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By Charles W. Perry

The options of enhanced oil recovery, coal syncrude, and shale syncrude are compared by approximately equivalent economics. The physical constraints for the major enhanced oil recovery processes are described, followed by new estimates of cost. The range for all three options in terms of light syncrude equivalent are $22 to $40 per barrel in 1980 dollars.

Jan 1, 1982

By Zay Jeffries

HOSTILITIES in Europe, Asia, and northern Africa were responsible for dislocations in rare-metal supplies during 1940. Although the consumption of some of the rare metals is small the dislocations may be relatively large. In some cases these are advantageous to North America and in others they are disadvantageous. Specific instances will be cited later. Barium T HIN films of barium metal on special steel balls greatly improve the life and reduce the friction of rotating anodes in highly evacuated small X-ray tubes and make possible the operation of these anodes at relatively high temperatures. These remarkable results are described in an article by Atlee, Wilson, and Filmer in the Journal of Applied Physics for September, 1940. Oil could not be used because of the high temperatures on the one hand and its volatility on the other. Fig. 3 shows diagramatically the rotating anode and the method of coating the steel balls with barium. The letters K.I.C. refer to "Kemet Iron Clad." The K.I.C. wire was mounted so that the barium could be evaporated by direct passage of the electric current. At high temperatures the barium dif-

Jan 1, 1941

By Joe B. Alford

Jan 1, 1971

By Goerge F. Weaton

Since 1909, when an agreement between Minnesota's Tax Commission and the University of Minnesota's School of Mines was worked out, it has been the annual responsibility of the School to evaluate and classify the iron ore deposits within the State. These unique duties of an academic institution have provided School officials with an excellent view of the past, present and probable future of the mining industry in Minnesota as the average grade of iron ore (excluding taconite) * diminishes while at the same time it competes with beneficiated taconites and foreign high-grade ores for use in America's eastern blast furnaces. SYSTEM OF EVALUATION In the latter part of November of each year, the Mining Division of the Department of Taxation makes a preliminary study of the active mines which the Department wants the School of Mines to review. These are discussed with the engineers of the Ore Estimate Division of the School of Mines and with the mining companies. After these discussions, a list of the mines of each of the major operating companies is submitted to the Ore Estimate Division of the School of Mines with the request that these properties be reviewed by them as of the next assessment date (May 1st). At the same time, a letter is sent to the mining companies requesting that they submit to the Division their own estimates on the selected mines operated by them, together with all computations, drill records, maps and cross-sections. The mining companies are re- quested to send in this information during the first half of the year, and, as far as is possible, they have always complied with this request promptly. Much of this information received by the School of Mines is of a confidential nature and is treated as such.

Jan 1, 1965

By George H. Deike

DURING the past year a survey was conducted by the Committee on the Promotion of Student Interest in Coal Mining to determine whether the program as laid down in past years was operating effectively. It is a source of satisfaction and pleasure to be able to report considerable headway among operating companies in putting cooperative scholarship plans into operation. In previous committee reports the pioneer work along this line by Eugene McAuliffe, president of the Union Pacific Coal Co., has been cited. That Company now has in its employ, in responsible positions, three men who received their education under such scholarship plans. One student under a similar plan is now studying at the Colorado School of Mines.

Jan 1, 1942

By Joseph P. Hodgson

JOSEPH P. HODGSON.-As to ".Safety First," I did not deal with that, but I will say that in 1913, the number of .men killed was nine, and that year the "safety first" program was commenced; the next year, 1914, the number was reduced to five. In 1915, I am pleased to say that the number was reduced to two in the Copper Queen's entire property, and we have none so far this year. THE CHAIRMAN (G. F. G. HERMAN, Bisbee, Ariz.).-I can say, further, that we have from eight to nineteen men per month incapacitated for more than 14 days. Those are classified in this State as serious accidents. The number of men injured has apparently increased, -but that is clue to our improved method of recording and classifying accidents, no matter how slight. C. W. GOODALE, Butte, Mont.-The importance of cooperation among the members of the staff of an industrial organization is well brought out by Mr..Hodgson's paper.

