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By Ancel St. John

AT THE New York meeting of the Institute of Metals Division in February, 1927, Jeffries and Tarasov presented a paper on Tungsten and Thoria,1 in which the experimental facts were interpreted in accordance with the prevailing point of view that the thorium is present as the oxide, thoria. In discussing that paper the writer of this article stated that his own investigations, which had been unavailable to Messrs. Jeffries and Tarasov, showed that the so-called "thoriated" tungsten filament failed to disclose any sign of the oxide when subjected to X-ray diffraction analysis, but did give plenty of evidence of the presence of metallic thorium and, in certain cases, of a material believed to be an alloy of tungsten in thorium. Since these results were completely at variance with the results reported in the paper under discussion and with other papers which had preceded it from time to time in the past, it was felt that further discussion should be withheld until the new evidence could be presented adequately. Arrangements were therefore made to present that evidence at this meeting. MATERIAL EXAMINED The material examined was high-emission filament such as is used in radio tubes, supposed to contain about 0.75 per cent. thoria. The actual analysis was not stated. SCOPE OF THE INVESTIGATION The investigation was undertaken because of a feeling that the thorium present in filamentary material of this type exists as metallic thorium or as an alloy of thorium and tungsten and not as the oxide. Attention was therefore directed to determining: 1. The minimum amount of thoria detectible in a mechanical mixture of thoria powder and finely divided tungsten. 2. The amount of thoria detectible in the filament. 3. The condition of any thorium present in other form than as thoria. 4. The amount of thorium dissolved in the tungsten.

Jan 1, 1928

By R. P. Marshall, L. P. Costas

The solid solubility of lithium in aluminum was determined by two independent techniques, electrical resistivity and microhardness, and the results are in close agreement. The solubility limits X-ray diffraction studies of the intermetallic compound LiAl indicate that its composition is nearly independent of temperature when in equilibrium with the terminal solid solution of aluminum. THE investigation of the aluminum-rich portion of the aluminum-lithium system at the Savannah River Laboratory was prompted by the observation that over-aged alloys consistently differed from the equilibrium states predicted by the latest published diagrams. Chemical analyses of these alloys showed their impurity contents to be quite low; therefore, the results obtained should have very nearly coincided with true equilibrium. A survey of the literature disclosed that previous studies had been made with metallographicig or electrical resistivity methods,4'5 but that agreement between results and technique was poor as evidenced in Fig. 1, which also includes the present results for comparison. The discrepancies have been attributed to impurities,3 and this is undoubtedly true in the early work.1'4'5 The latest Studies,''~ conducted with starting materials of higher purity, employed metallographic analysis, a technique that is quite sensitive to local homogeneity and depends strongly on subjective interpretation. In the present work the problem of defining solubility limits was approached in two ways. The first measured a physical property, electrical resistivity, at the equilibrium temperature. The second, a micro-hardness characterization of a diffusion zone, is a room temperature evaluation of a mechanical property under conditions removed from equilibrium. A close correlation between two such basically different approaches would strongly justify confidence in the results. I) MEASUREMENT OF SOLUBILITY OF LITHIUM IN ALUMINUM BY ELECTRICAL RESISTIVITY Experimental Procedure. Alloys for electrical resistivity measurements were made by melting and

Jan 1, 1962

By George A. Morrison

A deposit Of limestone Was known to exist at a depth of 2000 ft under the property of the Columbia Chemical Division of the Pittsburgh Plate Glass Co. at Barber-ton, Ohio. A 662-acre site was selected for the projected mine, some two miles northwest of the plant and near the main line of the Erie Railway. An electric railway 8800 ft in length connects the mine and the plant. The deposit is overlain by 18 ft of un-consolidated (sand and gravel), 100 ft of water-bearing sandstone, and finally 2080 ft of shale into which thin layers of sandstone are embedded. The limestone bed itself is 345 ft thick and overlies 200 ft of gypsum. A 300-ton-per-hour capacity mine was decided upon. Two shafts were deemed advisable, one for production and the second for service; and these were sunk 550 ft apart, one to a depth of 2323 ft and the other to 2258 ft. Each is 16 X , ft in the clear and timbered with 6-in. steel H-sets on 8-ft centers, using 3/8 X 4 X 4-in. angles as studdles. Twelve inch I-beams were used at 160 ft intervals as bearers set in deep hitches and concreted to a vertical depth of 8 ft. Wooden sheathing was first employed but sloughing of the shale created a pressure on this lining and finally concrete was deemed necessary. Water was encountered only within the first 315 ft, flowing at 60 gpm and by grouting this was reduced to 15 gpm. Temporary wooden sinking headframes were installed with 300 cu ft capacity storage pockets and with doors automatically controlled by air cylinders by hoistmen. Each shaft was operated on four 6-hr shifts. The usual V-cut was drilled at the center of the shaft and the round consisted of 34 holes- A 40 pet gelatin dynamite was employed with some 60 pet in the cut holes. Drilling crews consisted of four to six men. Shale drilled easily but became more bed in depth and sandstone wore away the gauge Of the bits rapidly. A room-and-pillar mining system was adopted whereby rooms turned off on 80-ft centers, each room 40-ft wide and 50-ft high. Rib pillars between rooms were cut into 100 ft lengths by frequent holes. Ventilation is achieved through the two shafts, the down-draft through the service shaft, and the return through the pr0duction shaft. The hoist has a a Of 300 tons per hour and is equipped with 10-ton balanced skips requiring. a 2-min cycle Or 30 trips Per hour- Hoisting is designed to Operate by automatic loading and no hoistman is required for normal Operation. The 48 X 60 in. jaw primary crusher is underground. It is fed through chute and chain feeders and is flood-oil lubricated and cooled. An inclined belt conveyor returns oversized material to the crusher. Tramming is by Diesel-powered trucks.

