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Jan 1, 1923

By I. S. Servi, N. W. Marr

TIN markedly increases the softening temperature of pure copper with only a moderate effect on conductivity. Smart and smith' indicated a substantial increase in softening temperature upon addition of different levels of tin up to 0.05 pct in oxygen-free copper. However, after finding no effect of tin in copper containing about 0.025 pct O, they concluded that "the presence of oxygen completely nullifies these changes in properties by precipitation of SnO2.'' Since preliminary tests on Cu-Sn-0 alloys indicated that this conclusion is not valid outside the extremely limited tin range investigated by Smart and Smith, research was primarily directed toward the partition of tin between the copper-base matrix and the oxide phases. Experimental. Material was prepared by sealing an 80 to 100-g charge consisting of oxygen-free copper, tin, and copper oxide into a y-in.-ID quartz capsule which was evacuated and back-filled with tank-grade argon to 3 atm. The sealed vials were heated to 1125ºC, kept at temperature for 30 min, occasionally agitated, and then allowed to air-cool outside the furnace ("as-cast"). The castings were cold-swaged to 0.370 in., annealed 1 hr at 600°C ("as-annealed"), and cold-swaged 16.5 pct ("as-swaged"). Cross sectional wafers were annealed for 1 hr at various temperatures and Rockwell F hardness measured. The "softening temperature" was defined as the interpolated temperature at which the hardness was 50 Rockwell F. Electrical resistance was measured by an ac poten-tiometric method on 0.040-in.-diam wires after a 1 hr anneal at 600°C. Relative accuracy was of the order of 1 pct. Chemical analyses for tin were performed by two methods, identified as "Acid flux" and "HN03 dissolution". The first consisted of fusing the sample with potassium pyrosulfate and leaching the resulting melt with 10 pct sulfuric acid. The spectrophotometric procedure which followed is described in Ref. 2. Oxygen analyses were performed by the vacuum-fusion method with a bath temperature of 1650°C. Tin content of oxides and copper phases was measured with the X-ray microprobe, using a calibration curve based on a series of oxygen-free Cu-Sn alloys. Results. In Fig. 1, the nominal tin composition for alloys containing nominally 400 ppm O was plotted vs the analyzed or the computed tin content—the latter derived from one of the following: 1) "acid flux" chemical analysis; 2) "HN03 dissolution" chemical analysis; 3) X-ray microprobe analysis of the copper matrix; 4) equivalent tin content, based on the measured increase in electrical resistivity (an increase in resistivity of 1.6 microhm-cm is approximately equivalent to 1 wt pct of sn1,3). It is evident from Fig. 1 that the results of the acid flux analysis are consistent with the nominal composition while the HNO3 dissolution method generally yields lower values, consistent with those obtained from electrical resistivity measurements and somewhat higher than those obtained by microprobe analysis. Microprobe and resistivity values are affected only by the tin in solid solution; hence the HN03 method

Jan 1, 1970

NEW MEMBERS The following list comprises the names of those persons who became members during the period July 10 to Aug. 10, 1915: Members ALBERTSON, MAURICE MERTON, Mine Surveyor, Mining Corporation of Canada, Cobalt, Ont., Canada. ARMSTRONG, GEORGE CHANDLER Mgr., Indian Refining Co., Lawrenceville, Ill. BARBER, MAX HAYDEN, Min. Engr Supt., Crosby Mine, Nashwauk, Minn. BARNESON, JOHN Merchant, 310 Sansome St., San Francisco, Cal. BENSEL, JOHN A., Cons. Engr 111 Broadway, New York, N. Y . BORGESON, ANSHELM CYRUS, fin. Engr Shenango Mule, Chisholm, Minn. BROOKS, CHARLES PETER, Min. Engr 228 Dooly Bldg., Salt, Lake City, Utah. BROWN, FRANK HAROLD, U'011',. Min. Engr., Federal Co., Inc., 50 Broad St., New York, N. Y. CLARK, DOUGLAS Kellogg, Idaho.