Jan 12, 1916

By R. S. Handy

THE properties of the Patiño Mines and Enterprises Consolidated, Inc., a New York corporation, are near Llallagua in the department of Chayanta in the west central part of Bolivia, South America, about 80 miles southeast of Oruro and 250 miles southeast of La Paz, the largest city in Bolivia and its virtual capital. The properties are accessible by railroad from three points on the west coast-from Mollendo, Peru, across Lake Titicaca, from Arica by way of La Paz, and from Antofagasta, Chile. The latter route, although the longest, is recommended by the companies as affording a more gradual introduction to the high altitudes; the mine being 13,000 ft. above sea level. The company operates its own railroad from its properties at Uncia to Machacamarca on the Chile & Bolivia R. R., a distance of 60 miles. This railroad is well equipped and well operated, and its location among the mountains surrounding Uncia represents excellent engineering skill. In fact all of the railroads, although they are of only a meter gage, are remarkable for the excellence of their construction, the arrangement of their dining and sleeping cars and the precision of their operation. There is only one drawback to rail- road and hotel accommodations and that is the absence of heating facilities, which does not seem to affect the natives but keeps a tenderfoot's teeth chattering continually. The company is a consolidation of the Patiño company, owning properties at Uncia, with the Compafiia Estanfera de Llallagua, a' Chilean corporation owning contiguous properties at Llallagua. Before the consolidation these companies were deadly enemies, and there still remain at the surface plant at Uncia the fortifications and underground defences provided during the warfare between the two factions. Also, in the Azul, or "Blue" tunnel at the junction line between the two properties is a strong steel barricade still bearing marks of the bullets fired during the various armed tilts between the workmen of the two companies. The headquarters for the mining operations and the milling plant have been moved since the consolidation from the original location at Uncia to the Llallagua side of the mountain, where the Chilean company's operations were carried on. The historic old town of Uncia, with its massive stone buildings of Spanish design, is a wreck, while the Llallagua side is being rapidly built up with modern structures.

Jan 1, 1929

By William J. Robinson

What is the cumulative rate of recovery of copper from a sulfide leach dump? The technical answers to this frequently asked question may vary from "I don't know" to "quite good" from people of the same company. Management also poses this question because it plays a vital role in planning future production. The answer is difficult because of the many variables between different operations such as physical construction of the dump, topography of the original site, characteristics of dump material, mineralization, and water application. Each of these factors and others have a bearing on the rate of recovery. Anaconda's method of water distribution at Butte is unique in that each dump is drilled to allow physical injection of water into the dump. The injection holes are drilled vertically on 25-ft centers from the surface of the dump [(Figs. 1 and 2)]. Normally, the holes are drilled 40 ft deep and cased with 4-in. PVC perforated pipe. The pipe is perforated at 1-ft intervals with four 1 -in.-diam holes at 90° spacing on the pipe circumference. Formerly, shallow holes (20-40 ft) were alternated with deep holes (80-180 ft) in an effort to cover the entire dump and hasten oxidation. The shallow hole depth varied according to the compaction thickness. The deep hole depth varied according to the height of the dump and the original ground profile. It is preferable to have the deep holes end 20-30 ft above the original ground level. This generally allows penetration of the coarse material at the bottom of the dump. Deep holes had to be discontinued in order to cover more

