutionized for 1 to 4 hr at 2250°F followed by aging at 1600°F for 32 hr which resulted in a 0.2 pct offset yield stress of 150,000 psi at room temperature. The microstructure of the material consisted of cuboidal, coherent particles of ordered, fcc Ni3(A1,Ti) (commonly designated y'), approximately 0.3 p on edge, distributed in an fcc y solid-solution matrix. MC carbides together with shrinkage and gas micropores were also distributed throughout the materials. The MC carbides and micropores were located preferentially in the interdendritic interstices, as well as in the grain boundaries in the columnar-grained castings. The (100) direction of all the single crystals and the common (100) axis of the grains in the columnar materials were aligned within about 5 deg of the specimen axis. Fatigue testing was carried out in the high-cycle (HCF) and low-cycle (LCF) fatigue regions, with the major difference being gross yielding of the specimen occurred during the first cycle in the LCF region. This division also corresponded with the more usual one in which the life of a specimen in LCF is less than lo4 cycles and that in HCF is greater than lo4 cycles. The designs of the high-cycle fatigue and low-cycle fatigue specimens are shown in Figs. l(a) and (c), respectively. The gage sections of both HCF and LCF specimens were electropolished prior to testing. The HCF specimens were tested in an MTS, closed-loop, hydraulic fatigue machine at 10 cps in air. The specimens were cycled between a tensile stress of 5000 psi and a maximum tensile stress which ranged from 35,000 to 125,000 psi, Fig. l(b). The LCF specimens were cycled under strain control from zero to a maximum tensile strain, Fig. l(d), in a Wiedemann-Baldwin testing machine. The experimental procedure has been described elsewhere.3'4 Both HCF and LCF tests were interrupted periodically in order to replicate the development of slip and cracking at the specimen surface. This was accomplished by placing plastic replicating tape around the gage section of the specimen while the specimen was in the mahine. The size of the MC carbides for all specimens was measured on a polished longitudinal section through the gage section after fatigue testing. The method of measurement consisted of carefully scanning the entire polished section in order to locate the largest MC carbides. Photographs were then taken of the six longest carbides oriented approximately normal to the