Jan 1, 1948

By George A. Morrison

A deposit Of limestone Was known to exist at a depth of 2000 ft under the property of the Columbia Chemical Division of the Pittsburgh Plate Glass Co. at Barber-ton, Ohio. A 662-acre site was selected for the projected mine, some two miles northwest of the plant and near the main line of the Erie Railway. An electric railway 8800 ft in length connects the mine and the plant. The deposit is overlain by 18 ft of un-consolidated (sand and gravel), 100 ft of water-bearing sandstone, and finally 2080 ft of shale into which thin layers of sandstone are embedded. The limestone bed itself is 345 ft thick and overlies 200 ft of gypsum. A 300-ton-per-hour capacity mine was decided upon. Two shafts were deemed advisable, one for production and the second for service; and these were sunk 550 ft apart, one to a depth of 2323 ft and the other to 2258 ft. Each is 16 X , ft in the clear and timbered with 6-in. steel H-sets on 8-ft centers, using 3/8 X 4 X 4-in. angles as studdles. Twelve inch I-beams were used at 160 ft intervals as bearers set in deep hitches and concreted to a vertical depth of 8 ft. Wooden sheathing was first employed but sloughing of the shale created a pressure on this lining and finally concrete was deemed necessary. Water was encountered only within the first 315 ft, flowing at 60 gpm and by grouting this was reduced to 15 gpm. Temporary wooden sinking headframes were installed with 300 cu ft capacity storage pockets and with doors automatically controlled by air cylinders by hoistmen. Each shaft was operated on four 6-hr shifts. The usual V-cut was drilled at the center of the shaft and the round consisted of 34 holes- A 40 pet gelatin dynamite was employed with some 60 pet in the cut holes. Drilling crews consisted of four to six men. Shale drilled easily but became more bed in depth and sandstone wore away the gauge Of the bits rapidly. A room-and-pillar mining system was adopted whereby rooms turned off on 80-ft centers, each room 40-ft wide and 50-ft high. Rib pillars between rooms were cut into 100 ft lengths by frequent holes. Ventilation is achieved through the two shafts, the down-draft through the service shaft, and the return through the pr0duction shaft. The hoist has a a Of 300 tons per hour and is equipped with 10-ton balanced skips requiring. a 2-min cycle Or 30 trips Per hour- Hoisting is designed to Operate by automatic loading and no hoistman is required for normal Operation. The 48 X 60 in. jaw primary crusher is underground. It is fed through chute and chain feeders and is flood-oil lubricated and cooled. An inclined belt conveyor returns oversized material to the crusher. Tramming is by Diesel-powered trucks.

Jan 1, 1948

By J. S. Kirkaldy, G. R. Purdy

THE formation of ferrite in supersaturated aus-tenite has been the subject of considerable speculation and investigation. Aaronson has recently reviewed the data pertinent to this reaction.' Since these data in all cases refer to ternary or high-order alloys it is not possible to put them to the test of simple binary diffusion formalism. It has not, therefore, been possible to make a certain statement as to the controlling mechanisms in the process. An assessment of the difficulties inherent in the conventional statistical metallographic approach suggested that a study of the problem by means of a macroscopic two-phase diffusion couple might contribute useful information. Accordingly, such a couple was synthesized, and the rate of motion of a ferrite-austenite phase boundary (the growth of an austenite layer at the expense of a ferrite layer) was determined. Wagner originally produced a diffusion solution applicable to the motion of a planar phase interface in a binary diffusion couple, assuming local equilibrium throughout the diffusion zone. This solution, which is stated free of typographical error* in Ref. where a is the position of the interface in A space (A = x/fi), C; and CL1 are the equilibrium inter-facial concentrations in phases I and 11, C: and C*1 are the initial bulk concentrations in phases I and 11, and & and are diffusion coefficients (assumed constant). If a diffusion couple consisting of homogeneous layers of ferrite and austenite in equilibrium is raised to a higher temperature, the austenite layer will grow at the expense of the ferrite. Provided that the thickness of the ferrite layer is much less than the diffusion length of carbon in ferrite, we can set , so that Wagner's solution reduces to

