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Part 1. Coal Part 2. Industrial Minerals

Jan 3, 1977

By Walter Harvey Weed

CONTENTS. [ ] INTRODUCTION. THIS paper deals with certain ore-deposits whose structural features or mineral contents (or both) result, directly or indirectly, from igneous intrusions and their after-effects. It is largely a discussion of contact metamorphic ore-deposits based upon the physical changes in rocks due to contact action. It involves a classification of ore-deposits only so far as is abso-

Jan 1, 1913

By Henry M. Rowe

Professor Ruff's most illuminating paper' describing his extremely valuable investigation of the carbon-iron equilibrium diagram assigns definite temperatures to certain very important lines in the diagram, viz.: the eutectic temperature EB (Fig. 1) and the " near-eutectic " temperature E'B', but without indicating clearly enough the reasoning which warrants these assignments. These temperatures are of such primary importance that it is well to indicate the apparent gaps in the reasoning, in the hope that they may be filled in. In his diagram, Fig. 1, the point X and the liues B'D'lII represent the experimental results reached by Ruff and Goecke;a AB, AEB, and SE represent the liquidus, the solidus, and the solubility of the carbon in solid austenite in the absence of graphite according to Gutowsky,3 AB being also in accordance with Spiecker's data; S'E' the solubility of carbon in solid austenite in the presence of graphite according to Ruer and Iljin;5 GS the line A3 after Ooerens and Meyer; 6 and EBC the true eutectic line as inferred by Prof. Ruff from Gutowsky's data. B'D' is the carbon content found in cast-iron which had apparently saturated itself with carbon in the presence of the graphite of the enclosing graphite crucibles in which the determinations were made. From its straightiiess and its sharp inflection near 6.67 per cent. of carbon, the carbon content of

Jan 1, 1913

By Edward H. Bzirdick

THE territory under particular consideration in this article comprises portions of La Plata and Montezuma Counties, situated in the southwestern corner of Colorado, and around the base of the La Plata Mountains. (See Fig. 1.) In southeastern Utah and northeastern Arizona there are several mountain systems whose origin and structure are practically identical with the La Platas so that ore occurrences found in the latter can be hopefully looked for in the former. With this assumption, there is an area around the laccolithic ranges which offers promise for a successful exploration for gold ores. Ore occurrences of the Silverton, Telluride, Rico, or Ouray Districts will not be discussed, although in these areas the Mesozoic sediments are more or less involved within the ore-bearing complex. These have been intensively studied and developed. The idea is to set forth what my mining experience has been within the largely unaltered . Mesozoic horizon which remains around the extreme bases of the La Plazas. This, until recent years, has been almost entirely neglected by prospectors and operators and, so far as similar territory in Utah and Arizona is concerned, so remains.

Jan 1, 1934

By Gordon MacVean

THE adoption of rock dusting, as a safety measure, has made notable progress in the West Virginia coal mines since May, 1925. At that time there were but two mines in the State that were thoroughly rock dusted, mines No. 2 and No. 12 of the Boone County Coal Corp., at Sharpless. Since then it is probable that 75 per cent of the coal operators in the State have given consideration at one time or another to rock dusting. This growth of interest followed the meetings of the various mining institutes all over the country, during the summer of 1925, at which papers were presented, drawing the attention of the coal mining operators to the merits of this safety measure. Yet outside of the experience with rock dusting at the Old Ben Coal Corp., of Southern Illinois, and the Carbon Fuel Co., of Rains, Utah, there had been no actual occurrence in the coal mines of the United States, which could be taken as positive evidence of the efficacy of rock dusting in the prevention of the propagation of coal dust explosions. The U. S. Bureau of Mines, however, had run innumerable tests under conditions which closely approximated actual coal mining conditions and had clearly shown that rock dusting was effective.

