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REPUBLIC STEEL CORP. and Armco Steel Corp. have joined in a $160,000,000 project for the production of iron ore from Taconite in the Lake Superior mining region. The two companies announced acquisition in equal shares of 100 pct ownership of the stock of Reserve Mining Co., which controls a vast deposit of magnetic Taconite iron ore on the eastern end of the Mesabi range in Minnesota. Through Reserve Mining the two companies will build a plant for manufacturing high grade ore from Taconite near Beaver Bay on the north shore of Lake Superior. The first announcement calls for about a $60,000,000 plant which will be built as soon as plans are completed and will have an annual capacity of about 2,500,000 tons of iron ore pellets. Longer range development plans call for future expansion of the plant to provide an annual capacity of 10,000,000 tons. This will amount to an additional investment of

Jan 10, 1950

PHILIP L. GILL, New York, N. Y. (written discussion*).There is one feature of the fire-refining of electrolytic copper which I believe should be mentioned when the relation of oxygen content to the "pitch" or "set" of refined copper is under discussion; that is, the segregation of impurities. Variation of "pitch" or "set" is frequently noted in castings of different shapes, cast at the same time from the same furnace, though the oxygen content remains identical. For instance, it is possible to cast two wire-bars in the same shaped molds from the same ladleful of copper, the one 2 in. thick showing a good level set, the other, 4 in. thick, being overpoled. Also, when two bars are cast of the same weight and at the same time from the same furnace, one bar in a copper mold at the proper temperature, the other in a mold that has been allowed to get overheated, the bar in the hot mold will show

Jan 8, 1918

By Frank Foote

PRECISION lattice-constant measurements have been widely used in the study of cubic solid solutions but as yet have been rarely applied to noncubic solid solutions. (See, however, references I and 2.) With the high precision at present attainable in the measurement of lattice constants, the X-ray method should be readily applicable to noncubic solid solutions. In the work reported here, hexagonal close-packed magnesium was used as the solvent and either lead, bismuth or gold as the solute. In the magnesium-lead and mag-nesium-bismuth systems the a and c lattice constants were determined as a function of composition, densities were calculated from these lattice-constant data, these theoretical densities were compared with those directly measured and the solid solubility limit was determined on quenched specimens over a considerable range of temperature. In the magnesium-gold sys-tem, the solid solubility is very small but we have obtained an indirect check on the solubility limit previously reported.

Jan 1, 1940

C. H. BIERBAUM,* Buffalo, N. Y.--I agree with Dr. Merica that the eutectoid has a distinct effect upon the alloy and also that, as yet, it is difficult to say at just what point this eutectoid occurs or the conditions under which it appears; that is, the percentages of copper, tin, zinc, lead, and the other elements together with the temperature of pouring and the rate of cooling that is necessary; all seem to have a contributing effect. Some authorities, Law for instance, gives it as 9 per cent. of tin, yet under certain conditions I have found it with a lower percentage of tin to copper contents than that. The hard delta and the soft alpha crystals are both necessary for a bearing alloy; the one supplements the other. I am not inclined to think that phosphorus has any effect upon the eutectoid forming. The phosphide, PCu3, forms in and around the delta but is and remains distinct and separated from it. Etching with ferric chloride and then with nitric acid shows this very distinctly; it darkens the eutectoid and the other parts and leaves the phosphide bright. The rate of cooling determines the size of the crystals and the eutectoid together with their distribution and orientation. It is possible to chill the alloy to such an extent Where no eutectoid appears. I think it has been positively demonstrated that only an alpha and a beta appear. when this copper-tin alloy has been poured between two polished ingots

