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By H. E. Montgomery

H. L. Burghoff.*—I have a question, Dr. Smith. A number of the alloys you mentioned contain lead, which, of course, is present as discrcte particles. At what level of concentration does lead begin to play an important part in determining these elevated-temperature characteristics ? A. J. Smith.—That is a difficult question to answer because of the complicating features of the alloys that arc lead free. I do not know of any work done on the subject. But for comparison, 85-5-5-5 has about the same characteristics at, say 450°F. as 88-10-2, which is lead free or contains at most 0.30 per cent. Both 85-5-5-5 and 88-10-2 precipitate delta. The specification limit of usage is 406°F., temperature of saturated steam at

Jan 1, 1945

[Trans. No. Place Date Vol. Page 1. Wilkes-Barre, Pa May, '71.. 1 3 2. Bethlehem, I's Aug., '71.. 110 3. Troy, N. Y Nov., '71.. 113 4. Philadelphia, PaFeb., '72.. 117 5. New York, N. YMay, '72120 6. Pittsburgh, Pa Oct., '72.. 125 7. Boston, MassFeb., '73.. 128 8. Philadelphia, Pa.*May, '73.. 23 9. Easton, PaOct., '73.. 27 10. New York, N. Y Feb., '74211] [ ]

Jan 1, 1925

By W. F. Holbrook

IN a previous paper1 a method for the measurement of the comparative desulphurizing power of slags was described and data were presented covering the range of likely slags containing up to 10 per cent MgO In the present work the range is extended to include slags containing up to 20 per cent MgO, and the effect of temperature on 5 per cent and 15 pen cent MgO slags over the range 1475° to 1525° C is included The method used was that described in the previous paper except that some of the temperature measurements were made with a noble-metal thermocouple instead of a tungsten-graphite thermocouple Twelve-gram charges of 0 8 per cent sulphur-metal and 5-gram charge-, of slag were subjected to heating for 30 nun at a prescribed temperature The charges were analyzed for sulphur content For purposes of comparison, desulphurizing power is defined as the ratio of the percentage of sulphur found in the slag to that found in the metal Six slag and metal charges were made coincidentally in 5/8-in holes in a section of an electrode graphite rod One slag and metal charge was used as a control by means of which adjustment in the desulphurization value could be made for small variations in temperature and other factors For convenient presentation of the data, the slags are arranged in groups in each of which one of the four main slag components is constant Thus, the 15 per cent MgO slags are presented separately from those containing 20 per cent MgO SLAGS WITH MAGNESIUM OXIDE CONSTANT 15 Per cent MgO -The data on slags containing 15 per cent MgO cover a composition range of 24 to 50 per cent SI02, 5 to 27 per cent A1203 and 24 to 53 per cent CaO Variation in composition has been in steps of 2 per cent over much of the area Because the change in desulphurization power is generally gradual with gradual change in composition, certain sections have been covered m steps of 4I per cent and even

Jan 1, 1938

By Benjamin C. Craft

As predicted, during 1937 South Louisiana witnessed one of the most active drilling campaigns in the history of the area, resulting in the discovery .of 14 new fields. The economic importance of 10,000-ft. production was far-reaching and the objective depths placed on some wildcats was 12,000 feet. Most of the important discoveries and deep tests were in the delta area between the Atchafalaya and Mississippi Rivers, where the upper Miocene sands were found productive between 10,000 and 11,000 ft. The casing program on these wells usually called for a protection string of 95/8-in. casing at approximately 9500 ft. Drilling barges with the heaviest equipment were used where water transportation was available. The oil production for South Louisiana during 1937 was 62,147,690 bbl., as compared with 51,968,727 bbl. during 1936, an increase of 19.5 per cent. There were 281 oil and gas wells and 172 dry holes completed during 1937 as compared with 262 oil and gas wells and 135 dry holes during the previous period. New Fields Gibson.—The first discovery for the year was in the Gibson area, where Shell Petroleum Corporation's Realty Operators No. 1, sec. 18, 17 S., 15 E., Terrebonne Parish, was completed flowing 780 bbl. of 38° A.P.I. oil daily through a 14/64-in. choke with a tubing pressure of 1700 lb. Production is from upper Miocene sand found from 9461 to 9483 feet. Abbevil1e.—The discovery well for the Abbeville field was Continental Oil Company's Hebert No. 1, sec. 20, 12 S., 3 E., Vermilion Parish, completed flowing 50 bbl. of distillate and 2 million cubic feet of gas through a 3/16-in. choke with a tubing pressure of 2550 lb. The well was plugged back from 12,216 ft. in the Chickisawhay, and is producing through perforations from upper Miocene sand found from 7668 to 7682 ft. Later in the year, the same operators completed Brookshire No. 1, sec. 66, 12 S., 3 E., flowing 366 bbl. of 42° A.P.I. oil per day through a 3/16-in. choke with a tubing pressure of 1800 lb. This well was com-

