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By David J. Mack, T. V. Philip

The effects on the Cu-A1 eutectoid transformation of the addition of a third element from the second long period and from Group IIB of the periodic table, were studied by isothermal transfomation techniques. The valency of the third element shows the most pronounced effect on the eutectoid decomposition. With some exceptions, the atomic size factor of the third element shows some consistent effects on pearlite nucleation and growth. The atomic concentration or the electronegative valency of the third element shows wo consistent effect on the eutectoid decomposition. Addition of the third element helps spheroidization of pearlite. SINCE the pioneering work of Davenport and Bainl on the eutectoid decomposition in steel by the isothermal transformation technique, an enormous amount of data has been accumulated on the eutectoid transformation characteristics of commercial steels. While the eutectoid reaction in steel is of tremendous industrial importance, it appears to be quite unique among the eutectoid reactions. Though the metal-lographic structures developed in the Fe-C and Cu-A1 eutectoids are similar, it is now evident that the two eutectoid reactions are quite dissimilar. The eutectoid decomposition in the Cu-A1 system is more complicated partly due to the appearance of transitional phases in addition to the equilibrium phases. * The first isothermal studies of aluminum bronzes were made by Smith and Lindlief2 and later by Mack,3 Klier, and Grymko,4 and recently Hayne 5,6 A few other systems, structurally analogous to the above, have been studied by the same technique.7-10 Kasberg and Mack1' studied the effects of iron on the transformation of commercial aluminum bronze. The effects of manganese and nickel on this aluminum bronze and those of iron, manganese, and nickel on the binary Cu-A1 eutectoid have been recently studied.12 The object of the present investigation was to study, by isothermal transformation techniques, the effects (with respect to the fundamental factors of alloy formation) of the addition of a third element on the transformation of a Cu-Al eutectoid alloy, 11.8 pct Al. The third elements chosen for the purpose were silver, cadmium, indium, tin, and antimony from the second long period, and beryllium, zinc, and cadmium from group 11B of the periodic table. They were added in nominal amounts of 0.5, 1.0, and 2.5 pct by weight to a eutectoid Cu-A1 alloy. These third elements were expected to show the effects of electron valency, atomic size factor, and electronegative valency effects on the binary eutectoid transformation. PFLEPARATION OF ALLOYS AND PROCEDURE All alloys were made as 400-g heats by induction melting in a graphite crucible with a graphite lid. The molten alloy with a layer of graphite powder on top was stirred at regular intervals by a graphite rod. When the melt was judged to have acquired sufficient superheat, a pinch of common salt was sprinkled on top and any crust scraped off to one side. It was then chill cast into a 5/8 in. rod. The alloys with silver were prepared by remelt-ing the high-purity Cu-A1 eutectoid alloy used by Mack3 with high-purity silver (99.99 pct pure from Hardy and Harmon, Inc.). In the preparation of all the other alloys, polished electrolytic copper shot (from Belmont Smelting and Refining Co.) and high-purity aluminum (99.99 pct pure from Aluminum Co. of America) were used.

Jan 1, 1962

By B. Paul

1. INTRODUCTION It is known that the elastic modulus of a metal may be considerably increased by dispersing

Jan 1, 1961

By Walter O. Snelling

IN combating mine-fires the use of carbon dioxide as a means of producing an atmosphere in which combustion cannot be sustained, has been many times suggested and frequently tried, generally with a fair degree of success. The carbon dioxide is produced by acting on limestone with dilute sulphuric acid, large wooden boxes being used to hold the limestone, and arranged in such a manner that one box may, be cleaned and refilled with blocks of limestone while another is being used in generating the carbon dioxide. The gas is led by means of pipes of large diameter to the location of the fire, tight brattices having been previously put up as close to the fire as possible on every side, so as to limit the space to be filled with the .gas to the smallest possible volume. The cost of producing Carbon Dioxide has been, however, a decided draw-back to the use of this method, and the danger of producing carbon monoxide by the reduction of the carbon dioxide by heated carbon, and consequently bringing about an explosion, has also tended to prevent the application of this method. The use of sulphur dioxide in combating mine-fires has not, I believe, been previously suggested or tried, and yet the method presents such decided advantages over the use of carbon dioxide that it seems proper to suggest the advisability of considering it as a cheap, convenient, and safe means of fighting stubborn mine-fires. 1. Cost, Preparation, etc.-One ton of brimstone, costing from $20 to $30, will produce about 25,000 cu. ft. of sulphur dioxide gas, and allowing for all sources of loss it is probable that sulphur dioxide gas can be produced for about $1,300 per 1,000,000 cu. ft. For carbon dioxide gas, produced by the action of sulphuric acid on limestone, a good estimate would be $4,000 per 1,000,000 cu. ft., provided that sulphuric acid

