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By Charles S. Barrett, F. W. Steadman

DEFORMATION bands of surprising regularity are found in large-grained polycrystalline copper after cold-rolling (Fig. I). Individual bands frequently are large enough to permit a determination of their orientation by means of etch pits and an optical goniometer. Measurements have been made on 21 areas in seven different grains, and these, combined with X-ray studies of nine single crystals that had been cold-rolled after mounting in a polycrystal-line block, have contributed to a better understanding of the preferred orientations in rolled copper just as similar studies have for rolled iron' and brass.2.3 Particular attention was given to determining orientations that are stable during rolling and to the manner of fragmentation and rotation of unstable grains. The possible role of twinning was also carefully investigated. The texture of polycrystalline copper after cold-rolling is well established by the pole figures that have been plotted by Schmid and Staffelbach,4 Iweronowa and Schdanow,5 and Brick and Williamson,3 all of which are in substantial agreement. There has been some divergence in the list of individual "ideal" orientations that have been used to describe the texture by these observers and others,6 although the orientation (110) [112]-that is, (110) parallel to the rolling plane and [112] parallel to the rolling direction-is generally recognized as the most prominent orientation and (I12) [111] one of the lesser orientations. Other orientations have been given by some observers as (236) [533], (100) [001], and (I 10) [001]. The texture of copper has also been described as (135) [533].6.1 The sum of these orientations provides a reasonable approximation to the complete pole figure, but it does not follow that these specific orientations are necessarily of fundamental significance, for the choice of indices is arbitrary, within limits. Furthermore, a detailed investigation of the ideal orientations in cold-rolled iron discloses continuous ranges of equally favored positions rather than definite positions of high stability,1 and similarly Brick's observations in a single crystal of a brass2 suggest that all orientations in the range between (110) [113] and (110) [117] are about equally stable. MATERIALS AND METHODS The material used was vacuum-cast electrolytic copper kindly supplied by L. L. Wyman, of the General Electric Co.* Slices 1/2 in. thick and 2 1/2 in. square, cut from the ingot, were rolled with 50 per cent reduction per pass to final thicknesses between 0.02 and 0.04 in., and etched to develop cube-face etch pits suitable for goniometric work.8 The etch was light on some strips and deep in others.

Jan 1, 1942

By Clarence Zener

THE internal friction of nonferrous metals vibrating at low stress amplitudes has so far always been successfully interpreted in terms of inhomogeneities of one sort or another. Examples are the fluctuation of stress across a specimen vibrating transversely,1,2,3 the stress inhomogeneities due to the elastic anisotropy and partial random orientation of the individual crystallites,4,5 localized weak regions introduced by cold-working,6,7 grain boundaries and possibly twinning planes.8,9 Perfect single crystals are, by definition, homogeneous. Actual single crystals usually, perhaps always, contains some imperfections. The present investigation. was undertaken to determine whether the internal friction of single crystals may likewise be attributed to inhomogeneities. This study was made possible through the gift of a large single crystal of 70-30 alpha brass by H. L. Burghoff, of the Chase Brass and Copper Co. The specimen, ½ in. in diameter and 10 in. long, was similar to samples previously described by Mr. Burghoff.10 EXPERIMENTAL METHOD The experimental method used has previously been described in Institute papers.5,6,9 The measure of internal friction adopted here, 1/Q, is (1/p) X the logarithmic decrement, a measure used by some writers, and is also (1/2p) X the specific damping capacity, a measure used by other writers. In all measurements the stress level was kept so low that the measurements were independent of stress level. In all measurements in which the temperature was varied, observations were made as the specimen slowly cooled from its highest temperature. The specimen was vibrated transversely. Observations were made at the funda¬mental frequency and at the first overtone, of about 620 and 1710 cycles per second, respectively. No attempt was made to avoid acoustical losses. EXPERIMENTAL RESULTS The specimen was annealed for several hours at 450°C. The temperature dependence of the internal friction was then determined from room temperature to 400°C. As shown in Fig. 1, the internal friction increased by only a factor of 2 from room temperature to 300°C., then by a factor of l00 during the next 100° interval. These measurements are consistent with the view that the observed internal friction is the superposition of two distinct parts. One, dominant at room temperature, is nearly independent of temperature. This part may be accounted for by acoustical losses and by transverse thermal currents. It was not further investigated. The second part, when plotted in the manner of Fig. I, lies upon a straight line. Therefore it has a heat of activation H; i.e., it varies with temperature as Internal friction e~H/RT [I]

Jan 1, 1942

By George A. Packard

The experiments here described were made under my supervision while temporarily acting as head of the Department of Metallurgy at the Missouri School of Mines, at Rolla. The work was done by Messrs. W. E. Brown, W. C. Richards, and F. L. L. Wilson, and the description of the results forms a portion of a thesis presented for the degree of Bachelor of Science. These results are submitted because I have seen no description of the application of pot-roasting to the treatment of a copper-concentrate. This work followed that already described in the discussion of the Lime-Roasting of a Galena-Concentrate,' and was similarly occasioned by the lack of a furnace of the reverberatory type in which the copper-concentrates could be smelted. The material for the tests was a mixture of three lots available. The first consisted of 8-mm. ,jig-concentrates and the second of 0.5-mm. table-concentrates, from the San Juan district, Colo. Both contained pyrite, chalcopyrite, and galena. The third was a lot of copper-ore, found in the laboratory, which had been crushed through 8-mm. screen, and had at some previous time, before the laboratory roasting-furnace was torn down, received a partial roasting. The analyses of these ores are given in Table I. In order to determine the applicability of pot-roasting as to each lot of ore, and the effect of varying proportions of lime, six preliminary tests were made in a " size N " Battersea crucible, 9 in. high by 6 in. in diameter at top, with a 5/8-in. hole bored through the bottom. The crucible was set in the upturned elbow of a 2-in. pipe, the joint being luted with clay; and air was obtained from a receiver supplied by a compressor. The

