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By M. Smutz, C. J. Baroch, E. H. Olson

IN 1949 an orebody containing some 10 billion lb of recoverable rare earth metals was discovered in the Mountain Pass district of San Bernardino County, California.' The following year Molybdenum Corp. of America purchased a number of claims at the deposit and a mill on the property which had been constructed to process the district's gold ores. Average composition of ore from the San Bernardino deposit is less than 0.1 pct Tho2, 25 to 35 pct calcite, 10 pct rare earth oxides, 15 to 20 pct silica, and 30 to 40 pct barite.' Rare earth content of the ore analyzes 50.7 pct CeO2, 4.2 pct Pr6O11, 11.7 pct Nd2O3;, 1.3 pct Sm2O3,, and 34.3 pct La2O3 and others.' By floating the barite and depressing the bastna-site, Molybdenum Corp. of America produced a concentrate that contained 60 to 70 pct rare earth oxides. More than 25 pct of the rare earths, however, was lost in flotation. It seemed likely that a more economical method could be found. At the present time most of the rare earths in the concentrates are converted to rare earth chlorides, which are either fed to ion exchange columns for separation of the individual rare earths or reduced to misch metal. Current investigation shows that solvent extraction may achieve this separation more economically than ion exchange. The study reported here was undertaken to develop an economical method of preparing a pure rare earth nitrate mixture from California bastnasite ore. Results indicated that more than 98 pct of the rare earths could be recovered. Several possibilities were considered for processing bastnasite ore, but only the method outlined in Fig. 1 was investigated. This involved leaching the calcined ore with nitric acid. The nitric acid process is discussed under the following headings: 1) calcination of the ore, 2) leaching of calcine, 3) filtration studies, 4) solvent extraction, and 5) nitric acid recovery. Calcination: Since California bastnasite ore contains 25 to 35 pct calcite and about 10 pct bastnasite, calcination was needed to reduce the violence of reaction with nitric acid. Weight losses of 26 to 30 pct were obtained by calcining the ore at 900°C for I hr or at 800°C for 4 hr. Longer periods resulted in no further weight loss. Leaching the Calcine: When the bastnasite calcine was leached with 30 pct nitric acid for 8 to 10 days, rare earth recoveries of only 45 to 50 pct were

Jan 1, 1960

Albin. B . R Billings. Mont . '28 Amnter . Nathan L 26 Broad St.. New York . N . Y . '28 Bache . Jules S 42 Broadway. New York. N . Y . '28 Borrett . C . P . 5338 Harper Ave .. Chicago. I11 '28 Baum . Frank G. . Cons . Hydro-Electric Engr Camel'. Shasta Co. . Cal. '23 Baylean, William S Russ Bldg .. San Francisco. Cal . '28 Bean, Louis H .. V.P.. Dwight P . Robinson & Co.. lnc 126 E . 46th St New York. N . Y . '28 Beatty . Roes J . 1106 First National Bank' Bldg .. Chicago . Ill . '28 Benwell . Oswald F . 110 Gilpin St .. Denver. 1310 . '28 Beymer. Albert 9.. V.P .. Keystone. National Bank Pittsburgh. Pa . '28

Jan 1, 1929

By A. G. Allten

EXAMINATION by metallographic and X-ray diffraction means of an austenitic steel containing 0.06 pct C, 1.26 pct Mn, 0.38 pct Si, 21.15 pct Ni, 18.72 pct Cr, 3.07 pet W, and 9.14 pet Mo indicated that a - phase, which had not been reported in the literature, existed in this steel. Both the s and car-bides of the M6 C type were present in the as-forged steel. The carbides dissolved completely in the aus-tenite at approximately 2200°F (1205°C). The s, however, was present at all temperatures up to the solidus temperature of the steel at approximately 2375°F (1300°C). Ferrite was not found in any condition of the steel. The faintness of some of the s lines in X-ray patterns obtained from samples of the steel made it desirable to isolate the s prior to verification of its entire pattern. It was found that the s phase could be separated from samples of the steel which had been water quenched from 2250°F (1230°C) by dis-

