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By H. I. Aaronson, S. M. Kaufman, G. M. Pound

WHETHER the carbides associated with bainite precipitate from the ferritic component of bainite, as originally suggested by Davenport and Bain, or from the adjacent austenite at aus-tenite:ferrite boundaries, as proposed by Hultgren, 2 remains in dispute.3-5 A recent metallographic investigation in this laboratory has shown that the bainitic carbides formed in a plain carbon hypo-eutectoid steel nucleate entirely within ferrite at higher reaction temperatures3 and in both ferrite and austenite at lower temperatures." The present investigation was undertaken to ascertain the effects of alloying elements on the nucleation sites selected by bainitic carbides. The compositions of the steels studied were as shown in Table I. Specimens of these steels were

Jan 1, 1958

By J. F. Gallie

From the standpoint of exploration and new discoveries, South Arkansas had a discouraging year in 1944. In January there were 73 untested drilling blocks, and 60 additions were made during the year. Of the total, 65 were condemned by dry holes on or adjacent to them, while 5 proved productive. The latter resulted in the discovery of the Salem Church, Calhoun Wilks, and Strong fields, and the extension of the Village field to the southeast. The year ended with 63 untested blocks, 41 of which were scheduled for tests to the Smackover lime, the state's deepest oil-producing formation. Geophysical activity in 1944 totaled 164 crew weeks, of which 110 were seismic, 43 gravity, and 11 radioactive (Fig. I), in contrast with 674 crew weeks reported for 1943, of, which 563 were seismic and in gravity, Five seismograph and two gravity crews were engaged in exploration in South Arkansas during January 1944. but only two seismograph crews were working there at the end of the year. In addition, exploratory core drills were used for a total of 38 weeks during the year. The year's few discoveries, none of which is considered as having added appreciably to state reserves, were the meager results obtained in the drilling of 62 wildcat wells 2000 ft. or deeper. Of this total (a detail of which appears in Table 2), 42 were drilled to the Smack-over lime or below, The average depth of the 62 wells was 5384 ft., as compared with 4992 ft. in the preceding year, while the average depth of the 42 wildcats in the lime was 5913 ft. in 1944. Fig. 2 has been prepared to show all , wells penetrating to the Reynolds oölitic lime. The 1944 dry holes are circled lightly, while discoveries are heavily circled and shown as producers. Smackover lime fields, producing from the Reynolds oolitic lime member, are indicated in black, and the locations of dry wildcat wells drilled prior to 1944 are also shown. Table 3 provides a listing of all Smackover lime wells drilled through the end of 1944. Production for the year was slightly more than in 1943, totaling 29,282,747 bbl., as compared with 27,521,943 bbl. for the preceding year. The increase was 1,760,804 bbl., or 6.4 per cent, bringing production to a peak exceeded only in the 1923 to 1928 period of flush production from the older shallow fields, principally Smackover. The increase was largely attributable to additional development in the Dorcheat-Macedonia, Atlanta, Fouke, Stephens-Smart, Haynesville, and Village fields, little production deriving from 1944 discoveries. These six fields accounted for loo of the 122 field wells drilled during the year. Annual and cumulative production for the producing life of the state are presented graphically in Fig. 3. Fig. 6 has been prepared by the author to show the producing ages and present known productive limits of all fields in South Arkansas. Production data, as usual, are assembled in Table 2, and provide a further breakdown of producing formations in the individual fields.

Jan 1, 1945

By C. A. Bruch, J. F. Duffey

On the basis of metallographic and cooling-rate studies of 15 U-Zr alloys, a new version of the 6 phase region of the U-Zr phase diagram is proposed. IN several published diagrams of U-Zr alloy system:' there is good agreement that at elevated temperatures complete solid solubility exists between y uranium and ß zirconium. Similarly, there is reasonably good agreement concerning the uranium-rich and zirconium-rich ends of the diagram. However, there is no agreement concerning the nature of the diagram at intermediate compositions and at temperatures below about 650°C. The early work of Saller et al.8 hows an intermediate phase, 6. In a later diagram by Saller and Rough' shown in Fig. 1, the d phase field is drawn with dotted lines, indicating doubt that this phase exists. The diagram of Summers-Smith2 does not show the d phase. More recently Holden and Seymour' have shown that in the composition range 40 to 60 wt pet Zr, the high-temperature ? phase, which is body-cen-tered-cubic, transforms to an ordered structure, 8. They found that the order-disorder transformation occurs between 595° and 610°C, and presented a diagram based on the study of four different alloy compositions. Most recently Saller et a1.5 presented a new diagram which differs with respect to the composition limits of the 8 field from the others proposed by these authors. The purpose of the present investigation was to determine the boundaries of the d phase field. Experimental Procedures and Results Alloys—Buttons, weighing 80 g of 15 different alloy compositions were prepared by arc melting Mal-linckrodt uranium and iodide-process zirconium in a water-cooled crucible. A controlled atmosphere of argon and helium was maintained in the furnace. Prior to making each button, a sacrificial button of zirconium was melted to increase the purity of the furnace atmosphere. Each alloy was then melted six times to improve its homogeneity. Subsequently the alloy buttons were jacketed in copper and hot rolled to slabs at 775°C. From these slabs, specimens were machined for chemical, thermal, and metallographic analyses, Table I gives both the estimated chemical composition of the alloys, and the values which were obtained by analysis. The oxygen contents varied from 0.013 to 0.032 pet, nitrogen from 0.0014 to 0.014 pet, and carbon from 0.0013 to 0.011 pet. The purity of the alloys ranged from 99.947 to 99.975 pet. Thermal Analysis—The specimens for thermal analysis were blocks 11/4 x 1/4 x % in. The bead of a calibrated thermocouple was placed between two of these blocks and molybdenum wire was wrapped around the assembly. Each assembly was sealed in a quartz capsule having an argon atmosphere. The capsule was placed inside a refractory crucible which was heated in a furnace. Using a method described by Smith,' the emf of a differential thermocouple, with junctions inside and outside of the refractory crucible, was used to activate the

