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SEC. 1. The membership of the Institute shall comprise seven classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Members; 6. Rocky Mountain Members; 7. Junior Foreign Affiliates. All shall be equally entitled to the privileges of membership, excepting that no member of any class whose residence shall be outside of the United States of America, except those residing in Mexico and Canada, shall be entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the class of Member must be at least 27 years of age and must have had at least six years' employment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which he must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain Members.

Jan 1, 1946

By James S. Browning

The Mineral Resources Institute and State Mine Experiment Station of the University of Alabama conducted Humphreys spiral tests on fine coal waste from nine preparation plants of Alabama strip mining operations to determine the feasibility of recovering low ash and sulfur fuel meeting steam coal specifications. The ash in the samples ranged from 9 - 5l%, and the total sulfur ranged from 0.4J- 2.39%. Continuous laboratory tests using a Humphreys spiral gave good recovery of the coal with excellent rejection of the ash and pyritic sulfur. Coal recoveries of 83.6 - 94.1% were achieved from the different samples. Ash content of the clean coal products fell within a range of 5 - 12.2%, with a total sulfur content of 0.62 and 1.10%. In quality, the products were comparable or superior to those now being shipped from the preparation plants.

Jan 1, 1980

By P. R. Gage, R. W. Bartlett

SILICIDE coatings on refractory metals are often applied by transporting a silicon halide vapor to a hot metal surface where dissociation or hydrogen reduction occurs. The subsequent chemical reaction to produce the coating requires diffusion of silicon or the refractory metal through the in situ silicide layer. This solid-state diffusion process step is often slower than the vapor-transport step and, therefore, rate controlling. This situation is analogous to the parabolic oxidation of metals in which the oxidation rate is controlled by diffusion through the oxide layer. The purposes of this study were to 1) measure the rate of formation of MoSiz and MoSi2 coatings under conditions such that the silicide diffusion process is rate controlling and lower silicide compounds are not formed and 2) determine by a marker experiment whether silicon or the respective refractory metals are the principal diffusing species in the disilicides.

Jan 1, 1965

By D. Malhotra, R. M. Hoover, F. N. Bender

The paper discusses the effect of aeration and agitation on grade and recovery of molybdenite. A series of factorially designed flotation tests were carried out in a "Leeds Automatic Laboratory Flotation Cell." Analysts of flotation results indicate that molybdenite has fast floating and slow floating components. The rates of fast floating components, which do not create a problem inflotation, could be varied by changing agitation or airflow rates. However, the rate of slow floating components was stable and was only a function of residence time. Aeration has a significant effect on the grade of MoS2 and only a slight effect on the recovery of MoS2. Agitation has a slight effect on the grade, but does not effect the recovery of molybdenite. The implications of the results on the design of flotation cells and control and optimization of the existing circuits are also considered.

Jan 1, 1981

By A. D. Bryant

APPROXIMATELY 2 1/2 million tons of silica sand and ground silica with a value of $7.25 million is produced annually from the Ottawa, Illinois, district. These silica products come from the well known St. Peter sandstone formation which covers part of the Mississippi Basin extending from St. Paul on the north to the central part of Arkansas on the south and from Muncie, Ind., on the east to Kansas City on the west. Practically the whole state of Illinois is underlain by this formation except where removed by erosion. Sand produced from the St. Peter sandstone in the Ottawa district is noted for its purity, uniformity, and quality. In addition to various screened grades for industry about 10 pct of the total production of the Ottawa district is ground into silica flour for use in glass, abrasives, enamel, porcelain, tile, for foundry and filter sand, and other uses.

