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THE Institute assembled in the rooms of the Geographical Society at the Cooper Union, Tuesday evening at 8 P.M. President Raymond called the meeting to order, and introduced Mr. Abram S. Hewitt, who welcomed the Institute to New York. President Raymond, in behalf of the Institute, replied. The President then read the following report of the Council for the past year. The Council respectfully report that the American Institute of Mining Engineers has held four meetings-at Wilkes-Barre, Bethlehem, Troy, and Philadelphia, respectively-all of which have been well attended, and socially and professionally most successful. The proceedings of these meetings having been published in the Engineering and Mining Journal, and sent to all members and associates, are sufficiently well known. Forty-Bur papers, by twenty-six authors, have been read. These papers embrace a wide range of subjects, and prove the practical character of the proceedings of the Institute. The finances are in a satisfactory condition. By the report of the Treasurer it appears that $1290.10 have been received, $519.90 expended, and that $770.20 now remains in the treasury exclusive of fees for 1872. This fund, it is hoped, will be so increased by voluntary subscriptions as to enable us before long to issue a volume of our most important transactions in a permanent form. The Council has made a favorable arrangement with the Scientific Publishing Company, publishing the Engineering and Mining Journal, by which that journal became the organ of the Institute for the first publication of the proceedings, papers, and notices to members. This arrangement it is proposed to continue through the present year unless the Institute shall otherwise direct. I t is not intended to supersede the publication of an annual or occasional volume, but to maintain an interest in the Institute, and to serve the convenience of members while our funds do not permit a more ambitious publication.

By T. P. Papazoglou, N. A. D. Parlee, W. C. Phelps

PRACTICAL designs for good "home made" molybdenum furnaces are hard to find in the literature. The one described briefly below left something to be desired but was good enough to operate as a rather long (30 in.) two-zone furnace for periods of over 2 months at temperature (1400° to 1600°C) without shutdown. The principal problem in our application was to establish a temperature profile with two distinct constant-temperature zones and no dip between the zones. This and other problems mentioned below would not arise, however, if both zones were operated at the same temperature and if a shorter furnace were acceptable. Since molybdenum windings oxidize very rapidly when heated in air, impervious refractory tubes were used for both the furnace core and the outer jacket tube shown in the accompanying figures. A protective atmosphere of forming gas (10 pct H2, 90 pct N2) was continuously passed through the gas-tight annular volume between the core and outer jacket. The water-cooled copper ends shown in Figs. 1 to 3 sealed the ends of the tubes. Annealed molybdenum wire (40 mil) was wound on the recrys-tallized alumina core (35.5 mm OD by 28.5 mm ID by 30 in.) at a spacing of 0.36 in. The spacing was reduced to 0.29 in. close to the ends to partially compensate for end heat losses. Fig. 2 shows two molybdenum-ground lead taps off the center of the winding to produce the two independect temperature zones. The ground lead was insulated with 1/4-in. alumina tubing and connected to the grounded copper end by passing the wires through the gas port tube and crimping each wire into notches cut at the mouth. To prevent sagging of the core at high temperatures, refractory "troughs" were cut from alumina and mullite tubing to cradle the core. The support "troughs" which were 6 in. long and located about 5 in. from each end of the annular volume also served as radiation shields. In view of the different expansion coefficients and operating temperatures of the core and outer jacket (3.5 in. OD by 3 in. ID by 30 in.), the ends of the tubes were smoothed and squared to produce good sealing surfaces, and the core was ground 1/32 in. shorter than the outer tube. The power terminals were passed through their respective conductor ports which were internally lined with alumina tubing and sealed with Armstrong adhesive A-6 leaving about 1 in. of protruding lead wire for external connections. (Adhesive A-6 is a two-component system consisting of an epoxy-type resin with a mineral fibrous filler and an amine catalyst.) Figs. 1 and 3 show the entire assembly of concentric refractory tubes, copper ends, and sealing o rings, held together with two brass flanges and 3/8-in. bolts with heavy springs for dimensional flexibility. The furnace shell (19 by 19 by 30 in.) consisted of a steel frame with sheets of transite forming a box. The copper ends protruded through two 3.75-in. circular holes cut at the center of each transite square end. Thermal insulation next to the transite exterior was effected by K-23 B&W bricks alld in a central volume of approximately 9 by 9 by 30 in. a row of K-30 bricks was lined up to support the hot assembly. The rest of the volume around the outer

