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Impact Transition Temperatures of Some Pearlite-Free Mild Steels As Affected by Heat Treatments in the Alpha Range H. P. Tardif (Canadian Armament Research and Development Establishment, Quebec)—Mr. Josefsson is to be congratulated for his study of a most difficult subject and for the theories proposed to explain the re- sults. One point which, however, might not have received proper attention is that of the shape of the stress-strain curve at the yield point of quenched and furnace-cooled specimens and of specimens strain aged

Jan 1, 1956

By L. S. Castleman, H. A. Froot

A study was made of the growth kinetics of B-brass layers in a-brass us y-brass diffusion couples in which both phases were saturated in the 6 phase. It was found that useful estimates can be made of the difhsion coefficients at the ß-phase interfaces from interface displacement data, which are relatively easy to measure experimentally; also, a useful estimate can be made of the mean heat of activation for diffusion from layer growth data. The effects of pressure on layer growth kinetics were explored and found to be consistent with a vacancy model for diffusion in 6 brass in both the disordered and ordered temperature range. 1 HE study of multiphase diffusion receives relatively little attention in comparison with that devoted to diffusion in homogeneous materials. Of the hundred or so papers on diffusion written each year,' only a few are devoted to the subject, and it is the rare review article2,3 that devotes any space to multiphase diffusional phenomena. This is unfortunate, since the metallurgist frequently encounters practical situations involving cementation processes such as cladding, protective coating of metals, and so forth in which he needs guidance of a fundamental nature. The investigation of multiphase diffusion phenomena is complicated by the fact that one must consider reactions at phase interfaces as well as the migration of atoms within the individual phases; these reactions cause the interfaces to be displaced within the diffusion zone. The relative displacement of two adjacent interfaces corresponds to the growth of an intermetallic layer, and it is not difficult to determine experimentally the kinetics of layer growth. In the past few years it has been pointed out4,5 that valuable fundamental information may be gained about diffusion coefficients and the concentrations at interfaces through a study of their motion. Accordingly, it is the purpose of this paper to report the results of an investigation of interface motion in a simple multiphase binary system. In the work reported herein, attention was focussed on the growth of a 6 -brass layer in a diffusion couple prepared from a- and y-brass compositions saturated with respect to the 6 phase. This particular system was chosen for a number of reasons. First, the bcc ß-brass phase is disordered for all compositions at temperatures above 468°C and becomes increasingly long-range ordered for all compositions at temperatures below 454° C;6,7 thus, the effects of a variation in order on interface displacement could be determined. Second, diffusion coefficients have already been obtained as a function of temperature in the ß phase both in the ordered and disordered Re- and a theoretical picture of the mechanism of diffusion in this and other ordered solutions is emerging.11'12 Third, some thermodynamic data are available for the a-, ß-, and ?-brass phases,13,4 and these data could be used to gain insight into questions of phase equilibria and concentrations at phase interfaces.

Jan 1, 1963

By E. N. Aqua, C. M. Owens

The microstructure in cold-rolled Zircaloy-4 sheet has been characterized by transmission electron microscopy and X-ray diffraction line-broadening techniques. The rate of work hardening is measured in terms of microstrains, particle sizes, micro hardness, the tensile yield strength. The tensile yield strength of Prestrained (less than 10 pet) Zircaloy-4 sheet is found to be a linear function of the square root of the dislocation density, us predicted by work-hardening theories. ZIRCALOY is one of the most important structural alloys for nuclear reactor applications.''2 In order to understand the effects of the nuclear environment on Zircaloy structural members, the preirradiation microstructure must be characterized. This report will describe the substructure existing in cold-rolled Zircaloy-4 sheet as observed by electron microscopy and by X-ray diffractometry. I) EXPERIMENTAL PROCEDURE Commercial Zircaloy-4 strip was cold-rolled and annealed in argon at 760°C for 1 hr. The annealed sheet was again cold-rolled to a maximum of 50 pct reduction in thickness with segments of the strip being retained after 2.5, 5, 10, and 20 pct reductions. One-inch-square portions were chemically polished (50 parts HNO3, 50 parts H2O, 10 parts HF) and mounted onto lucite blocks using double-sided tape to prevent bending during handling. Thin foils suitable for transmission electron microscopy were prepared from each of the sheet samples. The sheets were mechanically polished through 600-grit paper to a 3 to 4 mil thickness and were chemically polished by immersion for 1 to 2 min in a solution containing: 50 parts HNO3, 50 parts H2O, and 10 parts HF, and rinsed in distilled water. The final metallographic procedure was to electropolish for less than 10 sec with an electrolyte of 10 parts perchloric acid and 90 parts glacial acetic acid, at 20 v, at room temperature using stainless-steel point cathodes and a vigorous stirring action. These foils were examined in a Philips EM 200 electron microscope using a 100-kv accelerating voltage.

Jan 1, 1968

By S. J. McCarroll

J. Bruce Clemmer, J. B. Rosenbaum, and C. H. Schack (U.S. Bureau of Mines, Salt Lake City)—We have watched with considerable interest Three Kids development of Manganese Inc. and have been impressed by the ingenuity with which management and staff have solved their many obstinate handling problems. Mr. McCarroll has been lenient in describing the difficulties faced by the company in developing a process for beneficiating Three Kids ore. The operation, equivalent in size to a 20,000-ton sulphide ore plant, is treating a unique ore by a flotation process pioneered by Manganese Inc. Perhaps the magnitude of the conditioning and flotation problems peculiar to Three Kids ore can be better appraised when it is pointed out that two-thirds to three-fourths of the ore is floated in the rougher step and that the four stages of cleaning which follow are equivalent to floating the whole plant feed two to three times. Our experience in both laboratory and pilot plant flotation of Three Kids and other manganese ores leads us to agree with Mr. McCarroll that suitable conditioning is a prime requisite for successful oil-emulsion flotation. The difficulties of proper conditioning were demonstrated in pilot plant processing of Artillery Peak manganese ore at our Boulder City, Nev., experiment station. Over three months of experiments and extensive plant revision were required before satisfactory conditioning was obtained in the 25-ton-per-day plant. Such factors as time, type and intensity of mixing, aeration, surface to volume relationship, and power input are still being studied by the Bureau of Mines in hopes of learning how best to condition manganese pulps for oil-emulsion flotation. Other factors affecting flotation of manganese with oil emulsion also deserve attention. A few of these are the influence of stability and proportion of ingredients in the collector emulsion, the feasibility of grinding

