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By O. H. Hahn Eureka

I HAVE lately had occasion to conduct a campaign at the works of the Empire City Company, in Railroad District, Elko County, Nevada, which, if not highly satisfactory, was at least very interesting in a technical point of view, and which I therefore think worthy of communication to the Institute. The lead ores in this district occur in lenticular masses along and near the contact of crystalline limestone with a dioritic porphyry, and consist of argentiferous carbonate of lead and galena, the latter occurring in solid blocks, or in ribbons running through the limestone. Associated with these are silicate, carbonate, and suboxide of copper, and brown and calc-spar. Adding to this, that the proportion of galena in the ore is small, and that no iron pyrites exists in the district, it is at once evident that the ore-mixture is difficult to treat. For a successful reduction by smelting, it would be necessary to introduce into the charge : 1. The proper quantities of sulphur-bearing ingredients, to effect a complete separation of copper and lead ; and, 2. Sufficient silica and iron oxide, to form with the lime and magnesia of the ore, a slag of the required fluidity. The first condition could be fulfilled only very imperfectly, there being no iron pyrites in Railroad, nor in the surrounding districts. The nearest occurrence is in Battle Mountain, whence a supply could not be procured in time. The second condition, i. e., the addition of iron ore and quartz, was easily complied with, there being an abundance of these materials in the vicinity. The furnace of the Empire City Company, is a small shaft¬furnace, with an area of hearth of six square feet, and is supplied with blast by a No. 4 Root blower. In spite of this small size the furnace smelted during this campaign, which lasted 31 days, an average of 28 tons of ore, and 13 tons of fluxes, together 41 tons of charge, per twenty-four hours. The following tables give the complete data in regard to the smelting process, and the results obtained

Jan 1, 1875

By R. L. Pober, L. Kaufman, E. V. Clougherty

Composite structure of hafnium, zirconium, and titanium diboride with additions of metals and/or compound phases were prepared by reactive high-pressure hot pvessing and evaluated in air and in mixtures of oxygen and helium at temperatures up to 2400°K and at linear flow rates of 0.1 to 0.2 ft per sec stp. Oxidation characteristics, principally depth of conversion of diboride to dioxide, were determined by a gas analysis method and by postoxidation metallo-graphic analyses. The best oxidation resistance was observed for hafnium diboride-silicon carbide composite which exhibited a 6-mil conversion to dioxide for a 1-hv oxidation in air at 2200°K compared to a 20-mil recession for hafnium diboride with no additive. Analogous improvements in oxidation resistance were observed for the addition of silicon carbide to zirconium. EARLIER investigationof the oxidation behavior of the diborides of the transition elements of Groups IVA and VA in flowing gas mixtures have produced a ranking of these compounds according to which HfB2 is the most oxidation-resistant followed in turn by ZrB2 > TiB2 > TaBz > NbB2. Other ~tudies~-~ have examined the physical, thermal, and thermodynamic properties of these diborides to provide a sound basis for the more detailed and specialized investigations which are required to generate the information needed to assess the usefulness of such materials in high-temperature oxidizing environments. Recent oxidation studies7 have examined the effect of variations of metal and boron content on the oxidation characteristics of zirconium and hafnium diboride in flowing gas mixtures including air and helium plus oxygen. Results obtained in the latter investigation confirmed the superior oxidation resistance of HfB2 over ZrB2. Moreover, metal-rich compositions of hafnium diboride showed improved oxidation resistance over boron-rich compositions at temperatures up to 2000°K; at higher temperatures the differences are not distinguishable. In particular HfBI.7 exhibited a diboride to dioxide conversion depth of 4 mils in 1 hr at 2000°K; HfB2. 2 exhibited a conversion depth of 16 mils for the same exposure.~ Specimens for the study of metal and boron stoichiometry on the oxidation characteristics of HfB2 and ZrB2 were prepared by high-pressure hot pressing, a specialized type of fabrication which produced dense crack-free bodies of the desired compositions with no significant impurity introductions. The purpose of the present investigation was to explore the possibility of further improving the oxidation resistance of the metal-rich ZrB, and HfB2. The plan to accomplish this objective was based in the formulation of several diboride compositions containing other compounds and phases which are generally known to have good oxidation resistance in one or more types of test environment. Ideally, such additives would also enhance or at least not diminish other boride property values principally mechanical strength and those parameters related to thermal stress resistance. The additions selected for HfBz included zirconium, aluminum, and (Ta + TaB2) designed to produce ternary metal diborides, hafnium to form a discrete HfB phase, chromium to provide a metal skeletal phase, (Hf + Si) to form a discrete hafnium silicide phase, and Sic to provide a discrete second phase. Additions to ZrB2 included A1 + B designed to produce a ternary metal diboride, Zr + Si to form a discrete zirconium silicide phase, and Sic to provide a discrete second phase. All the specimens were prepared by high-pressure hot pressing which was used to advantage to fabricate billets of the variety of compositions desired and suitable for oxidation testing. The present investigation also included the evaluation of high-pressure hot-pressed TiB2and TiB2-20 vol pct Sic, conventionally hot-pressed Boride 2,' and KT silicon carbide. Boride