Jan 1, 1963

By C. M. Wayman, M. A. Gedwill, C. J. Altstetter

Cobalt Whiskers were grown by the hydrogen reduction of CoBr,. The fcc = hcp martensitic trans-formation in these whiskers was studied using X-ray and metallographic techniques. Present theories of the fee + hcp martensitic transformation were ex-amined in the light of the present findings Experimental evidence for slip as a part of the transformation mechanism is presented. In the bulk form cobalt is known to undergo a martensitic transformation1 from an hcp to an fcc structure upon heating above about 430°C. Upon cooling, the reverse transformation starts at about 400°C, but does not go to completion except in single crystalline or coarse-grained samples, or upon plastic deformation. The transformation may be thought of as the shearing of close-packed atomic planes in such a way as to change the stacking sequence from ABCABC to ABABAB with a contraction normal to the shearing planes and an expansion in the planes,2 producing a c/a ratio slightly less than ideal. This restacking to give {0001) and (112) 11 (1010) can be accomplished by the passage of a shockfey partial dislocation over every other (111)f plane resulting in a theoretical shear of 19.47 deg. To date there has been no completely satisfactory explanation of how the partial dislocations are produced on the close-packed planes or propagated from plane to plane to give the correct stacking sequence. The object of the present research was to study some of the characteristics of the fcc to hcp transformation in geometrically simple single crystals. It was felt that whiskers of cobalt grown by halide reduction would be ideal specimens with which to study the transformation, because whiskers have the following desirable features: 1) are easily grown as fcc single crystals; 2) exhibit relatively simple geometries; 3) have comparatively low dislocation densities;

Jan 1, 1964

By Charles Frey

TIE fundamental principle of resistance thermometry lies in the determination of temperatures by the measurement of an electrical conductor subjected to various temperatures and the translation of the resultant changes, in ohms, into temperature equivalents. Such resistance measurements can be made with maximum precision by the use of a standard Wheatstone bridge and a reflecting galvanometer of high sensitivity. Under such conditions, results are obtainable that may be accurate within 0.1 or even 0.01 per cent., and the "idiosyncrasies" of heated electrical conductors can be studied with advantage and profit, even if the latter is not of a financial nature. The chief requisites for producing a serviceable -commercial instrument may be enumerated as follows: First, there must be a resistor or "bulb" that can stand the maximum temperature without deterioration and which has a pronounced temperature coefficient. Second, there should be constructed an "even" bridge, having two fixed arms of equal values, in ohms. Third, a rheostat, the maximum resistance of which will be equal to the total change in the resistance of the bulb, between temperature extremes, is required. Fourth, there must be a sensitive galvanometer which is aperiodic, or nearly so. Finally, there should be a fairly steady source of direct current. The general scheme of this type of apparatus, in its simplest form, can be readily understood by reference to Fig. 1. Resistors A and B are constructed of manganin, therlo, or some other resistance wire having a negligible temperature coefficient. The sensitive D'Arsonval galvanometer G has its zero in the center. R is a rheostat and X is a resistor or bulb made of insulated platinum wire, or else of nickel, copper, or some alloy, according to requirements. K is a battery, but a direct-current service line is often used instead, with sufficient ballast in series to properly reduce the current.

Jan 8, 1919

By G. D. Van, Arsdale

IT IS particularly appropriate that a paper on this subject should be presented in Spanish, before a Spanish speaking audience, and in a South American country, first because of the facts that these countries today have not only the largest copper leaching plant in existence but also present great opportunities for future extension of hydrometallurgy; and second, because of the fact that the first copper made by any wet method was doubtless produced before existing records at the Rio Tinto deposits in present day Spain.

Jan 1, 1925

By O. K. Riegger, L. H. Van Vlack

The median angle of relatively few two-dimensional observations provides a satisfactory value for dihedral angle determinations. Those data that contain bimodal or non-equilibriated dihedral angle distributions are readily detected. THIS paper is concerned with a statistical simplification for determining dihedral angles in solids. Microstructures are partially controlled by relative energies of interphase boundaries and grain boundaries. smith1 has shown rather conclusively that such boundaries may be equilibrated to give a vectorial balance at grain and phase edges. Thus if an accurate measurement is made of the dihedral angle associated with grain and phase edges, an accurate calculation of the relative energies may also be made. The accurate measurement is difficult because the dihedral angle involves two planes in three dimensions, and only a two-dimensional cut through the dihedral angle is usually observed. Such a two-dimensional cut is statistically random provided there is no preselection or orientation. Harker and parker2 have shown that the mode of the frequency distribution of observed angles is within 5 deg of the true angle if the true dihedral angle is 120 deg. smith1 had calculations made to show that the same generalization could apply to dihedral angles of 30, 60, 90, and 150 deg. This procedure of requiring the determination of the statistical mode is time consuming because experience has shown that more than 200 angle observations are necessary before the mode is clearly indicated. It is possible to determine the dihedral angle with equal accuracy with only 25 angle observations if the median angle is used in place of the mode angle. Use is made of Harker and parker's2 basic equation tan =2 sin x cos

