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By David L. Holt, Walter A. Backofen, Anwar-ul Karirn

ANNEALING the binary alloy, Mg-0.5 wt pct Zr in a hydrogen atmosphere results in extensive precipitation of zirconium hydride. The morphology of these precipitates has already been investigated.lm3 Squires, Weiner, and phillips4 found, following creep testing of the hydrided alloy at 450" and 500°C, that hydride denuded zones formed along grain boundaries that were aligned approximately normal to the tensile axis. Zone formation was attributed to diffusional creep by magnesium transport down the prevailing stress gradients.4'5 Recently, electron microprobe analysis by Karim, Holt, and Backofen6 showed the zones indeed to be zirconium-free and furthermore it was shown that in compression, zones formed along boundaries approximately parallel to the stress axis. Thus it was confirmed that the zones are formed by diffusional creep. Typical zone-formation is shown in Fig. 1. Karim, Holt, and Backofen also measured the con- tribution to the total strain, from diffusional flow, slip creep, and grain boundary shear: results showed that diffusional strain tends to saturate with increasing imposed strain, while grain boundary shear eventually becomes the dominant deformation mode. It was suggested in explanation that the precipitate-denuded zones are soft and easily sheared, such deformation contributing to the grain boundary shear measurement. A point to be emphasized is that the Mg-0.5 Zr alloy was not superplastic for the index of strain rate sensitivity of flow stress, m = a log log 6 was only 0.25. It was recognized that diffusional creep in a poly crystalline aggregate must be accompanied by boundary shearing.' The suggestion was that the non Newtonian-viscous character of diffusional creep in the Mg-0.5 wt pct Zr alloy is due to resistance to sliding of boundaries lying approximately parallel to the tensile axis.= The work described in the present note should be seen against the above background for it represents initial efforts to observe in a similar way diffusional creep in a superplastic alloy. Previous work with the ternary-alloy Mg-6 Zn-0.5 Zr, pellet extruded, showed it to be superplastic however it does not contain resolvable precipitates to act as internal markers for diffusional creep. Also the fine grain size of the alloy (0.5 p) made conventional metallography rather difficult. Solubility relationships in the Mg-Zn-Zr system are not well known, however making reasonable guesses about the probable phase diagram of the ternary, Mg-Zn-Zr, various heat treatments were attempted to produce hydride precipitation. Finally a 16-hr anneal at 495' in hydrogen was found to pro-

Jan 1, 1970

By George Comstock

Results are given of scleroscope and Brinell tests on specimens of cast 10-per cent. aluminum bronze, quenched and reheated at various low temperatures. The scleroscope was not found as reliable as the Brinell machine for measuring the hardness, for the size of the piece tested seemed to affect the scleroscope results. The maximum hardness was obtained by quenching and reheating to between 315° and 370° C. Softening was produced by reheating above 370° or 400° C. A series of polished and etched microsections showed a more reddish color in those that had been reheated above 400° C., and a change in microstructure above 500° C. IT HAS been known for many years that the alloy containing 90 per cent. copper and 10 per cent. aluminum can be hardened, like steel, by quenching from a suitable temperature, and that the hardened alloy can be softened again by annealing or drawing the temper. It does not seem to be generally appreciated, however, that the effect of the first slight reheating after quenching is actually increased hardness, the softening effect not taking place until a certain temperature of "drawing" has been exceeded. This paper gives the results of a few experiments on various specimens of cast 10-per cent. aluminum bronze, quenched for maximum hardness, and subsequently annealed at different temperatures. The hardness measurements were made with both a scleroscope and a standard Swedish Brinell machine; some peculiarities of the scleroscope test on this material are described. The author is not aware of many previous investigations of the hardness of this alloy when quenched and drawn, but two important papers on the subject should be mentioned. The earliest was by Portevin and Arnou,1 in which it was stated that tempering quenched 10-per cent. aluminum bronze at 400° C. increased the hardness as compared with the quenched untempered alloy and that reheating above that temperature was necessary to obtain any softening effect.