Jan 1, 1965

By J. C. Williams, M. J. Blackburn

Several of the decomposition processes that can occur in supersaturated phases in a Ti:11.6 wt pct Mo and a Ti:20 wt pct V alloy have been studied by transmission electron microscopy. The deformation induced "marternsitic phase" in the Ti:Mo alloy has been found to have a bcc or bct structure rather than the previously reported hexagonal structure. The morphology of&apos; the transformed region is a rather complex asserrlblage of twins, twinning occurring in one or more systems; this internal twinning has been found to occur on (112). The w phase is formed in both alloys on aging and is present in the Ti:Mo alloy after quenching. The structure of this phase has been confirmed as hexagonal in both systems, however, differences in morphology and stability are found between the two alloys. Thus in the Ti-Mo alloy the w phase has an ellipsoidal morphology with the major axis lying parallel to <111>ß or [0001]w while in the Ti-V alloy the phase forms as cubes, the cube faces lying parallel to {100}ß or {2021}w Some observations on the particle sizes, volume fraction, and composition of the w phase in the Ti-Mo alloy are listed. The mode of formation of The a phase from the (ß + w) structures is also different in the two alloys. In the Ti-Mo alloy the a phase is formed by either a cellular reaction or by the growth of isolated needles, whereas in the Ti-V alloy the a phase is nucleated at an w:ß interface and grow to consume the w phase. Some of the difjerences in behavior of the w phase are attributed to the mismatch between it and the solute enriched ß matrix in which it forms. MaNY transition elements tend to stabilize the bcc or ß-phase when added to titanium. In general two types of phase diagrams are produced, either a ß-stabilized (ß-isomorphous) system, e.g., Ti:Mo, -Ti:V, Ti:Nb, or a ß-eutectoid system, e.g., Ti:Cr, Ti:Fe, Ti:Mn. In previous papers&apos;-4 the phase transformations in the a-phase and (a + ß)-phase alloys have been described and this work has been extended to ß-stabilized systems. Specifically, transformations in the alloys Ti:20 wt pct V and Ti:11.6 wt pct Mo have been studied; in both of these alloys the ß phase is retained at room temperature when quenched from the ß-phase field. A number of phase transformations can occur in such metastable ß phases and the two alloys were chosen to include most of the transformations reported for ß-stabilized systems. We list these possible phase transformations below. Ti:11.6 Mo quenched from >780°C to retain the ß phase: a) The w phase can form on quenching.5 b) Martensite can be produced by subzero cooling or deformation. Two martensite habit planes have been reported in Ti:Mo alloys; (334)ß and (344)ß=6 c) On aging at temperatures <-550° C the w phase is formed before the a-phase.5,7 d) On aging at temperatures >550°C the a phase is formed.7 e) The martensite can be tempered. It has been reported that the a phase rather than the ß phase is precipitated during tempering.&apos; Ti:20V quenched from >660°C to retain the ß phase:9 a) At aging temperatures <260°C separation into two bcc phases occurs. b) The w-phase is produced prior to the a phase on aging at temperatures <-400°C. c) At temperatures 2400°C the a phase is formed directly. T-T-T diagrams describing the temperature and time regimes for the formation of these phases have been published7,9 for a Ti:12 pct Mo and a Ti:20 pct V alloy. We have attempted to investigate these transformations using transmission electron microscopy, however thin foils undergo a spontaneous transformation in all conditions except the equilibrium (a + ß) structure. This transformation has been reported previ0usly10,11 and we will comment on its morphology and nature in the various sections of experimental results. EXPERIMENTAL The compositions in wt pct of the two alloys investigated were: Ti:11.6 Mo, 0.100 02, 0.006 N2, 0.0015 H2 Ti:20V, 0.0574 O2, 0.0111 N2, 0.005 H2 These alloys were cold-rolled to 0.020 in. thick sheet. Specimens were heat treated in vacuum or in inert gas at temperatures >500°C and in a circulating air furnace at temperatures <500°C. Thin foils were prepared using standard techniques, described in detail previously." Dark field micrographs were obtained using high resolution technique. RESULTS Martensitic Transformation in Ti:11.6 pct Mo. Detailed study of the deformation induced martensite is not possible due to a spontaneous transformation which occurs near the edge of thin foils as shown in Fig. 1. Similar transformations have been observed in iron-" and copper-base13 alloys as well as other titanium alloys, but some observations specific to the Ti:1l.6 Mo alloy are listed below. a) The boundaries of these transformed regions are glissile and move under the influence of the electron beam during examination. b) Selected area diffraction indicates the transformed regions have the same structure as the matrix, being separated by tilt boundaries. The misori-

Jan 1, 1969

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&apos;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.&apos; 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&apos;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&apos;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

[President and Director *JOSEPH L. GILLSON, &apos;62 Wilmington, Del. Past President and Director *HOWARD C. PYLE, &apos;61, Los Angeles, Calif. President-elect and Director *R. R. McNAUGHTON,&apos;63, Trail, B.C., Canada Vice-Presidents and Directors *JOHN CHIPMAN,&apos;62, Cambridge, Mass. *JOHN P. HAMMOND,&apos;61, Tulsa, Oklahoma *WALTER R. HIBBARD, JR.,&apos;61, Schenectady, N.Y. *BASIL P. KANTZER, &apos;61, Los Angeles, Calif. *S. D. MICHAELSON,&apos;61, Salt Lake City, Utah *J. W. WOOMER, &apos;62, Pittsburgh, Pa.]

