Search Documents

By FREDERICK LAISY

A NUMBER of new plants for the treatment of copper ores were completed or under construction during the year. Among these may be mentioned the plants of the International Nickel Co., those of the Hudson Bay Mining and Smelting Co. and of the Roan Antelope Copper Co. Three copper re- fineries have been constructed, one at El Paso, Tex., and the other two in Canada. Two more are projected, one in France and one in England. The International Nickel Co.'s plant consists of an 8000-ton concentrator and a smelting plant containing thirty 10-hearth Herreshoff roasting furnaces, five reverberatory furnaces, and eight Smith-Pierce converter5 . The smelting plant is estimated to have a capacity of 5000 tons of ore or concentrate per day. The roasters are superimposed on the reverbratory furnace plant. As a consequence of this arrangement, the furnace building is unusually high. being 183 ft. from yard level to highest roof elevation.

Jan 1, 1931

By John Wulff, Robert Kamm, M. A. Steinberg

IN a previous paper1 from this laboratory, the development of a lead grid method for exploring the distribution of strain and density within metal powder compacts was described, In that work thin lead foil with rectangular holes cut at regular intervals was inserted with the powder fill, the arrangement pressed and then radiographed to permit measurement of the deformation of the lead grid. Densities at each grid element obtained in this manner were plotted as a function of the die dimensions. From such plots it was, found that the densest part of a compact pressed from one side (the top) is at the top outer region and the least dense at the bottom outer region -of the specimen. The axial density maximum occurs more often nearer the bottom than at the top. As a result of such exploratory measurements, it appeared reasonable to conclude that variations in density could be attributed in the main to die wall friction. Thus compacts of large diameter appeared relatively uniform in density except where the die fill had been uneven. Finally it was found that lubrication of the finely finished die cavity contributed more to magnitude and uniformity of density within the compact than interparticle lubrication. Since publication of the above results, it was found that circular-hole grids could be more accurately made and, when deformed within the powder, more readily measured and analyzed. Much of the former work was repeated and new results which include the effect of lubrication, compact height, pressure, speed of pressing and vacuum pressing are reported in the present paper. CIRCULAR-HOLE GRIDS AND ANALYSES OF RADIOGRAPHS Commercial lead sheet 0.008 in. in thickness was used in all the work reported. The 0.0938-in. diam holes were punched in the sheet on 1/8-in, centers to an accuracy of 0.001 in. The finished grid used contained eight or more holes in a row and from I to 24 rows. The lead sheet was clamped between two pairs of brass strips bolted to a small milling machine table which was itself bolted to a bench in correct position near a vise which held the punch. Travel of the lead grid in two dimensions was controlled by two steel lead screws calibrated in 0.001-in. divisions. A stripper plate was used on the punch to avoid distortion of the lead foil. A high carbon-high chromium (chrocar) one-piece steel die was used throughout the work. The die cavity was 1,125 in. in diam and the clearance between plungers and die wall was 0.001 in, The die was also used for pressing from both ends with two long plungers. Finally, lapping of die and plungers gave a surface whose rms value on an Abbot profilometer was 5 micro-in. The die walls and plungers were, except where otherwise noted, lubricated with a stearic acid suspension in benzene. This was put on in multiple layers and allowed to dry before filling the die.

Jan 1, 1948

By G. D. Gemmell

Effects of solid-sdutidn alloying with titanium, molybdenum, and tungsten at concentrations up to 10 pct on the strength of pure columbium at elevated temperatures (mainly 2000°F) have been investigated by means of creep-rupture, hot-tensile, and hot-hardness testing and recrystallization studies. ThIS paper presents some results from the initial part of a study of the effects of alloying on the high-temperature strength properties of columbium. The elevated-temperature strength characteristics of pure columbium were first studied. Binary alloys of columbium with titanium, molybdenum, and tungsten containing 1, 5, and 10 pct of the solute elements were chosen on the basis of their high melting points, their known solid solubility in columbium, and results of separate oxidation-resistance studies of columbium alloys. EXPERIMENTAL PROCEDURE All the materials used were of highest purity. A typical analysis of the columbium is shown in Table I. Compositions of the alloys are also given in Table I. To evaluate the strength properties of pure co-lumbium and the alloys at elevated temperatures, creep-rupture, hot-tensile, and hot-hardness testing was done on recrystallized material. To prepare the pure metal and the alloys for these tests, 1- 1b buttons were made in a water-cooled copper crucible, inert atmosphere, tungsten arc furnace. Tapered ingots, 3 in. long, were made from these buttons by a skull-casting technique and these were machined to 1/2 in. diam, swaged to 50 pct reduction (pure columbium at room temperature, alloys at lowest temperature possible without cracking, generally in range 1100" to 1800°F) and heated in vacuum (lo-' mm Hg) for 16 hr at 2550°F for re-crystallization and homogenization. The resulting grain diameter was 0.1 to 0.3 mm. The 10 pct Mo alloy casting was not successfully swaged at temperatures up to 1800°F without cracking and was not included in the test program. Creep-rupture testing was done at constant load in vacuum on cylindrical specimens of 0.16 in. diam, using Instron capsules. The pressure at test temperatures was less than 10-1 mm Hg. Hardneas readings taken on the test specimen before and after testing were used as a check on possible gaseous contamination. Hot tensile tests in vacuum on cylindrical specimens of 0.125 in. diam were also made with Instron equipment at a strain rate of 0.067 min.-l. Hot-hardness measurements were taken with a unit constructed at the Du Pont Experimental Station. The test piece, supported on an alumina anvil, and the molybdenum indenter shaft with sapphire tip is heated in a platinum-wound furnace. The load applied to the pyramid indenter is measured by strain gages attached to a proving ring located outside the hot zone. In the measurements reported here the load was I kg. The tester operates in a vacuum of about 10"5 mm Hg and is capable of temperatures up to 1400°C.

