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By Paul M. Tyler

NOW that the dust of World War II has settled and we and our allies are faced with extravagant losses of men, money, and materials, virtually the only hope that the United States and Britain have in the way of reparations lies in the capture of industrial, technical, and scientific secrets. Even during the war American and British scientists and technicians gained access to German factories, questioned German personnel, studied German documents, and endeavored generally to keep pace with new discoveries in science, industrial technology, and process development. Under various agencies this work continued for two years after the war. Altogether at least 600 American scientists and industrialists have gone to Germany and brought back reports and several times as many British, Canadian, and. Australian investigators have been similarly engaged under co-operative arrangements designed to assure the maximum of coverage with a minimum duplication of effort. As a result of these investigations and document studies, about 500 or 600 reports have been prepared on metallurgical and allied subjects. Those by American authors or joint teams have been listed in the annotated Bibliography of Scientific and Industrial Reports, issued by the Office of Technical Services in the U. S. Department of Commerce. Many of the British reports are also available in this country through the same office or through a British representative in New York. Since it was my duty to read most of these reports for

Jan 1, 1948

Jan 1, 1942

By S. Senderoff, D. E. Couch

A PROCESS for the electrolytic preparation of molybdenum from molten salts has been described previously. This previous work centered on electrowinning and electroplating characteristics of the process. In this paper the properties of the process as a refining medium are discussed. In producing metals from ores, it frequently has proven most economical to obtain a comparatively impure metal by smelting, and to purify the product by electro refining. Direct electrowinning from molten salts is rather difficult when a porous diaphragm is required in the process, as in the case of molybdenum, since satisfactory refractory materials for such a diaphragm in molten salts have not yet been developed. In electrorefining, however, a soluble anode is used. By suitable control of anode and cathode current densities, the lower-valent molybdenum compound used in the electrolyte is not oxidized, and a diaphragm is not needed, thus avoiding difficulties which are encountered with other electrowinning processes. Electrorefining may result from two different processes in the cell: Dissolution of the molybdenum and the less noble impurities with a separation of the more noble impurities as an anode sludge; the electrodeposition of molybdenum and the more noble metals at the cathode, leaving the less noble metals in the electrolyte. The amount of separation which occurs in each process is determined by the potential of the operating electrode and the relative concentration of the various species at (or in) that electrode. Since molybdenum has a comparatively noble position in the EMF series in molten alkali halides,2 most refining would be expected to occur at the cathode. In this work only the cathodic process was studied. The objective was to determine to what extent various metallic ions, if they dissolve from the anode or are otherwise introduced, were concentrated in the electrolyte. The necessary conditions for the separation of each and the limiting concentration which may be tolerated in the electrolyte for effective refining were studied. The deposits were chipped from the cathode and analyzed spectrochemically for metallic impurities. Besides determining the major contaminant, a general qualitative analysis was obtained to be sure that other metallic ions were kept at a very low level during each series of runs and to be sure that the baths were not being contaminated accidentally. Samples of the bath, for analysis, were taken at the temperature of operation so there was no chance of selective crystallization during cooling. In this way the ratio of molybdenum in the bath to the other metal could be determined readily. These data permitted a check on the anode efficiency and any volatilization that took place during the electrolysis. Experimental Apparatus—The apparatus as shown in Fig. 1 was used to determine the effect of the various foreign ions upon electrodeposited molybdenum. The entry chamber A allowed the cathodes to be removed without cooling the bath and without allowing oxygen or moisture to enter." The cathodes were made Prom 0.25-in. tungsten rods and were rotated during the electrolysis. The balloon in the lower arm B was inflated with helium after the cathode was drawn up into the upper section for removal. A new cathode was then placed into the entrance chamber A after which the chamber was flushed