Jan 1, 1908

Members whose deaths were reported from Apr 9, 1921 to Apr 7, 1923 Elected Died 1876 ABADIE, E R. 1923 1906 ADAMS, ARTHUR K 1920 1902 AHLES, ROBERT L 1921 1876 Akerman, Richard 0000 1884 ALEXANDER, CURTIS 1921 1918 ALLEN, CARL A 1923 1880 ALMY, WILLIAM F 0000 1893 AMSDEN, 0. B 1923 1917 ARGALL, P. H 1922 1917 ARNOLD, E C 1921 1914 ASANO, K 1921 1920 AUGUSTINE, ALBERT BEARSS 1922 1906 BAIRD, GEORGE A 1921 1921 BALDWIN, GEORGE P 1922 1920 BASKERVILLE, CHARLES 1922 1915 BENSEL, J A 1922 1890 BENSON, A J 0000 1912 BEST, WILLIAM NEWTON 1922 1892 BILHARZ, OSCAR M 1923 1890 BLACKSTONE, RICHARD 1922 1921 BLOOM, GEORGE BARNETT 1921 1905 BOSTWICK, WILLIAM A 1922 1884 BRANNER, JOHN C 1922 1920 BRIDGE, SAMUEL D JR 1921 1893 BROWNE, ARTHUR, 1922 1871 BUCK, STUART M 1921 1897 BURGER, C C 1922 1882 BURT, CHARLES S 1921 1921 BUTZ, Louis N 1922 1917 CAMPBELL, DONALD G 1921 1915 CAPLES, JAMES WATTS 1919 1892 CARLETON, JAMES G 1922 1914 CARUTHERS, A WAYNE 1922 1911 CHASE, FRED M 1921 1892 CLEMENT, F H 1922 1922 COAN, WALTER ERLING 1923 1872 COGSWELL, WILLIAM B 1921 1881 COLVIN, VERPLANCK 1920 1882 COOLIDGE, WALTER G 1922 1907 CORKILL, FREDERICK 1922 1912 COX, Guy H 1922 1883 CUNNINGHAM, JAMES S 1921 1873 DAGGETT, ELLSWORTH 1923 1916 DAULTON, THEODORE M 1921 1888 DICKERMAN, ALTON L 1921 1902 DIEFFENBACH, H M 1921 1911 DUNSTAN, SIMON P 1920 1917 DYNAN, ALAN E 1922 1920 EASTWICK, THOMAS H A 1922 1876 EDWARDS, J WARNER 1921 1914 ELDER, ROBERT B 1923 1885 EMMONS, ARTHUR B 1922 1911 ENGEL, GEORGE W 1920 1887 FERNOW, B E 1923 1879 FIRMSTONE, H1922

Jan 1, 1923

Adams, Bernard, Student, South Dakota School of Mines. Rapid City, S. D. '30 Ahlskog, Harold A., Student, Washington State College Pullman, Wash. '30 Aldridge, John, Student, New Mexico School of Mines Socorro, N M. '30 Almstrom, Adne A., Student, Met. Engrg., Washington State College Pullman, Wash. '29 Ancell, Virgil F., Student, Missouri School of Mines Rolla, Mo. '30 Ankudinoff, N., Mill Draftsman, Arthur G McKee & (:o., 2422 Euclid Ave., Cleveland, Ohio. '30 Apablasa, Salvador C., Student, Univ. of California Los Angeles, Cal. '31 Armstrong, Robert H., Student, Lafayette College Easton, Pa. '31 Armstrong, Thomas E., Student, Univ. of California Los Angeles, Cal '31 Aud, Robert A., Student, Lafayette College Easton, Pa. '30 Backus, Robert Small, Student, Mass.- Inst. of Tech . Cambridge, Mass. '30 Bailey, William C., Student, Univ. of California Los Angeles, Cal '30 Banning, Lloyd H., Student, South Dakota State School of Mines Rapid City, S D. '81 Barclay, M. G., Student, Colorado School of Mines Golden, Colo. '30 Barger, Thomas, Student, Univ. of North Dakota Grand Forks, N. D. '29 Barker, C. L., Student, Colorado School of Mines Golden, Colo. '30 Barker, Edgar Morgan. Student, Univ. of Utah Salt Lake City, Utah. '31 Barnwell, Earl E., Student, Oregon State College. Corvallis, Ore. '30 Bartholomees, Geo. C Box 304, Bonne Terre, Mo. '29 Bartholomees, Louis P., Student, Colorado School of Mines Golden, Colo. '30 Bary, Robert L., Student, Univ. of Kansas Lawrence, Kans. '30 Basham, Lester G., Student, South Dakota School of Mines Rapid City, S D. '31 Bates, Walter H., Student, School of Mines, Univ. of Utah .. Salt Lake City, Utah. '30 Beardshear, George T., Student, South Dakota State School of Mines.Rapid City, S D. '31