Jan 1, 1926

By H. M. Woodroffe, H. K. Conn, S. J. Rice

World production of asbestos is estimated to be at a current level of almost 3.5 million tons, having more than doubled in the past ten years. A substantial part of the increase has been due to a rapid expansion in the Soviet Union. Production from that country during 1964 is estimated at 1.5 million tons and, as a consequence, Russia has displaced Canada as the leading world producer. Although traditionally the asbestos mining industry has been centered near Sverdlovsk in the Urals, two new producing areas have been under development for some time. It is expected that a new mine will be in operation in 1965 near Kiembi, Kazakhstan, some 300 miles south of Sverdlovsk, and an- other mine at Aktrovak in Tannu-Tuva, west of Lake Baikal. These developments will provide a significant increase in the production capability of Russia. Although internal consumption is expected to increase with the addition of new asbestos- cement producing facilities now under construction in Russia, there is some speculation that exports will also increase.

Jan 2, 1965

By AIME AIME

QUALITY and size do not ordinarily go hand in hand, but there is good evidence that both these attributes reached a new peak at the Annual Meeting of the Institute in New York just concluded. Certainly, the total attendance of 2500 was far above any yet attained, as might be expected with the recent rapid growth of Institute member- ship. General comment indicates that the quality of the papers also was notable, though not measurable by so definite a yardstick as attendance. During the meeting 49 technical sessions were held, at which more than 250 formal papers were presented. In addition, there were some thirty special meetings of committees, Divisions, and other Institute groups. In reporting the Annual Meeting eleven years ago the statement was made that "unless the Engineering Societies should build for themselves a new building it is probable that no meeting can be larger," and "the fifth floor, where a buffet lunch is served each day, has reached its full capacity and it seems quite evident that any future development of Institute meetings must be along the lines of quality, not size." Unfortunately the angel to succeed Andrew Carnegie, who financed the building of the present home of the Institute 35 years ago, has not yet ' appeared. Even if some one would merely build another elevator or two in the present building it would help. Fortunately, the modern auditorium of the American Radiator & Standard

Jan 1, 1940

By M. C. Manderson

Abstract-The sharp drop in world phosphate demand that took place in 1975, due to temporarily high prices, now seems to be reversing itself. And prices for both phosphate rock and phosphate fertilizers, which declined dramatically from their 1975 highs, now appear to be bottoming out. This recent price weakness has delayed new mining ventures that had previously been planned for completion by around 1980. While there is ample capacity to supply near-term rock needs, the stage seems to be emerging for a better supply-demand and price environment in the late 1970's and early 1980's.

Jan 1, 1978

By Charles A. Thomson

RECENTLY a prominent Brazilian' doctor wrote to an American friend: "I feel that cultural relations between the American and Brazilian people could be promoted in a very speedy and effective way by establishing contacts between men of the same professions. . . . A Brazilian mechanical engineer could be immediately interested in relations with American colleagues, even if he had never heard of Longfellow and was not interested in Stokowski's orchestra. . . . A large number of cultural ties could be established between specific groups of men who have already some common interest, and who, whenever they meet, can do something that naturally brings them closer, that is, `talk shop."' In appointing a committee on Inter-American Engineering Relations to cooperate with the Department of State in its program of fostering cultural relations with the other republics of this hemisphere, the American Engineering Council has taken a step which should lead to a greater sense of unity and fraternity among engineers of the Americas. That such unity and fraternity are part and parcel of the moral defense of the hemisphere is obvious. For years engineers of the United States have been traveling South and South-east to construct roads and bridges, dam rivers, harness waterfalls, build ports, install and operate mining equipment, and erect buildings and plants, often at the risk of life. Those in the teaching profession in this country have had as pupils a growing number of students from our neighboring republics whom they have sent back home trained in the most efficient engineering methods. In a sense, however, these relations with the other nations on this side of the globe have been haphazard and left to chance. Personal acquaintance among engineers has played its role but no organized attempt appears to have been made to take advantage of the natural relationship which geographical and historical factors should encourage.

