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By Donald B. Gillies

PROBABLY the most critical and difficult period in an engineer's career is that between the completion of his college work and his attainment of professional recognition and accepted status in the industrial world. Upon leaving school the young graduate breaks his immediate ties with his educational institution and in a sense finds himself adrift. At this time in his life a society like our Institute has both the responsibility and the privilege of meeting a vitally important need in his professional life. Some of these young men are Student Associates, in the year after graduation, and some are Junior Members, but all need advice and assistance. In some respects this situation will be accentuated by the war. Not only will thousands of young engineers be mustered out of military service but the process we describe generally as industrial reconversion will make necessary many readjustments in personnel. About two years ago the Institute recognized the opportunity of helping the younger member to help himself by appointing a new standing committee to be known as the Committee on Professional Development of Junior Engineers. Herbert Hoover is Honorary Chairman and it is my privilege to serve as Chairman. The name of the Committee is not entirely satisfactory but it expresses the general objective. The present article is in the nature of a progress report of the work of this Committee.

Jan 1, 1945

By C. M. Moncrief, B C. Craft

A bentonite-clay drilling mud when treated with tetrasodium pyroarsenate underwent substantially the same reduction in viscosity and water loss as when treated with the complex phosphates. The complex arsenate showed a slightly higher reversion after heating; the other arsenates showed poor viscosity-reducing properties. Introduction During the past 10 years the chemical control of drilling mud has become of major importance in affecting the successful drilling and working over of wells. The desired properties of drilling mud have been well established, and in obtaining these characteristics there has developed a large market for viscosity-reducing chemicals. Viscosity reduction produced by humic acid, tannic acid, sodium silicate, sodium tannate, Calgon, and the complex phosphates has been described by Loomis, Ford, and Fidiam.l The effects Of treatment with complex phosphates and ammonium PolyPhosPhates on the rheological properties of muds were investigated by Fancher2 and the alkali vanadates have been described by Williams.3 Laboratory Investigations It is the purpose of this paper to point out the effects of arsenates in controlling the viscosity and gelling characteristics of a drilling mud. Viscosities and gel strengths were measured at room temperatures with a Stormer viscosimeter calibrated in centipoises and operated at 600 r.p.m. Water loss was determined at 80°F. with the Baroid low-pressure wall-building tester at a pressure of I00 lb. per sq. in. for 30 min. The hydrogen-ion concentration was measured with a glass electrode. The bentonite-clay suspensions were prepared in the laboratory and allowed to age several days before testing. Members of the Arsenic Group in the periodic Table include arsenic, antimony and bismuth, but this investigation was limited to arsenic. Phosphorus also occurs in Group V of the Periodic system and phosphorus and arsenic form many closely related compounds such as pH3 and AsH3, P2O5 and As2O5, H3PO4 and H3AS04 Samples of tetrasodium pyroarsenate were prepared by fusing c.p. disodium arsenate (Na2HA5O4.7H2O). According to Friend,' this re-forms the ortho-arsenate on dissolution in water. Sodium trihydrodiorthoarsenate was prepared as described by Mellor,5 from arsenic pen-toxide as follows: As2O5 + 3H20 -> 2H3AsO4 2H3AS04 + 3NaOH Na3H3(AsO4)2 .3H20 Sodium dihydrogen orthoarsenateWaHz-As04) was obtained by fusing together equivalent quantities of arsenious Oxide and sodium nitrate, dissolving the residue in water and allowing it to crystallize.