Sep 1, 1908

By J. E. Johnson

Discussion of the paper of Mark A. Amnion, presented at the Cleveland meeting October, 1913, and printed in Bulletin No. 70, October, 1913, pp. 1167 to 1 79. J. E. JOHNSON, JR., Ashland, Wis.:-Mr. Amnion's paper is of great value and it is not with any desire to reflect. on it that I wish to make some comments on the use of the scleroscope. We obtained one on trial some months ago and made very extensive tests with it, but without getting very satisfactory results. The readings on good car-wheels and bad ones were just about the same, but the factor in its use most likely to produce erroneous results is a variation in the thickness of the specimen being tested. In order to find out something on this subject we cut a thin disk, about -1,: in. thick, off a brass rod; then one 0.25 in. thick, and another about 1 in. thick, put the surfaces of all in about the same condition and tested them with the scleroscope. The readings varied widely; the resilience of the anvil evidently entered to a very high degree on thin pieces. By putting a soft cushion between such a thin specimen and the anvil, and forcing it up against the tube, the softness of the cushion cut off the resilience of the anvil and the results were more like those of the thick specimens. After a thickness of 1 in. was passed, the specimen seemed to have mass enough so that the resilience of the anvil no longer played an important part, and above that thickness results on different materials would be comparable, even though the thicknesses differed. But in order to get comparable results on thin specimens the thickness of those being tested should be the same. I should like to ask how the variations introduced in this way were overcome, so as to get strictly comparable results. Mr. AMMON :-.I have not had much experience in that, but the scleroscope is simply an indication of the surface harden-

Dec 1, 1912

By J. W. Borough

THE electrical conductivity of pure copper is markedly decreased by small amounts of impurity in solution. The magnitude of this effect has been very carefully determined by numerous investigators who studied a wide variety of impurity elements. Much of this work is summarized in an excellent review by Pawlek and Reichel.' The case of zinc impurity in copper is an exception to the above in that there has been no well-documented study of the effect using high-purity starting materials. The values for the effect of zinc on conductivity, which are usually taken from unpublished work by Skowronki, indicate that zinc in low concentration has no effect whatever in lowering the conductivity of pure copper. This effect, if true, is unusual since it is generally known that even in lowest concentration, impurities exert an effect on conductivity which is proportional to the amount dissolved. It is more reasonable to suspect that in the original work on the effect of zinc some of the zinc was oxidized out of solution during specimen preparation. The following experi- and calculated d-spacings based on the unit cell dimensions of Baenziger et al. Since the single crystal studies of Baenziger et al. were limited to (hk0) and (hk 1) data, it was not possible to Compare all the intensities of the powder and single crystal patterns. However, the strongest reflections of both studies, the (321) reflection, agree very well when the appropriate multiplicity factor is used. Good agreement was also found in a number of other reflections of lesser intensity. Despite the precautions taken in annealing the U6Fe powder, an appreciable amount of UO, was detected in the powder pattern after heat treatment. The powder pattern reported by Groganoand Clews is given in Table I. Except for the 3.15A line, which is the strongest line of UO,, their pattern, as far as it goes, compares favoEably with the data from this study. Gordon and Kaufmann have reported a diffraction powder pattern purported to be U, Fe but it bears very little resemblance to the patterns of Table I. ments were carried out to redetermine the effect of zinc on conductivity using high-purity starting materials and processing conditions capable of producing oxygen-free alloys. Materials used in the experiment were ASR 99.999 pct Cu and Cumingo 99.999 pct Zn. Four 1 lb melts were prepared with identical procedure in argon atmosphere with crucibles made from Speer No. 580 graphite. The compositions were 0.0, 0.1, 0.3 and 1.0 pct Zn. Standard No. 14 wire (0.064 in. diam) was made from these melts as follows. The 1 pct Zn sample was first reduced 94 pct by cold swaging with five annealing treatments of 800o for 10 min in hydrogen between swagings, and then reduced 94 pct to the