Jan 1, 1940

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

By Arthur Zentner

THE PAST YEAR saw important developments in all the main branches of zinc metallurgy, which can only be douched on briefly here. Vertical Retort Smelting-The New Jersey Zinc Co. reports their operations to be about as last year when the number of vertical retorts at the Palmerton plant was increased from 16 to 28. The first unit of eight vertical retorts at Oker, Germany, to treat the Rammelsburg complex ore was completed early in the year. A second unit has been under construction and is probably ready to start operations about this time. Each unit is rated for 10,000 metric tons of zinc per year. A plant of 40,000 metric tons annual capacity is the goal. A reflux plant was also built to make high-grade zinc. The plant program is being -carried forward with government finan¬cial assistance, as was the case with the electrolytic zinc plant at Magdeburg. Government subsidies cover mining and 'smelting, and allow for depreciation and reasonable return on invested capital, according to U. S. Bureau of Mines reports.

Jan 1, 1938

By A. H. Daane, B. J. Beaudry

The Sc-Y and Sc-Zr systems were studied by thermal and X-ray methods. Both systems are characterized by complete solid solubility in the low temperature hexagonal form and in the high temperature bcc form. In the Sc-Y system, there is a minimum in the solidus at 50 at. pct and 1365°C, while the solidus in the Sc-Zr system follows a nearly straight line relationship between the melting point of scandium and zirconium. There is a minimum in the temperature of transition from hexagonal to bcc in the Sc-Y system at 43 at. pct Y and 1175°C; while the temperature of transition is raised in the Sc-Zr system to a maximum of 1415 °C at 30 at. pct Zr. INTEREST in the metals of the first transition series has usually stemmed from their useful properties; however, there is now a great deal of interest in determining the fundamental nature of these metals. Since scandium is the first of these transition metals, a study of the preparation and Properties1 and the alloying behavior of scandium2 was initiated. In a continuing study of the alloying behavior of scandium, the systems of scandium with zirconium and yttrium have been established. Extensive solid solubility in both the Sc-Zr and Sc-Y systems was expected from application of the classical rules of Hume-Rothery. Also, the modified Darken and Gurry plot as suggested by Gschneid-ner3 showed ideal conditions for solubility in the Sc-Zr system with less favorable conditions in the Sc-Y system. The effect of scandium on the transformation temperature of zirconium and yttrium was of interest, since a recent empirical observation by Uly and Burr4 predicted that the solute scandium would raise the transformation temperature of zirconium and lower the yttrium transformation. In addition to noting the validity of the above predictions, the SC-Y and Sc-Zr systems were established. EXPERIMENTAL METHODS Materials. The metals employed in this investigation were crystal bar zirconium, distilled scandium prepared by the method described by Spedding, et al.1 and yttrium prepared by the method described by Carlson, et a1.5 The major impurities present in these metals are listed in Table I in ppm. Alloy Preparation. All the alloys examined were initially formed by comelting the two metals in a nonconsumable electrode arc-melting furnace under an atmosphere of purified helium or argon. The buttons were inverted at least five times and re-melted each time to ensure homogeneity. During preparation of Sc-Zr alloys, approximately 1 wt pct was lost which was attributed entirely to the loss of scandium by distillation. When preparing Sc-Y alloys, approximately 1.5 wt pct was lost, but it was assumed that the intended composition was maintained, since the relative weight lost when arc melting the component metals was nearly the same. Samples weighing 15 to 20 g were prepared for time-temperature thermal analysis, while only 1- to 2-g samples were prepared for the optical pyrometer and X-ray diffraction studies. Thermal Methods. The solidus and the melting points of the metals were determined by an optical pyrometer method described previously.2 The temperatures at which the transformation from hexagonal to bcc occurs were determined by differential thermal analysis. Several points on the solidus and liquidus in the Sc-Y system were also determined by this method and are in good agreement with those obtained by the optical pyrometer method. The procedure followed in the preparation of samples for thermal analysis and the furnace used have been described elsewhere.2'6 Since a limited quantity of scandium was available, most of the alloys were not melted during thermal analysis, thus avoiding contamination by the crucible. The alloy could then be reused and the composition changed by adding the desired quantity of solute to obtain the next alloy. Heat Treatment and X-Ray Methods. In order to ensure homogeneity, the "as arc-melted" alloys Were wrapped in tantalum foil, sealed in quartz capsules and heated at 1100°C for 15 hr and then cooled at a rate of 8 deg per min. Samples for X-ray diffraction were filed from these heat-treated alloys, sealed in 1/8 in. by 1/2 in. tantalum capsules under

