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By G. W. P. Rengstorff, L. E. Olds

High purity molybdenum ingots containing controlled amounts of a single impurity element (oxygen, nitrogen, or carbon) were prepared. These ingots were tested for ductility by bending test specimens at various temperatures. The relationship between the plastic behavior of the ingots and their chemical composition has been determined. MANY proposed applications for molybdenum require ductility at or near room temperature. At the present time, it is possible to obtain wrought molybdenum with considerable ductility only if special fabrication techniques are used to control the grain structure. Starting with are-cast or powder metallurgy ingots, the usual methods for obtaining ductility rely on fabrication procedures that result in fibered microstructures in the finished product. Recently, it has been found that the ductility of either powder metallurgy or are-cast molybdenum can be improved by uniform recrystallization of the metal to a very fine equiaxed grain structure.' The need for a fibered or a fine grained structure may limit the practical usefulness of molybdenum. For example, welding. which may be used in fabricating the metal, generally produces coarse grained structures that lead to brittleness. This applies, certainly, to currently available commercial molybdenum. Although commercial molybdenum is brittle when the grains are coarse, it has been shown experimentally that fine grained structures are not always essential for ductility. For instance, as-cast molybdenum with a coarse columnar grain structure is ductile if it is sufficiently pure.' Because high purity cast molybdenum has good ductility even when coarse grained, it is probable that the brittleness in coarse grained commercial molybdenum is caused by the impurity content of the metal. Although the general effects of impurities on the cold ductility of molybdenum have been known in a qualitative manner for some time, no quantitative evaluation of these effects has been available. The present investigation was made in order to determine more accurately the effects of oxygen, nitrogen, and carbon on the cold ductility of cast molybdenum. Oxygen has long been known to be detrimental to ductility, although the minimum amount which will embrittle molybdenum has been open to speculation. Parke and Ham" showed that ingots with oxygen contents above 0.003 pct could not be forged. Maringer and Schwope have described the embrittle-ment of molybdenum wire by oxygen. A discussion on the effects of heat treatment on the distribution of oxygen in molybdenum has been given by Perry, Spacil, and Wulff." Although nitrogen would also be expected to have harmful effects on ductility, no extensive work has been done previously to determine whether this is so. However, Tury and Krausz" found that wires presumably with less than 0.007 pct N were brittle. Carbon is added to commercial cast molybdenum for deoxidation. Parke and Ham" have shown that molybdenum containing as much as 0.06 pct C could be forged if the oxygen was kept below 0.003 pct. Also, Bruckart and others' found that the room temperature ductility of sintered molybdenum improved with carbon contents up to 0.84 pct. However, Rengstorff and Fischer' found that residual carbide particles in cast molybdenum apparently had an unfavorable effect on room temperature ductility.

Jan 1, 1957

By S. I. Liu

THE effects of strain histories, consisting of several prestrains in opposite directions, on the flow and fracturing characteristics of metals determined in a final test have been investigated previously.'" Such strain histories vary from a single prestrain in tension or compression to the number of strain cycles leading to fatigue failure.' Between these two limits, various strain histories could be visualized and some can be attained readily. One such example is a strain history consisting of a first prestrain in tension of various magnitudes and a second prestrain in compression also of various mag-nitude. In this investigation the strain history was extended to the combination of these two limits, i.e., a single prestrain in tension or compression followed by balanced strain cycles of a selected magnitude e, = k0.12. It was found in this case that only compressive initial prestrains could be investigated with sufficient accuracy.* Such strain histories can be considered also as (low cycle) fatigue tests of a metal subjected to various amounts of cold working. It appears from previous publications that cold working within a wide range of reductions usually raises the un-notched fatigue strength of many metals.'-' This effect, however, has been found to be inconsistent and sometimes reversed for other metals?.7 Furthermore, Ludwik reports that the yield strength of cold-worked specimens may be reduced by cyclic strains, while that of materials without cold work is generally increased in the initial cycles." " In addition to the above tests, a study was made of the effect of intermediate re-solution heat treatment on low cycle fatigue behavior. Such anneals should eliminate the strain hardening induced by the cyclic strains. As far as their effect on the fracture characteristics is concerned, a few previous tests seemed to indicate that the damage resulting from cyclic strains is retained only partially after heat treatment." A further investigation was made in which one specimen was subjected to repeated unbalanced tension cycles in which the strain interval was approximately $ 0.013. This repetition of plastic tension damages the material slightly. This result appears to confirm Ludwik's observations." " Commercial 3/4-in. rod of the aluminum alloy 24ST4 was selected for this investigation. The material was subjected to the following treatments before machining: 1—Re-solution treatment at 920" ± 10°F for 45 min, 2—water quench at room temperature, and 3—aging for four days at room tem-perature.? The treated material then was machined to desired specimen contour and tested. A coolant was used during machining to minimize any artificial aging effects of heating during machining. In some cases the 24ST4 specimens were reheat treated after having been strained. In these cases, the heat treatment was the same as the re-solution heat treatment described above. Procedure As shown in Fig. 1, threaded end specimens with a minimum diameter of 0.266 in. and a contour radius of 2 in. were used for prestraining to an axial compressive strain ranging from 6, = —0.10 to E, = —0.48. For large prestrains, two consecutive corn-