Jan 3, 1953

By F. L. Grammer

THE analyses given in Table I. were made several years ado at my request at a plant using Lake ores. The, are of two furnaces, one making basic, the other Bessemer pig-they gave 6 casts each in 24 hr., also two flushes of cinder between each cast. They- are offered simply for the sake of reference as, so far as I know, it is unusual to find so frequent fall analyses made and none are on record. The variations iii manganese-content in the first and second flushes on the basic furnace are interesting, if no more than a freak-the first flash being invariably higher in manganese. The iron-content of the two slugs from an. average of 12 flushes shows: Basic. Bessemer. Per Cent. Per Cent. Total iron 2.55 1.70 Combined iron 0.72 0.52 Free iron 2.13 7.15

Jan 3, 1913

By Michael W. Roper

McDermitt mine is located southwest of McDermitt, Nev., ½ mile north of the old Cordero mine. Geologic structure of the district is that of a Miocene age collapse-type caldera in a region of Basin and Range normal faulting. The McDermitt ore body possess a tabular, gently dipping configuration within 150 ft of the surface over an area 2200 x 2500 ft. Indicated ore reserves are 3 million tons at 10 lb Hg per ton. The ore zone averages 20 ft in thickness and consists of cinnabar (HgS) and corderoite (Hg3S2Cl2) deposited parallel to bedding in argillized Miocene age tuffaceous lacustrine sediments. The ore body is localized above a silicious sinter-silicified lake-bed breccia. This "opalite" breccia unit possesses a gently dipping, apronlike configuration, striking northeast, parallel the trend of the Cordero deposit, and thinning to the north and northwest.

Jan 1, 1977

CHARLES H. FULTON (author's reply to discussion*).-Mr. E. E. Thum is kind enough to point out an apparent discrepancy between the conclusions drawn from experiments and the results of those experiments. It is stated on page 1383 that carbon dioxide in excess of 1 per cent. is not found in the gases above the carbon reduction temperature (of zinc oxide). This statement refers to such temperatures as occur in ordinary zinc distillation and is not meant to include temperatures above 1350° C., and it should have been so stated in the original paper. When the temperature of the distilling chamber reached 1400° and above, it was noted that the amount of carbon dioxide in the gases increased. This cannot be explained by the equilibrium of the reaction 2CO?CO2 + C, and in seeking reasons for the discrepancy, the experiments of Meyer

Jan 1, 1919

By William E. Ford, Edward Salisbury Dana

The monoclinic Wolframite Group and the tetragonal Scheelite Group are included here. Wolframite Group WoIframite (Fe,Mn)W04 a : b : c = 0.8300 : 1 : 0.8678 B = 89' 22' Hiibnerite MnW04 048362 : 1 : 0.8668 89' 73' WOLFRAMITE. Monoclinic. Axes a : b : c = 0.8300 : 1 : 0.8678; B = 89' 22'. mm"', 110 A 1TO = 79" 23'. ay', 100 A 101 = 62' 54' at, 100 A 102 = 61" 54'. $', 011 A 011 = 81" 54'. Twins: (1) tw. axis c with a (100) as comp.-face; (2) tw. pl. k (023), Fig. 449, p. 171. Crystals commonly tabular (1 a (100); also prismatic. Faces in prismatic zone vertically striated. Often bladed, lamellar, coarse divergent columnar, granular. Cleavage: b (010) very perfect; also parting (1 a (100), and 11 t (102). Fract,ure uneven. Brittle. H. = 5-5.5. G. = 7.2-7.5. Luster submetallic. Color dark

Jan 1, 1922

By Guy R. B. Elliott

If chemical mining is to work, it is extremely important to watch heat balances. Some reactions with coal give off heat and others absorb heat. The reactions of coal with oxygen or air give off heat, but the reactions of coal with steam or with carbon dioxide absorb heat. By balancing the proportions of the two types of reactions, the energy of the coal can be almost completely recovered and environmental damage is minimized. The chemical reactions are listed in Table 1 in the usual form with subscripts (s) and (g) indicating solid or gaseous materials. In reaction 1, solid corbon, C(s), reacts with gaseous oxygen, O2(g), to produce gaseous carbon dioxide, CO2 (g). H means enthalpy or available heat in the material; F is free energy, and it measures whether the reaction can go at all, and if so, how much.

Jan 9, 1973

By D. Moskowitz

IN the course of a general investigation of boride systems, sponsored by the Office of Naval Research, various vanadium boride powders of relatively good purity were prepared which could be used for a determination of the phases present. The X-ray pattern of one of these lots showed, in addition to the known VB1 and VB22 phases, an additional phase, almost certainly of composition V3B4, isomorphous with Cr3B4, Cb3B4, Ta3B4, and Mn3B,. Its pattern fitted in well with the indices worked out by Kiessling for Mr3B4.3 The unit cell for this new compound is orthorhombic, with the dimensions a = 3.030A, b = 13.18A, c = 2.986A7 V=119.2A.' Table I lists the X-ray diffraction data for V.3,.