Jan 1, 1946

By C. M. Moncrief

A bentonite-clay drilling mud when treated with tetrasodium pyroarsenate underwent substantially the same reduction in viscosity and water loss as when treated with the complex phosphates. The complex arsenate showed a slightly higher reversion after heating; the other arsenates showed poor viscosity-reducing properties. Introduction During the past 10 years the chemical control of drilling mud has become of major importance in affecting the successful drilling and working over of wells. The desired properties of drilling mud have been well established, and in obtaining these characteristics there has developed a large market for viscosity-reducing chemicals. Viscosity reduction produced by humic acid, tannic acid, sodium silicate, sodium tannate, Calgon, and the complex phosphates has been described by Loomis, Ford, and Fidiam.l The effects Of treatment with complex phosphates and ammonium PolyPhosPhates on the rheological properties of muds were investigated by Fancher2 and the alkali vanadates have been described by Williams.3 Laboratory Investigations It is the purpose of this paper to point out the effects of arsenates in controlling the viscosity and gelling characteristics of a drilling mud. Viscosities and gel strengths were measured at room temperatures with a Stormer viscosimeter calibrated in centipoises and operated at 600 r.p.m. Water loss was determined at 80°F. with the Baroid low-pressure wall-building tester at a pressure of I00 lb. per sq. in. for 30 min. The hydrogen-ion concentration was measured with a glass electrode. The bentonite-clay suspensions were prepared in the laboratory and allowed to age several days before testing. Members of the Arsenic Group in the periodic Table include arsenic, antimony and bismuth, but this investigation was limited to arsenic. Phosphorus also occurs in Group V of the Periodic system and phosphorus and arsenic form many closely related compounds such as pH3 and AsH3, P2O5 and As2O5, H3PO4 and H3AS04 Samples of tetrasodium pyroarsenate were prepared by fusing c.p. disodium arsenate (Na2HA5O4.7H2O). According to Friend,' this re-forms the ortho-arsenate on dissolution in water. Sodium trihydrodiorthoarsenate was prepared as described by Mellor,5 from arsenic pen-toxide as follows: As2O5 + 3H20 -> 2H3AsO4 2H3AS04 + 3NaOH Na3H3(AsO4)2 .3H20 Sodium dihydrogen orthoarsenateWaHz-As04) was obtained by fusing together equivalent quantities of arsenious Oxide and sodium nitrate, dissolving the residue in water and allowing it to crystallize.

Jan 1, 1946

By C. C. Whittier

CIVILIZATION'S PROGRESS, which has multiplied man's comforts, conveniences, a n d happiness, is based upon the extensive employment of natural minerals and sources of energy. Mineral resources are basic factors in modern economic development, machine industry, international trade and world power. A survey of mineral consumption shows that the United States leads the world in the production and consumption of energy materials, of metals, and of the large and diverse array of earth materials that fall in the nonmetallic mineral group. The use of nonrnetallic minerals exceeded both the metals and the fuels in the long period before the industrial age, but it is only in the last two decades that consumption of non- metals has kept pace with and approximated in value the output of metals. Although the data of production in the first half of the last century are meager and fragmentary, the record of the past fifty years-the period of most rapid growth-is available, and reveals an astounding growth.

Jan 1, 1933

By C. C. Whittier

PLANS are well matured for the joint meeting of the Coal Division and the Ohio Section of the Institute at Columbus, Ohio, Oct. 27 and 28, at which a large attendance is expected. The proceedings for a day and a half will be devoted largely to the uses of coal, the program providing for two technical sessions in the auditorium of Battelle Memorial Institute (505 King Ave.) on Friday, and various plant inspec¬tions on Saturday morning. By way of diversion on Saturday afternoon arrangements have been made for attendance en bloc at the football game between Ohio State and Northwestern, 100 seats having been reserved for the game at $2.40 each-as long as they last. An inventory of the high lights of the meeting would be incomplete without reference to the informal banquet at the Deshler-Wallick hotel on Friday evening, for which Eli T. Conner, Chairman of the Coal Division, is down for a talk, and Howard N. Eavenson, Vice-president of the Institute, will be the principal speaker. The program in detail is as follows:

Jan 1, 1933

By Ferid Kromer

This paper is the first in a series which will describe geology, mining methods, and production costs of some, of Turkey's more important minerals. In this paper the economically significant minerals-chromite, meerschaum, and magnesite-of the Tagtepe district are described. The cost data presented are believed by the author to be the first made public on Turkish chromite mining.

Jan 1, 1950

By R. F. Weber

The relation between the chemical composition and the refractoriness of fire-brick has long attracted the attention of manufacturers of fire-brick and others interested in their use, yet but little systematic work has been done along this line, especially in the United States. Analyses of fire-brick have been quoted for years, but fire-tests of brick, except those of durability in practical use, have usually been lacking. Although many tests and analyses of foreign fire-brick have been published, only a few have appeared in the United States; and even in the foreign literature, the references and facts are more or less scattered. The most elaborate foreign paper on the subject is that by Dr. Jochum.' One of the earliest, and perhaps the most detailed piece of work in the United States, is that of F. Platt, which was done for the Pennsylvania Geological Survey, in 1876.2 His investigation consisted of the analysis and heat-tests of 21 bricks, the testing being made in an experimental shaft-furnace at Har-risburg, Pa. All the bricks were more or less affected at the temperature reached, which was considerably higher than the melting-point of steel. The exact temperature at which individual bricks fused was not ascertained, hence the comparisons quoted in the paper are of value only for the bricks used in the test. The next comprehensive investigation, made by the New Jersey Geological Survey,³ deals chiefly with fire-clays; analyses and refractory tests having been made of 123 clays, kaolins, feldspars and fire-sands. Here; again, there was no accurate means of measuring the temperature, the only measurement of