Jan 1, 1959

By A. B. Kinzel

IT is with sincere appreciation and a deep sense of responsibility that I accept the honor of delivering the Howe Memorial Lecture. In our time metallurgical research has delved into phenomena ever more complex in character, so that much of this work must be done by organized teams. We, of the Union Carbide and Carbon Research Laboratories and the Electro Metallurgical Co., are truly a team and the lecture which is to follow is due largely to a few of the outstanding members of that team here cited and well known to you in their own right: John Lamont, whose work deserves special recognition, Walter Crafts, William Forgeng, William Binder, Robert Fowler, and David Swan. Thus it is a fitting pleasure to accept this honor for the research institution which I represent. Henry Marion Howe was truly inspirational and his breadth of view was such that he could use either the method of rigid proof or implied mechanism to further the broad understanding. But perhaps his outstanding characteristic was his sound judgment and his ability to weigh observations. The following is replete with observations and judgment as to their implication. We would like to feel that it is the type of dissertation which Howe, himself, would have enjoyed. Chromium carbides in stainless steel have, in a sense, been a key to the progress of the stainless steel industry. Brearley's first stainless steel, containing approximately 0.30 pct C, was successful because it differed from previous Fe-Cr alloys in that the carbides were present in such amount and form as to provide the stainless and cutting properties. Again, the 12 pct Cr die steels with a carbon content of 1.5 pct or more achieved their properties by virtue of the form and distribution of the chromium carbides. In the straight chromium steels with from 12 to 25 pct Cr, chromium carbide amount and distribution are once more the determinants with respect to physical properties and corrosion resistance. In each of the cases just cited the role of the carbide is in essence similar to that of iron carbide in carbon steel and this story is so well known that we need not dwell on it. In the austenitic stainless steels, the chromium carbide plays only a minor positive role with respect to mechanical properties, and for corrosion resistance the objective is to achieve maximum homogeneity. Thus the tendency has been to ever lower the carbon and correlatively the chromium carbide content of the austenitic steels. Today stainless steels with carbon less than 0.03 pct are beginning to find their true place, and this is being aided in major degree by our Company's introduction of a new type of ferrochromium having negligible carbon. The role of carbon in these austenitic steels has long been recognized, and a truly enormous amount of research has been devoted to the subject. Much has been learned about corrosion resistance, but the attack on the problem from the point of view of carbide precipitation and the nature thereof has left much to be understood. Because of its fundamental importance to the future of stainless steels, further study of the mechanism of carbide formation in austenitic steels is of interest. In the 18-8 Cr-Ni steels, which are typical of the austenitic class of steel, carbon is soluble in the aus-tenite to the extent of approximately 0.15 pct at 1832°F (1000°C). The solubility becomes less with decreasing temperature, so that at 1652°F (900°C) the solubility limit is approximately 0.06 pct, at 1472°F (800°C) it is about 0.03 pct, and at 932°F (500°C) it is approximately 0.01 pct. Obviously this is the ideal situation for the classical precipitation phenomenon. It is true that, in a sense, 18-8 austenite resulting from annealing is in a metastable state, and the phenomenon of ferritic precipitation from this austenite should be considered. However, in a so-called fully austenitic 18-8 steel this is secondary with respect to the carbides and can be neglected. A wide variety of chromium carbides is known. Only one chromium carbide, Cr,,C,,, frequently referred to as Cr,C, has been found in unmodified low carbon 18-8 steel. This, fortunately, simplifies the study of the precipitation phenomena. For this study an A.I.S.I. type 304 stainless steel of commercial quality was selected. Analysis showed C 0.07 pct, Mn 0.49 pct, Si 0.33 pct, Ni 9.34 pct, Cr 18.91 pct, and N 0.033 pct. As expected with this composition the steel was homogeneous after annealing except for a few pools of ferrite, which were disregarded in that their location was not coincident with subsequent carbide precipitation areas. On corrosion testing the steel was normal and typical of good commercial quality. Specimens 1/2xlx4 in. were annealed and subjected to precipitation heat treatment for 100 hr at 100" temperature intervals from 1000° to 1500°F and for ten selected intervals ranging from 5 min to 64 hr at 1300°F. These blocks were then cut into small pieces for metallographic studies. The first problem