Jan 7, 1924

By J. L. Weeks

THERMAL conductivities of several samples of uranium and uranium alloys were determined using an apparatus previously described.' The value previously reported for uranium,' 0.035 cal per sec per cm per "C at 70°C, is in error due to the failure of a thermocouple during the determination on uranium. The defective thermocouple was detected after a reanalysis of the data obtained during the run and since has been replaced. Subsequently, runs on several samples of uranium show the thermal conductivity of uranium to be 0.069 cal per sec per cm per 'C at 70°C. The accuracy of the determinations was checked by measuring a sample of synthetic sapphire whose thermal conductivity was previously reported and found to be in agreement with other values."-" The values given in Table I are believed correct to % 3 pct or 0.003 cal per sec per cm per "C, whichever is larger. The samples were provided by J. H. Kittel of the Argonne National Laboratory, Metallurgy Div. References J. L. Weeks and R. L. Seifert: Apparatus for the Measurement of the Thermal Conductivity of Solids. Review of Scientific Instruments (1953) 24, pp. 1054-1057. J. L. Weeks and R. L. Seifert: Note Regarding the Thermal Conductivity of Synthetic Sapphire. Journal American Ceramic Society (1952) 35, p. 15. :' J. Francl and W. D. Kingery: Thermal Conductivity: IV, Apparatus for Determining Thermal Conductivity by a Comparative Method; Data for Pb, Al2O3, BeO, and MgO. Journal American Ceramic Society (1954) 37, No. 2, Part 11, pp. 80-84. (Part 11: special issue on thermal conductivity.) ' W. D. Kingery, J. Francl, R. L. Coble. and T. Vasilos: Thermal Conductivity: X, Data for Several Pure Oxide Materials Corrected to Zero Porosity. Journal American Ceramic Society (1954) 37, No. 2, Part II, pp. 107-110. (Part 11: special issue on thermal conductivity.) Edwin Ruh: New Jersey Ceramic Research Station, Rutgers University. Private communication.

Jan 1, 1956

By J. R. Guard

Development of electrical power in coal mining has been an outstanding example of adaptbility. It has accommodated itself to new inventions, changing mining methods, increasing demands, increasing safety requirements and many other new conditions. With the appearance of the continuous miner in the mining machinery picture, those engineers interested in the application of electricity to mining have been thinking about what new comination of electrical apparatus will best suit this newcomer. It is the purpose of this paper to discuss the relative costs of supplying d-c versus a-c power to mining equipment with particular reference to continuous miner setups. Assume that a-c power will be delivered to the mine at some high voltage suitable for transmision to the various substation locations. Typical voltage for this purpose is 4000 volts. The problem then is to change the power to some kind of power suitable for driving the motors of mining equipment. For safety and other reasons the voltage to be delivered to the motor terminals must be under 600 volts.