Jan 1, 1905

By D. L. Wood, J. H. Westbrook

The tensile behaviors of the CsCl structure compound AgMg are extensively documented in terms of strain, strain rate, temperature, composition, and metallurgical processing treatment. The observations lend themselves to presentation in terns of three regimes of deformation behavior; 1) low temperatures where deformation is primarily by slip; 2) intermediate temperatures where the deformation mode is also slip but with the detailed behavior dominated by dislocation interactions with solute atoms; 3) high temperatures where defomation is primarily by diffusion controlled processes. Of all the material groups of potential interest as high-temperature structural materials, the inter-metallics have been the least studied, particularly with respect to their mechanical behavior. Moreover, the application and processing of intermetallics for uses which exploit their often unique physical properties have been impeded by a lack of understanding of their mechanical properties. Previous work in this area* has been largely *For a recent review, see Westbrook.' exploratory, aimed on the one hand at the direct empirical development of materials of engineering utility and ,on the other at identification of the important parameters affecting the mechanical behavior of inter metallics. As a consequence, there has not been available, heretofore—for any inter-metallic—data, sufficient in extent or precision to provide an adequate phenomenological description of the effects of metallurgical variables on deformation behavior. Such documentation is prerequisite to intelligent application or processing design and is also necessary for testing present and future theoretical analyses of mechanical behavior. It was therefore an objective of the present investigation to document the deformation behavior of a simple ordered intermetallic over as wide a range as possible of all the usual metallurgical variables. The compound AgMg was chosen as the subject of this investigation because it met all of a group of desired criteria, namely: 1) congruent but moderate melting point; 2) simple crystal structure; 3) ordered structure persisting to the melting point; 4) broad solubilities for the component elements. The first and last criteria were expected to aid in the preparation of homogeneous single-phase specimens: the second and third to help simplify the

Jan 1, 1962

By Frederic Benard

PRIoR to 1936, the Ontario Refining Co. received all incoming blister copper from The International Nickel Company's smelter in the usual form of 460-lb. cakes, or slabs. These were received in open cars in lots of 250 pieces. At the refinery the cakes were unloaded onto narrow- • gauge cars, for convenient handling and pickup by charging cranes. In March 1936, an investigation was started on the feasibility of transferring converter copper in the molten state from the smelter to the refinery anode furnaces, a distance of 1 1/4 miles. Although common in steel practice, the transportation of blister copper in this form had not previoisly been attempted and a preliminary study of the various factors involved was therefore necessary. For this purpose, a series of experiments was made in which molten copper, removed at different stages during the furnace cycle, was held in a small portable holding furnace. This vessel was essentially a refractory-lined steel cylinder provided with ports for filling and emptying, heated by an oil burner. Dimensions of the steel shell were 3 ft. 10 in. diameter by 7 ft. 3 in. long, and thickness of refractories depended on the design and combination used for the particular experiment. The vessel was filled with approximately 2 1/2 tons of copper at a predetermined temperature, the lining having been preheated to a definite point by means of an oil burner. All openings were well luted and temperature readings were made every 15 min. by means of an immersion-type thermocouple. In this manner the rate of heat loss resulting with different refractory design could be developed. The ratio of exterior surface to weight of metal was taken into consideration in comparing the experimental results with what might be expected for a full-sized unit, and observations were also made on type and degree of slag accretion. It was not possible to get as much information on this latter point as desirable, but all evidence showed that the problem would be control of slag build-up rather than attack on refractories. From the information derived, and in consultation with the engineering staff of the supplying company, an order was placed for the first