Jan 1, 1969

By Messrs. von Jonstorff

Continued Discussion of the Paper of Messrs. von Jonstorff, Blair, Dillner and Stead, presented at the New York Meeting of the Iron and Steel Institute, October, 1904.* (Bethlehem Meeting, February, 1906.) CLEMENS C. JONES, Richmond, Va. (communication to the Secretary+) :-In the chapter of this paper entitled "Method for the Determination of Phosphorus," by Andrew A. Blair, a form of the reductor used by Mr. Blair is illustrated. This form was employed by me in my earliest experiments, and abandoned after my adoption of the final apparatus described in my paper on the subject in 1889. The results reported by Mr. Blair are very closely accordant; but my experience was that, in the use of this form, a loss of the solution, amounting to almost a cubic centimeter, was occasioned by minute bubbles of hydrogen rising to the surface, and there exploding. My final reductor was designed to prevent this loss; and the most satisfactory results were obtained with a reductor having the open cup replaced by a bulb-shaped receptacle, provided with a glass stopper, similar to that of a separatory funnel of similar capacity, as suggested in a foot-note in my original paper. In my experience, the use of this later form of reductor repeatedly gave duplicate results which were, coincident to the fourth decimal place. R. W. RAYMOND, New York, N. Y.:-The. remarks of Mr. Jones recall to my mind an interesting part of the history of the Institute, and, of its relation to modern progress in the department covered by this interesting and valuable paper. In

Mar 1, 1906

By Albert J. Phillips

FOR the most part, recent changes in nonferrous physical metallurgy have been gradual and of a transition nature rather than abrupt modifications of existing methods. Development of new alloys containing vital constituents in what formerly would have been considered minute amounts has necessitated more precise control of metallurgical procedure than ever before. Realization of the remarkable effects of minute amounts of specific foreign elements in many alloys has brought about a revolutionary control in the selection of even the most commonplace raw materials. In addition, recognition of the widespread occurrence of precipitation hardness in metal systems, and the utilization of many of these, has emphasized not only the need for precise temperature control but also the necessity for considering the time factor in its effect upon properties in the treatment of most metals. These needs have caused the development and widespread installation of equipment that permits precision of control undreamed of a generation ago.

Jan 1, 1935

By S. C. Hollister

An evaluation of the function of the engineer, so that means whereby education can best serve his needs can be adopted. THERE has been a steady increase in specialized branches of engineering during recent years. Some of these are simply specializations in the function of engineering, such as welding engineering, tool and die engineering, petroleum engineering, and refining engineering. Others are associated more closely with the basic sciences, as for example, geological engineering or engineering physics. Still others tend toward the border line of business, such as administrative engineering or general engineering.