Jan 6, 1950

By S. Jana, C. M. Wayman

The reverse transformation of bcc martensite to the fcc phase was studied in an Fe-33.95 wl pct Ni alloy by nzeans oj dilatometry, melallography, and electron microscopy. Upon "slozc" heating (-1°C per min) length cJmnge us temperature plots showed u gradual contracLion over the temperature range 200" to 280"C ,followed by a more abrupt contraction beginning a1 -280°C. Howet,ev, zchen the heating rate was increased -4°C per tnin, no gradual contraction was observed and only the abrupt contraction starting at -2BO"C was found. Thus on slower heating- the AS "temperature" for the subject alloy, unlike the MS temperature, is better defined as a range of temperatures. Both optical and transmissiorl electron microscope observations showed that some of the martensite plates exizibited a partial loss of transformation twins during reversal. The midvib region of the martensite plates disappeaved relatively early duirng the reversal. Metallographic observations slowed that the earliest detectable stage of the rezlerse tvansforrvration begins (axd Moues inulardly) at The Martensens i te - parent interface. At higher temperatirres, the. formation of martensitically reversed jcc plates within the bcc martensite plales was observed. It is concluded that the reverse transformation consists of a diffusion less process (martensitic); but this is ps-obably aided by a prior or simultaneous dijjusiorz-comltvolled process, at leasl in the case of slower heat-ing' experiments. ALTHOUGH numerous investigations have dealt with the parent-to-martensite ("forward") transformation (fcc — bcc) in Fe-Ni alloys, comparatively little is reported on the ("reverse7') martensite-to-parent transformation.'-4 Even though such reverse transformations have been studied in detail in some nonferrous systems, one of the difficulties of studying the reverse transformation in most ferrous mar-tensites is that the martensite decomposes by tempering during heating. However, carbonless Fe-Ni alloys do not exhibit this difficulty since the transformation in these alloys is completely reversible. The present investigation represents an attempt to shed more light on the nature and mechanism of the martensite-to-parent transformation. 1) EXPERIMENTAL PROCEDURE 1.1) Alloy Prepatation. Fe-Ni alloys of compositions near 34 wt pct Ni were prepared from zone-refined iron (99.994 wt pct Fe) and high-purity nickel (99.999 wt pct Ni) by induction melting in recrystallized alumina crucibles in an argon atmosphere, with prior vacuum evacuation to 10"3 mm Hg. The alloys were homogenized by induction stirring in the molten state for 5 min. After solidification, the alloys were further homogenized in evacuated quartz capsules for 96 hr at 1230°C. 1.2) Dilatometry. Slices of the ingot were hot-forged (750°C in air) into approximate rod form and these specimens were then hot-swaged (750°C in air) into long cylindrical rods 0.55 mm diam. From the rods, specimens about 1 in. long were cut. These were then vacuum-annealed for 24 hr at 1200°C, cooled to room temperature, and subsequently transformed to martensite in liquid nitrogen (whereby about 40 pct transformation was obtained). Dilatation measurements were made by observing length changes in a vacuum dilatometer with an externally mounted LVDT sensing element. 1. 3) Preparation of Electron Microscope Specimens. Slices of the ingots were cold-rolled (with intermediate vacuum anneals) to -0.020 in. Out of these rolled sheets, specimens (about 1 by 1 in.) were cut. These were then vacuum-annealed, transformed to martensite by cooling in liquid nitrogen, and subsequently heated from room temperature to various temperatures to effect either partial or complete reverse transformation. These specimens were then chemically polished to 0.002 in. in l:l HsOz (30 pct) and &PO4 (85 pct) solution, and thinned to electron transparency in an electrolyte consisting of 150 g CraOs, 750 ml glacial acetic acid, and 30 ml ~~0.~ Observations were made with a 100-kv Hitachi HU-11 electron microscope equipped with an HK-2A tilting device. 1.4) Optical Microscopy. Metallographic observations were made with a Leitz MM5 metallograph on the same 0.020-in. sheet specimens as were used for electron microscopy and on bulk specimens which were 0.2 in. or more on a side. The chemical thinning solution when cooled below 20°C also served as an etchant for this alloy. Observations of surface relief were made with a Zeiss interference microscope employing a Thallium light source of wavelength 0.54 p. Specimens for interference studies were prepared by two-stage polishing on Buehler vibromet polishers using 0.3 and 0.05 p alumina abrasives. 2) EXPERIMENTAL RESULTS 2.1) Comparison of the MS,AS, and Af Tempera-tures wTth Previous Re sults. The AS aLd Af tempera -tures of several Fe-Ni alloys were determined dila-tometrically. The MS temperatures of the same alloys were determined by continuously lowering the temperature using a mixture of isopentane and liquid nitrogen and observing the highest temperature at which a prepolished specimen showed surface upheavals. For the present the As temperature is defined as the temperature at which an abrupt decrease in length occurs in the dilatation plot. The Ms,As7 and A determinations in the present investigation and those of Kaufman

Jan 1, 1968

By P. R. Kalischer

IN the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more components that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. Since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measurements and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. NATURE AND REMOVAL OF SURFACE BARRIERS The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 per cent Fe, 50 per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However, this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By Derek J. Fray, John Chipman