Jan 1, 1955

(Under this heading will be published notes sent to the Secretary of the Institute by members or other persons introduced by members) Member, Graduate Colorado School of Mines. Four years' experience in West and Northwest. Two years with American Smelting and Refining Co. Wishes to join field party on geological work, mining or areal, where opportunity will be given to be of direct assistance to chief of party in solution of field problems. Age, 26. Unmarried. At liberty June 1. No. 342. Member, technical graduate, aged 30, with' 7 years' experience in concentrating and mining, desires a position of authority with reliable company. At present employed. No. 343. Member. Ambitious, energetic, tactful engineer, college graduate, married, aged 30, desires location with a large coal mining organization. Seven years with present employers -n middle west; has had broad experience in the past eight years on examination, development and construction; successful record in handling men. Position must carry responsible work and a future. Will go anywhere for proper opportunity. Exceptional references as to reliability, character and capacity for work. No. 344.

Jan 3, 1917

By William E. Ford, Edward Salisbury Dana

URANINITE. Cleveite. Broggerite. Nivenite. Pitchblende. Isometric. In octahedrons (o), also with dodecahedra1 faces (d) ; less often in cubes with o and d. Crystals rare. Usually massive and botryoidal; also in grains; structure sometimes columnar, or curved lamellar. Fracture conchoidal to uneven. Brittle. H. = 5'5. G. = 9'0 to 9'7 of crystals; of massive altered forms from 6'4 upwards. Luster submetallic, to greasy or pitch-like, and dull. Color grayish, greenish, brownish, velvet- black. Streak brownish black, grayish, olive-green, a little shining. Opaque. Comp. -A uranate of uranyl, lead, usually thorium (or zirconium), often the metals of the lanthanum and yttrium groups; also containing the gases nitrogen, helium and argon, in varying amounts up to 2'6 p. c. Calcium and water (essential?) are present in small quantities; iron also, but only as an impurity. The relation between the bases varies widely and no definite for- mula can be given. Radium was first discovered in this mineral and it has been shown that it and the helium present are products of the breaking down of the uranium.

Jan 1, 1922

New York State Museum, Albany, N. Y. D H. Newland, State Geologist. A complete list of publications or the latest lists of available publications will be sent upon application. A series of Bulletins on The Mining and Quarry Industry of New York are available as follows: Bulletin 51 (1910), 15 cents; 161 (1911), 20 cents; 166 (1912), 20 cents, 174 (1913), 20 cents; 190 (1915), 15 cents; 277 (1925-26), 50 cents; 295 (1927-1929), 40 cents. Another series discusses the Geology of the State by Quad¬rangles, available as follows: Bulletin 153, Broadalbin Quad (1911), 25 cents; 154, Sche¬nectady Quad. (1911), 20 cents, 170, North Creek Quad . (1914)

Jan 1, 1933

By B. J. Guarnera

There have been major changes in the makeup and nature of the uranium exploration industry in recent years. Significant price increases precipitated an increase in exploration activity-according to the Department of Energy, exploratory drilling in 1977, by 140 companies, was almost 8 million m (26 million ft). This represents a 37% increase over the prior year's drilling. Projections for 1978 indicate at least 9 million m (30 million ft) of exploratory holes will be drilled in the US. Exploration expenditures in 1979, including land acquisition, drilling, and other costs, were estimated by DOE at over $236 million. Domestic expenditures for 1978 are estimated at over $250 million.