Jan 1, 1957

In mid-November, a long awaited announcement was made by John Drybrough, President of Granduc Mines Ltd. In short, he said that the extensive exploration conducted by his company and its parent organization, Newmont Mining Corp., have indicated the feasibility of a commercial copper mining operation at the company's prospect located slightly north of Stewart, B.C., and just east of the Alaskan Panhandle. The financing of the project is now being planned. SUMMARY OF PROJECT Granduc reasonably assured ore reserves are estimated at 32,510,000 tons averaging 1.93% copper content before dilution, of which 20,670,000 tons averaging 2.08;:; copper content are situated above the proposed mine access tunnel at elevation 2475 above sea level. The life of the reserves at the planned rate of production is 13 1/2 years. The probability of finding substantial additions to these present reserves is considered good.

Jan 12, 1963

By Garry M. Hughes

Sherritt's new, 3000 tpd, copper- zinc Fox mine is situated 30 miles southwest of Lynn Lake. The copper-zinc orebody is part of a large body of massive and semi-massive sulfides consisting chiefly of pyrite; with chalcopyrite, sphalerite (containing 7-9s Fe) and pyrrhotite in varying proportions which occur within a series of volcanic and sedimentary rocks. The average sulfide content is 67%. Higher zinc zones are masses of pyrite grains cemented by sphalerite with lower than average copper content. Zones higher in copper and lower in zinc are slightly more quartzose. Gold and silver are present in small amounts roughly proportional to the copper content. Surface diamond drilling indicated an orebody containing 12,269,000 tons grading 1.74% Cu and 2.35% Zn to the 2000 ft level. Underground drilling established the tonnage at 11,- 300,000 tons containing 1.96% Cu and 2.74% Zn.

Jan 4, 1972

By A. E. Jenkins, L. A. Baker, N. A. Warner

The electromagnetic levitation technique has been successfully applied to rate studies of the de-carburization of liquid Fe-C alloys from 5.5 to zero pct C at 1660°C using gas mixtures containing 1 to 100 pct CO2 with CO or helium as diluents. The rate was shown to be independent of carbon concen -tration in the melt and only slightly affected by total pressure. The results were shown to be consistent with control either wholly or predominantly by gaseous diffusion. As well as avoiding side reactions with the crucible, levitation allowed precise calculation of reaction rates since the geometry of the system was accurately known. It also enabled interpretation using the established mass-transfer correlations for a gas flowing past a single sphere, The existence of gaseous-diffusion control and the extremely high rates of reaction reported for gas flowing past small spheres are of great practical significance in relation to current investigations into the use of spray-refining techniques in continzcous steelmaking. PREVIOUS work on the kinetics of carbon removal from liquid iron has generally involved the use of oxygen as the gaseous oxidant. Investigations have been made on commercial steelmaking furnaces and in addition laboratory-scale experiments have been attempted with a slag phase present. The general lack of agreement and the obvious difficulty in interpreting the results is at least partly due to the complexity of the systems used. This work has been reviewed by carter1 and more recently by Bods-worth2 and ward.3 The gas-liquid metal reactions have also been studied with slag-free melts by the conventional technique of blowing oxygen onto the melt contained in a crucible. The reaction between the oxidant and carbon could be followed by sampling either the melt or the gas phase. Side reactions with the crucible material have precluded direct interpretation of the results. Fujii, 5-7 using O-A mixtures, attempted to correct for the crucible reaction and reported that the reaction between carban and oxygen occurred at the melt surface and was controlled by gaseous diffusion for carbon contents greater than a critical value and by carbon-diffusion control in the metal for carbon contents less than the critical. The critical value was given as approximately 0.15 pct C. However, whereas this was the case for oxygen contents in the gas stream up to 10 pct, between 10 and 20 pct the rate was found to be approximately independent of oxygen content, and Fujii attempted to explain this observation by postulating the presence of an oxide "film".7 Turkdogan et a1.' have studied iron fuming during decarburizing and suggested gaseous-diffusion control of the reaction above a critical carbon concentration, given as approximately 2 pct C. Filippov9-12 reports in a similar manner to Fujii but makes no mention of the crucible reaction with the carbon in the melt, even though this would be expected with the temperature, crucible material (MgO), and carbon contents used. Both CO2 and O2 were used as oxidant gases. In the present work the decarburization of liquid Fe-C alloys was studied using an adaptation of the electromagnetic levitation technique, and thus the complexities introduced by crucible side reactions were eliminated. In this technique a single sphere of the Fe-C alloy is freely suspended and heated by electromagnetic induction in a flowing stream containing the oxidant gas. The full range of carbon levels up to saturation was studied, the temperature of the melts in this instance being held constant at 1660°C. The oxidant was CO2 which was used either pure or in association with a diluent gas, the total gas pressure being maintained either at 1 atm or at a reduced pressure. Thus the reaction under study was:

Jan 1, 1964

By M. H. Caron

THE most outstanding property of ammonia liquors, used in the ammonia leaching process is their very limited ability to dissolve all compounds present in reduced ore except nickel and cobalt. Although they do have such a high degree of purity, even the smallest amounts of impurities contaminate the precipitate of basic nickel carbonate that may be obtained from pregnant liquors by straight distillation. Figures have been given in a separate paper regarding the extent of such contamination. The product of straight distillation is likely to contain small amounts of Fe, Mn, MgO and SiO2 as well as some sulphate and sulphide. The sulphur can be readily eliminated by calcination of the product at the proper temperature and MgO and SiO2 by reduction and melting of the metal with a suitable flux. After such treatment the metal is relatively pure, and the iron and manganese content will be very small. The cobalt content, however, may vary considerably, depending upon the ore treated. The metal obtained from pure true garni-erite ores usually has only a small cobalt content of less than 1 pct. Metal obtained from medium grade iron-rich nickel ores may show cobalt values from 2 to 3 pct, and the alloy obtained from laterite is likely to contain as much as 10 pct cobalt. By proper treatment a good deal of cobalt may be recovered from lateritic nickeliferous iron ores, and cobalt will become the major constituent of the pregnant liquor if asbolan ores or similar products are treated. The pregnant liquor of "run of mine" nickel ores may have a pinkish shade, indicating the presence of cobalt. It is evident that from such liquors the metals should be recovered separately. Even if cobalt is present in only very small amounts, it would probably be economically justifiable to recover both metals as pure as possible if a suitable process could be devised. The author has made investigations along this line and has patented some processes adapted to the treatment of this type of solutions. Selective Dissolution of Nickel from Basic Nickel Carbonate Containing Some Cobalt: Basic nickel carbonate obtained from true garnierite ores by straight distillation of the pregnant liquors, always contains some cobalt as well as the normal impurities. In. order to improve the quality of the nickel product and to recover most of the cobalt, the following process has been devised. By using liquors with a low CO2 to NH3 ratio, nickel can be redis-solved preferentially to cobalt. It is not a sharp and clean separation but a selective one, for the bulk of the nickel may be redissolved with a small amount of cobalt, and a small residue may hold the bulk of the cobalt. The greatly increased cobalt content of the residue is indicated by a pronounced olive green color, in contrast with the light green color of pure basic nickel carbonate. The following example is given from Dutch patent No. 52788, Klasse 40a. 43 granted June 17, 1942: The original precipitate contained about 0.55 pct cobalt calculated on total nickel + cobalt. Eight hundred and fifty grams of the basic nickel carbonate were redissolved in leach liquor containing 7.12 pct NH3 and 2.12 pct CO2. The weight of the dry residue was about 3.5 pct of the original weight. By analysis it was found that the residue contained: Fe 1.93 pct, Co 6.01 pct, Ni 34.87 pct and also a certain amount of silica. The clear filtered blue liquor was distilled and the precipitate of basic nickel carbonate from this analyzed: Fe 0.008 pct, Co 0.0146 pct, Ni 42.37 pct. It is obvious that this product is considerably more pure, since calculation shows that about 94 pct of the original cobalt remained in the residue. Cobalt and nickel can be recovered by further

