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By Harwick Johnson, E. W. Schilling

THE separation of hematite by hysteretic repulsion was first brought to the attention of the public in 1922, by W. M. Mordey1. Three years later another paper2 was published and after another four years a third paper3 appeared in the South African publications. Certain data were lacking in these papers. In order to continue the work intelligently a knowledge of the shapes of the hysteresis curves for certain minerals was very necessary. This information was not available until the present year4. It was known that reduction of certain ores rendered them amenable to this process of separation but definite data in the form of curves showing exactly the effect of such treatment were lacking. Probably our best source of information on the separation of minerals by the use of alternating-current magnetic fields today is the reports from the U. S. Bureau of Mines5-7. It is not the purpose of this paper to tell the reader in detail how to make a commercial separator. Experimental models have recently been made7 and the results obtained have been so good that it is the opinion of the authors that the public will soon take an active interest in the subject and its development. The writers have constructed a separator that is considerably different in construction and operation from the two types described by Mr. Davis. This will be described, but the real purpose of this paper is to outline certain experiments and give curves showing data that have a fundamental bearing upon the practical construction of a separator of this type.

Jan 1, 1935

By E. W. Schilling

THE-separation of hematite by hysteretic repulsion was first brought to the attention of the public in 1922, by W. M. Mordey1. Three-years later another paper2 was published and after another four years a third paper3 appeared in the South African publications. Certain data were lacking in these papers. In order to continue the work intelligently a knowledge of the shapes of the hysteresis curves for certain minerals was very necessary. This information was not available until the present year4. It was known that reduction of certain ores rendered them amenable to this process of separation but definite data in. the form of curves showing exactly the effect of such treatment were lacking. Prob-ably our best source of information on the separation of minerals by the use of alternating-current magnetic fields today is the reports from the U. S. Bureau of Mines 5-7. It is not the purpose of this paper to tell the reader in detail how to make a commercial separator. Experimental models have recently been made7 and the results obtained have been so good that it is the opinion of the authors that the public will soon take an active interest in the subject and its development. The writers have constructed a separator that is considerably different in construction and operation from the two types described by Mr. Davis. This will be described; but the real purpose of this paper is to outline certain experiments and give curves showing data that have a fundamental bearing upon the practical construction of a separator of this type.

Jan 1, 1936

By M. Vallée

This case study compares the actual production figures for the No. I and No. 2 copper orebodies of the Société Miniére Louvem, Val d'Or, Quebec, with the preproduction estimates and a postmortem geostatistical estimation using kriging techniques. The deposits considered are small subvertical sulphide orebodies which were mined from August 1970 to April 1973, producing 648,000 tons at 2.04% Cu versus the 1968 computed reserves of 671,000 tons at 2.51% Cu (with 20% dilution), thus showing a 25% overestimation of the copper contained. The postmortem geostatistical estimation based on the same 44 D.D.H. intersections available in 1968, shows 2.24% Cu (no dilution), compared to 3.23% Cu (no dilution) given by the conventional section method. Block by block kriging techniques were used, but within the ore contours as determined by the geologist. In this case, Characterized like many sulphide deposits by highly dispersed sample values, geostatistical kriging techniques permit a more realistic estimation of the metal contained within a given volume, than the conventional methods which overestimate it. This study has been conducted by the Mineral Exploration Research institute (IREM-MERI) for SOQUEM, and is one of the few case studies released with all pertinent data. More postmortem of this kind are required for geologists and geostatisticians to improve their methods and their "batting average".

Jan 1, 1977

By E. W. Schilling

THE separation of hematite by hysteretic repulsion was first brought to the attention of the public in 1922, by W. M. Mordey1. Three years later another paper2 was published and after another four years a third paper3 appeared in the South African publications. Certain data were lacking in these papers. In order to continue the work intelligently a knowledge of the shapes of the hysteresis curves for certain minerals was very necessary. This information was not available until the present year4. It was known that reduction of certain ores rendered them amenable to this process of separation but definite data in the form of curves showing exactly the effect of such treatment were lacking. Prob-ably our best source of information on the separation of minerals by the use of alternating-current magnetic fields today is the reports from the U. S. Bureau of Mines 5-7. It is not the purpose of this paper to tell the reader in detail how to make a commercial separator. Experimental models have recently been made 7 and the results obtained have been so good that it is the opinion of the authors that the public will soon take an active interest in the subject and its development. The writers have constructed a separator that is considerably different in construction and operation from the two types described by Mr. Davis. This will be described, but the real purpose of this paper is to outline certain experiments and give curves showing data that have a fundamental bearing upon the practical construction of a separator of this type.