Jan 1, 1923

By Ray W. Amstutz

The shaft was drilled on US government land m the Piceance Creek basin and was funded by the US Bureau of Mines (USBM). It was drilled to 723 m to provide access to rich deposits of oil shale, nahcolite, and dawsonite for geotechnical test work and environmental mining research. Rotary drilling and dual-string, reverse-air, jet-assist circulation methods were used. Drilling required eight months. Site preparation, running, and cementing the casing required another four months. A 2.44-m ID steel welded casing, 508 mm thick was installed and 2.7 kt of cement were slurried and pumped into the annulus.

Jan 1, 1982

By M. D. Banus, M. B. Bever, A. K. Jena

The heals of formation at 78", 195, and 273°K of the ternary compound h3SbTe2 based on the elements and based on the binary compounds In Sb and [inTe have been measured. The heats of formation at these temperatlcres of the binary compounds In Sb and In Te based on the elements have also been determined. Heal contents and free energies of the three compounds have been calculated from 0° lo 80I)°K. The free energies of joyrrzalion, heats of formations, and entropies of formation at 298°K have also been calculated. The results shown that the tertnary compound is metastable with vespecl to InSh and ln Te below 696 °K. bul is slable above that temperature. The weaker bonding of results in a positice entropy of formation which with incrensirzg temperature makes increasing negative conlvihtclions to the free energy and above 696°K renders the compound slable. THE ternary compound In3SbTez occurring in the quasi-binary system In Sb- In Te' forms on cooling at 829°K by a peritectic reaction.' Observations at 673" and 573 K have shown that this ternary compound decomposes slowly into the binary compounds InSb and1n~e.l'' It has not been possible to analyze the metastable behavior of the ternary compound because up to the present time data on its thermodynamic properties have been lacking. Some information on the binary compounds, however, is available. The heat of formation of InTe at 273°K and its free energy at 673°K are kn~wn.~'~ The heats of formation of InSb at 78", 273', 298", and 723°K have been measured5-' and its heat capacity between approximately 12" and 300"Kg9l0 is also known. In the investigation reported here the heats of formation at 78% 195% and 273°K of the ternary compound In3SbTez have been measured. The heats of formation of the binary compounds InSb and InTe at these temperatures have been obtained by combining new calorimetric results with previously published data. The heat contents and free energies of the three compounds at various temperatures from 0" to 800°K have been calculated. Against the background of this information, the metastability of the ternary compound will be discussed. 1) EXPERIMENTAL 1.l) Preparation of Specimens. The materials used consisted of the elements indium, antimony, and tellurium, the binary compounds InSb and InTe, and the ternary compound In3SbTez. The elements, obtained from American Smelting and Refining Co., had a nominal purity of 99.999+ pct. The compound InSb was Cominco semiconductor grade; the compound InTe was prepared from the elements by melting under a vacuum of 10-h m Hg followed by slow cooling. Three batches of specimens of the compound In3SbTez were used. One batch was prepared by melting appropriate amounts of the elements in an evacuated and sealed Vycor tube. The melt was held at approximately 100°K above the liquidus for about 8 hr, shaken repeatedly, and quenched into a mixture of ice and water. The specimen was annealed in vacuum at 760°K for 4 weeks. In preparing a second batch, a mixture of the component elements was melted and quenched in water. The resulting ingot was powdered. The powder was pressed into pellets, which were annealed in vacuum at 748" to 773°K for 4 weeks. A third batch was prepared in the same manner as the second, except that the starting materials were InSb and InTe rather than the elements. Metallographic examination of samples of the three batches and X-ray diffraction examination of a sample of the second batch did not reveal evidence of microsegregation or a second phase. The results obtained with the three batches showed no systematic differences. 1.2) Calorimetry. The calorimetric method has been described in detail." Samples of the compound In3SbTez, mechanical mixtures of InSb and InTe in the proportion of 1:2, and mechanical mixtures of indium, antimony, and tellurium in the proportion of 3:1:2 were added to a bismuth-rich bath at 623°K in a metal-solution calorimeter. These additions were made from 78°K (liquid nitrogen), 195°K (dry ice and acetone), and 273°K (ice and water). The heat effects of the additions were measured. The difference in the heat effects of the additions of a compound and the additions of the mixtures of its constituents, adjusted for differences in the concentration of the bath, is the heat of formation of the compound. In the concentration range not exceeding 1.5 at. pct solute, the heat effect of the additions was a linear function of concentration. The heat of formation refers to the temperature from which the additions were made, namely, 78", 195", or 273°K. Several calibrating additions were made in each calorimetric run. The calculated heat capacity of the calorimeter and hence the calculated heat effects of the additions of samples depend upon the values adopted for the heat contents of the calibrating substance. In this investigation bismuth at 273°K was used and a value of 4.96 kcal per g-atom was taken for (HGZ3"k . 2) RESULTS AND DISCUSSION 2.l) Heats of Formation. The heats of formation of the ternary compound In~SbTez from the component elements indium, antimony, and tellurium and from