Jan 1, 1974

W. L. SaundeRs, New York City (communication to the Secretary*):—Notwithstanding the sweeping statements made by Mr. Clarke in this paper, the friends of compressed air are not dismayed. There is no war between electricity and compressed air. Each one has its field of usefulness, and in that field each is supreme. In spite of commercial interests, in spite of prejudices and the enthusiasm of the inventor, the thing that is best will survive and flourish. At least ten years ago, our engineering papers contained large advertisements and pages of reading-matter about the application of electricity to mines, recording the introduction of numerous rock-drilling plants, and claiming that the problem had been solved, greatly to the advantage of the miner and with promise of large profits to the manufacturers of electrical apparatus. Edison and Thomson labored to apply electricity to mines, and each believed that the probabilities of success were great. This was the period of the solelloid rock-drill, which mas admirably suited, theoretically, to the percussive principle and in the development of which hundreds of thousands of dollars have been spent without satisfactory result. I have searched in vain for a standard mining equipment where electric rock-drills are in constant, commercial operation. During a recent trip made from New York to California, I visited most of the important mines of the West and failed to discover a single electric equipment, so far as this class of mining-work is concerned. If any one will inform me where there exists today an electric-drilling equipment in constant service in mines in the United States, I shall be glad to receive the information. Mr. Clarke has been for some years an active and intelligent writer on the subject of electricity for mining. Whenever his

Jan 1, 1904

By LUIS EAIYLNN SALAS

IF the ordinary wet method be attempted for silver-bullion containing tin, much trouble is experienced, varying with the amount of tin present. Even with a percentage as low as 0.05, the end-point is masked by a persistent turbidity, while with amounts ranging from 0.5 per cent. upward, the determination of the exact end-point is impossible, owing to the finely divided or colloidal metastannic acid resisting all efforts to cause it to settle, or to give a clear supernatant liquid. The object of the following experiments was to seek a remedy for these difficulties, and to find the conditions whereby the Gay Lussac method might be applied directly to these bullions. Material containing tin is met with frequently in bullion from Mexico or Bolivia; and tin is carried (sometimes in large quantities) in jewelers' sweeps. 1. A bullion was prepared containing Ag, 74; Cu, 25; and Sn, 1 per cent. A weighed amount was treated by the humid assay-method as if it were an ordinary bullion free from tin. Ten cc. of HNO3 (1.21) was added, and the bottle was heated until all traces of red fumes had been expelled. Before heating, the solutions were moderately turbid; and after heating, the turbidity greatly increased. One hundred cc. of normal NaCl solution was added and the bottle was shaken vigorously at intervals during 30 min. The turbidity persisted. The bottle was allowed to stand over

Mar 1, 1912

By ALFRED T. BARR

In certain areas of the New Cornelia pit, considerable secondary blasting is necessary to reduce oversized boulders, formed from primary blasting, to pieces which will pass the 41/2-cu yd dippers on the shovels. Some of the boulders are 'dobied, but when time permits they are blockholed and blasted. In most instances one hole drilled to a depth of 2 to 3 ft and blasted with 1/3 to 1/2 of a stick of powder will break a boulder satisfactorily. Blockholing is normally done by using a jackhammer of the 55-lb class, 1-in. round drill steel, and detachable steel bits, 2-in. gauge when new. A bit change is usually made after the completion of each hole. The use of light drilling equipment in blockholing is desirable, both from the standpoint of safety and ease of doing the work, and when it was seen there was a possibility of using a lighter jackhammer through the use of tungsten-carbide bits and at the same time get at least the same drilling efficiency as with the standard equipment, it was decided to test tungsten-carbide bits. The claims for long life of the bits and footage drilled before resharpening gave hopes of eliminating much of the delay time in changing bits which is unavoidable with the use of steel bits. and thus gain in actual drilling time.