Jan 1, 1935

By Guillermo Hileman

In March the President approved the new oil bill, .which became effective as Law No. 12161, providing among other things a contribution or tax on all producers varying from 8 to 12 per cent payable monthly. The new regulations, for chapter VI bearing on the tax feature, of this

Jan 1, 1936

By Guillermo Hileman

In March the President approved the new oil bill, .which became effective as Law No. 12161, providing among other things a contribution or tax on all producers varying from 8 to 12 per cent payable monthly. The new regulations, for chapter VI bearing on the tax feature, of this

Jan 1, 1936

Mining Methods LUCIEN EATON, Chairman GERALD F. SHERMAN, Vice-chairman CHARLES W. WRIGHT, Secretary Alluvial Mining CLINTON BERNARD CHARLES H. MUNRO CHARLES JANE N H. R. NORSWORTHY Open-cut Mining Iron MAX H. BARBER J. A. MacKILLICAN Copper MICHAEL CURLEY H. B. TEMPEST Underground Mining Iron C. H. BAXTER CARL BREWER TENNEY C. DESOLLAR Copper W. B. DALY A. H. WOHLRAB R. W. THOMAS

Jan 1, 1934

By A. R. Orban, R. B. Engdahl, J. D. Hummell

The initial phase of a research program on smoke abatement from Bessemer converters is described. In work sponsored by the American Iron and Steel Institute, a 300-lb experimental Bessemer converter was assembled to simulate blowing conditions in a commercial vessel. Measurements of smoke and dust were also made in the field on a 30-ton commercial vessel. During normal blows the dust loading from the laboratory converter averaged 0.51 lb per 1000 lb of exhaust gas. This was similar to the exhaust-gas loading of a commercial vessel. The addition of hydrogen to the blast gas of the laboratory converter caused a decided decrease in smoke density. Smoke was also reduced markedly when methane or ammonia was added instead of hydrogen. The research is continuing on a bench-scale investigation of the mechanism of smoke formation in the converter process. DURING the past 2 years, on behalf of the American Iron and Steel Institute, Battelle has been conducting a research program on the control of emissions from pneumatic steelmaking processes. The objective of the research program is to discover a practical method for reducing to an unobjectionable level the emission of smoke and dust from Bessemer converters. PRELIMINARY INVESTIGATION Although conceivably some new collecting technique may be devised which would be economically practicable for cleaning Bessemer gases, no such system based on presently known principles seems feasible because of the extremely large volume of high-temperature gases involved. Hence, the research is being directed toward prevention of smoke formation at the source. A thorough review was first made of former work to determine the present status of the cleaning of converter gases. No published work was found on work done in the United States on collecting smoke or on preventing its formation in the bottom-blown, acid-Bessemer converter. In Europe, however, a number of investigations have been made on the basic-Bessemer converter. Kosmider, Neuhaus, and Kratzenstein1 conducted tests on a 20-ton converter to obtain characteristic data for dust removal and the utilization of waste heat. They concluded that because of the submicron size of the dust, special equipment would be necessary to clean the exhaust gases. Dehne2 conducted a large number of smoke-abatement experiments at Duisburg-Huckingen in a 36-ton Thomas converter discharging into a stack. A number of wet-scrubbing and dry collectors were tried unsuccessfully. A waste-heat boiler and electrostatic collector with necessary gas precleaners was felt to be the best solution for this particular plant. Meldau and Laufhutte3 determined that the particle size was all below 1 µ in the waste gas of a bottom-blown converter. Sel'kin and zadalya4 describe the use of oxygen-water mixtures injected into a molten bath in refining open-hearth steel. They claim that with use of oxygen-water mixtures the amount of dust formed was reduced between 33.3 and 20 pct of its previous level, and emission of brown smoke almost ceased. Pepperhoff and passov5 attempted unsuccessfully to find some correlation between the optical absorption of the smoke, the flame emission, and the composition of the metal in a Thomas converter in order to determine automatically the metallurgical state in the melt. In a recent U. S. Patent (NO. 2,831,762)' issued to two Austrian inventors, Kemmetmuller and Rinesch, the inventors claim a process for treating the exhaust gases from a converter. By their method the inventors claim that the exhaust gases from the converter are cooled immediately after leaving the converter to a degree that oxidation of the metal vapors and metal particles to form Fe2O3 is inhibited in the presence of surplus oxygen. Gledhill, Carnall, and sargent7 report on cleaning the gases from oxygen lancing of pig iron in the ladle. They claim the Pease-Anthony Venturi scrubber removed 99.5 + pct of the smoke, thereby reducing the concentration to 0.1 to 0.2 grain per cu ft, which resulted in a colorless stack gas after the evaporation of water. Fischer and wahlster8 developed a small basic converter and compared the metallurgical behavior of the blow with that of a large converter. Later work by Kosmider, Neuhaus, and Hardt9 on the use of steam for reduction of smoke from an oxygen-enriched converter confirmed that the cooling effect of steam is detrimental to production. From review of all of the published information on the subject, it was concluded that a practical solution to the smoke-elimination problem had not been found. Accordingly, it was deemed desirable to investigate the feasibility of preventing the initial formation of smoke in the converter.