Jan 1, 1944

By William E. Ford, Edward Salisbury Dana

5. Crystallography. - The subject of Crystallography includes the description of the characters of crystals in general; of the various forms of crystals and their division into classes and systems; of the methods of studying crystals, including the determination of the mathematical relations of their faces, and the measurement of the angles between them; finally, a description of compound or twin crystals, of irregularities in crystals, of crystal- line aggregates, and of pseudomorphous crystals. 6. Definition of a Crystal.- A crystal * is the regular polyhedral form, bounded by smooth surfaces, which is assumed by a chemical compound, under the action of its intermolecular forces, when passing, under suitable conditions, from the state of a liquid or gas to that of a solid. As expressed in the foregoing definition, a crystal is characterized, first, by its definite internal molecular structure, and, second, by its external form. A crystal is the normal form of a mineral species, as of all solid chemical com- pounds; but the conditions suitable for the formation of a crystal of ideal perfection in symmetry of form and smoothness of surface are never fully realized. Further, many species usually occur not in distinct crystals, but in massive form, and in some exceptional cases the definite molecular structure is absent. 7. Molecular Structure in General.- By definite molecular structure is meant the special arrangement which the physical units, called molecules, assume under the action of the forces exerted between them during the formation of the solid. Some remarks are given in a later article (p. 22 et seq.) in regard to the kinds of molecular arrangement theoretically possible, and their relation to the symmetry of the different systems and classes of crystals.

Jan 1, 1922

By William P. Blake

THE use of diamonds upon a large scale in drilling rocks, and the substitution to a certain degree of rotary diamond drills for the ordinary steel percussion drills, marks a new era in the art of mining. Since the invention by Leschot of the diamond drill, it has steadily advanced in its utility and range of application, and in the appreciation of miners and engineers. I t must be claimed as one of the many gifts of science to the arts ; and it is, in particular, one of the fruits of the scientific education given at the Ecole Centrale, at Paris. Members are all, doubtless, more or less familiar with the construction of the drill and of the machinery by which it is applied in boring. I t is, therefore, my present purpose only to direct your attention to some recent marked improvements, made by the American Diamond Drill Company, by which the economy and efficiency of the machines have been increased. Form of Bit.-The annular or ring form of the drill-head or bit was, I believe, the earliest; and it is still in use, without essential modification, wherever it is desired to obtain a sample " core" or specimen of the rock traversed. But for mere drilling, regardless ~f the preservation of a test-core, a solid-head bit is preferred, except for very large holes. Until recently, these solid-head bits were made with a pointed cutting face shaped like an obtuse cone. This form was assumed to be the best, being most in accordance with the experience obtained with percussion drills. I t is found, however, that the exact reverse

By A. N. Winsor

Increased use of private aircraft in civil engineering, mining, forestry, and other land-use activities creates an opportunity for amateur aerial photography. Taking a photograph having less than 5° tilt requires precision equipment and skilled personnel, while controlled horizontal photography is primarily a terrestrial method that has passed to the limbo of forgotten things. But the remaining possibility – oblique aerial photography – can be…

Jan 2, 1955

By Albert C. Harding

FOR several years barite (BaSO4) production has topped such better known minerals as feldspar and fluorspar in annual tonnage and is now well established among our foremost nonmetallic industries. DESCRIPTION Of widespread occurrence in the United States, barite is relatively soft (hardness, 2.5 to 3.5), inert, heavy (specific gravity, 4.5), and is also called "barytes" (sometimes pronounced "bear-i-tease"), "heavy spar" and "tiff." It occurs with granular and earthy structure but usually has coarse, orthorhombic crystallization. It is commonly white, and although occurring in various shades of red, yellow, and gray, barite always gives a white streak and can be scratched by the ordinary prospecting pick. Its softness and weight are usually sufficient to establish field identification. Another aid is the "rotten egg" odor of H2S which sometimes emanates from freshly fractured surfaces. Barite can be readily distinguished from two other minerals which have somewhat similar occurrences and characteristics. The relatively rare celestite, strontium sulphate, has a specific gravity slightly less than 4.00 and gives a distinctively crimson color in a flame test. The very rare witherite, barium carbonate, has a specific gravity of 4.3 but readily effervesces with dilute hydrochloric acid. OCCURRENCE All known commercially important barite deposits in the United States occur as re placements or cavity fillings in schists, shales, limestones, dolomites, and quartzites, or as residual deposits from such formations. In Georgia, Tennessee, North Carolina, and Missouri, high-grade barite is recovered as fragments from residual clays covering quartzites and dolomites. In Arkansas, Nevada, and California, barite, usually of lower grade, is mined from replacement deposits. These seven states contributed the entire production reported by the U. S. Bureau of Mines for 1945 as given in Table I. [TABLE 1-Crude Barite Sold or Used by Producers in 1945 STATE SHORT TONS Arkansas260,660 Missouri225,467 Georgia110,393 Tennessee32,812 Nevada28,919 Other States37,811 Total 696,062] "Other States" included only California and North Carolina. Such a large part of this undistributed production came from California that that state probably outranked both Nevada and Tennessee. For the second consecutive year Arkansas was the leading producing state, particularly worthy of note because there was no commercial production of barite there prior to 1941 and because the entire production of Arkansas has come from one large deposit which is being operated by two companies. CONSUMPTION [The 1945 consumption as reported by the Bureau of Mines was: 482,442 tons as ground barite 139,288 tons in making lithopone 99,173 tons in producing barium -- chemicals Total 720,903 tons]