Jan 1, 1953

By A. Perry Thompson

I. GENERAL DISTRIBUTIONS APPEARANCE, AND RELATIONS MINING in Butte has seldom encountered covellite in commercial quantities. The notable occurrences, extending vertically and laterally perhaps several hundred feet, presented scattered, bladed lenses of this mineral in a matrix of quartz, pyrite, enargite, bornite, and chalcocite. But under the microscope covellite is seen to be widespread in the Butte ores, though in such small quantity that megascopic examination will not discover it. In early mining operations covellite was found in the Gray Rock vein, a member of the Blue vein system. As described by Sales,1 it persisted as an occasional ore mineral, associated with quartz, pyrite, tetrahedrite, bornite, chalcocite, and minor amounts of sphalerite, from the 700-ft. to the 1,200-ft. level of the East Gray Rock and Diamond mines. Crushed quartz-monzonite and later quartz completed the vein filling between

Jan 4, 1915

By George M. Fowler

DURING 1937 the subject of mining geology was probably given more attention and more mining geologists were usefully employed than at any previous time. Of the many contributing factors the most important were: (1) a higher degree of prosperity in many countries, (2) a. better understanding of geologic phenomena, and (3) the apparently diminishing reserves of several important minerals. Mining companies have come to look upon geology with a growing appreciation of its aid in the more effective exploration and exploitation of mineral deposits. Most of the larger and more active companies have one or more geologists permanently attached to their staffs and some have well organized and efficiently managed geological departments. Even the smaller companies, who feel they cannot afford to employ a geologist on a permanent basis, are seeking the advice of competent men in this field with increasing frequency. One of the most significant trends has been the growing tendency to base exploratory work on more thorough geologic studies instead of empirical "hunches,"on which so much off the work in the past has relied. Likewise, mining companies are apparently more willing to expend larger sums on the basis of geologic possibilities in a district.

Jan 1, 1938

By F. W. Glaser

Iron-silicon alloys have had a great influence, in many ways, in modern industry. Silicon steels have been used almost exclusively for the construction of electrical machinery, but have also become an important material for structures which benefit by the high tensile and yield strengths of this material. In elaborating on the early history of work done on iron-silicon alloys, Greiner, Marsh and Stoughton1 went back as far as 1808, and pointed to Berzelius as the first producer of ferrosilicon. During the last twenty years some very important contributions in the form of studies of the iron-silicon system, as well as of the physical properties of these alloys, have been published. In consideration of the brit-tleness and poor machinability of alloys containing more than 5-6 pct Si, commercial interests have stimulated the research done on iron-silicon alloys, but mainly in the range of 0 to 6 pct Si. Yensen2 has shown the influence of im- purities, such as carbon, sulphur and phosphorus on the magnetic properties of 2, 4, and 6 pct Si alloys. Corson3 extended his investigation of physical properties to approximately 32 pct Si, and attributed the brittleness of the high-silicon material to the particular constitutional features of the alloys. Though mentioned earlier in the literature, the effect of nitrogen on crystal growth and magnetic permeability of iron-silicon alloys has been demonstrated recently by Morrill4 and Rostoker,5 respectively. In all the above quoted investigations, except that of Rostoker,5 sand or chill casting processes were employed for the preparation of samples. A major advantage of the powder metallurgy process is that it does away with time-consuming machining in many applications. The powder metal industry is always interested in pro- ducing a finished product employing a material which has presented considerably greater difficulties in manufacture by other methods. Steinit26 described preparation and testing of various Fe-Si alloys which were produced by the powder metallurgy process for the manufacture of armatures for small electric motors or generators. While Steinitz investigated alloys up to 6 pct Si, Rostoker5 went as high as 9 pct Si. The author7 previously discussed the diffusion of iron-silicon compacts containing 6 and 10 pct silicon. It is the object of this paper to study the progress of diffusion occurring in iron-silicon alloys by electrical resistivity measurements. All samples were prepared by pressing and sintering of compacts. Iron, silicon, and Fe-Si powders of various mesh size and compositions were employed to obtain test samples. It was assumed that complete diffusion had been obtained when the electrical resistivity reached a constant value characteristic for that particular alloy. To this end, electrical resistance measurements were used to follow the progress of alloying under various conditions.