Jan 1, 1919

By Charles P. Williams

DURING the fall of the year 1873, attention was redirected to the occurrence of lead ores in Southwestern Arkansas (chiefly in Sevier County), and somewhat extensive explorations of the deposits have since been made in the hope of finding the ores sufficiently argentiferous to be profitably worked. How far the expectations have been realized I am not authentically advised, but samples of the galena ore, yielding 62.09 per cent. of lead, gave on assay at the rate of 15 3-10 ounces of silver to the ton of ore. This was the highest result obtained by myself, though I am informed that higher yields have been obtained by others. Among the samples of ores from this locality, forwarded to me in January last, was one specimen which I at once recognized as stibnite, and, on notification, other specimens of the same from Sevier County were forwarded me. The first specimen of the several received contained 11.51 per cent. of gangue, 57.62 per cent. antimony, 4.57 of bismuth, with small amounts of arsenic and iron. The latest result from a portion of another hand specimen I append in full, with duplicate estimations of the arsenic, bismuth, and gangue. The analyses were all conducted by Mr. C. R. Winters, under my direction, and in the case of those given below the ore was separated as closely as possible from the gangue before analysis. The results are for the mineral freed from hygroscopic moisture, and are as follows:

Jan 1, 1875

By Harold Cook

Discussion of the paper of HAROLD EARLE COOK, presented at the New York meeting, February, 1916, and printed in Bulletin No. 110, February, 1916, pp. 375 to 400. ALBERT SAUVEUR, Cambridge, Mass.-I think we must all agree with Lieutenant-Commander Cook when he says that there is a great deal of room for improvement in the annealing of steel castings and that better results would be attained if the annealing were conducted in closer agreement with scientific requirements. Whether even a carefully annealed steel casting can ever be made the equal of a steel forging of good quality is still a debatable question. Nevertheless, we all realize that very greatly improved results can be attained by careful annealing. Lieutenant-Commander Cook refers to some requirements calling for annealing steel castings above the Ac1 point. He is undoubtedly right where he says that this should be the Ac3 point. Take, for example, a steel casting containing, say, 0.35 per cent. of carbon, having a very coarse structure made up of coarsely crystalline ferrite. If this is heated just above the Ac1 point the ferrite remains, of course, just as it was before, while the pearlite is converted into a solid solution, austenite. Upon cooling, all this austenite is again converted into pearlite, or sorbite, while the coarse structure of the ferrite remains unchanged and the annealing has accomplished very little. It is therefore surprising that the requirement of annealing above the Ac1 point should appear, in these specifications.

Jan 5, 1916

By H. B. Charmbury, D. R. Mitchell

Recovery of fine coal from solids reporting to wash water has become increasingly important. These solids range from about 28 mesh to 0 and constitute 3 to 7 pct by weight of the feed tonnage to a coal preparation plant. In the past they were usually wasted to streams, but present clean stream legislation makes it necessary to remove them from the wash water and, if economically possible, recover the associated coal as a saleable product. Where these solids are not wasted to streams or to slime ponds they are recovered by thickeners and filters. Since filter cake is often high in ash or sulfur, or both, it is not readily marketed or used. Common practice is to mix it with other plant products, generally slack or cleaned run-of-mine. Uniform blending is difficult, not only because the impurity is usually high, but also because during certain operating periods it is possible to get a concentration of this filter cake in a railroad or barge. At some plants filter cake has been derived from the froth flotation clean-up of Dorr thickener underflow. The operating circuits required for a froth flotation plant make this a comparatively high-cost treatment, and in the last few years experiments have been carried out with bulk oil methods. These also are quite expensive and lend themselves only to special situations. Table I gives some characteristics of thickener underflows for plants in the Pittsburgh area treating Pittsburgh seam coal. It will be noted that there is a concentration of impurities in the -200 mesh sizes.

Jan 1, 1960

By W. C. Winegard, C. J. Simpson

BNINGESSNER et al.1 have shown that the solidification substructure in dilute cadmium alloys persisted after repeated deformation, recrystallization, and annealing treatments. On the basis of this and similar evidence, Whelan has suggested in a recent publication' that the solidification structure might affect the mobility of grain boundaries even after primary re-crystallization. This suggestion is important, since the technique used by previous investigators3-5 to fabricate grain growth specimens consisted only of casting, deforming, and recrystallizing prior to the grain growth anneal. Usually no attempt was made to homogenize samples with prolonged annealing. Experiments. To test the Whelan hypothesis, grain growth experiments were performed with samples in which the degree of solute segregation was altered by controlling the solidification rate of the alloys. The initial experiments were performed on the Pb-Ag system. Alloys containing 0.01 at. pct Ag were produced from 99.9999 pct Pb and 99.999 pct Ag. Cylindrical samples, 40 cm long and 12 mm in diam, were solidified in graphite-coated Vycor tubes by lowering them through a vertical furnace at varying rates with the furnace power settings constant. Six-centimeter sections were discarded from each end, and the 28-cm section from the center was cut into sections 25 mm long for grain growth experiments. These samples were deformed with the aid of a drophammer to a uniform thickness of 5.7 mm. After almost instantaneous recrystallization, the samples were given a grain growth anneal for various times at 260°C in a salt bath. Experimental results are shown