Jan 1, 1960

By R. J. Hafsten, E. S. Davenport, R. A. Grange

THE influence of austenite grain size upon the hardenability of steel is now fairly well understood; for a given austenite, increasing the grain size increases the depth of hardening, and, since the latter is related to the fundamental transformation behavior of austenite, it follows that austenite decomposition must, in general, be retarded by increasing grain size. To date, very little quantitative information bearing directly on the effect of austenite grain size upon the progress and result of isothermal transformation has been published. Davenport and Bain,1 and Zimmerman, Aborn and Bain2 have shown that the transformation is definitely retarded in hypereutectoid plain carbon steels at temperatures near and above the upper region of rapid transformation (Ar') when the austenite grains are increased in size. More recently, Griffiths, Pfeil and Allen3 investigated the effect of a series of different heating (austenitizing) temperatures upon the progress of isothermal transformation at 1245°F. (675°C.) and 745°F. (395°C.) in a medium carbon, low-alloy steel; while they reported no measurements of the austenite grain size, their results suggest that increase in grain size retards austenite transformation at 1245°F. (675°C.), but has no appreciable effect at 745°F (395°C.). The present paper deals with the results of a study of the isothermal transformation of austenite in a single commercial alloy steel in which a fine-grained or a coarse-grained state was induced by appropriate selection of austenitizing temperature. The data are presented in the form of isothermal transformation diagrams, which clearly show that coarsening the grains lessens the rate of transformation of austenite to proeutectoid ferrite and pearlite-that is, at temperature levels above about 1000°F. (540°C.)-but is without significant effect at lower temperatures where the transformation product is bainite or martensite. It is to be presumed that the foregoing statement would be valid, at least in principle, for many other grades of steel; it confirms again that the mechanism of transformation to a pearlitic structure is fundamentally different from that to an acicular structure. A number of related observations were made, which seem to throw some light on the transformation process as it takes place in alloy steels, particularly at temperature levels in the vicinity of 1000°F. (540°C.), where the transition from lamellar to acicular structures occurs. These data are discussed briefly in the belief that they may lead to a clearer understanding of this aspect of the subject. MATERIAL AND EXPERIMENTAL PROCEDURE The material investigated was a commercial grade of S.A.E. 4140 steel, the composition of which was as follows: 0.37 per cent C, 0.77 per cent Mn, 0.98 per cent Cr and 0.21 per cent M0. It was hot-rolled to a 1 1/8-in. round bar and normalized by air-cooling from 1800°F. (980°C.).

Jan 1, 1941

By M. A. Steinberg, J. Wulff, R. Kamm

In a previous paper1 from this laboratory, the development of a lead grid method for exploring the distribution of strain and density within metal powder compacts was described. In that work thin lead foil with rectangular holes cut at regular intervals was inserted with the powder fill, the arrangement pressed and then radiographed to permit measurement of the deformation of the lead grid. Densities at each grid element obtained in this manner were plotted as a function of the die dimensions. From such plots it was found that the densest part of a compact pressed from one side (the top) is at the top outer region and the least dense at the bottom outer region of the specimen. The axial density maximum occurs more often nearer the bottom than at the top. As a result of such exploratory measurements, it appeared reasonable to conclude that variations in density could be attributed in the main to die wall friction. Thus compacts of large diameter appeared relatively uniform in density except where the die fill had been uneven. Finally it was found that lubrication of the finely finished die cavity contributed more to magnitude and uniformity of density within the compact than interparticle lubrication. Since publication of the above results, it was found that circular-hole grids could be more accurately made and, when deformed within the powder, more readily measured and analyzed. Much of the former work was repeated and new results which include the effect of lubrication, compact height, pressure, speed of pressing and vacuum pressing are reported in the present paper. Circular-hole Grids and Analyses OF Radiographs Commercial lead sheet 0.008 in. in thickness was used in all the work reported. The 0.0938-in. diam holes were punched in the sheet on 1/8-in. centers to an accuracy of 0.001 in. The finished grid used contained eight or more holes in a row and from I to 24 rows. The lead sheet was clamped between two pairs of brass strips bolted to a small milling machine table which was itself bolted to a bench in correct position near a vise which held the punch. Travel of the lead grid in two dimensions was controlled by two steel lead screws calibrated in 0.001-in. divisions. A stripper plate was used on the punch to avoid distortion of the lead foil. A high carbon-high chromium (chrocar) one-piece steel die was used throughout the work. The die cavity was 1.125 in. in diam and the clearance between plungers and die wall was 0.001 in. The die was also used for pressing from both ends with two long plungers. Finally, lapping of die and plungers gave a surface whose rms value On an Abbot profilometer was 5 micro-in. The die walls and plungers were, except where otherwise noted, lubricated with a stearic acid suspension in benzene. This was put on in multiple layers and allowed to dry before filling the die.

Jan 1, 1949

By J. M. Snook, F. C. Langenberg

FOR a better understanding of the melting and refining processes, the oxygen content of the steel bath should be determined. The oxygen content influences many process and product variables such as the efficiency of alloy recoveries, the ingot structure (through reaction with carbon in the steel), certain reaction rates, cleanliness (formation of indigenous oxide inclusions), and mechanical properties. Many methods of sampling liquid steel for oxygen have been devised. These methods can be divided into two main groups: 1) taking samples directly in the furnace or ladle;'-'0 2) removing the metal from the furnace or ladle in a sampling spoon and pouring it into a mold, or drawing the metal from the spoon into a sample holder.11-l4 The advantages and disadvantages of the two general sampling methods are presented in Table I. The bomb-sampling technique described by Huff, Bailey, and Richards8 has been used by the Crucible Steel Co. in certain research projects where oxygen contents were needed. It was recognized that a localized boiling condition could result when the mold is introduced into the steel bath, although the work of Gilbert and Bailey9 seems to indicate that the carbon boil occurring in the bomb-sampler cavity has a negligible effect on the oxygen content. In order to confirm the reported negligible effect of a carbon boil, additional work was done with adaptations of the conventional bomb sampler. The methods used are shown in Fig. 1 and are as follows: 1) Type A: aluminum wire (0.125-in. diam) coil in cavity; steel cap over mouth 2) Type B: aluminum cup in cavity; aluminum cap over mouth, 3) Type C: aluminum cup in cavity; steel cap over mouth, 4) Type D: fine aluminum wire (0.013-in. diam) in cavity; steel cap over mouth. The amount of aluminum wire in the Type A and D samples varied from 0.8 to 1.2 pct of the sample weight. The aluminum cups averaged 2.0 pct of the sample weight; the latter were used to ensure that the steel contacting the walls of the bomb cavity was fully killed. Samples were taken from plain carbon heats made in open-hearth furnaces. This grade of steel before silicon additions is essentially an Fe-C alloy and the effects of other alloying elements on the oxygen activity can be neglected. The results of sampling with the bomb samplers is shown in Fig. 2 where the percent oxygen is plotted against the percent carbon on log-log paper. Spoon sample results on the same grade of steel where the sample was killed in the spoon are shown in Fig. 3. The oxygen contents were determined by the vacuum fusion method. A comparison of Figs. 2 and 3 shows that the oxygen concentrations obtained with the spoon-sampling method (metal killed in the spoon after slag removed