Jan 10, 1978

Jan 1, 1948

Jan 1, 1948

By Robert S. Young

During the last quarter-century, exploration for metallic deposits in Maine has been sporadic with peaks generally coinciding with periods of high metal prices. Known cases of regional or semi-regional evaluations are few; most efforts have been local and usually intensive. On the basis of broad geologic groups, the State has been divided into five fundamental environments: ( 1) coastal metamorphic belt; (2) southern volcanic belt; (3) Silurian slate belt; ( 4) northern volcanic belt; and ( 5) Devonian slate belt. Although not restricted to these areas, exploration in recent years has been concentrated in the northern and southern volcanic belts. Notable examples of recent exploration activity, directed to sulfide minerals, include: ( 1) the Knox County nickel-copper-bearing ultramafic rocks; (2) the Harborside (Cape Rosier) copper-zinc deposit; (3) the Second Pond (Black Hawk) zinc-copper-lead-silver deposit; ( 4) the Big Hill-Barrett lead-zincsilver- copper-gold zones; (5) the Parmachenee copper-zinc belt; ( 6) the Moxie Lake nickeliferous peridotite; and (7) the Attean quartzmonzonite molybdenum-copper occurrences. The Second Pond and Harborside prospects appear to be close to production. Systematic investigations for non-metallic deposits appear to have been aimed principally toward limestone, asbestos, diatomaceous earth, and spodumene-bearing pegmatites. Advances in prospecting methods, high metal prices, a favorable business outlook, increasing cooperation from large landholders, and some discoveries support the probability of increased exploration activity in Maine during the coming decade.

Jan 1, 1968

By William R. Jones, Robert M. Hernon

This report on the Central mining district of New Mexico is the partial culmination of an intensive U.S. Geological Survey effort dating back some 30 years. Robert M. Hernon went to Silver City in 1948 to finish a detailed restudy of the district that had been started in the thirties by Samuel G. Lasky. He was joined by William R. Jones in 1951, and Jones took over as project chief when Hernon resigned to do consulting work in 1953; it was under Jones' guidance that most of the work was brought to completion or nearly so ( 17, 22-24, 26-30). Hernon returned to the Survey in 1958 to work in .the southern Appalachians. Early in 1965 Jones urged that Hernon be reassigned to the Silver City project to help complete the Professional Paper report on the ore deposits of the Santa Rita quadrangle as well as to take over preparation of the report on the Central district for the Graton-Sales volume. This reassignment was approved, and Hernon began work on the present report. By late June he had completed most of it in draft form, and on June 28 Jones and Hernon left Denver for a short trip to Silver City to fill in a few gaps and to reacquaint Hernon with activities in the district, which he had not visited for 12 years. Late in the afternoon of June 29, 1965, as Bob and Bill were 85 miles short of their destination, their jeep collided head-on with a truck that was attempting to pass another vehicle in a cloud of dust. They both died instantly. As the most recent surviving member of the Silver City project (1958-1962), I was given the honorable though rather sorrowful task of putting the Hernon-Jones report "in shape" for publication. Fortunately the manuscript was already in good shape, so that the task has consisted of little more than minor reorganization and editing, and of preparation of the illustrations, abstract, and bibliography. The sections on wall-rock alteration had been left for Jones to complete in the light of his recently intensified interest in alteration geochemistry (25), and it is in these sections only that. the report may fall short, for they have been filled in from a 1958 manuscript by Jones on the ore deposits of the Santa Rita quadrangle that he intended to revise considerably. The shortcomings, however, are largely in the interpretation, not in the field data. As a brief but accurate summary of what was known about the geology of the Central mining district in 1965, this report stands as a fitting testimonial to the scientific dedication of two exceptional men.

Jan 1, 1968

By C. R. Van Hise

PART I.-GENERAL PRINCIPLES. [ ]