Jan 1, 1955

By G. W. Neighbor, M. S. Abrahams

The actice slip plane in InSb is found to be of the {111} type by using the method of two-tmce anulysis. Measurements of the rotation of the tensile axis with increasing plastic shear strain indicate that the tnacroscopic slip direction is a <110>. Recrystal-lization is first observed at a sheav strain of about 70 pct for a crystal deformed at a temperatzcre of 473° C and at a shear strain rate of 2.90 times 10- %ecc-I; the dislocation density corresponding to this value of the strain is 1 x 108 em-&apos;. At a shear strain of about 170 pct, the recrystallization process is complete. This appears to be the fimt time re-crystallization has heen observed in a semiconductor. V HE operation of the {Hi} glide plane in Ge was first noted by Gallagher.&apos; This finding was confirmed by Treuting who also extended the result to Si. Using X-ray techniques, Treuting3 demonstrated that the macroscopic slip direction in Ge was of the <110> type. The choice of the (111) <110> slip system in Ge is exected since in the diamond-type structure the {Ill7 plane is the plane of highest density and the <110> direction is the direction of closest packing.4 There is little reason to expect that the glide elements of InSb are different from those of Ge, since the zinc-blende structure characteristic of InSb is quite similar to the structure of Ge. With regard to InSb, Allen5 has indicated that the glide plane is the {111} type. There appears to be no quantitative determination of the glide direction, however. The present work was undertaken to establish both the glide plane and glide direction in InSb and also to see if recrystallization occurs at large shear strains. EXPERIMENTAL PROCEDURE Mechanical Deformation. The single crystals of InSb used in this investigation were deformed in uni-axial tension. The tensile axis of the specimens was [145] and the periphery was bounded by (111) and (321) planes as shown in Fig. 1. The metallographi-cally polished specimens were deformed in a dynamic atmosphere of He, using an Instron machine. The tensile tests were performed at temperatures in the range of 300°C to the melting point (525OC) and at shear strain-rates varying between 1.94 X 104 sec-&apos; to 1.94 x 103 sec-&apos;. Additional details concerning the preparation and deformation of the specimens have been presented previously.&apos; Analysis of the Glide Elements. The traces of the active slip plane in both (111) and (321) planes were analyzed according to the usual method of two-trace analysis." The macroscopic slip direction was determined by measuring the rotation of the tensile axis as a function of plastic strain,8 These measurements were made from Laue back-reflection X-ray photographs. The X-ray beam was perpendicular to the (111) plane. A given crystal was used for only one measurement of the rotation of the tensile axis after it had been strained to a predetermined value. Therefore, care was taken at all times to insure that the X-ray beam was parallel to the [Ill ] direction of all the samples. RESULTS AND DISCUSSION Glide Plane. After 3.4 pct plastic shear-strain, at a temperature of 369°C and a shear strain-rate of 1.94 x 104 sec-&apos;, the slip traces on the (111) and (3.21) planes appear as in Figs. 2(a) and 2(b), respectively. The results of an analysis of these glide markings demonstrate that the slip plane is (111). The operation of this plane is expected on the basis of the orientation of the specimen, since glide on this plane and in the [I011 direction will result in

Jan 1, 1962

By S. P. Ray, B. D. Sharma

THE activation energy values for self-diffusion in pure metals have been correlated with a number of physical properties such as melting points,1 valences,&apos; Debye temperatures,3 and cohesive energy densities.4 Extending the melting point correlation, the self-diffusion activation energy values for the alloys can be similarly correlated with the solidus temperatures. For metals and alloys which exhibit phase transformations, such a correlation is not feasible because of the uncertainty of various physical properties of the corresponding phases. Using thermodynamical approach, Ardell5 calculated the hypothetical melting points of the low melting phases of the polymorphic metals. However, these calculated melting points do not show reasonable correspondence with the activation energy of self-diffusion. Recently, a new approach treating metals and alloys as electron concentration phases has been developed by Engel6 and Brewer.7 These workers have attempted to correlate the crystal structures with the electron configurations of the atoms existing either in ground state or in an excited state of low promotion energy. The basic postulate of this theory is that whereas the contribution to the bonding of the metal comes from the interaction of both d and (s-p) electrons existing either independently or in hybridized states, the existing crystal structure is controlled by the (s-p) electrons alone. Specifically, a metal is supposed to crystallize in bcc, hcp, or fcc phase provided the metal has one, two, or three valence electrons per atom in the (s-p) configurations. The diamond, or ZnO and ZnS structures, occur with four (s-p) electrons per atom. Secondly, the contribution of d electrons to bonding is supposed to increase with atomic number

Jan 1, 1970

By AIME AIME

C. H. BENEDICT, chief metallurgist of the Calumet and Hecla Consolidated Copper Co., has pioneered for nearly half a century. Noted for his ammonia leaching process, lie has Iong been responsible for all Calumet and Hecla mill, concentrator, and reclaination plant flowsheets. His influence has spread far beyond his own organization. lie is dean of Lake Superior metallurgists and has contributed greatly toward raising his specialty-the country over-to an honored profession; not merely an honored profession but a profitable one for industry and the public. The leaching process which he developed in 1912 has, since 1915, produced for Calumet and Hecla 250,000 tons of copper from waste tailings at a cost per pound, in 1929, below five cents. It has yielded profits of $35,000,000. In the war just ended, this process proved the only one adaptable to the recovery of copper from gilding-metal¬clad steel strip, and Calumet and Hecla treated more than 50,000 tons of such scrap for the Government.