Jan 1, 1961

By C. F. Quest, T. S. Washburn

The steel industry has a definite need in its tonnage mills for a formula relating expected tensile strength to the analysis of the steel. The McWilliam-Barnes1 and other less comprehensive formulas are used for this purpose, but these formulas were designed for an analysis range that does not include the medium manganese and silicon-bearing steels. This type of steel is being produced to meet the demand for tensile strength slightly higher than that of ordinary structural steel but not high enough to justify expensive alloy steels. The purpose of this paper is to present a somewhat more comprehensive formula based on data accumulated over a number of years by the Inland Steel Co., and to discuss the method followed in obtaining a formula to fit the data. The resultant formula admittedly is still weak in some respects, but for the expanded analysis range appears to be an improvement over the other formulas. It is hoped that with the collection of more data and possible collaboration with other mills studying this problem it will be possible to work out a more nearly perfect formula. Several publications have been issued on this subject. In some, the equation type of relation was evolved while others made a combination of tables and an equation. The latter include work by Campbel12,3 and Webster.4,5 Campbell classified the steels as acid and basic and applied a different formula to each. For basic steels, he used the equation: Teosile etrength = 41500 + 770C + 1000P + yMn [1 y was a variable depending on the carbon and manganese content of the steel and was listed in tables. Webster investigated acid Bessemer steel and developed the equation: Tensile strength = 38000 + 800C + xTP+ yMn [2]

Jan 1, 1940

By C. F. Quest, T. S. Washburn

The steel industry has a definite need in its tonnage mills for a formula relating expected tensile strength to the analysis of the steel. The McWilliam-Barnes1 and other less comprehensive formulas are used for this purpose, but these formulas were designed for an analysis range that does not include the medium manganese and silicon-bearing steels. This type of steel is being produced to meet the demand for tensile strength slightly higher than that of ordinary structural steel but not high enough to justify expensive alloy steels. The purpose of this paper is to present a somewhat more comprehensive formula based on data accumulated over a number of years by the Inland Steel Co., and to discuss the method followed in obtaining a formula to fit the data. The resultant formula admittedly is still weak in some respects, but for the expanded analysis range appears to be an improvement over the other formulas. It is hoped that with the collection of more data and possible collaboration with other mills studying this problem it will be possible to work out a more nearly perfect formula. Several publications have been issued on this subject. In some, the equation type of relation was evolved while others made a combination of tables and an equation. The latter include work by Campbel12,3 and Webster.4,5 Campbell classified the steels as acid and basic and applied a different formula to each. For basic steels, he used the equation: Teosile etrength = 41500 + 770C + 1000P + yMn [1 y was a variable depending on the carbon and manganese content of the steel and was listed in tables. Webster investigated acid Bessemer steel and developed the equation: Tensile strength = 38000 + 800C + xTP+ yMn [2]

Jan 1, 1940

By Tribhawan N. Srivastava

The Henderson Mine started production in 1976 utilizing a unique, push-pull, mine ventilation plan. As the mine expands in size, the mine ventilation requirements will increase and a more comprehensive system for maintaining ventilation will be needed. A computer simulation study was completed and has resulted in a revised, systematic, mine ventilation plan which is being implemented as mine development proceeds. Based on the computer simulation study, the new ventilation plan takes into account mining of the orebody simultaneously from both the 8100 and 7700 production levels. Present experience and empirical data indicate that volumes of air needed to adequately ventilate both production levels cannot be obtained utilizing the existing mine layout. The total volume of air needed for the mine excluding haulage tunnel will increase from 708 m3/s (1 500 000 cfm) to 1652 m3/s (3 500 000 cfm), thus a new No. 5 exhaust shaft and connecting drifts are being developed to expand the mine ventilation system to service both production levels. The original ventilation plan for the 7500 haulage level was to bring air from the No. 2 and No. 3 intake shafts and exhaust it through the 94X raise to the 8035 exhaust level and then through the No. 1 exhaust shaft to surface. Control of air volumes in loading drifts was initially planned to be achieved by air doors and air curtains. Air doors on the 7500 level require large cutouts, expensive installations and constant maintenance. The computer simulation study indicates that air- flow in the 7500-level production drifts can be con- trolled exclusively by air curtains which are less expensive to install and more effective in regulating airflows than air doors. Air from the 7500 level can be exhausted through a new raise to the new 7635 exhaust level and then through the new No. 5 exhaust shaft.