Jan 1, 1950

NEW MEMBERS The following list comprises the names of those persons who became members during the period Nov. 10 to Dec. 10, 1914: Members ABBOTT, Louis BENJAMIN, Chief Engr., Consolidation Coal Co., Elkhorn Div., Jenkins, Ky. ANDERSON, THORVALD J 542 S. Seventh Ave., Mt. Vernon, N. Y. BALFOUR, A. M P. 0. Box 301, Republic, Wash. BOUDWIN, WALKER J., Mech. Engr 159 Pierpont Ave., Salt Lake City, Utah. BRADLEY, LINN, Engr Research Corpn., 63 Wall St., New York, N. Y. BROKAW, ALBERT DUDLEY, Asst. Prof., Min. and Econ. Geol., Univ. of Chicago, Chicago, Ill. BUTLER, PERCIVAL PACE, Asst. Supt., Copper Queen Reduction Wks., Douglas, Ariz. CAJANDER, SVEN G., Mech. Engr Braden Copper .Co., Rancagua, Chile.

Jan 1, 1915

By H. Biloni

PORE formation during solidification has recently been studied theoretically by Piwonka and Flemings.1 For the ordinary conditions of cellular solidification, these authors state that there is a difficulty in explaining the formation of pores. The difficulty arises because the conditions necessary for pore formation are not those obtained during cellular growth. Therefore Piwonka and Flemings1 had to examine various unusual possibilities in order to explain the apparent presence of pores in a cellular substructure of aluminum, taken from Doherty.2 For aluminum, Doherty and Davis3 have developed a pitting technique to reveal substructure, which depends upon the condensation of vacancies from supersaturated solution after quenching. This technique as further developed4 was used to study solidification substructures. In the case of striations, delineation of the substructure is produced by the absence of surface pitting after quenching: in the vicinity of the striations the dislocations which constitute this substructure are sinks for vacancies. In the case of the cellular substructure the experimentally observed effect is the same. However, in this latter case Doherty and Davis4 suggested that micropores associated with the cellular substructure were the agent responsible for providing sinks for vacancies. This interpretation seemed necessary for the cellular substructure because no misorientation arising from a dislocation array could be observed. It is noted especially that Fig. 1 presented by Piwonka and Flemings1 and Fig. 5 by Doherty and Davis,4 as

Jan 1, 1968

By Walter Miller

PETROLEUM refining, like other industries in the United States in 1940, focused much attention on its duties and opportunities in the field of national defense. In counter-distinction to the situation during the World War; the industry is well constituted as LO existing equipment, processes, and capacity together with planned additions to handle any demands that may be made upon it by the defense program needs. Evident throughout was the growing sense of ability to manipulate oil molecules for the production of materials not hitherto considered as being available commercially from petroleum The development and application of catalytically-induced reactions on a broad front is one of the distinguishing characteristics of refining progress during the year.

Jan 1, 1941

By Wilbur Nelson

Little drilling has been done in Kentucky and Tennessee in 1923, with the exception of the Kettle Creek area on the Kentucky-Tennessee line. Oil prices fluctuated between $2.86 and $1.36 Per bbl. for light oil. The Kentucky production was slightly over 8,000,000 bbl., being 1,000,000 bbl. less than during 1922. Tennessee production was approximately 8500 bbl., being a decrease of 1000 bbl, over. 1922. During 1923, the first producing well was brought in, in Clay County, Tenn. Production in Tennessee will undoubtedly increase considerably in 1924, and Kentucky production will probably increase slightly. THE year 1923 has been a dull period in oil development in Kentucky and Tennessee, with the exception of the Kettle Creek area along the Tennessee-Kentucky line, in Clinton and Cumberland Counties, Kentucky, and Clay County, Tennessee. The price of oil during the year has been so low that wildcatters have shown little interest in drilling. At the beginning of the year, light oil sold for $2.31 per barrel and medium oil for $2.06 per, barrel. Prices increased to the highest point for the year in February, when light oil brought $2.86 per barrel and medium oil, $2.61. In April, prices had declined 35 c. while in May an additional decline of 25 c. went into effect. During June, prices declined 20 c. per barrel; during July, 45 c. per barrel; remained stationary during August and September, and dropped during November and December to the low price of $1.36 per barrel for light and $1.21 for medium oil. At present, an increase of 29 c. has brought the price of light oil up to $1.55, and indications are that the price will continue to increase during the coming months. It can readily be seen that during 1923 the price of oil was such as to prevent any drilling except that necessary to hold leases and to maintain production enough to take care of overhead expenses.