Jan 1, 1952

By D. W. Lillie

Property changes produced by irradiation of Al-0.4 wt pet Li alloys at 270°C to a burnup of 0.155 pct of all atoms are described. Metallographic evidence of the formation of internal pores and the concentration of gases at grain boundaries is shown. Some conclusions are drawn concerning desirable property characteristics for resistance to radiation swelling. RADIATION induced gases are of great practical significance in nuclear engineering since they affect the behavior of fissionable fuels and control rod materials. In fuels the gases xenon and krypton are the major offenders, producing serious em-brittlement at low irradiation temperatures and gross swelling at high irradiation temperatures. In control rod materials containing boron, the production of helium from the B 10 (n, 0) Li7 reaction produces similar reactions. Since the trend in reactor design is for operation at increasingly high temperatures, the phenomenon of high-temperature swelling by these induced gases has been the subject of considerable recent study. The objectives of such work have been to obtain engineering information and quantitative data on the effects in specific fuels and control rods and to obtain further understanding of the mechanism of gas damage so that more intelligent corrective steps can be made. Analogue systems are often useful for the latter objective and in this case alloys containing Li are suitable in view of the reaction Li6 + n - He4 + He 4. Both products are gases and no serious radiation problem is produced to complicate post irradiation handling. Considerable caution is, of course, necessary in any operations in which tritium release is possible. The present program was initiated to provide a detailed study of the effects of He + H3 generated by irradiation in Li-bearing alloys. The results on Mg-Li solid solution alloys have been reported elsewhere.' This paper presents information on irradiation of an A1-0.4 pct Li alloy in which the lithium was present as highly enriched Li6 in order to maximize the radiation burnup. PROCEDURE The original intent in the selection of the alloy content was to have Li in solid solution at all temperatures. It became apparent, however, that the solubility of Li in A1 was substantially lower than that reported in the original reference consulted.' This was substantiated by the work of Nowak3 who reported solubility of less than 0.01 pct Li at 100°C. The alloy used (0.4 pct Li) was therefore two phase at room temperature. The irradiation temperature was estimated to be about 270° C, and at that temperature all or almost all of the Li would be soluble under equilibrium conditions. The precise state of the alloy under irradiation is not known. Aluminum used was 99.996 pct purity (max. impurities Si 0.002 pct, Mg 0.001 pct, Fe 0.0005 pct, and Cu 0.0005 pct). The lithium was obtained from Oak Ridge National Laboratory; 96.1 + 0.1 pct of the lithium was ~i~, but chemical impurities were 0.25 pct Ca, 0.05 pct Fe, 0.02 pct Na, 0.02 pct Cu, 0.01 pct Sr, and 0.01 pct Ba. The two metals were melted in an alumina crucible in a resistance heated furnace in an atmosphere of helium. A l-in. ingot was cast in an iron mold, machined to %-in. round, hot swaged (350°C) to 0.080-in. round, cold swaged to 0.060-in. round, and finally cold drawn to 0.040-in. round. Four-inch wire lengths were then cut and annealed at 250°C for 4 hr in helium. Irradiations were carried out in a VT hole in the Argonne CP-5 reactor. The wires were held in an aluminum jig, sixteen wires per capsule, and were maintained in a helium atmosphere for maximum heat transfer. Eight wires of pure aluminum and eight of Al-Li alloy were placed in each capsule. Argome Laboratory statements were accepted as establishing flux and exposure levels. These were based on previous experience and flux map-

Jan 1, 1961

By G. W. Form, W. A. Spitzig

The effects of hydrogen and vacuum shtering treatments on the physical and mechanical properties of arc plasma-sprayed tungsten were inuestigated. Temperatures examined ranged from 3000" to 4000°F in vacuum and 2000" to 3000°F in hydrogen for both single and duplex sintering cycles. Densities of 92 pct of theoretical density were obtained when a long-time hydrogen treatment at 2000°Fpreceded sintering in vacuum at 4000°F for 4 hr. This cycle also produced the highest ualues for modulus of rupture and bend angle. The results of this investigation point out the desirability of using a low-temperature long-time hydrogen treatment prior to a high-temperature vacuum sinter for arc plasma-sprayed tungsten. ADVANCES in the development of arc plasma-generating equipment have provided a high-temperature heat source that makes the fabrication of tungsten shapes possible by a metallizing process. Tungsten in the as-sprayed condition is very brittle. It has a density between 80 and 85 pct of theoretical density, a lamellar structure with elongated pores, and a high interstitial impurity content. To improve these properties, sintering treatments can be applied to the as-sprayed material, similar to those used for the densification of compacted tungsten powder. However, in view of the differences in the density and microstructure of as-sprayed tungsten as compared with compacted tungsten, responses to sintering were expected to be different. EXPERIMENTAL PROCEDURES The tungsten powder used in this investigation had a particle size varying from 3 to 13 p with an average diameter of 8p. The impurity level was less than 0.1 pct. The arc plasma spraying was done with an F-40 Thermal Dynamics Corp. plasma jet. Spraying was performed in air and thus required cooling of the substrate by an air blast in order to minimize oxidation. The spraying parameters employed in the fabrication of all specimens are listed below: Power input, kw 12 Arc-gas flow, cfh 95N2 + 5H2 Powder feed rate, g per min 33 Powder carrier gas flow, cfh ION, Spray distance, in. 3 Traverse rate, in. per min 30 Mandrel speed, rpm 100 Nozzle orifice, in. 7/32 These values of the spraying parameters correspond to optimum conditions ascertained in a previous study. Sintering was conducted at 3000°, 3500, and 4000°F in vacuum (< 0.1 Hg), and at 2000 and 3000°F in hydrogen. Duplex sintering treatments investigated are listed in Table I together with the designations that will be used for reference throughout this paper. The samples were fabricated by spraying onto a copper mandrel which was removed prior to sintering. The specimens used for the sintering analyses had the shape of small hollow truncated cones 1 in. high with an inside diameter varying from 0.500 to 0.125 in. and a wall thickness of 1/8 in. Specimens for bend testing were taken from hollow hexagonal prisms 1-1/2 in. high with a 1-in. diam across the flats and a wall thickness of 1/8 in. The bend-test specimens were ground to the dimensions 0.085 by 0.350 by 1-1/2 in. Prior to bend testing 0.0025 in. of stock was removed from each surface by electro-polishing. Density measurements were made by the water-displacement method. In addition, a porosimeter was used to determine the amount of interconnected porosity for representative samples. Strength and ductility were determined from recorded values in transverse bending using a cross head speed of 0.020 in. per min. The load was applied at the midpoint of a 1-in. span. The deflection data reported herein refer only to the plastic portion of the total deflection. RESULTS AND DISCUSSION The as-sprayed samples had a density corresponding to 83 pct (l pct) of the theoretical density of tungsten. Fig. 1 shows a representative as-sprayed tungsten structure.