Jan 1, 1960

By E. H. GRAFF

PREPARATION of mechanically loaded coal in mines where seams contain considerable impurities is a subject that requires careful consideration before machines are installed, unless provision is made at the tipple for its preparation. Conditions vary a great deal in the different seams, so much so that a mechanical loader may be unsuccessful in one seam and yet the same machine may make good in another where conditions are different. The effect of impurities in the coal seam on mechanical loading will also vary according to the thickness of the seam. In thin seams impurities will be more difficult to remove than from thick seams, as will appear later. For the past several years the New River Co. has done considerable experimenting with loading equipment and during this process has changed from one machine to another.

Jan 1, 1926

By E. Miller, K. L. Komarek, M. Ettenberg

The activity of aluminum in solid Co-A1 alloys has been measured by an isopiestic technique between 850° and 1200°C from 45 to 80 at. pct Al. The activity shows a Precipitous decrease around the stoichzornetric composition of CoAl. Free energies of mixing have been calculated over a limited composition range. Considering an antistructure-vacancy defect mechanism, the degree of intrinsic disorder, a , in CoAl was related to the alunminum activity. Excellent agreement between the calculated and experimental activity curves was obtained for a = 1.25 x 10-4. ThERMODYNAMIC properties of solid aluminum-transition metal alloy are being studied in an investigation of disordering in ordered compounds. In a continuing series of investigations, activities of solid Fe-1,' Ni-A1, kd r-A13 alloys have been measured. From the results for Fe-A1 and Ni-A1, the degree of intrinsic disorder for the equiatomic compounds was calculated2 using equations derived by Wagner and chottk. From the results for Cr-A1 the degree of intrinsic disorder was calculated from equations derived by Orr.' In this paper, the results of the study of Co-A1 alloys are described. Published activity data in the Co-A1 system has been limited to liquid alloys at 1600°C.° A heat capacity study7 of stoichiometric CoAl indicated that a second-order phase transformation occurs at 790° C, attributed to an order-disorder reaction. Oelsen and Middel,' employing the calorimetric mixing of pure liquid metals, obtained heats of formation for compositions from 6 to 90 at. pct Co. Heats of formation for 50 and 78 at. pct Co alloys have also been measured by acid solution calrimetr. The Co-A1 phase diagram, as compiled by Hansen and Anderko,lo is in good agreement with more recent X-ray evidence. The method for measuring activities of aluminum in this study is essentially that employed in the studies of the Fe-1,' i-Al, and r-A13 systems. This isopiestic method entails placing cobalt specimens, in a temperature gradient, in a sealed alumina system containing a pure liquid aluminum source of fixed vapor pressure. The specimens are equilibrated, cooled to room temperature, and their final compositions determined. From the measured temperature of the specimens and the known vapor pressure of pure aluminum the activities of aluminum in the alloy can be calculated. EXPERIMENTAL PROCEDURE The cobalt was 3-mil-thick sheet of 99.9 pct purity (herritt Gordon Mines Ltd., anada). The major impurities were 0.1 pct Ni, 0.014 pct C, 0.018 pct Fe, 0.004 pct S, and 0.005 pct Cu. The aluminum metal had a purity of 99.99 pct (Aluminum Corp. of America) and all alumina parts were 99.7 pct A1,O3 (Triangle RR Grade, Morganite Refractories, Inc.) with major impurities 0.05 pct SiOz, 0.1 pct Fe203, 0.2 pct NazO, and 0.05 pCt K20. Runs 1 to 3 were made with annular cobalt specimens (12 mm ID by 21 mm OD) punched from the sheet. The specimens were deburred and degreased in carbon tetrachloride and in acetone. The samples, each weighing about 150 mg, were then positioned along an alumina rod, a in. OD by 14 in. long, separated by alumina spacers, i in. ID by | in. OD by & in. long. The lower end of the rod was placed in a hole drilled in the center of an 80-g aluminum cylinder. This assembly was put into an alumina crucible, 1+ in. ID by 13 in. OD by 3+ in. high, and the position of each sample was measured to within 50.5 mm relative to the bottom of the crucible. An alumina tube, 28.5 mm ID by 35.5 mm OD by 14 in. long, closed at the top, was slipped over the whole assembly, so that it fitted snugly into the bottom crucible. The entire reaction assembly was tied with molybdenum wire and lowered into a mullite tube, closed at the bottom. A quartz thermocouple tube, closed at one end, containing a t/Pt-10 pct Rh thermocouple, calibrated according to the specifications of the National Bureau of standards,'' was placed along the reaction assembly inside the mullite tube. The temperature of each specimen could be determined by gradually raising the thermocouple and measuring the temperature gradient along the reaction assembly. The combined error in temperature measurement and sample position resulted in a total error of Q°C in the recorded temperature of each sample. The mullite tube was sealed at the top by a water-cooled brass head, connected to a conventional glass vacuum system. The aluminum reservoir is heated to its melting point sealing the alumina system containing the samples. During this process the pressure is maintained below 0.01 li Hg. During subsequent heating to establish the proper temperature gradient and throughout the entire run the pressure is maintained below 2 1 Hg by means of a two-stage mechanical pump. Equilibration runs lasted from 4 to 6 weeks and were terminated by air cooling. The temperature of the liquid aluminum reservoir was brought below its melting point in less than 20 min. For runs 4 and 5, alloy buttons with 49 and 69 at. pct A1 were prepared from the initial high-purity metals by arc melting under purified argon. The alloy buttons were comminuted to powder with an alumina mortar and pestle until the powder passed through a 400-mesh screen, particle size 0.0014 in. Portions of this powder weighing between 50 and 200 mg were placed in small alumina trays, 25 by 15 by 5 mm, which were then