Jan 1, 1951

By I. R. Kramer, H. Shen, S. E. Podlaseck

The tensile and creep properties of aluminum in vacuum have been investigated. It was found that the general effect of a vacuum environment was to reduce the rate of work hardening. Results obtained from creep tests showed that lowering the test pressure from 2 x 10-4 to 10-7 torr produced a decrease in the activation energy as much as 500 cal per mole. An attempt is made to explain these effects in terms of how the surface-stress field of a specimen may be affected by a vacuum environment during plastic deformation. In a previous paper,' the results were reported of some of our early work on the effect of vacuum environment on the stress-strain curve of aluminum single crystals. This effort has been extended to the studies of the tensile and creep properties in vacuum as a function of various metallurgical parameters. Some of the recent surface-effect studies2'3 have revealed that a region of high dislocation density, the so-called "debris" layer, is formed near the surface of the specimen as a result of plastic deformation. This layer acts as a surface barrier to oppose dislocation movement. The strength of this barrier depends on the surface condition such as oxidation or surface removal. Experimental results obtained from surface-removal work2, 3 indicate that such a surface barrier, which may be characterized by a stress field, affects the applied stress and the rate of work hardening. In the case of aluminum, this stress field was found to be directly proportional to the strain and the strain rate; however, the slope of this curve is independent of orientation of the crystal and may be altered by using different surface treatment. Since the escape of dislocations may be retarded by the presence of an oxide on the surface of a specimen, it is expected that a change in the rate of oxidation in vacuum will affect the process of dislocation accumulation in the debris layer. Consequently, it also affects the plastic behavior of a metal. This paper reports the changes in some of the creep and tensile properties of aluminum in vacuum and discussions of the observed effects in terms of the concept of the "debris" layer. EXPERIMENTAL PROCEDURE Tensile Tests. A sketch of the tensile apparatus is given in Fig. 1. This apparatus was contained in a bell jar (14 in. diam by 24 in. high) connected to a 10-in. vacuum system. The load was applied to the specimen by means of a gear train which was driven by a magnetic clutch located outside the vacuum chamber. The specimen, held by a pair of square shoulder grips, was attached to the load cell at the top and the drive gear at the bottom. A displacement transducer was placed between the two grips as shown in the figure to measure the elongation. Signals of elongation and load were amplified and recorded on an X-Y recorder. The system was capable of detecting loads as small as 0.025 lb and displacements of 0.0002 in. Shoulder-grip specimens of aluminum single crystals, having a nominal square cross section of 1/8 by 1/8 in. and a 3-1/2-in, gage length, were grown by the Bridgeman techniques. The original purity was 99.997 pet. The orientations of the crystals investigated are shown in Fig. 4(a). The crystals were annealed at 600°C for 2-1/2 hr, electropolished, and placed in the vacuum test chamber without any delay. All the crystals were deformed at a strain rate of 4 x 10-5 sec-1 at 24o ± 3°C. A study was made to find whether a chemically passive surface film would give the same effect as a vacuum environment. Specimens of aluminum 1100 (0.187 in. diam with a grain size of 0.1 mm)