Jan 1, 1964

By Nicholas J. Grant, Gordon D. Gemmell

CREEP rupture characteristics of high purity Al-Mg solid solution alloys were studied by Mul-lendore and Grant&apos; to investigate solid solution strengthening of pure aluminum and the accompany- ing effects on deformation and fracture characteristics. This paper presents the results of an extension of that work to A1-Cu and Al-Zn alloys to permit a comparison of the relative effects of the three solute elements on the high temperature strength and on the deformation and fracture characteristics. Experimental Procedure A total of nine alloys was studied. They were all made of ultra high purity aluminum alloyed with high purity copper, zinc and magnesium. The corn-

Jan 1, 1958

By J. P. Hammond, C. J. McHargue, S. E. Adair

Cold-rolled sheet textures have been determined for binary solid solutions of aluminum, columbium, tantalum, and zirconium in titanium. An alloy containing 3.8 pct Al had a (0002) [10101 texture, whereas alloys with the other elements had rotated (0002) [10101 textures similar to that of iodide titanium. THERE have been relatively few studies of the effect of alloying on deformation textures. A second element may be present in the base metal in solid solution and/or as a second phase. The literature offers no satisfactory explanation for the effects of solid solution alloying on textures noted thus far. For example, there is no satisfactory explanation of the difference in the textures of copper and a brass. The most complete study of the effects of solid solution alloying on deformation textures has been that of Brick, Martin, and Angier.¹ These investigators reported that the copper texture was retained by alloys of copper with up to 30 pct Ni, less than 5 pct Zn, less than 2 pct A1 or Co up to the limit of solubility. Copper containing more than 5 pct Zn, more than 2 pct Al, or the maximum soluble concentration of tin, silicon, or manganese showed the deformation texture of a brass. Bakarian² reported that additions of 0.20 pct Ca to 99.98 pct Mg or 2.0 pct Mn plus 0.15 pct Ca to magnesium resulted in entirely different textures than for the pure magnesium. The texture obtained for high-purity magnesium sheet showed the basal plane to be concentrated parallel to the rolling plane. The texture obtained for the alloy containing 0.20 pct Ca had the basal planes concentrated in elliptical areas whose centers were tilted 15" from the center of the pole figure toward the rolling direction. This split basal orientation was even more pronounced in the alloy containing 2.0 pct Mn and 0.15 pct Ca. Fuller and Edmunds" studied the rolled sheet textures in a zinc alloy containing 1 pct Cu and 0.01 pct Mn. The basal pole figure of this alloy contained a region of strong concentration not found in the pole figure for pure zinc.&apos; In the above cases, results were discussed in terms of possible changes in slip and/or twinning systems and critical shear stresses. However, there were no experimental data to relate these speculations with the observed textures. It has been suggested that the deformation textures of titanium, zirconium, and beryllium could be directly ascribed to their low c/a ratios. The complex deformation mechanisms of titanium" also have been suggested to be characteristic of hexagonal close-packed metals with low c/a ratios. The purpose of this investigation was to study the cold-rolled sheet textures in binary titanium-base a alloys in which the c/a ratios were greater than, less than, and about the same as the c/a for iodide titanium. The annealed textures of these alloys will be reported in a subsequent article. Materials and Methods The chemical analyses of the metals used in this investigation are given in Table I. The alloys were prepared as 15 g buttons on a water-cooled copper block in a vacuum arc-furnace. The furnace was evacuated to pressures of the order of 10.&apos; mm Hg, flushed with 99.98 pct pure argon, and melting was carried out in 0.2 atm pressure argon. Each button was remelted until radiographs and chemical analyses indicated complete solution of the solute elements. All buttons were forged and homogenized 72 hr at 500°C. The buttons to be rolled were ground and etched to sizes and shapes suitable for the rolling

Jan 1, 1954

By Y. Nakada, U. F. Kocks, B. Chalmers

The stress-strain behavior of the gold single crystals in easy glide was found to be affected by the specimen dimension which is parallel to the projection of the Burgers vector of the primary-slip system. The larger this dimension is, the larger is the slope of easy glide. Previously severa1 investigators attributed the size effects to either the existence of surface films or the grip constraints. However, in this experiment both of these possible causes were not present. It is proposed that the length of slip path (defined as the crystal dimension parallel to the Burgers vector of the primary system) is the controlling factor in the size effect observed in gold. THERE are many possible effects of the specimen dimension on the work-hardening behavior of single crystals: grip effects which prevent end regions of the crystal from deformation or rotation; effects of a surface film, for example a coherent oxide; effects of a subsurface layer of accidental or intentional