Jan 1, 1962

By Sylvan Z. Beer

The factors that determine the yield and crystal size in the two-temperature synthesis of A lp were examined. Low yields and small crystals were associated with low temperatures and pressure. Attempts to grow large crystals in the critical and supercritical region of phosphorus were unsuccessful. Crystal size increases markedly at elevated temperatures. Crystals grown at temperatures as high as 1450° C fluo-resced, under uv excitation, at energies close to the estimated band gap of about 2.4 ev, while crystals grown at lower temperatures tended to fluoresce in the red region of the spectrum. Those grown in the supercritical region showed no ALP fluorescence. Heating the high-temperature-grown ALP under vacuum greatly increased its fluorescence efficiency and moved the emission peak to higher energies. I HE III-V compounds, with few exceptions, have been prepared by the two-temperature method. In its classic form this technique is applicable to closed systems where at least one of the components, in this case the column V element, is a liquid or a solid with a high vapor pressure. One advantage of this method over flow systems is in its simplicity. In addition, because it is a closed system, it can, under the circumstances to be described later, be run at higher pressures of the volatile species than in flow systems. In instances where the III-V compound is soluble in the parent III metal to about 1 mol pct or higher, solution growth can be made to take place by slow cooling. This, for instance, is one way in which single-crystal GaP1 and Inp2 have been grown. Initial attempts to synthesize and grow A1P by this technique were not too successful; the yield was low and the crystals obtained were exceedingly small. The conditions required for improving the yield and growth by this technique were, therefore, sought. Two obvious conditions which could be controlling were examined. These were the temperature of the aluminum and the pressure of the phosphorus. The range of temperatures studied extended from about the melting point of aluminum, 660° to about 1450°C. The latter is dictated by the vapor pressure of aluminum which reaches about 1 Torr at that temperature and the limitations of the materials of construction as described in the next section. The pressure range of interest covers from below 1 atm to above the critical pressure of phosphorus, 82.2 atm. EXPERIMENTAL The Temperature of Aluminum as a Variable. A series of experiments were run in the conventional two-temperature manner. All refractories and quartz were dried by heating at 800° to 900° for a minimum of 24 hr, and usually much longer, before use. The aluminum

Jan 1, 1969

By W. W. Gerberich, P. L. Hemmings, V. F. Zackay

ThE strain-induced martensitic transformation may be used to attain desirable combinations of strength, ductility, and fracture toughness. One of the parameters is the relative stability of the austenite. For example, it has been shown by Zackay et al.1 that the volume percent of strain-induced martensite is related to the combination of strength and elongation obtained. It has also been shown that the degree of transformation is an important factor in the crack propagation resistance of metastable austenitic steels.2 Considering both tensile and crack-propagation tests, it was of interest to see if there was any functional relationship between the amount of strain and the volume of strain-induced martensite. Previously,9 it had been shown that at room temperature, there was a relationship between uniaxial tensile strain and the volume percent of resulting martensite given by The data were obtained by plastically elongating tensile samples to a certain strain and then measuring the field strength to determine the strain-induced ferromagnetic volume. This was accomplished for two conditions having yield strengths of 229 and 233 ksi. The nominal composition of this material was 9Cr-8 Ni-3 Mo-2 Mn-2 Si-0.25 C-0.09 N. In evaluation of the strain-induced martensite at a crack tip: the question arose as to whether Eq. [1] would also be valid under triaxial stress conditions. Tests were conducted on 1/2-in. thick plate material having a composition of 9 Cr-8 Ni-4 Mo-2 Mn-2 Si-0.27 C. It was found that sectioning, polishing, and etching of fractured specimens could reveal the strain-induced martensite occurring at a crack tip. Care had to be taken to minimize the final polishing steps so as to avoid a smeared layer of strain-induced martensite. The method for taking metallo-graphic samples from fractured crack-line loaded type samples is shown in Fig. 1. Observations of the strain-induced martensite occurring at room tem-

Jan 1, 1970

By Edward Steidle

Those who have followed the rapid progress in rock-dusting bituminous-coal mines must admit that opinion crystallized during the year just closed in support of this preventive of coal-dust explosions. Up to 1924 only one mining company in America practiced rock-dusting on a large scale, but during 1924 forty-two companies had adopted this safety measure, and the "boom" is expected to extend over the next two or three years. Alabama is represented by 1 company, Colorado by 3, Illinois by 4, Kentucky by 1, New Mexico by 4, Pennsylvania by 20, Utah by 8, and Wyoming by 1. A total of about 500 miles of entry has been dusted. Illinois leads with 275 miles of dusted entries and Pennsylvania holds second place with about 175 miles. In each case there is a sense of great security, not only on the part of the operator but by the miner as well. It is also interesting to note that during 1924 the compensation rating or inspection bureaus in twelve of our coal-producing states revised their rating schedules so that a credit would be given for rock-dusting. This credit ranges from 10 to 20 cents per $100 payroll. Recent drastic federal and state regulations approved by mine operators made rock-dusting compulsory in bituminous coal mines in Utah, beginning July 1, 1924. Legislative action favorable to rock-dusting may be expected in other states. Colorado has already proposed a change in its laws, and Pennsylvania, Maryland, Washington, and West Virginia are giving the matter consideration. If the rock-dusting problem is handled properly and proves to be entirely successful, no mining man of any standing will delay applying it in his mine. State legislation regarding this matter may or may not solve the problem. At present, the mining companies that are rock-dusting of their own choice are doing it carefully and thoroughly. In Utah, some are doing it conscientiously, trying to get what benefits can be obtained while others are reported to be doing it only to keep within state regulations. In any event, if we are to have new legislation, it is essential that the various states know what they are about and then, if possible, work for uniform regulations.