Jan 1, 1945

By J. Pinto, F. Galasso

THE current emphasis in preparing boron fibers by reduction of gaseous boron compounds on a resistively heated metal wire substrate has renewed interest in the borides of those metals which have relatively high melting points and are available as fine wires. A knowledge of the structures and properties of the borides, which are formed when boron diffuses into the metal core during boron deposition, can be of assistance in the understanding of the boron fiber formation process and the fiber properties. Many of these borides are well-known and their properties have been measured. However, when an unidentified boride is found in the core, it may be difficult to establish its composition because of the small amount of material available, the preferred orientation effects on the reflections in its X-ray pattern, and the possible overlap of X-ray reflections if several borides are present in the core. For example. the proper indexing of the X-ray pattern of WB4, which was formed in the tungsten substrate core during boron fiber formation, was accomplished only after small single crystals of this boride were grown and X-ray precession investigations were conducted.&apos; This note presents the results of a study of the phases formed in the core when tungsten, tantalum, and molybdenum metal wires were used as substrates in the boron fiber preparation process with particular emphasis on the identification and characterization of a higher boride of molybdenum analogous to WB,. Boron was deposited on resistively heated stationary 0.0012-in.-diam tantalum, tungsten, and molybdenum wires at 1050°C for various times up to 60 sec using boron trichloride and hydrogen as the reactant gases. After 60 sec of boron deposition the fibers were approximately 0.006 in. in diam. Examination of photomicrographs of fiber cross sections showed that the boron had diffused nearly to the center of the tungsten and molybdenum cores in 15 and 30 sec, respectively, and only halfway to the center of the tantalum core in 60 sec. X-ray diffraction photographs of the fibers indicated that it was also after 15 and 30 sec deposition times that the tungsten and molybdenum metal reflections, respectively, had disappeared from the X-ray patterns of the fibers. The patterns of the boron fibers produced using tantalum wire as a substrate showed that amorphous boron, TaB2, and tantalum metal were present after a few seconds deposition time and remained even after deposition times of 60 sec. Until a deposition time of 15 sec was reached, the tungsten substrate fibers contained amorphous boron,273 6WB, W2B5, and WB4 as well as tungsten metal, while the molybdenum substrate fibers contained amorphous boron, MoBa, Mo2B5, and molybdenum metal for deposition times up to 30 sec. Just before the molybdenum metal pattern disappeared, a pattern similar to that of WB, appeared, suggesting that a phase, MOB,, isomorphous with WB,, was present in the fiber. This same pattern was obtained from the product formed by heating a mixture of molybdenum metal and excess boron powder in a boron nitride crucible at 1960°C in an argon atmosphere. As was the case with the WBn pattern, this pattern could best be indexed on the basis of a hexagonal unit cell rather than the tetragonal unit cell Chrktien and Helgorsky reported for ~0~4,~ see Table I. The unit cell parameters for MoB4 were calculated to be a, = 5.214A, co = 6.358A. Assuming the space group P63/mmc and positions5 2M01 in 2b and 2MoII in 2c found for tungsten in WB~,&apos; a logical structure for MOB, was determined using geometrical considerations to place the boron

Jan 1, 1969

By Robert T. Ault

The nature of fracture in unnotched tensile and notched tensile sheet and round specimens and V -notched and precracked Charpy-type sheet specimens of both wrought stress -relieved and re-crystallized molybdenum was investigated over the temperature range of -78° to 300°C. The sharp rise in fracture stress, for unnotched tensile samples, as the temperature is increased above the brittleness transition temperature (Tb), is found to be a result of an increase in flow stress due to plastic constraint and an increased strain rate which results from the onset of necking at Tb . Quasi-brittle fracture in notched tensile samples is found to occur when the tensile stress at the elastic-plastic interface, beneath the root of the notch, reaches a maximum critical value, which is independent of test temperature over the range from —78° to 25°C, but dependent on microstructure. In the temperature range between 150° and 300°C, unnotched tensile and notched tensile samples alike are found to fracture by a ductile fibrous tearing process which is discontinuous in nature, as a result of the competition between the processes of tearing, through continued plastic flow, and local work hardening. Results from the V-notched and fatigue-cracked Charpy-type impact tests demonstrate that crack initiation is the governing factor in the low-temperature (-78° to 25°C) fracture process for molybdenum. In recent years, there has been considerable interest, and a commensurate number of investigations, concerning the duc tile-to-brittle transition in refractory metals. There has not developed, however, a satisfactory explanation for the uniaxial tensile fracture-stress transition which accompanies the well-known ductility transition. This matter therefore warranted investigation. In a similar manner, the increased importance of notched tensile strength values in evaluating materials and in design criteria requires a better understanding of the factors which control the fracture behavior of notched tensile samples. In a previous investigation1 of the nature of initial yielding and fracture in notched sheet molybdenum at room temperature, it was suggested that plastic constraint was the controlling factor in governing the fracture behavior of notched samples. The final portion of this investigation was concerned with the fracture toughness of molybdenum. Of particular interest was the comparison of effective surface energies for fracture in V-notched samples with fatigue-cracked, Charpy-type samples in order to ascertain the relative importance of the initiation and propagation phases of the fracture process. MATERIALS AND TEST PROCEDURE Sheet tensile, notched tensile, and V-notched Charpy specimens were prepared from 50-mil, stress-relieved molybdenum sheet.* Half of these specimens were vacuum-annealed for 1 hr at 1200°C and 7.5 x l0-5 Torr and furnace-cooled to produce a relatively uniform grain size of 0.30 mm diameter. Round notched and unnotched tensile specimens were prepared from warm-rolled and swaged 5/8-in.-diam bar.* These specimens were vacuum-annealed for 1 hr at 1350°C and 5 x lom5 Torr and furnace-cooled to produce a grain diameter of 0.11 mm. Material analyses in ppm were: C N O H Sheet 290 10 4 1 Bar 50 30 30 2 The unnotched tensile sheet specimens had a 1/4-in. gage width and a 1-in. gage length. The unnotched tensile round specimens had a 9/32-in. gage diameter and a 1-1/4-in. gage length. The sheet and round notch tensile specimens are shown in Fig. 1. All of the notched tensile specimens tested were tandem-notched in order to study the location and mode of fracture initiation. The tandem-notched specimens were carefully machined so that the largest variation in notch depth on a single specimen was 0.001 in. Thus, when fracture occurs, the extent of plastic deformation that exists in the un-fractured notch section is that which exists just prior to fracture. All of the tandem-notched sheet specimens were electrolytic ally polished and chemically etched prior to testing. The V-notched Charpy-type specimens machined from the 50-mil sheet material had the standard dimensions of 2.125 in. long, 0.394 in. deep, and a 0.010-in. root radius. The unnotched tensile and notched tensile tests were conducted over the temperature range of -78° to 300°C, in a 10,000-lb Instron Universal Testing Machine, at a constant crosshead speed of 0.020 in. per min. The V-notched Charpy-type