Jan 1, 1949

By T. Sterry Hunt

WET processes for the extraction of copper from its ores have of late attracted much attention, especially in Europe, where the use of oupriferous iron-pyrites as a' source of sulphur prevails. These processes present an additional interest, when, as is often the case, the copper-ore's to be treated contain one or both of the precious metals, since the complete separation of these from copper, either in the dry or the moist way, is, as is well known, one of the difficult problems of metallurgy. The principal wet processes hitherto in use for the extraction of copper from its ores, may be included under three classes : I. Those in which the copper in snlphuretted ores is rendered soluble in water by calcining them, after a preliminary roasting which removes the greater part of their sulphur, with a portion of common salt, by which the copper is converted into a chloride (Long-maid and Henderson), or with sulphate of soda, by which sulphate of copper is formed (Monnier). Allied to these is the method by which a portion of the copper is got as soluble sulphate by roasting without addition, a process which is sometimes modified and rendered more complete by re-roasting the lixiviated residues with the addition of a portion of raw sulphuretted ore (Bankart). II. Those methods in which free chlorhydric or sulphuric acid is used to dissolve the copper- from oxidized or roasted ores. These, while simple and efficient, are too costly, except in certain localities where chlorhydric acid is a waste product. Related to them is the plan which consists in exposing the oxidized and moistened ores to the slow action of sulphurous acid mixed with air, by which a soluble sulphate of copper is formed. It has been proposed to decompose the solutions of sulphate or chloride of copper by sulphuretted hydrogen, thus separating the copper as sulphide, and using the liberated acid to dissolve fresh portions of oxidized copper. It is, however, the almost universal practice to throw down the copper from its solutions, however obtained, in the metallic state by the use of iron, either scrap-iron or iron-sponge; although in some instances

Jan 1, 1882

By T. Sterry Hunt

Jan 1, 1882

By Philip Bucky

THE term "longwall mining" is best known to coal men, although modifications of the method are continually being used in other fields. Longwall mining is of interest today because it makes for greater mecha-nization and better supervision at the working face, and therefore lower production costs and increased safety. It is an approach to the factory system of production, the high efficiency of which as compared to that in mines is well known. There is available an accumulation of experience regarding this work but coordination of experience is lacking and this series of experiments was undertaken to help serve this purpose. Model experiments were used for reasons of safety, cost and time, and because it has been previously shown1,2,3 that a scalar model built of the same material as the prototype will behave in a manner similar to that of the prototype, with time effects the same, if the effective weight of the model is increased in the same proportion as its linear dimensions are decreased. This is accomplished by substituting a centrifugal for the gravitational field; i.e., placing the model in a centrifuge and controlling the strength of the centrifugal field by varying the rate of rotation. Many factors affect the behavior of the geologic material overlying a bed, therefore results and conclusions contained in this paper apply only to the conditions presented herein.

Jan 1, 1938

By S. D. Strauss

The marketing of nonferrous metals and of the ores and concentrates from which these metals are recovered is a fascinating trade, international in character, sensitive to every change in the economic tide, and complex in its organization. Each individual metal has its own marketing mechanism; no two are exactly alike. The differences sometimes are a matter of tradition rather than of necessity, but usually they have developed because of the very nature of the problems of producing or consuming the individual metal. This description, because of limitations of space, can do no more than indicate the major aspects of the trade and touch lightly on the marketing structure of each metal. The dictionary states that a market is a "meeting of people for selling and buying." In the case of nonferrous metals this meeting may occur on a half-dozen different occasions between the time the ore has been first mined and the time the refined metal is available for use by industry; or it may not occur at all until after the metal itself has been rolled, drawn, stamped, cast, or forged into a useful semifabricated shape. To illustrate: A Chilean miner may sell his small ore production to a custom mill, which produces concentrates that are sold to an ore dealer, who finances shipments of the concentrate to a custom smelter, which buys them for conversion into blister, to be subsequently refined into electrolytic copper (sometimes by a refinery having no corporate ties with the custom smelter) and sold. Conversely, aluminum production is mostly by integrated concerns that mine bauxite, convert it to alumina, smelt that to produce aluminum, and then fabricate that into semifinished or even finished products before title to the material changes hands for the first time. Some nonferrous ores are not converted into metal at all but are sold by the miners or dealers directly to the ultimate consumers. A good example would be chrome ores used by the chemical industry. And of course a substantial part of the commerce in nonferrous metals is in scrap, which is the reconversion into useful form of metals that have long since been mined and smelted. Thus, one-third of all the lead used in the United