Jan 1, 1970

By P. R. Sperry

In an investigation of the decomposition of the solid solution in a cold worked high-purity aluminum alloy containing 7 pct Mg, aged at temperatures from 30o to 82°C, the nucleating sites at the earliest stages of precipitation were observed to be of two types. Nucleation occurred at the high angle grain boundaries both when the alloy was initially cold worked and when solution annealed. Nucleation also occurred at certain unique deformation markings which began to appear in abundance at approximately 30 pct reduction in thickness by cold rolling. These deformation markings were identified as deformation (kink) bands rather than as the usually assumed "slip planes." Zn material that was cold rolled 15 pct, only the grain boundary Fig. 2—A1-7 pct Mg alloy, cold worked 60 pct and heated at 230° C for 5 min. Etched with Perryman's reagent. X500. Reduced approximately 25 pct for reproduction. (a) Bright field illumination, precipitate deeply pitted. (b) Phase contrast, showing slip markings.

Jan 1, 1962

Department of Conservation and Development, State of North Carolina, Raleigh, N C H J Bryson, State Geologist. The latest list of publications will be sent upon request. Of the many Bulletins, Economic Papers, Circulars and Volumes issued by the Department of Conservation and Development, the following are available and relate to mining and geology of the state ? Bulletin 18, Bibliography of North Carolina geology, mineralogy and geography (1909), 50 cents, 21, The Gold Hill mining district (1910), 15 cents, 22, Report on Cid mining district (1911), 15 cents, cloth 75 cents, 25, Zircon, monazite and other minerals, 15 cents, cloth, 75 cents, 28, Limestones and marls, 15 cents, 29, Kaolins of North Carolina, 50 cents, 31, Deposits of brown iron ore, 50 cents, 32, Magnetic iron ores, 15 cents, 33, The Deep River coal field, 50 cents, 37, Pyrophyllite deposits, 35 cents A series of the Economic Papers review the mining industry in North Carolina for the years cited Those now available are Economic Paper 23 (1908-1909-1910), 10 cents, cloth, 50 cents, 49 (1913-1917), 20 cents, 55 (1918-1923), 25 cents, 60 (1924¬1925), 15 cents, 63 (1927-1928), 25 cents. Other available Economic Papers on geology and mining are No 3, Talc and pyrophyllite deposits (1900), 25 cents; 58, Oil prospecting well near Havelock (1927), 5 cents, 59, Oil-bearing shales of Deep River Valley (1927), 10 cents Available volumes on geology. Vol 1, Corundum and the basic magnesian rocks (1905), 35 cents, cloth, $150, 5, The Cretaceous formations of North Carolina (1923), cloth $1 75

Jan 1, 1933

Michigan State Department of Conservation, Lansing, Mich The Department of Conservation has two divisions issuing publications which should be listed in this directory. Geological Survey Division. R. A Smith, State Geologist Land Economic Survey Division L R Schoenmann, Head. A price list of publications of either division will be sent upon request to that division Geological Survey Division.-Citizens of Michigan may obtain publications of this Division on payment of forwarding charges Prices to others for available publications are given below: Vol 5 (1881-1884): Pt 1, Geological report of the Upper Peninsula of Michigan, by L L Hubbard, pt 2, Geology of Lower Michigan with reference to deep borings, by A C Lane, $125. Annual Report for 1908. Pt b, Geological section of Michigan, by A C. Lane and A E Seaman, 50 cents. Publication No 5, The Late Glacial and Post Glacial Uplift of the Michigan Basin, and earthquakes in Michigan, by W. H