Jan 1, 1964

By A. E. Bellis

THERE is a wide difference of opinion among rifle experts in the matter of barrel steel, and the relative importance to the life of the barrel of the steel&apos;s composition, heat-treatment, structure, and physical properties. In order to promote discussion, which it is hoped may lead to the discovery of the source of &apos;some of the traditional beliefs on the subject, the results of some tests are presented here, with data on heat-treating, physical tests, and erosion. The detailed metallographic study of this steel is given in another paper.1 The conclusions from these tests should be capable of wider application than their direct bearing on the barrel-steel problem. The Government specifications for barrel steel for model 1903 rifle (Springfield) call for carbon 0.50 to 0.60 per cent., manganese 1.00 to 1.29 per cent., silicon under 0.25 per cent., sulfur under 0.06 per cent., phosphorus under 0.08. per cent. The minimum physical requirements are: Tensile strength,- 110,000 lb. per sq. in. (7733 kg. per sq. cm.); yield point, 75,000 lb. per sq. in (5472 kg. per sq. cm.); elongation, 20 per cent.; reduction of area, 45 per cent. Material fulfilling these requirement&apos;s gives practically no failures when proof-fired, with charge of 70,000 lb. per sq. in. pressure, which is 40 per cent. in excess of the service charge. The turning and drilling operations show up any seams or laps such as accidentally occur even in- the best heats of open-hearth steel, so that&apos; faulty stock is practically all eliminated before proof-firing. These physical requirements are met either by rolling billets at, a proper temperature clown to the form of tapered barrel blanks or by heat-treating bars that have been upset to enlarge the breech section. The transformation temperature of this steel, on heating, is around 1350° F. (732° C.), varying somewhat with the composition and the rate of heating. The actual treatment of the barrel blanks, as carried out by different

Jan 7, 1919

By AIME

D R. GILLSON, who was born in Evanston, Ill., in 1895, is another one of those geologists who received his early inspiration and foundation in his science from that great teacher at Northwestern University, the late Professor U. S. Grant, and then went on to give his time and interest to Institute affairs-like those other Northwestern men, Arthur Blair, Gilbert Cady, Charlie Behre, Evan Just, Ian Campbell, Clayton Ball, and many others. After serving in the Navy in the first World War as, of all things for a geologist, a commissary officer on a transport, he went on to MIT and took his doctor&apos;s degree under Waldemar Lindgren in 1923. He even assisted in mineralogy at Harvard and thus had training under another great teacher, Charles Palache. He taught mineralogy and petrography at MIT from 1923 to 1928. After several summers of field work as an assistant in the U. S. Geological Survey, Dr. Gillson joined the staff of the du Pont company.

Jan 1, 1947

By K. P. Mukherjee, K. P. Gupta, J. Bandyopadhyaya

Even though a lot of work has been done in the past to establish phase equilibrium in the Cu-Si system a re cent investigation casts some doubt about the existence and crystal structure of some of the phases that form in the composition range of 15 to 25 at. pct Si in Cu. The present investigation was carried out using high temperature X-ray diffraction technique along with other standard techniques to study the phases in this composition range. The high temperature 6 phase appears to be tetragonal with parameters a,, = 8.815A, c, = 7.903A, and co/ao = 0.896. The reported bcc E phase exists at room temperature and at least up to 780°C and appears to undergo a transformation near 600°C. The phase appears to be cubic but not of the bcc type. The ? phase appears to undergo a transformation, as has been indicated by earlier investigators, and the low temperature form of .? phase is tetragonal with parameters a, = 7.267A, co = 7.8924, and co/ao = 1.086. THE Cu-Si binary system has been investigated by several investigators1" and several intermediate phases,?,e,?&apos; at lower temperatures and ?,ß,0,e, and ? at higher temperatures, were observed between terminal solid solutions of copper and silicon. Even though the existence of the e phase and the transformation in the ? phase were reported in many early works, in a recent study of this system Nowotny and Bittner6 doubted the existence of the e phase and phase at 550°C. Among the high temperature phases, the 6 phase was reported to have a complex cubic structure with parameter a, = 8.805A.7 Nowotny and Bittner, however, suggested that the structure of the 6 phase might be of CsCl type. In order to check these contradictory reports the present study was taken up to investigate the Cu-Si binary system in the composition range of 17 to 25 at. pct Si. EXPERIMENTAL PROCEDURE Weighed amounts of copper (99.99 pct) and silicon (99.9 pct) were induction melted in recrystallized alumina crucibles under argon gas atmosphere. The alloys containing 17, 18, 20, 21, 21.2, 22, and 24 at. pct Si were annealed in evacuated and sealed quartz capsules at 700°C for 3 days and subsequently water quenched. Other than this annealing, the 21.2 at. pct Si and 24 at. pct Si alloys were annealed at 550°C for 10 days, the 17 at. pct Si alloy was annealed at 750°C for 3 days, and the 22 and 24 at. pct Si alloys were annealed at 780°C for 2 days. All annealing temperatures were controlled to within *l°C. Alloys after quenching were subjected to metallographic and X-ray diffraction investigation. A solution containing 5 g FeC13 + 10 cc HCl + 120 cc H2O diluted with six times its volume with water was used as etching reagent. A 114.6 mm diam Debye Scherrer camera was used for obtaining diffraction patterns. The 17, 21.2, and 24 at. pct Si alloys were subjected to high temperature diffractometry using a Tempress Research High temperature attachment and a GEXRD VI diffractometer. For the 6 phase (17 at. pct Si alloy) powder specimen from a 750°C annealed alloy was reheated to 750°C in the high temperature attachment for 1½ hr before taking a diffraction trace. A 550°C annealed and slowly cooled phase (24 at. pct Si) alloy was first reheated to 550°C. a diffraction trace was made after annealing it for 2 hr, and subsequently it was heated to 716OC and kept at this temperature for 2 hr before taking a diffraction trace. For the e phase (21.2 at. pct Si alloy) a 550°C annealed and slowly cooled specimen was heated first to 425°C and annealed at this temperature for 2 hr before taking a diffraction trace. Subsequently, the specimen temperature was raised to 495", 540°, 603", 635", 682", 720°, and 748°C and homogenized at each temperature for 1 hr before taking diffraction traces. The powder specimen temperature was controlled to within +2oC at each temperature and argon gas, purified by passing it at slow rate through a fused CaC12 column, hot (800°C) copper and titanium chips and finally through a P2O5 column, was used to prevent oxidation of the powder. For all X-ray work copper-radiations at 25 kv, 15 ma (for Debye Scherrer technique), and 40 kv, 20 ma (for diffractometer tech-nique) were used. RESULTS AND DISCUSSION At 700°C the alloys containing 17 to 21 at. pct Si showed two phases while the 21.2 at. pct Si alloy was found to be single phase. The X-ray diffraction patterns of the two-phase alloys were consistent with the phase (ßP-Mn type structure) and the phase (21.2 at. pct Si) patterns. The diffraction patterns of the 17 at. pct Si alloy quenched from 750" and 700°C were identical. According to the accepted Cu-Si phase dia-gram4,5,10 the 17 at. pct Si alloy at 750°C should be in the (k + 6) two-phase region and very close to the -phase boundary. The identical patterns possibly resulted from the decomposition of the 6 phase on