Jan 9, 1915

By Gerhard Derge

Metallurgists have used borax as a fluxing agent traditionally, but until recently elemental boron has played an insignificant role as an alloying element. Neither the metal nor its compounds have been regarded as important metallurgical materials and there is a surprising lack of knowledge concerning their metallurgical behavior. The new applications to steel-making of both boron and borates, which arose in part from wartime incentives and restrictions, have been seriously handicapped by this lack of data. For example, rasorite, a naturally occurring sodium borate, has been shown to be an effective substitute for aluminum as a ladle deoxi-dizer in rimming steels.' Likewise, the effectiveness of boron as an alloying agent has been demonstrated,2,3 giving deep hardening when used in restricted amounts. The exploitation of both of these uses has been retarded by the difficulty of attaining suitable metallurgical control. Recognizing that the most important information required was a knowledge of the equilibrium between boron and oxygen dissolved in liquid iron. Gurry4 calculated this relation from the best thermal data available. However, estimates of the entropy of melting of boron, the activity coefficient of boron in liquid iron and the activity coefficient of B2O3 in slag were involved, and experimental work on this problem was obviously desirable. The experiments to be described were planned to establish the boron-oxygen relations in liquid iron and to demonstrate at the same time the ferroborate slag compositions in equilibrium with various amounts of oxygen in liquid iron. Accordingly, slags containing varying proportions of iron and boron oxides were held in contact with molten iron, and samples of both slag and metal were analyzed. The limitations upon the accuracy of the data will be considered, but in a practical sense the oxygen levels that can be attained in iron by iron borate slags, and the amounts of boron in iron at these oxygen levels were established. Experimental Procedure No entirely suitable refractory was found for the mixtures of iron oxide and boron oxide used as slags. Crucibles of silica, magnesia, Ramix, beryllia, and zirconia were all tried unsuccessfully. The must satisfactory method discovered for handling them was the rotating-crucible technique, which creates a parabolic crucible of liquid iron.5,6 Even this was not entirely successful, for at steelmaking temperatures (1600°C.) the slags had such a low surface tension that they crept up to the refractory and slowly dissolved it. These difficulties made it impossible to maintain a constant slag composition for an unlimited period Of time. However, by using the rotating technique, short runs could be made in

Jan 1, 1947

By Gerhard Derge

Metallurgists have used borax as a fluxing agent traditionally, but until recently elemental boron has played an insignificant role as an alloying element. Neither the metal nor its compounds have been regarded as important metallurgical materials and there is a surprising lack of knowledge concerning their metallurgical behavior. The new applications to steel-making of both boron and borates, which arose in part from wartime incentives and restrictions, have been seriously handicapped by this lack of data. For example, rasorite, a naturally occurring sodium borate, has been shown to be an effective substitute for aluminum as a ladle deoxi-dizer in rimming steels.' Likewise, the effectiveness of boron as an alloying agent has been demonstrated,2,3 giving deep hardening when used in restricted amounts. The exploitation of both of these uses has been retarded by the difficulty of attaining suitable metallurgical control. Recognizing that the most important information required was a knowledge of the equilibrium between boron and oxygen dissolved in liquid iron. Gurry4 calculated this relation from the best thermal data available. However, estimates of the entropy of melting of boron, the activity coefficient of boron in liquid iron and the activity coefficient of B2O3 in slag were involved, and experimental work on this problem was obviously desirable. The experiments to be described were planned to establish the boron-oxygen relations in liquid iron and to demonstrate at the same time the ferroborate slag compositions in equilibrium with various amounts of oxygen in liquid iron. Accordingly, slags containing varying proportions of iron and boron oxides were held in contact with molten iron, and samples of both slag and metal were analyzed. The limitations upon the accuracy of the data will be considered, but in a practical sense the oxygen levels that can be attained in iron by iron borate slags, and the amounts of boron in iron at these oxygen levels were established. Experimental Procedure No entirely suitable refractory was found for the mixtures of iron oxide and boron oxide used as slags. Crucibles of silica, magnesia, Ramix, beryllia, and zirconia were all tried unsuccessfully. The must satisfactory method discovered for handling them was the rotating-crucible technique, which creates a parabolic crucible of liquid iron.5,6 Even this was not entirely successful, for at steelmaking temperatures (1600°C.) the slags had such a low surface tension that they crept up to the refractory and slowly dissolved it. These difficulties made it impossible to maintain a constant slag composition for an unlimited period Of time. However, by using the rotating technique, short runs could be made in

Jan 1, 1947

By Andrew E. Nevin, Sidney A. Williams, James N. Lukanuski

Three porphyry copper districts in southern Arizona are partly overlain by post-ore fanglomerates with certain physical and petrologic characteristics which define a distinct and significant class of rock. These units are the Locomotive fanglomerate at Ajo, the Helmet fanglomerate at Twin Buttes-Mission-Pima, and the Cloudburst formation at San Manuel- Kalamazoo, herein termed “Locomotive-type fanglomerates.” Post-ore units at Poston Butte and Lakeshore, Ariz., and Sar Chesmeh, Iran, also appear to fit this class. Locomotive-type fanglomerates may be genetically related to porphyry copper deposits as subsequent products of differentiation, volcanism, uplift, and sedimentation in short-lived basins of limited areal extent. These units are sufficiently distinct to be utilized as exploration guides for porphyry copper deposits in the Southwestern U.S., northern Mexico, and elsewhere.