Jan 1, 1950

Jan 1, 1942

By W. T. Isbell

Although the pressure to meet the heavy demand for lead still took precedence over new metallurgical developments in the field of roasting, smelting, and refining of lead in 1948 there nevertheless has been considerable activity in the experimental development of new processes and improvements as well as plans for the modernization of many plants both here and abroad. Increasing labor and material costs have stimulated the trend to greater mechanization, revamping of flow sheets, and construction of larger units wherever possible. Although there have been many serious labor stoppages in the United States, Mexico, and Europe, labor supply has improved in most plants even if it has fallen off in efficiency.

Jan 1, 1949

By R. J. Stevens

THE Roan Antelope Smelter commenced operations in October, 1931. As originally designed, its equipment consisted of one reverberatory furnace, 120 X 25 ft, two Peirce-Smith converters 12 X 20 ft, and one straight line casting machine. Since that time the following additions have been made: One reverberatory furnace 120 ft X 28 ft (1934) One reverberatory furnace 95 ft X 28 ft (1943) Two 12 X 20 ft Peirce-Smith converters (1934 and 1938) One 13 X 30 ft holding furnace 6 (1938) One straight line casting machine and 2 ladle tilting quadrants (1934) The metallurgy of the smelting process is comparatively simple. However, there are several features of operation which are uncommon to most copper smelters: (1) The high grade of concentrate treated; this has always been about 50 pct copper. (2) The high flux burden on the charge. This is necessary because of the deficiency of bases'in the concentrate and the high alumina content of the concentrate. (3) The frequent necessity of adding coal to the furnace charge to control the matte grade. (4) The high grade of matte produced. This has led' to unusual converter problems. From the commencement of operations, the ore mined has come from the Roan Basin orebody. The concentrate produced from this ore consists mainly of chalcocite and shale with small proportions of other copper minerals. As mining operations extend to the Roan Extension orebody, the proportions of bornite and chalcopyrite in the concentrate will increase with a corresponding decrease in the copper content of the concentrate. Because of the concentrate grade the capacity of the reverberatory . furnaces in terms of tons of copper produced per ton of coal burned is high.. This ratio is usually over 2.2, and on especially favourable runs has reached 2.6. Reference to Table , shows that the iron content of the concentrate is unusually low. Only part of this iron is available for slag formation, the balance going to the matte. To make up this deficiency in bases, limerock is added to the furnace charge. This flux ensures a slag that is of the correct silicate degree, is sufficiently fluid, of low specific gravity, and it counteracts the thickening effect of the alumina present. An ample supply of flux is obtainable from Ndola, 2 2 miles distant by rail. Although the reverberatory slag has a high copper content, the slag fall is low and the copper loss in the slag now rarely exceeds 1.0 pct of the total copper charged. The blister copper shipped is of such purity that only one fire refining operation has been necessary to produce a wirebar with properties comparable to electrolytic copper. Bismuth has always been the most troublesome impurity and consequently the problem of its control in the finished product has been of prime importance. Practically none is removed in the reverberatory furnace. The bulk of the elimina-

Jan 1, 1947

Jan 1, 1889

By W. H. Adams

One of the most attractive subjects for technical writers is the gigantic industry of the manufacture of sulphuric acid. This is no doubt, natural when we take into account that it has grown in this country during the past twenty years, from a production of 60,000 tons in the year 1867, to that of nearly 450,000 tons in 1887. We may well excuse much of the literature which but repeats the same old story, as it serves to bring to the public notice, at proper intervals, the hidden resources of our land; and this constant application of essential truths will sooner or later be the means of freeing us from dependence upon the Old World for necessary chemical products. The present increase in manufacture of this acid in the United States is almost wholly from pyrites ores, which we have in unlimited quantities close at hand. The largest consumption of such acid is for treatment of other native products, petroleum, rock-phosphates, etc.; and, considering the knowledge we have gained during the past twenty years, it is safe to say that the industry is but fairly established, and the causes which have operated to place us in our present proud position are but natural incentives for a further growth and an increased consumption of the many other undiscovered or undeveloped resources of our American soi1. In one of his earlier editions Muspratt says: " It would seem that the manufacture of sulphuric acid, though as extensively carried on as any other business, yet seems to be the least understood; and the ignorance of some manufacturers appears to be only equalled by that of writers, who, in their description of the production of this acid, give figures of apparatus, and vaunt as improvements, things which have been exploded for years. It is possible to find in the works of eminent men drawings of apparatus, for the production of sulphuric acid, which never could possibly have worked one day—some, in fact, could never have worked at all."