Jan 1, 1969

By N. S. Stoloff, J. N. Mushovic

Age hardening response of a Mg-Th-Zr alloy has been studied at temperatures in the range 60° to 450°C. Transmission microscopy revealed clustering of thorium atoms at low aging temperatures, supporting a previous report of GP zone formation. Peak strengthening, which is observed at 325°C, is due to the formation of a coherent, ordered, DO19 type superlattice structure, of Hobable composition Mg3Th, as plates parallel to the matrix prism planes. These plates later reveal a Laves phase structure of composition Mg2Th. The equilibrium Mg4Th phase begins to precipitate in two different forms at an early stage, competitively with the Mg2Th plates. RECENT work on the Mg-Th system indicated that, unlike most magnesium-base alloys, complex precipitation phenomena may be occurring. The partial phase diagram of the Mg-Th system indicates that an equilibrium phase, Mg5Th, is the sole intermediate phase.' sturkey,' however, has reported, using X-ray and electron diffraction techniques, that a metastable fcc Laves phase, Mg2Th, precedes the formation of the equilibrium compound, which he identified as closer in composition to Mg4Th. Murakami et al.3 reported that the equilibrium phase precipitates preferentially on grain boundaries and dislocations in a Mg-1.7 wt pct Th alloy; Kent and Kelly4 aged a more dilute alloy, Mg-0.5 wt pct Th, for 4 days at 220°C and found similar results. In addition, they reported that a platelike phase with a structure close to that of the magnesium matrix forms perpendicular to the basal plane and is probably ordered. Research on a Mg-4 wt pct Th alloy by electrical resistance measurements and transmission electron microscopy has suggested that GP zones may form at low aging temperatures.3 However, the electron micrographs purporting to show this phenomenon were not conclusive. In view of the fragmentary evidence concerning the nature of the precipitation processes in the various Mg-Th alloys, an aging study was undertaken to clarify the characteristics of the various precipitates which form and to correlate the mechanical properties of the system with the direct precipitate-dislocation interactions. The latter results are presented elsewhere.' The purpose of this paper is, therefore, to discuss the precipitation sequence in this system. EXPERIMENTAL PROCEDURE Sheet stock (0.060 and 0.010 in. thick) of a commercial Mg-3.93 wt pct Th-0.42 wt pct Zr alloy (designated HK3lA) similar to that studied by sturkey2 was supplied through the courtesy of Dr. S. L. Couling of Dow Metal Products Co. Zirconium does not enter into any precipitation reactions,' but is present primarily as a grain refiner. The alloy was chill cast, warm rolled to 0.090 in. thick stock, and then finally reduced by a combination of hot and cold rolling. The alloy chemistry is given in Table I. This material was solution treated at 580°C for 4 hr in a dry CO2 atmosphere, and then water quenched. Material in this condition was fairly clear of precipitate particles and was fully recrystallized. Aging at temperatures less than 200°C was accomplished by immersing the alloy in a silicone oil bath; for higher temperatures, aging was done in a salt pot. Age hardening treatments were conducted at 60°, 80°, 105°, 135°, 160°, 250°, 325°, 350°, and 450°C for times ranging from 5 min to 400 hr. Hardness tests were performed on chemically polished 0.060-in.-thick blanks of solution treated material which were aged at the various temperatures for increasing lengths of time. For aging temperatures above 150°C the Rockwell Superficial 30T scale was employed, while samples hardened at temperatures below 150°C were monitored with the 45T scale. Each data point consists of at least three separate readings. Yield stresses also were measured at room temperature on both 0.060 and 0.010 in. sheet specimens aged at 325°C. The aged foils were thinned by the window method in a solution of 80 pct absolute alcohol and 20 pct concentrated perchloric acid (70 pct) maintained at 0°C. A stainless steel cathode was used and the applied voltage was 10 to 15 v. Thinned samples were rinsed in distilled water and pure methanol. After the me-thanol rinse the thin foils were quickly dried between filter paper. Foils prepared by the above method were examined in a Hitachi HU11B electron microscope operating at 100 kv. RESULTS A) Hardness. The hardness data are depicted in Figs. 1 and 2. Peak strengthening occurs at 325°C after aging about 6 min, see Fig. 1. Significant strengthening is achieved also at 350°C, but aging at 450°C produces only softening. The stepped curve at 250°C indicates that a complicated precipitation process may be occurring at that temperature. Fig. 2 suggests that at least two hardening mechanisms exist since the lowest temperature hardness peaks are displaced to the left of the peaks obtained at 135° and 105°C. A great deal of scatter is observed at long times in all cases due to magnesium surface degradation caused by the silicone oil bath. B) Identification of the Strengthening Precipitates. The structure formed atlowagingtemperatures (c10O°C) was not clearly resolvable by transmission microscopy. The only bright-field evidence for a change in structure was a mottled appearance which could be observed at extinction contours, as shown in Fig. 3(a), and the disappearance of this effect when dislocations produced under the influence of the electron beam passed through the matrix, as noted in