Jan 1, 1925

By Richard Moldenke

Note.—At the request of the American Society for Testing Materials, this paper wau presented at the New York Meeting, February, 1923, in connection with the "A. S. T. M. Tentative Specifications for Foundry Pig Iron" and The Physics of Cast Iron and Its Bearing on All Cast-iron Products and Specifications for Cast Iron," by William R. Webster. The discussion of this paper was not published by the Institute, having been referred to the American Society for Testing Materials, as these papers were again presented for discussion at the meeting of that Society at Atlantic Cit;, June, 1923. The result of these discussions is shown in the following abstract from the Committee A3 report on cast-iron specifications: During the past year, the adaptability of the tentative specifications for pig iron for the steel and the malleable foundry, in addition to the iron foundry proper, have been studied and suitable changes and rearrangements are being made which appear to cover the situation properly. In spite of the experience of foundrymen to the contrary, there is a persistent call from consumers of castinga for defixute compositions for given lines of castings. To respond to this call for information desired by the consumer—information every modern foundryman should have and guide his procedure with—the committee has requested the Sub-committee on General Cast!rigs to take up this matter with a view of constructing tables of analyses rang? for Important lines of foundry product. These analyses ranges however, are to be given as "recommendgd practice" and not intended for actual spkcification. In this way, the consumer of the foundry product will get the information he wants; the furnace-man will be gulded in the production of his pig irons to prepare for analyses ranges which are more closely standardized and have less of "freak" requirements made by Inexperienced metallurgists; and the foundryman will not be bound by chemical requirements he knows will not work out well with his particular reglonal supphes of melting stock. Doctor Moldenke's paper is published in full as it shows clearly the good results of the Institute's work in 1895 and a comparison of the same with the present knowledge of the metallurgy of cast iron—Bradley Stoughton, Chairman, Iron and Steel Committee. In MaRch, 1895, William R. Webster contributed a carefully prepared scheme for the study of the physics of cast iron to the American Institute of Mining Engineers at its Florida meeting. This summary of the interrelation of the chemical and physical characteristics of cast iron with the operations of daily foundry practice caused a wide discussion of the then little understood though universally used material. Mr. Webster has requested the author to bring the subject up to date and, while glad to comply, he must pay that with all the knowledge that has been gained in the quarter century that has passed since the subject was brought to the attention of the Institute—and we now are pretty familiar with cast iron in all its aspects—there is practically noth-

Jan 1, 1923

By Richard Moldenke

Note.—At the request of the American Society for Testing Materials, this paper wau presented at the New York Meeting, February, 1923, in connection with the "A. S. T. M. Tentative Specifications for Foundry Pig Iron" and The Physics of Cast Iron and Its Bearing on All Cast-iron Products and Specifications for Cast Iron," by William R. Webster. The discussion of this paper was not published by the Institute, having been referred to the American Society for Testing Materials, as these papers were again presented for discussion at the meeting of that Society at Atlantic Cit;, June, 1923. The result of these discussions is shown in the following abstract from the Committee A3 report on cast-iron specifications: During the past year, the adaptability of the tentative specifications for pig iron for the steel and the malleable foundry, in addition to the iron foundry proper, have been studied and suitable changes and rearrangements are being made which appear to cover the situation properly. In spite of the experience of foundrymen to the contrary, there is a persistent call from consumers of castinga for defixute compositions for given lines of castings. To respond to this call for information desired by the consumer—information every modern foundryman should have and guide his procedure with—the committee has requested the Sub-committee on General Cast!rigs to take up this matter with a view of constructing tables of analyses rang? for Important lines of foundry product. These analyses ranges however, are to be given as "recommendgd practice" and not intended for actual spkcification. In this way, the consumer of the foundry product will get the information he wants; the furnace-man will be gulded in the production of his pig irons to prepare for analyses ranges which are more closely standardized and have less of "freak" requirements made by Inexperienced metallurgists; and the foundryman will not be bound by chemical requirements he knows will not work out well with his particular reglonal supphes of melting stock. Doctor Moldenke's paper is published in full as it shows clearly the good results of the Institute's work in 1895 and a comparison of the same with the present knowledge of the metallurgy of cast iron—Bradley Stoughton, Chairman, Iron and Steel Committee. In MaRch, 1895, William R. Webster contributed a carefully prepared scheme for the study of the physics of cast iron to the American Institute of Mining Engineers at its Florida meeting. This summary of the interrelation of the chemical and physical characteristics of cast iron with the operations of daily foundry practice caused a wide discussion of the then little understood though universally used material. Mr. Webster has requested the author to bring the subject up to date and, while glad to comply, he must pay that with all the knowledge that has been gained in the quarter century that has passed since the subject was brought to the attention of the Institute—and we now are pretty familiar with cast iron in all its aspects—there is practically noth-