Jan 1, 1902

By Edward Griffith

The anthracite industry, which produces about 50 million net tons of coal annually, has been talked of as being able to last for another century; but if the water record of the past century continues into the expected century, this expectation of many years production still to come out of the remaining reserves will not be attained. The industry will be a submerged one in fact as well as in name. A recorded forecast of what has since occurred appears on page 34 of the Mine Inspectors' reports of 1897: It should also be noticed that bodies of water had accumulated in parts of abandoned mines before duplicate surveys of the same were required by law; and as a result we have today to contend with bodies of water, the exact location and position of which are not correctly known. Since that date, 47 years ago, the implications of the foregoing comment have grown enormously. This is shown in Fig. I and in the following table showing flooded and partially flooded areas that have come into existence since the early 1930's in the northern anthracite field: Number of Year Flooded Areas 1932...................... 2 1933...................... 3 1934..................... 3 1935...................... 5 1936...................... 7 1937...................... 9 1938.................... 11 1939...................... 11 1940...................... 11 1941...................... 14 1942...................... 14 1944...................... 26 Similar conditions exist in other fields in the anthracite region. In the period between 1923 and 1940, abandonment of collieries in the southern field resulted in the flooding of approximately 60 sq. miles (30 per cent) of the field. The ahandonment of collieries in this field has imposed additional expense for pumping on the collieries still operating. This condition will be aggravated by the extension of developments and cause suspension of operations if economic conditions do not justify the assumption of additional pumping costs. During the years, the region's rainfall has not altered, but the quantity going inside the mines through breakages in the surface, brought about by extraction of the coal, has increased materially, as indicated by the ratio of tons of water pumped to tons of coal produced underground for one of the large companies in the northern anthracite field: Year Ratio 1920................. 8.4:1 1925.................. 10.6:I I930.................. II.4:I 1935................. 26.2:1 1940.................. 32.7: I 1942.................. 30.3:I The data in Table I shows the total amount of water pumped and its ratio to underground production for one of the large companies in the southern anthracite field, and shows a rapidly growing serious situation. Rainfall quickly affects the workings in all the fields. In mine inspection district 7 of the southern field the rainfall in 1935 was 92,083,000,000 gal. The total water pumped was 36,274,000,000 gal. (39.4 per cent of the rainfall). The operating mines

Jan 1, 1947

By Edward Griffith

The anthracite industry, which produces about 50 million net tons of coal annually, has been talked of as being able to last for another century; but if the water record of the past century continues into the expected century, this expectation of many years production still to come out of the remaining reserves will not be attained. The industry will be a submerged one in fact as well as in name. A recorded forecast of what has since occurred appears on page 34 of the Mine Inspectors' reports of 1897: It should also be noticed that bodies of water had accumulated in parts of abandoned mines before duplicate surveys of the same were required by law; and as a result we have today to contend with bodies of water, the exact location and position of which are not correctly known. Since that date, 47 years ago, the implications of the foregoing comment have grown enormously. This is shown in Fig. I and in the following table showing flooded and partially flooded areas that have come into existence since the early 1930's in the northern anthracite field: Number of Year Flooded Areas 1932...................... 2 1933...................... 3 1934..................... 3 1935...................... 5 1936...................... 7 1937...................... 9 1938.................... 11 1939...................... 11 1940...................... 11 1941...................... 14 1942...................... 14 1944...................... 26 Similar conditions exist in other fields in the anthracite region. In the period between 1923 and 1940, abandonment of collieries in the southern field resulted in the flooding of approximately 60 sq. miles (30 per cent) of the field. The ahandonment of collieries in this field has imposed additional expense for pumping on the collieries still operating. This condition will be aggravated by the extension of developments and cause suspension of operations if economic conditions do not justify the assumption of additional pumping costs. During the years, the region's rainfall has not altered, but the quantity going inside the mines through breakages in the surface, brought about by extraction of the coal, has increased materially, as indicated by the ratio of tons of water pumped to tons of coal produced underground for one of the large companies in the northern anthracite field: Year Ratio 1920................. 8.4:1 1925.................. 10.6:I I930.................. II.4:I 1935................. 26.2:1 1940.................. 32.7: I 1942.................. 30.3:I The data in Table I shows the total amount of water pumped and its ratio to underground production for one of the large companies in the southern anthracite field, and shows a rapidly growing serious situation. Rainfall quickly affects the workings in all the fields. In mine inspection district 7 of the southern field the rainfall in 1935 was 92,083,000,000 gal. The total water pumped was 36,274,000,000 gal. (39.4 per cent of the rainfall). The operating mines