Jan 1, 1965

By C. C. Martin, M. C. Fuerstenau, R. B. Bhappu

Experiments revealed that quartz could not be floated in conductivity water at any pH with a long-chained sulfonate as collector. Various cations, Fe+++, Al+++, Pb++, Mn++, Mg++, Ca++, are shown to function as activators when the pH is such that the cation hydrolyzes. As the solubility product of the various cation-sulfonates was exceeded at the concentrations involved, precipitated cation-hydroxy-sulfonates, e.g. Fe (RSO3)2OH must be functioning as the collector in these systems. A number of interesting and important phenomena were revealed during a study of the response of beryl to sulfonate flotation.' Perhaps the most important observation is the effect of various cations on flotation response. Experiments showed that in the vicinity of pH 3.0, about three ppm Fe+++ increased recovery of leached beryl from about 60 pct to 100 pct, whereas about four ppm Ca+ + reduced the recovery from 60 pct to 2 pct. With the exception of ferric iron, all of the other cations investigated reduced flotation recoveries drastically at this pH. As postulated in the paper Sulfonate Flotation of Beryl,' even with low concentrations of polyvalent cations and sulfonate (on the order of one ppm), cation-sulfonates are precipitated immediately in solution. That is, blueish-white clouds were noted to form after given additions of salts to known solutions of sulfonate. Furthermore, it was also shown that one-hundred-fold more ferric iron than necessary to form the precipitated cloud had to be added to effect complete flotation. In other words, some form of solid ferric sulfonate was found to function as the collector in these systems. The form of the compound was suggested to be Fe(RCO3)2OH and that bonding to the surface occurs through the hydrogen of the hy-droxyl. As the form of this compound was shown to be dependent on the extent of hydrolysis of ferric iron, it is to be expected that ferric iron will be unique in some pH region. Further, if the presence of hydroxyl in the neutral precipitated compound is of primary importance, then other cations should function similarly but at different values of pH, since they will hydrolyze at different concentrations of hydroxyl ion. To determine whether the premise of hydrolysis is correct, the study was extended to quartz systems in the presence of various cations at various values of pH. EXPERIMENTAL MATERIALS AND METHOD Sodium alkyl aryl sulfonate was chosen as the collector for the experimental work. The reagent, sup plied as a courtesy sample by the Shell Chemical Co., has the following physical properties: Physical form Solid — Finely ground Sulfonate content, pct wt 95 to 97 Molecular Weight 450 to 470 Number of carbon atoms in hydrocarbon chain 25 to 30 Melting Point, OF 250 to 260 Solubility Soluble in water with gel formation at concentrations higher than 25 pct by weight sulfonate This particular reagent was chosen because of its high active sulfonate content, long-chain length, and solid form. With the exception of the frother and sulfonate, all other chemicals were of reagent grade quality. Conductivity water was used in the experimental work. This water, made by passing distilled water through an ion exchange column, had an average measured conductivity of one micromho. Experiments were conducted at room temperature in a small glass flotation cell with the following procedure: 1) A redetermined amount of water and salt solution (e.g. CaC12 . 2H2O) were combined and the pH adjusted to a given value. 2) A given amount of sulfonate was added so that final solution volume was 130 cc. 3) One drop of Dow 250 frother was added. 4) Five g of quartz were added and the system conditioned for five minutes. 5) The pH of the system was measured (termed flotation pH).