Jan 1, 1947

By A. C. Dittrick

THE Simon-Carves washer, originally known as the Baum jig washer, was first built in Europe about 1892. It was probably the first washer to use intermittent pressure of air on water in one part of the wash box to obtain water pulsations in another part. This type of washer was also the first to successfully clean various sizes in the same unit. Previous practice was to size closely before washing. Today there are several large firms abroad, and a few in the United States, that are constructing the Baum type washer. The design of all is practically the same, their differences being only in details. In 1928, the Hanna Coal Co. first gave consideration to the question of coal cleaning. It was believed at that time that by efficient removal of so-called noncombustibles appearing in the Pittsburgh No. 8 seam, certain markets that had been lost due to poor preparation might be recovered. Mechanical cleaning and mechanical loading were under consideration. This type of cleaning was considered the most practical means of removing impurities in the sizes below 4 in. It was decided to adopt mechanical cleaning and develop a system of mechanical loading that would be successful on No. 8 coal.

Jan 1, 1935

By Walter H. Bucher

This symposium is designed to lay the basis for a general discussion of the place of geophysics in the training of geologists. As there is danger that in the ensuing debate individual interests may be given emphasis out of proportion to their place, we shall do well to view the whole field of geological inquiry in order to see the problem in true perspective. The Nature of Geological Inquiry "Basic" and "Complex" Sciences It is convenient to divide all science into two major divisions, the basic and the complex sciences. The basic sciences separate out from reality such entities as "substances" and "movements," describe their behavior in terms of arbitrary units of measurement and derive from them by progressive abstractions concepts and patterns of behavior that exist between them, so-called general "laws" and "properties" of nature. The complex sciences, on the other hand, deal, with little or no abstraction, with those objects of reality that are accessible to man in the atmosphere, the hydrosphere, the lithosphere and the biosphere. Their work comprises two types of inquiry. One is concerned with abstractions to the extent of dealing with types rather than individuals—that is, with such things as plants, animals, protoplasm; clouds, streams, gla- ciers; volcanoes and mountain ranges. It comprises the search for general properties and patterns of behavior or "laws" that characterize the objects and their reactions to each other. These properties and laws apply always, everywhere. They are independent of the stream of time. We may call the results of this sort of inquiry timeless knowledge. The other type of inquiry is concerned with the objects themselves—that is, with this animal and that plant; this river system and that mountain chain; this glacier and that valley. Like all concrete objects in nature, they are subject to change with the passage of time, especially when it is measured in years, centuries, eons. The characteristics by which we recognize them —indeed, their very existence—are dependent on their position at this point in the stream of time. This we may call time-bound kntowledge. The so-called descriptive sciences are all bound to the past of which the objects of their study are the product and through which alone their present properties call be understood. They are historical sciences. This obvious fact is easily overlooked, which leads to serious misunderstanding, as we shall see later. Dynamic Geology With this broad picture in mind, let us now examine the nature of geological inquiry, defining, for the purposes of this discussion, geology as the science of rocks. Air is not a rock; water is. Meteorology and climatology are, correspondingly, gen-