Jan 1, 1964

By R. J. Arsenault

The yield drop that occurs in tantalum, Cu-AZ. and Ag-Al was investigated as a function of strain rate and at several temperatures. From the strain-rate dependence of the yield drop an activation volume was calculated and found to agree with that obtained from differential strain-mte tests. The temperature dependence of the yield drop can he explained in terms of the parameter temperature divided by activation volume. The yield drop is attributed to the rapid multiplication of dislocations during their motion. THE yield-point or yield-drop (upper yield stress minus the lower yield stress) phenomenon has been the subject of numerous investigations1-9 in both bcc and fcc metals. Also, there is no dearth of theoretical explanations10-20 to account for the yield-point phenomenon. The present explanations can be divided into two categories: the concept of dislocation locking and subsequent unlocking and the concept of multiplication of dislocations due to their motion. The Vottrell10,11mechanism of locking and unlocking, as applied to bcc metals, is the best known of the three proposed locking mechanisms. The two additional mechanisms, short-range order (SRO)7,16,17 and Suzuki-type locking,14,15 have been employed to account for the existence of yield points in fcc metals. The experimental evidence supporting the locking of dislocations, especially in bcc metals, is well-established. The dependence of the yield point on interstitial concentrations,&apos; the kinetics of strain aging,2 and the observations by electron-transmission microscopy18 are some of these experimental results. The number of experimental observations supporting dislocation locking in fcc metals is not as extensive as in bcc metals. The unlocking of dislocations, which actually is supposed to account for the yield drop, is by no means well-established by experimental results for either bcc or fcc metals. The similar temperature dependence6 of the yielding and plastic flow is one of the experimental factors that cannot be explained in terms of the unlocking of dislocations. The mechanism based on the rapid multiplication of dislocations has been proposed by several investigators. 18-20 Johnston and Gilman19 have proposed a detailed model of yielding, which was later employed by Hahn21 to predict quantitatively the yield drop in iron. This mechanism was discussed in a previous paper22 and several limitations were pointed out. In the same paper it was shown that an activation volume could be obtained from the strain-rate dependence of the yield drop and that a correlation existed between the activation volumes obtained from the yield-drop tests and from differen-

Jan 1, 1964

By Y. Nakada, B. Chalmers

The work-hardening behavior of surface layers of aluminum and gold single crystals was investigated by alternately deforming and then removing a thin surface layer by electropolishing or by etching. Aluminum crystals exhibited lower flow stresses after the surface removal; gold crystals did not. Abrasion of surface eliminated easy glide in both gold and aluminum crystals. By alternately deforming and removing the surface layer, it was shown that the abraded crystals work-harden preferentially under the abraded layer. It is suggested that this phenomenon is caused by the difficulty of propagating dislocations through the abraded layer. It has been demonstrated in numerous cases&apos;-3 that the plastic behavior of metals in either single-crystal or polycrystal form is sensitive to the environment and to the condition of the surface; it has also been reported4-6 that single crystals of some metals, when deformed in tension, exhibit more work hardening near the surface than in the interior. A third type of effect that has been attributed to the special part played by the surface in plastic deformation is the influence of the dimensions of the specimen on the various parameters that define its plastic-deformation characteris- tics.?-&apos;&apos; Many of these experiments were made on aluminum, on which an oxide film is always present under available experimental conditions; many of the effects have been attributed to the oxide film, either in terms of its higher elastic moduli, which would cause local stress redistribution, or its higher strength, which would oppose the escape of dislocations at the surface of the metal. On the other hand, it has been suggested II,12 that the mere presence of a surface should be sufficient to produce the observed results. A rigorous examination of this question could, in principle, be carried out by comparing the behavior of aluminum with its oxide film with that of the same material without oxide. This experiment would present great difficulties. The most practical alternative is to compare aluminum with gold, which has no crystalline surface film at room temperature, and to study the effects of various surface treatments on gold. The experiments described in this paper fall into two groups, the objectives of which were to determine 1) whether single crystals of gold shared the property of aluminum that the removal of a surface layer after some plastic deformation reduced the flow stress for further deformation and, since the result of this was negative, 2) whether a surface treatment could be found that caused gold to behave in this way. I) EXPERIMENTS AND RESULTS All the tests described below were carried out on single crystals of about 6 by 6 mm cross section and of sufficient length to provide a gage length of about 10 cm.

Jan 1, 1964

By C. S. Barrett

Measurements of impact hardness of ß-brass are reported for a wide range of temperatures. Abrupt softening is observed when temperatures are raised above 425ºC, accompanied by abrupt widening of deformation bands in the deformed samples. Current theories of these effects, and of the lack of twinning, are discussed. HARDNESS1 and flow stress2 of a sample of ß-brass at room temperature depend upon the temperature from which the sample is quenched. It is believed that the state of order in the superlattice is responsible for this dependence—not the order within individual domains, which reaches near-perfection during the quench from any temperature, but the size of the domains which is presumed to be a minimum in the hardest samples, those quenched from temperatures near the critical disordering temperature of 468°C. Measurements of impact hardness made over a range of temperatures and microstructural studies of samples deformed both rapidly and slowly over a range of temperatures, reported herein, should be of aid in reaching a more complete understanding of the underlying factors controlling the properties of the disordered body-centered-cubic material and the ordered material. It appears that such data have not