Jan 1, 1982

H. H. Campbell, Steelton, Pa. (communication to the Secretary) : I wish to thank Mr. Webster for the copious quotations he has made from my writings, as he has given nearly all the arguments I wish to advance. It is necessary to note, however, his statement that most of his experiments were made on universal-mill plates, and that these were not subject to my condemnation of irregularity. I think this is a mistake. It is well known that universal-mill plates are finished under very different conditions of temperature, with the express purpose of regulating the tensile strength. This is a perfectly legitimate practice; but it renders almost worthless any calculations on the relations of the chemical and physical equations when the influence of such finishing is omitted. Another important point Mr. Webster has not answered at all. I have shown by an excerpt from his own table that two entirely different formulæ may be constructed; and it is undeniable that one is as valid as the other, since Mr. Webster started with no premise at all save an assumption that the effect of carbon was constant. This was an assumption pure and simple, and hence has no special virtue. The whole result of Mr. Webster's investigation is not that the effect of carbon is a constant, and that those of phosphorus and manganese are variables. On the contrary, there are two answers, with nothing to show which is right. We learn that if carbon is a constant, then phosphorus and manganese are variables; but that if phosphorus and manganese are constants, then carbon is a variable. This is a distinct advance over complete ignorance, but it is not final and satisfactory from either a mathematical or metallurgical standpoint. Regarding my own formulæ, I would say that they are used regularly in the testing-laboratories of the Pennsylvania Steel Company. The tensile strength of every heat is calculated

Jan 1, 1899

ASIDE-from the John Fritz Medal, in which the Institute participates through its representation on the John Fritz Medal Board, the Institute itself has four awards it may make annually, as follows: the Robert W. Hunt Medal and Prize, the J. E. Johnson, Jr., Award, the James Douglas Medal, and the William Lawrence Saunders Medal.

Jan 1, 1928

By John E. Riddell

This review is based on a questionnaire sent out in 1959 to 24 Canadian exploration companies, known to be active in the mineral exploration field, concerning their practice in the use of applied geo-chemical techniques in Precambrian terrains. Of the companies questioned, 21 returned completed questionnaires and of these, 15 companies stated that they had some experience in this type of work. Of the companies who stated that they had no experience in geochemical prospecting in glaciated Precambrian areas it is interesting to note that only three have reported that they do not use applied geochemistry at all. The others have reported that they make use of applied geochemistry in New Brunswick and in the Cordillera in areas of light glaciation. Their opinion is that it is a useful aid when accompanied by other techniques in evaluating mineralized areas. GEOCHEMICAL SURVEYS Table I reviews the type of geochemical surveys used by these companies, and the following points of interest should be noted.