Jan 1, 1933

By R. G. Fenish

THE B-Ni system was chosen for this study because of the great interest being shown in boron-fiber-strengthened composite materials. Boron fibers were obtained from Texaco Experiment, Inc. They average 4.2 mils in diam with a 0.5-mil tungsten wire in the center. In order to make the diffusion couple, the fibers were included in the nickel matrix by electroforming. The samples were placed in a preheated furnace for the desired temperature and length of time. Sectioning and polishing the samples revealed concentric rings as shown in Fig. 1. The average penetration distance, X, was calculated by measuring the radius of the second phase (the white shell in Fig. 1) and subtracting the original radius. The second phase was identified as NiB by X-ray diffraction. This allows the kinetics of the formation of the phase NiB to be calculated by Eq. [I], which is taken from Hoffman:"

Jan 1, 1967

By P. Barnes

(Read at the Wilkes-Barre Meeting, May, 1877.) THESE furnaces are of the ordinary Siemens type, and present no special peculiarities of construction. The bed of each is 8 feet by 20 feet clear inside of the walls and ports. The producers are placed at a distance of about 200 feet from the furnaces, and the gas is collected in an iron tube and led across the yard overhead. It then drops underground into the gas flue, and is distributed to the furnaces. A considerable weight of floor-plates over the valve-pits is included in account 39, but none of the general stock of floor-plates for the mill were charged to the furnaces. In Table No. 1 is shown the money cost of the furnaces as distributed to the several accounts named. In Table 2 is shown the proportion of each account due to each of the several items or classes of expenditure named.

Jan 1, 1878

By Charles Catlett

An examination of the census reports' for 1880, which contain a large number of complete analyses of typical American iron-ores, indicates that the existence of barium sulphate in intimate association with iron-ore is rather unusual. Of 94 analyses reported there, but four show any barium sulphate, and the maximum content amounts to 3.04 per cent. The note of the occurrence of considerable quantities of barite in connection with certain iron-ores found in the Pinar del Rio Province of Cuba may be of interest. These deposits are found near the little village of Francisco, about 25 miles west of the city of Pinar del Rio on the Western Railroad of Havana. The principal ridges are anticlines, and consist of very thick deposits of sandy shales and slates containing a large number of little veins of white quartz, which, by the gradual disintegration of the mass of the material, is left covering the surface. This quartz occasionally shows sulphide, but is generally barren of any such indication. At times lenticular masses of a more or less pure limestone mere observed in these slates. The shales, which are of light color, are occasionally talcose. The formation would tentatively be classed as the Lower Cambrian, arid the heavy ridges of comparatively horizontal limestone found in the anticlinal valleys as the Upper Cambrian. Along the crest of these slaty ridges deposits of iron-ore are found which are apparently in place, and were probably formed by replacement of masses of limestone similar to those noted elsewhere. The ready disintegration of the slates, arid the

Jan 1, 1908

By G. K. Dumbauld, B. E. Morgan

A satisfactory well-cementing composition must retain its fluidity long enough to be pumped into Place; then it must develop within a reasonable length of time sufficient strength and impermeability to anchor the casing in position and to form an effective seal between the casing and the formations. These properties may be evaluated by pumpability, strength (compressive or tensile), and permeability tests. Laboratory test procedures for the determination of pumpability time and strength development have been outlined previously and are readily available,1 but a satisfactory and convenient laboratory procedure for the measurement of the permeability of set cement has not been developed heretofore. some permeability data have been obtained previously by passing air through dried cement specimens.2 such a procedure is unsatisfactory because the drying of set cement alters it physical and chemical properties and subjects it to conditions dissimilar to well conditions. A more realistic method would be one wherein the cement remains water-saturated durin

Jan 1, 1952

By P. B. Barton, P. M. Bethke, R. O. Rye

Rhyolitic welded-tuff wallrocks of the epithermal base and precious metal veins of the Creede district were pervasively altered by the addition of more than two billion metric tons of potassium some 1.5-2 million years before mineralization. Sodium, calcium and magnesium were strongly depleted, yielding a nearly binary quartz + potassium feldspar assemblage containing as much as 13 weight percent K 0. This large-scale metasomatism, originally noted by Steven and Rattle (1965), took place progressively by initial alteration of plagioclase phenocrysts to orthoclase or microcline followed by alteration of the groundmass feldspar to orthoclase and gradual change of the sanidine phenocrysts to more Or-rich compositions. Oxygen isotope and chemical studies show that the metasomatism resulted from the interaction of the tuffs with deeply circulating heated ground water and suggest that the potassium metasomatism of rhyolitic rocks is the facies equivalent of propylitization of volcanic rocks of more basic composition.