Jan 1, 1961

By Axel Sahlin

Having no business interest in any of the various machines used for granulating ores, my remarks on the subject are prompted solely by my desire to contribute towards the determination of the best apparatus such information, as I have been able to gather,

Jan 1, 1893

By E. W. Hart, W. R. Hibbard

The room temperature flow characteristics of a series of Cu-Cr alloys are found to be related to the amount and characteristics of the chromium-rich precipitate. The results are consistent with the theory of Fisher, Hart, and Pry, which considers the trapping to dislocation loops around precipitate particles. THE use of dispersed phases for hardening metals, particularly high temperature alloys, has been practiced for several years. Current theories describing the effects of dispersions on the basis of dislocation theory have been proposed by Mott and Nabarro.l-4 rowan," and Fisher, Hart, and Pry.8 These theories recently have been discussed by Hart,&apos; who pointed out that the experimental data available for comparison with theoretical calculations for overaged alloys are confined to studies by Gensamer, Pearsall, Pellini, and Low,8 Shaw, Sher-by, Starr, and Dorn,9 and some hitherto unpublished data on Cu-Cr alloys which will be described herein. Certain difficulties were associated with the interpretation of the first two studies. Gensamer, Pearsall, Pellini, and Low were concerned principally with interparticle spacing and did not document particle sizes. Shaw, Sherby, Starr, and Dorn included all the data in their report which was necessary for the theoretical evaluation, but their study is subject to some question1" due to difference in prior history of various specimens and due to systematic differences in particle characteristics" which appeared to be associated with differences in the magnification of their microscopic examination. The current study was undertaken to obtain critical data in a manner which avoids some of these limitations. Specimens of eight Cu-Cr alloys remaining from a previous investigation&apos;&apos; were available in the form of 100 mil sheet of the compositions shown in Table I. At 200 mil this material had been previously an- nealed ½ hr at 1000°C, water quenched, and cold rolled 50 pct. Samples were further cold rolled to a thickness of 20 mil for a total reduction of 90 pct. Sheet tensile specimens of standard geometry with a gage length 2½ in. long and 0.20 in. wide were machined from this sheet. These specimens were then annealed in a dried N2-H2 atmosphere for the times and temperatures indicated in Table I. This anneal served two purposes: 1—to obtain a fairly uniform and nearly constant grain size of 0.015 to 0.022 mm average diameter, and 2—to precipitate a fairly uniform, nearly spherical over-aged dispersion of essentially pure chromium. A typical microstructure illustrating the grain size and the uniformity of the dispersion is shown in Fig. 1. A typical dispersion illustrating the range of sizes and shapes of the particles is shown in Fig. 2. The tensile specimens were tested in the Instron equipment described in ref. 11 at room temperature at a strain rate of 0.04 in. per in. per min. Three tests were run on each alloy with sufficient repro-ducibility that a single true stress-true plastic strain curve could be drawn through the three sets of data for each alloy. Typical curves are shown in Fig. 3.

Jan 1, 1956

By J. C. Allen, E. V. Herring

CHILE EXPLORATION CO&apos;s. oxide plant at Chuquicamata, the largest of its kind, started in 1915 with initial operations at the rate of 10,000 tons of ore per day. Anaconda Copper Mining Co. acquired the controlling interest in 1923 and in the next few years modernized the plant and mine, extending operations to a nominal capacity of 490 million lb of electrolytic copper yearly by 1942. Plant production averaging 495.7 million lb of copper per year was maintained for the eight-year period extending from 1941 to 1948 inclusive. During the World War II production reached its highest level when in 1944 the output was 531.8 million lb. The maximum production for any one month was 49.6 million lb, achieved in May 1947. E. A. Cappelen Smith, consulting metallurgist for M. Guggenheim&apos;s Sons, worked out the first process for the treatment of Chuquicamata copper oxide ore about 1913, and directed a staff of 20 young engineers operating a pilot plant at Perth Amboy, N. J., on three shifts for an entire year. The copper is extracted from the oxide ore by a hydro-metallurgical treatment described in detail by T. A. Campbell in AIME Transactions, Vol. 106, Copper Metallurgy, 1933. The Oxide Plant is divided into five main operations as follows: (1) Crushing, (2) Leaching, including dechloridizing and sulphur dioxide treatment, (3) Tailing disposal, (4) Electrolytic precipitation, (5) Smelting and melting. Crushing The present Primary Crushing Plant has been in operation 25 years, during which time 4,342,112 cars of 70 tons net capacity have passed through the dumpers. The ore as received from the mine is frequently blocky and up to 5 feet in section. It is reduced to 9-in. size by two 60-in. gyratory crushers, and transported to the east and west ore bins by 60-in. conveyors. In the secondary crushing operation the ore is first reduced to 2 to 3-in. size by five standard 7-ft cone crushers and two No. 10 gyratories. This product is then reduced to 3/8-in. size by fifty-two 48-in. vertical Symons disc crushers and is transported by belt conveyors to the loading bridges from which it is charged° into the leaching vats. Conveyor belt No. 14 which serves the eight vats in the east section of the leaching plant has transported over 125 million tons of ore, which is a record for any type of conveyor. This 60-in. belt travels at a speed of 600 fpm and carries loads up to 5500 tons per hr. Leaching The ore is leached in 14 vats, averaging 13,500 short tons net capacity each. These vats are lined with a natural mastic which adequately resists the sulphuric acid leaching solutions. The leaching process as presently conducted comprises soaking the ore with successive volumes of leaching solution and spent electrolyte and withdrawing successive volumes of enriched solution from the vat to a total of approximately 3.2 million gal. The first 1.6 million gal of this volume withdrawn is called strong solution and contains about 35 parts of copper per 1000. The balance of 1.6 million gal subsequently withdrawn is stored in a