Jan 1, 1964

By S. D. Strauss

The marketing of nonferrous metals and of the ores and concentrates from which these metals are recovered is a fascinating trade, international in character, sensitive to every change in the economic tide, and complex in its organization. Each individual metal has its own marketing mechanism; no two are exactly alike. The differences sometimes are a matter of tradition rather than of necessity, but usually they have developed because of the very nature of the problems of producing or consuming the individual metal. This description, because of limitations of space, can do no more than indicate the major aspects of the trade and touch lightly on the marketing structure of each metal. The dictionary states that a market is a "meeting of people for selling and buying." In the case of nonferrous metals this meeting may occur on a half-dozen different occasions between the time the ore has been first mined and the time the refined metal is available for use by industry; or it may not occur at all until after the metal itself has been rolled, drawn, stamped, cast, or forged into a useful semifabricated shape. To illustrate: A Chilean miner may sell his small ore production to a custom mill, which produces concentrates that are sold to an ore dealer, who finances the shipments of the concentrates to a United States custom smelter, which buys these' concentrates for conversion into blister, which is subsequently refined into electrolytic copper and sold. Conversely, much of the production of aluminum is in the hands of integrated concerns that mine bauxite, convert bauxite to alumina, smelt the alumina to produce aluminum, and then fabricate the aluminum into semifinished or even finished products before title to the material changes hands for the first time. Some nonferrous ores are not converted into metal at all but are sold by the miners or dealers directly b the ultimate consumers. A good example would be chrome ores used by the chemical industry. And of course a substantial part of the commerce in nonferrous metals is in scrap, which is the reconversion into useful form of metals that have long since been mined and smelted. Thus, one-third of all the lead used in the United

Jan 1, 1959

By G. P. Moore

BOLIVIA still remains among the oil countries that have proved oil acreage but no production which is being marketed. No steps have been taken during the past year to provide facilities for transport of Bolivian oil to market nor are any known to be contemplated for 1930. The only active operator to date is the Standard Oil Co. of Bolivia, subsidiary of the Standard Oil Co. of New Jersey. The potential production from completed wells is practically unchanged from the 1928 figure of 6000 bbl. daily. As far as is known, there has been only one completion during the year 1929. This is the Machareti well, which is about 50 km. north of Villa Montes along the road to Charagua. The well is reported at about 250 bbl. daily initial production. The gravity of the oil is not known but is presumed to be about 40" Bé., the average for the region. The Standard Oil Co. of Bolivia has five strings working on various parts of its concession. No new locations have been made definitely. Company Activities There was no change in the situation of American holdings in Bolivia during 1929. The oil rights of an English company, acquired under a special colonization contract with the Bolivian Government, are being negotiated in New York and may mean the entrance of another of the large American oil companies in Bolivia. The Sucre Syndicate sold its holdings to the Standard Oil Co. of Bolivia during the past year. .A local company called the "Aguila Doble" was formed during 1929 to drill a well or wells near the town of Cochabamba on structures mapped by a local geologist. It is reported that the Government is buying about one-fourth of the capital stock of this company for 500,000 Bolivianos (about $180,000). The company has not yet raised sufficieht funds to buy drilling equipment so that no operations have been started. According to the statements published in La Pas, this company has acreage on seven anticlinal structures near Cochabamba. This area lies about 8500 ft. above sea level on the eastern Hank of the Andes Moun-