Jan 1, 1947

By R. R. Vandervoort

The creep behavior of Nb(Cb), Ta, Mo, and W was determined under conditions of constant atomic dif-fzisivity, constant stress to elastic modulus ratio, and nearly equivalent grain size, and the steady-state creep rates obtained from these tests were correlated with calculated stacking fault energies for the metals. These results, in conjunction with similar data for several fccMetals,13 suggest that stacking fault energy may influence the creep strength ofbcc metals. The interrelationship between steady-state creep rate, subgrain size, and stacking fault energy was examined. It was found that the subgrain size for a given creep stress, increased as stacking fault energy increased, but that this relationship did not cormpletely account for the effect of stacking fault energy on creep rate. The crystallography and energetics of stacking fault formation in bcc metals has been discussed by a num-ber of authors,1-5 and impurity stabilized stacking faults on (112) planes have been observed in Nb,6,7 w,8,9 Fe,] and V" by transmission electron microscopy. However, a crucial question is whether or not stack-ing faults influence the mechanical strength of bcc metals. Potentially, stacking faults could increase strength by reducing the mobility of the partial dis-locations bounding the fault, by acting as barriers to slip dislocations, and by retarding the climb of dislo-cations during high-temperature deformation. The objective of this study was to seek a correlation be-tween creep strength and stacking fault energy for several bcc metals; namely, Nb, Ta, Mo, and W. The creep behavior of most polycrystalline metals and alloys at high temperatures and moderate stresses can be described by the following relation:11,12 im=Af(s) where i, = minimum creep rate, A = constant, j(s) = a function involving metallurgical structure, a = applied stress, E = average elastic modulus at the test tempera-ture, w = constant (equal to 5 for most pure metals), D = diffusion coefficient. One factor in the structure function F(s) which sig- R. R. VANDERVOORT, Member AlME is Research Metallurgist, Process and Materials Development Division, Chemistry Department, Lawrence Radiation Laboratory, University of California, Livermore, Calif. Manuscript submitted February 28, 1969. IMD nificantly affects the creep resistance of fcc metals is stacking fault energy, and creep rate has been shown to vary directly with stacking fault energy to the 3.5 power." In the latter investigation, four fcc metals of widely different stacking fault energies (Ag, Cu, Ni, and Al) were creep tested at a constant stress to modulus ratio of 1.21 x 10-4, at a constant diffusivity of 2.7 x 10-12 sq cm per sec, and at nearly equivalent grain sizes of about 0.7 mm. The creep data were then correlated with stacking fault energies. In the present study, a similar procedure was followed. All materials used in this work were consolidated by powder metallurgy techniques. Impurity contents in the as-received materials are listed in Table I. Chemical analyses showed that no measurable contamination of the test specimens occurred during pretest annealing treatments or creep testing. Specimens with a gage section 0.75 by 0.125 by 0.050 in. were creep tested in tension in a vacuum of less than 10-9 torr. Deformation at temperature was measured by tracking fiducial marks on the gage section of the specimen with an optical comparator. Optical deformation measurements also permitted observation of the macroscopic characteristics of the deformation Table I. Typical Specimen Impurity Content, ppm Nb Ta Mo W C 45 10 155 6 O 185 30 4 10 N 30 6 3 2 H 5 I 1 <1 als 3 10 2 15 Ca <5 I3 5 Cr 5 <3 10 <5 Cu 10 50 2 15 Fc 10 10 150 35 Ni 2 150 20 <5 Si <I0 1 3 <10 Ta 100 Ti 10 8 1 Zi 15 50 1 3 Table II. Test Conditions for Constant Stress-Modulus Ratio of 6 X 10.&apos; and Constant Diffusivity of 2.7 X 10-12 sq cm per see, and Grain Size Values for the Given Pretest Annealing Treatments Literature references Pretest Annealing for E and D Treatment Stress, Temperature, ___"&apos;Values__ Grain Tempera-Metal psi "C E D Size, mm ture, .C Time hr Nb 745 1525 14 15 to 17 0.83 1650 I Ta 1220 1770 18 19.20 O.91 1800 I Mo 1975 1630 18 21 0.77 2200 I W 2140 2265 18 22 040 2400 5