Jan 1, 1961

By Michael Tenenbaum

THE importance of semikilled steel as a high tonnage grade has long been recognized. The increasing severity of the applications for which semikilled steel is used makes it desirable to obtain further information regarding the features of open hearth practice and ingot structure that can affect steel performance in subsequent rolling and fabricating operations. Accordingly, an investigation is being carried out studying the structure of various types of semikilled steel ingots. This paper reviews some of the observations made and information gathered in this investigation. By definition, semikilled steel may be considered to include all nonrimming steels in which the natural shrinkage occurring during ingot solidification is offset to an appreciable degree by gas formation. Accordingly, this type of steel includes the entire range intermediate between rimmed and fully killed steel. The resultant ingot structures range from those of steels that have been capped to suppress a weak rimming action to those steels that have been killed in the furnace or ladle to the extent that no mold deoxidizer is required. A survey reported to the 1946 AIME Open Hearth Conference' reviewed the practices being used at 28 major plants for the deoxidation of semikilled steel. It was found that most plants divide the deoxidizing additions between the ladle and the mold many of the plants adding only minor amounts of deoxidizer to the bath or none at all. Silicon, aluminum and titanium were the only elements used for ladle and mold deoxidation. Mold deoxidizers were added as capping additions or as uniformly fed additions. Several practices were reported in which the steel was deoxidized in the ladle to the extent that little or no mold deoxidation was needed. No reference was made to grades capped by using special mold designs or special closures over the top of molds. Accordingly, specific examples of this type of practice will not be considered in this paper. It appeared from this survey of deoxidation practice that semikilled steel can be divided into three types, namely, capped semikilled, in which aluminum is added near the end of pour or after shut-off, intermediate semikilled steels, in which aluminum is fed uniformly throughout the pour, and semikilled steels requiring no mold deoxidation. In an attempt to cover the ingot structures obtained by the range of practices reported in the preceding survey, three series of experimental heats were made using increasing amounts of aluminum, silicon and titanium for ladle deoxidizers. The ladle deoxidizers were added as stick aluminum, 50 pct ferrosilicon and 20 pct ferrotitanium (4 pct carbon), respectively. Two methods of studying ingot structures were used. Ingots were removed from production, burned longitudinally and machined to allow observation of the central pipe and coarse blowholes. During the machining operation much of the finely porous subsurface structure was obliterated. Accordingly, observations were also made

Jan 1, 1947

By P. Barnes

It may he of interest, and perhaps of inzportance, to the members of the Institute that specific mention should be made in detail of the great value of this method of copying or photographing all kinds of tracings." Several samples are laid upon the table which may serve as illustrations of the results obtained. Some of these show slight imperfections, depending upon the character of the tracing, and upon the length of the exposure to the light, but it may be clearly seen that even a faint copy would be quite available for actual use. The process is believed to be of French origin, and has been used for many years. Special attention seems to have been directed to it recently, and its great value to engineers appears likely to be fully recognized. The manipulations required are of the simplest possible kind, and are entirely within the skill and comprehension of any office boy who can be trusted to copy a letter in an ordinary press. These particulars may be summarized somewhat thus: 1. Provide a flat board as large as the tracing which is to be copied. 2. Lay on this hoard two or three thicknesses of common blanket, or its equivalent, to give a slightly yielding backing for the paper. 3. Lay on the blanket the prepared paper with the sensitive side uppermost. 4. Lay on this paper the tracing, smoothing it out as perfectly as possible so as to insure a perfect contact with the paper. 5. Lay on the tracing a plate of clear glass, which should be heavy enough to press the tracing close down upon the paper. Ordinary plate-glass of 3/8" thickness is quite sufficient. 6. Expose the whole to a clear sunlight, by pushing it out on a shelf from an ordinary window, or in any other convenient way, for six to ten minutes. If a clear skylight only can be had, the exposure must be continued for thirty or forty-five minutes, and under a cloudy sky, sixty to ninety minutes may be needed.