Jan 1, 1977

By Francis Lucas

ANY metal which contains even a small percentage of aluminum possesses certain peculiarities of appearance and properties which are exhibited both when the metal is melted and after it solidifies. Pure aluminum, or an alloy containing a small proportion of aluminum, can be melted without flux-except for a layer of charcoal-because a film of aluminum oxide and metal forms at the surface of melted aluminum. Although very thin, this film is air-proof, and it prevents the metal underneath from oxidizing. This oxidized film does not move easily on account of its toughness and high surface tension. One very important point in connection with this process of still casting has not been strongly enough stressed, namely, that the same kind of surface film with the same peculiarities forms over the surface of all melted alloys that contain even a small proportion of aluminum. Experienced foundrymen know how desirable it is to cast aluminum under its "skin" or-under the surface of the film which tends to remain still. In the case of red copper, when in fusion, the surface shows pure copper only. This is due to the fact that liquid copper constantly absorbs the copper oxide which forms on the surface. By closely examining melting copper the oxide can be seen dissolving in the bath, and going into solution just as pulverized sugar dissolves in water. When copper is cast in the open, either in wire bars or cakes, the surface of metal exposed to the air is covered by a film of black, oxide that cannot be absorbed by the metal.

Jan 1, 1927

By Ferit Gurses

EXTENSIVE coal and lignite deposits exist in Turkey. Bituminous coal is the nation's principal mineral resource; important not only as fuel for the industrial development of the country, but also as a means of obtaining foreign exchange. Of the electrical power generated during 1939, 82.8 per cent was derived from coal.1 It is anticipated that the lignite deposits will be one of the major sources of power for the electrification of the country. BITUMINOUS COAL The locations of the four principal bituminous-coal2 basins are indicated on Fig. 1. The Eregli-Zonguldak basin lies on the Black Sea northwest of Ankara; the Canakkale basin lies near the junction of the Dardannelles; the Trakya basin is in European Turkey northwest of the Bosphorus and the Erzurum basin lies far to the east. The Eregli-Zonguldak basin is the most important of the four. This coal basin was discovered in 1829 but did not arouse interest until 1848; up to 1865, its annual production had not exceeded 50,000 metric tons. In 1865, during the Sultanate, working of coal mines was started by the Navy department, and the annual production was 61,145 metric tons. In 1908, the Minister of Commerce and Agriculture was authorized to develop the whole coal basin. Production reached 264,397 metric tons in 1910, and during 1915-1922, preceding the revolution, the total production of the basin was 2,676,043, or an average of 334,000 metric tons annually. The period of national revolution that followed was marked by a steady increase in coal production in Turkey, although world production decreased, because of the crisis of 1929-1932, about 52 per cent. AREA AND GEOLOGY OF THE COAL BASIN The geology of the Eregli-Zonguldak area is not yet completely known. The basin begins at Gungazi, to the west of Eregli, and extends to Sogutozu, a distance of about 106 miles. The coal beds, however, appear only in places and the overlying Cretaceous strata hide them elsewhere. This area includes the most important centers, such as Kandilli, Alacaagzi, Teflenli, Kozlu, Gelik (see Fig. 2). The geological sequence of the district is correlated with the Cretaceous of the Balkans; which is, in turn, a prolongation of the Alpine zone. Geological surveys made by G. Ralli, R. Zeiller and P. Arni3 show that the Eregli-Zonguldak formations fall into three natural divisions. Series a, The Alacaagzi in the district of that name (Fig. 2), is of the Culm stage. The strata strike generally east-west and dip about 30° south. This series appears also around Kandilli and Camli, with a steeper angle of dip, but the deposits there lack regularity. The Alacaagzi stage appears also farther east, to the south of Kozlu and Gelik. The Alacaagzi series contains 15 seams of an average thickness of 2 ½ ft. of good coal. Series b, the Kozlu, best represented in Zonguldak, Kilimli, Catalagzi, and between

Jan 1, 1944

Meeting of Apr. 23, 1915.-The Iron and Steel Committee was authorized in its discretion to defer the date of acceptance of papers for the Hadfield Research Prize to Nov. 1, 1916. The sum of $250 was appropriated as a guarantee fund to establish a Library Research Bureau in co-operation with the other Founder Societies. The sum of $50 was appropriated to the Puget Sound Section. The sum of $250 was appropriated to the San Francisco Section. The sum of $125 was appropriated to the St. Louis Section. The matter of memorializing the New York State Constitutional Convention was referred to the New York Section of the Institute with authority to act as a Section only. Upon recommendation of the Committee on Membership, 50 Mem¬bers, 1 Associate, and 6 Junior Members were elected.