Jan 1, 1952

By Harvey Cline, Donald P. Ferriss

THE violent outgassing of commercial tungsten and other refractory metals when melted in an electron beam zone refining apparatus1"3 is dealt with experimentally by one or both of two approaches. One is to provide a suitable emission current control1,2 the other is to purify the metal in the solid state before melting.4 The first of these is usually sufficient, but the authors chose also to investigate the source of the troublesome gases and to devise means of solid-state purification. Some further insights into the use of tungsten as a structural material at temperatures near its melting point were also revealed in the course of the work. One may speculate on the causes of gas formation in tungsten at high temperature by inferences from the literature and an examination of the impurities in commercial wire. Davenport5 observed microporosity in both tungsten and molybdenum filaments heated to several hundred degrees below their melting points. Studying the function of oxygen in molybdenum welds, Perry, Spacil, and wulff8 attributed similar porosity to the disproportionation of Moo2 to molybdenum metal and Moo3. Tungsten dioxide also disproportionates7 above 2000oC to yield WO3 vapor at considerable pressure. Commercial tungsten contains some 5 to 20 wt ppm O and a similar concentration of carbon depending on the details and precautions of processing. Therefore, evolution of CO is also a strong possibility as a source of gas at high temperatures. Furthermore, even for activities in the order of 0.01, it may be calculated that the pressure of CO at 3000°C would be over 4000 psi, which is in excess of the tensile strength of tungsten at this temperature.9,10 Powder metallurgy tungsten contains some 0.02 pet Fe and 0.002 to 0.005 pet of the elements Ni, Si, Al, Ca, Mn, Mg, and Mo; at temperatures over 2800°c, therefore, these elements will exhibit appreciable vapor pressure, though small compared to that of WO3 and CO. Some of these impurities may react to form high-pressure monoxides such as SiO and A10. Finally, dissolved and occluded nitrogen is an ever-present source of high-pressure gas. Commercial Type 218, General Electric filament wires, 0.025 in. diam, were heated by resistance in 10 -4 mm of Hg and in argon or hydrogen at pressures from 50 µ to atmospheric. For temperature determinations in vacuo, the Jones - Langmuir8 current-temperature relationship was employed. For gaseous atmospheres, the burn-out temperature was assumed to be the same as in vacuo so that a small, constant correction could be made for temperatures below burn-out conditions (i.e., local heating to failure). Several dozen experiments may be summarized by pointing out some structural observations. At 3050oC in 1 atm of A, porosity is very evident after 30 min, as shown in Fig. 1. For the section in Fig. 2, failure occurred 200°C below the melting point and many voids have grown in the grain bound-

Jan 1, 1962

By Charles Luner

ALTHOUGH the kinetics of the atmospheric oxidation of tin have been studied,1-3 the kinetics in pure oxygen have not been reported. This note presents some results of the kinetics of the oxidation of tin foil in pure oxygen. The tin foil used in this investigation was 99.78 pct pure, the two major impurities being Pb (0.17 pct) and Sb (0.024 pct). The foil was degreased and air-dried prior to oxidation. The air-formed film was estimated by coulometric reduction4 of the surface oxides to be about 25A. The samples, which were in strip form and had a total geometric surface area of about 300 sq cm, were first evacuated at room temperature in an oxidation bulb to 1 X 10 -5 mm Hg and subsequently degassed for 1 hr at the temperature of the experiment. Spectroscopically pure oxygen was then introduced into the bulb. The rates of oxidation were measured by following the rate of pressure change due to oxygen consumption in a closed system, the volume of which was sufficiently large so that the pressure change during an experiment was 10 to 15 per cent of the total pressure. An oil-mercury manometer,5 with a sensitivity of 3 X x mm Hg (which corresponds approximately to 5 X 10 -7 gm of oxygen) was used to measure the pressure change. The oxidation bulb was heated by an oil-bath and controlled to within -10.3 C. The reproducibility of the rates was good, as determined by the coincidence of rates at 190oC for duplicate experiments. Fig. 1 shows the oxidation curves in the temperature range 168 to 211.5oC at 8 mm Hg pressure. The effect of pressure on the rate of oxidation at 190°C is also shown. The rate of oxidation was not markedly affected by changes in pressure in the range 4 to 9 mm Hg, except perhaps at the lowest pressure, 4 mm Hg, where after about 70 min there appeared to be a decline in the rate, as compared with the rate at the higher pressures. At the lower tem- perature, 168oC, and for short reaction times, it is difficult to distinguish between a linear relationship and a slight curvature in the oxidation rate. However, for longer times, there was a somewhat larger indication of curvature. The samples after oxidation were gold-colored in appearance. The oxide that was formed at 170°C was identified as a-SnO by reflection electron diffraction. This is in agreement with results obtained by other workers.6, 7 The rate data best fitted the logarithmic-oxidation rate law, w = K1n ln(1 + -t/to) [1] where w is the weight of oxygen consumed, t is the time, and K In, and to are constants. First estimates to were obtained according to the method of Taylor Thon8 and were then employed to obtain the best simuItaneous estimates of to and K In, that would fit the logarithmic expression. These estimates were found numerically, so that the residual variance could be minimized. The calculations were performed on an