Jan 1, 1938

By A. U. Seybolt

In part 111' of this series it was shown that during the selective oxidation of a 3 1/4 pct Si-Fe alloy in damp hydrogen, only silica, (observed at room temperature) as low cristobalite or low tridy-mite or both, was formed as an oxidation product. In some in- „ stances where the film was fairly thin (probably well under 100A) there was some suggestion of an amorphous form of SiO2. The present investigation of oxidation rate showed that the selective oxidation of silicon-iron can be rather complicated, and apparently impossible to rationalize in an unequivocal manner. In some temperature regions, notably near 800" and 1000°C, the data seem to obey the familiar parabolic rate law. However, at intermediate temperatures complications were noted, some of which are possibly due to the order-disorder reaction in the silicon-iron solid solution. IN an earlier report' it was shown that during the oxidation of 3 1/4 pct Si-Fe alloys in H2O-H2 atmospheres only silica films were formed in the temperature range from 400° to 1000°C in hydrogen nearly saturated with water at room temperatures, or at dew points as low as -45°C. In the work to be reported here, some observations are made on the rate of oxide film formation. As in the earlier investigation, electron diffraction patterns generally showed either low tridymite or low cristobalite or both, except for some very thin films. These sometimes showed diffuse rings, presumably due to a very small crystallite size, or in a few cases, diffuse bands probably caused by an amorphous film. EXPERIMENTAL PROCEDURE Vacuum-melted silicon iron made of high-purity materials was rolled into strips 0.014 in. thick, and cut into samples 1/2 in. wide by 1 in. long. Chemical analysis showed 3.2 pct Si and 0.002 pct C. All samples were surface abraded with 600-grit paper, were solvent cleaned, and then placed in an paper,apparatus containing a "Gulbransen type"2 micro-balance. Here the gain in weight of the samples of about 5 sq cm area could be followed as a function of time during the oxidation caused by the water in atmospheres of various controlled water-hydrogen ratios. The water-hydrogen ratios can most easily be described as varying from a dew point of 0°C (PH2O-p^2 = 6.2 x 10-3 , to K (P j -40°C (PH2O/PH^= 1.3 X 10-* Most of the experiments were conducted at the 0°C dew-point atmosphere because drier atmospheres caused so little gain in weight that the accuracy of measurement was poor. Because of this, only the data obtained at PH2O,/P,,,= 6.2 x X3 will be reported. The temperature range extended from 800" to 1000°C; and most of the oxidation runs lasted for about 24 hr. The reproducibility of any reading was about ± 1 ?, but the sensitivity of the balance was about 0.2 ?. The atmosphere, flowing at 200 cm per-min, was preheated to the furnace temperature before contacting the specimen. While the gas flow caused a measurable lift on the sample, it was ordinarily sufficiently constant so that it was not an appreciable source of error. X-ray and electron diffraction checks of the samples before and after oxidation showed no evidence of preferred orientation, either on the metal samples or on the silica films formed. EXPERIMENTAL RESULTS The data obtained are summarized in Table I, and some are given in detail in Figs. 1 to 4. In the fourth column of Table I, kp refers to the parabolic rate constant in the expression (?/cm2)2 = kpt + c [1] where ? = micrograms gain in weight kp = parabolic rate constant in units r2 /cm4 t = time in minutes c = constant It will be noted that in many cases no value for kp is given; this is because in these instances the data did not obey the parabolic rate law. The silica film thicknesses given in the last columns are values calculated from the weight gain, an average tridy-mite-crystobalite density, and by assuming a perfectly plane surface. Fig. 1 shows the data plotted in the form of Eq. [I], hence a linear plot indicates parabolic behavior. It has been frequently observed in the literature that