Jan 1, 1888

By E. P. Klier, Taylor Lyman

THE structures formed when austenite is quenched to subcritical temperatures and allowed to transform isothermally have been the subject of intensive study since the work of Davenport and Bain.1 Isothermal transformation diagrams summarizing the results of many of these studies have become widely familiar to metallurgists. Of particular interest to metallographers are the dark-etching, acicular products of transformation formed by isothermal reaction below the temperature of maximum velocity of the austenite to pearlite reaction. These products, the bainite structures, can be formed in a wide variety of steels. However, the constitution of bainite is not well understood and divergent views have been expressed as to its mode of formation. In this investigation a combination of dilatometric, microscopic and X-ray methods has been brought to bear upon the problem in the hope of some elucidation of the bainite reaction as it occurs in hypoeutectoid steels. MECHANISM OF BAINITE FORMATION Davenport and Bain1 considered the mechanism of bainite formation to consist of two steps-an allotropic transformation followed by precipitation of carbide. The separation in time of the two processes was considered to be very slight in the upper temperature range and very marked at temperatures just above the martensite range. This concept has been restated by Vilella, Guellich and Bain2 in the form of a definition of the acicular mode of transformation as: The successive, abrupt formation of flat plates of supersaturated ferrite along certain crystallographic planes of the austenite grains; this supersaturated ferrite begins at once to reject carbide particles, (not lamellae), at a rate depending upon temperature. In effect, this is the acicular mode of transformation, even though the temperature be such as to limit the actual life of the quasi-martensite to millionths of a second. The investigation of isothermal decomposition of austenite in certain alloy steels (notably those containing chromium or molybdenum) has revealed that there may be a range of temperatures between the pearlite and bainite reactions in which the austenite decomposes at a relatively low rate.3-6 Further, it is characteristic that in the second region of fast reaction the decomposition of the austenite is incomplete by one reaction but goes to completion by a second reaction. These observations led Wever7 to a description of the bainite reaction as follows: I. The reaction takes place by initial precipitation of a martensitic intermediate structure. 2. In the upper temperature range this structure readily decomposes into ferrite and cementite. In the lower range carbon separates in an unknown form. 3. In the upper temperature range the precipitated carbide nucleates the precipitation

Jan 1, 1944

By Fred C., Bond

IN CYANIDE milling, little attention has been paid to the effect of the viscosity of the mill solution on the extraction speed. The viscosity of the solution varies with the amount of dissolved salts present as impurities. These salts build up to a maximum depending on the character of the ore, the grade of cyanide used, the lime and salts added, and the impurities originally in the water. The viscosity will change from month to month and week to week as these factors vary; and that this variation affects the extraction is unquestioned, although methods for calculating it are lacking. The character of the ore is probably the most important of the four factors, as the amount of minerals present that are soluble in cyanide solution will vary constantly, and each variation affects the viscosity of the mill solution. When the cyanide consumption increases as the character of the ore changes, the viscosity of the solution will increase and the extraction will decrease, for the cyanide consumption is usually a measure of the impurities dissolved from the ore. In other words, as the difference between the total and free cyanide increases the extraction will decrease, other factors remaining constant.

Jan 1, 1926

By AIME

PROBABLY no greater world traveler has ever been Chairman of one of the Institute's Divisions than Henry Frederick Hebley. To begin with, he was born almost as far away as possible-in Christchurch, New Zealand, Dec. 15, 1893. There he grew up, studying mechanical engineering at the local Seddon Memorial Technical College. Then he went over to Sydney, Australia, for a bit of work before sailing for the U.S.A. in 1915. After a few months as draftsman in a San Francisco office he moved over to Clarkdale, Ariz., in the engineering department of the United Verde copper smelter, which had just gone into operation. But the war was on, and Henry thought he belonged in France with the Canadian Engineers, the United States still remaining aloof from the conflict, and that was the last the copper industry saw of him. After almost two years in France he was wounded, convalesced in England and Canada, and then went back to his native New Zealand to design concrete factory buildings. But soon the United States called again, and this time he landed in Salt Lake City with the Oregon Short Line R.R. Co. Then to Chicago in 1920. where he really got into the coal industry for good, working for the Allen K Garcia Co. on the design and operation of coal mines, beneficiation plants, and combustion equipment; and joining the Institute.