Jan 1, 1963

By P. L. Raffo, T. E. Mitchell

Single crystals of Ta-Re alloys have been deformed in tension and compression as a function of solute concentration and temperature. The temperature dependence of the yield stress is decreased by alloying. At low temperatures there is a minimum in the yield stress (at about 2 at. pct) as a function of concentration. Three-stage hardening was not observed in the alloys. Linear hardening rates, where observed, were characteristic of stage II in pure tantalum. At low temperatures and high concentrations, work softening was often prominent at high strains. Electron microscopy revealed that dislocations are mostly of screw orientation, although heavily jogged and cusped, and often occurring in dipole pairs. The alloys become more prone to cleavage with increasing rhenium content, due mostly to an increasing yield stress rather than a change in cleavage strength. Alloying apparently decreases the Peierls stress of bcc metals at low temperatures by facilitating kink nucleation at solule atoms on screw dislocations. Higher solute concentrations further increase the yield stress. Quantitative calculations and comparisons with other bcc alloy systems are made to show that the predominant hardening mechanism is due to the interaction of dislocations with misfitting solute atoms close to their slip planes. The interaction is so localized that the core dilatation of dislocations could be important. CONSIDERABLE interest has arisen in recent years concerning the mechanical properties of unalloyed bcc metal single crystals.'-7 These and similar studies on polycrystalline materials have resulted in a considerable understanding of the macroscopic yielding characteristics8, 9 and the process of work hardening.'' This latter advance is due in a large part to the increased use of transmission electron microscopy in P I RAFFO junior Membar AlMF is Metallyureist Iewis such studies and the general observance of three stages of work hardening in the shear stress-shear strain curves. The properties of substitutional alloy single crystals of bcc metals have not been determined in as much detail as in the pure metals. Insufficient systematic studies have been made on the effect of alloying on the magnitude and temperature dependence of the yield stress or the stress-strain curves. The alloy systems which have been studied to some extent have been Ta-W,11, 12 Ta-Mo," Ta-Nb,12'14 Mo-Re,15 W-Re,16 and alloys of iron with nickel,17 platinum,17 vanadium,18 and aluminum.18 A large body of data exists on Fe-Si alloys, but these have mainly been a result of the experimental convenience of using this material in place of unalloyed iron, rather than a comprehensive study of the mechanical properties of the alloy system per se. The present authors have previously reported additional data on the properties of Ta-Re, Ta-W, and Ta-Mo alloy single crystals.1g Some of the data on Ta-Re alloys will be described later in this paper. Briefly, single crystals of Ta-Re (1.2 to 10.6 pct), Ta-W (6.2 and 10.2 pct), and Ta-Mo (2.9 and 9.0 pct) were grown by the floating zone method in vacuum. Compression tests were performed in the temperature range 77" to 623°K. Slip was found to occur in Ta-Re alloys at 77' and 298°K on the (~ll)[lil] system and slip lines were coarser and straighter than in unalloyed tantalum. No three-stage hardening was observed in any of the alloy systems and the curves were nearly parabolic. At temperatures above 175°K the yield stress* increased monotonically with in- creasing composition while at 77" and 175°K the yield stress initially passed through a minimum after which it began to increase again for concentrations greater than about 2 pct Re. Similar minima were observed in Ta-Mo alloys and to a lesser extent in Ta-W alloys. The minimum was interpreted as being a result of a

Jan 1, 1969

By Sidney G. Parker, Jack E. Pinnell

Cubic ZnSe crystals have been grown with HCl, HBr, and I, as chemical transport reagents. The growth of large, well faceted crystals is in the order HCl < HBr < I, with some produced by I, transport being 1 cm on an edge. ZnSe:I crystals showed no strain in cross polarized light and were homogeneous as determined by electron microprobe. These ZnSe:I crystals had a mobility at 25°C of about 300 sq cm per v-sec and contained 103 dislocations per sq cm; further, these crystals were pure cubic and showed both photolumi-nescence and photo conductance. Doping was attempted during crystal growth. ZnS and Zn (S,Se) crystals were also grown by I, transport. ZnSe crystals have been grown by most of the common techniques.1"6 Of these, chemical vapor transport as developed by Kaldis2 showed promise of producing high perfection, cubic ZnSe. With chemical transport, crystals can be grown far below the transition temperature for conversion of cubic to hexagonal structure. A small temperature gradient between source and growth region tends to allow near equilibrium growth, which should lead to good crystalline perfection. Because it is necessary to form volatile compounds, halogens or their compounds are extensively used as transport agents. HCl, HBr, and I, were compared as transport agents for growth of ZnSe crystals. Doping during crystal growth was attempted. ZnS and ZnSxSe1-x crystals were also grown by chemical transport. Electrical and optical properties of the crystals were examined. EXPERIMENTAL Fig. 1 is a sketch of the growth apparatus, which was a modification of Kaldis&apos;. A quartz rod which butted against the seed crystal served as a heat sink to promote growth only on the seed. Initially, crystal growth was attempted with ZnSe prepared by wet chemical methods. Because such a material contained oxides and selenates, HC1 reacted with these oxygen compounds to form H2O and no ZnSe transport occurred. Further, this ZnSe contained about 10 ppm Cu plus other impurities. High purity ZnSe, containing small amounts or no oxygen compounds, was prepared by reaction of H2Se with zinc vapors at 600° to 800°C in an atmosphere of palladium diffused H2.7 The ZnSe thus produced was usually copper free and contained only 1 ppm by weight of magnesium as determined by emission spectrographic analysis. G.E.&apos;s electronic grade ZnS, which had about 10 ppm metallic impurities, was used without further treatment. ZnS-ZnSe charges were prepared by mixing the two compounds together, then sintering 24 hr at 1100°C in an H2S ambient. The gases, HBr and HC1, were commercial grade, of 99.9 pct purity, while the I2 was 99.999 pct pure. The single crystal seeds with (111) faces for growth were mechanically held in place by sealing the outer quartz tube to the growth tube. After the charge was introduced, the system was outgassed at l0-5 torr while heated to 500°C. The desired quantities of transport reagents were then sealed off in the system, which had been cooled to 25°C. The growth tubes were inserted into a furnace with the desired temperature and thermal gradient. The system was allowed to cool for 1 to 12 hr from growth temperatures of about 850" to 25°C. The tubes remained stationary during crystal growth. HCl CHEMICAL TRANSPORT GROWTH Preliminary runs with HC1 had a temperature gradient of 100° to 200°C and no seed or heat sink. Only small crystals were obtained in these experiments as