Jan 1, 1969

By J. E. Flinn, E. R. Gilbert

Recently, Green reported some high-temperature, 0.60 to 0.89 T3, creep results on unalloyed tantalum. From his study he determined an activation energy of 114 kcal per mole for steady-state creep using the T, differential-temperature method25 for testing. He accounted for the difference between this value and 110 kcal per mole for self-diffusion by the temperature dependence of the elastic modulus, 4 kcal per mole. This reported activation energy is in apparent disagreement with that which can be determined from Green's isothermal data, which we have plotted as log creep rate vs 1/T in Fig. 15. From this figure, it appears that there are two activation energies of -185 kcal per mole at the higher temperatures and -75 kcal per mole at the lower temperatures. It is not obvious that the data can be fitted to a straight line corresponding to an activation energy of 114 kcal per mole. One is led to two possible conclusions regarding Green's study: there are two discrete processes controlling the creep rate from 0.60 to 0.89 Tm or the apparent activation energy is not discrete but continuously increases with increasing temperature. The former speculation would be in closer agreement with the high-temperature creep behavior of tungsten.28 The apparent disagreement between the activation energies determined by the AT and isothermal methods certainly suggests that further study on the high-temperature creep of tantalum is needed.

Jan 1, 1967

By Joseph Daniels

(San Francisco Meeting, October, 1911.) I. THE FRITZ ENGINEERING LABORATORY. TEE Fritz Engineering Laboratory was built under the direction of John Fritz, and presented by him to the University. A view of the building, looking east, is shown in Fig. 1. . The building was started in 1909, and completed in 1910, although all of the equipment was not placed until later. Mr. Fritz gave his personal attention to the details of construction and equipment, and it was his custom to drive over every day to the University from his home in Bethlehem, and spend some hours watching the work, offering suggestions, making changes, and planning new work. The result is a building and an equipment which embody his practical ideas. The laboratory structure is of the steel mill-building type, of light-colored brick, 91 by 114 ft., of which a section is shown in Fig. 2 and the floor-plan in Fig. 3. The steel frame carries the roof and traveling crane-way. Ample light has been provided by numerous windows in the side and end walls, in the clerestory, and by a skylight, 84 ft. long and 9 ft. wide, in the north roof. The main aisle of the building is 49 ft. 2 in. between centers of crane-columns, and has a clear height of 40 ft. The remainder of the width is taken up by two side aisles, 18 ft. high. The laboratory consists of four sections: (1) A general testing-section, containing the testing-machinery, a small machine shop, and an office; (2) a cement-testing room; (3) a room for making and storing concrete test-specimens; (4) a hydraulic section.

Feb 1, 1912

By D. J. DeLazaro, W. Rostoker, R. E. Riley, M. Hansen

At very low concentrations, carbon dissolves interstitially in molybdenum resulting in a linear expansion of lattice parameter with increase of carbon in solid solution. Geometrical consideration of the relative size of carbon atom to size of interstice approximately predicts the observed volume expansion. THE element carbon, occurring in molybdenum, either as an unavoidable impurity, or purposely added, markedly affects the mechanical properties of molybdenum. Several investigators1-" have noted the occurrence of molybdenum carbide at the grain boundaries of cast molybdenum, and Fischer and Rengstorff' have shown that this intergranular constituent can induce intergranular brittleness. The appreciable change, with temperature, of the solid solubility of carbon in molybdenum, found by Few and Manning," suggests other important effects upon mechanical properties. Finally the relative atom diameters of carbon and molybdenum (the ratio of atom diameters is 0.59) are indicative, by analogy with iron (ratio of carbon atom diameter to iron atom diameter is 0.65), of a possible interstitial solid solution. If carbon dissolves intersti-tially in molybdenum, anelastic effects and age-hardening effects, similar to those observed in other body-centered cubic metals, could be expected. However, from the work of Sykes, Van Horn, and Tucker," it might be inferred that carbon forms only a substitutional solid solution with molybdenum. These considerations made it desirable to study the effect of carbon on the lattice parameter of molybdenum in greater detail than heretofore. All heat treating was done in a high temperature furnace7 built specifically for heat treatment of molybdenum. The temperatures and times of heat treatment were determined from the a solubility limit for the Mo-C system." These heat treatments were carried out in argon which was purified with respect to N, and H.!0." Purification of the argon was accomplished by passing the argon over hot (750°C) titanium and then through a magnesium perchlorate drying tower. As many as six samples were run concurrently and quenched at different times without interrupting the furnace cycle. Both the purity of the furnace atmosphere and ability to quench samples from any temperature up to 4000 °F were of prime importance in the successful heat treatment of samples for the lattice parameter investigation. Carbon Analysis The Leco Combustion apparatus was used for carbon analysis. This apparatus is capable of an accuracy of & 0.003 pct for a 1 g sample in the range below 0.10 pct. However, it is felt the degree of accuracy is somewhat better than this limit in view of the consistency evident by cross checking a number of determinations. The Battelle Analytical Laboratory consistently reported check results to within k 0.001 pct C. X-ray Measurements The molybdenum wire specimens (20 mils) were carefully filed down to about 12 mils and then etched with nitric acid to 8 mils. Carbon analyses were made on specimens before reduction in size; however, since there was no evidence of surface carburization, it is probable that the carbon was uniformly distributed throughout the sample. The resultant specimens were strain free and small enough to minimize the error in the lattice parameter determinations due to X-ray absorption. Diffraction patterns were obtained with a Debye-Scherrer powder camera 114.59 mm in diam utilizing the Straumanis type asymmetrical film mounting. Nickel-filtered copper. Ka radiation and zirconium-filtered molybdenum Ka radiation were used. Line positions on the film were measured with a traveling microscope equipped with a vernier scale permitting measurement to 0.001 cm. The average of five readings was used to determine the position of each line. The lattice parameter for each specimen was determined from the data by the extrapolation method of Bradley and Jay, Y.e., the intercept at 90" of the straight line obtained by plotting the apparent lat-