Jan 1, 1946

By Arthur Forsyth

A SEARCH through the available literature shows that the cobalt-nickel-silicon system has not been systematically studied. This seems rather odd because all three elements are fairly abundant and have better than average corrosion resistance; however, they have high melting points, which makes experimental work difficult. Cobalt and nickel form a continuous series of solid solutions and each metal dissolves about 7.5 per cent silicon. Many ternary alloys have been studied and the results have been published in a great many different ways, but to present such data in a short but clear and understandable manner is still a problem. The following pages describe the results of the study of 76 alloys from which the partial ternary diagram (Fig. 1) of the cobalt-nickel-silicon system has been drawn. The alloys were chosen according to the plan in Fig. la by taking definite ratios of cobalt and nickel, such as 70 Ni, 30 Co or 40 Ni, 60 Co, and adding silicon in various percentages. Each section was studied in detail by means of thermal analysis and microscopic examination, but only two of these detailed sections were thought necessary in the point perspective drawing to give a comprehensive picture of the liquidus, solidus and solid transformations that take place over the temperature ranges studied. Complete thermal analyses and microscopic data are given in Table 1.

Jan 1, 1940

By JAMES J. PURDY

The great majority of stokers used in residential heating installations are of the clinkering type. Because of inherent characteristics of the under- feed combustion process as it occurs in these small stokers, and because of the wide range of operating conditions encountered in residential heating schedules, not all bituminous coals can be used successfully in residential underfeed units. The problem of providing consumer satisfaction has been attacked by the joint efforts of the stoker manufacturers and the coal industry; the stoker manufacturers have been concerned with improving their product to permit the use of a wider range of coals, and coal operators have made every effort to market selected and better prepared coals. In view of the wide range of physical characteristics and chemical properties of bituminous coals, the problems are real and are receiving increased attention.

Jan 1, 1949

"In the spring of 1927, six members of the American Institute of Mining and Metallurgical Engineers met for dinner at the Chemists' Club in New York to discuss the possibility of setting up a committee within the Institute to further the current interest in the science of steelmaking. Attention' to this subject had been crystallized by a symposium held by the Faraday Society in 1925. ' After a prolonged discussion, ranging from thermodynamics to slag conditioning, it was decided to approach the Institute with the request that a standing committee on "The Physical Chemistry of Steel Making" be set up. This committee proposed to promote scientific and practical papers on the subject, and was designed to cooperate with the Open Hearth Committee of the Institute in bringing scientific developments to the attention of open-hearth operators throughout the country... . "As the life of the [Physical Chemistry of Steelmaking] Committee lengthened and general interest in the technical phases of steelmaking grew, it became evident that there was a distinct need for a book that might serve the open-hearth interests to better advantage than standard texts whose scope is necessarily wide and whose detailed exposition of the open-hearth process is, therefore, somewhat limited. With this thought in mind, the Committee, after some years of consideration and debate, embarked on the venture of writing a manuscript on `Basic Open Hearth Steelmaking'." The foregoing paragraphs, taken from the introduction by C. H. Herty, Jr. to the first edition, well describe the circumstances which led to the publication of "Basic Open Hearth Steelmaking" in the spring of 1944. The book consisted of nineteen chapters contributed by twenty-three authors and edited by the staff of Alloys of Iron Research and T. S. Washburn, B. M. Larsen, and J. S. Marsh with Frank T. Sisco as consulting editor. The Engineering Foundation and the Open Hearth Steel Committee of the Iron and Steel Division, AIME, made financial grants; steel companies and other organizations supported the publication by contributing time and expenses of staff members in their capacity as authors or editors. The volume was sponsored by the Seeley W. Mudd Memorial Fund and appeared under the

Jan 1, 1951

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 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