Jan 1, 1879

By G. W. P. Rengstorff, R. B. Fischer

A study was made of the effect of impurities on the bend ductility of cast molybdenum. High purity molybdenum was repared by re-melting under high vacuum. The ductility of "transverse-grain" specimens indicated that intergranular brittleness decreased with an increase in purity of the metal. THE production of as-cast molybdenum with high ductility at room temperature would make working of the metal easier and increase the usefulness of the as-cast metal. Furthermore, a .knowledge of the factors that influence the ductility of as-cast molybdenum might be applied to the problem of making fusion weldments having satisfactory room-temperature ductility. Individual grains of commercial as-cast molybdenum are slightly ductile at room temperature. However, the presence of carbides at the grain boundaries may cause the metal to fracture in a brittle manner. This behavior has been discussed.' The amount and distribution of the impurities in as-cast molybdenum would be expected, from previous research on the metal, to have considerable influence on its ductility. Some effects of oxygen and carbon on the mechanical behavior of the metal were discussed by Parke and Ham,2 Woodside,3 and Zappfe. Landgraf, and Worden.4 Parke and Ham2 found that, if a sufficient number of molybdenum oxide particles were present at the grain boundaries, the intergranular cohesion was reduced to the extent that arc-melted molybdenum would rupture intergranularly during hot forging. They also found that if the oxygen content was less than 0.003 pct, the cast molybdenum was hot forgeable. It is suspected, however, that forgeable molybdenum may contain a small amount of oxide that could reduce the ductility of the as-cast metal at room temperature. Also, there is the possibility of the unfavorable distribution of other impurities having a detrimental effect on the ductility of cast molybdenum. The results of a study of the influence of purity on the room-temperature ductility of cast molybdenum are presented here. Vacuum Arc-Melting to Produce High Purity Mo One way of determining the effect of impurities on the ductility of molybdenum is to prepare and test metal as free of all impurities as possible. Accordingly, the present investigation was undertaken with this in view. Arc melting in high vacuum (less than 0.1 micron of mercury) was chosen as the method for reducing the impurities below the concentrations occurring in commercial molybdenum. Commercial arc melting of molybdenum is carried out at about 50 microns pressure. During the arc melting, carbon and oxygen in the metal react to form carbon monoxide. By virtue of the vacuum process, the partial pressure of carbon monoxide is maintained at such a low value that the reaction greatly lowers oxygen and carbon contents. An excess of at least 0.03 pct C is used in commercial arc melting to insure that the oxygen content will be below 0.003 pct. The excess carbon remaining after the deoxidation step forms carbides on freezing. Some of the carbides precipitate at the grain boundaries and, as will be shown, have an unfavorable effect on the room-temperature ductility. In the present work, only the small amount of carbon (0.003 pct) contained in the commercial powder-metallurgy molybdenum used for melting stock was present. Partial removal of oxygen from the melt probably occurred as the result of the volatilization of molybdenum oxides, or by distillation of oxygen at the high melting tem-

Jan 1, 1953

MONTANA SECTION J. L. BRUCE, Chairman W. C. SIDERFIN, Vice-Chairman WALTER E. GABY, Secretary-Treasurer, 834 W. Granite St., Butte, Mont. N. B. BRALY W. T. BURNS A special meeting of the Directors of the Montana Section was held on July 24, 1916, with W. C. Siderfin, Vice-Chairman, presiding. The meeting was called for the purpose of electing a Secretary-Treasurer to fill the, vacancy created by the resignation of M. H. Gidel. Upon proper motions, the resignation of M. H. Gidel was, accepted, and Walter E. Gaby was elected to fill the office for the balance of the fiscal year. No further business was transacted, and upon motion the meeting adjourned WALTER E. GABY, Secretary.

Jan 9, 1916

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

Jan 1, 1925

By R. E. Zimmerman

The separation of fine sizes of coal from its impurities by means of various flotation methods has become of increasing importance in the coal industry. This, no doubt, will be even more so in the future as the quantity of high grade coal is depleted, particularly that used for metallurgical purposes. The purpose of this paper is to describe and report the results of research work done under the auspices of the Pittsburgh Coal Co. to determine the amenability of their bituminous fine sizes of coal to flotation, to investigate the value of various reagents and factors affecting their use, and compare the results between froth flotation and bulk oil flotation. Compared with the preferential flotation of complex minerals, or ores, the flotation of coal is comparatively easy. However, this statement should not lull one into the feeling that there are no special problems involved. For instance, the separation of coal from pyrite in high sulphur coals is still far from being 100 pet successful. Size consist has considerable effect on reagent consumption and recovery. Other factors will be described and finally it must be remembered that in the flotation of coal a low priced material is being treated and thus economic considerations govern more closely its application than is generally the case in treating other minerals. As a result of the research work done by the Pittsburgh Coal Co. on the flotation of coal, it was concluded that it was practical to clean the —48-mesh coal commercially by froth flotation and after several different types of flotation units and circuits were investigated by means of pilot plants, large scale units were installed at their Champion Nos. 1, 4 and 5 Preparation Plants for the cleaning of —48-mesh slurries. These large scale operations have been recently described by D. H. Davis.' C. P. Proctor and C. B. Carlson2 in their chapter on Froth Flotation of Coal in the AIME Seeley W. Mudd series book on Coal Preparation describe some of the practical applications of our Pittsburgh Coal Co. laboratory work in actual plant practice as well as summarizing part of the investiga-tional work. The author presents this paper, however, as a supplement to their reports, and records the basic research accomplished in the laboratory investiga-tional work as well as the results of experiments using bulk oil flotation. In presenting this work the author wishes to state much more work must be done in applying the principles of flotation to cleaning coal, especially in view of recent studies and practices in other mineral beneficiation fields. Methods of Conducting Laboratory Tests The bulk of the research work was conducted in the laboratory of the Champion No. I Preparation Plant. This plant has elaborate facilities for sampling and analyzing coal and proved to be an admirable location for the investigational work. Four types of laboratory flotation ma-