Jan 1, 1970

By Arnulf Muan, W. C. Hahn

Activities of "FeO" in "FeO"-MgO solid solutions have been determined in the temperature interval 1100" to 1300"C by equilibrating oxide samples with pure metallic iron in atmospheres of known oxygen partial pressures. The end members "FeO" and MgO form a complete solid solution series. The system shoztls a considerable positive deviation from Raoult's law. A large amount of data has been accumulated during the past 50 years on stability relations existing among various crystalline and liquid phases in oxide systems of importance in metallurgical processes. By comparison, very little is known about the thermodynamic properties within the various homogeneous phases present in the systems, particularly the crystalline phases. The present paper deals with determination of activities as a function of composition in solid solutions of wüstite ("FeO") and periclase (MgO). Such solid solutions ("Magnesiowustites") have simple sodium chloride structure and are known to be continuous between the end members at elevated temperatures (> 1000°C) and strongly reducing conditions such as prevail in contact with metallic iron. Wiistite has a defect structure in which the ratio of oxygen to iron varies and never has as low a value as 1:1 corresponding to the simplified formula FeO. Within the range of stability of this phase, the composition changes between a maximum oxygen content of approximately 25.6 wt pct (corresponding to the formula FeO.83O) and a minimum oxygen content of approximately 23.2 wt pct (corresponding to the formula Fe0-96O). The activity data to be reported in the present paper are based on using as standard state the wüstite which is in equilibrium with metallic iron at a particular temperature, i.e., "FeO" of minimum oxygen content at each temperature. For sake of simplicity, the formula FeO will be used to represent the wustite phase in the remainder of this paper. Consider the reaction 2 FeO solid solution = 2 Femeta1 + Ozgas in which FeO dissolved in another oxide dissociates to metal and gas. The activity of FeO in the solid solution, relative to "pure FeO" in equilibrium with metallic iron as a standard state, is then expressed as Here Po, and po2 * are the partial pressures of oxygen of the gas phase in equilibrium with metallic iron and the oxide solid solution or "pure FeO", respectively. The equation holds only if the metal phase is essentially pure Fe. The oxide combinations used in the present investigation fulfill this requirement. Magnesia is so much more stable than FeO that for all practical purposes aFe = 1 in the metal phase present in all mixtures used in this investigation. I. EXPERIMENTAL METHOD 1. General Procedure. The experimental method used was analogous to that developed by Foster and Welch1 and used recently by Hahn and Muan.2 It consisted of four steps: a) Determination of the equilibrium between FeO and Fe. b) Determination of d-spacing change with composition in oxide solid solutions (FeO-WO). c) Equilibration of various members of the solid solution series with a metal phase and a gas phase of known oxygen partial pressure. d) Determination of compositions of solid solutions resulting from step (c) by means of data obtained in step (b). 2. Starting Materials. General Aniline and Film Corp. carbonyl iron powder, type HP, was used as the source of metallic iron. A representative analysis was as follows: Fe, 99.6 pct; C, 0.01 to 0.04 pct; 0, 0.1 to 0.3 pct; N, 0.00 to 0.05 pct. Other elements were present as traces only. Wiistite was prepared from "Baker Analyzed" Reagent grade Fe2O3 of reported analysis as follows: Assay (Fe2O3), 98.8 pct; insoluble in HC1, 0.02 pct; not precipitated by NH,OH, 0.02 pct; Zn, 0.003 pct. Production of wüstite was achieved by a two-step

Jan 1, 1962

By Earl Greiner

THE constitution of the iron-silicon alloys containing from 14 to 33.4 weight per cent silicon has been studied by a number of investigators, whose results have been reviewed in a monograph published by the Engineering Foundation1. In these previous researches, the solubility of silicon in iron was determined by thermal, microscopic or magnetic methods and the compound Fe3Si2 was reported to be stable at tempera-tures from 0 to approximately 1030° C. This paper describes the results of an X-ray investigation of the solubility of silicon in iron and gives data which prove that the Fe3Si2 phase is unstable below 825° C. In order to obtain the present results on the solubility of silicon in iron, the authors have utilized the lattice constants of the alpha-phase iron-silicon alloys given in a previous publication2, and also some addi-tional data which will subsequently be described.

Jan 1, 1936

By W. W. Wen, S. C. Sun

The objective of this investigation was to study the electrokinetic behavior of oxidized coals to indicate the feasibility of separating oxidized coals from ash materials and pyrite by an amine flotation process. The effects of soluble inorganic electrolyte products from coal oxidation were also examined. The electro-kinetic behavior of coals of different rank and degree of oxidation were studied by an electro-phoreses technique. Generally, increasing the oxidation increases the negative value of the zeta-potential and decreases the isoelectric point (IEP). Flotation results indicate that the flotation recovery increases with decreasing pH values, and that with ferrous sulfate at pH 6.5 the flotation recovery is optimum while the pyrite is depressed. Comparing the flotation results with the electokinetic results verified that in the presence of ferrous sulfate, the maximum hydro-phobicity of oxidized coal with dodecylamine and frother is near its IEP, which is around pH 6.5 to 7.0.