Jan 1, 1985

A letter has been received by the Secretary of the Institute from Mr. C. W. Purington, Honorary. Secretary of the. American Committee of Engineers in London, whose offices are at 6, Copthall Avenue, London, E. C. 2, which will be of interest to any member who may be intending to go to England. Mr. Purington says: "A Committee of Americans has been formed here, consisting mostly of Mining Engineers, and those interested-in mining and allied industries. We should be very glad, among other duties, to give assistance to any American engineers arriving in England on official business connected with the war. This assistance would probably take the form of offering advice and hints as to saving time in approaching British official Departments, and generally in getting. about." This Committee of Engineers was organized with the approval of the American Ambassador to Great Britain, who has recommended its services to the United States Government in connection with the conduct of the war.

Jan 7, 1917

By A. N. Holden

A DISLOCATION mechanism has been described by Cottrell' by which metals can yield locally, I. form Liiders bands, giving rise to a characteristic stress-strain curve with a sharp yield point and appreciable strain at constant or decreasing stress. It is undoubtedly the best mechanism that has been suggested to date." In its present development, however, the dislocation mechanism provides a more satisfying explanation for the sharp yield point than for the extensive localized flow occurring at the lower yield stress. The primary objective in this paper is to extend the dislocation mechanism to account for localized cataclysmic flow by a dislocation collision process and to give experimental evidence to support such a process. Only the yielding of iron containing carbon -will be discussed, although other metal-solute systems are known to behave similarly. Cottrell Mechanism In brief, Cottrell explains the yield point in the following way: The dislocations in iron which must propagate to produce slip usually lie at the center of local concentrations of carbon atoms, since segregation about these dislocatlons relieves some of the local stress resulting from them. A dislocation surrounded by a "cloud" of carbon atoms is thus anchored, and a higher stress is required to set it in motion than to move a free dislocation. Considering all available dislocatlons to be anchored in this fashion, the iron exhibits a yield point when the first dialocations break free and move through the lattice causing slip. This first breaking away of a dislocation enables other dislocations to break loose by "interaction" and the process becomes a cataclysm producing local deformation or Luders bands. The yield point in the stress-strain diagram for iron is absent in freshly deformed material, but returns gradually with time; the phenomenon is one aspect of what is called strain aging. The rate at which the yield point returns following straining depends on the temperature of aging. According to Cottrell the rate of return of the yield point in strained iron is limited by the rate of diffusion of carbon at the aging temperature, the mechanism is onr: of reforming the solute atmospheres around carbon-free dislocations that had stopped moving coincident with the removal of stress. If the specimen is retested immediately after straining and unloading, carbon will not have had time to diffuse to, and re-anchor, dislocations and the yield point will not occur. The carbon diffusion limitation for the rate of strain aging apparently applies if the criterion for strain aging is either the change in hardness" or the change in electrical resistance" of the strained speci- men with aging time. The possibility exists, however, that the yield point actually returns to strained iron at some rate other than that deduced from hardness or electrical resistance data. Therefore, as a preliminary experiment, the rate of yield point return in a rimmed sheet steel strained 6 pct in tension was measured at 27°, 77°, and 100°C. A plot of yield-point elongation for each of these temperatures against aging time appears in Fig. 1. The aging process is described by curves which rise to a plateau value of elongation that seems independent of temperature, but at a rate that depends on temperature. Very long times lead to a further rise in the yield-point elongation above the plateau value. However, if the later increase in yield-point elongation is ignored and the log of the time to reach half the plateau value of elongation is plotted against 1/T, a straight line results for which an activation energy of about 25 kcal pel- mol may be assigned. Within the accuracy of this sort of experiment this is approximately the activation energy for the diffusion of carbon in iron (20 kcal per mol), and the carbon diffusion limitation suggested for the yield-point return on strain aging is valid. The Cottrell mechanism thus explains in a qualitative manner the occurrence of a yield point in iron and its return with strain aging. It fails, however, to explain some of the other experimental observations that have been made of the yielding behavior of iron. For example, it is known that the yield point in iron becomes less pronounced with increasing grain size. Annealed single crystals of iron have very small yield-point elongations .if indeed they have any,' compared to a polycrystalline steel. If the only requirement for a yield point is that the dislocations in the lattice of the annealed. material be anchored by carbon atoms, the difference in the behavior of single crystals and polycrystals is not explained. That a dislocation mechanism may be entirely consistent with little or no yield point in an annealed single crystal will become apparent later when dislocation interaction is discussed. Strain aging produces a definite yield point even in single crystals. This accentuation of the yield-point phenomenon in single crystals after strain