Jan 1, 1959

By S. W. Kennedy, M. Cohen, L. D. Calvert

A high-temperature X-ray diffraction method has been used to study the composition and the kinetics of formation of oxide scales at 800 °C on iron and pure iron-nickel alloys containing 25.6, 75, and 84 pct Ni. This technique has been combined with chemical analysis, and metallographic examination, and determination of weight-gain time curves. The 75 and 84 pct Ni alloys form a three-layer scale consisting of porous NiO next to the metal, a spinel layer, and a -Fe203 on the outside. The 25 pct Ni alloy produces a scale of spinel and Fe,O,, in which, however, traces of FeO and NiO are observed near to the metal. On all the nickel alloys the Fe20, is orieqted with the (107) plane parallel to the surfaces. The exposed surface of the Fe20, is in the form of needles whose axis is perpendicular to the specimen surface. Although the alloys show nonuniform oxidation rates as determined from weight-gain measurements, the X-ray data indicate that the total scale and individml scale layers grow uniformly and parabolically. Deep subscale formation is observed in the 25 pct Ni alloy only. This appeared to be associated with cracking of the scale and penetration of the oxygen along the grain boundaries. ALTHOUGH film formation has been investigated by high-temperature electron-diffraction techniques, for example by Gulbransenl and Hickman,' there have apparently been no investigations of scaling by methods permitting study of the scale during formation at the reaction temperature. Methods involving quenching of scales are based on the working assumption that no significant changes take place on cooling. In general, however, compounds may disproportionate, and the different thermal expansions of constituents may cause disruption of the scale on cooling. In particular, some scales cannot be quenched without spalling. These difficulties are avoided by X-ray diffraction examination at the temperature of formation. High-temperature diffraction procedures also provide a method of determining the kinetics of formation of each phase separately in a multicom-ponent scale. The scaling of binary iron-nickel alloys Containing up to 30 pct Ni at a temperature of 800°C has been studied by Benard and Moreau using cooled specimen~,~ whilst Foley, Druck, and Fryxel14 made an electron-diffraction study of cooled oxide films formed on an iron 42 pci Ni alloy. In the present work the scaling of three iron-nickel alloys containing 25.6, 75, and 84 pct by weight of nickel, at 800°C in oxygen at atmospheric pressure was investigated by X-ray diffraction techniques using a Norelco Geiger-counter diffrac-tometer. The oxidation of iron was investigated for comparison. In addition normal metallographic examinations and chemical and X-ray analyses were made, and weight-gain time curves obtained. EXPERIMENTAL Materials Used—The analyses of the alloys were as follows: Percent by Weight Nickel 25.6 pct 75.4 pct 83.2 pct Aluminum 0.004 None found 0.002 Cobalt — 0.05 0.05 Chromium — — — Silicon — 0.01 None found Carbon All less than 0.05 pct The chemical analysis of the iron was: Al— 0.002 i 0.001 pct, C—0.007 pct, Cr less than 0.001 pct, Cu—0.002 ± 0.001 pct, Mn—0.003 ± 0.001 pct, N—0.0002 pct, 0-0.013 pct, P—less than 0.0002 pct, Pb—not detected, S—0.0017 pct, Si—0.0095 pct, Sn—none detected. This iron was the same as that used to make the alloys and was obtained from the same source-Vacuum Metals Corp. One specimen of pure iron from The British Iron and Steel Research Association was used for preliminary investigation. Specimens were machined to shape from cast rod, polished (the final polish being with 600 Sic paper), degreased in trichlorethylene, washed, and etched. The etching and neutralizing procedure adopted by

Jan 1, 1960

By C. S. Westerberg, C. P. Heiner

Observation of the clinkering action of coal from the Castle Gate D seam in underfeed stokers over a period of years has given rise to the present investigation of the effect of bony coal on clinkering. Some very costly examples of slagging clinkers in particular cases have been of especial interest to the authors. In such cases coal analyses and ash-softening and fluid temperatures have been found of little value. In general, it was noted that slagging mas accompanied by a somewhat higher ash content of the stoker slack, and the suspicion naturally arose that foreign matter was the troublemaker. One would naturally suspect bony coal and rock impurities because of their occurrence and prevalence within the seam and the relative absence of sulphur or other impurities in the coal mined. The test results given herein indicate that the concentration of the bony coal and rock impurities in the coal determines the clinkering tendencies of the ash during combustion. Castle Gate D Seam Extending from the Utah-Colorado line near Grand Junction, Colo., westward to Greenriver, Utah, and thence in semicircular form north and westward to Castle Gate, and from there southward to Mt. Hilgard in central Utah, is a line of nearly perpendicular cliffs, composed of interbedded massive sandstone and shales, making up the coal-bearing horizon of the Mesaverde formation of Upper Cretaceous age. The cliffs face roughly concentrically toward the south and southeast and the strata, with conformably enclosed coal beds, gently dip away from the face of the cliffs and at right angles to their front line. Back of these cliffs the mountain masses rise to an altitude of from 8000 to 10,ooo ft. above sea level. Stretching away from their foot is a great shale plain, on which the towns are situated and over which the railroad lines and highways run. The Castle Gate mines enter the coal beds at their outcrop; the workings extending within a particular coal bed away from the outcrop and under the mountain mass back from the cliff line (Fig. I). Throughout the Mesaverde formation in the Castle Gate general area, there are from two to five workable coal beds. Usually not all of these are coincidentally of workable size and merchantable quality throughout any given large tract. In the Castle Gate mine area, the base of the Mesaverde horizon and coal measures is marked by a massive, cliffmaking, gray sandstone bed 60 to 80 ft. thick. Locally this is referred to as the "Castle Gate sandstone floor." Frank R. Clark, in U. S. Geol. Survey Bull. 793, designates it as the "Aberdeen sandstone." At Castle Gate the various coal beds are designated by the letters A, B, C, etc., commencing with the lowest bed.