Jan 1, 1970

Thomas H. Beddall, so we are informed by Major J. B. Carlock, has been promoted and is now Adjutant of the 1st Battalion, 1st Gas Regi¬ ment. He was awarded, last summer, the Croix de Guerre. R. A. Bull. See letter in Proceedings of Milwaukee Meeting. Captain Stanley C. Bullock&apos;s record since entering the service is given as follows in a letter recently received from Mrs. Bullock: Resigned position of mine manager in Chile in November, 1915, to return to England to obtain commission in Royal Engineers. Joined Officers&apos; Training Corps, Dec. 20, 1915. Commission gazetted, Jan. 27, 1916, 2d Lieut., R. E. Landed in France, Feb. 6, 1916. Posted to 179th Tunnelling Co., R. E. Took part in following battles: Somme, 1916; Ypres;1917; Arras, 1917; Somme, March and July, 1917; Messines, 1917. Gazetted: Acting Captain, July 11, 1916; Temp.-Lieutenant, Oct. 26, 1916; Captain, Sept. 29, 1918. Awarded Military Cross, Jan. 1, 1918, for conspicuous bravery and devotion to duty under a heavy enemy gas bombardment, when, by his example and perseverance in spite of every difficulty and obstacle, mining work was successfully completed which was vital for the success of the operations. The Cross was presented to Capt. Bullock by the King, on Sept. 25, 1918. First Lieut. J. J. Cadot, in a letter sent to Mr. H. `V. Hardinge from France, says he has been at the "Front." He also mentions that the Boche "is a good sprinter."

Jan 12, 1918

By Frank G. Snyder

The Precambrian of Midcontinent United States includes a metamorphic belt of probable Middle Precambrian age, a belt of Keweenawan volcanics and sediments, and widespread igneous activity that extended from Iowa to Texas. Most of the present structural configuration of the Midcontinent was developed by epeirogenic movements during the Paleozoic. The dominant elements are basins and arches. Three major metallogenic provinces occur in the Midcontinent. They include the Missouri Precambrian iron ores, the Lake Superior copper ores, and the Mississippi Valley lead-zincbarite- fluorite deposits. Several large iron deposits, occurring in rhyolite and andesite host rocks, are known. Both discordant massive bodies and replacement- type bodies occur. The iron deposits are believed to have been formed during the period of igneous activity. They are essentially the same age as the volcanics and older than the granites that intrude the volcanics. The Lake Superior copper ores include two established districts, the Keweenawan district and White Pine, and the copper-nickel deposits in the Duluth gabbro. The lead-zinc-barite-fluorite deposits include four major districts, Southeast Missouri, Upper Mississippi Valley, Tri-State, and Illinois-Kentucky, and at least eight minor districts. Ore may occur in stratiform deposits and in veins. The major districts all contain stratiform deposits, but several have produced appreciable quantities of vein ore. Only vein deposits are known in some of the smaller districts. The major features of all districts can be catalogued in terms of host rocks, structural patterns of districts, types of ore-bearing structures, and mineralogical characteristics. From these features, a Mississippi Valley type ore body, in its type area, can be defined.

Jan 1, 1968

By J. Hoover Mackin

The iron ore bodies of the Iron Springs district are replacement deposits of magnetite and hematite in Jurassic limestone around the borders of three intrusions of quartz-monzonite porphyry. Production in the period 1923-1965 was about 72,000,000 tons, nearly all of which was direct-shipping ore from open pits. The intrusions are laccolithic in form; all three were emplaced at the same stratigraphic horizon, which had been a zone of decollement gliding during the Laramide orogeny. The intrusions and associated volcanic rocks are post-orogenic. There was no change in the thickness of the limestone during the metallization. Comparison of the composition of the limestone and stratigraphically equivalent replacement ore indicates that, with every million tons of iron, there were additions of 40,000 tons of silicon, 20,000 tons of magnesium, and 10,000 tons of aluminum. The ore-forming fluid was derived from the exposed porphyry. The iron was first incorporated in hydroxyl-bearing mafics, which crystallized in depth and were carried upward in the magma that formed the hypabyssal intrusions. The mafic phenocrysts decayed deuterically in the new environment, releasing iron into the interstitial fluid of a consolidating crystal mush in the interior of the intrusions. Primary tension joints, which opened in areas of late intrusive distention, served as roots through which the ore-forming fluid was drawn from the crystal mush.

