Search Documents

All the TECHNICAL PUBLICATIONS and CONTRIBUTIONS published in 1935 are available at Institute headquarters, unless otherwise noted. They are also on file in many public, university and technical libraries and, when so indicated in the list, may be found in the TRANSACTIONS. Copies of the TECHNICAL PUBLICATIONS have been mailed to members of the Institute that are registered in the different classes: A-Metal Mining; B-Milling and Concentration; C-Iron and Steel Division; D-Nonferrous Metallurgy; E-Institute of Metals Division; F-Coal Division; G-Petroleum Division; H-Industrial Minerals Division (Nonmetallics); I-Mining Geology; J-Mineral Industry Education Division; K-Mining Administration; I-Geophysical Prospecting. Other members may obtain copies by writing to the Secretary. Copies of CONTRIBUTIONS may also be obtained from the Secretary's office. Additional copies are sold at the rate of 1 cent per page; minimum charge, 25 cents. Nonmembers may purchase the papers at the prices mentioned. [ ]

Jan 1, 1936

Members whose deaths were reported from Mar. 5, 1919, to Apr. 5, 1920. Elected Died 1895 ANDERSON, ROBERT HAY 1920 1916 ATWATER, M. W 1919 1905 BARD, D. C 1920 1893 BECKER, GEORGE F 1919 1914 BIGELOW, BRAXTON 1917 1917 BLACK, HERBERT F 1919 1911 BOWLER, ROBERT P 1919 1902 BROWN, ARTHUR H 1919 1913 BURNHAM, WILLIAM 1918 1905 Carnegie, Andrew 1919 1900 CARPENTER ROLLA C 1919 1908 CONNER H. MCKEAN 1919 1883 COOK, ROBERT A 1919 1903 COOPER, JOHN 1919 1875 CROXTON, SAMUEL W 1919 1889 DICKMAN, R. N 1919 1893 DUFOURCQ, EDWARD L 1919 1917 FAY, CHARLES H 1918 1875 FOHR, FRANZ 1919 1879 FRICK, H. C 1919 1880 GAYLEY, JAMES 1920 1917 GARVIN, JOHN C 1920 1915 GIBBS, CHARLES H 1919 1917 GODBE, RALPH T - 1918 GREGORY, A. E 1919 1917 HAMILTON, A. McL 1918 1914 HEISE, HENRY C - 1913 HINCKLEY, E. R 1918 1884 JENNINGS, HENNEN 1920 1895 JOHNSON, J. E., JR 1919 1895 KANN, MEYER M 1919 1895 KAYSER, H. W. F 1919 1918 KENNEDY, DANIEL J 1903 KING, PAUL S 1919 1901 LANGTON, JOHN 1920

Jan 1, 1923

The Lead-Line Update held in conjunction with the 1977 SME-AIME Fall Meeting in St. Louis provided sessions on mining, mineral processing, extractive metallurgy, and economies to brief the record on the industry's activities and developments since the 1970 World Symposium on Lead and Line convened, also in St. Louis. Changes in the industry since 1970 have not been profound, notes the program committee, consisting of D. O. Rausch, F. M. Stephens, and B.C. Mariacher, cochairmen; and H. L. Clifford, S. C. Fall), and M. Snedeker. However, various environmental and conservation factors have had a direct impact on process consideration and operating practice; the result has been new mines, improved technology, and changing market opportunities. The general consensus of the participants is that the future for the Lead-zinc industry looks promising as new applications are found and new products resulting from intensive research reach the marketplace. The highlights of the HS technical papers presented at the 1977 session follows.

Jan 11, 1977

"Acta Metallurgica" Dennis Carney, '59 Alfred Noble Joint Prize Committee F B Foley, Dec '61 American Association for the Advancement of Science F T Agthe, Dec '59, William L Fink, Dec '60 American Geological Institute Arthur Montgomery, Oct , '59, F C Kruger, Oct '60 American Power Conference J P Weir, T D Hess American Society for Testing Materials

Jan 1, 1959

F A. THOMSON, president of the Montana School of Mines, gave an interesting talk on mining schools of the past, present and his ideas of the future before a recent meeting of the Montana Section of the A. I. M. E. He covered the history .of the various mining schools and com- pared the three main types of schools; those attached to or forming part of an endowed college or university such, for example, as' the Columbia School of Mines, the Mining Department of the Massachusetts Institute of Technology and the Mining Department of Stanford University. These resemble in a general way the second class, those attached to the state universities and colleges. The schools of this general type have had varied success.