Jan 1, 1949

By J. A. Goebel, S. Rosen

IN the NiAl phase diagram the NiAl (CsC1-type) phase field extends over a large composition range. At elevated temperatures the nickel-rich phase boundary extends to a composition of about 70 at. pct Ni, a value which is within 5 at. pct of the Ni3A1 (Cu 3 Au-type) phase boundary.' At room temperature, however, the maximum nickel content is only about 60 at. pct. Experiments have shown that alloys containing greater than 63 at. pct Ni when quenched from temperatures below 1000°C contain the equilibrium phases NiAl and Ni3A1. On the other hand, when these same alloys are quenched from temperatures above 1000°C and examined microscopically, a typically martensitic decomposition product appears in the microstructure as shown in the micrograph of Fig. 1. The structure of the martensitic phase has been determined by employing powder X-ray diffraction techniques to be an "ordered" AuCu type (Strukturbericht Llo, space group P/4 mmm - DL). The diffraction pattern of this phase differs from that of AuCu in the appearance of superlattice lines. The structure is shown in Fig. 2. The open circles represent nickel atoms and the half-shaded circles represent nickel and aluminum atoms which are randomly distributed. The sites represented by half-shaded circles would be occupied solely by nickel atoms at a stoichiometry of Ni3A1. The alloys used in this investigation were prepared from 99.99 wt pct Al and 99.99 wt pct Ni by arc melting charges of varying compositions in a water-cooled copper hearth using a tungsten electrode in a gettered argon atmosphere. In all cases chemical analysis agreed within $ at. pct with the nominal compositions of the alloys. Annealing treatments were carried out in a vertical resistance furnace through which a stream of argon gas was flowing. Specimens, which were wrapped in tantalum foil, were quenched by allowing the specimens to drop into a bucket containing iced brine. X-ray diffraction patterns were obtained from -325 mesh powder specimens by using a 114.8-mm