Jan 1, 1960

By C. L. T. Edwards

In the preparation of this paper, the author has drawn upon experience with the operation of a blast furnace on Ioo per cent scrap burden, which he believes was the first operation of its kind in the country. It is the writer's further belief that much of the controversy attending discussions of this subject may be obviated by the presentation of a group of facts that should be known by blast-furnace men and open-hearth men alike. The following question has been raised: "Is iron made with scrap in the blastfurnace charge as good iron as that made without scrap—made with straight ore?" This question may he answered in part by the fact that the open-hearth men of the Bethlehem Steel Co. who used pig iron from a blast furnace that operated on Ioo per cent steel scrap found no difficulty in the processing of such iron other than that to be expected from the known analysis. Operation with ioo PeR Cent Steel Scrap During World War I, there was accumulated at the Bethlehem plant of the Bethlehem Steel Co. some 22,000 tons of alloy-steel turnings and borings. This scrap material was highly corroded and, like alloy-steel turnings of that period, were as a drug on the market. There was also a small tonnage of scale, rich in valuable metal. If this scrap could be worked up into pig iron, it would become readily available for use in the open hearth. In order that the pig iron should contain the maximum percentage of nickel, permission was obtained from the Management to try a Ioo per cent scrap operation. Accordingly, a blast furnace was swung over on July 25, 1919; the percentage of steel scrap increased more or less irregularly until July 29, when Ioo per cent steel turnings were charged. Except for occasional charges of nickel scale as an "cxtra," the operation continued uninterruptedly until Aug. 27, when the furnace was swung back to the regular ore—ore and scrap—operation. During this period, the furnace production ranged from a low of 568.60 tons to a maximum of 766.07 tons. At the swing-over from Ioo per cent scrap to the regular burden, the charge I hung up rather severely. While the latter condition has nothing to do with the object of the paper, a brief discussion of the experience will appear later because of the interest it may have for blast-furnace operators. In Table I, results of the first and last days of the ore charge are shown, July 25 and July 29. The last column shows a summary for the period of maximum scrap ' charge. The furnace employed had a hearth 16 ft. o in., bosh 22 ft. o in., stock line 15 ft. 6 in., bell 11 ft. 6 in., batter in., bosh angle 73' 27' and a Balrer-Neuman top, with gas-engine blowers. Analyses Range of material charged Gravel: SiO2, 64.40 to 70.54 per cent; A1203, 3.52 to 4.58; CaO, 7.27 to 9.49; MgO, 5.09 to 6.14; FeO, 1.67 to 3.34, ignition loss, 9.50 to 13.83. I

Jan 1, 1942

By C. L. T. Edwards

In the preparation of this paper, the author has drawn upon experience with the operation of a blast furnace on Ioo per cent scrap burden, which he believes was the first operation of its kind in the country. It is the writer's further belief that much of the controversy attending discussions of this subject may be obviated by the presentation of a group of facts that should be known by blast-furnace men and open-hearth men alike. The following question has been raised: "Is iron made with scrap in the blastfurnace charge as good iron as that made without scrap—made with straight ore?" This question may he answered in part by the fact that the open-hearth men of the Bethlehem Steel Co. who used pig iron from a blast furnace that operated on Ioo per cent steel scrap found no difficulty in the processing of such iron other than that to be expected from the known analysis. Operation with ioo PeR Cent Steel Scrap During World War I, there was accumulated at the Bethlehem plant of the Bethlehem Steel Co. some 22,000 tons of alloy-steel turnings and borings. This scrap material was highly corroded and, like alloy-steel turnings of that period, were as a drug on the market. There was also a small tonnage of scale, rich in valuable metal. If this scrap could be worked up into pig iron, it would become readily available for use in the open hearth. In order that the pig iron should contain the maximum percentage of nickel, permission was obtained from the Management to try a Ioo per cent scrap operation. Accordingly, a blast furnace was swung over on July 25, 1919; the percentage of steel scrap increased more or less irregularly until July 29, when Ioo per cent steel turnings were charged. Except for occasional charges of nickel scale as an "cxtra," the operation continued uninterruptedly until Aug. 27, when the furnace was swung back to the regular ore—ore and scrap—operation. During this period, the furnace production ranged from a low of 568.60 tons to a maximum of 766.07 tons. At the swing-over from Ioo per cent scrap to the regular burden, the charge I hung up rather severely. While the latter condition has nothing to do with the object of the paper, a brief discussion of the experience will appear later because of the interest it may have for blast-furnace operators. In Table I, results of the first and last days of the ore charge are shown, July 25 and July 29. The last column shows a summary for the period of maximum scrap ' charge. The furnace employed had a hearth 16 ft. o in., bosh 22 ft. o in., stock line 15 ft. 6 in., bell 11 ft. 6 in., batter in., bosh angle 73' 27' and a Balrer-Neuman top, with gas-engine blowers. Analyses Range of material charged Gravel: SiO2, 64.40 to 70.54 per cent; A1203, 3.52 to 4.58; CaO, 7.27 to 9.49; MgO, 5.09 to 6.14; FeO, 1.67 to 3.34, ignition loss, 9.50 to 13.83. I