Jan 1, 1928

By Harold Margalin, Elmars Ence

M. H. Mueller, M. V. Nevitt, and H. W. Knott (Argonne National Laboratory)—We have reported1 the crystal structure of Ti2CU as body centered tetragonal with a. = 2.944A and co = 10.786A, six atoms per unit cell, and space groupl4/mmm(MoSi2 type). This cell is larger but definitely related to the unit cell reported by the authors. It permits definite positions for the titanium and copper atoms in the cell located as follows: 2 Cu (a) 0 0 0; 1/2 1/2 1/2 4 Ti (e) 0 0 z; 1/2 1/2 1/2 + z; 0 0z; 1/2 1/2 1/2- z where z = 0.341 The face centered tetragonal cell reported by the authors can be transformed to a small body centered tetragonal cell with flo (small bet) = ao(fct)v2 Both unit cells have the same CO. Neither the face centered tetragonal cell with four atoms per unit cell nor the small body centered tetragonal cell with its two atoms per unit cell lend themselves conveniently to an orderly arrangment of the 2 to 1 ratio of titanium to copper atoms. When the co of this small body centered cell is tripled, however, a large body centered tetragonal cell results with six atoms per unit cell as described above. We had also noted that the X-ray patterns of Ti2Cu indicated that the structure could be approximately described by the face centered tetragonal cell as reported by the authors; how- ever, there was evidence for a few additional very weak lines whose positions indicated a larger unit cell. Since the X-ray scattering amplitudes of titanium and copper are nearly equal, it is evident that it is difficult to distinguish their positions especially from X-ray powder patterns. It was therefore decided to look at a powder pattern obtained by neutron diffraction since the scattering amplitudes of the two elements are considerably different in magnitude and opposite in sign. The sample used for neutron diffraction was selected from a group of three alloys prepared by arc melting using crystal bar titanium of 99.92 pet nominal purity and 99.999 pet pure Cu. The alloys designated as A, B, and C had the following respective compositions: Ti-32.8 at. pet Cu, Ti-33.3 at. pet Cu, and Ti-33.8 at. pet Cu. On the basis of the melting losses incurred, it was established that the actual concentration of either component in any of the alloys probably did not deviate from the intended value by as much as 0.1 at. pet. The alloys were annealed for 5 days at 700°C in evacuated Vycor capsules and quenched in tap water. The metallographic structures of these alloys are shown in Fig. 1. None of the alloys contained sufficient second phase to permit its positive identification. Since alloy B contained the least amount of second phase and since its composition placed it closest to the ideal stoichiometry, it was chosen for the neutron diffraction study. The oxygen content of alloy B was found by chemical analysis to be 0.06 at. pet. This particular intermetallic compound is especially suitable for investigation with neutron diffraction since if the titanium and copper atoms have a random statistical distribution, a near null-matrix would result in which there would be practically no coherent scattering of neutrons, and hence no Bragg diffraction peaks. Such a condition could come