Jan 1, 1969

By J. A. Bailey, J. H. Tundermann

The dihedral angles of the solid-liquid interfaces were measured at various temperatures above the solidus and the interfacial energies calculated when small additions of copper, indium, lithium, magnesium, antimony, and silicon were made to an aluminum alloy containing 3 pct Sn. When the results were compared with those of the Al-Sn alloy some differences were found which could be interpreted in terms of the ability of the added element to enter into solution or form intermetallic compounds with the aluminum and tin. It was shown that in some cases considerable changes in the shape of intergvanular liquid films can be brought about by comparatively small compositional changes in the alloy. DURING the melting or solidification of an alloy a temperature range is usually found where the presence of a liquid phase may be detected at the grain boundaries of a solid. It is believed that the presence of this liquid phase is responsible for hot tearing in castings and welds and hot shortness in the working of some alloys at elevated temperatures. Rosenberg, Flemings, and Taylor1 in a study of the solidification of aluminum castings have indicated the importance of intergranular liquid films and shown that their shape and distribution at the end of solidification effect the hot tearing characteristics of the material. The shape of such intergranular liquid films are determined largely by the ratio between the solid-liquid interfacial energy (yLS) and the grain boundary energy (ySS). A measure of this ratio (yLS/ySS , relative interfacial energy) is the dihedral angle 8. The dihedral angle 0 is related to the relative interfacial energy by the following expression: Rogerson and Borland 2 have also suggested that the shape of the intergranular liquid is an important factor in determining the susceptibility of a material to hot shortness. They showed that on a comparative basis materials having the lowest dihedral angles at a given temperature gave the greatest severity of cracking. They stated that liquid in the form of globules should be less harmful than liquid in the form of extensive films as more intergranular cohesion should be possible. Rogerson and Borlland 2 also showed that the susceptibility of an A1-Sn alloy to hot cracking can be reduced by small additions of cad- mium. It was found that the cadmium gave an increase in the dihedral angle at all temperatures. Ikeuye and smith3 investigated changes in the dihedral angle and relative interfacial energy with temperature for a number of ternary alloys formed when small additions of bismuth, cadmium, copper, lead, and zinc were made to an A1-Sn alloy. They found that in most instances changes in the dihedral angle were caused by compositional changes in the liquid phase; as the composition of the liquid approached that of the solid the dihedral angle decreased. They noted that the addition of a third element which was soluble in both the liquid and solid phases at a given temperature may decrease the dihedral angle (e.g., the addition of copper or zinc) but otherwise the ternary alloys formed exhibited dihedral angles between those of the A1-Sn binary alloy and those of the binary alloy of aluminum with the added element. Dwarakadasa and Krishnan4 investigated the changes in dihedral angle and relative interfacial energy with temperature when small additions of magnesium, iron, silicon, manganese, sulfur, cobalt, and silver were made to a copper alloy containing 3 pct Bi. They found that in all cases the added elements gave an increase in the dihedral angle and relative interfacial energy when compared with the values obtained for the simple binary alloy at the same temperature. It was noted that an increase in temperature gave a decrease in dihedral angle and relative interfacial energy in each of the ternary alloys studied. Similar results have been obtained by Ramachandran and Krishnan5 for the addition of small quantities of lead. This paper describes the application of dihedral angle measurement to the determination of the shapes of liquid phases at various temperatures above the solidus when small additions of copper, indium, magnesium, lithium, antimony, and silicon are made to an aluminum alloy containing nominally 3 pct Sn. An attempt is made to correlate the measurements with the relative solubility of the added elements in tin and aluminum. The work was undertaken to provide more data concerning the effects of temperature and composition on the shape of liquid films above the solidus. EXPERIMENTAL PROCEDURE In the present work ternary aluminum alloys containing nominally 3 pct Sn and small additions of high-purity copper, indium, lithium, magnesium, antimony, and silicon were made. The alloys were melted in a graphite crucible under an inert atmosphere of argon and cast into ingots 6 in. long by 0.5 in. diam. The ingots were then cut into rods 1.5 in. long, given a 50 pct cold reduction, and machined into test pieces 0.5 in. long by 0.5 in, diam for heat treatment. The alloy samples were annealed at the various test temperatures between the liquidus and solidus for approxi-