Jan 1, 1963

By Robert M. Keeney

Important recent developments in the melting and annealing of non-ferrous metals include: 1. Melting of nickel silver in the vertical ring induction furnace. 2. Electric melting of stereotype metal. 3. The rotary-drum gas-fired brass melting furnace. 4. The low-frequency coreless induction furnace. 5. Finishing annealing of brass sheets with city gas1 replacing wood in the large brass-rolling mill. 6. Electric annealing of brass and copper tubing and sheets. 7. Replacement of oil by gas and electricity in the annealing of nickel-silver shells and stampings. Melting Nickel Silver in Vertical Ring Induction Furnace Although over 90 per cent. of the output of the brass rolling mills in the United States is now melted in electric furnaces,2 until recently a considerable part of the output of nickel silver has been the product of the pit fire. The application of the electric furnace to the melting of nickel silver has been slow for several reasons: (I) Until recently no lining has been available that gave a satisfactory life in the vertical ring induction furnace when melting nickel silver; (2) the rocking arc furnace so widely used in the foundry does not appear to have been favored by the rolling mill for melting nickel silver, possibly because the gases present may affect the quality of the alloy; and (3) the exclusive rights to the use of the high-frequency coreless induction furnace (which has proved very satisfactory for melting nickel silver) for the wrought brass industry are controlled by one concern. A little over one year ago the first vertical ring induction furnace to be used for melting nickel silver in the Naugatuck Valley was placed in operation. This was followed by two more in the same mill, and by

Jan 1, 1930

By M. D. Curran

AS applied to coal, the term processing is subject to many interpretations. To some it means preparation of coal for the market by mechanical means such as crushing, sizing, washing, or treating with oil or chemicals to eliminate dust or improve combustion quality. To others it means conversion of the coal to other commodities as in carbonization to produce coke and by- products, or to liquids by application of the hydrogenation process. I prefer to classify the various forms of mechanical treatment under the heading of beneficiation and apply the term processing to those methods of treatment that destroy the coal sub- stance through distillation or hydrogenation.

Jan 1, 1939

By J. H. Westbrook, R. W. Guard

The influence of a number of alloying additions on the structure and hardness of Ni3Al (?') has been studied. Three general effects have been observed.. solid-solution hardening, strain aging, and defect hardening arising from deviations from stoichiometry. The solid-solution hardening phenomena are complicated relative to binary terminal solid solutions due to the possibility of virtually independent substitution for the component elements and to the concomitant effects of strain aging. In many superior nickel-base high-temperature alloys the elevated temperature strength is attributable to the presence of a dispersion of Ni3A1 (?') in a solid-solution matrix. Examples of such alloys are Inconel X-550, Inco 713, Waspalloy, and Nimonic 80. It is, therefore, appropriate to seek a further understanding of the properties and alloying behavior of this compound. Ni3Al, the compound most rich in nickel in the nickel-aluminum binary system, was first detected by litakal but not established with certainty until the much later studies of Bradley and Taylor' and Alexander and Vaughan.3 More recently the mechanism of formation was clarified by Floyd4 who showed that Ni3Al is the product of a peritectic reaction at 1395°C between the melt and the compound NiAl in agreement with the original suggestion of Alexander and Vaughan.3 Ni3Al has the ordered face-centered-cubic or Cu3Au structure in which the nickel atoms occupy the face centers and the aluminum atoms the cube corners, a0 = 3.570A. Despite earlier reports to the contrary. the compound apparently remains ordered at least to 1000oC.5 It exists over a narrow range of compositions (-3 pct wide) whose limits and temperature dependencies thereof have been reviewed recently by Taylor and Floyd.' Most previous workers have found Ni3Al to be both hard and brittle7,8 although Maxwell and Grala8 obtained 2.5 to 6 pct tensile elongation at room temperature and Alexander and vaughan3 described the material as "hard and tough" on the basis of observations made while preparing metallographic specimens. In a recent study one of the present authors found that although considerable intergranu-lar brittleness was evident: individual grains of a coarse-grained inert atmosphere arc-melted specimen were readily deformable.l0 The same study also showed Ni3Al to have an anomalous temperature dependence of hardness in that such a curve exhibits a number of peaks between room temperature and 800°C which could not be associated with any microscopically observable precipitation reactions or polymorphic transformations. It was, therefore, proposed in the present study to elucidate the anomalous high-temperature strength behavior and to examine the solid-solution alloying of this compound and the effects of such alloying on hardness. Sample Preparation and Experimental Procedure-Samples, both of pure Ni,Al and of various alloyed solid solutions based on Ni3Al, were prepared by arc melting 100-g buttons in an inert atmosphere arc furnace. All buttons were heat treated for 4 hr at 1275oC and examined metallographically for homogeneity. Microstructures were typically homogeneous and single phase with ASTM grain size about 1 and unusually clean grain boundaries. Chemical analyses showed good correspondence (within a few tenths of a percent) with intended compositions. Microindentation hardness data were obtained from room temperature to 800°C in vacuo using a balanced-beam type loading system in an instrument to be described in detail elsewhere." In general a 100-g load, a loading rate of 1 mm per min and an indentation time of 15 sec were used. Various indenter materials were used according to the materials bein tested because of specimen-indenter interaction. Fl Measurements of the Vickers-type indentations were made at room temperature. Hardness-temperature curves were run at least twice on each sample to ensure that surface work-hardening effects had been eliminated." Precision lattice-parameter measurements were made on powder samples using a back-reflection