Jan 1, 1923

By Charles L. Harness

STRONTIUM is an essential constituent of celestite (strontium sulphate), of the rarer strontianite (strontium carbonate), and of a few very rare minerals. Celestite is the chief ore but strontianite is more valued except for making the purest strontium salts, because of its ease of processing. The public knows strontium mainly as the source of the red flame in fireworks but it has many other uses. PROPERTIES The celestite of commerce is a massive mineral of varying texture: coarsely crystalline, fibrous, bladed, very fine grained or earthy. The color varies greatly with the nature of the impurities but the purer specimens are light blue (Latin, caelum, sky) or white. The strontianite of commerce is a massive mineral, more or less coarsely crystalline. The color varies with the impurities. Distinctive characteristics are effervescence with acids, density (3.68 to 3.71), and crimson strontium flame. A typical British celestite before World War II analyzed: SrSO4, 96.55 pct; SrCO3, 0.17; BaSO4, 0.25; CaSO4, 0.54; MgCO3, 0.15; R20,, 0.90; Si02, 1.38.10 A German strontianite analyzed: SrCO3, 90.9 pct; CaCO3, 7.5; BaCO3, 0.1; Fe2O3, 0.05; A1203, 0.1; SiO2, 0.04; S, 0.1; P, 0.005.10 ORIGIN AND MODE OF OCCURRENCE According to Clarke,9 strontia forms about 0.02 pct of the crust of the earth and is present in most igneous rocks, but in smaller quantities than barium. Under certain conditions, large masses of celestite are deposited from sea water with anhydrite. The presence of large amounts of celestite in some saline deposits and its absence in others suggests that the deposition of celestite depends on whether certain as yet undetermined concentrations of sulphate and chloride ions are reached in the brines. The most extensive of these sedimentary deposits are those of the Keuper (Triassic) in England, of the Zechstein (Permian) in Germany, and of various Cretaceous formations in Texas, Arkansas, and Utah. Of the deposits of southeastern California and western Arizona,

Jan 1, 1949

By John M. Hartman

An examination as to irregularity of wear around the nose of the Witherbee tuyeres showed a section through the nose near the top as per Fig. 1, and a section only a half-inch beyond as per Fig. 2. The molten iron flowing over the nose of the tuyere had melted off the metal until the water in the tuyere prevented further melting. These tuyeres have a division in the annular water-space (see Fig. 2) to turn the current of water at the top, and the watersupply pipe is carried to within 1 inch of the nose. The constant supply of cold water in the nose of the tuyere kept it well cooled and preserved. But half an inch on the other side of the division the metal had melted off, as is shown by Fig. 1. There was no means of effecting a circulation at this point so long as the water was discharged from the butt of the tuyere. A pipe having been placed on the discharge-side of the division, the same as on the supply-side, in order to secure a circulation of the water at the nose on the discharge-side, it was found that the metal did not burn off. The nose being found to give out at the bottom, a division was placed in the annular water-space at the bottom, terminating 1 inch from the nose. This made a sharp current of circulation in the nose at the bottom, and prevented the burning of the metal there. A positive circulation at the nose, top and bottom, is a necessity with the present fast driving of furnaces, and prolongs the life of the tuyeres. The proper metallic composition of tuyeres is a question constantly agitated. A trial of ordinary yellow-metal* tuyeres was made 12 years ago. They did their work just as well

Jan 1, 1899

By J. C. Wright

A practical program of education for workers of the mining industries is being formulated by the Federal Board for Vocational Education in cooperation with the states in which this industry is a dominant one. The Federal Government last year passed a law, known as the Federal Vocational Education Act, that provides for the promotion of vocational education and for cooperation with the states in the promotion of such education in agriculture and trades and industries and in the preparation of teachers of vocational subjects. More than 1,000,000 men in the continental United States are employed in mines and quarries. The following table, from the 1910 Census Report, shows the relative importance of mining and manufacturing pursuits: Manfactures Mines and quaRRies Employees.......... 7,405,313 1,109,410 Capital............. $18,428,269,706 53,380,525,841 Value of product..... $20,672,051,870 $1,238,410,322 Of the more than 1,000,000 men employed in mining, almost three-fourths are engaged in the production of bituminous and anthracite coal; one-fifth, in the production of copper, iron, lead, zinc, and other metals; and the remainder in getting out structural and miscellaneous materials from quarries. The meeting of the needs of the coal-mining industry, therefore, is the problem of greatest importance in the point of numbers to be served. Moreover, the dangers in coal mining are greater than in metal mining. Practically all states have set up educational and technical standards for the position of foreman, boss, superintendent, etc., and every applicant for these positions must have a certificate of competency. The qualifications, too, are becoming increasingly difficult in the field of technical information. In some states, every miner must have a certificate, which is issued by the mine examining board only after an oral examination. Did these state laws not call for definite and comprehensive plans for the vocational education of men in the mining regions, the conditions