Jan 1, 1953

By Elmars Ence, Harold Margolin

The titanium-aluminum system has been investigated in the composition region 0 to 34 pct Al in the temperature range 800" to 1450°C. The phases encountered in this region were: a,ß, TiAl3, The reactions observed are as follows: 13 ; L - 6T. A1, 0 (15 pct Al) + 6 (18 pct Al) - yTi Al (16.5 pct Al) at -1170°C andP (7 pctpct Al) + y (9.2 pet Al) - ah(9 pct Al) at - 1060°C. A eutectoid reaction: y — a +d belm 700°C is postulated. THE Ti-A1 system has been the sub.ect of a number of investigations. Several of these1-3 have indicated extensive solubility of A1 in both a and ß titanium. Ence and Margolin, as a result of work on the Ti-A1-0 system:'5 have shown that the a solubility ofalumi-num is considerably restricted, and found that a compound, Ti2A1 existed in the region formerly designated as Q a This structure was identified as hexagonal with c/a = 0.803. Pietrokowsky confirmed the existence of this phase7 and pointed out that the structure was isomorphous with Ti3Sn.8 Although the existence of Ti,A1 has been confirmed by others,9-12 there has been considerable disagreement regarding the composition and mode of formation. A detailed reinvestigation of the Ti-A1 system has been published by Sagel et al.13 The tentative diagram indicated two phases, a, and e, occurring in the former all a region. The a, phase has the same structure as Ti2A1 and was indicated as having a broad region of solubility. Epsilon, a tetragonal phase, was shown to form within the a, solubility region. AS a result of unpublished work,14 Ence and Mugy3 olin disagreed with the interpretation of Sage1 et al., although some common features existed. The present study was conducted in an attempt to clarify prevailing uncertainties. EXPERIMENTAL PROCEDURE Alloy Preparation—Alloys were prepared from iodide titanium (99.9 pct Ti with less than 0.01 pct Zr) or Bureau of Mines electrolytic titanium (BHN-73) and high purity aluminum (99.99 pct). Alloys were arc-melted in argon or helium atmosphere as 15-g buttons in the composition range up to 34 pct Al. Depending on need, alloys were made in increments varying from 0.25 to 2 pct Al. Up to five 15-g buttons of some compositions were made. Weight losses during melting did not exceed about 1 pct of the charge and chemical analysis revealed that both titanium and aluminum were evaporated. In general, nominal and analyzed compositions agreed within 0.5 pct and therefore nominal compositions were used in plotting the data. Unavoidably, some overlap of composition occurred, particularly where small increments of A1 were used. The small increments were primarily used to obtain alloys which would fall into the narrow a -, r region and this purpose was achieved. In general, the data obtained from Bureau of Mines base titanium and iodide titanium alloys were in agreement. Forging—Both as-cast and forged samples were employed. Samples were heated for hand forging by an oxygen-hydrogen torch to the region 1200" to 1300°C. A titanium anvil and cover plate were used to prevent any iron pick-up and consequent formation of a low melting point compound. Frequent reheating kept the temperature in the desired range. Under these conditions, alloys containing up to 15.5 pct could be successfully forged. To check on the depth of contamination, forged alloys were heated slightlybelow the ß transformation temperature. Metal was removed to a depth below the contaminated surface so revealed, and the subsequent results obtained from these samples agreed closely with those secured from as-cast material. Heat Treatment—Prior to heat treatment, all alloys were vacuum annealed to remove hydrogen. Samples