Jan 6, 1915

THE paper on "Specific Efficiency of the Blast Furnace" by Richard Franchot, which was pub-lished in the September issue of MINING AND METALLURGY, was presented for discussion at the Pitts-burgh meeting. The session opened with a discussion among S. P. Kinney, Mr. Franchot, and J. N. Reese as to the methods and results in sampling for cyanides in the blast furnace. This is covered in detail in writ-ten discussion below. T. T. Read objected to the use of the term specific efficiency as likely to be confusing. The blast furnace has to perform the function of reducing Fe, 03 to Fe as well as that of fusing the metal and, since the reduc-tion of Fe, 0? involves a CO equilibrium, it seems mis-leading to calculate efficiency on the basis of burning the , all carbon to CO? since it is not possible. Mr. Franchot replied that he used the term in the sense defined by Richards in his "Metallurgical Calculations;" but a subsequent search failed to reveal the term in Richards, who says (page 245, 1st edition): The practical conclusion is that a blast furnace generates in itself not much over 40 per cent of the calorific power of the fuel used, and rejects nearly 60 per cent; by using part of the waste gases to heat the blast, however, some of this rejected heat, to an amount representing net 5 to 10 per cent of the calorific power of the fuel used, is returned to and injected bodily into the furnace, thus rendering available for the purpose of running the furnace about 50 per cent of the calorific power of the fuel as a maximum. The efficiency with which the furnace applies this 50 per cent usefully to the objects of the reducing and smelting is another question for investigation.

Jan 2, 1927

By Michael J. Messel

W. P. MOULD*—Has consideration been given to the problem of retreating the 4,000,000 ton tailings pile to recover the very considerable amount of asbestos fiber that was lost over the years due to insufficient operation and poor recoveries? Also, what was known about the possible content of chromite and the sulphides of nickel and cobalt? M. J. MESSEL (author's reply)—Consideration was given to the problem but nothing concrete has been done up to this time. W. P. MOULD—I am certain the tail- ings contain a very considerable quantity of fiber, not all of which is in the shortest lengths, because in the milling of talc rock from a neighboring location having a common origin with the asbestos bearing serpentine source of the tailings pile, a concentrate carrying 15 pct Ni and Co in complex sulphides and constituting about 4/10 of 1 pct of the talc rock was recovered. In the belief that the tailings also contained an appreciable content of chromite (then in demand, 1937) it was suggested to the management of the asbestos company that a truck load of the current tailings be sent to the flotation plant of the talc company where it would be put over the concentrating tables in an effort to discover the presence and roughly the percentages of chromite, nickel, and cobalt. Preparations for the test were woefully inadequate and the test was completely snarled up by the surprisingly large quantity of asbestos fiber from 1 in. long down to very short fiber, all of which matted up and plugged launders and pumps with disastrous effects and practically the total loss of the sample. If anything was indicaded by the test, it was that a wet process for milling asbestos was worthy of very serious consideration. M. J. MESSEL—A wet milling process for tailings retreatment only, is at present under study at our plant. One asbestos mining company in Canada has constructed a fairly large test plant for this purpose, but as yet no definite results have been obtained other than in a small test unit plant which were in some respects quite encouraging.