THE solubility of graphite in y-iron has been determined by several workers'12 with reasonable agreement. With the increasing use of more complex steels, it is necessary to understand more fully the thermodynamics of the austenite phase. The activity of carbon in a number of alloys is known but the maximum solu- bility of graphite has only been measured by Sohnchen and piwowarsky3 for Fe-Ni and Fe-Si alloys. Recently, Chipman and Brush reviewed the published data on the activity of carbon in binary and ternary austenite and also obtained expressions for calculating the solubility of graphite in Fe-Ni, Fe-Co, and Fe-Si alloys. On comparing the theoretically derived solubilities with the limited results of Sahnchen and Piwowarsky, it was found that the agreement for Fe-C-Si was excellent but there was considerable discrepancy for Fe-C-Ni and no data for Fe-C-Co. It was therefore decided to measure the solubility of graphite in a series of Fe-Ni and Fe-Co alloys. The alloy samples were made up by induction melting a high-purity master alloy under an inert atmosphere in an alumina crucible and drawing the molten metal into four-bore alumina tubes. Using this technique, it was possible to form alloy rods approximately 2 in. long and 1/18 in. in diam. Sixteen lengths of fine rod could be made without solidifying the master alloy. These were then allowed to cool under the inert atmosphere before being sectioned. The samples were packed in a graphite crucible with spectroscopic graphite powder, together with a piece of pure iron foil. Dry hydrogen, which had been saturated with isopropyl alcohol at room temperature, was passed over the crucible at 1000°C for 72 hr. At the end of the 72 hr argon displaced hydrogen in the reaction tube and the crucible was quickly pushed to the water-cooled end. The samples were thoroughly cleaned of the adhering graphite and analyzed. The pure iron samples always contained 1.5 0.02 pct C, which compares favorably with the data of smith2 and

Jan 1, 1970

Mining Methods GERALD F. SHERMAN, Chairman JOHN A. CHURCH, Vice-chaiman CHARLES W. WRIGHT, Secretary Alluvial Mining CLINTON BERNARD CHARLES JANIN H.R. NORSWORTHY Open-cut Mining Iron MAX H. BARBER J. A. MACKILLICAN Copper MICHAEL CURLEY R.B. TEMPEST Underground Mining Iron C. H. BAXTER TENNEY C. DESOLLAR

Jan 1, 1934

By G. L. Kulcinski, R. D. Leggett

Irradiated uranium containing 635 ppm of carbon, mostly in the form of UC precipitates, was annealed at temperatures from 650" to 900°C under hydrostatic pressures of 0 to 1000 bars. Postirradiation examination revealed that the carbide particles are not stable in the r phase of irradiated material but are stable in unirradiated material annealed under identical conditions. The degree of carbide dissolution appears to be connected with the fission product concentration and independent of annealing pressure. THIS paper describes the change in appearance of carbide particles in irradiated uranium after the uranium has been postirradiation-annealed. It has been proposed by several investigators&apos;-5 that fission gas-induced swelling in irradiated uranium may be reduced by incorporating a fine dispersion of second-phase particles into the metal. Because of the low solubility of carbon in uranium6 and the apparent stability of UC precipitates at high temperatures,6-8 this system has received some attention. The stability of UC particles to low-temperature irradiation has been demonstrated many times, as well as their stability during postirradiation anneals in the high a or B phases.9 Unirradiated uranium containing UC particles has been annealed high in the r phase, and the solubility of carbon was found to be only -115 ppm at 1050ºC.6 Vacuum annealing of irradiated uranium to the same temperature produces a spongelike sample, due to the formation and growth of fission gas bubbles."14 This highly disrupted lattice has made any determination of the stability of UC at these temperatures impossible. Nevertheless, it has always been tacitly assumed that the UC particles were still present. Recently, postirradiation, high pressure-high temperature tests have been performed on irradiated uranium containing a secondary phase of UC. 14 Examination of these samples after 100-hr, 900°C tests revealed that the carbides are not stable, and the results of these tests are presented here. 1) EXPERIMENTAL PROCEDURE The samples, high-pressure equipment, and subsequent analytical techniques are the same as those described elsewhere.14,15 Briefly, cylindrical samples of commercial-purity uranium that had been irradiated at <350°C to 0.37 at. pct B.U. were subjected to 90O°C, 100-hr anneals in NaK at pressures ranging