Jan 1, 1962

By G. P. Conard, E. H. Rennhack

The creep behavior of hot-rolled, hypoeutectic Zn-Ti alloys was investigated in the temperature range from 0.43 to 0.53 TM. Secondary flow was found to originate primarily from strain-induced gvain growth where grain boundary )nigvation served to relieve the strain energy of distortion introduced by slip, grain boundary sliding, and subgvain formation. The extent to which this recovery mechanism operated was determined by the ratio of grain width to the spacing between planar fibers of TiZn,, compound particles generated in these alloys during rolling. When this ratio was unity, creep resistance demonstrated a marked improvement. In this condition, which was fulfilled by annealing following rolling, structural stability was enhanced with decreasing grain size below the equicohesive temperature (-0.5Tm), while the reverse was true above this temperature. TITANIUM concentrations approaching the eutectic composition of 0.23 wt pctl have been shown to promote a significant increase in the creep resistance of rolled zinc,2 The alloying effect created with titanium is somewhat unique; a structure closely resembling that of a fiber-reinforced metal composite can be developed which selectively modifies creep strength in preference to other mechanical properties. In an earlier investigation,~ the present authors found that, while the fiber network, composed of individual TiZn,, compound particles, had a distinct influence on rolled texture, the crystallographic variations produced were of minor importance with respect to creep. Rather, creep resistance seemingly increased when the grain size appeared to coincide with the in-terfiber spacing. The work described here was undertaken to explore this effect in greater detail. EXPERIMENTAL PROCEDURE Three zinc-base alloys containing 0.05, 0.12, and 0.16 wt pct Ti were prepared from CP zinc and iodide titanium in the form of 4 by 2 by f in. chill-cast ingots. The melting and casting procedures for these alloys have been detailed el~ewhere.~ Individual ingots of each alloy were hot-rolled at 200°C (392°F) to total reductions of 10, 25, 50, 75, and 90 pct in from one to five passes, respectively, employing a 10-min reheat prior to each rolling pass. With grain, tensile-type creep specimens with a 1-in.-long, -in.-wide gage section were machined from the rolled strips for test purposes. Annealing studies to explore the influence of grain size on secondary creep flow were carried out at 400°C (752°F) in argon for times extending up to 60 min. The grain-size effect was evaluated in terms of average grain width and length values statistically derived from lineal intersection measurements.4 A similar method was applied in establishing the average interfiber spacing, i.e., average perpendicular distance between adjacent planar fibers. The creep characteristics of the alloys were investigated by means of constant-load and constant-stress creep tests. The former tests were conducted at 25°C (77°F) under an initial stress of 10,000 psi, while the latter were performed in the range from 25°C (77°F) to 90°C (194°F) at stress levels varying from 8000 to 22,000 psi. Total specimen strain, as determined with Budd HE-1161-B strain gages, was in excess of 0.10. Maintenance of constant stress was achieved through periodic load reductions made at 0.01 strain intervals to compensate for the attendant incremental reduction in specimen cross-sectional area. The maximum indicated error in the applied stress at these strain intervals was less than 3.0 pct. RESULTS AND DISCUSSION Constant-Load Creep. In an effort to clarify the in-terrelation between interfiber spacing and grain size with respect to the creep resistance of the Zn-Ti alloys, their separate effects on secondary creep rate were determined as a function of titanium content and rolling reduction. These results are set forth in Figs. 1 and 2, respectively. The average grain diameter plotted in Fig. 2 was resolved from average grain width and length values. No data are presented for reductions of less than 50 pct because of the inability to obtain consistent measurements on these strips. The curves of Fig. 1 indicated that, for a given titanium content, a decrease in interfiber spacing, as produced with increasing reduction, promoted a decrease in creep rate. Depending on titanium content, however, wide variations in creep rate occurred at the same interfiber spacing suggesting that interfiber spacing, by itself, has little or no influence on creep resistance. Grain size, on the other hand, decreased progressively with both increasing rolling reduction and titanium content, the effect of which led to a pronounced decrease in creep rate, particularly when the average grain diameter became smaller than 3.0 x 10"4 in., Fig. 2. The continuity of this relationship tended to support the view that grain size rather than interfiber spacing was predominant in controlling secondary creep. Annealing Effect. The observed dependence of creep flow on grain size suggested that a further contribution to creep resistance would result when the alloys were annealed to effect a coincidence between grain width and interfiber spacing, see Fig. 3(b). ~eiides creating an immediate barrier to grain boundary movement, annealing offered the possibility of providing increased structural stability by eliminating many high-energy, mobile grain boundaries.= To test this hypothesis, specimens from the Zn-0.16 Ti strips reduced 75 and

Jan 1, 1967

By S. S. Shen, M. J. Pool, P. J. Spencer

Heats of solution of gold and copper in dilute Au-Cu-Sn alloys have been determined using a liquid metal solution calorimeter. The self-interaction coefficient, Au - has been calculated at constant copper concentrations and n cu has likewise been determined at constant gold contents. Good experimental agreement is obtained between the interaction coefficients and nAu Cc thus demonsbating the reliability of the measured heat values. The measured data are compared with the Predictions of certain solution models. In previous publications,1,2 the results of calori-metric investigations of dilute Ag-Au-Sn and Ag-Cu-Sn alloys have been presented. The present work on the Au-Cu-Sn system concludes a program of studies of enthalpy interaction coefficients in dilute alloys of the Group IB metals with tin. Since the definition and derivation of an enthalpy interaction coefficient has been discussed previously,1,2 no restatement of this theory will be presented here. From the determination of the partial heat of solution of gold and copper in ternary alloys of various copper and gold contents, values of the interaction coefficients can be calculated. These coefficients give an insight into the various solute interactions that occur in the liquid solutions since changes in their magnitude and sign reflect bonding changes that are taking place in alloys of varying solute contents. EXPERIMENTAL Details of the design and operation of the liquid metal solution calorimeter used in this work may be found in a paper by Poo1.3 For the present studies copper of 99.999 pct purity was supplied by American Smelting and Refining Co., gold of 99.999 pct purity by A. D. Mackay, Inc., and tin of 99.99 pct purity by Baker Chemical Co. At the commencement of each series of experimental drops, a tin solvent bath consisting of between 70 and 90 g of the pure metal was inserted in the calorimeter. The weight of the bath was accurately determined and to it were added appropriate amounts of gold or copper to give alloys of the desired composition. For determinations of approximately 0.0015 g-atom samples of Cu were used and for measurements of ?HAu approximately 0.0025 g-atom additions of Au. The heat capacity of the bath was determined at regular intervals during a series of drops using tin calibration samples. Measurements were made of the heat of solution of copper in alloys containing a constant 0.01, 0.02, 0.03, and 0.04 mole fraction of Au, respectively, in order to determine ?HCu in each alloy, and the same mole fractions of copper were used to determine equivalent values for nAu at constant copper concentrations. The composition of the bath was maintained at the desired constant gold or copper content by making calculated additions of the appropriate solute throughout the experiments. The limiting values ?HAu in alloys of constant copper content and of %c, in alloys of constant gold content were studied as a function of the mole fraction of copper or gold respectively in order to determine and nCu. Heat content and heat capacity data used in calculating values of ?ºHAu and ?HCu at the experimental temperature of 720°K were obtained from Hultgren et a1.4 ' RESULTS AND DISCUSSION Determinations of ?HAu. The partial heat of solution of gold in pure tin as a function of gold concentration was determined in the previous study of dilute Ag-Au-Sn alloys1 and can be represented by the least-squares expression: ?HAu(l) =-8075 + 2413xAu [l] which is valid between XAu= 0.00 and xAu = 0.05. The standard error in the constant term, which represents the partial heat of solution of gold at infinite dilution in tin,?HºAu(l)is 35 cal per g-atom, while the standard deviation of the slope, which represents n Au is ± 619 cal per- agtom. Corresponding expressions for ?HAu(l) in alloys containing constant mole fractions of 0.01, 0.02, 0.03, and 0.04 copper were obtained from the data listed in Table I and are themselves given in Table II. Fig. 1 illustrates the partial heat of solution of gold as a function of its concentration in each of the alloys. For the four alloys of constant copper concentration, the values obtained for ?HºAU(l) (in order of increasing copper content) are -8141 i 36 cal per g-atom, -8210 ± 42 cal per g-atom, -8202 ± 46 cal per g-atom and -8268 ± 51 cal per g-atom. The corresponding values of the self-interaction coefficient, n Au, for these alloys are 3103 * 644 cal per g-atom, 2425 ± 676 cal per g-atom, 2574 * 717 cal per g-atom and 2523 ± 899 cal per g-atom. In Fig. 2 these values of n Au are plotted as a function of the copper content of the alloys and are seen to remain approximately constant within the experimental limits. The addition of increasing, small amounts of copper to dilute binary Au-Sn alloys thus has no apparent effect on Au-Au interactions in these dilute liquid solutions, although more exothermic values of ?HºAu(l) do result from an increase in the copper content of the alloys. Analogous behavior was observed with additions of silver to dilute Au-Sn alloys.' By