Jan 1, 1919

By J. J. Ormsbee

Attempts at coal-washing have been made in the southern states during the last twenty years; but it is only within the last four or five years that the practice has become at all general. It might perhaps be claimed as one of the blessings derived from our departed " booms;" for, during their sway, the supply of coal of all qualities, good and bad, could not equal the demand; but, with the subsidence of the inflated demand, came imperative calls for fuels of better quality; and washers, previously regarded as luxuries, became necessities. Among those now in use in this section are representatives of the following types or classes: the trough washer; the jig washer; the percussive table; and those washers in which a constant upward current of water effects the separation. Without having full statistics, it is safe to say that there are in successful operation in the South more washers of the last class than of any of the others. The purpose of these notes is to present data with regard to the constructiOn, operation, and results of one of these current-washers, based mainly on the plant at No. 2 Slope, Pratt Mines, Alabama. The coal is mined from the well-known Pratt seam, having here an average thickness of 3 feet 6 inches. It has distinct cleavage-planes, and breaks in cuboidal lumps; is bright black in color, firm in structure, and air-slacks only after considerable exposure. It burns freely, leaving a gray or buff-colored ash. The lump- and nut-coals are used for domestic and steampurposes (chiefly, however, for locomotive firing), and the slack for making coke. The specific gravity is 1.272. Analyses of Pratt Coal. I. 11. 111. IV. Min. Resources Authority. Phillips. McCalley. of U. s.,1892. Lupton. Fixed carbon,. . 67.90 61.600 64.30 63.82 Volatile material,.. 29.80 31.480 32.08 31.85 Moisture,.,...... 1.508 1.07 1.02 Ash,.... 2.30 5.416 2.08 3.31 Sulphur,. .. 0.83 0.918 0.47 0.70

Jan 1, 1896

By H. E. Crum, W. E. Hubbard

This review covers the northern 32 counties of the Texas Panhandle, an area 180 miles square. The westerly three-fourths of the district lies wholly within that great area known as the Llano Estacado or "staked plains." Six of the counties produce oil and gas and three produce gas alone. All of the production is associated with the Amarillo arch, a huge anticline superimposed upon a buried mountain range which is undoubtedly a continuation of the Wichitas of southwestern Oklahoma. Oil Production The production of the Texas Panhandle up to Jan. 1,1930, was slightly over 157 million barrels, 90 per cent. of which came from Hutchinson and Gray counties. About 33,000,000 bbl. was produced during 1930. Though this was about 9 per cent. above the 1929 production, it was over 8,000,000 bbl. less than was produced during the peak year, 1928. The present daily production is slightly over 40,000 bbl., which is the allowable production under state-wide proration. The assumed potential for the purpose of proration is 124,500 bbl. and the actual capacity of the wells probably would be in the neighborhood of 100,000 barrels. The total initial production of the oil wells completed in 1930 was 157,289 bbl. from 308 wells, or 511 bbl. per well, as compared to a 734-bbl. average from the 350 oil wells drilled during the preceding year. The completions in Gray County numbered 232, with an average initial of 614 barrels. Completions During 1930, 526 wells were completed in the Panhandle as compared to a total of 503 during 1929. Of the year's completions, 308 were oil wells, 169 produced gas and 49 were dry holes. Of the 3027 wells drilled in the Panhandle to date, 2780 have produced oil, gas or both, making the ratio of dry holes to producers about 1:11.3. Ignoring the 63 dry holes drilled in nonproductive counties, the ratio becomes 184:2780 or 1:15.1 which is slightly less favorable than that which obtained at the end of 1929.

Jan 1, 1931

By W. M. Hirthe, E. H. Greener, D. R. McCann

It has been proposed1'2 that, at low temperatures, point defects are a strengthening factor in inter-metallic compounds whereas, at high temperatures, the deformation is diffusion-controlled and, therefore, an increase in the concentration of point defects tends to soften or increase the plasticity of a compound. More recent investigations, including those of Bloem and Kroger' on PbS, Kramers and smith4 on TiO, and Nadeau5 on LiF, have extended this concept to ionic crystals. Rutile (TiO2) is a tetragonal transition metal oxide which has a defect structure over at least the compositional range. The defect in near-stoichiometric rutile is either an oxygen ion vacancys or a titanium ion interstitial.' This investigation does not contribute to resolving the defect question but either defect would satisfy the results obtained. Six specimens having the same orientation, see Fig., 1, utilized in an independent investigation1' were cut with a diamond saw from a single-crystal boule purchased from the Linde Co. Three specimens were annealed in air at 1200°C for 4 hr and slowly cooled to room temperature in a period of 12 hr. The remaining specimens were reduced in a vacuum of l0 mm Hg at 1200°C for 4 hr and cooled at the same rate in vacuum. The reduced specimens were weighed before and after reduction and, assuming the weight loss to be oxygen, the corresponding oxygen-to-metal ratio is 1.998. All specimens were chemically polished and etched utilizing the techniques described by Hirthe, Adsit, and Brittain." The specimens were embedded in acrylic resin and mounted on a leveling vise in a Kentron micro-hardness tester. A 200-g load was applied to a Knoop indenter with a descent time of 18 sec and a dwell time of 20 sec. Eight indentations were made on a near (171) surface, approximately 3 deg from the (lii) plane, for each orientation of the major axis of the indenter relative to the crystal structure. The dependence of microhardness on orienta-