Jan 11, 1960

By J. V. Gluck, Ping-Wang Chiang

The tellurium-rich region of the Sb-TI-Te ternary system was investigated by means of DTA, metallo-graphic, X-ray, and electron beam microprobe techniques on the sections Sb2Te3-T12Te3, SbTlTe2-Te, SbT1Te2-Sb2Te3, and SbTlTe2-T12Te3. The phase behavior of this region is summarized in terms of four ternary invariant reactions and a schematic reaction diagram is suggested. Isopleths for the sections SbT1Te2-Sb2Te3, Sb2Te,-T12Te3, and SbTlTe2-Te were constructed, and a schematic diagram of the projections of the liquidus lines and invariant planes is presented. No evidence was found to support the existence of the ternary compound "SbTlTe3", or pseudo-binary behavior of the section T12Te3-Sb2Te3, as reported by Borisova and Efremova. Electrical conductivity, Seebeck coefficient, and thermal conductivity measurements were made at room temperature on fully annealed samples. 1 HE phase relationships in chalcogenides are often complex and difficult to resolve, particularly since the approach to equilibrium is a rather slow process. For example, the phase diagram of the T1-Te binary system was in doubt until clarified by Rabenau et al.,1 the phase fields at compositions near Bi2Te3 in the Bi-Te binary system have only recently been satisfactorily elucidated by Glatz,2 and there may still be some question as to the extent of the Sb2Te3 field in the Sb-Te system.3-5 In ternary systems, the existence of the compound "AgFeTe2" was the subject of a number of conflicting reports6-8 and the stoichiometry of the composition "AgSbTe2" was in doubt for a period of time.9 Recently, questions have arisen regarding the existence of certain compounds in the ternary systems Bi-Tl-Te10-14 and Sb-Tl-Te.15 The impetus for studies of these latter systems stemmed from the report of Borisova et a1.10 of a congruently melting ternary compound, "BiTlTe3", which apparently had extremely favorable thermoelectric properties for room-temperature cooling applications. Attempts by other investigators to produce the compound or confirm the transport properties proved to be unsuccessful.12-14 Recently, Chiang and Gluck14 reported studies of the phase relations in the tellurium-rich region of the Bi-T1-Te system which indicated that the section T12Te3-Bi2Te3 was not pseudobinary as suggested by Borisova et a1.10 The contention of Spitzer and sykes12 was supported that the composition "BiT1Te3" was multiphase, with the primary constituent actually being BiTlTe2, a compound whose existence has been well demonstrated.16,17 The investigation reported in the present paper was prompted by a later report of Borisova and Efremova15 on a similar study of the section T12Te3-Sb2Te3 from the Sb-T1-Te system. They also claimed this section to be pseudobinary, and that a ternary compound "SbTlTe," was formed peritectically. Some "preliminary" crystallographic data were given for the compound and thermoelectric transport properties were presented. In view of the questions concerning the behavior of the Bi-T1-Te system and the existence of the compound "BiT1Te3" it was suspected that the Sb-T1-Te system might behave in a similar fashion, particularly in light of the known existence of a compound SbT1Te2, iso-structural with BiT1Te2.17 Consequently, an investigation was undertaken to clarify the phase relationships in the tellurium-rich region of the Sb-T1-Te system. It is the purpose of this paper to present the results of this study, including a representation of the phase relations, isopleths for various composition sections, and the determination of some phase compositions and transport properties. EXPERIMENTAL PROCEDURES Commercially available high-purity (99.999+ pct) elements, purchased from the American Smelting and Refining Co., were used for the sample preparation. All samples were made from thoroughly mixed powders of previously prepared master alloys: SbTlTe2, Te, Sb2Te3, and T12Te3. Stoichiometric quantities of the constituents for each 10-g sample were weighed into a specially cleaned fused silica tube and sealed under a vacuum of better than 5 x 10-5 torr. The sealed constituents were fused and reacted at 650° to 750°C for at least 4 hr under continuous agitation in a "rocking" furnace, and the resulting product was air-cooled. The tube was opened and the sample was ground to a powder. A portion of the powder was rebottled in a DTA tube under vacuum, and the rest of the material was similarly resealed in a separate tube, re-fused in the rocking furnace, and again cooled to make the ingots for electrical and microstructural studies. All samples were subjected to further heat treatments as discussed in the section on experimental results. Each DTA tube was made of 7-mm-OD fused silica tubing with a concentric 2-mm-ID depression about 4 mm long formed in the bottom to accommodate a thermocouple. The size of a DTA sample was 0.5 to 1.0 g. An Aminco Thermoanalyzer whose accuracy was within 2°C18 was used for the DTA measurements. The metallographic samples were prepared by conventional techniques. A solution of FeCL dissolved in a methanol-HC1 mixture was found to be the most satisfactory etchant. Electron beam microprobe scanning and point-count examinations were made on polished and unetched samples using an ARL Electron Microprobe at an electron beam voltage of 20 kv. The detectors were set to receive characteristic La1 radiation. Calibration standards of the pure elements were incorporated in each sample mount; quantitative point counts were calibrated by a method similar to Ziebold

Jan 1, 1969

By Faustino Roel

AMONG the problems confronting the mining engineer in Mexico in recent years, labor conflicts have come to occupy s prominent place. Each day they have become more serious and frequently have caused- the ruin of companies. It is therefore necessary for the engineer to understand the Federal Labor Law, the rights and obligations of companies and of their workmen, and the reasons for conflicts; to keep in mind the expense which may be caused companies; and to endeavor to avoid difficulties as far as possible. Our labor legislation is primarily to protect the workman and the constant tendency of the tribunals, including the Supreme Court of Justice, is to support the work- man in his demands against employer$, even at times granting him more than he asks, with no limit other than the economic capacity of the company to com-