Jan 1, 1950

By S. L. Lopata, E. B. Kula

A variation of yield and tensile strength with direction has been noted in heat-treated 4340 steel which had been warn-worked by rolling in the austenitic condition prior to quenching. Measurements by X-rays showed a preferred orientation of martensite crystals. Various ideal preferred orientations of martensite were calculated by assuming a preferred orientation for austenite and transforming this to martensite by the Kurdjumov -Sachs and Nishiyama relationships. Comparison with the measured preferred orientation showed that the ideal rolling texture for austenite in 4340 steel could be expressed as a (112) [111] texture with a component of (110) [112]. No evidence was found for any fiber axis in the rolling direction, or fop- a (123) [412] texture. The observed martensite pole figures can be adequately accounted for by these ideal austenite textures and by the Kurdjumou-Sachs or Nishiyama transformation relationships between austenite and martensite. ALTHOUGH preferred orientations are found in cold-rolled steel sheet and in many nonferrous metals, they are not generally encountered in wrought, heat-treated high-strength steels, since such steels are generally not cold worked sufficiently to develop a strong texture, and any texture that is present is removed during heat treatment by the phase transformations taking place. This report gives details on a preferred orientation found in warm-rolled and hardened 4340 steel. In a recent study, a special combination heat-treating and working technique was used in which 4340 steel was deformed in the austenitic condition, and before re crystallization of the austenite could occur, quenched to form martensite.' Since the austenite was unrecrystallized, it was cold worked and hence could have contained a preferred orientation which could be transmitted to the martensite on quenching, and this in turn could be manifested as a directionality of mechanical properties. Such a directionality of properties was found as a result of working, and this prompted an X-ray study of the preferred orientation. Literature Survey— Rolling Texture in Face-Cen-tered-Cubic Austenite—M a preferred orientation is found in a rolled and hardened steel, it is first appropriate to consider what texture existed in the austenite as a result of the rolling but prior to the transformation to martensite. The changes taking place as a result of the austenite-martensite transformation are then considered. In view of the instability of austenite in 4340 steel at low temperatures, no direct determination of the austenite texture was made. However, an estimate of the texture for austenite in 4340 steel may be made by considering the textures found for other face-centered-cubic metals. Barrett' has reviewed the rolling textures for many materials. The most common orientation in face-centered-cubic metals has the (110) planes parallel to the rolling plane and the [112] directions parallel to the rolling direction, or (110) [112]. Other orientations found are (112) [111], as well as (100) [001], (110) [001], and others. Beck and his co-workers, using quantitative pole figures, report that (123) [121],3 later corrected to (123) [412],4 better describes the ideal orientation. smallman5 reported that the ideal preferred orientation for high-purity face-centered-cubic metals is (123) [121], but that there is a transition to (110) [112] as solid solution elements are added. The latter texture tends to occur more readily at lower temperatures. This transition between the two textures was explained by differences in the slip characteristics with concentration or temperature. More recently, Jones and Fell6 concluded that the (123) [412] texture for face-centered-cubic metals could equally well be represented by a mixture of (110) [112] and (112) [111] textures, and hence it had no physical reality. From the above results it can be seen that there is no agreement on the "ideal" texture for fcc metals and, hence, no firm basis for assuming a texture for austenite in 4340 steel. Therefore, the orientations (110) [112], (123) [412], and (112) [111] have been considered in the following.* *The (123) [4121 is identical to the (123) [121] rotated 90 deg. Orientation Relationship between Austenite and Martensite—When martensite forms from austenite, certain crystallographic planes of the martensite are parallel to planes in the austenite. This orientation relationship was first determined by Kurdjumov and

Jan 1, 1960

By E. O. Kirkendall

The investigation reported herein was undertaken to obtain data to supplement those presented in an earlier paper,l particularly for longer times at a higher temperature. This information may further develop our knowledge of the mechanism of diffusion in substitutional solid solutions. Diffusion of solute atoms interstitially dissolved is not difficult to visualize: it can take place without much disturbance of the solvent atoms. The mechanism of diffusion of solute atoms substitutionally dissolved is not so easily understood. Many theories have been advanced. Rosen-hain,2,3 Frenkel,4 Smekal,5 Langmuir,3,6 Steigman, Shockley and Nix,' and Johnson8 all proposed theories to explain diffusion. Langmuir's proposed mechanism consisted of a simple cyclic interchange of atoms involving an interchange in lattice positions of four or more atoms. This mechanism, accepted by the author at the time of his previous publication,1 and apparently quite generally accepted, required a net exchange in positions of both solute and solvent atoms in equal numbers. In other words, the rate of diffusion of the solvent and solute atoms would be the same. That this cyclic interchange in lattice positions of solute and solvent atoms in equal numbers is the only true mechanism of diffusion is denied by the evidence presented in this paper. Experimental Procedure This modification of similar procedure1 will be outlined briefly. The method consisted of the following steps: I. A pure Muntz metal (60.6 per cent Cu, 0.1 per cent total impurities) that was almost all beta brass at 780°C. was chosen. 2. The brass was turned between centers in a lathe to a diameter of 0.5965 inches. 3. After the brass was cleaned, it was electroplated with pure copper to a diameter of about one inch. 4. The sample was heated slowly to 400°C. under reduced pressure and held at that temperature for 4 hr. to remove occluded gases. It was then cooled to room temperature. 5. The sample was heated to 780°C. ± 3°C. and held at that temperature for different lengths of time; then quenched. Samples were cut off each time after quenching. Metallographic samples 1/4 in. thick were removed at I hr., 6 hr., 24 hr., 96 hr. and 701 hr. After 96 and 701 hr. samples of about I in. were removed for X-ray analysis. 6. The metallographic samples were polished on the cross section and photomicrographs were taken. 7. The I-in. samples were polished and etched on both ends. With the aid of a microscope each was carefully mounted in a four-jaw chuck in a lathe, so that they could be accurately bored for an arbor. 8. Turnings were taken for each X-ray sample. After each set of turnings, the sample was heated in an oil bath for about 1/2 hr. at 300°C. It was then etched in 25