Jan 1, 1963

By Emerson F. Heald

A systematic study was made of new and old data on chemical activities in Fe-Pt alloys at elevated ternperatuves. Experimental results may be expressed in terms of the excess free energy using Least-squares analysis of the data gave the following values for the constants: for the temperature range 1130° to 1350°C, and tentatively to 155O°C, B = -3.326564 and C = 0.221051; for the temperature range 650" to 850°C, B = -2.555690, C = 1.762735, and D =0.097196. In the study of iron-containing silicate systems, it is sometimes desirable to have a direct experimental measure of the activity of iron in the system. The well-known solubility of iron in platinum, often a headache in experimental work on iron compounds under reducing conditions, can be used to advantage in this respect. If the activity of iron in an Fe-Pt alloy in equilibrium with the silicate is known as a function of the composition of the alloy, chemical analysis of the alloy will give a knowledge of the activity of iron in all of the phases in the system. The present study was undertaken in order to elucidate the characteristics of Fe-Pt alloys as iron activity indicators. This work is intended to tie together some previous work, which may be summarized as follows. Larson and Chipman1 determined the activity of iron in Fe-Pt alloys at 1550°C by equilibrating platinum metal with calcium oxide-iron oxide-silica melts of known iron activity. Compositions of the resulting alloys were determined by chemical analysis. A similar study was carried out by Taylor and ~uan,' who worked at 1300°C. They brought the Fe-Pt alloys into equilibrium with iron oxide under conditions of known partial pressure of oxygen, and thus, from the work of Darken and ~urr~,~ conditions of known iron activity. Compositions were determined indirectly, by following the change in weight of the sample. Sundaresen et el* used the electromotive force of cells in which the alloy formed one electrode in order to measure the activity of iron in the alloy at 650" and 850°C. These temperatures were chosen to be above and below the first-order phase transition which takes place upon the ordering of Fe3Pt and the second-order transition which occurs upon the ordering of FePt3. EXPERIMENTAL 1) High Temperatures. The starting materials used were thin platinum foil, about 0.002 mm thick, and Fisher Certified reagent ferric oxide, Fez03, which had been heated for 24 hr at 1000°C. An intimate mixture of 80-mesh Fez03 and platinum platelets was placed in a thin platinum foil envelope. The latter was suspended from thin platinum wires in the hot zone of a vertical-tube, platinum-wound furnace of the type described by Muan and ~sborn.~ A capillary gas mixer similar to that used by Darken and Gurry3 was used to prepare a precisely known mixture of carbon dioxide and hydrogen, which was allowed to flow upward through the furnace tube. The partial pressure of oxygen in contact with the sample was thereby fixed at a value which was calculated from the charts prepared by porter? Temperatures were measured with a Pt-10 pct Rh-in-platinum thermocouple, which was calibrated using the melting points of gold (1062 .@C) and diopside, CaMgSizOB (1391.5"C). Temperature control was maintained to within i3"C with a Geophysical Laboratory proportional controller, using the furnace resistance as the sensing element. Samples were quenched by passing a small current through the platinum suspension wires, allowing the sample to drop into a bath of dibutyl phthalate at the bottom of the furnace tube. Prior to chemical analysis the samples were washed with acetone and dried. 2) Chemical Analysis. It proved possible, in almost all cases, to separate the Pt-Fe platelets physically from particles of iron oxide. The platelets were dissolved in a small volume of aqua regia, evaporated to dryness, and redissolved to 0.1 M HC1. In order to determine iron in the platinum alloy potentiometrically, it is necessary first to remove the platinum. A 10-cm column of Amberlite IR-120 cation exchange resin in the hydrogen form provided separation quickly and quantitatively: The mixture of iron and platinum in 0.1 M HC1 was added to the top of the column, and washed with about 100 ml of 0.1 M HC1. Under these conditions, the iron, principally in the form of cations such as FeC1" and FeCl;, is held quantitatively in the uppermost centimeter of the column. The platinum, in the form of anions such as PtC&- , is washed through without being adsorbed. After a qualitative test with stannous chloride indicated all of the platinum was removed, the iron was