Jan 1, 1970

By T. J. Koppenaal

The surface slip line structure has been investigated by optical microscopy during the easy glide deformation of Cu-A1 single crystals as a function of composition, testing temperature and prior thermal treatment. The slip line structure in alloys of 2.5 or less at. pct Al is similar to pure copper, while alloys of 5 or more at. pct Al show slip tracings typical of a brass. Cross slip is observed in the "a-brass type" crystals and the amount of this type of slip increases rapidly with aluminum content. The cross slip tendency in 14 at. pct Al crystals is signicantly higher when tested at 150°C as compared to 4.2" and 77°K. In addition, cross slip is more pronounced in this alloy in the furnace cooled condition than when quenched from 450°C. The cross slip behavior is analyzed in terms of existing models for this type of deformation. In two previous investigations, reports of yield points1 and solid solution strengthening2 in Cu-A1 single crystals have been given. This paper enlarges upon the brief description of the slip line structure discussed in these reports. Since the easy glide slip line pattern of copper changes markedly with the addition of -30 pct Zn (-brass),3 a study of slip lines as a function of solute additions in Cu solid solutions should help to explain some of these differences. In addition to composition variables, slip lines have also been studied as a function of testing temperature and prior thermal treatment. PROCEDURE The slip line observations were made on single crystals of 0.5 to 14 at. pct Al using a light microscope. Details concerning the preparation and basic testing procedure are given elsewhere.&apos; Prior to testing, each crystal was homogenized at 900°C for 24 hrs, furnace cooled, and electrolytically polished in a 60 pct phosphoric acid solution. The strain rate was-5 X 10 sec-I in each case. Unless otherwise stated, all observations reported upon here were made during the early stages of easy glide. RESULTS AND DISCUSSION The maximum magnification generally used was 1000X, and slip lines could be resolved down to about 105 cm (1000A). This resolution is appreciably less than obtainable with electron microscopy replica techniques where the replication can resolve slip lines down to about 40 A. Thus, while many qualitative features could be studied, the type of quantitative data obtainable with an electron microscopy replica study could not be made. Crystals containing 0.5 and 2.5 at. pct Al deform much like pure copper exhibiting a high density of fine slip lines that cover the entire gage length of the specimens. Fig. 1 shows the surface slip line pattern in a 2.5 at. pct A1 extended 0.01 shear strain at room temperature. Crystals having 5 to 14 at. pct A1 showed appreciably coarser slip lines that were generally concentrated at one end of the gage length. During easy glide these coarse slip lines propagate along the gage length in a manner similar to that observed in a-brass single crystals by Piercy, Cahn, and cottrel14 and refered to by them as a Lüders band propagation. Fig. 2 shows a typical area of these coarse slips in a 14 at. pct A1 crystal after a room temperature shear strain of 0.01. Two slip systems were apparently active. Using a method described by Cullity, the angles, between the specimen axis and the normals of the primary and secondary slip planes were determined to be 50 and 84 deg, respectively. &apos;From the Laue photograph, was 52, 81, 66, and 30 deg for the primary, cross, conjugate, and fourth slip planes, respectively. The secondary active plane in Fig. 2 is thus established as the cross slip plane, and the operative slip system is evidently the cross slip system, e.g., slip

Jan 1, 1963

By Anne Nicholson Hird, H. A. Schwartz

Of the outstanding investigators of the system iron-carbon-silicon Gontermann,1 Charpy and Cornu-Thenard,= and Honda,3 only the first touched on the chemical composition of the solid and liquid phases in equilibrium with one another. He concluded that his data did not permit a decision as to which of an indefinitely large number of pairs of compositions of liquid and solid would be found in any given case. If through the three dimensional equilibrium diagram of the iron-carbon-silicon system an isothermal plane is passed in the region of partial solidification, two lines of intersection with the liquidus and solidus, respectively, are obtained, also a point marking the alloys&apos; composition. If, in this plane, a straight line is drawn through the point, and intersecting both the liquidus and solidus isothermals, the two intersections mark a liquid and a solid alloy that may be chemically in equilibrium at the chosen temperature. From thermal data alone, Gontermann could not assign any particular direction to the line and, hence, could not determine which pair of conjugate points to choose, A separation of the liquid and solid for analysis, obviously, presents grave experimental difficulties. During the solidification of white cast iron, austenite of progressively higher carbon will separate as the temperature falls and cementite will appear suddenly at the freezing point of the eutectic. This cementite will be accompanied by a corresponding amount of austenite which, for our purpose, will be chemically inseparable from the primary austenite. We have attempted to decide on the conditions at the end of the freezing by a chemical separation applied to the solid metal.