Jan 1, 1955

By J. H. Bechtold

Tensile properties of annealed molybdenum were investigated from 1000" to—200°C. In the vicinity of room temperature a well-defined transition in tensile properties occurs. Reduction in area decreases from over 80 pct to 0 pct and, simultaneously, the yield strength increases about 60,000 psi. MOLYBDENUM, tungsten, iron, and many other metals and alloys with the body-centered cubic and hexagonal close-packed crystal structures change from ductile to brittle behavior over some relatively narrow temperature range. The temperature at which this transition in ductility occurs depends on chemical composition, microstructure, and method of testing. When fine grained, completely recrystallized molybdenum of commercial purity is tested in uniaxial tension at a slow strain rate, the transition occurs at slightly below room temperature.&apos; Iron2 and tungsten3 tested under similar conditions become brittle at temperatures close to the boiling point of nitrogen, — 195°C and at about 200°C, respectively. A sharp change in ductility is uncommon in metals with the face-centered cubic crystal structure, however, a relatively sharp transi- tion in notched bar impact properties has been observed below room temperature in a face-centered cubic copper-antimony alloy.4 A transition from ductile to brittle behavior is usually explained by the concepts originally developed by Ludwik,5 and discussed and elaborated on by others including Orowan,6 Hollomon and Jaffe,7 and Gensamer8 In brief, there are two aspects to strength, first the resistance to flow and second the resistance to fracture. Both are functions of temperature, strain, strain rate, stress system, composition, and microstructure. With decreased test temperature the flow stress required to initiate plastic deformation increases more rapidly than the fracture strength and brittle fracture occurs at that temperature where the yield strength equals or exceeds a brittle fracture strength. This investigation was conducted to determine the effects of temperature, strain, and rate of straining on the flow and fracture strengths of molybdenum above, through, and below the ductile-to-brittle transition. Other variables were held constant during testing. This information is believed to show

Jan 1, 1954

By E. F. Bailey, L. S. Birks

The effect of stress on the austenite to ferrite transformation in carbon steel was studied by X-ray diffraction techniques. Tensile stress was found to cause reorienta-tion of austenite above the transformation temperature, to accelerate equilibrium conditions at the transformation temperature, and to cause precipitation of large carbides at a critical value of stress. IN the past, a number of papers&apos; have discussed the effect of stress on the austenite to martensite transformation at relatively low temperatures. In general, it has been shown that tensile stress induces some transformation at a given temperature, while compressive stress retards the transformation. Very little work has been reported on the effect of stress on the transformation from austenite to ferrite plus carbide near the A, point in steel. One of the few papers in the literature2 reports an increase in A1 of about 1°C in pearlitic steel upon the application of tensile stress. In this paper, the effect of tensile stress on eutec-toid steel at, and above, the A, point was studied in

Jan 1, 1956

By J. A. Snyder, W. L. Finlay

SEVERAL notable studies of the effects of sub- stitutional solutes have been reported. Outstanding among these for its elucidation of general principles, is the summarized work of Hume-Rothery and coworkers.1 For a systematic study of the effects of substitutional solutes on the mechanical properties of the solvent lattice, the work of Brick, Martin, and Angier² on copper; of Frye and coworkers³,4,5 on copper and silver; and of Lacy and Gensamer6 and of Austin7 on iron may be mentioned. Titanium is one of the few elements offering the possibility of a similar study of interstitial solutes since, unlike most metallic elements, it exhibits extended solid solubility for most of the interstitial solutes—hydrogen, boron, nitrogen, oxygen, and carbon. This paper reports a survey of the effects of dilute solutions of nitrogen, oxygen, and carbon on the mechanical properties of high-purity alpha titanium. Previous Work: Van Arkel and De Boer showed" that high purity titanium was quite ductile and De Boer, Burgers and Fast established".&apos; that not only were oxygen and nitrogen very soluble in solid titanium but that, long before the limit of solid solubility of either had been reached, these interstitial solutes rendered the metal brittle. Their electrical resistance data as a function of

Jan 1, 1951

By J. A. Snyder, W. L. Finlay

G. Edmunds—Solid solubility is considered to be of either the interstitial or the substitutional type. Is it possible, in a binary alloy as the simplest case, that some of the solute atoms are present in the normal lattice sites (substitutionally or filling lattice vacancies) while simultaneously others are in interstitial positionss One might even ask whether a distribution of the two types may be the normal situation. H. M. Meyer—Metastable states of interstitial atoms occupying vacant lattice sites possibly occur as well as of substitutional atoms squeezed in between regular matrix positions. However (as we know since Hume-Rothery), the solute atoms choose between the two kinds of solutions; consequently, every solute will be unequivocally either substitutional or interstitial in the equilibrium state of the solid solution. M. Balicki—In view of the fact that the authors apparently correlate the analysis of the alloys at the ingot stage with the properties exhibited at the testing stage, I would like to ask whether this is a fully justifiable procedure. In other words, how good are their determinations of solute concentration for correlating them with the mechanical properties. The answer to this question may explain some of the divergencies. Assuming good enough homogenization of the samples and exact determination of mechanical properties the position of the plotted experimental points will depend solely upon the accuracy of composition determination. If this is not accurate, say due to loss or pickup of elements during processing from the ingot to the testing stage, or due to a systematic error in the method employed for obtaining solute concentration data, the points will deviate from their true position and may align themselves along a different curve than the one expected. H. V. Kinsey—We have been studying the creep-rupture properties of titanium-base alloys at 1000°F. In the course of this work, anomalies in behavior of the alloys that would suggest that the material under test was becoming stronger as the test progressed have been observed. If this was so, the most likely explanation that we could think of was that the test bars were absorbing oxygen and nitrogen from the air during the test and were thereby becoming strengthened. In an attempt to determine the strengthening effect of absorbed oxygen and nitrogen the following experiment was conducted. A length of cold-rolled titanium was supplied by the E. I. du Pont Co. Two test bars, having a 1/4 in. diam gauge length, were prepared from this material. One bar was tested in the as-received condition. The second bar was heated in air at 1550°F for 100 hr and subsequently air cooled prior to testing. A testing temperature of 1000°F was employed. The results of these tests are tabulated in table 11. In the author&apos;s opinion, is it reasonable to assume that the bar that was exposed to air at 1550°F for 100 hr was stronger because it absorbed oxygen and nitrogen from the air during this heat treatment? W. L. Finlay (authors&apos; reply)—Direct experimental evidence for or against Mr. Edmunds&apos; interesting suggestion will probably never be available. It seems possible, however, that mixed interstitial-substitutional solid solution might well occur with interstitial elements. The less likely possibility of interstitial solution of a normally substitutional element like copper in aluminum was recently discussed at length by the