Jan 1, 1962

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The room-temperature Knoop hardness of single -crystal titanium diboride has been determined. Variations in microhardness have been correlated with orientation and structural imperfections in the crystals. Maximum differences in hardness values of 750 kg per sq mm with respect to orientation and 450 kg per sq mm with respect to substructure were found. The effects of etchants, load on indenter, and degvee of cracking of indentation were studied. The average hardness was determined as 2800 kg per sq mm on the as-grown crystals. Annealing increased the average hardness to 3375 kg per sq mm. ThE microhardness of polycrystalline titanium diboride approximating the stoichiometric composition TiB, has been studied by several investigators. The values for the Knoop hardness number range from 2710 kg per sq mm (Khn = 2710 kg per sq mm) to 3400 kg per sq mm.'-4 Samsonov et al.' reported a Vickers hardness number of 3400 kg per sq mm (Vhn = 3400 kg per sq mm) at 120-g loads for a 98 pct Ti + B material of 96 pct theoretical density. Recently Dunegan measured the Vickers hardness and obtained 2060 kg per sq mm with a 10-g load (Vhnlo = 2060 kg per sq mm), 1425 kg per sq mm for Vhnloo, and 1320 kg per sq mm for Vhnlooo. We have obtained a Khnloo = 3000 * 350 kg per sq mm for hot-pressed polycrystalline TiB2 that was 99.1 pct Ti + B and 96.6 pct of theoretical density. The present investigation has been made on single-crystal titanium diboride boules, and is believed to be the first such study on TiB, crystals of known orientation. EXPERIMENTAL The single crystals were prepared by a Verneuil-type process using an electric arc by the Linde Division of Union Carbide Corp. The largest specimens were 6 mm in diameter by 12 mm long. The crystals were of theoretical density (4.50 g per cm3) with a Ti + B content of 99.8 pct. The major impurities present were: 0.03 pct (by weight) 0, 0.06 pct C, 0.01 pct Si, 0.05 pct Fe, 0.01 pct Cr, and 0.01 pct Ni. The crystals were boron-rich, the average boron content being 31.S7 wt pct (stoichiometric value is 31.12 wt pct), and titanium-poor, the average titanium content being 68.2 wt pct (stoichiometric value is 68.88 wt pct). Titanium was determined gravimetrically by cupferron precipitation and boron by titration of H3B03 from a NaOH-fused specimen after removal of titanium with BaC03. The outer edge of the boule accounted for some of the excess boron. An electron-microprobe analysis showed that the titanium content increased from 60.0 wt pct at the edge to 68.5 wt pct at D, ~ 1000 p, where D, = distance from outer edge (see Fig. 5). X-ray measurements indicate that the boules are single crystals with considerable substructure. Upon etching this structure is seen in the form of a Widmanstatten-type rhombohedral line pattern in the basal (c) plane and a parallel "lines" pattern in the prism (a) planes. A typical WidmanstHtten-type pattern is seen in in Fig. 1. Electron microscopy reveals that the lines are less than 1 p across, which does not allow direct electron probe or microfocus X-ray determination of their composition. The identity of the second phase has not been established. It might be a higher boride or a nonstoichiometric TiB2. On annealing above 2200°C the precipitate is dispersed and dissolves in the matrix. The best etchants found were HF/HNO/HO, KF(CN)$NOH/HO (Murakami's Etch), and A large number of other etchants were previously Studied. The acidic etchant produced an acicular or "needles" pattern in the (a) planes which is an etchant effect on the "lines" pattern.

Jan 1, 1965

By AIME AIME

AT the Morenci branch of the Phelps Dodge Corporation, of which Frank Ayer is manager, several new types of machines that have been developed by Charles Mitchell, shop foreman in the drill steel shop, invite comment for their time and labor-saving qualities. Foremost of these is an adjustable gage-block and gaging device for attachment to drill-sharpening machines, developed and patent applied for by Mr. Mitchell. It replaces the blocks on the standard Ingersoll-Leyner drill steel sharpener No. 5. Features of the device are gage blocks with a flat surface which can readily be removed when worn and planed in any flat planer; blocks that can be adjusted with a templet to give a far more accurate gage than was formerly possible; and a center stop that is adjustable and can be accurately set to center any standard size drill steel.

Jan 1, 1930

Gus C. Henning, New York City: In taking up the discussion of these specifications it is necessary that I give definitions of what I understand under the term " Specifications." There may be three kinds, viz.: (1) Specifications in general; (2) Standard Specifications; (3) Standard International Specifications. 1. A Specification is a document used in commerce which should clearly define the qualities of material to be supplied by the producer, the tests which shall be applied for their determination, and the methods which shall be applied for the purpose of determining that the entire product shall possess such qualities, properties and finish as are desired. The terms used in such document must be applied in accordance with their strict technical definitions as used by those most conversant with them, and the language should be of such accuracy that there can be but a single interpretation of each and every clause. A specification is a part of a contract, and should be legally perfect and accurate. Inaccuracy of definition and dic-

Jan 1, 1903

Taking advantage of the lessons in administrative organizations which were taught by the war, Director Van H. Manning has put into effect a new form of organization in the Bureau of Mines. The Bureau is divided into two branches, one the investigations branch and the other the operations branch. F. G. Cottrell, who has been chief metallurgist of the Bureau, has been promoted to the position of assistant director and will be in charge of the investigations branch. F. J. Bailey, who has been chief clerk of the Bureau, has been placed in charge of the operations branch with the title of, assistant to the director. All research and technical control will be exercised through the investigations branch, while the non-technical work, administrative duties, and dissemination of the results of the Bureau's activities will be handled by the operations branch. Under the investigations branch comes the division of mineral technology, in charge of Dr. C. E. Parsons; the division of fuels, under the chief mechanical engineer, 0. P. Hood; the division of mining, under the direction of George S. Rice, the chief mining engineer; the division of petroleum and natural gas, under the direction of J. 0. Lewis, the chief petroleum technologist; and the division of experiment stations, under the direction of D. A. Lyon.