Jan 1, 1968

By Donald E. Meyer

High current-low voltage EB-gun evaporation in an oil-free ultra-high vacuum system was found to be necessary, though not sufficient, for stability (300°C, 106 v per on) of aluminium gate MOSFET's and MOS capacitors not stabilized by a phosphorous glaze. five characteristics of the equipment used: 1) Vacuum purification of the aluminum charge, 2) Ionization of the evaporant by the electron beam, 3) X-ray formation, 4) Residual gases during evaporation, and 5) Metal film structure were studied as Possibly significant in MOS fabrication. EVAPORATION of contact metals common to the semiconductor industry historically has been accomplished with oil diffusion pump systems and various resistance heated evaporant sources as dictated by the type of metal evaporated. To meet a need for greater reliability of semiconductor devices, other metallization methods were developed. A good example would be application of the moly-gold contact system to integrated circuits with deposition by RF or triode sputtering.' More recently, fabrication of stable metal-oxide-silicon devices and circuits has put new demands on metallization. The purity of the thin metal films composing MOS structures is critical, particularly at the metal-oxide interface, and ultra-high vacuum metallization using sputter-ion pumping and electron beam gun (EB-gun) evaporation are well suited for the task. At this laboratory aluminum has been the most common contact-gate metal for both MOS capacitors and MOSFET's. In the earliest work with MOS capacitors, aluminum was evaporated from wetted tungsten filaments using both diffusion pump and ion pump vacuum systems. In spite of clean oxide techniques these capacitors were unstable under bias-tempera-ture stressing. Only after a switch to EB evaporation of aluminum were stable capacitors produced. Using the same techniques it was possible to make MOSFET's with equivalent stability. Stability data for a discrete MOSFET is shown in Fig. 1. This is a "clean" oxide gate (no phosphorus stabilization or no etch back of a thicker gate) having a thickness of lOOO? thermally grown on the (111) plane. Gate length after diffusion was 0.24 mils, and the devices were hermetically sealed. Stressing conditions were 300°C and 106 v per cm applied alternately as a positive and negative field for 10 min, 50 min, and 4 hr for a total stress time of 10 hr. An initial shift in turn-on voltage of 0.1 v was detected for 10 min of positive bias. All evidence at this laboratory indicated that while EB-gun evaporation of ultra-high purity aluminum was not sufficient for 300°C stability, it did seem to be necessary. There may well then be something inherent in the EB-gun deposition used which enhanced stability, and probably no single factor existed but rather a series of factors. It is the purpose of this paper to report on some of the investigations carried out to learn more about EB-gun evaporation in ultra-high vacuum systems. EXPERIMENTAL DESCRIPTION The EB-gun was self accelerated, had a maximum power rating of 10 kw, and used a water-cooled copper crucible able to hold a 20-g aluminum charge. The electron beam was bent 180 deg and focused by an electromagnet which also provided movement of the beam across the crucible. Normal power conditions in this work were 9 kv and 300 to 600 mamp. The gun can be described as high-cur rent/low-voltage and was quite different in its mechanism of operation from EB-guns with much higher acceleration potentials. An oil-free vacuum system capable of 5 x 10- l0torr, a quartz crystal rate and thickness monitor and a quadruple mass spectrometer completed the evaporation system, Fig. 2. A typical evaporation cycle consisted of a 3 to 4 hr pumpdown to the upper l0-9 range and evaporation at l0? per sec with the pressure in the bell jar not rising above 1 x 10"7 torr. Thickness control was 5 pct or less and could be automatically monitored and controlled. Five phenomena associated with the EB evaporation and considered as possible contributors to Ma performance included a purification effect, ionization of evaporating aluminum, X-rays, constitution of vacuum ambient during evaporation, and film structure dependence upon evaporation rate. These phenomena are now discussed. Vacuum Purification. The design of the EB-gun permitted purification of the aluminum charge by vacuum outgassing. Particular features included an efficiently water-cooled copper hearth with a capacity of over 20 g of aluminum and the capability for sweeping the beam across the charge. Such capacity meant that aluminum had to be added only after about every fifth evaporation. A new charge was not required each evaporation as is necessary with filament evaporation. An oxide "scum" which appeared on the charge could be completely cleared from the top hemisphere of the charge by sweeping with the beam prior to opening the shutter. An indication of the purifying effect was obtained by a series of analytical measurements on incoming aluminum, after melting but with little vacuum out-gassing, after 30 min outgassing, and the evaporated film itself. Either a solids (spark source) mass spectrometer or an emission spectrometer were used for analyzing the aluminum charge. Analysis of the evapo-