Jan 1, 1951

By A. R. Elsea, E. E. Fletcher

This paper describes a metallographic investigation of the influence of tungsten or molybdenum additions upon the transformation and precipitation reactions occurring in Co-rich Co-Cr alloys. It is shown that tungsten has little effect upon the a-ß transformation temperature range, while molybdenum tends to raise it. Both elements tend to promote the formation of ? phase, molybdenum being more potent in this respect than tungsten. HIGH temperature alloys, that is, alloys which have load-carrying ability at elevated temperatures, have been developed at an increasing rate during the past few years. This has resulted from the requirements in the design of modern aircraft engines. Although many alloys of this type are available, they have been developed on an empirical basis. Metallurgists do not have a clear understanding of the phases or structures that are responsible for these high temperature properties. In order to determine why these alloys possess this particular ability, a project was started at Battelle Memorial Institute with the object of learning more about the fundamental factors which promote high temperature strength in alloys. This study was to include a correlation of microstructure and the high temperature properties of Vitallium, an alloy which is widely used for high temperature service. Vitallium is a complex material both from the standpoint of composition and microstructure. Consequently, it was necessary to obtain informa- tion regarding the phase relationships in this alloy. The Co-Cr binary diagram was determined as the first phase of this investigation.&apos; A second paper described the effects of iron, nickel, or nitrogen on the reactions occurring in the Co-rich end of this system.&apos; The present paper covers a continuation of this investigation in which the effects of tungsten or molybdenum on the reactions occurring in Co-rich, Co-Cr-base alloys were determined. Preparation of &apos;rest Materials Two series of ternary Co-Cr-base alloys, representing Co-Cr ratios of 80:20 and 68:32 ( Cr x 100 =20 and 32 ) , were prepared containing ( Co + Cr = up to 6 pct W and up to 12 pct Mo. Melting stock consisted of electrolytic Co, electrolytic Cr, 99.9 pct pure W, and 99.9 pct pure Mo. Table I lists the chemical analyses of these materials. The melting furnace was a vertical porcelain tube

Jan 1, 1952

By Dell P. Williams, Howard G. Nelson

The tensile behavior of magnesium single crystals at a temperature of 26º ± 2ºC was investigated at varying pressure levels from 760 to 8 X 10-8 tow. For crystals deformed at a constant linear strain rate of 0.061 min-1. there was no apparent effect of the vacuum environment down to 10-8 torr. However, from a vacuum of 10-5 torr down to the lowest pressure attained (8 x 10-8 tor,), the effect of the vacuum environment was to increase the strain at the end of the first linear (or easy-glide) stage and to decrease the slope of this stage; the magnitude of this effect was found to be dependent on pressure. The slope of the second linear stage was also decreased at the lower pressure levels; however, this effect appears to be caused primarity by the vacuum effect on the first linear stage. The magnitude of the vacuum-environmrnt effect was also found to be dependent upon strain rate. The reduction in flow stress at 5 x 10-8 torr, as compared to the stress in air, was obserced to be about 10 pct for a strain rate of 0.0250 min-&apos; and 70 pct for a strain rate of 0.67 min-1. No systematic effect of pressure on the critical resolvled shear stress was observed. The data interpreted in terms of a modified form of Mott&apos;s work-hardening mechanism for hexagonal metals. It has long been known that surface conditions influence the mechanical behavior of materials. Roscoe 1 demonstrated the importance of surface conditions on mechanical behavior by testing cadmium crystals with oxide layers. He found that the "apparent" critical resolved shear stress for cadmium was increased approximately 2.5 times by the presence of an oxide layer 1000 atoms thick. The magnitude of this effect was dependent on film thickness with crystals having films less than 20 atoms thick still showing a definite increase. This observed strengthening could not be attributed to any strength of the oxide film because of 1) the thinness of the films and 2) an observed increase in the flow stress as deformation proceeded. Harper and cottrel12 obtained similar results on zinc crystals which had been etched and steamed to give artificially thick oxide films. However, in the course of this study, they also carefully examined the very early stages of plastic flow for zinc crystals which in one case had been electrolytically polished and in the other had been lightly etched to produce a thin film. They then found that the critical resolved shear stress for both surface treatments of the crystals was actually identical but that the etched crystal exhibited a much more rapid initial hardening rate. This had not been noted previously. This result indicated that, in fact, the film caused an increase in the stress for continuation of slip, rather than for the initiation of slip. Lipsett and King3 investigated the effect of evaporated gold films on the plastic behavior of cadmium single crystals. For large angles (=75 deg) between the specimen axis and the normal to the slip plane, they found that the stress-strain curve of the coated specimen always lies above that for a clean specimen. The shear strain at the end of the first linear stage was greater in clean specimens than in coated specimens and the slope of the second linear stage was