Jan 1, 1942

Aamot, Olav Crone, Chem. Engr., Norsk Elektrokemisk, Kongensgt. 18, Olso. Norway. '29 Abadilla.-Quirico A., Dir., Bureau of Mines Manila, P. I. '38 Abbott, Clarence E., V.P., Charge of Raw Materials, Tennessee Coal, Iron & R.R. Co., 1212 Brown-Marx Bldg., Birmingham, Ala. '04 Abel, Raymond L., Prof., Dept. of Pet. Refin., Univ. of Pittsburgh Pittsburgh, Pa. '29 Abel. Walter D., Cons. Engr 1839 Holmby Ave., W. Los Angeles. Calif. '32 Abele, Louis T R. F. D. 5. Susquehanna Trail, N., York. Pa. '31 Abell, Leo M., Ore Dressing Investigator, School of Mines Adelaide, S. Australia. '31 Abenius. Hakan V., Mine Supt., Bolidens Gruvaktiebolag Boliden, Sweden. '37 Aborn, Robert H., Asst Met., Research Lab., U. S. Steel Corp. Lincoln Highway, Kearny, N. J. '19 Abraham, W. E. V., East India United Service-Club, 16 St. James' Sq., London, S. W. 1, England. '28 Abrams. Charles Jackson 1624 17th St., Denver, Colo. '36 Abstein, Henry T., Engr. & Mgr., Profile-Tamarack Mines Co Yellow Pine, Idaho. '27

Jan 1, 1938

THE CHAIRMAN (F. K. COPELAND,* Chicago, Ill.).-At this particular time conditions existing in this, country, and elsewhere, make all questions of milling or smelting or mining, or anything else, absolutely secondary to the one question of labor. We have always devoted our attention largely to the efficiency of machinery, and to reductions in costs, etc., and have let this tremendous problem of our relation to labor more or less take its own chances. There has never been a time when those who are responsible for the operation of business of different kinds were as com-pletely at a loss as they are now, so that anything that can be brought out that relates to labor is, to my mind, of utmost importance. T. T. READ, Washington, D. C.-This formulation of a method of curtailing forces at the Copper Queen is a notable step in advance of our treatment of personnel in the mining industry. So far as I know, it is the

Jan 12, 1919

By S. K. Bradford

For years past I have traveled in quest of promising mining-properties, over almost impassable mountain-trails to remote places in the mining-regions, usually many miles from an assay-o5ce. If, upon examination, the fornlation and the ore-deposit appeared favorable, a quick determination of the value of my samples was necessary, in order that I might take intelligent action with reference to the acquisition of the property. A journey with my samples to civilized regions often meant weeks of delay, and perhaps loss of opportunity. How many, under similar circumstances, have returned with their assay-results from such a journey, only to find that some audacious speculator had optioned" the property! True, a first payment could have been made and the chances taken on the results; but experience has taught that rich-looking ore is not of necessity valuable. Personally, I would not hazard a ten-dollar bill on any property without first determining by assay the value of the ore. To carry the usual complete assay-paraphernalia over such mountain-trails was impracticable by reason of the loss of time involved, the great expense of transportation (charged -

Jan 1, 1911

By N. A. Gokcen, E. S. Tankins, G. R. Belton

Equilibrium in the reaction H2(g) + O[in liquid iron, cobalt, or nickel] = H2O(g) has been investigated over wide temperature and composition ranges. Oxygen has been found to obey Henry's Law in each of the three metals at 1550°C. The standard free-energy changes for the above reaction are given by: (1550° to 1700°C) ?Foco = -45,360(±290) + 16.16(±0.16)T (1490° to 1700°C) ?Fo Ni = -48,170(±220) + 16.12(±0.12)T (1465° to 1700°C) where the standard state for dissolved oxygen is the I wt pet solution. ThE thermodynamic behavior of dilute solutions of oxygen in molten iron has been the subject of many investigations over the last thirty years,'-'4 the majority of the investigators having utilized the reaction:

Jan 1, 1964

By William R. Webster

At the Florida meeting of the Institute, in March, 1895, I presented a Note on a Proposed Scheme for the Study of the Physics of Cast-Iron,1 giving an outline which, for convenience of reference, I here repeat. Suggested Lines for DiScuSsion and IvestiGation. I.—Correspondence between chemical composition and melting-point, fluidity, shrinkage, fracture, chill, micro-structure, and other physical properties. II.—Influence of: 1. Cupola-mixture, use of steel and other scrap, oxidized or clean material, 2. Manner of melting, flux, etc., 3. Casting-temperature, A. Fracture. 4. Manner of handling melted metal and B. Micro-structure. method of casting, C. Physical properties. 5. Size and form of casting, D. Shrinkage. 6 Kind of mold, green sand (under dif- on E. Chill. ferent conditions of ramming, amount F. Residual strew of moisture, and skin-dried), dry sand, G. Condition and quan- loam, and chills, tity of carbon and 7. Rate and mode of cooling castings, other elements. 8. Manner and temperature of heating for annealing, 9. Additions of nickel or aluminum, III. —-Segregation as affected by : 1. Composition ; 2. Casting-temperature; 3. Rate of cooling ; 4. Size and shape of casting. IV. —Blow-holes, their volume and position as affected by: 1. Composition; 2. Casting-temperature; 3. Casting-pressure ; 4. Rate of cooling; 5. Size and ehape of casting ; 6. Special additions. It was hoped that a discussion might thus be elicited, similar in interest and value to the discussion of the physics of steel, which had been so widely and gratefully welcomed by students and practitioners in that department. That this hope was not

Jan 1, 1905

AN intermetallic compound, Ni3A1, has an ordered fcc structure of type Ll2, and shows peculiar dependence of the yield stress upon temperature; i.e., the yield stress increases by a factor of six upon raising the temperature from 77" to 900K1, 2 This compound is technologically important, since many nickel-base superalloys owe their high-temperature strength to the peculiar yield stress behavior of Ni3Al. The only study of the elastic behavior of this compound was made by Davies and Stoloff,1 who determined Young's modulus of poly crystalline Ni3A1 between 300" and 730°K. The determination of single-crystal elastic constants of Ni3A1 is therefore of interest in connection with dislocation dynamics and is reported in this paper. A single-crystal specimen, 1 by 1 by 3 cm, was cut from an ingot generously supplied by Dr. B. H. Kear of Pratt & Whitney Aircraft. Following initial machining with a Servomet and a surface grinder, the specimen was etched and annealed at 1100°C for 5 hr in vacuum followed by furnace cooling. Two parallel faces were oriented normal to within ±l deg of a [I101 crystallographic axis by the back-reflection Laue technique. The parallel faces were hand-lapped, etched, and polished by the usual metallographic procedures. Final thickness along the [I101 axis was (0.9325 * 0.0005) cm. Chemical analysis gave an average composition of 87.35 pct Ni. Total impurity content is esimated to be no more than 0.1 pct. The elastic constants were calculated from measurements of ultrasonic waves which were propagated along the [110] axis. A longitudinal wave and two shear waves whose displacements are aligned along the [ 110], [li~], and [001] directions, respectively, are necessary in order to completely specify the three elastic constants. Two 3/6-in. quartz transducers were bonded to the parallel faces of the sample with ~ac-seal.3 Although this bond was sensitive to thermal shock, it performed satisfactorily over the entire temperature range for both longitudinal and shear wave propagation. A frequency of 5 mHz was employed in the method of Williams and Lamb4 in order to measure the absolute value of the ultrasonic velocity. The pulse-overlap technique of Mcskimin5 was also used at this frequency in order to determine the shift in the ultrasonic velocity

Jan 1, 1970

By M. J. Mullikin, J. B. Conway

Several different equation forms were studied to determine the extent to which each particular equation type yielded an accurate representation of a given set of first-stage creep data. Specially developed least-squares computer programs were employed to obtain unique solutions for the creep-equation constants. In studies of creep data for lead at 14.5"C, nickel at 70OCC, and arc-cast tungsten at 2400°C consistently good representations were afforded by a third-degvee polynomial in t113. Other effective correlations were obtained with the Andrade, Cottrell-Aytekin, and de Lacombe equations along with a third-degree polynomial in t112. A newly proposed creep equation involving a hyperbolic-sine term in t1'3 was also found to yield very satisfactory results. This appears to be the first use of such a functional relationship in the analysis of transient creep behavior. In general, the deformation behavior of a material subjected to a tensile load is described in a strain-time plot. Experiments have shown that, following the instantaneous elongation which results on loading, the instantaneous slope (i.e., creep rate) of the strain-time curve decreases gradually with time and approaches what appears to be a constant value. Equations, therefore, which are proposed to provide an analytical representation of such first-stage or transient creep behavior must be consistent with these observations. In other words, at time zero, these equations must yield a finite deformation value corresponding to the elongation on loading. Furthermore, the first derivative of these equations must exhibit a fairly high although finite value at time zero, and then values which decrease with time. It is also preferable, in general, that the derivative eventually assume a constant value at high time values. Although many studies of first-stage creep behavior have been made and numerous equation forms have been proposed for expressing this type of deformation behavior, it is still not possible to state with any assurance which functional relationship will be adequate for a given set of measurements. Parabolic relationships have been employed most extensively although logarithmic expressions have been shown to be applicable in some instances. Combined forms1 have been studied in considerable detail and have on occasion been found to be very effective. One such expression is that of iXndradea and involves a modified parabolic expression: where 1 is the instantaneous length, lo is the length immediately following load application, t is the time, and p and k are constants. Another combined form has been proposed by weaver3 as follows: where E is the instantaneous strain, is is the linear creep rate, t is the time, and a and b are constants.