Jan 1, 1970

By E. Rudy, St. Windisch

The only complete phase diagram investigation of the Ti-W system is by Maykuth and coworkers,&apos; Fig. 1. Although previous work by Gonser2 indicated complete miscibility, later investigations3°5 essentially confirmed the diagram depicted in Fig. 1. The present study was undertaken because preliminary results on metal-rich ternary Ti-W-C alloys indicated complete solid solubility between 0 titanium and tungsten at temperatures above 1300°C—in contradiction to the presently accepted diagram. The powdered elements, as well as crystal bar titanium and tungsten sheet, were used in the preparation of the experimental alloys. The iodide titanium, obtained from Foote Mineral Co., Exton, Pa., had a total impurity content of less than 410 ppm, of which 150 ppm were interstitials (H, O, N, C). The overall purity of the titanium powder (Var-Lac-Oid Chemical Co., New York) was better than 99.7 pct. Major contaminants, in ppm, included: 0, 800; N, 10; H, 1500; Fe + Co + Ni + Cu + Zn, 50; C1, 200. The measured lattice parameters of the titanium were a = 2.94A and c = 4.68,A. The tungsten sheet and the tungsten powder (Wah Chang Corp., Albany, Ore.) contained the following impurities (in ppm, values in parentheses refer to the sheet tungsten): Mo, 50 (70); 0, 140 (110); Fe, 20 (60); Ni, 20 (not determined); N, 110 (not determined); sum of other impurities, <60 (<100). Samples from the iodide titanium bar stock and from tungsten sheet were prepared by repeated melting of the chipped materials in a nonconsumable electrode arc furnace under high-purity helium. The melted alloys were heavily cored, and homogeneity of the alloys could only be achieved after prolonged heat treatments at subsolidus temperatures. The majority of the alloys were therefore prepared by cold compacting the well-mixed powders in steel dies and pre-homogenizing the compacts for 6 hr at 1300°C in a tungsten-element furnace. The vacuum was better than 10"6 Torr, but for additional protection the sample container was wrapped in zirconium foil. Both preparation methods led to identical results. The measurements of the solidus temperatures were carried oat in the Pirani-type furnace described in a previous paper.6 Incipient melting in alloys containing between 20 and 90 at. pct W was rather difficult to detect visually, and therefore a photoelectric transducer system7 was employed to indicate the phase change. For the investigation of the solid-state equilibria, the specimens were first homogenized for 2 hr at slightly subsolidus temperatures in the Pirani fur- nace and then reequilibrated at, and rapidly cooled (-100°C per sec) from, the selected equilibrium temperatures. After the runs, the alloys were analyzed microscopically and by X-ray diffraction. With the exception of spot checks for oxygen and nitrogen in processed alloys, no other chemical analyses were performed. However, as the weight changes of the alloys during processing were within 0.05 pct and the lattice parameters of indeqendently prepared alloy series agreed within 0.0015A, it is reasonable to assume that no significant concentration shifts with respect to the nominal compositions had occurred. The measured solidus temperatures, shown together with literature data in Fig. 2, ascend smoothly from

Jan 1, 1969

By P. R. Kalischer

In the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more cornponents that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measuremerits and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. Nature and Removal of Surface Barriers The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 Per cent Fe, So Per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However. this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By P. R. Kalischer

In the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more cornponents that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measuremerits and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. Nature and Removal of Surface Barriers The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 Per cent Fe, So Per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However. this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By Heribert Wiedemeier, Ali Khan