Jan 1, 1946

By Walter H. Bucher

This symposium is designed to lay the basis for a general discussion of the place of geophysics in the training of geologists. As there is danger that in the ensuing debate individual interests may be given emphasis out of proportion to their place, we shall do well to view the whole field of geological inquiry in order to see the problem in true perspective. The Nature of Geological Inquiry "Basic" and "Complex" Sciences It is convenient to divide all science into two major divisions, the basic and the complex sciences. The basic sciences separate out from reality such entities as "substances" and "movements," describe their behavior in terms of arbitrary units of measurement and derive from them by progressive abstractions concepts and patterns of behavior that exist between them, so-called general "laws" and "properties" of nature. The complex sciences, on the other hand, deal, with little or no abstraction, with those objects of reality that are accessible to man in the atmosphere, the hydrosphere, the lithosphere and the biosphere. Their work comprises two types of inquiry. One is concerned with abstractions to the extent of dealing with types rather than individuals—that is, with such things as plants, animals, protoplasm; clouds, streams, gla- ciers; volcanoes and mountain ranges. It comprises the search for general properties and patterns of behavior or "laws" that characterize the objects and their reactions to each other. These properties and laws apply always, everywhere. They are independent of the stream of time. We may call the results of this sort of inquiry timeless knowledge. The other type of inquiry is concerned with the objects themselves—that is, with this animal and that plant; this river system and that mountain chain; this glacier and that valley. Like all concrete objects in nature, they are subject to change with the passage of time, especially when it is measured in years, centuries, eons. The characteristics by which we recognize them —indeed, their very existence—are dependent on their position at this point in the stream of time. This we may call time-bound kntowledge. The so-called descriptive sciences are all bound to the past of which the objects of their study are the product and through which alone their present properties call be understood. They are historical sciences. This obvious fact is easily overlooked, which leads to serious misunderstanding, as we shall see later. Dynamic Geology With this broad picture in mind, let us now examine the nature of geological inquiry, defining, for the purposes of this discussion, geology as the science of rocks. Air is not a rock; water is. Meteorology and climatology are, correspondingly, gen-

Jan 1, 1946

By Albert Sauveur

(Winces-Barre Meeting, June, 1911.) THE instrument about to be described meets so perfectly the special needs of the metal microscopist that there seems to be little doubt but its merits must be readily appreciated by those who have had any experience in the microscopical examination of metals. The Microscope-Stand.-The microscope-stand proper, Fig. 1, consists of a microscope-tube, provided with both coarse and fine adjustments of the best construction, and with a draw-tube, rigidly mounted on a bar supported at both ends on substantial and firm cast-iron legs. The height between the table and the under side of the supporting bar is 5 in. and the distance between the supporting legs 12 inches. This arrangement' affords free space below the objective for the examination of large specimens of metals, such as full rail-sections, without detracting in the least from the value of the instrument when applied to the examination of the usual small specimen, as explained later. Many metal microscopists frequently have to examine bulky specimens, and this is altogether impossible with the ordinary microscopes as well as with the special metallurgical microscopes which have been designed and described from time to time. Recourse must be had to all sorts of makeshifts for the proper support of large specimens, or, more often, the microscopist gives up the attempt altogether, or else resigns himself to the cutting of the bulky samples into small pieces to -be laboriously polished and separately examined. It is believed that an instrument permitting the examination of large as well as of small specimens with equal ease and accu-

Dec 1, 1911

By M. S. Burton, B. W. Christ, G. V. Smith

Evidence of the effects which high-angle grain boundaries and veining subgrain boundaries have on the yield phenomenon of zone-refined iron is reported. Room-temperature tensile tests on 50-mil wive at several gram sizes produced upon recrystallization at diffevent temperatures below 910C (a-y phase-transfornzatzon temperature) show that upper and lower yield stress decrease with increasing grain size. The upper yield point effectively disappears at grain sizes of 81 and 102 u in samples of this diameter. However, samples of 129 p grain size. produced during recrys-tallization at 950°C, exhibit a pronounced upper yield point and an increased lower yield stress. Possible causes of the reversal in the grain-size dependence of yielding are discussed. Veining substructure, detected with picval-HC1 etchant, but not with 2 pct nital, is formed during the a-y transformation, and is believed to account for the observed effecls. The strengthening associated with high-angle boundaries in zone-refined tron is discussed in terms of: 1) the stress dependence of slzp multiplicity, and 2) the stress dependence of dislocation emission from grain boundaries. WIDE use of transmission electron microscopy and dislocation etch-pitting techniques has led to a growing awareness of the presence of dislocation substructures in annealed pure metals. Whereas much speculation'-4 has developed about the influence which subgrain structures have on the mechanical behavior of metals, particularly the yield strength, only limited experimental evidence correlating subgrain structures with lower yield strength has been presented. 2,3,5-7 It is the purpose of this note to present experimental evidence of the effects which grain boundaries and subgrain boundaries have on both the upper and lower yield strength of zone-refined iron. Effects due to high-angle boundaries formed upon recrystallization below the a-y phase transformation are compared with effects due to veining subgrain boundaries formed upon "recrystallization" above the a-y phase-transformation temperature. These effects are further compared with the reported influence 2,3,5-7 which low-angle boundaries have on the lower yield strength of bcc transition metals. EXPERIMENTAL PROCEDURE The starting material for these experiments was a 1-in.-diam zone-refined ingot prepared at Battelle Memorial Institute. Initial purification of electrolytic iron by vacuum-induction melting was improved by a floating zone-melting treatment in ultrapure hydrogen.' Chemical analysis of this zone-refined iron appears in Table I. Tensile samples of 50-mil wire were prepared by rolling and drawing portions of the ingot. An intermediate recrystallization anneal at 625°C after rolling to a reduction in area of 85 pct was carried out in an evacuated Vycor capsule (10-=5 mm Hg). Further reduction in area of 91 pct was followed by recrystallization in evacuated Vycor capsules at temperatures between 600" and 950°C, see Table 111. All samples