Jan 1, 1961

By M. L. Samuels

DURING the period from 1910 to 1920, there was a lively interest in the subject of grain growth and many papers were published, followed by interesting discussions. Questions dealing with the fundamentals of grain growth-why and how it occurs-were treated in papers by Howe,1 Jeffries,2 Sauveur,3 Chappell,4 Beilby,5 Mathewson and Phillips,6 McAdam,7 Carpenter and Elam,8 Stead and Carpenter,9 Ruder,10 as well as others. Since that decade, much indeed has been done regarding the practical control of grain size, and it is now possible to order material having a size specified in the American Society for Testing Materials classification. Also, one hears the term "spliced boundaries" used in connection with certain tungsten lamp filaments" wherein it is important to prevent "sagging" between consecutive turns of the helix." This practical use of a certain knowledge as to the things that influence or even control grain growth should not be taken as an indication that the subject has been thoroughly explored and that nothing more can be learned from fundamental studies. It is with this thought in mind that a report of some observations and experiments on abnormal grain growth is believed justified. Abnormal grain growth is met with in heat-treating high-carbon steels in the austenitic range,13 in the hardening treatments of high-speed steels, 14.11 and in the low-temperature annealing of strained low-carbon steels as in sheet and wire material. Entirely aside from these instances of exaggerated grain growth, which some might consider as freakish, it is thought that abnormal growth is simply a case where the growth forces and the forces tending to prevent growth are almost, but not quite, evenly balanced. Information relative to grain-growth characteristics in general may be obtained from a study of abnormal growth conditions, which may be looked upon as vantage points. Reflection will show at once that if growth forces are great in comparison to inertia or resistance to growth, many crystals start to grow and, for that reason, none becomes very large, whereas if inertia is predominant no growth at all takes place. Under conditions in which

Jan 1, 1938

By Leroy Gardner

EVERY reader of this paper is well aware of the fact that the prolonged inhalation of large amounts of free silica dust results in fibrosis of the lungs, and that other inorganic dusts, except those of asbestos and the mineral poisons, are thought to be relatively harmless. But probably few have had opportunity to visualize the effects of silica, asbestos and other minerals upon living tissues. The ideal demonstration would be based upon sections of lungs from human beings that had inhaled com-parable concentrations of different dusts for a unit period of time. Such material is generally difficult to obtain and in some instances is of ques-tionable value because the subject has been exposed to more than one kind of dust. A demonstration could be prepared from the lungs of animals. However, so many months or even years are required to com-plete the exposure to each kind of dust that enough material has not been accumulated. For a general survey of the action of different types of dust, I am therefore compelled to use the tissues of animals that have been injected with suspensions of dust particles. The injection method offers certain advantages. The quantity, the particle size and the state of dispersion can be controlled with sufficient accuracy so that the tissue responses to different minerals can be accu-rately compared. The method insures contact between the tissues and the mineral particles; protective mechanisms, which may prevent the inhalation of certain types of foreign body, never come into play. If the pathway of injection be one that minimizes nonspecific injury, the tissue responses may simulate those produced by inhalation but they develop somewhat more rapidly. It should always be remembered that injection methods merely demonstrate the capacity of various kinds of minerals to provoke reaction in the tissues; whether the same substances are inhaled from atmospheric suspension and accumulate in the lungs in dangerous quantities can be demonstrated only by inhalation.

Jan 1, 1938

By Ralph K. Foster

During five underground mine fires which occurred in Arizona during 1980 and 1981, sealing the fire area became necessary. To minimize leakage into the fire area, ventilation control measures were instituted to balance pressure across the bulkheads. Problems en- countered in sealing the fire areas and measures taken to improve these conditions are discussed. The routing of the ventilation and ventilation control to en- sure the workers&apos; safety were also important considerations in reopening the mines. The use of continuous CO monitors is discussed. One important consideration was the condition of the fire, and chromatographic analysis was used to establish this. Graphs comparing the Trickett ratio, carbon monoxide, carbon dioxide, and oxygen concentrations are given. The Trickett ratio was useful but needed to be augmented by the comparison of CO, C02, and 02. Problems with getting good samples from sealed areas and recommended procedures that were developed during these fires are discussed.