Jan 1, 1978

By N. Tiner

In an article on magnesium and its alloys, Gann and Winston! stated that manganese has a limited solubility in the liquid state. W. Schmidt2 showed a diagram according to Joseph Ruhrmann indicating that the solubility of manganese in liquid magnesium falls from about 2.65 per cent at 790°C. to about 0.5 per cent at 675°C. The curve was extrapolated to show zero solubility at the melting point of pure magnesium (Fig. I). This work suggested that at the lowest manganese contents it was not possible to detect either a eutectic or the formation of a solid solution, so that manganese was stated to be present in the structure as large individual crystals. Two years after the presentation of, these results, Gann3 brought evidence to show that some manganese is capable of dissolving to form a solid solution, any excess of manganese present then assuming chiefly the form of small blue-gray particles scattered throughout the primary magnesium crystals, occasionally in clusters but seldom at the boundaries. He presented micrographs of cast alloys containing 0.1, 0.4 and 1.0 per cent manganese that show a small amount of coring around the individual particles due to solid solution, and indicate that the location of the manganese particles is closely associated with the original dendritic structure of the primary crystallization. He also pointed out that the amount of manganese that can be dissolved in magnesium depends on the amount of other alloying elements present, the effect of the second alloying element being to decrease the amount of manganese retained in the alloy. E. Schmid and G. Siebe14 have determined the solid solubility of manganese and its variation with temperature by means of precision X-ray diffraction measurements. They found that the solubility is 3.4 per cent at 645°C. and decreases to practically zero at 200°C. It is apparent that the X-ray diffraction measurements of Schmid and Siebel are not in agreement with the results of Ruhrmann as presented by Schmidt. This disagreement, and also the lack of data on magnesium-aluminum-manganese and magnesium-zinc-manganese systems, led the author to the present investigation, to determine accurately the liquid solubility of manganese and its variation with temperature. Experimental Method The experimental method for making solubility determinations consists of saturating the molten magnesium or the alloys with manganese at various temperatures and analyzing the dip samples taken from these melts. Melting is carried out in a cylindrical steel pot heated by an electric resistance furnace. The pot had a metallic outside coating to protect the steel against oxidation, and a graphite inside lining to prevent the contamination of the melt by prolonged contact with iron. The inside diameter of the pot was 4 in. and the depth 12 inches.

Jan 1, 1945

By J. E. Hanlon, S. R. Butler, R. J. Wasilewski

The temperature, orientation, and strain-rate dependence of tensile flow in single-crystal NiA1 of equiatomic composition have been investigated up to 800°C. Compression tests at room temperature have also been carried out. Optical and replica electron microscopy and X-ray diffraction methods were used to investigate the slip mechanisms. NiAl exhibits {110)(001) slip and cube slip {l00)(010) was also observed. This results in very high strength of single crystals in cube orientation. The implications of this slip mode, with the resultant small number of possible slip systems and three mutually perpendicular slip vectors, are discussed. ThE CsCl structure compounds represent a class related to the bcc elements, but their behavior is affected by three additional variables: composition (within the stability range of the compound), extent of long-range order perfection, and bonding energy. Very little data are available on the effects of these variables on mechanical properties. Rachinger and ~ottrell' suggested slip to occur along (111) in compounds of low ordering energy; in compounds of higher bond strength (>0.06 ev), they observed (110) (001) slip. As pointed out by copley,' only three in- dependent slip systems are available in the latter case; hence general deformation is impossible. Brown3 carried out a theoretical calculation of the yield-point variation with the degree of long-range order in the CsCl structure, based on the assumption of superdislocations. More general approaches, based on considerations of superlattice dislocations and antiphase domain boundaries in ordered structures, were carried out by Flinn~ and by Vidoz and Brown.' These, however, give no information on changes in the slip structure—if any—between the ordered and the disordered compounds. This aspect was investigated experimentally and theoretically by Stoloff and Davies' and by Marcinkowski and chessin7 in FeCo. The latter workers proposed the deformation behavior of the ordered FeCo to be essentially the same as that in many other bcc metals. Investigations of polycrystalline A~M~'-'O indicate considerable variation in mechanical properties with composition and test temperature. The existence of {123)(111) slip was reported in AgMg.'9'9'0 (The formation energy of this compound, presumed to be ordered at all temperatures below melting, is 4.38 cal per g-atom," i.e., 0.024 ev per bond.) The yield strength has been reported as relatively independent of temperature below 0.45 T, (where T, is the absolute melting temperature). Tensile deformation of single-crystal AgMg was also investigated by Kurf-man," who observed marked tendency to single glide on{112}(111) and {110)(111). From observations of slip lines in deformed poly-crystalline NiA1, Westbrook et a1.I3 suggested the