Jan 1, 1967

By E. Miller, J. M. Eldridge, K. L. Komarek

Aclivilies of magnesium in liquid Alg-Si alloys have been delermined between 5 and 60 at. pcl Si, close to the melling point of Mg2Si, by an improved isopieslic melhod. Silicon specinrens, held in alumina crucibles and graplrile conlainevs of special design, were healed in a letrlpevalure gvadient and equilibrated with mag-nesilcrrl rapor in a closed lilanium system. The ther-madynamic Junctions were calculated and compared with the thermodyuamic properties of the other three mg- Gvoup IVB systems. Lattice paramelers of three Mg2X compounds were measured. The bonding in the Mg2X compounds is largely covalent with small and uarying amounts of metallic and ionic conlvibutions. The Mg-Si phase diagram1 has one congruent melting compound, Mg2Si, of essentially stoichiometric composition, two eutectics, and very limited terminal solid solubilities. Little information is available on the thermodynamic properties of this system. The free energy of formation of Mg2Si has been determined by the Knudsen cell technique2 in the range 572" to 680oC, by the transportation method3 between 858" and 950oC, and by the electromotive-force method4 in the range 400o to 600°C. Kubaschewski and villa5 and caulfield6 have measured the heat of formation of Mg2Si. An electromotive-force study of magnesium-rich liquid alloys was recently published by Sryvalin el al.7 The present investigation was undertaken to complete a general survey of the thermodynamic properties of the homologous series of Mg-Group IVB systems, i.e., Mg-Pb,a9,Mg-Sn,10,11 mg-Ge,12and Mg-Si. An isopiestic technique, previously developed for similar measurements on liquid Mg-sn11 and Mg-Ge alloys,12 was modified for the Mg-Si system. Specimens of the nonvolatile component, silicon, were contained in dense alumina crucibles placed inside covered graphite crucibles which were heated in a temperature gradient in an evacuated and sealed titanium reaction tube and equilibrated with magnesium vapor of known vapor pressure. The alumina crucibles prevented contact between the highly corrosive liquid Mg-Si alloys and graphite. The graphite cruci- bles effectively preserved the high-temperature equilibrium composition of the liquid alloys containing highly volatile magnesium on termination of the experiments during the quench to room temperature. EXPERIMENTAL PROCEDURE Silicon of semiconductor-grade purity (E. I. du Pont de Nemours and Co., Brevard, N.C.) and 99.99+ pct Mg (Dominion Magnesium Ltd., Toronto, Canada) were used. Graphite crucibles with press-fitted lids were machined from high-density (1.92 g per cu cm) rods (Basic Carbon Corp., Sanborn, N.Y.) which had a maximum ash content of less than 0.04 pct. The alumina crucibles had a purity of 99.7+ pct (Triangle RR grade, Morganite, Inc., Long Island City, N.Y.). In preliminary runs the liquid alloys were contained in graphite crucibles following the exact procedure developed for the Mg-Ge system.'2 These runs failed due to appreciable reaction between the molten Mg-Si alloys and graphite, and the results have been discarded. The procedure was then modified and the Mg-Si alloys were subsequently held in alumina crucibles. For most of the runs alumina crucibles of known weight and approximately 6.3 mm ID, 12.5 mm height, 1.0 mm wall thickness were loaded with weighed amounts of silicon and encapsuled in tightly covered weighed graphite crucibles 5/16 in. ID, 2 in. helght, 3/32 in. wall thickness). The graphite crucibles were machined from rods which were 85 pct of the theoretical density. These crucibles were therefore sufficiently porous so as to permit magnesium vapor to effuse through the silicon under the experimental conditions of approximately 970O to 1220°C and 1 day equilibration time. However, negligible magnesium was lost from the crucible during the quench due to the slow effusion rate through the pores of the graphite. The inner alumina crucible prevented the liquid alloys from contacting the graphite, and the very tightly fitting graphite crucible lids served to retain any magnesium vaporizing from the alloys inside the crucibles during the quenching step.12 The loaded silicon-alumina-graphite cells were positioned, one above another, on a 16-in.-long titanium thermocouple well and tied securely to the titanium tube with thin molybdenum wires held in grooves around the circumference of the graphite crucibles. A thin (0.005-in.) molybdenum strip prevented contact between the graphite crucibles and the titanium. This assembly was lowered into a titanium reaction tube (la in. ID, 16 in. long, $ in. wall thickness) closed on one end which contained a 11/2-in.-long cylinder of magnesium at the bottom. The inner titanium thermocouple well was positioned eccentrically in the large tube because of the eccentric mounting of the cells on the well. Appropriate modifications of the titanium cap"'12 were made to join the inner and outer titanium

Jan 1, 1968

By E. F. Sturcken, J. W. Croach

A grain orientation distribution function, P(u,F), was developed for use in predicting physical properties in oriented metals. Examples are given of the use of the function to predict thermal expansion coefficients in rolled uranium rods and plate. The P(u,F) function was synthesized from X-ray difpaction intensity measurements, Ii, norrnally used to plot inverse pole figures. The symbols u and F specify the angles that the crystallographic axes of the grain make with the normal to the sample surface and P(u, F) gives the number of grains oriented in each direction, (u,F). P(u,F) is obtained from a least squares fit of the Ii to an orthonormal set of spherical harmonic functions. The P(u, F) function was also used to define a quantity, J, which is a measure of the departure of the orientation distribution from unifomzity (or "randomness"). The J parameter may be used to follow, quantitatively, the amount of preferred orientation induced as a function of mechanical working or heat treatment. An example is given of the application of the J parameter to prefevred orientation studies of hot- and cold-rolled uranium rods and hot-rolled uranium plate. Because P(u,F) is derived from relative intensity measurements by the powder diffraction technique, it is applicable to material with large absorption coefficients and/or grain size and is particularly suitable for characterizing the preferred orientation of large numbers of samples such as fuel elenzents for a nuclear reactor. IN general the physical properties of an oriented metal depend on the direction in which the properties are measured. Hence to predict physical properties the grain orientation must be known as a function of the direction of the specimen. The conventional methods of expressing preferred orientation measurements are the pole figure1 and the inverse pole figure.2-8 Both methods are difficult to use for predicting physical propertiess because they are graphical and because they are stereographic projections and hence are not "area-true." In the present report a quantitative orientation distribution function, P(u,F), is synthesized from pole density measurements normally used to plot inverse pole figures. For inverse pole figure plots the pole densities, pi, are obtained by powder dif-fractometer intensity measurements of their reflections from a flat surface of the sample, normal to the direction of interest. Each pole density, pi, represents a single orientation, i, and is proportional to the volume of material with orientation, i; hence a set of pi gives an approximation for the general orientation for the sample direction measured. The expression8'7 for calculating the pole densities, pi, from the diffraction measurements was previously