Jan 1, 1942

By E. O. Kirkendall

The investigation reported herein was undertaken to obtain data to supplement those presented in an earlier paper,l particularly for longer times at a higher temperature. This information may further develop our knowledge of the mechanism of diffusion in substitutional solid solutions. Diffusion of solute atoms interstitially dissolved is not difficult to visualize: it can take place without much disturbance of the solvent atoms. The mechanism of diffusion of solute atoms substitutionally dissolved is not so easily understood. Many theories have been advanced. Rosen-hain,2,3 Frenkel,4 Smekal,5 Langmuir,3,6 Steigman, Shockley and Nix,' and Johnson8 all proposed theories to explain diffusion. Langmuir's proposed mechanism consisted of a simple cyclic interchange of atoms involving an interchange in lattice positions of four or more atoms. This mechanism, accepted by the author at the time of his previous publication,1 and apparently quite generally accepted, required a net exchange in positions of both solute and solvent atoms in equal numbers. In other words, the rate of diffusion of the solvent and solute atoms would be the same. That this cyclic interchange in lattice positions of solute and solvent atoms in equal numbers is the only true mechanism of diffusion is denied by the evidence presented in this paper. Experimental Procedure This modification of similar procedure1 will be outlined briefly. The method consisted of the following steps: I. A pure Muntz metal (60.6 per cent Cu, 0.1 per cent total impurities) that was almost all beta brass at 780°C. was chosen. 2. The brass was turned between centers in a lathe to a diameter of 0.5965 inches. 3. After the brass was cleaned, it was electroplated with pure copper to a diameter of about one inch. 4. The sample was heated slowly to 400°C. under reduced pressure and held at that temperature for 4 hr. to remove occluded gases. It was then cooled to room temperature. 5. The sample was heated to 780°C. ± 3°C. and held at that temperature for different lengths of time; then quenched. Samples were cut off each time after quenching. Metallographic samples 1/4 in. thick were removed at I hr., 6 hr., 24 hr., 96 hr. and 701 hr. After 96 and 701 hr. samples of about I in. were removed for X-ray analysis. 6. The metallographic samples were polished on the cross section and photomicrographs were taken. 7. The I-in. samples were polished and etched on both ends. With the aid of a microscope each was carefully mounted in a four-jaw chuck in a lathe, so that they could be accurately bored for an arbor. 8. Turnings were taken for each X-ray sample. After each set of turnings, the sample was heated in an oil bath for about 1/2 hr. at 300°C. It was then etched in 25

Jan 1, 1942

I. The Property. The Homestake Mining Co. has acquired through consolida tion the ground and equipment of the Father De Smet Con solidated Gold-Mining Co., the Deadwood-Terra Mining Go., the Caledonia Gold-Mining Co. and the Highland Mining Co., at and near Lead, Lawrence county, South Dakota, in the northern portion of the Black Hills. The company owns or controls 250 claims, comprising 2,616 acres and covering about 8,000 ft. along the strike of the lode. At the surface there are several veins, of which three have united in depth, where the main vein ranges from 300 to 500 ft. in width. The 1,100-ft. level is the lowest at present. The rock of both walls is, so far as known at present, carboniferous alate, and the country is penetrated by a system of porphyry dikes, and in some places capped with porphyry. The output of the company up to January, 1903, has been, approximately, $70,000,000. II. The Ore. The oxidized, open-cut ore is nearly all treated in the three mills on the northern part of the property, which are as follows : The Mineral Point (formerly the De Smet), of 100 stamps, the Monroe (formerly Caledonia), of 100 stamps, and the Pocahon tas (formerly the Deadwood-Terra), of 160 stamps. A cyanide plant, to treat the leachable portion of the tailings from these North End mills, has recently been installed and put into oper ation at Gayville, or Blacktail as it is now known. The Homestake lower-level ore, which comprises the greater part of that being milled at Lead, may be described as a horn blende, garnetiferous schist or slate, which has been crushed and infiltrated with free silica and pyrites, the latter being

Jan 1, 1904

By C. M. Marquardt

Tramp iron and steel moving on a conveyor belt cause small currents to be generated in a coil situated in a strong magnetic field, which are converted to an alternating current and are amplified. The output voltage from the amplifier fires a thyratron with a relay in its anode circuit, which actuates a howler and simultaneously drops a spot of marker material on the belt.