Jan 1, 1970

By N. M. Langdon

Spokane Meeting, September, 1909.) THE following corrections to the paper of Mr. Langdon (Bulletin No. 34, October, 1909, pp. 919 to 940), received after the publication of the paper in the Bulletin, will be incorporated in the paper as finally published in the forthcoming Vol. XL. of the Transactions, but are here presented for the information of members:' Page. 921. Table I., furnace M2, item 11. For " 8801 " read "0.8801." 922. Table II., furnace C, item 2, under gas. For " 0.011 C " read " 0.011 0." Furnace G, item 13, under gas. For " 5.074 air " read " 3.074 air." Item 15, 114.269 " should be " 4.289." Furnace H, item 2, under iron. For " 0.04 " read ".0.01." 923. Table II., furnace J, item 1, under iron. For " 0.95 " read " 0.93." Furnace N2, item 6, under gas. For " 0.66 CO," read 0.066 C02." 924. Table III., furnace C, item 17. For " 379 " read " 397." 927. Table IV., furnace C, item 4. For " 0.0124 " read 0.0424." Furnace G, item 15.. For " 4,060 " read " 4,066." 928. Line 2. Items 19 and 20 of heat-supply, should be items 20 and 21. 930. Line 3. Expunge remainder of paragraph after the word " supplied," and substitute the following : "As compared with the fusion-zone, the loss by radiation n C was 25.5 per cent. of the total (2,278 units) supplied to that zone, while in D it was 22.5 per cent. of the total heat (1,824 units) supplied to that zone. Finally, as compared with the reduction-zone, C lost by radiation 36.8. per cent. of the 1,580 units supplied to that zone,

May 1, 1910

By G. S. Cole

The temperature has been measured ahead of stationary solid-liquid interfaces under conditions approximating luzidirectional heat flow and therefore unidirectional solidification. Natural convection flow patterns may be deduced from the temperature distributions , temperature fluctuations, and shape of the interface. Fluid flow increases with the height and the rate of heat transfev through the interface and this is further manifested by a deviation of the interface from aflat vertical plane. The influence of fluid flow on solute inhomogeneity during alloy crystal growth can be inferred from the observed temperature distributions. A buoyancy force exists in the liquid ahead of a vertical solid-liquid interface, caused by a difference in density between cold fluid near the interface and warmer fluid in the bulk liquid. When the viscous and inertia forces in the melt exceed this buoyancy force, a flow of fluid takes place, termed natural or free thermal convection. Natural convection in purely liquid systems has been extensively studied for many years. 1"u On the other hand, fluid flow during horizontal crystal growth has oniy recently been the subject of experimental investigation."-25 The requirements for horizontal crystal growth differ from other heat flow systems. The small aspect ratio (ratio of height of cold wall to length of fluid) has never been considered. The uniform furnace gradient which supplies heat radially (and not necessarily symmetrically) differs from previous boundary conditions of uniform heat flux at the cold and hot ends. And most important of all an isothermal s/l interface is present which can adjust its shape and position to conform to heat and fluid flow. All of these boundary conditions involve complexities which cannot be readily solved analytically. Preliminary observation has demonstrated the penera1 shape of the natural convective flow pattern in transparent media.20'24'25 The flow is circulatory, directed toward the interface at the surface of the liquid, down and away from the interface at the bottom, and then up at the hot end of the melt. During crystal growth such a flow may interact with the solute boundary layer at the s/l interface to affect solute incorporation.M'1B|28'i!T Evidence has also been presented recently to show that thermal convective flow will affect the structure of ca~tin~s.~~-~~ The rate of heat transfer (conduction plus convection) in a given fluid system is a function of the temperature difference between the hot end of the liquid and the s/l interface and the height of the interface. At the lowest values of these variables* all heat is *It has been shown' that adverse temperature gradients as low as O.OOS°C oer cm are sufficient to cause convection. transferred by conduction. When the temperature difference or interface height are increased, laminar fluid flow commences and heat transport takes place by laminar convection as well as by conduction; turbulent heat transfer takes place at higher values of these variables. In the transition region between laminar and turbulent flow, boundary layer separation takes place; fluctuations in temperature are also noted and increase in amplitude and frequency as turbulence becomes dominant. In this paper, fluid flow patterns in the melt ahead of a stationary interface are deduced from observations of temperature distribution and fluctuations, heat flow rate, and interface shape. The fluid flow ahead of advancing interfaces and the effect of such flow on solute incorporation may be inferred from these measurements on stationary interfaces. Observations during enforced fluid motion will also be considered. EXPERIMENTAL PROCEDURE The metal was contained in a lava boat 10 cm in length, 1+ cm in width, and 2 cm in height, as shown in Fig. 1. A water-cooled, molybdenum block heat-sink is at one end of the boat; surrounding this assembly is a slotted stainless-steel tube noninductively wound with a nichrome heating element. Temperature was measured by 38-gage Chrome1 vs Alumel thermocouples sheathed in 0.05-cm-diam graphite-coated stainless-steel tubing, which were moved longitudinally and vertically through the melt by means of a two-dimensional motorized micrometer stage. In some experiments the thermocouple junction was exposed, but in the majority of experiments the junction was welded to the sheath tip; no significant difference