Jan 1, 1925

By C. G. Dunn, F. W. Daniels, M. J. Bolton

IN recent investigations1. a data on relative grain boundary energies in silicon iron have been obtained. The present investigation is a continuation of this work along similar lines for the purpose of obtaining additional information on boundary energies. One aim has been to extend the data for a (110) series, which was formerly studied,&apos; to small differences in orientation, since a recent theory3,4 based on a dislocation model of grain boundaries predicts a E. ? (A-ln ? )* form of energy curve for small differences in orientation. Another aim has been to provide data for a (100) series—all grains having (100) planes parallel with the surface of sheet speci-mens—and to compare the results with the predicted form of energy curve. Finally, information on the nature of approach to equilibrium conditions was to be obtained through observations on the movements of grain boundaries. Recently published papers2,3,5 have treated the mathematical problem of expressing equilibrium conditions for grain boundaries for the general case when boundary energy depends upon boundary orientation. The equilibrium equations, which relate equilibrium angles and grain boundary -free energies, contain additional terms that express the variation of energy with boundary rotation. It has been necessary in the present investigation, however, to neglect these additional terms since no data for their evaluation were available. Dropping the additional terms leads to the following approximate equations which were used: E12/sin ?3 = E18/sin?2 =E28/sin?1 or those of the form: E28 + E13 cos ?3 + E12 cos ?2 = 0 Experimental Procedure Except for sample F1, all specimens were made from two lots of silicon iron called C and L respectively. The compositions of these are listed in table I. In the preparation of 12 three-grain specimens for the present investigation, a controlled grain growth technique, which has been described previously,&apos; was used. After preparation, the specimens were notched at the boundaries to shorten them as a means of providing more rapid approach to equilibrium in the anneals. Initial grain boundary angles were determined from micrographs taken at X500. Seven anneals, totaling about two days at 1300°C and two to four days at 1400°C, were run in an atmosphere of pure dry argon as described in a previous paper.&apos; Boundary changes generally could be followed without metallographic surface preparation, because thermal etching occurred during the anneals. These observations indicated angle changes of as much as 35" in some instances, with the major changes occurring during the first anneal. Annealing was discontinued when the angles reached stationary values. Fig. 1 gives a schematic diagram for purposes of defining crystallographic and boundary directions for three grains with common plane parallel with the sheet. Differences in orientations (expressed by A) are the angles between [00l] directions. They can be calculated with the aid of the ?&apos;s. The grain boundary angles can be calculated from the w&apos;S. Results Results are given in table 11. Types of crystal-lographic planes refer to those parallel with the sheet. Orientations are given in terms of [00l] direc-tions as shown in fig. 1. Except for grain 3 of specimen H6, which was unintentionally tilted 7" out of a (100) plane, all grains generally were within 1" or 2" of the plane specified. The directions of boundaries were measured generally to within 1" on both upper and lower surfaces, and the average direc- tions were determined for use in calculating the grain boundary angles. Variations in grain boundary directions refer to deviations from average directions. Boundaries near the junction point for all specimens generally were very close to perpendicu-

Jan 1, 1951

By E. W. Dewing

The solubility of A14C3 in cryolite melts has been determined by holding the melt with aluminum in a graphite crucible for 4 hr at temperature, quenching the crucible in water, and analyzing the frozen salt by CH4 evolution. The solubility is given by log(wt % Al4C3) = 1.298 -1.l74 (wt ratio NaF/AlF3) independent of temperature in the range 985" to 1080°C. Additions ofA1203, .NaCl, CaF2, or LiF up to 10 wt pct do not affect the solubility, provided that LiF and CaF2 are replaced by equivalent NaFin calculating the ratio. The variation with ratio can be accounted for quantitatively on the hypothesis that the Mechanism of solution is Al4C3 + 2AIF3 = 3Al2CF2 since the solubility varies as (aAIF3) 2/3; Mechanisms involving C", C2- , AlC- , A12C2+, and Al2CF+are re-jected. At ratios above 1.5 truces of c;- are also present. It was noticed some years ago in this laboratory that carbon specimens made cathodic in a cryolite bath decrease in diameter over a period of time.&apos; It was also found that cryolite which had been melted with aluminum in a graphite crucible was sometimes yellow, and that A14C3 could be seen intimately embedded in the cryolite crystals. CH, could be recovered by acid attack. There was thus reason to believe that A14C3 had a genuine solubility in molten cryolite, and the object of this work was to measure it. EXPERIMENTAL AND RESULTS A graphite crucible, 2 in. ID and 2.5 in. deep with a close-fitting lid, contained about 150 g of cryolite (plus additives) and about 20 g of 99.99 pct pure Al. It was placed in a vertical Inconel furnace tube, covered with refractory brick to provide thermal insulation, and the top of the tube was roughly sealed with disks of asbestos paper. An alumina tube led argon down to the level of the top of the crucible to expel air, and an alumina sheath with a Pt-10 pct Rh ther-mocouple inside was positioned between the crucible and the wall of the Inconel tube. The tube was heated in an electrical resistance furnace for the desired length of time; the refractory bricks were then removed, and the crucible was lifted out with tongs and quenched in water. After such a crucible was broken open it could be seen that its inner surface was yellow owing to the presence of A1,C3, and sometimes needle-like crystals could be observed (at X75 magnification) growing out into the nielt. It was concluded that Al,C, had been present as a separate phase when the crucible was at tenlperature and that the melt had been saturated: in