Jan 3, 1924

By M. C. Leverett

THE behavior of mixtures of immiscible liquids in porous solids is of rapidly increasing interest to those engaged in the production of petro-leum. The operation of artificial water-floods and the control of natural ones immediately raise questions concerning the fundamental nature of such processes. Moreover, it is now recognized that often water occurs dispersed throughout the rock from which the oil issues into the well,1 and thus tends to move toward the well simultaneously with the oil. The work reported here is a laboratory investigation of the simultaneous, steady-state flow of oil and water through the same column of uncon-solidated sand. It is thus directly related to the situation in which water occurs in oil-producing sands; it may have less direct implications for the displacement of oil from sands by water. However, it is to be clearly understood that the experiments to be described were performed pri-marily to obtain information of a more or less fundamental nature, and are not an attempt to reproduce, on laboratory scale, any part of an oil field. The dynamic behavior of a system in which oil and water are flowing simultaneously through sand is best described in terms of its "effective permeability" to either phase. For incompressible fluids flowing through a system of uniform cross section, the effective permeabilities to the two phases, in darcys, may be defined by the equations:

Jan 1, 1938

By F. R. Scauzillo

Equilibrium data which should be useful in the design and/or evaluation of glycol dehydration units were prepared from an analysis of various published data and the correlation of these data by the use of the thermo-dynamic equilibrium ratio. The equilibrium ratios of water are used to solve the glycol absorber problem; such solutions are necessary to define the number of trays and the glycol circulation rate needed to meet drying requirements. Activity coefficients were obtained which relate directly to the equilibrium ratios of water in the water-TEG-natural gas system. These activity coefficients have been used to calculate the equilibrium dew points for aqueous TEG concentrations of 60 to 99.9 weight per cent for the temperature range of 40° to 120° F. They also provide a means of calculating equilibrium ratios for water in the water-TEG-natural gas system; this applies to any desired TEG concentration and to the temperature range from 40° to 120°F. INTRODUCTION During the last several years, the drying of natural gas with aqueous triethylene-glycol (TEG) solutions has become very prominent. Most users of TEG as a drying agent have been satisfied with the performance of TEG solutions at the conditions used; however, there always has been some discussion of the drying ability of TEG solutions at conditions not commonly encountered such as temperatures below 50° or 60°F, but more particularly temperatures above 100°F, and pressures above 1,000 psia. Today, when higher wellhead temperatures such as 120°F are more commonly encountered many are skeptical of TEG's ability to dry sufficiently well to provide dew points around 32°F, which is generally the maximum tolerable when attempting to dry a gas to contract specifications of 7 Ib/MMscf. These views probably have evolved to some extent from the days when suppliers would not guarantee dew-point depressions in excess of 65° to 75 °OF. Also, the feelings about TEG drying may have arisen from the lack of information about the equilibrium relation of water in the drying operations. Porter and Reid' have reported equilibrium data for a 95 per cent TEG solution, while Townsend2 reported equilibrium data for 95, 98 and 100 per cent TEG solutions. Townsend also presented a calculational method which obtains activity coefficients in the liquid phase and, subsequently, the equilibrium water content of a saturated gas over glycol from published3 atmospheric dew points. Wise, Puck and Failey' presented activity data for the water-TEG system at atmospheric pressure. In the past, the equilibrium ratios published for water in a 95 per cent by weight aqueous TEG solution have been used indiscriminately by many for all concentrations of TEG encountered in gas drying operations. Since essentially all such gas operations require the use of more concentrated TEG solutions, a study was undertaken to correlate the existing equilibrium data for aqueous TEG and gas systems and to provide some means of calculating the equilibrium ratio of water in the natural gas-water-TEG system where TEG concentrations were other than 95 per cent. The data presented herein consider only the equilibrium drying ability of the TEG solutions and do not consider the effect of temperature and pressure on the tray eficiency of contactors. In other words, this paper is concerned primarily with the development of the equilibrium relationship between water in the dried natural gas and the water in the lean TEG entering the top tray of the absorber. BASIC EQUILIBRIUM RELATIONS A relationship which relates the K value of water in the natural gas-water-TEG system to the vapor pressure of water at the system temperature, the total pressure of the system and the activities of the liquid and gas phases has been evaluated. It is well known that, for any component of a mixture at equilibrium between a gas phase and a liquid phase,