Jan 1, 1982

By L. R. Weisberg, E. A. Miller

Single-crystalline films of silicon of good quality were vacuum-deposited on sapphire. The improved crystallinity was achieved by the strict exclusion of oxygen from the evaporation system, including the use of a "oxygen-free" silicon source. To minimize possible contamination of the source, the silicon was sublimed from the solid at about 1390° C. using a simple electron bombardment system to heat the silicon. This resulted in deposition rates of about 5 to 7 µ per hr and film thicknesses of 4 to 20 µ. The vacuum during deposition was ordinarily about 5x 10-8 Torr, DESPITE the success achieved in the chemical vapor deposition of silicon on sapphire using Silane,1-4 vacuum deposition has not provided comparable properties. For example, Chu et a1.5 vacuum-deposited silicon on single-crystalline substrates of A12O3, Sic, ThO2, and other compounds, and, although some epi- but the use of ultrahigh vacuum (about 1 to 3 x10-9 Torr) during deposition did not significantly improve the results in the oxygen-free system. The crystalline quality of films deposited on (0001) sapphire was found to be considerably superior to (1102) sapphire surfaces. Using (0001) sapphire, single-crystalline films were deposited at temperatures as low as 780° C and as high as 1075°C, with the best crystalline quality obtained at about 1000°C. At this temperature, hole mobilities over 250 sq cm per v-sec were achieved. taxy was indicated, single-crystalline films were not produced. More recently, Salama, Tucker, and young6 evaporated silicon on single-crystalline sapphire, but only poor crystallinity was observed, and low carrier mobilities were measured. In the present experiments, good-quality single-crystalline films of silicon on sapphire have been achieved by specifically excluding oxygen from the evaporation. This included not only the use of a "clean" vacuum system but, of special importance, the use of an oxygen-free silicon source. This has also been shown to provide a dramatic improvement in silicon homoepi-taxy.7 As a result, silicon-on-sapphire films with hole mobilities over 250 sq cm per v-set were achieved, and single-crystal films were grown as low as 780°C and as

Jan 1, 1969

By C. G. Rhodes, D. Kramer

High-field critical transport current density (J) measurements at 4.2 °K as a Junction of applied magnetic field (H) were made on samples of cold-rolled and annealed columbium with H parallel to J. Microscopic examination of the samples revealed a well-defined planar fiber structure produced by the cold rolling. J was found to he lower when fibers are parallel to the direction of magnetic field penetration than when they are perpendicular. This effect may he a consequence of the interaction of flux movement with fiber boundaries. THE severe changes in microstructure brought about by cold working superconductors leads to profound changes in their superconducting behavior. In particular, the ability of a superconductor to carry a transport current with zero resistance (the maximum value of this current density will be called "J" in the presence of large external magnetic fields (to be referred to as "H") is greatly influenced by the microstructure. In the case of columbium, LeBlanc and Little1 and Autler et a1.2 have observed an increase in J due to cold work. LeBlanc and Little also observed an anisotropy in J in cold-rolled columbium strips, which Hake et al.3-6 have shown to depend upon the angle between H (H ? J) and the rolling plane. An increase in J due to cold work has been found in a variety of high-field superconducting alloys3&apos;4&apos;7-9 as has the anisotropy effect.10 First explanations of why cold work raised J invoked the idea that dislocations carried the high-field supercurrents,8,11 since cold working drastically increases the dislocation density and presumably the number of supercurrent paths. However, recent ideas on the nature of high-field superconductivity together with new experimental evidence reveal that the bulk of certain superconductors can remain superconducting in high fields while carrying high transport currents. These later developments have been discussed by Berlin-court and Hake12 and a comprehensive review has been prepared by Berlincourt.13 According to the ideas of Gorter14 and Anderson,15 one would expect that the influence of microstructure on high-field supercurrent density will depend on tine interaction between microstructure and penetrating flux and on the direction of the Lorentz