Jan 1, 1960

By M. D. Hassialis

THE object of a technical paper is to communicate new technical knowledge, the paper being the vehicle of communication and the existence of new knowledge its reason for being. It follows that the development of information worthy of communication, the criterion being novelty, is prerequisite to exercising the privilege of communication. The act of communication is achieved when the reader perceives the nature of the new knowledge, i.e., when he understands it. A paper achieving this objective is an acceptable technical paper. Development of new knowledge has as one of its purposes the increase of the existing state of knowledge and the enjoyment of the benefits derived therefrom. Technical knowledge is a collection of facts so ordered as to make apparent, relations existing between the facts. When the interrelations have been exposed the facts have been interpreted or explained Three broad, overlapping categories of technical papers may be recognized: papers consisting of (a) a report of facts, (b) an explanation of facts, or (c) a combination of a report and an interpretation. Ideally a technical paper should belong to one of the last two categories but current practice is to accept papers belonging to any of the three categories. Based on a small sample drawn from the scientific and engineering literature, the relative frequency of the three types is a: b: c:: 20:1:14. If the sample be limited to engineering literature, the ratios become a:c::2:1; type (b) being nonexistent. This large departure from the ideal is a consequent of the

Jan 1, 1948

By Milnor Roberts

WAR struck the mineral industry of Washington with cross currents that produced a peculiar result. The State's production of coal, industrial minerals, and metals for 1941, valued at $28,507,282, was increased in 1942 under war pressure to approximately $35.000,000. Meanwhile a tremendous demand had arisen for men to construct airfields and many other large projects for the Army and Navy in Washington and Alaska, and Government plants for the mineral industry costing $140,000,000 or more, as well as a call for employees in the U. S. Navy Yard at Bremerton, the sixty shipyards, the four Boeing airplane factories with many auxiliary shops, and hundreds of other plants turning out war materials. In spite of an influx of nearly 300,000 people, causing an increase of 17.1 percent in the population since 1940, according to the Census Bureau, the State clearly is still engaged in an unusual amount of war production in proportion to its population. A large proportion of the workers have been drawn from the mineral industry to the war plants, whether through motives of patriotism, high wages, or, in the Boeing plants at least, the glamour of the operation