Jan 1, 1970

By G. R. Heckman, H. J. Murphy, C. T. Sims

An incestigation has been made of the effects of heat treatment and alloy composition on the long-time stress-rupture properties and structural stability of the similar nickel-base alloys Udimet-500, Lrdimet-520, and Udimet-700. Rupture test data are presented at stresses ranging from 4 to 50 ksi at temperatures from 1450° to 1900°F for times up to 14,000 hr. Ductility response is emphasized. Optical and electron tnicroscopy were complemented by X-ray diffraction analyses of extracted phases to relate microstructural stability to the observed rupture properties. Particular attention is paid to Udimet-520 since structural characteristics of this alloy appear to vary somewhat from its sister alloys. Both cast and wrought performance of Lrdimet-500 are discussed. The computerized PHACOMP calculational technique, based on electron-vacuncy theory, is discussed and related to structural stability where appropriate. Electron microscopy and microprobe techniques were used to conduct evaluation of the oxidation characteristics of Udimet-500 exposed in air for 16,100 hr. The steady advance in strength and reliability of nickel-base superalloys continues to be one of the high points of modern metallurgy. The stress capability of these materials has increased steadily, allowing higher and higher operating temperatures in the highly sophisticated aircraft and industrial gas turbines now on the market. The attendant increase in efficiency, of course, means greatly improved power output. Gas turbines for industrial and marine use have long been designed with these objectives paramount the usual design requirements in terms of time of service being 100,000 hr. High-efficiency, long-life aircraft such as the supersonic transport require superalloy engine materials with high-strength and long-time structural stability. Thus, materials studied for and operating experience from industrial gas turbines provide a good reservoir from which technology of high value to the SST program can be drawn. This study is one such case. Three prominent nickel-base super alloys—Udimet 500, Udimet 520, and Udimet 700 were extensively evaluated for industrial gas turbine bucket use. Particular attention was directed toward structural stability as a requisite property. Within the present context, structural stability is defined as freedom from the propensity to form strength-robbing or embrittling phases such as u,p,x,or Laves, and the ability to maintain useful rupture strength and ductility throughout design life. MATERIALS The three alloys, cast Udimet 500 (U-500C), Udimet 520, and Udimet 700, were chosen for detailed evaluation based on preliminary studies which indicated that U-500C and U-520 possessed comparable rupture strength capabilities, and that U -700 had a greater strength capability but somewhat poorer ductility than wrought U-500. The nominal compositions of the three alloys, along with the compositions of the heats investigated, are presented in Table I. PROCEDURE Dimensionally rejected U-520 buckets from Special Metals Corp. heat 63370 were heat-treated using the four cycles delineated in Table 11. Cycle A was investigated to determine the effects of a shortened 1700°F primary age. Cycle B was considered a "standard" treatment. Cycle C investigated a higher solution temperature in combination with a shortened primary age, while cycle D assessed the effect of the higher solution temperature alone. These heat treatments were designed to produce optimum combinations of rupture strength and ductility through maximum y&apos; development, the development of a y&apos; grain boundary cushion, promotion of MC carbide degeneration reactions, and agglomeration of resultant M23CB. Since one of the premises of the evaluation of U-520 was that rupture strength would be equivalent to U-500, forged U-500 buckets from Special Metals Corp. heat 62916 were heat-treated with cycles A, B, and C to provide comparison. The heat-treated structures of U-520 and U-500 are illustrated in the 8700 times electron micrographs of Fig. l. The U-700 tested was all from 3-in.-diam hot-rolled and centerless-ground rod from Special Metals Corp. heat 2-1426. Two heat-treatment cycles were employed, E and F of Table 11. Cycle E is a standard four-step, triple-age treatment intended to provide an optimum match of strength and ductility through well-developed matrix and grain boundary y&apos;, as recommended by U-700 vendors. Treatment F is a shortened , single-age cycle which could provide a significant processing cost reduction should adequate strength and ductility be maintained. Following heat treatment, rupture specimens of U-500 and U-520 were machined from the buckets and tested. Standard rupture bars of U -700 were machined from the heat-treated rod and rupture-tested. Failed and withdrawn rupture bars were prepared and examined by optical and electron microscopy. Select specimens were electrolytically digested, and the residues analyzed for carbide and topologically close-packed phases using CrKa or CoKo radiation. Of the six different U-500C heats evaluated, five were cast by Misco Precision Casting Co. and one was cast by Haynes Stellite Co. Cast-to-size rupture bars

Jan 1, 1968

September 1 to 6, 1918 COMMITTEE IN CHARGE Spencer Penrose, Chairman. George M. Taylor, Vice-Chairman. A. E. Carlton, Chairman. Finance Committee J. Dawson Hawkins, Secretary DENVER COLORADO SPRINGS CRIPPLE CREEK Finance Finance Thomas B. Crowe T. B. Stearns A. E. Canton , E. P. Arthur, Jr. Richard A. Parker Spencer Penrose N. S. Greensfelder T. B. Burbridge George M. Taylor A. E. Carlton. A. L. Blomfield, Treasurer B. F. Hill Arrangement I F. G. Willis Dave G. Miller Registration Norris E. Eads Frank Bulkley Loren C. Lennox 1V. E. Ryan Geo. E. Collins Horace F. Lunt Fred Jones .1. M. Tippett F. D. Smale Entertainment J. H. Haynes F. H. Bostwick Arrangement and Entertainment L. W. Lennox F. E. Shepard George M. Taylor A. L. Blomfield M. R.. Valentine Howland Bancroft J. D. Hawkins Thomas B. Crowe B. P. Morse A. E. Carlton E. P. Arthur J. G. Perry G. H. Clevenger Etienne A. Ritter Ladies Ladies , PUEBLO Mrs. T. B. Stearns, Mrs. C. M. Taylor, Mrs. C. H. Clevenger J. F. Welborn Chairman. Chairman H. B. Carpenter Mrs. C. Loughridge Mrs. S.-Penrose Mrs. A. E. Carlton L. B. Eames Mrs. H. Bancroft Mrs. J. D. Hawkins Mrs. A. L. Blomfield F. Robinson Mrs. G. Bancroft Mrs. L. C. Lennox Mrs. J. M. Tippett . Mrs. W. D. Leonard Mrs. H. F. Lunt -Mrs. E. C. van Diest Mrs. C. Chase Mrs. E. A. Ritter Mrs. AV. Strieby Mrs. F. H. Bostwick Mrs. L. S. Harner Mrs. C. L. Bailey Mrs. F. Bulkley Miss F. Dickerman Mrs. E. P. Shove Mrs. C. L. Tutt Mrs. F. C. Peck Mrs. F. D. Pastorius