The tetnperature-conposition phase diagram of the syste,n MnS-CdS has been investigated over a range fro)n 600° to 1000° C. The small degree of solid solution on the MnS rich slde cornpared to the large CdS rich single-plzase region could be esplained by the difference in strzrctures of the cotnponents and the relative sizes of the metal ions. The change in lattice parameter as a function of cot)zposition is linear atzd jollous Vegavd&apos;s rule within experittzental limits of error. Mns and CdS have gained considerable attention in recent years because of their interesting solid state properties. In order to investigate such properties and thermodynamic quantities of mixed compositions of transition metal chalcogenides, it is necessary to establish their phase diagrams. Two earlier publications are concerned with the MnS-CdS system. Schnaase&apos; found complete miscibility when MnS and CdS were co-precipitated in aqueous solutions at room temperature. However, there is evidence that the mixed crystals were not stable over the entire range of composition. roger&apos;s&apos; investigation of the ternary system ZnS-CdS-MnS at 900" C indicates a solution of 48 mole pct MnS in CdS. During the course of this work which covers a temperature range from 600" to 100O° C, emphasis has been placed on the use of high-purity materials and well-defined modifications of starting products. EXPERIMENTAL Starting Materials. The stable green modification of MnS with NaCl structure was prepared by direct fusion of the elements and by chemical transport reaction. Stoichiometric amounts of manganese of 99.99+ pct purity and of sulfur of 99.999 pct purity from Gallard-Schlesinger Corp. were sealed in an evacuated quartz tube at a pressure of 10"5 mm Hg and annealed for 48 to 60 hr at 800°C. The quartz tubes used throughout this work were outgassed under high vacuum at a temperature of 90OU to 1000° C for 12 to 18 hr. For the synthesis of MnS by chemical transport3 stoichiometric ratios of elemental manganese and sulfur and small amounts of iodine were sealed under vacuum in a quartz tube, which was placed in the temperature gradient, 900/800-C, of a two zone furnace. Single crystals of MnS in form of platelets and octahedra were deposited at the cooler end of the tube. The manganese content was determined by EDTA titratin. A typical result of several analyses was 63.05 pct Mn which agreed well with the computed value, 63.14 pct. Commercially available CdS of 99.9+ pct purity, a mixture of the cubic and hexagonal forms, was converted into the hexagonal high-temperature modification by annealing CdS under vacuum in quartz tubes at 700° C for about 36 hr. As a second method, cadmium sulfide was transported in a temperature gradient, 70O° /650" C, with in vacuo sublimed iodine from the hot to the cooler zone of the tube. Large sized crystals in form of hexagonal columns and some platelets were obtained. An average result of the cadmium analysis by EDTA titration4 was 77.93 pct in good agreement with the computed value, 77.81 pct. Only the NaCl modification of MnS and the wurtzite modification of CdS were used for the solid solutions. Preparation of Solid Solutions. Finely powdered MnS and CdS samples were thoroughly mixed in molar ratios and compressed into pellets of about 6 mm diam and 2 mm in height at a pressure of approximately 13,500 atm.

Jan 1, 1969

By E. H. Jr. Dix

OF all the alloying elements used in commercial aluminum alloys, copper stands out as by far the most important, and it is perhaps for this reason that the constitution of the aluminum-copper system has received the attention of a number of experimenters covering a period of approximately 20 years. It would be expected that during this time the equilibrium relations had been thoroughly and exactly worked out. In a general way this is true, but there is a surprising lack of agreement in the details of the high aluminum end of the diagram, particularly in regard to the solid solubility of copper in aluminum, which has been given variously as 2 per cent. to 5 per cent. at the eutectic temperature. The importance of this is much greater than might at first appear to one unfamiliar with modern commercial aluminum alloys. This is true because, with one exception, the susceptibility of the strong alloys to heat treatment depends, in part at least, upon the solid solubility relations of copper in aluminum. In 1919, Merica, Waltenberg, and Freeman1 published the first detailed information on these solubility relations. They found that the solubility of copper decreases with falling temperature from about 4 per cent. at 5.25° C. to about 1 per cent. at 300° C. and is apparently still diminishing at lower temperatures. In 1921 there was published a brief account of the results obtained in the National Physical Laboratory, Teddington, England.2 This laboratory, however, reported that 5 per cent. of copper is soluble in aluminum at 540° C., and that this amount decreases to about 3 per cent. at 20° C.