Jan 1, 1968

By J. J. Casey, R. S. Busk, D. L. Leman

The mechanical properties and the phase-temperature relationships of magnesium-lithium-aluminum, magnesium-lithium-zinc, and magnesium-lithium-aluminum-zinc alloys are presented. It is shown that the strengths of some of these alloys can be tripled by heat treating and aging but that the high strength is accompanied by brittleness and lack of stability. MAGNESIUM-LITHIUM alloys are interesting because the hexagonal structure of magnesium can be changed into the more ductile and workable body-centered cubic structure by the addition of only 10 pct lithium.1 After Loonam2 determined that the ductility of the magnesium-lithium alloys is destroyed by even trace quantities of sodium, it was possible to prepare ductile alioys and study their mechanical properties. Jackson3 and coworkers have ably described their results with both the binary and polynary magnesium-lithium alloys. The present paper is a report of the mechanical properties of wrought magnesium-lithium-aluminurn, magnesium-lithium-zinc, and magnesium-lithium-aluminum-zinc alloys. Experimental Procedure The alloys were made by melting 7 lb of magnesium in a steel crucible under a molten flux of 75 pct LiCl + 25 pct LiF3 previously dried at 1600°F. The metal was heated to 1300°F for alloying aluminum and zinc and then cooled to 1250°F for adding lithium (sodium content: 0.01 to 0.04 pct). After the lithium had been alloyed, dry LiF powder was sprinkled on the melt to thicken the excess flux. After a 15 min holding period, the flux was skimmed off. Paraffin vapors were used to protect the metal as it was poured into 3 in. diam by 11 in. long magnesium molds. Billets were extruded into 3/8-in. diam rod and 1/16 x 3/4-in. strip; sheet was prepared from 1/8x 7/8-in. extruded strip, first by hot rolling and then by cold rolling 2 pct per pass. Hot rollability, or the temperature range through which the alloys could be rolled, was determined by rolling the strip two passes at 30 pct reduction per pass. Cold rollability, or the percentage of cold reduction to cause detrimental cracking, was determined on 0.064-in. hot-rolled sheet. Standard ASTM procedures were followed to obtain the mechanical properties, using 0.2 pct offset for the yield strengths. The level of properties produced with commercial magnesium alloys using the procedure described is given in a previous publication." Results Magnesium - Lithium - Aluminum System: The good workability of magnesium-lithium alloys is illustrated by the data in table I, which shows approximately how the extrusion pressure decreases as the amount of cubic phase increases. Binary magnesium-lithium alloys are soft and weak, but aluminum raises their strengths con-

Jan 1, 1951

By Walter Showak

The published phase diagrams for the copper-zirconium system1,2 indicate that the solid solubility of zirconium in copper is not accurately known. Studies made on relatively impure alloys by Pogodin, Shumova, and Kugucheva3 yielded a maximum solubility value of 1 wt pct Zr at the eutectic temperature. Allibone and sykes5 reported that an as-cast 0.2 wt pct Zr alloy is single phase at room temperature. Limited results obtained by Raub and Enge14 indicated that zirconium solubility in copper is less than 0.13 wt pct Zr at 940°C. Tn 1960, on the basis of a microstructural examination of several copper-rich Cu-Zr alloys, saarivirta6 placed the maximum solubility of zirconium in copper at 0.15 wt pct at the eutectic temperature, 980°C. The present note describes results obtained during a re-investigation of the Cu-Zr system for the purpose of accurately establishing the solidus and solvus curves and the eutectic temperature in copper-rich alloys. High-purity copper (99.99 pet) and zirconium (99.64 pet) consolidated reactor grade sponge were used to prepare several alloys, containing up to 2 wt pct Zr, by induction melting in graphite crucibles in vacuum and chill casting into a split steel mold. The melting procedure consisted of first melting the copper charge and then adding the bulk zirconium wrapped in pure copper foil. Chemical analyses were made of both the cold-rolled alloy ingots after homogenization at 925°C for 450 hr in evacuated quartz capsules and of small specimens which had been used in the phase diagram studies. 'The carbon content of each alloy was also determined and was found to be less than 0.001 wt pct in every case. Metallographic and electrical resistivity measurements were used as the primary methods for this investigation, although some thermal analysis studies were also performed. Heat treatments of all the alloys were carried out with the specimens wrapped in molybdenum or alloy foil (of the same composition as the specimen) and sealed in quartz tubes either in vacuum or under a purified helium atmosphere. Following high-temperature anneals for long periods of time, slight depletion of zirconium from the specimen surface was observed. Therefore, careful preparation of samples for microscopic examination and chemical analysis of the samples themselves was necessary to check the composition of samples used in determining phase boundaries. Points on the solvus curve were determined on quenched specimens by both isothermal reaction after solution heat treatment at 950°C for 8 hr and by isothermal annealing of alloy specimens at successively higher temperatures for times ranging from 24 to 500 hr. Liquation studies for positioning of the solidus and eutectic temperatures were performed by holding a pre-

Jan 1, 1962