Jan 1, 1965

By B. C. Allen, W. D. Kingery

Surface tension and its temperature dependence have been determined for pure liquid Fe, Cu, Co, Ni, and Sn and for Fe-C, Co-C, and Ni-C alloys. The temperature coefficient of surface tension is negative for all these liquids. The surface tension and wetting behavior of tin and tin-titanium alloys on A120,, Si,N,, MoSi,, and Sic, as well as the behavior of titanium-containing nickel alloys on A1 20, have been determined over a wide temperature range. For all the solids investigated titanium additims markedly lower the contact angle. Some limits for the solid-surface energies have been calculated from liquid surface tension and wetting behavior. SURFACE tension and interface energy are important variables in a number of metallurgical and ceramic phenomena, and have been discussed at some length in connection with determining micro-structure of polyphase systems,&apos; solid-state sintering,&apos; thermal etching of grain boundaries, heats of solution and fine powders,&apos;1 grain-growth phenomena,&apos; the mechanical behavior of fine foils and fibers, nucleation, soldering and brazing,&apos; and other phenomenz of academic or practical interest However, until recently few quantitative data have been available for high-temperature systems. Among available data are some indicating positive temperature coefficients for the surface tension of liquid copper,*,11,&apos;2 cast iron,l3 and iron-carbon14 alloys. Although carbon was found to be not surface active in iron at 1570" some preliminary studies had indicated the possibility of a positive temperature coefficient for the eutectic composition at lower temperatures.16 One part of the present study has been largely concerned with determining the temperature coefficient of surface tension for several metals at elevated temperatures, In addition to surface-tension studies, the wetting behavior of alloys containing titanium has been investigated over a wide temperature range. Previous measurements indicated that titanium was selectively adsorbed from nickel at a liquid nickel-solid alumina interface,17 and the use of titanium hydride or titanium-alloy techniques for metal-ceramic soldering is well known. In the present study, previous data have been extended to new alloy systems, and measurements have been carried out with other oxidation-resistant ceramics. EXPERIMENTAL The sessile-drop method was employed to measure liquid surface tension and contact angle between liquid and solid, utilizing apparatus and techniques which have been described previously.&apos;g The shape of a sessile drop depends on equilibrium between forces of surface tension tending to form a spherical surface of minimum area and forces of gravity tending to flatten the drop. Typical sessile drops are shown in Fig. 1. From precise measurements of maximum drop diameter and drop height the surface tension and drop volume were calculated. Four solid materials were employed as supporting plaques for the liquid-metal drops. Aluminum oxide (99.9 pct, J, T. Baker, reagent grade) was pressed and sintered at 1800°C. Molybdenum-disilicide powder (99.0 pct, Electro Metallurgical Co.) was pressed and sintered at 1650°C. Plaques were cut from silicon carbide (99.4 pct, hot-pressed at Alfred University) and silicon nitride (95.1 pct, with Al, Fe, 0 as major impurities, Norton Co.) rods. All plaques were polished, cleaned, and dried prior to use. A number of metals and alloys were employed. Chemical analyses of vacuum-melted ingots of iron, nickel, cobalt (National Research Corp.), commercial nickel-base alloys, electrolytic copper (International Smelting and Refining Co.), and tin (Mal-linckrodt Chemical Works) are given in Table I. Alloys were prepared in the laboratory by vacuum melting the base metal with either titanium hydride (Metal Hydrides, Xnc.) or spectroscopic-grade carbon (National Carbon Corp.). Nickel-titanium alloys contained between 0.001 and 0.005 pct oxygen and the ferromagnetic metal-carbon alloys contained 0.001 pct. Cylindrical metal specimens (1 to 2.5 g) were machined and bevelled at the bottom to insure a uniform advancing contact angle on melting. Before use the samples were acid-etched, cleaned with acetone, and rinsed in petrol ether.

Jan 1, 1960

By R. M. Rose, K. A. Jones

Resistive measurements ulere made on superconducting niobium single crystals in transverse magnetic fields. Crystals were grouln in both high and ulfrahigh vacua, doped with stnall quantities of oxygen, and annealed in ultrahigh vacua at temperatures from 900&apos; to 1350°C. Maxima in the fluxoid pinr~ir~g force were observedfor the [100] and [210] directions. The increase of the critical current density with dissoved oxygen was seen to saturate at relatively low concentration. This behavior, and the variation of J, and residual resistivity (as a function of oxygen content and annealing) of both clean and dirty gassy) crystals, is seen as a consequence of the formation of clusters with (210)~b habit planes and (200)ffo common boundaries. These suboxide clusters are apparenlly stable at high temperatures and very low oxygen concentrations. It is generally known that dissolved oxygen at concentrations well below the solubility limit sharply increases the critical current density of superconducting niobium.&apos; Such a result would not be expected if Nb-0 solutions were random, not even as the result of segregation on the scale usually encountered in solid solutions. According to the Kim-Anderson theory of flux creep,&apos; the critical transport current density is determined by the pinning force Fp associated with some feature of the microstructure. As the Lorentz force. a or (J X R), of the transport current in the magnetic field approaches Fp, flux creep and then flux flow occur. The pinning force is expected to be quite small if the heterogeneity involved is significantly smaller than tte range of coherency which for niobium is circa 250~.~ Although the strain field of an individual oxygen atom in the niobium lattice is relatively large, it does not seem plausible that individual atoms could be so effective as to account for the data. Also, ~ramer~ found that straining and strain aging specimens containing small amounts of oxygen on occasion decreased the residual resistivity. A possible explanation for the above behavior may be found in the work of van Ooijen and van der Goot,= who found that annealing changed J, for niobium foils containing oxygen, and they attributed the changes to ordering of the oxygen atoms. This phenomenon has been observed by other investigators using X-ray and PROCEDURE Cylindrical 4-in.-diam niobium single crystals with axial orientations [ill], [110], [112], and [oo~] were grown from pure niobium, see Table I for analysis, in an ion-pumped ultrahigh-vacuum system using the electron beam floating zone technique. Total pressure during growth was lo-&apos;9 torr: the oxygen partial pressure was less than lo-" torr, as determined by a mass spectrometer. These crystals will be referred to as the "clean" crystals. Similar crystals were also grown in another system at a pressure of 5 X 10"6 torr. These crystals will be referred to as the "dirty" crystals. Specimens 14 in. long were cut from the as-grown crystals and one end was polished down to no. 600 carbide paper smoothness. A back-reflection Laue photograph was then taken in order to fix the crystallo-graphic directions transverse to the crystal. The critical current density J,, the current density necessary to produce a voltage drop of 1.0 pv between voltage leads placed a in. apart, was determined as a function of the magnitude and direction of the transverse magnetic field and of the oxygen concentration. The technique and experimental arrangement was essentially similar to that of Tedmon et al.&apos; In the remainder of this paper, the azjmuthal angle $ for the field H is referenced to the [ I101 direction in all four crystals, and oxygen was added in small equal increments by anodization and annealing.7 The resistivity ratio, RR, of the resistance at room ternperature to that at 4.2"K (H =7.00 kG) was determined as well.