Jan 1, 1953

By A. L. Pranatis, G. M. Pound

Changes in length of copper foils of varying thickness and grain size were measured under such conditions of low stress and high temperature that it is believed that creep was predominately the result of interboundary diffusion of the type recently discussed by Conyers Herring. The surface tension of copper was calculated and results confirmed previous work within the limits of experimental error. Under the assumption of viscous flow, viscosities were calculated as a function of temperature and grain size. Predictions of the Nabarro Herring theory of surface grain boundary flow were borne out fully and the Herring theory of diffusional viscosity is strongly supported. ONLY a relatively few techniques for obtaining the surface tension of solids are presently available. Of these, the simplest and most straight forward is the direct measurement of surface tension by the application of a balancing counterforce. Thin wires or foils are lightly loaded and strain rates (either positive due to the downward force of the applied load or negative if the contracting tendency of surface tension is sufficiently greater than the applied stress) are observed. By plotting strain rates against stress, the load which exactly balances the upward pull is found and a simple calculation yields a value for the surface tension. The technique is of comparative antiquity, and solid surface tension values were reported by Chapman and Porter,' Schottky; and Berggren" in the early part of the century. Later, the filament technique became fairly well established as a method for determining the surface tension of viscous liquids, and Tammann and coworkers,'. " Sawai and co-worker and Mackh howed good agreement between the values of surface tension for glasses and tars obtained by the filament technique and by more conventional methods. With the increased confidence in the technique gained in these experiments, the method was applied to solid metals and the first reliable values of surface tension of solid metals were reported by Sawai and coworkers10' " and by Tammann and Boehme." More recently, Udin and coworkersu-'" have reported the results of experiments with gold, silver, and copper wires. Similar experiments with gold wires were carried out by Alexander, Dawson, and Kling.'" The excellent review articles of Fisher and Dunn" and of Udinl@ should be referred to for detailed criticism of the foregoing work and for discussion of underlying theory. In all the foregoing calculations, it is assumed implicitly that the material contracts or extends uni- formly along the length of the specimen and also that it flows in a viscous fashion, i.e., that strain rates are proportional to stress. For an amorphous material, such as glass, tar, or pitch, the assumptions are quite valid and good agreement is obtained with values of surface tension measured by other techniques. The values reported for metals, however, are occasionally regarded with misgiving, since it can be argued that, because of their crystalline nature, true solids can not deform in a viscous fashion. If this is true, then the results reported for solid metals over a long period of years are of only doubtful value. Thus it is clearly necessary that a mechanism be established that would explain both the viscous flow and the uniform deformation that has been assumed. Such a mechanism has been proposed by Herring."' Briefly, he suggests that, under the conditions of the experiment, deformation takes place by means of a flow of vacancies between grain boundaries and surfaces. This is a direct but independent extension of the theory proposed by Nabarro" in an attempt to explain the microcreep observed by Chalmer~.In a condensed form the Herring viscosity equation is TRL there 7 is the viscosity, T the absolute temperature, R and L grain dimensions, and D the self-diffusion coefficient. In its complete form, all constants are calculable and it includes such factors as grain shape, specimen shape, and degree of grain boundary flow. When applied to existing data, good agreement was obtained between predicted and observed flow rates. The theory received provisional confirmation from the work of Buttner, Funk, and Udin" who observed viscosities in 5 mil Au wire much higher than those in the 1 mil wire used by Alexander, Dawson, and Kling.'" More significant were the completely negligible strain rates found by Greenough" in silver single crystals. Opposed to these observations were those of Udin, Shaler, and Wulff'" who found indications of viscosity decreasing as grain size increased. Thus, complete confirmation of the theory was lacking in that the data to which it could be applied contained only a limited number of grain sizes. Hence, it was proposed that a series of experiments be carried out with thin foils of varying grain size up to and including single crystals, where, according to the Herring theory, deformation would occur only at almost infinitely slow rates.