Jan 1, 1967

By F. R. Hensel

PURE silver and silver-lead alloys have been studied as to their suitability for bearings.1-8 A review of the properties of thallium and the silver-thallium constitutional diagram was made by the author to analyze the possibilities of silver-thallium compositions for antifriction materials.† The silver-rich end of the diagram as reported in the literature9-11 was found to be sketchy and it was necessary to carry out considerable experimental work to arrive at definite conclusions. Some of the results of this work are reported in this paper. TEST MATERIALS In the beginning of the work, only fused alloys were investigated. Later, research [TABLE I. Composition of Fused Silver thallium Alloys Tested for Antifriction Properties PERCENTAGE ALLOY No.OF THALLIUM 15330.48 153406 231 HT2.04 2312.10 232 HT3.83Balance 2324.07Silver 233 HT5.86 2336.38 2349.84 234 HT10.07] was carried out on electroplating methods and diffusion processes. In preparing the fused alloys, care was taken to exhaust the toxic fumes caused by the thallium content. The compositions of the series of fused alloys are listed in Table I. The silver-thallium alloys were melted in clay-graphite crucibles and cast into preheated steel molds of 3/4-in. diameter. In the cast condition, they showed a cored structure, as indicated by the micrographs of Figs. I to 3. The etching reagent used was a mixture of 2 grams K2Cr2O7, 8 c.c. H2SO4, and 100 c.c. H2O. The cored structure is unsatisfactory for the type of corrosion resistance required for bearing applications, and homogenizing experiments were carried out at various temperatures, the results of which are shown in Figs. 4 through 8. The alloys with a lower thallium concentration, which were heated for 2 hr. at 525°C. show an almost completely homogenized solid solution type of structure. With higher thallium concentration, the homogenizing temperature was dropped to 475°C. to eliminate the formation of a liquid phase. It is evident that heating for 2 hr. at this temperature did not result in complete elimination of the cored structure. As would be expected, cold-working of the cast structure is an expedient in establishing equilibrium conditions. The fine homogeneous grain structure shown in Fig. 7 corresponds to the cold-worked area under the Rockwell ball penetration when the hardness was taken before heat-treatment. A detailed structural study was made on a cast silver-thallium alloy containing 3.67 per cent thallium. Three micrographs (Figs. 9, 10 and 11) show the transition

Jan 1, 1945

By James J. Halbouty, Michel T. Halbouty

Drilling activity in the South Texas area, which includes the South Corpus Christi and Laredo districts, showed a marked decline during 1941 from that of the preceding year. The rate of new discoveries, however, 'compared favorably with exploratory results of 1940 because of the many new productive sands opened in existing fields. South Texas completions for 1941 were about 12.3 per cent below the 1940 figure, compared with an increase of approximately 5.5 per cent in the total number of completions in the United States during 1941 over the 1940 total. During the year, 1452 wells were drilled in this area; of these, 1205 were drilled in or as extensions to the proven fields, and 247 were rank wildcats drilled in search of new producing pools. The comparable 1940 figures were: 1320 field or extension wells and 336 rank wildcats, a total of 1656 completions. This represents a decline in 1941 of approximately 8.7 per cent in proven-area wells, and of about 26.5 per cent in rank wildcats. It must be stressed that wells that were considered rank wildcats at the beginning of operations, but which opened production later classified as additions to existing fields, are not regarded as rank wildcats in this and previous annual reports on this same area. These wells are classified as semiwildcats (Table 2). There were 13 new oil or distillate fields and 4 new gas areas opened during the year, as listed in the next column. This listing represents a decline of 32 per cent from the 25 new areas found during the previous year, and to a great extent can be attributed to the 26.5 per cent decline in wildcatting. The rate of new discoveries based on the 247 wildcats was 14.5 to I, which compares somewhat unfavorably with the 13.4 to I ratio obtained in 1940 (Table 5). Dry wildcats totaled 230. The proof of the prolific character of the South Texas area as a source of petroleum reservoirs is to be found in the fact that of the 1205 field or extension (semiwildcat) wells completed during the past year 61 opened production from new sands or found crude in formerly distillate-producing sands. The 1940 total of 1320 such wells accounted for 50 horizons that provided either new production or crude in distillate sands, and in this respect the 1941 rate of discovery shows to greater advantage, the ratios for new sands being 19.7 to I for 1941 and 26.4 to I for 1940. The 1205 field or semiwildcat wells completed in 1941 resulted in 926 oil or dis-