By W. C. Spence, Burt C. Mariacher

Methods employed to beneficiate ores utilize relatively few fundamental principles to effect size reduction and concentration. In crushing and grinding only impact and compressive forces with a minor amount of shear are employed. In concentration, gravity, magnetic, electrostatic and flotation constitute the major methods of concentration with minor use of sizing, hand picking and adhesion. This industry, as all others, can expect in the near future to see the development of new techniques for improved efficiency, cost reduction, and exploitation of raw materials hitherto considered unmanageable. NATURAL AND INDUCED RADIOACTIVITY At the Canadian Department of Mines in Ottawa in 1946, C. M. Lapointe developed a picker belt system whereby radioactive ores could be concentrated by electromechanical means. This invention ultimately led to development of what is now refer- red to as the Lapointe Picker and which has been used commercially at Port Radium and Port Hope for the upgrading of jig concentrates. Basically, the system consisted of conveying sized uranium ore on a belt under a radioactivity detection device which in turn electronically operated a kicker or plunger that separated the ore from the gangue constituents. Thus, a new principle for mineral concentration, radioactivity, was introduced commercially.

Jan 7, 1962

By Kenneth K. Humphreys, R. M. Quinlan, Stan Venkatesan

INTRODUCTION 1 * The coal industry in the United States has undergone significant economic changes in recent years. For example, the price of coal remained relatively constant from 1950 to 1969 (see Figs. 5-1 and 5-2) but steam coal prices tripled and metallurgical coal prices doubled from 1969 to 1974. This price structure has created a new economic environment for coal preparation. Contributing factors to these price trends include: 1) Coal Mine Health and Safety Act of 1969. 2) Mid-East oil embargo of 1973.

Jan 1, 1979

By HARRISON W. CRAVER

THE principal purposes of library-catalogs are to enable a reader to find a book of which the author, the title, or the subject is known; to show what the library has. by a given author, or on a given subject; and to assist in the choice of a book, as to its edition, or as to its character. The author, in a narrow sense, is the person who writes a book; in a wider sense it is applied to him who is the cause of the book's existence, e.g., editor, translator, compiler, etc. Bodies of men, societies, and countries are, from a cataloging point of view, con¬sidered the authors of their official publications, memoirs, transactions, etc. All names selected as author names are arranged in strict alphabetical order. A subject catalog fulfills its purpose by entering or registering each book under the name of that subject or topic of which the book chiefly treats. It may or may not be alphabetical in arrangement. If the arrangement is not alphabetical, the catalog is commonly called a classed subject catalog, although this name might with equal propriety be applied to some alphabetical arrangements.

Jan 1, 1920

By N. Arbiter, C. C. Harris

Analysis of ball and pulp flow in ball mills indicates that three factors may become critical with increasing mill diameters: ball size, fraction critical speed, and average pulp flow velocities. Ball diameters may need to be decreased and fraction critical speeds increased with ores which show decreased breakage rate coefficients above 1.2 mm (14 mesh). With 5.5-m (18 ft) and larger mills at higher circulating loads, pulp flow velocities may become capacity limiting and also may limit increases in ball mill diameters.

Jan 1, 1985

By R. W. Smith, R. J. Charles

Fractions of glass particles in the size range 0.5 to 5.0 µ were prepared by an elutriator that operates in a centrifugal field. Although mean sizes of commercially graded abrasive powders were ten times greater than those of samples prepared by the elutriator, frequency size plots for elutriator samples compared favorably. Efficiency of separation was low and amounts of material recovered by the elutriator were small, but the method should find use in preparation of small amounts of sized materials for laboratory investigations.