Jan 1, 1956

By J. Brett, S. Friedman

A study of the diffusion of nickel into both fibrous and recrystallized 0.065-in.-diam silica-alumina doped tungsten wire at 1200°C has been conducted. The diffusion profiles were determined by chemical dissolulion of successive circumferential layers and spectro-photometric determination of nickel in the etchant. It was shown that the diffusion of nickel into tungsten is markedly structure-sensitive. No significant amount of nickel could be introduced at 1200°C into tungsten which had first been recrystallized at temperatures of 2300°C, leading to an upper limit estimate for the bulk diffusivity of nickel in tungsten of 10-11 sq cm per sec at 1200°C. However, nickel did diffuse into initially fibrous wires, caused re crystallization, and was alsays present at the advancing recrystallization front. The accumulation of nickel in an initially fibrous region ceases when the recrystallization front arrives. The characteristics of the resulting diffusion profiles are explained in terms of the relation between diffusion processes and micro structural changes. WHILE it is well-known that the presence of nickel and certain other metals causes low-temperature recrystallization of the cold-worked fibrous structure of doped tungsten,''' the character of the phenomenon is not well understood. Recently it was shown that the recrystallization reaction can be induced at low temperatures by the presence of solid nickel on the surface of doped wire, but not by exposure to nickel vapors.3 Once recrystallization was initiated, a continued source of nickel was required for propagation of the recrystallization front. The phenomenon appeared to be a complicated solid-state reaction since, in addition to the change in structure of the tungsten from fibrous to equiaxed grains, diffusion of nickel from the surface into the recrystallized and fibrous structures was occurring with possible chemical reaction between nickel and tungsten at the surface and interaction of nickel with the dopants which ordinarily stabilize the fibrous structure within the wire. The objective of the present work was to study the diffusion of nickel into fibrous and recrystallized tungsten structures in order to clarify the relationship of the diffusion process to nickel-induced recrystallization. Studies of interdiffusion in the Ni-W system4"7 have been principally concerned with the mobility of tungsten in nickel. Information on diffusion of nickel in tungsten is meager, and there seem to be no studies of the mobility of nickel in tungsten which elucidate the structural aspects of the phenomenon. The present experiments were designed to determine the diffusivity of nickel at 1200°C in fibrous tungsten, in large-grained tungsten prerecrystallized at high tem- perature, and in tungsten recrystallized at 1200°C due to the presence of nickel. Although the concentration profiles were determined in these experiments, unexpected changes in boundary conditions or complex diffusion paths complicated the analysis of these profiles so that the interpretation could not be readily expressed in terms of simple diffusivities. EXPERIMENTAL PROCEDURE The experiments were conducted on Sylvania 0.065-in.-diam silica-alumina doped commercial tungsten wire, hereafter designated as ordinary doped wire. A special lot of 0.065-in.-diam silica-alumina doped low-nickel wire was also used. Impurity analyses of the wire are given in Table I. The experimental design is shown in Fig. 1. All heat treatments were conducted in vacuum. Two groups of ordinary doped wire were prepared for diffusion with nickel. One group in the as-received (fibrous) condition was elec-tropolished, nickel-plated, and annealed at 1200°C for 20 and 40 hr, or was exposed to nickel vapor at 1200°C for 20 and 40 hr. The second group was recrystallized to an equiaxed grain structure at 2300°C for 3 hr, electropolished, nickel-plated, or exposed to nickel vapor for anneals at 1200°C for 20 and 40 hr.

Jan 1, 1969