Jan 1, 1942

By C. P. Heiner, C. S. Westerberg

Observation of the clinkering action of coal from the Castle Gate D seam in underfeed stokers over a period of years has given rise to the present investigation of the effect of bony coal on clinkering. Some very costly examples of slagging clinkers in particular cases have been of especial interest to the authors. In such cases coal analyses and ash-softening and fluid temperatures have been found of little value. In general, it was noted that slagging mas accompanied by a somewhat higher ash content of the stoker slack, and the suspicion naturally arose that foreign matter was the troublemaker. One would naturally suspect bony coal and rock impurities because of their occurrence and prevalence within the seam and the relative absence of sulphur or other impurities in the coal mined. The test results given herein indicate that the concentration of the bony coal and rock impurities in the coal determines the clinkering tendencies of the ash during combustion. Castle Gate D Seam Extending from the Utah-Colorado line near Grand Junction, Colo., westward to Greenriver, Utah, and thence in semicircular form north and westward to Castle Gate, and from there southward to Mt. Hilgard in central Utah, is a line of nearly perpendicular cliffs, composed of interbedded massive sandstone and shales, making up the coal-bearing horizon of the Mesaverde formation of Upper Cretaceous age. The cliffs face roughly concentrically toward the south and southeast and the strata, with conformably enclosed coal beds, gently dip away from the face of the cliffs and at right angles to their front line. Back of these cliffs the mountain masses rise to an altitude of from 8000 to 10,ooo ft. above sea level. Stretching away from their foot is a great shale plain, on which the towns are situated and over which the railroad lines and highways run. The Castle Gate mines enter the coal beds at their outcrop; the workings extending within a particular coal bed away from the outcrop and under the mountain mass back from the cliff line (Fig. I). Throughout the Mesaverde formation in the Castle Gate general area, there are from two to five workable coal beds. Usually not all of these are coincidentally of workable size and merchantable quality throughout any given large tract. In the Castle Gate mine area, the base of the Mesaverde horizon and coal measures is marked by a massive, cliffmaking, gray sandstone bed 60 to 80 ft. thick. Locally this is referred to as the "Castle Gate sandstone floor." Frank R. Clark, in U. S. Geol. Survey Bull. 793, designates it as the "Aberdeen sandstone." At Castle Gate the various coal beds are designated by the letters A, B, C, etc., commencing with the lowest bed.

Jan 1, 1942

By Charles Smeal, Robert J. Schafer, Max Quantinetz

Normally metal powders cannot be ground to sub-micron sizes because of welding and agglomeration phenomena. Through the use of selected grinding aids and grinding fluids, nickel and other metal powders have been ball-milled as fine as 0.1 It was found that certain inorganic salts are more effective grinding aids for metal powders than conventionally used surfactants. METAL and alloy powders are used to produce reagents, pigments, coatings, solders, brazes, and parts for industry by powder metallurgy techniques. They are also combined with refractory compounds to produce cermets and dispersion-hardened products. One of the interests at the Lewis Research Center has been to explore the potentialities of the dispersion strengthening process. Since the work of Ir-mann, many investigators have shown that the strength of dispersion-hardened products may increase with decreasing interparticle spacing.24 One approach to achieving small interparticle spacing is to combine fine refractory compounds and metal powders, preferably below 1 in size. In attempting to obtain fine metal powders, it was found that until very recently the best that could be obtained from commercial suppliers, particularly of ductile metals, was about 1.0 . Interest was therefore developed in providing finer metal powders for dispersion-hardening studies. Information obtained from the literature, from others working in the field, and from prior experimental work performed at NASA, led to a consideration of ball-milling as a technique to produce the desired materials. Some of the variables associated with ball-milling are the size, material, and nature of construction of the grinding container; the nature and amount of the grinding material and material to be ground; and the nature and amount of the grinding liquid and grinding aid, if employed, and the grinding time. In all ball-milling, welding and agglomeration can oc- cur as well as grinding. Because of the tendency of ductile metals to weld together, they are difficult to grind.5 The ultimate particle size obtained on grinding is generally the one at which the rate of grinding becomes equal to the rate of welding. To help delay welding and thus obtain smaller particle sizes, grinding aids are often employed. The principal objective of this investigation was to produce submicron metal powders by ball-milling the powders with selected grinding aids and grinding fluids. A secondary objective has been to attempt to explain the variations observed in grinding behavior by considering possible grinding mechanisms and correlating various parameters with grinding effectiveness. Three groups of ball-milling experiments were run; one in which the grinding aid was varied, a second in which the grinding fluid was varied, and a third in which the material being ground was varied MATERIALS, APPARATUS, AND PROCEDURE In the first group of experiments in which the grinding aid was varied Inco Carbonyl Grade B nickel powder initially 2.5 (all sizes refer to average particle size as measured by Fisher Sub -sieve Sizer) was used as the material being ground and 200-proof ethyl-alcohol as the grinding fluid. Surfactants, representative of typical organic structures, were selected as grinding aids. Inorganic salts used as grinding aids were chosen on the basis of the size and valence of their ions. Water soluble salts were used in order to facilitate their removal from the slurry after grinding. In the second set of experiments, grinding of the 2.5- Ni powder was tried in four different grinding liquids; water, cyclohexane, n -heptane, and methy-lene chloride. In this study seven grinding aids selected from those tried in the first group of experiments were employed. In the third group of experiments 200-proof ethyl alcohol was again used as the grinding fluid to mill Cu, Cr, Fe, Ag, and Ni powders of various initial particle sizes' All mill charges contained 300 ml of grinding liquid and 3000 g of 1/2 in. stainless steel balls. When inorganic salts were used as the grinding aid, 70 g of salt and 210 g of metal powder were employed, and with surfactants 6 g of grinding aid and 300 g of