Jan 1, 1970

By G. R. Leverant, M. Gell

The high- and low-cycle fatigue poperties of MAR-M200 directionally -solidified into columnar-grained and single crystal forms were determined at 1400" and 1700°F. These results were compared with the corresponding properties of conventionally -cast MAR-M200. The low-cycle fatigue lives of the columnar-grained and single crystal materials were similar at both temperatures and were one to two orders of magnitude greater than those of conventionally-cast material. The variations in the fatigue lives among the three forms of MAR-M200 were related to the more rapid rate of intergranular muck propagation compared to that of transgranular propagation. In conventionally-cast MAR-M200, cracks were initiated in grain boundaries and crack popagation occurred rapidly along an almost continuous grain boundary path. In the columnar-grained material, crack initiation occurred on short transverse segments of grain boundaries, but crack propagation was transgranular. The fatigue lives of columnar-grained and single crystal materials were approximately the same because most of the life in both materials was spent in trans-granular propagation. For the directionally -solidified materials, the number of cycles to failure, Nf, can be related to the total strain range, , by: heT = K where n and K are 0.16 and 0.044 at 1400'F and 0.29and 0.098 at 1700, respectively. In addition to intergranular crack initiation in the columnar-grained material, initiation also occurred at we-cracked MC carbides and micropores in both directionally-solidified materials. At 1400°F, fatigue life was reduced with increasing MC carbide size, but at 1700 there was no effect of carbide size. THE creep and stress-rupture properties of conventionally-cast nickel-base superalloys can be greatly improved by directional solidification into either single crystal or columnar-grained forms. The improvement in properties results from a reduction in intergranular cavitation and crack growth in the columnar-grained materials and the complete absence of this fracture mode in the single crystals. This paper describes the effect of grain boundaries on the elevated temperature fatigue properties of the nickel-base superalloy MAR-M200. The effect of cycling frequency on cracking arid fatigue life and the role of MC carbides and micropores on crack initiation are also emphasized. The fatigue properties of columnar-grained and single crystal MAR-M200 at room tem- perature,4,5 and the change in the mode of fatigue crack propagation with temperature6 have recently been described. I) EXPERIMENTAL PROCEDURE The material used in this study was the nickel-base superalloy MAR-M200, directionally-solidified into columnar-grained and single crystal forms. The columnar grains were approximately 0.5 mm in diam. The nominal composition of these materials in wt pct was 0.15C, 9Cr, 12.5W, loco, 5A1. 2Ti, lCb, 0.05Zr. 0.015B, bal Ni. They were solutionized for 1 to 4 hr at 2250°F followed by aging at 1600°F for 32 hr. which resulted in 0.2 pct offset yield stresses of 150,000? 144,000, and 95,000 psi at room temperature? 1400°, and 1700°F, respectively. The corresponding elastic moduli parallel to the testing direction were 19.2. 15.0, and 12.5 x 106 psi, respectively. Specimen design, testing procedures and alloy mi-crostructure have been described previously and will only be summarized here. Following the 1600°F aging treatment. MAR-M200 contains an ordered, cuboidal, y' precipitate 0.3 1 on edge, which is coherent with the 1 matrix. The y' precipitate is quite stable; even after testing at 1700°F. the precipitate is only slightly enlarged and its corners somewhat rounded. The alloy also contains a small volume fraction of micropores, and MC carbides. some of which contain preexisting cracks5 formed during casting. These cracks are always parallel to the long dimension of the carbide. Measurement of MC carbide size has been described previously.5 Axial fatigue tests were conducted in air over a wide range of strain amplitudes in both the high - and low-cycle fatigue regions, with specimen lives varying from about 10' to 10' cycles. Low-cycle fatigue (LCF) tests were strain-controlled with strain varied between zero and a maximum tensile value at a frequency of about 2 cpm. High-cycle fatigue (HCF) tests were stress-controlled with the stress varied between 5000 psi and a maximum tensile value less than the yield stress at a frequency of either 10 cps or 0.033 cps (2 cpm). The temperature in the gage section was controlled to 52°F. Specimen axes were within 5 deg of the [001] growth axis of the single crystals and the common [001 ] growth axis of the columnar-grained material. Specimen gage sections were electro polished prior to testing. After the standard heat treatment, three specimens were coated with a typical aluminide coating applied as a slurry. An additional specimen was given the coating heat treatment without actually being coated. In all cases: specimens were reaged at 1600°F for 32 hr after receiving the coating heat treatment at 1975'F for 4 hr.