Jan 1, 1968

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

By Emile Gyss

THE speed of drilling rock has become an impor-tant factor in mining operations, while the place-ment of holes, kind, and quantity of explosive used. are equally important. These are a function of the rock hardness and toughness. Both of these fac-tors must be considered in compiling a table that will enable a mine operator or engineer to estimate drilling speeds in a given rock, knowing its hardness, and from its toughness, the dynamite required. The hardness of a homogeneous rock may be defined as its resistance to a penetrating medium, such as a drill-steel bit, and toughness, its resistance to with-stand rupture by the tearing apart of its minerals or parts of the same mineral. Rock hardness, as it has here been defined, is a function of the hardness of the component grains composing it, as well as grain size, shape, arrangement, and binding minerals. Rock tough-ness depends on substantially the same factors, but is measured by a totally different method. The units in which rock hardness is usually ex-pressed are either relative values or alphabetical desig-nations which carry no definite quantitative meaning. R. M. Raymond has suggested the measurement of com-posite rock hardness, based on mineral hardness as ob-tained by the Moh scale. This is done by multiplying the percentage of each mineral in a rock by the Moh mineral hardness and dividing by 100. These values convey a clearer conception in the minds of men in-terested in rock work -and are the basis of the units used in Tables 1 and 2. The hardness of rocks as it has been variously de-fined may be determined by different methods. The first method is one in which the proportionate average of the hardness of minerals making up a rock is the basis for classification. The other factors of grain size, shape, arrangement, and binding power are not considered.

Jan 6, 1927

By C. J. Huffman

MAGNESIUM alloy tubing and hollow shapes are finding increasingly wider usage in practical applications today. Square and rectangular tubing and hollow shapes find [ ] greater diversification in use than standard round tubing. Typical applications are roller conveyors, ladder rungs, spools, furniture, tank car loading tubes, athletic equipment, and business machine parts. In general, the amount of tubing and hollow shapes produced represent a minor portion of the magnesium extrusion business. The magnesium alloys in which tubing and hollow shapes are being produced together with typical properties are presented in Table I. MI A alloy is a low cost alloy possessing good welding and stress corrosion characteristics together with moderate formability and corrosion resistance. It is widely used for low strength applications. AZ31 B, alloy is used for moderately stressed applications and possesses good corrosion resistance and formability with fair welding characteristics. AZ61 A alloy has slightly higher physical properties than AZ31 B alloy together with good formabil- [ ] ity and corrosion resistance but slightly poorer welding characteristics. AZ80 A, ZK60 A-F, and ZK60 A-T5 alloys are used where the maximum in physical properties is required. AZ80 A alloy possesses fair corrosion resistance but with formability and welding characteristics inferior to' the other alloys. ZK60 A-F and ZK60 A-T5 alloys, while only recently offered for com¬mercial use, are finding favor due, to the higher permissible extrusion rates. These alloys possess greater toughness than AZ80 A alloy and, while of moderate formability at room temperature, are very formable at 300° to 500°F. The major portion of tubing and hollow shape production at the present time is in AZ3I B alloy. Magnesium alloy tubing is commercially available in the as-extruded condition or, in the case of ZK60 A-T5, in the as-extruded and aged

Jan 1, 1951

By Arthur Coffinberry

EVE have studied the gold-aluminum system by X-ray diffraction and by the microscope over the entire range of composition for temperatures between 300° and 500° C. Results obtained are shown in Fig. 1, com-bined with the work of Heycock and Neville1 at higher temperatures. The diagram differs in important details from that given by Hansen2 in his critical compilation of the literature of binary alloy systems. This work was, undertaken both because of the intrinsic value of a knowledge of the phase diagram of this system and because of the need of theoretical metallurgy for precise and accurate data, particularly X-ray diffraction data. Systematic studies of equilibrium diagrams, particularly by Hume-Rothery,3 have shown regularities that yield a certain insight into the nature of alloying forces. It has been shown, for example, that solid solubility depends on the concentration of free electrons in the alloy, on the relative radii of solvent and solute atones, on the forces of attraction between atoms, and on the relative stability of intermediate phases. The well-known Hume-Rothery rule states that the crystal structures and compositions of many intermediate phases depend on the electron-to-atom ratio. This has been confirmed and extended by wave mechanical calculations.4 A knowledge of the forces between atoms in alloys, even an imperfectly developed empirical one, should be a valuable guide in the preparation of technological alloys of desirable properties. Furthermore, such informa-tion is basic in such problems as rate of diffusion, age-hardening, phase transformations, and others. The most valuable data for this purpose are furnished by X-ray diffraction studies. Unfortunately, work has been

Jan 1, 1938

ORE at the Jeffrey mine of Canadian John Mansville at Asbestos, Que., is hoisted by two 12 1/2 - ton capacity aluminum skips, counterbalanced. When the loaded skip reaches the surface it empties, via its sliding door, into a bin. Simultaneously, the skip tender, who operates at the 940 level, loads ore into the alternate skip from a 12 ½ -ton measuring pocket. This done, he sets the skips in motion. Problem: When moisture content of the asbestos ore is high, the ore, unknown to the skip tender, some- times sticks in the dumping skip, preventing complete discharge. Moreover, the sliding skip doors sometimes jam and stay open after the ore is discharged. If a skip in this condition is lowered, the result is either an overflow of ore, or the ore discharges through the open skip door, down the shaft. Spilled ore must then be mucked out of the spill pocket and hoisted in 2-ton cars. Cost is high, time is lost, and the shaft is sometimes damaged. Solution: A television apparatus was installed so that the skip tender might quickly spot improper door operation or hang-ups at the dumping station.