Jan 1, 1942

By James J. Halbouty, Michel T. Halbouty

Drilling activity in the South Texas area, which includes the South Corpus Christi and Laredo districts, showed a marked decline during 1941 from that of the preceding year. The rate of new discoveries, however, 'compared favorably with exploratory results of 1940 because of the many new productive sands opened in existing fields. South Texas completions for 1941 were about 12.3 per cent below the 1940 figure, compared with an increase of approximately 5.5 per cent in the total number of completions in the United States during 1941 over the 1940 total. During the year, 1452 wells were drilled in this area; of these, 1205 were drilled in or as extensions to the proven fields, and 247 were rank wildcats drilled in search of new producing pools. The comparable 1940 figures were: 1320 field or extension wells and 336 rank wildcats, a total of 1656 completions. This represents a decline in 1941 of approximately 8.7 per cent in proven-area wells, and of about 26.5 per cent in rank wildcats. It must be stressed that wells that were considered rank wildcats at the beginning of operations, but which opened production later classified as additions to existing fields, are not regarded as rank wildcats in this and previous annual reports on this same area. These wells are classified as semiwildcats (Table 2). There were 13 new oil or distillate fields and 4 new gas areas opened during the year, as listed in the next column. This listing represents a decline of 32 per cent from the 25 new areas found during the previous year, and to a great extent can be attributed to the 26.5 per cent decline in wildcatting. The rate of new discoveries based on the 247 wildcats was 14.5 to I, which compares somewhat unfavorably with the 13.4 to I ratio obtained in 1940 (Table 5). Dry wildcats totaled 230. The proof of the prolific character of the South Texas area as a source of petroleum reservoirs is to be found in the fact that of the 1205 field or extension (semiwildcat) wells completed during the past year 61 opened production from new sands or found crude in formerly distillate-producing sands. The 1940 total of 1320 such wells accounted for 50 horizons that provided either new production or crude in distillate sands, and in this respect the 1941 rate of discovery shows to greater advantage, the ratios for new sands being 19.7 to I for 1941 and 26.4 to I for 1940. The 1205 field or semiwildcat wells completed in 1941 resulted in 926 oil or dis-