Jan 1, 1968

By B. A. Joyce, R. W. Bicknell, R. J. Bennett, P. J. Etter

Epitaxial layers of silicon have been grown on single-crystal quartz and alumina by two types of chemical reaction the hydrogen reduction of trichlorosilane and b) the pyrolysis of silane. These reaction systems are described. The cqsfallography of the two systems, as determined by electron and X-ray diffraction, is discussed, and epitaxial mechanisms suggested. The electrical behavior is briefly considered, and the design and properties of field-evert devices fabricated in the epilaxial material are also discussed. RECENT work carried out in these laboratories" has shown that it is possible to obtain epitaxial deposits of silicon on single-crystal quartz and alumina. The purpose of this paper is to describe the method of preparation of these layers using both the hydrogen reduction of trichlorosilane and the pyroly-sis of silane, to compare the crystallographic behavior of films on the two substrates, and to present some initial results of the electrical behavior of silicon layers on alumina. The structural study has been carried out using electron and X-ray diffraction and electron microscopy. The electrical assessment has been made in terms of conductivity and mobility determinations by the van der pauw3 technique, and by measurements on metal-oxide-semiconductor assemblies. 1) FILM PREPARATION Both quartz and alumina substrates, approximately 1 sq cm in area and 0.4 mm thick. were prepared from slices cut parallel to within a few degrees of (11.0), (10.0), and (00.1), and polished mechanically down to about 0.3 p diamond grade. Chemical polishing of alumina slices, using phosphoric acid at elevated temperatures, has also been used; epitaxial silicon layers have been grown on these substrates, but the process is not entirely reliable, possibly because the large strain present in the Verneuil-grown alumina crystal affects the chemically prepared surface. The two reaction systems are fairly conventional and are described briefly below. a) Trichlorosilane-Hydrogen System. The apparatus is shown schematically in Fig. 1. The substrate was heated by induction, with a fused-quartz encapsulated graphite hemicylinder as susceptor. The procedure for carrying out a deposition was to heat the substrate to reaction temperature in a stream of

Jan 1, 1965

By E. W. Johnson, M. L. Hill

Equilibrium concentrations of hydrogen in iron were measured at H2 pressures up to 136 atm and temperatures down to 145°C. Residual hydrogen was prominent near 600°C in air-melted but not in vacuum-melted iron. The diffusible hydrogen solubility is abnormally high below 390°C, confirming the hypothesis of hydrogen trapping.' It appears that the traps for hydrogen in iron form suddenly on cooling. The estimated H2 pressure in equilibrium with 5 ppm hydrogen in steel at room temperature is less than 1000 atm. It was shown previously1 that the diffusivity of hydrogen in a-Fe below 200°C is anomalously low, a behavior attributed to the presence in the metal structure of hydrogen "traps." The energy of the trapped hydrogen was computed as 4.8 kcal Per g-atom below that of the interstitially dissolved hydrogen. The strongest confirmation of the trap hypothesis should be obtainable from measurements of the hydrogen solubility at low temperatures. such measurements have been performed and are reported in this paper. The "residual hydrogen" effect1'' must be carefully controlled if valid measurements of the solubility are to be obtained, and such an effort was made in the present work. Previous data for the solubility of hydrogen in iron have been summarized by Geller and Sun.3 Their equation for the most probable solubility at 1 atm in a-Fe above 400°C is

Jan 1, 1962

By Colin G. Fink, Leslie G. Jenness

Tantalum and columbium occur together in tantalite and columbite ores, which may be considered as ferrotantalate (FeTaz06), with part of the iron and tantalum replaced by manganese and columbium respectively, the general formula, therefore,becoming (Pe, Mn)O.(Ta, Cb)2Os. The ratio of tantalum to columbium is not fixed; the amount of tantalum may vary from one-third to three times that of columbium. Minerals having a high content of tantalum are called tantalite, while those possessing larger amounts of columbium are classified as columbite ores. These minerals are found in pegmatites and often occur in veins associated with cassiterite and wolframite, and may contain small amounts of tin, tungsten, titanium and si1ica. l Methods of Extraction Several methods have been proposed for the extraction of tantalum and columbium from their ores, among them being: 1. Fusion with Potassium or Sodium Bisu1fate.—The finely ground ore is fused with potassium bisulfate, after which the mass is boiled with water and the fusion repeated several times. The residue finally resulting is digested with ammonium sulfide to remove traces of tin and tungsten, boiled with hydrochloric acid, filtered and washed. These oxides are then dissolved in hydrofluoric acid, the silica evolved as silicon tetra-fluoride and the hydrofluoric acid solution used for the potassium double fluoride separation of tantalum. 2. Fusion with Sodium Carbonate and Sodium Nitrate.2—This fusion renders the tantalum and columbium soluble, and they are extracted

Jan 1, 1931