Jan 2, 1926

By Don M. Jackson, Robert W. Howard

Techniques for the epilaxial growth of single -crystal silicon carbide films on silicon were developed. The vapor-phase decomposition and bydrogen reduction of silicon tetrachloride (SiC14) and Propane (C3H8) resulted in clear films of silicon carbide, lip to seveval microns in thickness. The growth took place in a horizontal . silicon epilaxial reactor at 1100°C (pyrometer) at a rate of- 3000Å per minute. Electron diffraction and X-ray diffraction studies demonstrated that the films were single-cyrstal, ß -phase, or cubic silicon carbide. SiO2 film were used to mask areas of the silicon sur-lace in order that the silicon carbide might be grown in controlled geometries. Both n- and p-type films were grown on p-type silicon waters.. Heavily doped silicon films of the same conductivity type as the silicon carbide films were deposited over the silicon carbide in order to affect better probe contact to the structures. when n-type silicon carbide mesas were grown on p-type silicon substrates the de vollage-current relationships between films and substrates were that of junction diodes. These diodes showed a sensitivity to while light ill that the incident light increased forward- and reverse-satro,ation currents, P-type silicon carbide mesas grown on p-type silicon were ohmic rather than rectifying in their voltage -current relationship. No conclusions could he reached concerning heterojunc-tiou rectification in the structure. SILICON carbide is a semiconductor with many interesting properties. It decomposes at temperatures above 2200°C.1 It occurs in two general crys-tallographic forms—hexagonal (a Sic) and cubic (ß Sic)—with the cubic form having a forbidden-gap energy of 2.32 ev and the hexagonal form (specifically the 6H polytype) a gap energy of 2.86 ev.3 It behaves as an extrinsic semiconductor at temperatures approaching 5003C. It has been shown to have a high resistance to radiation damage4 and p-n junctions formed in Sic have been shown to radiate visible light under forward- or reverse-bias conditions. Epitaxial silicon carbide on silicon carbide has been successfully grown through the use of a variety of techniques, such as gaseous cracking of SiCL4 and CC4, nearly all of which require a deposition temperature above 1500°C.6 This paper will cover very recent work on the gas-phase deposition of highly ordered films of silicon carbide on high-quality silicon single-crystal substrates. The films have been shown to ex- hibit junction-rectification properties when geometrically isolated regions are electrically biased with reference to the silicon substrate. There will be no discussion of the mechanism of heterojunction rectification, but the methods of film fabrication, geometry control, and structural evaluations will be covered in detail. Electron diffraction, X-ray diffraction, and diode electrical properties were used to characterize the films and the junctions. GAS-PHASE DEPOSITION OF Sic The techniques for the deposition of silicon carbide films were a logical outgrowth of the standard silicon epitaxial process. The major premise followed was that, for any film to nucleate in an ordered fashion where there is considerable mismatch in lattice parameters (in this case 22 pct), an extremely clean, damage-free substrate surface must be presented to the gas stream. Thus a standard gas-phase HCl etching step was used to prepare the substrates for growth. A minimum of 5 µ of substrate-surface material was removed prior to the deposition of Sic overgrowth films. The techniques used for growing silicon carbide films were those of growing silicon alone, with the added injection of a hydrocarbon gas into the hydrogen and silicon tetrachloride gas stream. The hydrocarbon gases used thus far have been research-grade (99.99 pct) methane (CH4) and propane (C3H8). Propane ultimately gave the best results. The gas flows were controlled through a panel shown schematically in Fig. 1. A hydrogen main stream of 30 liters per min passed through the horizontal quartz-tube epitaxial reactor, while SiC14, C3H8, HC1, and doping gases were injected as side streams. The

Jan 1, 1965

ALABAMA. Aldrich, Aldrich, W. F. Anniston, Noble, A. E. Auburn,&apos; Brown, R. L. Bessemer Abbott, C. E., Ferguson, V., Williams, E. P. Birmingham, Aldrich, T. H., Aldrich, T. H., Jr., Allen, A. W., Bowron, J., Burbidge, T. A., Crawford, G. G, Crockard, F. H., Dimmick, F. D., Ellis, E.,E., Hiller, E., Johnson, G. R., Ludwig, C. P., McCormack, G B., McCrery, Moffett, C. A., Morris, B.H, Peters, R., Jr., Pill, J. R., Ramsay, E. Gadsden, Hudson, J. B. Helena, Squire, J. Holt, Shook, J. W. Huntsville, Moss. Lehigh, Toulmin. Rock Run, Garvin, J. M. Thomas, Kluttz, W. L., Johnson, J. E., Jr. University, Litchman, H. B., Smith, E. A. Woodward, Woodward, A. H.