Jan 1, 1942

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

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

Jan 1, 1968

By G. Wakefield, A. H. Daane, D. H. Dennison, F. H. Spedding

Preparation of pure scandium metal was accomplished by calcium reduction of the fluoride by two methods; a low-temperatzdre alloy process and direct reduction with subsequent distillation of the product. The following properties were determined: melting point: 1181OK; boiling point (calculated): 3000°K; lattice constants at 298°K (hexagonal lattice): a = 3.308 * 0.001 A, c = 5.267 * 0.003A; calculated density at 298°K, g per cm3: 2,990 + 0.007; electrical resistivity, ohm-cm: 299°K, 66.6 ± 0.2 x 10 -6; 373oK, 77.4 * 0.2 x 10 -6; thermal coefficient at 299°K, ohm-cm per deg: 5.4 X x; heat of sublimation at 298°K, kcal pel- mole: 80.79. The vapor pressure was determined as a function of temperature between 1505o and 1748°K, with the data fitted to a straight line shielding the equation: Log Pmm = -1.718 X 104/ToK + 8.298. SCANDIUM, element number 21, was first discovered by Nilson in 1879 and was recognized as the Ekaboron as predicted by Mendeleff. As it is in group III of the periodic table, the general properties are a little like aluminum and also resemble quite closely the properties of yttrium and the rare-earth metals, in both the metallic and ionic form. Although the earth's crust contains approximately 5 ppm of scandium (the element is as abundant as arsenic and twice as abundant as boron) it generally occurs so widely distributed that it has earned the reputation of being very rare. The one exception to this is the mineral thortveitite, which has been found in Madagascar (20 pct Sc2O3) and in Norway (35 pct Sc2O3). Scandium also occurs in small but distinct amounts in uranium and rare-earth ores; the recent larger scale processing of these materials has made some scandium available from these sources. As with other naturally-occurring monoisotopic elements (except Be), scandium contains an odd number of protons and an even number of neutrons. Scandium metal was first prepared by Fischer and coworkers1 in 1937 by electrolysis of scandium chloride in a molten eutectic mixture of lithium and potassium chlorides, using molten zinc as a cathode and collector of the scandium metal produced. The zinc was removed from the Zn-2 pct Sc alloy by vacuum distillation, leaving a product reported to be 94 to 98 pct Sc, with the main impurities being iron and silicon. They reported a melting point of 1400° C for this material. Scandium has also been prepared by the reduction of scandium chloride with potassium metal in a glass apparatus by Bommer and Hohmann in 1941,' resulting in a mixture of metal and potassium chloride; these workers did not isolate the metal proper, but the X-ray diffraction of the slag-metal mixture showed it to be hexagonal with a = 3.30A, c = 5.45A. petru3, 4 and coworkers have recently reported the preparation of the metal in a compact form by the reduction of either ScF3 or ScC13 with calcium metal and subsequent distillation of the product. This process probably yielded a metal of high purity, but they list no chemical analysis nor do they list any of the properties of their product. Previous related work in this Laboratory has been concerned with the production of yttrium and the rare-earth metals and the determination of their physical properties. Because of its similarity to these metals, scandium is being included in this study. PREPARATION OF SCANDIUM METAL The preparation of yttrium and the rare-earth metals may be accomplished by reduction of their fluorides with calcium metal in tantalum crucibles.5 This process leads to the introduction of tantalum (up to 0.5 pct) as an impurity in the higher melting rare earths, but since the tantalum occurs as dendrites, uncombined with the rare-earth metals, its presence is not objectionable in some cases. The preparation of scandium metal in this manner, however, was found to yield a product containing 2 to 5 pct Ta. To obtain a purer product, the following two methods were developed for the reduction of scandium fluoride with calcium metal: i) a low-temperature process utilizing zinc to form a low

Jan 1, 1961

By E. A. Gulbransen, W. S. Wysong

The behavior of molybdenum and its surface oxides in oxidizing and reducing gas atmospheres and in high vacua at elevated temperatures is a question of scientific and technical importance. The use of molybdenum as a metal or as an important component in alloys in oxidizing atmospheres at elevated temperatures has been limited because of the unprotec-tive nature of its oxide film and the volatility of this oxide at moderate temperatures. This communication will present results of a vacuum microbalance studyl, 2 of the following problems: (I) the oxidation kinetics in the temperature range of 250°to 450°C; (2) the reduction with pure hydrogen of thin oxide films formed on molybdenum; (3) the volatility of the thin oxide films; and (4) the vacuum oxidation of molybdenum at high temperatures. Molybdenum is an interesting metal to study for the following reasons: (I) although the oxide-to-metal-volume ratio is greater than one, the metal is not considered protective; (2) the metal oxidizes readily at temperatures of 2 50°C and higher; (3) the oxides of the metal are reduced at temperatures as low as 500°C by pure hydrogen; (4) the oxide Moo3 melts at 795°C; and (5) the oxides of molybdenum are volatile at moderate temperatures. The following variables are studied in the oxidation kinetics: time, temperature, pressure, surface preparation, surface area, concentration of inert gas in the lattice, cycling procedures in temperature, vacuum effect and high temperature vacuum oxidation. The general interpretation of many of these factors has been previously discussed. Literature The oxidation of molybdenum has not been studied critically. Although many studies have probably been made on the kinetics of the oxidation process, none has been reported in the literature available to us. The crystal structures found in the oxidation of molybdenum have been studied by Hickman and Gulbransen." Their results showed that Moo2 is the oxide which is stable in contact with the metallic substrate throughout the temperature range 300 to 700°C. As the film thickens in the low temperature range, MoO3 becomes predominant on the surface. Above 400°C, Moos is no longer observed, MoO2 being the only oxide found. Hagg and Magneli6 have shown from an X ray study that the a-phase, orthor-hombic Moo3 is stable up to 1050°C. Two other phases, ß and ß with compositions close to MoO2.90 are also obtained. The formula for the 0 phase is not given but that of the ß phase is defined as Mo9O26 The 0' phase is found to be built upon a monoclinic unit cell. A ?-phase is isolated from a preparation MoO2.75 heated for 17 hrs at 670°C. This phase is

Jan 1, 1949