Jan 1, 1970

By Charles Will Wright

I. INTRODUCTION. THE application of the camera as an adjunct to topographic mapping began practically with its invention, and it has been employed with varying success since that time. With the exception of the camera to be described, the plate-camera has been universally used in this work, thus giving a projection of the area photographed on a flat surface. From such projections or photographs, by the rules of geometry and of perspective, points defining topographic features and seen from at least two camera-stations may be projected upon a ground-plane-the map.1 In 1904 I employed the plate-camera for this purpose in Alaska, but found that the labor necessary to plot the maps, even in a general way, was long and tedious. In 1905 a small Eastman panoramic camera was fitted with spirit-levels, a sightalidade and a transparent scale, introduced inside the camera to register the degree-points in the sky-line of the film-negative; also, arrows to indicate the horizon-line. This was, on the whole, successful; but the details in the topography were not brought out in the views with sufficient clearness, and the photographs were too small. These difficulties were overcome by obtaining a larger and more carefully constructed instrument, which was satisfactorily employed in the field during the year 1906. A panoramic view is made up of an integral number of perspective views upon flat surfaces, and logically is the most ac-

Jan 1, 1908

By Elliot P. Rexford

B. C. Burgess-—Prior to hearing this paper presented at the San Francisco meeting, I travelled by car from Yuma, Ariz., across south-central California and up through the San Joaquin Valley. After hearing the paper I returned by the coast route to San Diego then along the Mexican border to Yuma. The striking feature of these trips, related to this paper, was the dry river and creek beds at a time of year not the dry season. Contrasted with this was the wasteful use of water in irrigation canals and laterals. Poland says "at least 90 pct of the ground water pumped is used for irrigation." That being the case, it would appear that first consideration should be given to conservation of this use. Probably a small part of this is actually reaching the plants. Some measure of this loss between pump and crops would be revealing. Methods that might be employed to reduce this loss are pipe lines and spraying of some crops such as the banana planters are using in Central America. Another idea which might be investigated is to line canals and ditches with some water-repelling mineral like pyro-phyllite. Perhaps a comparatively thin sprayed-on

Jan 1, 1951

By Elliot P. Rexford

B. C. Burgess-—Prior to hearing this paper presented at the San Francisco meeting, I travelled by car from Yuma, Ariz., across south-central California and up through the San Joaquin Valley. After hearing the paper I returned by the coast route to San Diego then along the Mexican border to Yuma. The striking feature of these trips, related to this paper, was the dry river and creek beds at a time of year not the dry season. Contrasted with this was the wasteful use of water in irrigation canals and laterals. Poland says "at least 90 pct of the ground water pumped is used for irrigation." That being the case, it would appear that first consideration should be given to conservation of this use. Probably a small part of this is actually reaching the plants. Some measure of this loss between pump and crops would be revealing. Methods that might be employed to reduce this loss are pipe lines and spraying of some crops such as the banana planters are using in Central America. Another idea which might be investigated is to line canals and ditches with some water-repelling mineral like pyro-phyllite. Perhaps a comparatively thin sprayed-on

Jan 1, 1951

By Richard N. Hunt

Bingham has produced 6 per cent. of this country's copper. In total production, it ranks fourth among the copper camps of North America, the order being Butte, Michigan, Bisbee, and Bingham. In its annual production, it held that same rank until 1919, when its production was exceeded by the combined production of the Globe-Miami district of Arizona. Bingham has also been a lead camp of the first order. Utah ranks third among the lead-producing states, and its production comes largely from three camps which, in the order of their productivity, are: Bingham, Tintic, Park City. Bingham's silver production is important, but it does not rank high as a silver producer. Utah owes its rank as first among the silver-producing states to Tintic, a camp 40 miles due south of Bingham. The United States Mineral Resources reports a total production from Bingham for the period 1865-1920 having a gross value of $528,043,432. History of the Bingham District Bingham is on the eastern flank of the Oquirrh range 30 miles southwest of Salt Lake City, from which it can be reached in an hour by auto, or by the Denver & Rio Grande or the Bingham & Garfield railroads. The automobile route is a paved road across the floor of Great Salt Lake Valley, through farming country. The Bingham & Garfield railway leaves the level of Great Salt Lake at the northern end of the Oquirrh range, and in 20 miles it climbs 2100 ft., and deposits the traveler upon a shelf cut in the side of Bingham Canyon below most of the mines, which are farther up Bingham Canyon and its tributary Carr Fork. Below lies the town, a narrow ribbon running for a couple of miles along the bottom of a canyon 2000 ft. deep—an almost impossible site for a community numbering, in prosperous times, 5000 to 7000 inhabitants drawn from all quarters of the globe. Up the canyon and down, and beneath the steep slopes nearby, and beneath the town itself, are the mining operations of over half a century. During the past two decades one mine, the Utah Copper, has become so gigantic an operation as to dominate all other activity in the camp. It has become the greatest copper mine on the continent in production,

Jan 1, 1924

By D. M. Blacknall, N. N. Winogradoff, E. W. Williams

Low-temperature measurements of photolumines-cence were used to evaluate the progvess in materials development. Variation of the impurity type, impurity concentration, and method of growth were used to clarify the chemical origin of defects in GaAs. Melt-g~ozun, epitaxial vapor-, and solution-grown samples were studied. A comparison of measurements at 77" and 20°K shows that more defects can be observed at the lower temperature. Th'vee residual defects were identified in relatively pure GaAs. These were: silicon, copper, and a gallium vacancy-donor complex. Solution growth from a gallium solution inhibits the formation of the latter two. Eleven defects were studied and the "optical" activation energy of some of these, namely, silicon, cobalt, and chromium, has not been reported in the literature before. THE discovery of the injection laser in 1962 prompted extensive measurements of the photoluminescence of GaAs. The measurements were made at 77°K on GaAs doped with shallow impurities at various doping levels and compared with electroluminescence1'2 and absorp- tion data.374 In addition, lower-temperature studies were made on relatively pure GaAS' and on GaAs doped with oxygen,5'" manganese,' and copper.' The observation of defects* in GaAs with photolu- *The word "defects" ~efers to both chemical impurities and native defects. minescence at low temperatures makes photolu mines-cence an invaluable tool in evaluating the progress in materials development. The only previous evaluation was done at 77°K when solution-grown and melt-grown GaAs were compared.O No identification of defects was made but it was shown that some of the deep-level luminescence seen in melt-grown GaAs was absent in solution-grown GaAs. The present work extends the comparison of preparation techniques to lower temperatures and to a study of epitaxial vapor-grown GaAs. It is particularly valuable for thin epitaxial layers since they cannot be analyzed by conventional analytical techniques. In addition, by varying the impurity type and impurity concentration the chemical origin and nature of defects in GaAs was demonstrated. Eleven defects were studied in all. Three of the defects were identified as residual defects which often contaminate GaAs prepared from the melt and the vapor. Only one such defect was observed in GaAs grown from a gallium solution and this was identified as silicon.

Jan 1, 1968