Jan 1, 1965

By Paul F. Sikora, John W. Weeton, Philip A. Clarkin

Effects of variations in carbon content and micro-structure on the stress-rupture properties of a liquid-phase-sirztered, Izeut-resistunt alloy were studied. Using the powder rnetallurgy technique, specimens could be produced having stress-rupture profierties equivalent to or better than those of the alloy in wrought form. In addition, sintered specimens were easily hot worked even when carbon contents were as high as I pct. Correlations between stress-rupture properties and micro structure were obtained in some cases. IT is well known that many alloys used in high-temperature service are quite complex both from the standpoint of chemical composition and microstruc-ture. During the development of these alloys their complexity has in some cases led to treatment schedules which, while practical, often do not fully utilize available alloying elements. For example, in some alloys, massive carbides that form during ingot practice may never be dissolved by reasonable solution treatments and therefore are unavailable for subsequent precipitation hardening, Ref. 1. This investigation was undertaken to determine whether the powder metallurgy method of consolidation might provide distinct advantages over the conventional melting method. First, segregation of alloying elements might be eliminated or reduced and thus a more efficient use of these elements obtained. Second, the structures produced in powder specimens might differ considerably from those normally seen in castings, which would perhaps result in better response to subsequent mechanical or thermal treatments. If these results could be achieved, it was felt that both forgeability and stress-rupture properties might be improved. The alloy used in this investigation was S-816 produced by powder metallurgy methods. The influence of carbon content over the range of 0.1 to 1.0 wt pct was studied for the alloy in the as-sintered condition and after three additional treatments involving heat treatment, hot swaging, and combinations thereof. EXPERIMENTAL Standard S-816 has the composition shown in Table I. It is a cobalt-base alloy having a nominal carbon content of 0.4 pct and is classified as a precipitation-hardening alloy. This alloy was chosen because it is representative of a class of heat-resistant alloys and because adequate information was available concerning its response to various treatments and its subsequent properties. For this study, -100 mesh alloy powder having essentially the same composition as shown in Table I but without the 0.4 pct C was used. Desired carbon variations, achieved by wet mixing the alloy powder with graphite, ranged from 0.1 to 1.0 wt pct. Specimens were hydrostatically pressed and then sintered in vacuum by slowly heating until incipient melting was observed. Sintering this way gave a liquid phase in the interstices of the powder particles and achieved reasonably high densities. The average density of as-sintered specimens was about 95 pct of wrought alloy density. In order to obtain various microstructures, some specimens were heat treated (solution treated for 24 hr at 2150°F, water quenched; aged 16 hr at 1400°F, air cooled); others were hot swaged at 2150 o F (50 pct reduction in area), while still others were hot swaged (50 pct reduction in area) and then given the above heat treatment. During hot swaging it was observed that forgeability was quite good even when specimens contained as much as 1.0 pct C. Specimens were evaluated by stress-rupture test-

Jan 1, 1962

By Leonard R. Weisberg

HE procedure of directional freezing by the Bridgman technique1 is frequently used in crystal preparation. On those occasions where the crystal is regrown, it can be advantageous to Crop part of the ingot before regrowth to achieve purification. This note describes some simple, yet interesting, observations concerning the effects of cropping an ingot between successive freezes. First, it is not effective to Crop the front end of an ingot, whether or not the distribution coefficient, k , of the impurities is greater or less than unity. This can be shown as follows. The concentration C, of an impurity in a directionally frozen ingot of length d with a uniform cross section is given by where x is the distance along the ingot, and C0 is the initial concentration per unit length. It is assumed in deriving this equation that diffusion is negligible in the solid, is complete in the melt, and that k is constant. Consider that a section of the ingot Ad is removed from the front end. Then the average impurity concentration in the remaining (d- Ad) section of the ingot can be shown by integration to be given by When the ingot is remelted and refrozen, the new impurity distribution is given by where xl is the distance along the refrozen ingot. Substituting the value of c into Eq. [3], one finds This is identical to Eq. [11 when x = (x, Ad), which represents the original impurity distribution in the (d - Ad) section of the ingot after the first directional freeze. Therefore, the cropping and re-freezing accomplished nothing. This can also be seen physically by realizing that the average impurity content in the melt after the first Ad section is frozen, is identical to that after the resulting ingot has been cropped and remelted. Hence, it is assumed in the following sections that only the tail end of the ingot is cropped. However, it must be realized that for impurities with k greater than one, the pieces cropped from the tail end are purer, and are therefore saved. After cropping an amount Ad from the tail end of an ingot, the average impurity concentration of impurities in the remaining portion of the ingot is given by wheref= d/d. For the case of k < 1, the purification is defined as c,/c. It is obvious from Eq. [5] that the purification increases asf increases, but the increase in purification is not large. For example, iff is doubled from 0.1 to 0.2, the purification increases by only 10 pct for k = 0.5, by only 24 pct for k = 0.1, and by 32 pct for k =0.01. Much smaller values off than 0.1 are not desirable since insufficient purification is achieved. These figures indicate that much larger values off do not lead to substantial improvement, especially considering that much of the original ingot is lost. Therefore, it is generally useful to Crop about 1/10 of the ingot to achieve purification. As compared to doubling the value off, it is much more helpful to remelt, refreeze, and crop the ingot twice. Using Eq. [51 reiteratively, and assuming f= 0.1, it is found that the purification after this process is found to be increased over the purification after a single freeze and cropping by 33 pct for k= 0.5, 450 pct for k = 0.1, and 4100 pct for k = 0.01. This indicates that considerable purification can be obtained by this procedure. However, if purification is the main goal, one should resort to zone refining,3