Jan 1, 1968

By E. P. Sadowski, R. J. Raudebaugh

A study of micro structural characteristics of a 30 pct Cr, 42 pct Ni, 26 pct Fe alloy has been correlated with its behavior in creep and rupture tests at 1400°, 1600°, and 1800°F. Nitrogen pickup observed at 1600" and 1800°F was associated withfissur-ing of specimens prior to fracture. IN studying the high-temperature characteristics of a nominally 30 pct Cr, 42 pct Ni, 26 pct Fe alloy certain anomalies were observed, namely: The alloy had greater stress rupture and creep strength at 1800" than at 1600° F for time periods beyond 550 hr. As placed in test, this alloy was nonmagnetic. After test, some specimens were found to be fairly magnetic. The gain observed in magnetic response was not solely a function of time and temperature of testing. This is a report of the observations and a recounting of the results of studies made in an attempt to explain the behavior of the material under investigation. MATERIAL AND PROCEDURE All test material was taken from a production size heat of an experimental alloy melted and processed using commercial practice and having the following percentage composition: C Fe Cr Ni Ti 0.05 25.83 30.13 41.59 0.41 Al Mn Si S Cu 0.42 0.75 0.45 0.011 0.34 The material was tested in two conditions, namely mill-annealed and grain-coarsened. Mill annealing, which consisted of heating to about 1900° F in a continuous furnace for about 30 min and air cooling, gave a grain size of ASTM 8 and finer. To produce the grain-coarsened condition, mill-annealed material was soaked for 2 hr at 2050°F in a laboratory furnace and air cooled. This resulted in an ASTM grain size of 4 to 5. Rupture tests were carried out at 1400, 1600, and 1800° F in accordance with ASTM procedures. In tests where only rupture life and elongation at fracture were determined, specimens of 0.252 in. diam and 1 in. gage length were used. In tests where creep curves were obtained, specimens were of 0.375 in. diam and 4 in. gage length. Several of the tests under relatively low stress were discontinued short of rupture. Three low-stress tests are still in progress at this writing. Structural changes which occurred during testing were determined from examination of the tested specimens by light microscopy and X-ray diffraction. Diffraction pattern recordings were made with a diffractometer using copper radiation on samples heavily etched in a picric-hydrochloric

Jan 1, 1960

By Frederick Rhines

PURE copper that has been allowed to oxidize at an elevated tempera-ture in the air is found to be covered with two distinguishable layers of oxide scale. The outer of these, which is very thin, is composed of cupric oxide, while the inner layer, comprising the bulk of the scale, is made up chiefly of cuprous oxide (Fig. 1a). If a small quantity of an alloying element, such as silicon, is present in the copper, silica particles are found disseminated through the cuprous oxide, deposited most abundantly near the metal surface, and, in addition, silica particles occur to a limited depth within the copper itself (Fig. 1b). It is this inner layer, composed of oxide particles precipitated in a matrix of metallic copper that is known as the "subscale" or the zone of internal oxidation. Under a low oxygen pressure it is possible to produce the subscale without the formation of external layers of copper oxides, thus leaving the metal surface bright and apparently clean while oxidation has occurred, in fact, to a considerable depth within the metal (Fig. 2). Although little is yet known in a detailed way of the mechanism of internal oxidation, the general nature of the process is evident. By virtue of the considerable solubility of oxygen in copper,1 it is possible to bring the alloying element in contact with oxygen within the metallic solid solution. If the oxide of the alloying element is more stable than cuprous oxide, the foreign oxide may form and, since most oxides are relatively insoluble in copper, it will not long remain in solution, but will separate as a precipitate. As the metallic solute is exhausted in the zone of precipitation, oxygen that is constantly being supplied at the surface diffuses farther into the alloy and thus produces an ever-thickening shell of subscale. The distribution of the reacting elements in the subscale and adjoining zones must be somewhat as indicated in Fig. 3. The conditions requisite to internal oxidation to be anticipated are thus: (1) a solubility of oxygen in the alloy, (2) the ability of oxygen to diffuse at an appreciable rate into the alloy, (3) the possibility of the

Jan 1, 1940