Jan 1, 1967

By Victor A. Phillips

A series of strips of a Ni-12.7 at. pct A1 alloy were Prepared containing cubical y'(NisAl) precipitates with edge lengths from 60 to 500A. A particle-free solution-tveated strip was included for cornparison. They weve cold-rolled 95 pct and the effects of particle size on the isochronal (1/2 hr) annealing behavior between 300° and 950°C studied (by hardness and light and electron microscopy). It ulas inferred that the particles deformed with the lnatvix becoming lamellae which remained coherent. Comparison with published data fov pure nickel showed that aluminum greatly re-tavded softening and recrystallization, but it made little difference whether or not particles were present. The presence of pakticles led to a heterogeneous distribution of precipitates after annealing at 700" to 750°C. Recovery was not detected. Recrystallization occurred by the growth of new grains into unrecrys-tallized material. In a previous study by the author,' the growth of Ll2-type ordered yl(Ni3Al) precipitates was followed in Ni-12.7 at. pct A1 alloy as a function of aging at 600" and 700°C. The particles were showo to be cubical in shape in all sizes from 50 to 3000A and remained coherent. This work was used as a guide in preparing the starting structures for the present study of the effect of these particles on the annealing behavior of heavily cold-rolled strip. Another question of present interest was whether dislocation and particle hardening were additive, since the structures before rolling ranged from solution-treated to peak-aged to overaged. Also, precipitation might occur on annealing after cold-rolling. Reference may be made to other papers2"5 for previous work in this relatively unexplored field and only some recent work will be mentioned her:. phillips2 studied the effect of deformable 0 to 590A-diam cobalt particles on a Cu-3.23 pct Co alloy rolled 95 pct and found that the particles, which rolled out into thin lamellae, impeded softening and recrystallization. Tanner and servi3 likewise studied the annealing of cold-swaged Cu-2 pct Co alloy containing 150A-diam particles and found impeding effects. Haessner et a1.,4 on the other hand, found that incoherent 2-p-diam non-deformable particles of B4C (0.04 vol pct) tended to increase the rate of recrystallization of copper rolled up to 95 pct reduction. They attributed this to the formation of new grains at the particle interfaces. Humphreys and artin' found that nondeformable silica particles in copper rolled to 30 pct reduction accelerated recrystallization if the particle spacing was large and retarded it if the spacing was smaller. Haessner et a1 4 also studied a rolled Ni-Cr-A1 alloy; however, the particles of y'(Ni3Al)-type precipitate were not put in before rolling, but separated during the isothermal annealing at 750°C. No previous work appears to have been carried out on the effect of y' (Ni3A1) particles on the annealing of Ni-A1 alloy. Hornbogen and ICreye7 redetermined the solubility c of aluminum in nickel as a function of temperature T and showed that it was given by c = 32.6 exp(-1940/RT). This relation gives aluminum solubilities of 15.1, 14.2, 12.0, and 10.7 at. pct at 1000°, 900°, 700°, and 600°C, respectively. The phase precipitated from the nickel-rich solid solution is fcc y1 (Ni3A1) which has a Cu3Au -type ordered structure8 and remains ordered up to 1000°C.B EXPERIMENTAL PROCEDURE The alloy used was identical with that used before. Chemical analysis showed 6.27 wt pct (12.71 at. pct) Al, the principle impurities being 0.065 pct Fe, 0.022 pct Co, 0.020 pct Cu, and 0.004 pct C. Bar stock of 1 in. diam was cold-swaged to % in. diam, cold-rolled to 0.300-in.-thick strip, and annealed at 900°C in dry hydrogen. It was cold-rolled to 0.100-in. thickness and solution-treated for 1 hr at 1000°C while sealed in a quartz tube in argon, quenching in iced brine with the aid of a device to snap off the nose of the tube. Lineal analysis gave an average grain size of 0.055 mm. Pieces of strip were aged at 700°C in vacuo for 30 min, 51/4 hr, and 1 week to produce nominal average particle widths of 60, 150, and 500A, respectively, as known from the previous work.' The average diamond pyramid hardness was determined. The heat-treated strips were rolled from 0.100 to 0.005 in., a reduction of 95 pct, and the rolled strips stored at about -5°C. Small pieces were annealed within 1 week for 30 min at temperatures from 300° to 950° ±2°C in a horizontal vacuum furnace. Strips were withdrawn into a cooling zone, giving an estimated initial cooling rate from 950°C of about 50°C per sec. Average diamond pyramid hardnesses were determined on a lightly electropolished spot on the surface of each strip using 300-g load. Each point on the softening curves represents a separate annealed specimen. Sections containing the rolling direction were examined by optical metallography. Selected specimens were electrothinned to the center plane' and examined by transmission at 100 kv in a Siemens Elmiskop I electron microscope. It is well-known that changes in the structure tend to occur when a deformed strip is electrothinned below a thickness of a few hundred angstroms, although this is less serious with a material such as nickel which has a high melting point, and also is apt to be less serious when particles are present. Observations were nevertheless confined to thicker regions of the foils with estimated thicknesses over 1000A. No changes were observed due to beam exposure.