Jan 8, 1958

By T. H. Alden, H. W. Schadler

The strain rate dependence of the flow stress of the eutectoid Zn-Al alloy has been determined as a function of mechanical processing, microstructure, and temperature. The best superplastic properties result from the ultrafine, equiaxed structure produced by solution treatment and isothermal transformation at 0°C. Lamellar structures produced by isothermal transformation and coarse equiaxed structures produced by annealing also exhibit strain rate sensitivity in excess of 0.5, but at higher stresses and lower strain rates than the finest structure. Solution treatment and isothermal transformation eliminate the effect of prior processing history. Small composition variations in the binary alloy do not influence the mechanical properties. Below the eutectoid transformation temperature (.275C) increasing temperature lowers the flow stress at all strain rates. The data do not favor any of the present proposals for the mechanism of superplastic flow. ALLOYS of zinc and aluminum, near the eutectoid composition, have been investigated for: 1) the flow stress-strain rate and elongation behavior,1, 2) the transformation kinetics,3 and 3) structure,3"5 but the structure sensitivity of the mechanical properties is poorly understood. Using a near eutectoid alloy water-quenched from 380°C, Backofen et aL2 estab- high and increases with increasing strain rate. They found a correlation between strain rate sensitivity and tensile elongation as expected from the increased resistance to necking that a high strain rate sensitivity provides.296 The large elongation at high strain rates is attractive for metal forming. Since most other superplastic alloys7-l3 do not show high strain rate sensitivity at such a high strain rate (for the exception see Ref. 12) there is the possibility of a unique deformation mechanism for this alloy. The sensitivity of the mechanical properties of the eutectoid alloy to thermal history1 suggests a structure sensitivity that has not been demonstrated. Gar-wood and Hopkins3 identified a lamellar product for material transformed between 200" and 260°C. The size of the lamellae decreased with decreasing temperature. They also demonstrated that an unresolved transformation product formed below 200°C. A granular two-phase material was resolved for specimens quenched to below 150°C by Mitbauer and sauerwald4 who observed coarsening of the structure after annealing. The role of grain boundaries in superplastic deformation is suggested by the strong effect of grain refinement in encouraging this phenomenon at high strain rateS7-11, 13 and is emphasized in several proposals about rnechanism7, 8, 12 and in a theory14 of high-temperature deformation. Alden8 showed metallographic evidence that grain boundary sliding is occurring extensively at strain rates where m is large but less at high strain rates where normal plasticity is observed. Holt and Backofen10 have shown that sliding also oc-

Jan 1, 1969

By A. L. Bailey, B. A. Landry

W. W. ANDERSON and G. E. KELLER*—We want to compliment the authors on this very thorough paper. It gives information which the coal industry has needed for some time. We hope that the additional information which the authors are collecting will he available shortly. The mixing and riffling procedure that was followed for experimental purposes is obviously not practical in routine float-and-sink testing because of the particle size degradation which would result in handling the sample so many times. It is important to obtain our tloat-and-sink fractions with a minimum amount of handling of material. A statement is made in the paper (p. 80) that "the variable most likely to affect the size of sample required to meet a given preassigned accuracy would be the state or degree of mixing of the coal." We agree that this is a large factor, but do not believe it is the most important factor. Our own opinion is that the most important single factor governing the total gross weight of sample that must be collected is the percentage of the weight of material in the smallest fraction that results from the screening and float-and-\ink operations. In other words, size of sample is governed by the total number of fractionations that must he made, and the distribution of material within the fractions. We can imagine a coal with perfect mixing, but with such a small amount of material in some float-and-sink fraction in one of the coarse sizes that a much larger sample would have to be taken than would be the case with very poorly mixed material, but with a large percentage of coarse material more evenly distributed in all float-and-sink fractions. Our own observation of many float-and-sink tests that we have run in our own organization on many types of coal is that the size of sample that must be used on fine size float and sink is governed more by the requirements for weight of material to be used for analysis in the laboratory than by weight of material necessary to obtain accurate float and sink percentage of weight values. In other words, it is our opinion that very small samples can be used for float-and-sink fractionation in the fine sizes, but that accurate analysis of the fractions will depend on a larger weight of sample being pulverized for the laboratory than is necessary to establish the float-and-sink distribution with respect to weight. A. L. BAILEY and B. A. LANDRY (authors' reply)—The authors thank Messrs. Anderson and Keller for their comments based on long experience. It is agreed that the involved mixing and riming technique used may be disadvantageous from the standpoint of degradation. Fortunately, the paper does point out that the extended riming was unrewarding in causing further mixing. Two large unknowns remain, however: (1) how much of the mixing from the presumed highly unmixed state in the bed was achieved toward the random state during blasting, loading, transportation, screening, and further transportation to the point where the gross sample was taken, and (2) how much of the mixing took place during the preparation described preceding riming. As has been pointed out by one of the authors.6 the degree of mixing has a very large effect on the size of sample required and there are still too few experimental data to show at what stage of coal handling most of the mixing occurs. The discussion states that the weight of material in a screened fraction, or in a float-and-sink fraction, is more important than the mixing factor. We do not believe that these factors are comparable in this instance inasmuch as our purpose was to give minimum sampling requirements to achieve a preassigned accuracy in the percentages of float, middlings, or sink, and nothing more. The gross sample had already been screened and no further division by screening was made or contemplated; also, it was not intended that the middlings and sink fractions would necessarily be adequate for percentage ash or other determination. In other words, the sample obtained by the method outlined is not intended for washability studies but only for preparation plant control. Further experimental work has been done, since the paper was prepared, to investigate the effect of increasingly larger top and bottom sizes on the variability of float, etc., of a double-screened coal from Western Pennsylvania. Results will be published and eventually attention is to be given to the preparation of sampling specifications. E. H. M. BADGER*—I should like the authors to explain more fully the fundamental assumptions on which their Eq 4 is based. The equation is of the form s2 = p(l - p) which is the usual expression for the (standard deviation)2 when the chance of finding a particular kind of particle in the sample is proportional to the number fraetion, p. But instead of the number fraction, the authors have used the weight fraction, WF/W. The chance of finding a particular kind of particle in the sample can only be proportional to the weight fraction, if the average ?eig?ts of all kinds of particles, that is, float, midlings, or sink, are the same. Surely a much more justifiable assumption would be that the average volumes of the particles are the same, and, if this is so, Eq 4 would not be true. This may be demonstrated as follows: Let be the weight fraction of float, middlings, or sink, dl the density of this fraction, and d2 the density of the rest of the coal. Then assuming that the average volumes of the pieces in the three classes are the same, the number fraction, p, is given by ? P = d1/l-?/d2 + ?/d1 = ?d2/d1 + ?(d2-d1) The weight fraction, w, in terms of p is given by ? = pd1/(l-p)d2 + pd1 = pd1/d2 + p(d1-d2) _____ [61