Jan 1, 1962

By R. J. Stoehr, F. Howell

Since the ore mined in the Grants-Ambrosia Lake uranium area is taken from a water-saturated sandstone formation, part of the milling operation includes a drying process. The authors discuss the merits and disadvantages of two methods: natural drying and mechanical gas-fired drying; operating and cost data are included. In the Grants-Ambrosia Lake uranium area, approximately 7000 tons of ore are mined each day from a water-saturated sandstone formation. This ore is sampled and treated at four separate milling operations. Prior to the design and initial construction of the milling facilities, very little was known as to the physical properties of the ore which would be handled in the sampling and crushing facilities at the mills. All four mills initially were constructed without ore-drying facilities. As mining proceeded, it was determined that, even after drying the ore in place by use of drainage development underground, the moisture content of the ore as hoisted averaged approximately 18 pct. Actually, some of the mines produced ores which resembled cream-of-wheat in character and had a moisture content in excess of 24 pct. Each of the four mills had a differently designed sampling and crushing plant; therefore, the moisture content of the ores had varying adverse effects upon the operation of the plants. It was determined after some experience that most of the sampling and crushing facilities could not economically handle ore if the moisture content was greater than 10 pct—one operator considers 12 pct moisture as a maximum. In all of the plants, moisture content over 8 pct increases costs to some extent. In addition to the added sampling and crushing costs, some of the mills were located 15 to 20 miles from the mines and the high moisture content of the ores increased the haulage costs from the mine to the mill. It was generally conceded that it was necessary to employ some method to reduce the moisture content of the ore prior to sampling. Several methods were considered: 1) natural drying at the mine site, 2) mechanical gas-fired drying at the mill site, 3) mechanical gas-fired drying at the mine site, 4) radiant heating on concrete clabs, and 5) infrared shed drying. After preliminary investigation all possibilities but natural drying and mechanical gas-fired drying at the mill site were eliminated. NATURAL DRYING A cooperative feasibility study was conducted on the natural drying method. This study indicated the following: 1) During summer months May through September, ore piled 4-ft deep would dry from +20 to +10 pct HzO in 30 days with no mechanical turning. 2) In the first four days after piling a reduction of 5 to 7 pct total moisture content was accomplished by drainage and absorption of the water into the underlying ground on which the ore was piled, providing the ground surface absorption rates approached 10 gal per sq ft per day. After the first four days the decrease of moisture caused by drainage was practically nonexistent. 3) In the summer months drying by evaporation amounted to approximately 0.1 pct decrease in total moisture per day and mechanical turning of the ore could increase this as much as three times. 4) Climatic conditions of the area indicated that: a) Air temperatures averaged 64' May, June, July, August, September; 41" October, November, December, March, April; 31" January, February. b) Average rain fall was 10 in. with 40 pct of this occurring during July and August. c) Only on very rare occasions were there over five consecutive days with below freezing temperatures. d) The annual evaporation rate was approximately 75 in. On the basis of this study, two of the mill operations decided to attempt to meet the moisture specifications by natural drying supplemented by mechanical turning. The other two operations decided upon rotary gas-fired drying at the mill site. The natural drying method has been quite successful in practice. The ore running approximately 18 pct moisture is trucked from the head frame and piled in rows about 6 ft wide, 3 1/2 ft deep, 5 feet apart during the months of May through September. In approximately 30 days this ore will

Jan 1, 1961

By S. L. Couling, G. W. Pearsall

MOTT and Hainesl have summarized the available techniques for the examination of aluminum and some anisotropic metals under polarized light. Many of these techniques are rather complicated and cumbersome. This note presents a simplified procedure for using polarized light to obtain information about the crystallographic orientation of any particular grain in a magnesium alloy. Since other hexagonal metals are more anisotropic than magnesium, similar methods might well be applied to them. Ernst and Laves2 produced a double-refracting layer on magnesium alloy specimens by SuCCeSSiVe etches in solutions of perchloric acid in alcohol, magnesium perchlorate in perchloric acid and alcohol, and calcium and magnesium carbonates in water. They examined their specimens under polarized light and were able to determine the direction of the hexagonal axis in any particular grain from a measurement of the extinction behavior of that grain. The disadvantages of their technique were the complexity of the etching procedure and the explosive hazard of the perchloric acid-alcohol solutions. Results equivalent to those of Ernst and Laves were obtained in this investigation after etching specimens for 6 to 8 sec in an acetic picral solution containing 100 parts 6 pct picral, 10 parts distilled water and. 5 parts acetic acid. A. similar etch has been used by George3 in earlier metallographic

Jan 1, 1958

By William L. Batt

FROM the time the Japs overran the Far East, the United Nations faced a serious military problem in the critical shortage of many raw materials desperately needed to prose¬cute the war on two fronts. For many months this critical shortage threatened substantially to limit the gigantic effort to get shooting equipment into the hands of the fighting men on the far-flung battle lines. Now this crisis has been met. Solvency in raw materials has been achieved. Simply stated, this job of producing solvency has been done by "cutting cloth to fit the garment." This does not mean that we have all the raw materials we need. Unfortunately, a few raw materials are still short, thereby limiting the total production of certain war goods, or making these goods less effective. Where the supply of raw materials is known to be limited, however, substitutions have been made or production schedules have been geared to the amounts available, and an over-all balance has been achieved between various parts of the war-production program.