Jan 1, 1970

By Bauer. Larry G.

The vast coal reserves in the Wyoming, Montana, North and South Dakota region are sufficient to supply the total energy needs of the United States for several hundred years. Not only is there an abundance of this sub-bituminous and lignite coal available, but it is easily obtainable by strip-mining . The overburden varies from several feet to several hundred feet. This western coal has yet another asset, namely, a low sulfur content. Whereas eastern and midwestern coal has a sulfur content of 2.5%, the upper Great Plains coal contains sulfur in the 0.5% range. The importance of the sulfur content of the coal is a direct result of federal government emission standards for sulfur dioxide (SO2). Hand (1) points out that "sub-bituminous coals and lignites have a propensity for retaining this sulfur in the ash under certain conditions which is not evident in higher rank coals." This would tend to reduce further the SO2 concentration in the combustion gases of boilers. Western coal is no panacea, however, in that it is far removed from most population and industrial centers. Furthermore, the moisture content of the coal varies from 20 to 40%. This moisture is almost exclusively inherent, that is, it is chemically and physically bound to the organic matter of the coal. It is believed that the water forms a part of the coal structure perhaps as water of hydration of organic salts or organic acids, perhaps by hydrogen bonding, or perhaps by simple adsorption (2). The primary market for this coal is the electric power industry. Lesser markets will be as coke for the steel industry and possible as a raw material for coal gasification and coal liquefaction plants.

Jan 1, 1983

By Hans Strack

Electroluminescence of GaAs p-n junctions fabricated by simultaneous diffusion of sulfur and iron was investigated at 77°K. A narrow emission peak with a half width of about 4 kT in the energy range between 1.14 and 1.155 eu was attributed to iron. Other transition elements exhibited light emission in the vicinity of the iron peak, namely nickel between 1.15 and 1.16 ev and cobalt between 1.16 and 1.17 ev. The efficiency of the doping with iron depended on the amoz~nt of arsenic present. A weight ratio of arsenic to iron of 4:l was sufficient to observe the emission lines associated with transition elements. The presence of oxygen reduces the intensity of the light emission. In addition to the levels associated with transition elements, levels at 1.05 and 1.28 ev, probably due to lattice defects, are observed except in diodes fabricated in solution-grown GaAs. THE near band edge emission of GaAsp-n junctions has been studied extensively in the past.&apos; GaAs devices utilizing spontaneous and stimulated near band edge emission are of considerable practical importance. Typical junctions are fabricated by diffusion of a heavily doped p region into degenerate n-type GaAs. Much less work has been done on investigating the radiative recombination via deep levels in lightly doped p-type material. This area is of interest in understanding the performance of GaAs n-p-n transistors. GaAs transistors show remarkable improvement in high-frequency performance and current-gain stability at high temperatures, when iron is added to sulfur during the emitter diffusion process. The present work was initiated to investigate deep-level electroluminescence of iron-doped GaAs p-n junctions fabricated on vapor-phase epitaxial GaAs and on solution-grown GaAs. For comparison several diodes doped with cobalt and nickel were studied. Iron, cobalt, and nickel have an electron configuration of the type

Jan 1, 1968

Flaubert, as we know, laid stress on the selection of the right word, le mot juste, the precise epithet, the word that belongs to the thing. A sentence, or even a paragraph, may be spoiled. by the use of a word that is not proper, that does not fit or is foreign to the meaning intended. An Australian mining expert is reported to have said: You have a property of considerable value, and what I saw warrants s good development of very rich cubicular galena, with gossan intermixed. &apos;Cubicular&apos; means &apos;belonging to a small bedroom&apos;, a &apos;cubicle&apos; being a sleeping compartment. He meant &apos;cubic&apos;, of course. This is a malapropism, and reminds me of the lady from Chicago that, on her return from Europe, said how much she had enjoyed the rural parts of France, because, among other things, it was "so delightful to hear the French pheasants singing the mayonnaise to the tune of the Los Angelus". It is impossible to amalgamate coal-tar thoroughly with the pulp in the agitating-tank. In metallurgy, &apos;amalgamate&apos; refers to the combination of mercury with one or both of the precious metals, forming an amalgam, which is an alloy of mercury with another metal. It differs from other alloys, such as brass or bronze, in being made without the aid of heat, inasmuch as mercury is molten at the ordinary temperature. The word comes to us from the Greek through Old French and means &apos;something soft&apos;. It is a mistake to use technical terms, having a specific meaning, for purposes that are foreign to that meaning. The writer of the quotation is not discussing any combination of metals; he is dealing with the physical process of mixing and is using &apos;amal-

Jan 1, 1931