Jan 1, 1944

By B. Egeberg, H. B. Smith

Britannia metal is a white alloy consisting primarily of tin and antimony, the tin greatly predominating. The alloy usually contains a small amount of copper and occasionally very small amounts of one or two other metals, such as bismuth, zinc, and lead. It is capable of being cold-rolled, it takes a high polish, and it is fairly noncorrosive; properties which make it a popular metal for many household and traveling utensils. Britannia metal is similar in many respects to pewter and has largely replaced pewter in the arts, but it should not be confused with that alloy, because pewter is essentially a tin-lead alloy, while Britannia is a tin-antimony alloy. In view of the fact that so little has been published concerning Britannia metal, the authors feel justified in presenting the results of their investigation, particularly since the behavior of this alloy under cold rolling and heat treatment differs so greatly from that of other metals and alloys. The old craftsman, engaged in the making of ornaments or tableware, heated the cold-rolled sheet metal or his finished product to a straw color corresponding to about 375" I?., claiming to produce thereby a harder and more rigid article. The fact that possibly led him to this heating was that a reheated article or sheet made from Britannia metal has a distinct metallic ring when struck a sharp blow, whereas an unheated article or sheet has a leady, dead note. No doubt he has associated the metallic ring with a greater rigidity and strength, and justly so, as will be seen later. The approximate analysis of the metal we investigated was 91 Sn, 7 Sb, 2 Cu, and the molten metal was bottom-poured into an iron mold yielding an ingot 7 3/4 in. wide by 11 in. long and % in. thick, the casting temperature being 800" F. The ingot was cold-rolled to a sheet 0.032 in. thick, sufficiently large samples for experimental purposes being cut from the sheet at intermediate stages. The samples were all tested for hardness with scleroscope and Brine11 machine, then heated to 212" F. for 30 min., and again tested after cooling to room temperature. The same samples were heated successively at 300°, 400°, and 440" F., followed

Jan 1, 1929

By H. B. Smith, B. Egeberg

Britannia metal is a white alloy consisting primarily of tin and antimony, the tin greatly predominating. The alloy usually contains a small amount of copper and occasionally very small amounts of one or two other metals, such as bismuth, zinc, and lead. It is capable of being cold-rolled, it takes a high polish, and it is fairly noncorrosive; properties which make it a popular metal for many household and traveling utensils. Britannia metal is similar in many respects to pewter and has largely replaced pewter in the arts, but it should not be confused with that alloy, because pewter is essentially a tin-lead alloy, while Britannia is a tin-antimony alloy. In view of the fact that so little has been published concerning Britannia metal, the authors feel justified in presenting the results of their investigation, particularly since the behavior of this alloy under cold rolling and heat treatment differs so greatly from that of other metals and alloys. The old craftsman, engaged in the making of ornaments or tableware, heated the cold-rolled sheet metal or his finished product to a straw color corresponding to about 375" I?., claiming to produce thereby a harder and more rigid article. The fact that possibly led him to this heating was that a reheated article or sheet made from Britannia metal has a distinct metallic ring when struck a sharp blow, whereas an unheated article or sheet has a leady, dead note. No doubt he has associated the metallic ring with a greater rigidity and strength, and justly so, as will be seen later. The approximate analysis of the metal we investigated was 91 Sn, 7 Sb, 2 Cu, and the molten metal was bottom-poured into an iron mold yielding an ingot 7 3/4 in. wide by 11 in. long and % in. thick, the casting temperature being 800" F. The ingot was cold-rolled to a sheet 0.032 in. thick, sufficiently large samples for experimental purposes being cut from the sheet at intermediate stages. The samples were all tested for hardness with scleroscope and Brine11 machine, then heated to 212" F. for 30 min., and again tested after cooling to room temperature. The same samples were heated successively at 300°, 400°, and 440" F., followed