Jan 1, 1943

By P. Gobin, J. Perez, P. Peguin

The strain-amplitude- dependent part of the internal friction of alluminum after several ther momechanical treatments has been measured in the I-cycle range and at the ambient temperature. The internal friction in the outer layer of the torsional specimen us stress is computed from the experimental data. The curues obtained are analyzed in tevnzs of u coirzbinntion of AH and p, which aye, respectively, due to the vecersible unpinning from weak pills and to the plastic strain. Considerirlg the notion of thermally activated unpinning and repinning, it is shown that in our experimental conditions tlze dislocation lines acl as in the H model of Granato and Liiclze. It is also seen that the internal friction p which appears at higher- strains call be described by a simple expression which is in good agreement with our results. A qualitative interpretatiorz is proposed by combining these new types of intelpnal fviction. We define the internal friction 6 as half the ratio of the dissipated energy aW during one cycle to the maximum supplied strain energy W of a material submitted to a periodic stress. Experiment and theory show that internal friction varies with stress above a critical value.' Below this value the internal friction is strain-amplitude-independent and is often masked by an experimental background; so we shall call it AB. ~bove this critical value, the internal friction is strain-amplitude-dependent. This quantity is usually called aH:' and it can be explained as a thermal unpinning of dislocations.3-6 Furthermore, at higher stresses, a rapid increase of internal friction appears. This phenomenon could be caused by the plastic strain,' so we shall call it Ap. It seems interesting to us to study the influence of several t her momechanical treatments on the curve internal friction 6 vs strain E, in order to study the variation of AH and p with the concentration and the repartition of linear and point defects. In order to try to explain the results obtained, we shall propose and discuss models for H and hp and shall show that we obtain a combination of these two types of internal friction. 1) EXPERIMENTAL PROCEDURE 1) Preparation and Treatment of Specimens. We

Jan 1, 1968

By K. M. Rolls, J. Wulff, D. A. Colling

Solid-solution alloys of the Ta- Ti system containing up to 70 at. pct Ti were melted and fabricated into wire. Steady magnetic-field measurements of cold-worked wires at 4.2°K indicate that the resistive critical field increases smoothly with increasing titanium, reaching a maximum of 93 kG (J = 1 amp per sq cm) for a composition of about 50 at. pct Ti. The composition dependence of the resistive critical field indicates it is largely paramagnetically limited for alloys containing more than 35 at. pct Ti. For cold-worked wires the value of the critical current density, Jc , was found to be insensitive to composition changes for compositions in excess of 20 at. pct Ti. It was observed that Jc could be increased by final-size heat treatment at 400°C without altering the value of- the resistive critical field. Experimental data are used to calculate the electronic specific-heat coefficient and the "upper critical field" for the alloys studied. THE effect and importance of metallurgical structure on superconducting properties have been summarized by Livingston and Schadler.1 Specific work on solid-solution alloys such as Nb-zr2-7 and Nb-Ti5-7 have shown that critical current density (Jc) and superconducting transition temperature are structure-sensitive. Berlincourt et al.6,8,9 in their studies of transition-metal alloys find that Ta-Ti alloys remain superconducting at fields comparable to Nb-Ti alloys. 6,8 Transverse critical current tests of a Ta-10 at. pct Ti alloy10 and longitudinal critical current tests of a Ta-25 at. pct Ti alloy1' indicate that such alloys are capable of carrying high currents at intermediate fields (-40 kG). The work reported in the present paper was undertaken to explore the superconducting properties of further compositions in the Ta-Ti alloy system as well as the structure sensitivity of the superconducting properties. I) EXPERIMENTAL PROCEDURE Alloys were prepared by melting tantalum (Fansteel Metallurgical Corp., 99.96 pct purity) and iodide, crystal bar titanium (Foote Mineral Co., 99.92 pct purity) mixtures in an arc furnace on a water-cooled copper hearth using a tungsten electrode. Melting was accomplished in a purified, gettered argon atmosphere at pressures from 250 to 400 Torr. Each alloy was turned and remelted fourteen times to assure complete mixing of tantalum and titanium. Ex- cessive coring in the cast samples was, nevertheless, observed. This was somewhat reduced by annealing in vacuo at 1000°C for 13 hr. The ingots were then machined to 0.250 in. diam, jacketed in Type 304 stainless-steel tubing, and swaged to 0.140 in. diam. They were then drawn to 0.010-in.-diam wire. Alloys containing up to 70 at. pct Ti were readily cold-drawn to wire in this manner. Later experiments showed that oxygen additions up to -3000 ppm could also be cold-worked into wire. Test samples for superconductivity measurements in the 2-in, air-core Bitter solenoids of the M.I.T. National Magnet Laboratory were prepared from 10-in. lengths of 0.010-in.-diam wire, cleaned of residual wire-drawing lubricant. Current contacts were made by clamping clean copper tubing over both No. 18 current lead wire and the ultrasonically indium-tinned ends of the specimen wire.12 Potential leads of No. 32 copper wire were connected to the specimen by ultrasonic soldering in an indium bath. The potential lead separation was about 4 cm, corresponding to the circumference of the Bakelite rod to which the wire was affixed with half-mil Teflon tape. The final specimen configuration is shown in Fig. 1. Specimens were lowered into a liquid helium bath (4.2oK) in a double solenoid dewar and positioned so that the maximum magnetic field was oriented transverse to the wire axis of the gage section. Measurements were made by passing a current through the specimen at a preset solenoidal magnetic field. The current was increased until a 1-pv potential difference appeared across the gage section (1/4 µv per cm). At low magnetic fields, however, it was not possible to use this criterion because power-dissipation difficul-