Jan 10, 1918

By Ulf S. Landergren

Diffusion coefficients and marker movements have been determined in brass using welded couples. Three different concentration ranges were employed at 750°C, while a fourth concentration range was measured at 500°, 600°, 700°, and 800°C. Marker displacements toward and porosity development in the high zinc side of the couple were observed in all cases. The results were interpreted as favoring a vacancy diffusion mechanism. IN the large amount of diffusion literature which has accumulated during the past half century, very few experimental data have been presented on body-centered-cubic metallic phases. The impressive combination of experimental and theoretical studies which has given the vacancy mechanism a fairly secure position as the preferred mechanism for most face-centered-cubic metals has no counterpart for body-centered-cubic phases, although the theoretical picture seems to be in a better state than the experimental work. The attempts to select diffusion mechanisms by the theoretical calculation of the activation energy for the various conceivable unit diffusion processes and the energy of formation of the type of lattice defect required have been based on models of two kinds. The first kind utilizes potential functions fitted for certain properties of pure crystalline copper; the second kind is fitted for sodium. The latter is an example of an open metal in which the metallic ion is small compared with interatomic distance,&apos; while the former is characteristic of the larger class of metals in which the ions have diameters about as large as the interatomic distance. brass should resemble copper in this fundamental property. It should be evident that results on the mechanism of diffusion obtained for one of these classes need not necessarily apply to the other. Huntington and Seitz, using a model of the copper type, showed that the activation energies to be expected for interstitial migration or a two-atom direct interchange were much higher than that for vacancy diffusion. Zener pointed out that a four-atom ring rotation would involve an activation energy considerably lower than the two unlikely mechanisms although still higher than the vacancy mechanism in the face-centered-cubic structure. Furthermore, he argued, the four-atom rotation would be relatively easier in a body-centered-cubic lattice and might be competitive with the vacancy mechanism. Paneth showed that a body-centered-cubic crystal-like sodium could form interstitial defects of special type, called a crowdion, by crowding an extra atom into < 111 > directions where the defects would affect a line of about eight atoms. The defect was constrained to move along the defining line. Unlike the face-centered-cubic case, therefore, the theoretical calculations for the body-centered-cubic mechanism do not provide a very clear-cut answer, and the absence of adequate experimental studies is the more serious. This investigation was undertaken for the purpose of obtaining useful information on diffusion in body-centered-cubic phases. brass was chosen for several reasons: 1—the phase field is sufficiently wide at high temperatures to permit the use of diffusion couples with adequate concentration ranges for satisfactory chemical analysis, 2-—thermodynamic activity data are available for the calculation of mobilities from diffusion coefficients, 3—the phase is as close to the theoretical model of the copper -type on which the calculations have been done as any body-centered-cubic metallic phase is likely to be. Measurements of the movements (if found) of inert markers during the diffusion process would indicate that a vacancy or Or mechanism played a major role in diffusion in brass. If no marker movement should be found, a ring mechanism would be indicated but not assured. Experimental Procedure The alloys used in these experiments, listed in Table I with analyses, were supplied by the Naval Research Laboratory. They were from ingots of 3x3 in. cross-section, heated to 760°C, reduced under a

Jan 1, 1957

The Development of Research and Quality Control in the Modern Steel Plant. By Leo F. Rein-artz. (Metals Technology, April 1943) Blast Furnace and Raw Materials Essential Considerations in the Design of Blast Furnaces. By A. L. Foell. (,Metals Technology, December 1942) Results Obtained from Surveys of Gas at Furnace Tops. By James M. Stapleton. (Metals Technology, January 1943) Physical Aspects of the Dust Catcher, Gas Washer and Precipitator on No. 3 Furnace at Carrie. By C. P. Clingerman and C. J. FleiscH. (Metals Technology, January 1943) Slag Control by Introduction of Flux through Blast-furnace Tuyeres. By Carl G. Hogberg (Metals Technology, January 1943) The Electrical Conductivity of Molten Blast-furnace Slags. By A. E. MaRtin and GerRard Derge. (Metals Technology, August 1943) Some Physical Characteristics of By-product Coke for Blast Furnaces. By CEarles C. Russell and MichaeL Perch. (Metals Technology, December 19+2) Pyrometry at the Coke Oven. By Robert B. Sosman. (Metals Technology, December 1942) Calcination Rates and Sizing of Blast-furnace Flux. By T. L. Joseph, H. M. Beatty and Gust Ritsianes. (Metals Technology, December 1942) The Low-temperature Gaseous Reduction of a Magnetite. By M. C. Udy and C. H. Lorig. (Metals Technology, October 1942) Steelmaking Problems of Total Operation in Steelmaking. By William C. Marshall and Frank G. Norris. (Metals Technology, April 1943) Silicon-oxygen Equilibria in Liquid Iron, By C. A. ZapFFe and C. E. Sims. (Metals Technology, September 1942) Equilibria of Liquid Iron and Simple Basic and Acid Slags in a Rolating Induction Furnace. By C. R. Taylor and John Chipman. (Metals Technology, September 1942) Rapid Analysis of Oxygen in Molten Iron and Steel. By Gerhard DeRGe. (Metals Technology, January 1943) Silver Chloride as a Medium for Study of Ingot Structures. By Karl L. Fetters and Margaret Dienes. (Metals Technology, August 1943)

Jan 1, 1943