Jan 1, 1930

By S. J. Hruska

Rate expressions for the formation of two-and three-dimensional nuclei on foreign substrates are developed, taking into account previously neglected contributions to the standard Gibbs free energy of formation of critical nuclei. The temperature dependence of critical super saturation data predicted using these expressions is in accord with data for cadmium on copper and sodium on CsCl. EXPERIMENTAL data on the heterogeneous nuclea-tion of metal crystals from the vapor phase1&apos;2 exhibit the temperature dependence predicted by a nucleation rate equation derived by Pound et al.3 In their treatment, the critical nuclei are visualized according to the Volmer4 model as cap-shaped (three-dimensional). Accordingly, it seems desirable to compare these data with a nucleation rate equation which is derived on the assumption of disk-shaped (two dimensional) nuclei. Further, Lothe and Pound5 have recently shown that the standard Gibbs free energy of formation of these critical nuclei contains a contribution which has heretofore been neglected. Thus it is necessary to re-examine these nucleation data using a rate equation which contains this contribution. The van&apos;t Hoff isotherm relates n(i), the concentration of nuclei of critical size i (i = number of atoms), to nil), the concentration of adsorbed single atoms: where standard Gibbs free energy of formation of critical nuclei given by is temperature insensitive and is the bulk free energy change/volume of transformed material], T = substrate temperature and k = Boltzmann&apos;s constant. Previously,3 was determined by considering only the contributions of bulk and surface free energies in transforming i atoms from the population nil) to a cluster of i atoms. It has been shown5 that this procedure does not take into account the free energy contribution arising from the multiplicity of sites, q, where the clusters can be situated. If this contribution, -kT In q/n(l),is added to iG3 [Note that this increases n(i) by a factor q/n(l).] Since the above does not affect the remaining terms in the rate expression of Pound et al., the details are referred to their paper. The resulting nucleation rate is If the experimental AGV and T values at some common value of are employed, a plot of vs T(ln C3/l + In p&apos;) should yield a straight line of slope k/B<p and intercept . The corresponding plots for / = 1 nucleus per sq cm sec and C3 = 1018 are shown in Figs. 1 and 2 for cadmium on copper1 and sodium on CsCl2 and the values of obtained therefrom are entered in Table I. It is apparent that the data yield reasonable straight lines with about the same scatter as found using the equation of Pound et al. When the configuration of minimum free energy for a nucleus is a circular monatomic layer, the standard free energy of formation is

Jan 1, 1963

By Ernest F. Burchard

A Reconnaissance of the manganese- and chrome-ore deposits of Cuba was made by the writer, as a representative of the U. S. Geological Survey, in company with Mr. Albert Burch of the Bureau of Mines, under instructions of the Secretary of the Interior, in the spring of 1918. The Cuban Government courteously detailed Sr. E. I. Montoulieu, a mining engineer connected with the Treasury Department, to act as escort and associate throughout the work on the island. The object of the study was to obtain authentic information for use of the United States Government as to the location, character, quantity, and availability of the manganese- and chrome-ore deposits in Cuba. Accordingly, the work comprised examination of such deposits as seemed to be of promise, without regard to stage of development, with a view to a determination of the quantity and quality of ore likely to become available for shipment during 1918 and 1919, and of the tonnage of ore in reserve. Wile it was possible to visit most of the deposits that seemed to be of promise, there was not sufficient time to visit all that were brought to our attention, some of which may have merit. Moreover, the necessity for paying particular attention to the ore deposits and the mines precluded the possibility of making more general studies of the geology of the region, and of making satisfactory collections of country rock and of fossils, and so for other details as to the geography and geology of Cuba the reader is referred to the report by Hayes, Vaughan, and Spencer.l Mr. Burch returned to the United States about 10 days in advance of the writer, who continued, in company with Sr. Montoulieu, investigations of reported deposits in Pinar del Rio, Matanzas, and Santa Clara Provinces. On his arrival in Washington, Mr. Burch submitted to the Director of the Bureau of Mines a summary of the results of the work to date. Later the writer published, as Press Bulietin 190. 380 of the U. S. Geological Survey, a statement concerning the chrome and man-

Jan 1, 1920

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.&apos; 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