Jan 1, 1967

By F. Weinberg

Measurements have been made of solute segregation during dendrilic growth by using radioactive solute elements and ,measuring the activity of den(12-ites cut from decanted specimens. This has been done for both lead awl tin based binary alloys contaitzing the following solute additions: Ag, T1204, was dependet on ko, the equilibrium distribution coefficient in the following way Fay k &apos;c 0.1, C/C 0.6; for k0 >0.1. 0.6 <c,/c,< I. Qualitative obse?-vations were madc of dendritic segregation, by using autoradiographic techniques, for the Sn + Ag110 and Sn + Tlo4 systems. The observation were found to he in general agreement with the measurements ofCA/Co. Autoradiographic were also obtained of scctiolccl delzr11-iie stalks. These indicated that the stalks had a substructure, dclileated by solute corzetlt?atio?zs nlolg the substructure walls. A new dendrite growth direction <JI2> is reported for tila. SOLUTE segregation in dilute binary alloys has been investigated by Pfann,&apos; Smith, Tiller, and Rut-ter,&apos; and others. They considered the case of a slowly advancing plane solid interface, and derived expressions for the distribution of solute in both solid and liquid during solidification. To determine these expressions, they assumed no diffusion in the solid and either complete mixing in the liquid:&apos; or diffusion controlled solute movements in the liquid without any convective mixing.&apos; The present investigation considers solute segregation during dendritic growth, in which case the solid-liquid interface is not plane, and the growth rates are rapid. Segregation under these growth conditions has not been treated mathematically, because of the relative complexity of the system. It has been suggested by Chalmer, on the basis of preliminary results, that an alternative to the diffusion and heat flow controlled conditions during growth is &apos;diffusionless" dendritic growth in which solid is formed with the same composition as the liquid. He suggests this type of growth may depend upon a solvent-solute relationship that permits some solid solubility without excessive increase in internal energy, as is the case for solutions of tin in lead. On the other hand, Montariol,4 and others, have shown experimentally that some segregation does occur during dendritic growth in metals using etching and radioactive tracer techniques to indicate the concentrations of the solute. The present investigation was undertaken to determine, both qualitatively and quantitatively, the extent of solute segregation associated with dendritic growth in a series of binary alloys, as a function of solute concentration. PROCEDURE The solvent materials used were Vulcan Electrolytic tin (99.997 pct purity) and Tadanac lead (99.998 pct purity). The solute materials were Zn, Sn, and Sb (better than 99.998 pct purity), Ag and Co (99.5 pct purity), and T1 (Fisher "purified" metal sticks). Activation of the solute metals was carried out in the reactor at Chalk River, Canada. Master alloys were prepared by induction heating from the radioactive solute metal and the pure solvent, under argon, in graphite crucibles. Pieces of these alloys were then added to the solvent to give the required solute concentration. Dendrites were grown in essentially the same manner as that described by Weinberg and Chalmer, , in which controlled orientation single crystals were grown dendritically in horizontal graphite boats, and the liquid decanted. The crystals were grown and decanted in an atmosphere of tank argon. Before decanting, a sample of the liquid was drawn up in a glass tube and allowed to solidify rapidly. The orientations of the single crystals were such that <loo> was parallel to the growth direction, and (100) in the horizontal plane for lead, and [1101 and (110) respectively for tin. With these orientations long dendrite stalks formed along the bottom of the boat in the dendrite direction (<100> for lead and [I101 for tin) from which secondary branches grew. Only these secondary branches, which grew freely in the liquid from the dendrite stalk to the liquid surface, were used in the measurements. Accordingly, effects due to substrates and oxides on the surface of the liquid need not be considered. In order to measure the solute concentration C, of the dendrites, individual dendrite stalks were cut from the decanted specimens, remelted, and formed

Jan 1, 1962

By J. K. Brooke, F. A. Renninger

During 1966, crushed stone production in the United States totaled just over 811 million tons valued at almost $1.2 billion. This represented in- creases of 4 % in tonnage and 5 % in value over that for 1965. Excluding the crushed stone used for agricultural and certain industrial purposes (cement, lime and flux), crushed stone mineral aggregate production totaled 616.3 million tons valued at almost $910 million, also up roughly 4% in tonnage and 5% in value over the 1965 figures. Limestone was by far the most widely used rock variety, followed by basalt, granite and sandstone in that order. Concrete aggregate and roadstone continued as the main uses for stone, accounting for 63% of all tonnage produced in 1966 and 60% of total stone value. Sand and gravel production in 1966 increased 3% over that for 1965. Total 1966 output was just in excess of 934 million tons valued at almost $985 million as compared with 908 million tons at $957 million for the previous year. Excluding the higher valued industrial sands, 903.2 million tons of sand and gravel valued at $891.6 million were used directly as mineral aggregates, representing a 2.9% increase in tonnage and a 2.4% increase in value over 1965.