Aug 1, 1956

The Duluth Engineers' Club was formally organized on the evening of Aug. 5, 1918, at a meeting .attended by over l00 members of the several engineering professions. W. G. Swart, a member of our Institute, was elected the first President of the Club. At the organization meeting, an opportunity was given, to Alfred D. Flinn, Secretary of the United Engineering Society, to outline the assistance that is being rendered to the Federal Government in the present contingency by members of the engineering profession. Membership in the Duluth Club is to be open to mining engineers on the iron ranges as well as to the residents of the city of Duluth.

Jan 10, 1918

By I. P. Pardee

In our mixture at Musconetcong Iron Works we have an exceedingly hard, dense, magnetic ore, which contains some iron pyrites. The sulphur runs from 0.5 to 1.5 per cent. To prepare this ore better for the furnace, and with a view of making a softer iron, we tried roasting the ore in a Gjers kiln. When it worked well, the improvement in the iron was very perceptible ; but the ore was continually sintering and forming scaffolds across the bosh of the kiln.

Jan 1, 1887

By C. G. Bieber, J. R. Mihalisin, R. T. Grant

A growing demand for longer service life of gas turbines has placed increasingly rigorous requiret~rents upon superalloys employed for that application. Long-titne testing at high temperature has revealed that phase transformations occur in all superalloys. A common one of particular interest is o formation. Presented here are studies made to identify a and to characterize its formation and effect on properties in three cast nickel-base superalloys—IN 100 alloy, alloy 713C, and alloy 713LC. Methods are discussed by which o can be eliminated or inhibited in IN 100 alloy and alloy 713C. Evidence was obtained to indicate that some types of o may be more detrimental than others. Limitations in the electron vacancy approach to o prevention are pointed out, and it is shown how alternative approaches, such as reducing a complex superalloy matrix to the form of a pseudo-ternary system permitting equilibrium diagram treatment, lead to additional insights into the formation of in these alloys. AROUND 1960. Beiber1 developed IN 100 alloy, which still remains one of the strongest commercially available nickel-base superalloys. The principle used in the design of this alloy was to produce large quantities of y' phase in a y matrix through the use of copious amounts of aluminum and titanium. In 1963, ROSS' showed that when certain heats of this alloy were held for a long time at 1650°F they formed an acicular phase, subsequently identified as a.3 a is a hard and brittle phase first discovered in the Fe-Cr system by Bain and Griffiths.4 They termed it the "B" constituent. Subsequently this same phase was found in other systems, primarily those of the transition elements, and acquired the name "a" by which it is now known. The crystal structure of the a phase was first determined in the Fe-Cr system in 1950.5 It was shown to be tetragonal with a c/a ratio of about 0.52. as is the case with a found in other systems. This characteristic crystal structure is now the means by which a is identified. In superalloys, such as IN 100 alloy. large amounts of o impair the high-temperature creep strength and drastically reduce room-temperature tensile ductility. Discovery of o phase in some heats of IN 100 alloy quickly led to investigations of other superalloys for similar transformations. It was found that many of the stronger, more highly alloyed. super-alloys were indeed susceptible to o formation. This investigation has been concentrated on three commercial alloys: IN 100 alloy, alloy 713C, and alloy 713LC. J.R.MIHALISIN,MemberAIME, and C.G.BIEBER are with The International Nickel Co., Inc., Paul D. Merica Research Laboratory, Sterling Forest, Suffern, N. Y. R. T. GRANT, Member AIME, is with The International Nickel Co., Inc., Pittsburgh, Pa. Manuscript submitted May 22. 1968. IMD A detailed study has been made of the phase transformations and their relation to a formation along with a consideration of electron vacancy approaches for predicting a-forming propensity in these alloys. EXPERIMENTAL PROCEDURE Phase transformations were studied by light and electron microscopy, electron diffraction, microprobe investigations, and X-ray diffraction. Specimens for light micrographic examination were prepared by conventional grinding and polishing followed by etching with glyceregia (2:l HC1/HNO3 + 3 glycerine by volume). Photomicrographs of stress-rupture specimens were taken adjacent to the fracture unless otherwise noted in the text. Negative replicas for electron microscopy were taken from surfaces electropolished with a solution of 15 pct H2SO4 in methanol. For carbon extraction replication, a solution of 10 pct HC1 in methanol was used. A Siemens Elmiskop I was used for all electron microscopy. Selected-area diffraction studies were made at 80 kv using evaporated aluminum for standardizing the patterns. A nondispersive electron microprobe attachment was used to analyze the extracted precipitates chemically. The fluorescent X-rays were recorded using a flow counter containing P10 gas (90 pct Ar-10 pct methane) with a beryllium window and a single-channel pulse-height analyzer. The pulses from the analyzer were passed to a scaler-ratemeter and differential curves of counting rate vs pulse amplitude were obtained. The base line of the analyzer was driven with a synchronous motor at 0.5 v per min and a channel width of 0.5 v. The time for 105 counts was printed out for each 0.5-v increment. The microscope was operated at 80 kv with beam currents of 1 to 20 pa. This equipment detects elements from atomic number 13 to 40. X-ray diffraction studies were usually made on residues electrolytically extracted in 10 pct HC1 in H2O, although in one case a pattern was obtained from an etched surface of a metallographic specimen. A Siemens Crystalloflex IV was used with iron-filtered CoKa radiation. X-ray patterns were recorded using a goniometer speed of : deg per min. The scintillation counter and pulse-height analyzer operated at a channel height of 10 v and a channel width of 12 v. The equipment was calibrated with a powdered gold standard. The residues usually contained a number of phases. several of which could not be found in the ASTM card file. In addition, as is shown for the case of a phase in IN 100 alloy, other phases had a somewhat different lattice parameter from that reported in the ASTM card file, making it difficult to separate and identify constituents by comparison with ASTM d spacings. For these reasons, phases were identified on the basis of the lattice parameter obtained by indexing the ob-