Jan 1, 1963

By Ross W. Smith, M. E. Wadsworth, T. James Smolik, A. S. Peck

Ross W. Smith (Acting Instructor, Department of Mineral Engineering, Stanford University, Stanford, Calif.) and T. James Smolik (Kennecott Copper Corp., Salt Lake City, Utah) - Professors Peck and Wads-worth have made an interesting contribution to the study of fluoride activation of beryl. We have a few comments to make regarding the paper and a question to ask of the authors. We note that glass containers were used in the study. Hydrofluoric acid should react with glass to produce SiFg2 in quantity which could adsorb onto the beryl surface (onto either beryllium or aluminum sites). The authors propose that individual F- ions actually go into the mineral surface lattice rather than onto the surface by adsorption of siFi2 ions. Based on infrared reverse bands with an untreated

Jan 1, 1969

By D. G. Westlake

Alloys of poly crystalline Nb-H have been tensile tested at 77" and 120°K after slow-cooling and after quenching from room temperature. A rationale has been developed to explain the effect of cooling rate on ductility in terms of microstructure. The inferior ductility of the slow-cooled alloys in this temperature range can be attributed to the precipitation of coarse hydride particles that fracture in the early stages of plastic deformation. Quenching Produced much smaller hydride particles and a decreased tendency for initia-tion and popagation of cracks. Prismatic dislocation loops, punched into the matrix of quenched alloys, eliminate the yield point and may Play some role in the low temperature ductility of the quenched alloys. The difference in ductility between quenched and slow-cooled V-H alloys was even greater than that observed in the N b-H alloys. It is well known that the ductility of Nb-H and V-H alloys decreases with increasing hydrogen concentra-tion and with decreasing temperature.1-l1 The follow-ing are some of the numerous mechanisms that have been adopted in attempts to explain these observations: 1) hydrogen-dislocation interarction,4'6 2) lowering of the crack surface energy by adsorbed hydrogen,9'10 3) localized lowering of the niobium bond strength,9 and 4) exertion of pressure inside voids by molecular hydrogen.6 A recent study1' indicates that, in some way, the embrittlement is related to the precipitation of a hydrogen-rich phase, because embrittlement and hydrogen solubility have the same temperature dependence. Most of the investigators observed that at very low temperatures there was a return of the ductility. Thus, hydrogenated niobium and vanadium may be said to exhibit a low temperature ductility minimum."1'8'9 It has been reasoned by most observers that diffusion is required for the embrittlement mechanism to be operative, and that as hydrogen becomes immobile at very low temperatures, the ductility increases. This investigation of the mechanical behavior of Nb-H al-loys under various conditions is an attempt to gain a better understanding of the low temperature ductility minimum. EXPERIMENTAL Tensile specimens, with gage length dimensions 20 by 3 mm, were machined from sheet stock" and both faces were ground on wet 600 grit Sic paper to obtain a final thickness of 0.5 mm. Annealing as described earlier12 resulted in average grain diameters of 0.3 mm. The recrystallized niobium tensile specimens were electropolished in 90 parts H2S04, 10 parts HF (48.9 pct) by volume, at 287°K and 30 v. Hydrogen, which may have been present in the starting material and/or added during specimen preparation, was removed by annealing at 1073°K in a dynamic vacuum of 2 X 10-6 torr. Hydrogenated specimens (1.15 at. pct H) were prepared by reaction with a known quantity of pure hydrogen (obtained by thermal decomposition of UH3) at 1073oK, followed by cooling at the rate of 100" per hr. These were vacuum encapsulated, homogenized at 573°K for 3 to 5 hr, and furnace-cooled. Tensile tests were conducted on an Instron machine at a strain rate of 4 x l0-5 per sec. The gripping device was such that the specimen was positioned below the crosshead. Thus, subambient test temperatures could be obtained by immersion of the device in a cooling bath of either liquid nitrogen or Freon-12. The temperature of the Freon-12 was controlled within ± 0.1°K of the desired temperature by automatically monitoring the flow of liquid nitrogen through a copper coil in the bath. Slow-cooling to 77°K was accomplished as follows. The testing device was surrounded by a rubber jacket, open at the top and with small holes in the bottom. Liquid nitrogen, brought up to the bottom of the jacket, entered the holes and vaporized quickly. The temperature was monitored at the specimen with a copper-constantan thermocouple, and a constant cooling rate of 2 deg per min was easily achieved by controlling the level of the liquid nitrogen outside the jacket. RESULTS AND DISCUSSION Low Temperature Ductility Minimum. Resistometric studies of both Nb-H12 and V-H13 indicated that at tem-peratures less than 150°K, virtually all of the hydrogen

Jan 1, 1970