Jan 1, 1937

By H. F. Bishop, F. A. Brandt, W. S. Pellini

The solidification mechanism of experimental steel ingots (7x7x20 in.) was studied by thermal analysis. It was determined that solidification proceeds in wave-like fashion at rates which are determined by the carbon level, superheat, and mold thickness. The thermal cycles of the mold walls were related to the course of solidification. ESPITE marked advances in the field of solid state transformation, metallurgical research has contributed comparatively little exact quantitative data on the mechanism of solidification of metals. There is, therefore, a great need for such data in the various metallurgical industries. The mechanics of solidification of ingots have been investigated in the past primarily by studies of the rate of skin formation as indicated by bleeding or "pour out" tests. The "pour out" method, however, is a tool which gives only approximate information. In the case of alloys with wide solidification ranges, such as irons and certain nonferrous alloys, the method will not work at all; in the case of alloys of intermediate solidification ranges, such as commercial steels, the information may be misleading. Thus, the general adoption of this method has resulted in divergent conclusions regarding the solidification process. Chipman and Fondersmith1 by means of bleeding tests have shown that the linear growth of a solidifying ingot wall follows a parabola of the general form, D = K C, with the start of solidification delayed until superheat is exhausted, as indicated by the constant C. These tests were carried only to a wall thickness of about 5 in. using an ingot of approximately 17x39 in. in cross-section; hence the latter stages of solidification were not studied. Matuschka2-3 indicated that linear solidification of ingots is rapid at first, then slow, but toward the end of solidification the rate becomes extremely rapid again. Spretnak's4 bleeding studies indicated that, wall growth is expressed more rigorously by two parabolas, and that their point of intersection corresponds to a change of solidification mode from columnar to equiaxed. Spretnak also showed that the K values of the first parabola are always the same regardless of superheat. Nelson bled ingots of square cross-section and found that linear wall growth is initially rapid but decreases continually until the end of solidification. He also concluded that rate of solidification in ingots of square cross-section increases 2.15 pct for every 10 pct increase in cross-sectional area of the mold. The mold ratios considered (ratio of cross-sectional area of the mold to cross-sectional area of the ingot) were all less than 2 to 1. The subject of solidification has also been treated mathematically in many cases, but because of the lack of accurate thermal constants and the simplifying assumptions required, as their authors generally acknowledge, they represent only approaches to the actual conditions of ingot solidification. A third method of studying solidification is the electrical analogue method promulgated by Pasch-kis6-7 and by Jackson and coworkers.8 This method treats solidification as a heat transfer problem with the solidification cycle synthesized on an electrical circuit. Paschkis in his treatment of solidification considered the fact, which was generally ignored, that solidification of steel is not simply the growth of a plane solid wall but a more complex process occurring over a temperature range as indicated by the constitution diagram. Undoubtedly, the anomalous results obtained by bleeding tests arise from the inability to measure quantitatively this mushy condition. The shape of Paschkis' solidification curves are more nearly in accord with those of Matuschka, in that they indicate rapid linear solidification at the beginning and end of solidification with intermediate solidification occurring at a slower rate. Paschkis indicates a definite lengthening of solidification time with increasing superheat. Thermal analysis is a direct method providing exact information for all types of metals regardless of solidification range and was thus adopted in the present program to follow the entire course of solidification from the surface to the centerline of the ingots. The method has the added advantage of being adaptable to following the thermal cycle of the ingot mold during the course of solidification. Test Methods The ingots studied were of square cross-section, 20 in. long, tapered from 71/4 in. at the top to 63/4 in. at the bottom, and fed with a hot top 7 in. in diam and 12 in. high. The molds were uniform in wall

Jan 1, 1953

By R. W. Bartlett

The rates of oxidation of tungsten have been determined at temperatures between 1320" and 3170°C and oxygen pressures to 1 amn using a surface -recession measurement technique. Above approximately 2000°C and 10-6 atm the rate is independent of temperature and can be calculated from gas collision theory assuming a constant reaction probability, e, of 0.06. Oxygen molecules react at surface sites where oxygen atoms have previously chemisorbed. This provides a direct pressure dependence at low pressures but at high pressures tungsten oxide molecule s form an adjacent gas boundary layer which lowers the PO2 at the tungsten surface. A correction for this effect using free-convection theory fits the rate data over the entire oxygen-pressure range from 10-8 to 1 atrn as well as data using O2-A mixtures. Below 10-6 atrn and above 2000°C, e decreases with increasing temperature because of desorption of oxygen atoms. Below 2000°C the rate decreases with decreasing temperature at all oxygen pressures following an apparent activation energy of 42 kcal per mole and depending on (Po2)n with n varying between 0.55 and 0.80. MOST of the previous tungsten oxidation studies have employed gravimetric methods and have been limited to temperatures below 1000°C where the weight loss associated with evaporation of tungsten oxides is negligible compared with the weight gain from oxidation.' At higher temperatures, oxygen-consumption rates have been determined from pressure measurements, usually at constant flow rates, by Langmuir,2 Eisinger,3 Becker, Becker, and Brandes,4 and Anderson.5 The sensitivity of this method decreases with increasing pressure and, with the exception of Langmuir's work, these investigations were confined to pressures below 10-6 atm. Above approximately 1300°C, depending on the oxygen pressure, the rate of oxide evaporation is greater than the oxide-formation rate and the recession of the tungsten surface can be measured optically without interference from an oxide layer. This was first done by Perkins and crooks6 who heated tungsten rods in air pressures from 1 to 40 torr at temperatures between 1300" and 3000°C. The present investigation of the oxidation kinetics of tungsten at high temperatures emphasizes oxygen pressures from 10-6 to 1 atm. This is the range of interest for earth atmosphere re-entry applications of tungsten for which little data were previously available. APPARATUS The apparatus is a modification of the type used by Perkins and crooks.' Ground tungsten seal rods, 6 in. long by 0.125 in. diam, were mounted vertically between two water-cooled electrodes, one fixed and the other having free vertical travel. The movable counter-weighted electrode is prevented from undergoing horizontal displacement by three sets of runners mounted at 120-deg intervals. Electrical contact is made by means of a water-cooled mercury pool. A 24-in. vacuum bell jar having a volume of approximately 267 liters was used as the reaction chamber with the sample holder mounted in the middle of the chamber. Power was supplied from an 800-amp dc variable power supply. Temperature readings were made by means of a Latronics automatic two-color recording pyrometer. With this instrument, corrections for emissivity are not necessary provided the spectral emissivi-ties at two closely spaced wavelengths are equal. Supporting measurements were made with a micro-optical pyrometer corrected for emissivity of bare tungsten and window absorptivity. The micro-optical pyrometer was calibrated against a National Bureau of Standards calibrated tungsten lamp and both pyrometers were periodically checked against the melting points of tungsten and molybdenum using the oxidation apparatus. Above 10-6 atm, pressures were measured with an Alphatron gage calibrated against a McCleod gage. At 10-6 atm, a hot-filament ionization gage was employed. A magnified image of the self-illuminated tungsten rod was formed using a 360-mm objective lens mounted outside the bell jar. When the experiment exceeded 1 hr, the image was focused on a ground-glass plate about 10 ft from the tungsten rod at about X8 and the recession of the thickness of this image was monitored with a Gaertner cathe-tometer. When faster rates were encountered, a 35-mm time-lapse cinecamera with a telephoto lens and bellows extension was substituted for the ground-glass plate and cathetometer. Diameter recession rates were determined from the photograph image projected on the screen of an analytical film reader. EXPERIMENTAL PROCEDURE After installing the rod in the apparatus and cleaning it with acetone, the system was evacuated to 5 1 x 10-5 torr. Before oxygen was introduced,