Jan 1, 1969

By David L. Holt, Walter A. Backofen, Anwar-ul Karirn

ANNEALING the binary alloy, Mg-0.5 wt pct Zr in a hydrogen atmosphere results in extensive precipitation of zirconium hydride. The morphology of these precipitates has already been investigated.lm3 Squires, Weiner, and phillips4 found, following creep testing of the hydrided alloy at 450" and 500°C, that hydride denuded zones formed along grain boundaries that were aligned approximately normal to the tensile axis. Zone formation was attributed to diffusional creep by magnesium transport down the prevailing stress gradients.4'5 Recently, electron microprobe analysis by Karim, Holt, and Backofen6 showed the zones indeed to be zirconium-free and furthermore it was shown that in compression, zones formed along boundaries approximately parallel to the stress axis. Thus it was confirmed that the zones are formed by diffusional creep. Typical zone-formation is shown in Fig. 1. Karim, Holt, and Backofen also measured the con- tribution to the total strain, from diffusional flow, slip creep, and grain boundary shear: results showed that diffusional strain tends to saturate with increasing imposed strain, while grain boundary shear eventually becomes the dominant deformation mode. It was suggested in explanation that the precipitate-denuded zones are soft and easily sheared, such deformation contributing to the grain boundary shear measurement. A point to be emphasized is that the Mg-0.5 Zr alloy was not superplastic for the index of strain rate sensitivity of flow stress, m = a log log 6 was only 0.25. It was recognized that diffusional creep in a poly crystalline aggregate must be accompanied by boundary shearing.' The suggestion was that the non Newtonian-viscous character of diffusional creep in the Mg-0.5 wt pct Zr alloy is due to resistance to sliding of boundaries lying approximately parallel to the tensile axis.= The work described in the present note should be seen against the above background for it represents initial efforts to observe in a similar way diffusional creep in a superplastic alloy. Previous work with the ternary-alloy Mg-6 Zn-0.5 Zr, pellet extruded, showed it to be superplastic however it does not contain resolvable precipitates to act as internal markers for diffusional creep. Also the fine grain size of the alloy (0.5 p) made conventional metallography rather difficult. Solubility relationships in the Mg-Zn-Zr system are not well known, however making reasonable guesses about the probable phase diagram of the ternary, Mg-Zn-Zr, various heat treatments were attempted to produce hydride precipitation. Finally a 16-hr anneal at 495' in hydrogen was found to pro-

Jan 1, 1970