Jan 1, 1962

By J. F. Smith

ELASTIC constants of yttrium and eleven of the rare earth elements have been measured. This has been accomplished by measuring the propagation velocities of ultrasonic pulses. The velocity measurements were made by noting the elapsed time between an applied pulse and the appearance of successive echoes. The pulse-echo technique has become relatively common, and the basis of the measurement is outlined in several standard tests, e.g., Heuter and Bolt.1 Two important assumptions are made when using this method for the determination of elastic moduli. First, the pulse is assumed to propagate as a plane wave. To justify this assumption, the cross section of the test specimen should be large compared to the wave length of the transmitted pulse. For these measurements on the rare earth elements the minimum cross section wave length ratio was about 20. A second assumption which must be made when using polycrystalline specimens is that the grains are sufficiently numerous and randomly oriented so that the specimen may be approximated as elasti-cally isotopic. The grain size in the as-cast specimens which were used is believed to be sufficiently fine for this approximation, and the degree of preferred orientation is believed to be small. Supporting this viewpoint is the fact that elasticity measurements by the pulse-echo technique on as-cast specimens of other metals give results which are in satisfactory agreement with values obtained by other techniques. Hence, it is believed that the measured elasticity values for the rare earth elements are not apt to be seriously in error due to the assumption of elastic isotopy. The apparatus used in this determination was a modified Sperry Reflectoscope with a precisely calibrated time base circuit. Piezoelectric transducers were used both to generate the pulse and to detect the echoes. X-cut quartz crystals were used for the longitudinal modes, and Y-cut quartz crystals were used for the shear modes. Frequencies of 2.25 and 5 megacycles per sec were employed. Most of the specimens were 2.5 to 5.0 cm in length. Results Table I is a tabulation of the measured propagation velocities of longitudinal waves and of shear waves, together with densities obtained by Sped- ding, Daane, and Herrmann2 from lattice parameter measurements. The shear modulus, Poisson&apos;s ratio, and Young&apos;s modulus were calculated from the data in Table I through use of the following relationships: µ = pv32 [1] s=2-(vb/vs)2/2[1-(vb/vs)2] [2] and Y= 2µ(l+s) [3] where s is the shear modulus, Y is the Young&apos;s modulus, s is Poisson&apos;s ratio, p is the density, V0 is the longitudinal wave velocity, and v, is the shear wave velocity. The calculated quantities are shown in Table 11. Compressibility values can be computed from the relationship and the computed values may be compared with measured values obtained by Bridgman.8 Table III lists the data for such a comparison. The agreement is satisfactory, being particularly good for neodymi- um and gadolinium, poor for samarium, and intermediate for the other elements. Some variation is expected since Bridgman&apos;s measurements are isothermal, whereas the present measurements are adiabatic. In addition there may be some effect due to small variations in purity. Though most of the rare earth metals measured by Bridgman and all of the metals used in the present measurements were prepared at this laboratory, minor purity variations might exist since the samples came from different lots. Also, any imperfections such as dislocations, vacancies, voids, grain boundaries, microcracks, etc., should contribute to the volume change of a com-

Jan 1, 1958

By R. J. Wasilewski

The variation of elastic modulus with terrzperature between -150° and 600°C has been investigated. Compounds close to equiatomic cornposition exhibit very low modulus values and very high damping near room temperature. The modulus rises steeply with both decreasing and increasing temperature. The modulus minimum and the high damping are believed to be connected with a martensitic transformation of TiNi. In bulk material this transition takes place slightly above room temperature quite rapidly and reversibly, with a hysteresis of some 30°C, depending on the Ti:Ni ratio. Oxygen impurity affects the reaction time. THE inter metallic compound TiNi has been reported to exist in an ordered CsCl (B2) structure,l-6 the homogeneity range varying rather markedly with temperature.7 Some investigators reported this compound to decompose peritectoidally to Ti2Ni and TiNi, between 650° and 800°C,3 or below,&apos;,g the latter workers also suggesting the decomposition to be strain-sensitive. Purdy and Parr were the first to report a structural transformation to a new, possibly hexagonal, structure at 36°C,7 a temperature indubitably too low to allow the significant amount of diffusion necessary for a peritectoid reaction. Mechanical-property investigations of compositions close to TiNi just above room temperature have qualitatively shown remarkable anomalies, particularly with respect to clamping,&apos; and to a "memory" effect, that is, plastically deformed material returning to its original shape on being heated through the "decomposition" temperature.9 The original explanation of this effect—based on the apparent experimental observation of Ti2Ni or TiNi, formation in the material subjected to tensile or compressive stresses, respectivelp—does not appear plausible. It appeared more probable that the change involved may be a martensitic, diffusionless structural transformation, similar to those observed in other B2 structures such as 0 brass,&apos;&apos; AuCd,ll and AuZn.12 The existence of such transformation has been established recently,&apos;, although the symmetry of the low-temperature structure is not yet known. The present paper describes the elastic modulus and damping behavior of polycrystalline TiNi in both structures. EXPERIMENTAL METHOD 1) Specimens. All the specimens to be investigated were prepared from premelted electrolytic nickel and iodide titanium by nonconsumable arc melting and casting in a water-cooled copper mold. The cast billets were canned in mild steel, extruded, and swaged to approximately 0.375 in. diam. The cans were then removed by pickling or machining. Preliminary material balance checks indicated no significant weight losses on melting (less than 5 mg on a 50-g button); hence nominal compositions have been used throughout. In agreement with previously reported observations7 no single-phase material was obtained at—or close to—Ti 1.00 Ni1.00 a small amount of finely divided second phase always being present. It was found that most of the oxygen impurity was associated with this minor phase, which was identified as oxygen-bearing Ti2Ni—possibly Ti,Ni,O. The amount of this phase—at any given Ti:Ni composi-

Jan 1, 1965