Jan 1, 1964

By W. S. Reid

In March, 1938, E. P. Fleming, metallurgist for the American Smelting and Refining Co. inaugurated an investigation into the possibilities of recirculating the gases from Dwight-Lloyd sintering machines operating on lead charge, with the twofold object of concentration of the SO2 content and reduction in volume of total gas produced. The possibility of recovering a commercial grade of SO2 gas from D & L machines operating on lead charge had previously been considered by several investigators. Early History of Recirculation The Selby Smelter Commission Report, published by the Bureau of Mines in 1914, contains a chapter by A. E. Wells regarding results obtained at Selby, wherein some of the richer gas was recirculated through a hood over the pallets. Oldright and Miller of the U. S. Bureau of Mines had also made tests at Trail, B.C., and at Kellogg, Idaho. R. C. Rutherford, while at the Chihuahua, Mexico, Smelter of the American Smelting and Refining Co., in May, 1937, proposed recirculation of D & L gases to decrease the volume of gas handled by the baghouse. At none of these plants, however, was the operation commercialized. In July, 1938, Mr. Fleming, in correspondence with the Selby Plant, inquired regarding the possibility of obtaining 6 pct SO2 gas from the Selby D & L machines. At that time, the writer advised that there was slight possibility of obtaining 6 pct SO2 gas without re- circulation, but believed that it was possible with recirculation, and that experimental work toward that end should be tried at some plant where spare D & L machines were available. The foregoing statement was based on the following information then available— 1. Tests on Selby first-over machines showed 2.28 pct SO2 from first windbox and 1.03 pct SO2 from second windbox, and corresponding figures for second-over charge of 0.81 pct SO2 for first windbox and 0.08 pct SO2 for second windbox. 2. Oldright and Miller (US. Bureau of Mines) in 1932 at Bunker Hill, on 42 in. X 22 ft machines found: a. First-over charge—Maximum SO2 concentration (leaving cake) of 9.5 pct. b. First-over charge—SO2 concentration of over 8 pct from the 4 ft to the 12 ft points beyond the front dead-plate and that the concentration then dropped rapidly. c. That approximately 80 pct of the total sulphur eliminated on the second-over machines occurred during the travel of the pallets from the 1 ft to the 6 ft distances from the dead-plate. d. That approximately 94 pct of the total sulphur eliminated on the second-over machines occurred over the first windox. 3. Oldright and Miller (US. Bureau of Mines) in 1932, at Trail, on 42 in. X 50 ft machines found: a. First-over charge—SO2 varied from 2.0 pct to 5.5 pct (leaving cake) from the 12 ft to 28 ft points from the deadplate. b. That the average SO2 increased from 1.0 pct at 7 ft from dead-plate to maximum of 3.3 pct at 20 ft, then dropped to 1.5 pct at 40 ft. c. That on a 22 ft, second-over machine with an 11 in. bed the SO2 varied from 4.5 pct to 6.5 pct from the 2 ft to the 8 ft points from the dead-plate. d. That on the final roast, the SO2 concentration also varied across the pallets; that is, 2 1/2 pct at the side, increasing to 6.0 pct, 5 in. in, and to 7.0 pct at 10 in. to 20 in. in, then decreased vice versa at the opposite side. e. Concluded that most of the sulphur on a 22 ft machine was removed over the first 7 ft of the first windbox; therefore, they partitioned the first windbox so that the exit gas from the second 4 ft section was returned to the surface of the pallets over the fist 7 ft section, and during a seven-day trial the gas from the 4 ft section averaged 2.4 pct SO2, while the recirculated gas from the first 7 ft section only increased to 3.8 pct SO2. (Excess suction over the 7 ft section to prevent escape of SO2 laden gas from the 4 ft section caused dilution by air.)

Jan 1, 1950