Jan 2, 1968

By L. F. Mondolfo

An aluminum-copper 4 pct Cu alloy aged at room temperature for times increasing up to 78,000 hr was annealed at 170°C and the hardness and electrolytic potential determined during retrogression and subsequent aging. It was found that there is a change of behavior with increasing time of aging at room temperature which indicates that, given sufficient time, retrogression disappears and the room-temperature aging tends to progress directly into the high-temperature aging. WHEN an age-hardenable alloy is aged at low temperature after proper quench, changes of properties and structure take place. If this material is then heated to a temperature higher than the previous one, but still well below the solution-treatment temperature, the properties and structure changes produced by the low-temperature aging disappear and the material apparently reverts to the as-quenched condition, ready to undergo aging from the start. This phenomenon is termed reversion or retrogression. First discovered by Cayler3l it has been extensively investigated, as shown by the number of publications listed in the bibliography. From all the information available the following facts emerge: 1) All aeg hardenable alloys can be retrogressed.9 13, 19) 24, 33, 41, 42, 44, 47, 53, 54, 61, 63, 64, 66, 73, 78 2) All the properties changes that take place during aging at low temperature can be retrogressed to a smaller or larger extent.4,5,7,12,19,32,49,50,57,58,60,67,75,76 67, 75, 76 3) Retrogression requires that the temperature be well above the preliminary aging temperature. If the difference between the two temperatures is small, Little or no retrogression takes place.7,20,32,33,41,49 57. 65 4) The larger the difference between the preliminary aging and the retrogression temperature, the faster and more complete is the retrogression.20, 33, 41, 48, 65, 67 5) Retrogression can be produced several times in the same alloy.23, 35,41,57,59 6) The amount of retrogression that can be obtained depends on the aging temperature. Alloys aged at the lower temperatures can be retrogressed the most. The higher the preliminary aging temperature the less retrogression can be produced.20,25,33,37,44,49,54,58 7) Appreciable retrogression after aging at elevated temperatures is possible only if the preliminary aging has lasted a short time. After a certain time of aging at high temerature retrogression does not take place any more,:5,6,9,10,11,21,40,58 8) During retrogression the Guinier-Preston zones redissolve and disappear. The other precipitate

Jan 1, 1960

By J. R. Mihalisin, J. S. Iwanski

The response of Inconel "700" to heat treatment has been studied by light and electron microscopy combined with X-ray and electron diffraction techniques. A heat treatment which vesults in low ductility for this alloy appears to be associated with the formation of MC carbide in a Widmanstdtten distribution. This type of precipitation can be suppressed by suitable heat treatment with concurrent increase in ductility. Various other phases precipitated in this alloy are also identified. RECENT studies of commercial nickel base su peralloys have demonstrated the importance of the morphology of carbide phases upon physical properties.&apos; For example, empirical heat treatment studies applied to Nimonic "80" and Inconel "X" have resulted in prescribing double aging treatments for optimum physical properties. These treatments have subsequently been related micro-structurally to grain boundary carbide morphology.2 The purpose of this study was to obtain information about the morphology and identity of some of the phases precipitated in Inconel "700" after heat treatment. It was hoped that some correlation could be made of micro structure with heat treatment similar to that observed with Inconel "X" and Nimonic "80." EXPERIMENTAL PROCEDURE Specimens were obtained from a hot-rolled bar of Inconel "700" of the following composition: C Mn Fe S Si 0.10 0707 0.42 0.007 0.12 Cu Cr -A1 -Ti- Co Mo Ni 0.02 -14.90 TM 2.22 27.61 2.92-- Bal. Specimens were prepared in the following heat-treated conditions: (A) 2275°F for 2 hr WQ (B) 2275°F for 2 hr WQ + 2000°F for 1 hr (C) 2275°F for 2 hr WQ + 1600°F for 48 hr. (D) 2275°F for 2 hr WQ + 2000°F for 1 hr + 1600°F for 48 hr. Empirical stress-rupture studies had shown that treatment (D) resulted in optimum stress-rupture life and ductility. Treatment (C), although giving a good aging response, resulted in low ductility. Treatments (A) and (B), respresenting individual. steps in treatments (C) and (D) were added here for microstructural comparison studies. The procedure was to make an optical and electron microscopic investigation supplemented by X-ray diffraction analysis of electrolytically extracted residues. Electron diffraction studies were made utilizing selected area diffraction techniques with extraction

Jan 1, 1960

By R. L. Wilcox, M. L. Fuller

Owing to the nature of the die-casting process, fresllly cast alloys are undoubtedly not at equilibrium from the standpoint of alloy phase relationships. After casting, therefore, they tend to undergo phase changes, with the ultimate effeet of reaching a state of equilibrium at the aging temperature, beyond which no fnrther change takes place. This phase alteration undoubtedly is one of the primary causes of the changes in dimensions and physical properties that zinc-alloy die castings undergo during aging. It is planned to report on this problem in a series of papers of which this is the first. The writers have made a study of commercial zinc die-casting alloys over a period of several years, utilizing the X-ray diffraction technic of determining the phase composition changes in the alloys. Up to the present, two principal phase changes have been observed which are capable of causing dimensional changes: (I) the segregation of secondary constituents from the zinc-base solid solution and (2) the beta aluminum-zinc decomposition. The latter is the subject of the present paper and studies on the former will be reported upon at a future time. Scope of Study In the present investigation a special technic for the study of the beta phase in zinc-alloy die castings has been developed, making possible the determination of the period of existence of the beta phase after casting. The pure beta constituent and its decomposition have been studied in detail. The effect of magnesium and copper on the velocity of the decomposition is reported. The heat of decomposition, the eutectoid temperature arid the accompanying density change have been measured. The density change lias been calculated from data on crystal structure and the result thus obtained has been compared with the actual change.

Jan 1, 1935

By R. L. Wilcox, M. L. Fuller

Owing to the nature of the die-casting process, fresllly cast alloys are undoubtedly not at equilibrium from the standpoint of alloy phase relationships. After casting, therefore, they tend to undergo phase changes, with the ultimate effeet of reaching a state of equilibrium at the aging temperature, beyond which no fnrther change takes place. This phase alteration undoubtedly is one of the primary causes of the changes in dimensions and physical properties that zinc-alloy die castings undergo during aging. It is planned to report on this problem in a series of papers of which this is the first. The writers have made a study of commercial zinc die-casting alloys over a period of several years, utilizing the X-ray diffraction technic of determining the phase composition changes in the alloys. Up to the present, two principal phase changes have been observed which are capable of causing dimensional changes: (I) the segregation of secondary constituents from the zinc-base solid solution and (2) the beta aluminum-zinc decomposition. The latter is the subject of the present paper and studies on the former will be reported upon at a future time. Scope of Study In the present investigation a special technic for the study of the beta phase in zinc-alloy die castings has been developed, making possible the determination of the period of existence of the beta phase after casting. The pure beta constituent and its decomposition have been studied in detail. The effect of magnesium and copper on the velocity of the decomposition is reported. The heat of decomposition, the eutectoid temperature arid the accompanying density change have been measured. The density change lias been calculated from data on crystal structure and the result thus obtained has been compared with the actual change.