Jan 1, 1910

PROF RICHARD ÅKERMAN Stockholm, Sweden DR FRANK DAWSON ADAMS Montreal, Canada PROF RICHARD BECK Friberg, Germany ANDREW CARNEGIR New York, N.Y. DR. JAMES DOUGLAS New York, N.Y. PROF HATON DE LA GOUPILLIERE Paris, France SIR ROBERT A. HADFEILD London, England PROF HANS HOFFER Leoben, Austria HERBERT C. HOOVER Leoben, Austria JAMES FURMAN KEMP New York, N.Y. PROF HENRI LOUIS LE CHATELIER Paris France EZEQUIEL ORDONEZ Mexico City, Mexico DR ROSSITER W, RAYMOND New York, N.Y. PROF RICHARD H, RICHARDS Boston Mass. DR. ING H. C. EMIL SCHROEDTER Dusseldorf, Germany JOHN E. STEAD Middlesborugh, England PROF DIMITRY CONSTANTIN TSCHERNOFF St Petersburg, Russia PROF TSUNASHIRO WADA Tokyo, Japan CHARLES D WALCOT Washingtion D.C.

Jan 1, 1923

YEAR OF ELECTION 1913. FRANK DAWSON ADAMS, Montreal, Canada. 1921. WILLIAM CUTHBERT BLACKETT Sacriston, Durham, England. 1935. GUILLAUME DANIEL DELPRAT Melbourne, Vic., Aust. 1920. HENRY STURGIS DRINKER Merion Station, Pa. 1933. KARL EIKERS NEW YORK, N. Y. 1922. FEDERICO GIOLITTI Torino, Italy. 1906. SIR ROBERT A. HADFIELD London, England. 1928. JOHN HAYS HAMMOND New York, N. Y. 1921. FRANK WILLIAM HARBORD London, England. 1917. HERBERT HOOVER Washington, D. C. 1905. HENRI LECHATELIER Paris, France. 1931. WALDEMAR LINDGREN Cambridge, Mass. 1921. C. McDERMID London, England. 1913. EZEQUIEL ORDONEZ Mexico City, Mexico. 1935. ROBERT PEELE New York, N. Y. 1911. ROBERT H. RICHARDS Cambridge, Mass. 1934. T.A. RICKARD Victoria, B.C., Canada 1933. ALBERT SAUVER Cambridge, Mass.

Jan 1, 1936

Elected Died 1895 *ABBOTT, AI ATTHUR 1908 1882 *ABBOTT, ARTHUR V 1906 1905 * ABE, MASAYOSHI 1909 1903 * ADAMS, CHARLES C. 1905 1905 * ADAMS, WILLAMS 1909 1903 * ADAMS, W. EDWARDS 1910 1884 *ADDY, MATTHEW 1896 1906 * AFFLECK, WILLIAM A. 1911 1889 * AKERS, WILLIAMS 1906 1905 * ALABASTER, RUPPERT C. 1911 1899 * ALBERGER, LOUIS R. 1911 1894 *ALLEN R B 1896 1905 * ALLEN, R. SCOTT 1906 1874 * AMIOT, H. 1892 1886 *AMSLER, CARL 1894 1898 ** ANFERSON, JOHN w. 1905 1895 *ÅNGSTROM, CARL 1901 1887 * ARCHBALD, JAMES 1910 1900 * ARLETT, GEORGE H 1906 1895 *ARMSTRONG, JOHN F 1898 1882 *ARNOLDS, HUGO 1886 1875 *ASHBURNER, CHARLES A 1889 1872 *ASIIBURNER, WILLIAM 1887 1883 *ATKINS, C M , JR 1885 1905 * AUSTEN, PETER T 1907

Jan 1, 1917

THE CHAIRMAN (J. W. RICHARDS, South Bethlehem, Pa.)-The first point on which I wish to speak is that sufficient attention has not been given to the quality of the ores, in estimating the reserves. I made this same criticism of the work on the iron-ore resources of the world issued by

Jan 12, 1918