Jan 1, 1929

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The microhardness of single crystals of tungsten disilicide has been investigated by the Knoop method. The average random room-temperature hardness of the WSi, matrix was 1350 kg per sq mm. Hardness crnisotropy was noted with respect to plane and indenter orientation as determined by single-crq.stal X-rny studies. Annealing at 1600" and 1800°C decreased the average hardness to 1310 and 1230 kg per sq tnm, respectively, and produced a second phase identified by X-ray diffraction and electron-microprobe analysis to be wSio.7. Ball-impact experiwzents produced rosettes at 850°C. Optical and electron microscopy showed evidence of slip and cross slip and twinning produced by microhardness indentations. Prismatic (100), [001] slip was found and cor~elated with hardness data. THE present study was undertaken to investigate the hardness anisotropy of as-grown and annealed single crystals of tungsten disilicide. The existence of the silicide WSiz in the W-Si system has been well-established and its structure thoroughly investigated zachariasen2 found WSi, to have a tetragonal C type of structure, similar to that of MoSi, with lattice parameters a = 3.212A, Kieffer et al. studied the W-Si system and measured the density and microhardness (at a 100-g load) of both polycrystalline WSi, and WSi,.,. The values found were 9.25 g per cu cm and 1090 kg per sq mm for WSi,, and 12.21 per cu cm and 770 kg per sq mm for WSi0.7, respectively. According to Samsonov et a1.5 the microhardness of polycrystalline WSi2 is 1430 kg per sq mm (at a 120-g load). EXPERIMENTAL The WSi, single-crystal boules investigated in this paper were grown by a Verneuil-type process using an electric arc by the Linde Division of the Union Carbide Corp.6 The largest specimens were 8 mm in diameter by 16 mm long. The crystals had an average density of 9.01 g per cu cm with a tungsten • silicon content of 99.9 wt pct. The major impurities were: 87 ppm O, 41 ppm N. 54 pprn C, 500 ppm Zr, 50 ppm Na, and 50 ppm Mn. The crystals were silicon-poor, the average silicon content being 22.20 pct (stoichiometric value is 23.40 pct), and tungsten-rich, the average tungsten content being 77.70 pct (stoichiometric value is 76.60 pct). As-received single crystals were ground and analyzed by powder X-ray diffraction technique using Cu Ka radiation. Laue and layer line rotation patterns were obtained on cleaved sections of WSi, single crystals. Electron-microprobe traverses of representative crystals were done using a Phillips-AMR electron microanalyzer. Carbon replicas were used to prepare electron micrographs. This work was done with a JEM-6A electron microscope. Prior to the metallographic examination, the specimens were mounted in Lucite and then polished for short times on polishing wheels using 9-, 3-, and 1-p diamond-grade pastes. Finally they were fine-polished with Linde A powder for 24 hr on a Syntron vibratory polisher. The samples were etched with 4H 2 O:1HF:2HNO3, which is a medium fast-acting etchant. The combination 1HF:2HNO3:5 lactic acid is also a satisfactory etchant. Annealing runs for selected specimens were made at 1600" and 1800°C for 3 hr at 1.0 to 3.0 x 10-5 mm Hg. A Brew tantalum resistance furnace with WSi2 powder for setters was used. The WSi2 powder was the same as that used for the crystal growth. Temperatures were measured with a calibrated W, W-26 pct Re thermocouple and a microoptical pyrometer. Powder X-ray diffraction, emission spectrographic, and electron-microprobe analyses were done after the annealing runs. For microhardness measurements a Tukon Microhardness Tester Type FB with a Knoop indenter was used. Although measurements were taken at loads ranging from 25 to 1000 g, the 100-g load was chosen as the standard load. All measurements were taken at room temperature. Only indentations of cracking classes 1 and 2 were considered.' DISCUSSION OF RESULTS Powder X-ray diffraction analysis showed the as-received crystals to be single-phase WSi2. Laue and layer line rotation patterns obtained on cleaved sections of WSi2 single crystals proved them to be tetragonal WS 2 2 The results also indicated that the c axis of the crystal was oriented parallel to the boule or growth axis. Electron-microprobe traverses across the matrix of the as-grown crystals showed them to be homogeneous WSi,. Optical and electron microscopy of etched crystals, however, revealed that they contained minute amounts of the "golden" and the "blue" second phases as opposed to the "white" or WSi2 phase. These two second phases were concentrated in inclusion and etch-pit

Jan 1, 1965