Jan 1, 1970

By H. E. Cline, T. H. Alden

A study zvas made of rate-sensitive plastic deformation and superplasticity in alloys of lead and tin. These alloys (lead, PO-19 pct Sn, Sn-38 pct Pb, Sn-2 pct Pb, tin) were extruded, aged at room temperature, or melted and resolidified to produce a variety of ~nicrostrnctures. Flow stress us strain rate data were obtained frorn tension tests for strain rates between 10-6 and 1 min-1. The curve log o .us log £ was S-shaped jor fine-grained materials and approxinzately linear for coarse-grained nzaterials. At constant grain size, the behavior was relatively insensitive to conposition. High rate sensitivity (d log o/d log k) and superplasticity occurred at intermediate strain rates in fine-grained materials and are believed to be associated with a transition with strain rate in the mode of plastic flow. This transition was shifted to higher strain rates with increasing temperataire or decrensing grain size. The high rate rneclzanisrn is presunzed to be slip, while rnetallographic evidence sug-gests that the low rate lnechanism is pain boundary sliding. PEARSON&apos; discovered that extruded eutectic alloys of Pb-Sn and Bi-Sn could be elongated as much as 2000 pct in tension. The ability for stretching decreased with aging time or annealing to increase the grain size. At high strain rates, or if the material was in the cast condition, normal ductility was observed. Following deformation of the extruded Pb-Sn eutectic at low rates, Pearson observed an equiaxed granular structure on an initially flat surface, while rapid straining produced elongated grains. He attributed the large deformation in the extruded alloys to the persistence of extremely small grains to a temperature sufficiently high for inter granular flow. Avery and backofen2 measured the strain rate sensitivity of the flow stress, m = d In old In 6, in the Pb-Sn eutectic and established a correlation between m and the tensile elongation. In the extruded eutectic alloy the strain rate sensitivity was 0.1 to 0.2 at rapid rates and the elongation was small, while at low rates m increased to 0.4 to 0.6 and superplastic elongation was observed. They also noted a grain size effect. In the case of the cast Pb-Sn eutectic the strain rate sensitivity remained at 0.1 over the range of strain rates of their experiment (3 x 10"3 to 2 min-I). These authors suggested that diffusional (Nabarro-Herring) creep was the mechanism by which deformation occurred at low strain rates, while climb-controlled creep occurred at high rates. Two predictions of this model are that, at low strain rates, the strain rate sensitivity approaches 1, i.e., Newtonian viscosity, and that the strain rate at constant stress varies as D/L2, where D is the coefficient of self-diffusion and L the grain size. More recently, a mechanical and microstructural investigation of the dilute superplastic alloy, Sn-5 pct Bi, has been done.3 The results show that the high strain rate sensitivity is associated with a transition with strain rate of the mechanism of plastic flow. At low strain rates, grain boundary sliding and its associated accommodation processes were evident, while at high strain rates quasi-uniform slip was concluded to be the dominant deformation process. The following experiments were performed to extend our knowledge of the phenomena of superplasticity to a larger range of strain rates, compositions, temperatures, and microstructures in the Pb-Sn alloy system. The question of why a cast structure does not exhibit viscous behavior although it appears to have a fine microstructure2 was investigated.

Jan 1, 1968