Jan 1, 1968

By Michael Hoch, Seong Kwan Rhee

The ternary system Zr-Cr-0 was investigated at 1200°, 1500°, and 1700°C. The isotherms at these temperatures were determined by metallographic and X-ray diffraction analysis of carefully selected alloys. AS a part of a series of investigations1-4 of the ternary and quaternary phase diagrams on refractory metals and their compounds, the ternary system Zr-Cr-O was investigated at 1200°, 1500°, and 1'700°C. The binary diagrams Zr-Cr, Zr-O, and Cr-0 as reported by Hansen5 and Levin et a1.' and the existence of a ternary coompound ZrsCrsO (q-carbide structure a. = 11.96A) provided a good base for this investigation of the Zr-Cr-O phase diagram. MATERIALS The materials used and their suppliers were: Zirconium powder, 99.4 pct pure, Charles Hardy, New York; Zirconium dioxide, Fairmount Chemical Co., Newark, N.J.; Chromium powder, 99.85 pct pure, Fairmount Chemical Co., Newark, N.J.; Chromium sesquioxide, 99.86 pct pure, J. T. Baker Chemical Co., Pillipsburg, N.J. Though the materials used were not "hyperpure", the impurities present do not affect the results (lattice parameters, phase boundaries) within the experimental accuracy. EQUIPMENT AND PROCEDURE The detailed procedures and equipment used for this investigation were similar to those described elsewherel' "ith the exception that in this study an induction-heated argon-atmosphere furnace was used. The latter furnace was used to prevent the vaporization of chromium metal in samples in the higher temperature range (above 1200°C). The tungsten crucible was induct ion-heated in a vertical quartz tube filled with argon gas. The quartz tube was 1-1/2 in. in diameter and 10 in. long; it was connected at the top and bottom to water-cooled copper plates. The argon gas of a purity 99.995 pct was further purified by being passed through zirconium metal chips which were maintained at 800°C in a silica tube 1 in. in diameter and 30 in. in length. The furnace was flushed with argon gas for an hour before starting heating; during heating, a slight (3 cm oil) overpressure of argon was maintained in the system. Power was supplied by a 20-kw Ther-Monic Induction Generator. The samples rested on a tungsten-wire basket; the wire basket was connected to a tungsten wire which passed through the tungsten crucible lid, and entered the system on top through a Wilson-type seal. By pulling on the wire, the sample was removed from the crucible and dropped to the water-cooled copper base of the furnace. Because of the presence of argon gas, the cooling of the sample was even more rapid than in the vacuum furnace.' EXPERIMENTAL RESULTS AND DISCUSSION 1) Isothermal Section at 1200°C. The compositions investigated have been numbered within the phase diagram, Fig. 1, and all the pertinent information about the samples can be found in Table I. This table lists the composition of the samples, the phases present in the room-temperature diffraction patterns, the phases detectable in the microstruc-ture, and calculated lattice parameters of the a-zirconium phase. The shapes of the various phase

Jan 1, 1964