Jan 1, 1935

By P. Rama Rao, D. H. Sastry, T. R. Anantharaman

Deformation (a) and twin (a&apos;) stacking-fault densities in cold - wor ked filings of fcc silver alloys containing 2, 4, and 6 wt pct Sb have been estimated from Debye-Scherrer peak shifts and asymmetries, respectively. Evidence has been obtained for a possible strain-induced transformation in a two-phase alloy containing 9.0 zut pct Sb. Using Fourier analysis of X-ray line profiles, the effective particle sizes and root mean square strains have been determined for the three fcc alloys in the cold-worked condition. The values of the compound fault probability 0.5a + a&apos;) evaluated from peak shifts and asymmetries are in reasonable apeement with those derived from peak broadening. COLD work of fcc metals may produce both deformation and twin (also called growth) stacking faults, which can be detected and quantitatively estimated by X-ray diffraction techniques.&apos; In addition to peak broadening, deformation faults produce a shift in peak positions and twin faults an asymmetry of the Debye-Scherrer reflections. Besides stacking faults, a reduction in the size of coherently diffracting domains and distortion within these also broaden the powder reflections of deformed fcc metals and alloys. Fourier analysis&apos; of peak shapes provides quantitative infor- mation about the effective domain sizes, lattice strains, and also the compound fault probability (1.5a + a&apos;), where a and a&apos; represent deformation-and growth-fault density, respectively. The Paterson method2 for determination of a from peak shifts, the warren3 or wagner4 method for evaluation of a&apos; from peak asymmetries, and the Fourier analysis for quantitative estimates of all the contributory causes of peak broadening have, in the course of the last decade, been extensively applied to obtain data for a number of deformed fcc metals and alloys. One of the useful results of earlier measurements of a in several solid solutions is a correlation between a and the solute valence as well as electron concentration per atom (p) in alloy systems based on a particular solvent. The work of Smallman and westmacott5 on Cu-Zn, Cu-A1, and Cu-Sn, of Foley, Cahn, and ~aynor&apos; on Cu-Si and Cu-Ge, and of Rama Rao and Anantharaman7 on Cu-Si and Cu-Sb has revealed a common trend in the increase of a with p and also a with valency of the solute. Cahn and Davies&apos; and Ad-ler and wagnerg have observed similar trends for silver alloys containing cadmium, indium, and tin. Data on a for silver alloys with a pentavalent solute element are not, however, available. It is primarily to fill this need that the present investigation on Ag-Sb alloys was undertaken. Utilizing the Patersonand Warren methods, values of a and a&apos;, respectively, have been determined in three silver alloys containing 2, 4, and 6 wt pct Sb. By Fourier analysis of the broadening of Debye-Scherrer peaks, effective particle sizes, lattice strains, and the compound fault probability (1.5a +a&apos;) have also been evaluated.

Jan 1, 1967

By J. A. Berger, R. J. Towner

A method for determining the disorientation between sub-grains that .share a common tilt or twist boundary from measurements on X-ray micrographs is described. The method may be applied to subgrains of almost any orientation having boundary angles in the range from about 1 min to 1 deg of arc. An adaption of the Berg-Barretl method has been made to allow calculation of small angles of about 1 min to 1 deg of arc: between adjacent subgrains from the relative displacement of their images on X-ray micrographs. schulz4 gave equations for determining subgrain disorientation where the axis of subgrain rotation and the reflecting crystal planes were parallel to the specimen surface. In our method, however, they need not be parallel and, indeed, may have va:rious orientations. His camera setup, involving a fine-focus X-ray tube for obtaining high resolution with continuous radiation, was different from the one used in the present investigation (a 1.2 x 1.2 mm effective source and characteristic radiation). The X-rays produced a slight magnification in the subgrain images in the Schulz method, but not in the present method. The commonly available type of X-ray tube used permitted relatively short exposure times with a fine-grained photographic plate, which could be magnified optically many times for the examination of small subgrains. The method is illustrated by results obtained on {110} tilt boundaries in a polygonized aluminum single crystal of 99.994 pct purity. The flat crystal was stretched 6 pct in tension and then heated at 500°C for a cumulative time of 5 hr. Earlier, cahn5 studied subgrains formed by polygonization in stretched and heated aluminum crystals. He observed kink bands to have well defined boundaries lying in (110) planes, at least in the early stages of deformation. Cahn found that the (110) tilt boundaries formed by polygonization were directly related to the lattice bending about the <211> axis which lay in the (111) slip plane perpendicular to the <110> slip direction. DESCRIPTION OF THE CAMERA Our camera was similar in detail to Honey-combe&apos;s.6 Unfiltered copper radiation was used at 35 kv, and 20 ma. With the particular specimen used here to illustrate the method, a 1.2 by 1.2 mm effective source and a distance of 780 mm from target to specimen were employed, giving a convergence of 5 min of arc in the primary beam. The distance was 9.5 mm from the specimen to film. The upper 1/2- by 1-in. portion of the front surface of the specimen was irradiated with the film in parallel position. Since the specimen had been inhomogeneously deformed, many regions were in a position to reflect characteristic radiation at the Bragg Angle. Five minute exposures were satisfactory with Kodak Single Coated X-ray Film, 1 1/2 hr

Jan 1, 1961