Jan 1, 1950

By A. U. Seybolt, J. L. Walter

The effects of the addition of 0.5 pct ThO2 (by volume) on the grain structure and texture of heavily rolled tungsten sheet were studied. Powder metallurgy ingots were rolled to sheet, 0.001 in. thick, and samples were annealed at temperatures from 1200" to 2500°C. The heating rate to the anneal temperature was varied from 3°C per min to 6500°C per min. The orientations of the largest grains were determined by X-ray diffraction. The disposition and loss of the ThO2 particles were determined by electron transmission microscopy and the activation energy for remozlal of the thorium was measured by mass spec-troscopy. Heating rates below about 800 C per min produced large, highly elongated grains. Higher heating rates produced much smaller, less elongated grains. The grain structure and texture of the slowly heated samples were identical to the structures and textures of heavily rolled tungsten foil conventionally doped with aluminum, silicon, and potassium but the recrystallization temperature was about 200°C lower. There was stringer-like dispersion of larger ThO2, particles superimposed on a uniform dispersion of fine particles. The particles increased in size and decreased in number with time at temperature. The loss of particles was accompanied by formation of grain boundary voids and surface pits. The activation energy for removal of the ThO2 was about 40 kcal per mole. THE addition of small amounts of aluminum, silicon, and potassium to tungsten has a profound effect on the grain structure of heavily rolled sheet1 or drawn wire."4 Thus, "doped" tungsten sheet, rolled to 0.001 in. and recrystallized, develops a structure consisting of large, highly elongated grains of a specific preferred orientation.' It has been shown that the elongated grain structure was caused by a dispersion of particles, identified as mullite (Al6si2O13),1,4 in strings parallel to the rolling direction in sheet or to the wire axis. Identical results were obtained for iron which was doped with glass and rolled to 99 pct reduction of thickness and recrystallized.5 Again, the glass particles were disposed in strings parallel to the rolling direction. The strings retarded boundary migration in the lateral direction but grain growth was able to proceed relatively unhindered along the direction parallel to the strings.1,5 In both the doped tungsten and the glass-doped iron, the particles were highly plastic during the high-temperature deformation. Since mullite melts at about 1800°C and the glass employed melts at about 810ºC, the particles were probably molten during the recrystallization anneals (above 1800°C for the doped tungsten and 850°C for the glass-doped iron). There are indications in the literature that particles not plastic at hot-working temperatures (up to about 1550°C for tungsten) may also impart elongated grain structures by primary recrystallization of worked alloys. Examples are dispersions of tantalum carbide in chromium,6 and ThO2 in nickel where elongation ratios of recrystallization grains of up to 20:l were obtained.7 Strings of ThO2 particles in W-ThO2 wire have been seen by Rieck.8 In view of the available evidence, it was of interest to extend the previous studies of doped tungsten and glass-doped iron to include W-ThO2 sheet materials. Of specific interest was the grain structure, preferred orientation, recrystallization temperature, and disposition of the thoria particles. EXPERIMENTAL PROCEDURE A) Material Preparation. About 380 g of blue tungsten oxide (approximate composition WO3) was wet with a sufficient amount of aqueous solution of Th(N03)4 to provide 0.5 vol pct ThO2. The wet mixture was stirred to distribute the doping material uniformly throughout the powder. Stirring was continued while the mixture was heated until it was completely dry. The dried, doped mixture was then reduced to tungsten powder by heating at 850°C for 2 hr in a stream of dry hydrogen. The doped tungsten powder was hydropressed in a rubber sack at pressures of 50,000 psi to produce an ingot approximately 2 cm diam by about 5 cm long. Next, the pressed cylinder was heated in hydrogen for 2 hr at 1350°C to render it strong enough for machining. The cylinder was machined to a square cross section of 1.6 by 1.6 cm with rounded corners. Finally, the bar was heated for 2 hr at 2150°C in hydrogen to provide a sufficiently dense mate rial to withstand the hot-rolling operation. Prior to rolling, the ingot was reduced in thickness by about 20 pct by forging at 1550°C. This served to increase the density of the material and to widen it slightly for better rolling characteristics. The forged ingot was then rolled at 1550°C to a reduction of 45 pct of thickness, following which the rolling temperature was reduced to 1300°C and the slab rolled, with several reheats, to 0.050 in. Further reduction was accomplished at 800°C in tungsten sheet packs to a total reduction of about 99.85 pct. B) Annealing Treatment and Observation of Structure. Small samples of the rolled foil were annealed in one of two ways. Some of the samples were suspended in a covered tungsten can and annealed at temperatures from 1200" to 2200°C for various times in vacuum of l0-7 to 10-6 mm Hg. The can was heated by induction and temperatures were determined by optical pyrometry