Jan 1, 1950

By J. Parke Channing

ALTHOUGH the original thought of investigating waste in industry came from a mining engineer, Herbert Hoover, and although the chairman of that committee was a mining engineer (although the real work was done by the vice-chairman, L. W. Wallace), it is an interesting commentary that when the report first saw light, at St. Louis, on the first of June, 1921, some people most violently went up in the air when it was submitted by the representatives of the mining engineers. At the time they resented most markedly the report of the committee that 50 per cent. of the waste in industry, or as Mr. Ingalls in his paper has properly said, inefficiency in industry, was to be laid upon management. The reason for that seems to have been that, as a whole, the mining industry is pretty well organized and is superior to a large number of manufacturing industries including those studied by the Report. However, this very meeting shows that even the min-ing engineers have finally realized that there is waste or inefficiency in mining and that a large proportion of it can, with propriety, be assessed against management.

Jan 3, 1922

By Raymond C. Johnson

GASIFICATION is important to the anthracite industry, as it is to the entire solid-fuel industry and to the nation. However, to the anthracite industry it may have particular significance in that it would increase the market value of many millions of tons of a by-product fuel, which the industry now has in storage and is currently producing, in addition to increasing the potential market for all its products. The by-product fuel is of usable quality but the ash content is higher than it can be in other products and therefore it must be converted or used at the point of production. Gasification is one method by which the product may be given increased value. The inherent characteristics of anthracite make it well suited for producing a fuel or synthesis gas. It is the most concentrated form of natural commercial carbon, noncaking and noncoking; it does not produce smoke, tar, or soot and has a low sulphur content; and the volatile matter, which ranges between 2 and 8 pct, is 80 to 85 pct hydrogen with small amounts of methane, carbon dioxide, carbon monoxide, and nitrogen. The ash fuses at high temperatures, which allows it to be burned at high rates without slagging. However, with the addition of small amounts of dolomite, the ash will form a slag, or glass, which is very fluid. Anthracite has long been used in the manufacture of city gas and it is extensively used in various parts of the country to make water gas to be converted to hydrogen. Buckwheat and rice anthracite are used in Galusha producers to make producer gas. Excellent synthesis gas has been made in a Galusha producer with rice and barley anthracite with oxygen in tests at the Consolidated Mining and Smelting Co., Trail, British Columbia. In these tests, anthracite was shown to have advantages over competitive fuels, in that the gas had a higher hydrogen content and could be cleaned with less difficulty. The anthracite seams are steeply pitching and in mining the parting strata and some of the roof and bottom materials are taken with the coal. In preparation, these materials are separated by gravity from the commercial product and stored in refuse banks. This refuse contains a mixture of rock, slate, or shale, and high-ash anthracite with bone coal, which is low-ash coal that is interspersed with thin bands of shale. The bone coal contains between 25 and 50 pct ash with an average ash content of approximately 30 pct, with a

Jan 1, 1953

GWILLIAM H. CLAMER (Philadelphia, Pa.).-About 16,000 tons of tin is used annually in the production of white metals. The real reason for using the so-called genuine babbitt, which is a high-tin base babbitt, perhaps in the majority of cases, is that tin has always been. a high-priced metal and people naturally believe that what they pay a high price for must be good. Mr. Jones has shown that the common metal, lead, is a superior base for most purposes for Which babbitt metal is used. The addition of lead is often looked upon as adulterant to genuine babbitt, and specifications for this reason rigidly restrict the lead content. A sub-committee of the Society for Testing Materials, at the meeting in June, presented tentative specifications on babbitt metal, in which were included twelve formulas, containing from zero to: 20, per cent. of tin, and several containing from 65 and 92 per cent. Babbitts. containing

Jan 1, 1919