Jan 1, 1970

By R. A. Meussner, R. J. Goode

Six intermediate phases occur in the Nb-Zn sysThese phases form by peritectic reactions at 1120°, spectively. The Nb Zn 15 phase appears as the minor phase in the eutectic structure, and the terminal phases remain nearly pure niobium and zinc even at high temperature. Vapor -pressure measurements on the four high-temperature phases (Nb Zn to Nb Zn 3) permitted estimates of the composition limits of these phases and the calculation of approximate values of AFO, AH°, and AS°. 1 HE present study of the constitution of the binary Nb-Zn system was a part of an analysis of the mechanism by which coatings of the Nb-Zn intermediate phases protect niobium against oxidation at high temperature.' Since the primary interest in these phases was in coating service, attention in this study was given principally to the four phases stable at high temperature with only cursory attention to the two low-temperature phases. The solubility studies of niobium in zinc by Martin, Knighton, and Feder2 and the reports from the present study of the Nb-Zn coating represent the only published data pertaining to this system. Previously Hodge, Evans, and Hoskins, in an experimental survey, had noted that niobium was not resistant to attack by molten zinc, but no further observations were reported. EXPERIMENTAL PROCEDURES a) General. The nature of the binary Nb-Zn system precluded the use of more conventional methods of determining the phase equilibria such as thermal analyses of a series of cast alloys. An extrapolation of the liquidus data of Martin, Knighton, and Feder2 to higher temperatures suggested that the solubility of niobium in zinc would remain low in the entire temperature range of interest. The preliminary results of the present studies showed that all of the high-temperature intermediate phases form by peritectic reactions. Thus the sluggish nature of this type of reaction and the steepness of the liquidus indicated that thermal analyses would not yield reliable data. The peritectic reactions, of course, precluded the direct formation of samples of the individual phases from the melt. b) Materials. The niobium and zinc used in the present studies were of high purity. The niobium, in the form of 0.1-in.-diameter rods, contained 30 ppm 0, 30 ppm N, and 15 ppm C. Aside from 0.05 pct Ta, the metallic impurities (iron, titanium,

Jan 1, 1965

By E. A. Gulbransen, W. S. Wysong, K. Andrew

INTRODUCTION THE reaction of carbon in solid solution in a metal with the surface oxide film on many metals may be inferred from thermodynamic calculations for high vacua and high temperature conditions. Holm1 has recently shown that oxide films may be removed from ferrous materials by heating in a vacuum at high temperatures and that carbon is the essential element in the reaction. Considerable work has been described in the literature on the decarburization reaction. Several general references may be noted.2,3,4 However, the nature of the mechanism involved in the decarburization is not well understood. Our interest in this reaction resulted from many attempts to degas and to reduce by pure and dry hydrogen the surface oxides 0n strips of various types of chrome-nickel alloys. Some of the early experiments on the behavior of 13 pct chrome-iron in vacua of the order of 5 X 106 mm and at a temperature of 600°C have been reported.5 These experiments showed a slow reaction with the residual oxygen or water vapor in the system and no reaction with hydrogen. This is in accord with thermodynamic data which would lead to the prediction that it is extremely difficult to maintain a hydrogen atmosphere at 600°C pure enough to reduce Cr203 formed on the surface. The crystal structure of the superficial oxide film formed on 13 pct chrome iron and Nichrome V has been investigated in the thin film range by Gulbransen, Phelps and Hickman,6 and shown to be Cr203. It was surprising to us to note that when a specimen of Nichrome V containing approximately 80 pct nickel and 20 pct chromium was heated to 850°C in a high vacuum, the specimen' lost weight. The rate of weight loss was very temperature sensitive. A study of this reaction in vacua and in a hydrogen atmosphere is the subject of this communication. TYPE REACTIONS Let us consider the various reactions which may occur when a metal is heated in vacua, in a hydrogen atmosphere, or in an oxygen atmosphere. The number and kind of reactions will depend upon the chemical nature, of the metal, its alloying constituents and the location of the alloying constituents. The metals used in this study are chrome-nickel alloys of the heater type. They consist essentially of chromium, nickel and iron, small amounts of carbon, silicon and manganese and traces of zirconium, calcium, aluminum and magnesium. The trace elements are added to improve the lifetime and other characteristics of the alloy when used as a heater. Seven of the more important reactions with which we are going to be concerned here are as follows: [I. Metal • (gas) ;--* metal + gas - degassing of the metal 2. xM(s) + y ½ 02(g) tom- M.0„ (s) – oxidation]

Jan 1, 1948

By Paul H. Price

The history of the salt industry in West Virginia dates back nearly two hundred years; however, the history of salt as an important raw material for the chemical industry is much more recent. The earliest record of West Virginia salt was in 1753, when a raiding party of Shawnee Indians attacked frontier settlements in Virginia taking captive a number of the pioneers. One of these, who later escaped and returned to her friends, described how the Indians camped at a salt spring on the banks of the Kanawha River and evaporated the water to obtain a supply of salt to take back to Ohio with them. Settlement of the Kanawha Valley began in 1774, that same year the Battle of Point Pleasant ended the Indian's power in the Ohio Valley; and settlement of the Kanawha Valley progressed rapidly with a consequent increase in the importance of the Kanawha Licks as a source of salt. In those days the evaporation of the brine was a family matter for which the family wash-kettle was commandeered.

Jan 1, 1949