Jan 9, 1919

By D. F. Coolbaugh

Successful mine exploration requires sound planning and modern exploration techniques, but it also requires perseverance and the right timing. The La Caridad mineral area has been known for over 70 years, but as with many mines, it was not "discovered" until viewed under new economic conditions and exploration philosophies. Present exploration of the La Caridad area began in 1964 and was carried out under a joint Mexican Government-United Nations Project. Detailed exploration was begun by Asarco Mexicana S.A. in late 1968. The geology of the La Caridad deposits conforms, generally, to the "porphyry copper" deposits of Arizona. However, breccias and pegmatites play a very important part in the emplacement of mineralization.

Jan 1, 1972

By J. F. Kemp

Introduction The Bulletin of the Institute for March, 1911, is chiefly devoted to papers upon the iron ores of northeastern Cuba. At that time information about the new developments in the peculiar brown hematites of the region was becoming widely circulated and interest was especially keen. For some years exploration had been conducted with pits and trenches and so great an area had been shown to contain ore in the Mayari, Moa, and Cubitas or San Felipe districts, that the reserves conveniently situated for the consumption of American furnaces were estimated as quite two billions of tons. In the subjoined footnote will be found a list of the principal papers of special interest which have already been published.1 The further remark may, however, be made that the

Jan 2, 1915

By W. Mckewan, W. M. Fassell

The oxidation rates of copper have been determined at temperatures from 600" to 900°C in oxygen from 14.7 to 400 psi total oxygen pressure. The oxidation rate of copper is unchanged by oxygen pressures within the range studied. The observed data extend Feit-knecht's conclusion concerning the pressure independence of copper from atmospheric pressure to 400 psi. All samples studied in the above-mentioned temperature and pressure range have both Cu2O and CuO present in the oxide film. NUMEROUS papers have been published on the oxidation of copper, some of which have noted the effect of oxygen pressure on the oxidation rate of copper. It must be noted, however, that no data on the oxidation rates of copper at pressure in excess of 1 atm have been reported in the literature. (Le Chatelier¹ reported that a black oxide of silver was formed at 300°C and 15 atm pressure.) This is likewise true for the other metals. This investigation was initiated to obtain experimental oxidation rate constants for pure metals at elevated temperatures and high oxygen pressure. Copper was selected as the first metal since probably more reliable data are available on its oxidation rates and related physical and chemical properties than for any other metal or alloy. As a general summary, the following conclusions appear well established for the oxidation of copper: 1—The oxide coating consists of Cu2O with a superficial coating of CuO providing the ambient oxygen pressure exceeds the equilibrium pressure for the coexistence of Cu2O and CuO.² The following sequence of phases is then Cu/Cu2O/CuO/O2 (gas). The Cu2O consists of large crystals that have no relation to the orientation of the metal crystals, except for a very thin layer adjacent to the metal." The CuO consists of very fine crystals randomly oriented. If the oxygen pressure is below the equilibrium pressure for the coexistence of Cu2O and CuO, the coating consists of Cu,O only. 2—The rate-determining factor in the parabolic oxidation of copper is the diffusion of Cu+ ions through the Cu,O layer.4,6,7 The Cu+ ions are accompanied by electrons to maintain electrical neutrality. The mechanism of the reaction at the Cu2O/CuO interface and the method of growth of the CuO is in some doubt. 3—On copper, there are three reported pressure effects: (a) At pressures below 0.3 mm Hg oxygen pressure, the oxidation rate increases directly with pressure.', ' .Vxygen starvation at the surface may account for this effect. (b) At oxygen pressures from 0.3 to 63 mm, the oxidation rate increases as the 7th root of the oxygen pressure providing the temperature is such that only Cu2O is present in the film. (c) At pressures from above the equilibrium pressure for the coexistence of Cu2O and CuO (varies with temperature) to atmospheric pressure, the oxidation rate is independent of the oxygen pressure.' Equipment In order to determine the oxidation rates of metals in an oxidizing atmosphere at pressures up to 400 psi, the equipment is somewhat different than for low pressure work as is shown in Figs. 1 and 2. A Leeds and Northrup Micromax recording controller (A) is used to control the temperature of the Ni-chrome furnace winding in conjunction with a Micromax electric drive unit. The drive unit adjusts a 20 amp Variac (variable transformer) to control the power input into the Nichrome furnace winding. Due to the "self heating" of the sample by oxidation, frequently encountered in oxidation rate studies, it is essential that the sample temperature be measured independently. This is done by means of a series of six chromel-alumel calibrated thermocouples located spirally around the oxidizing metal sample. Each thermocouple is partially shielded from the direct radiation of the furnace wall by

Jan 1, 1954

Executive R. C. ALLEN, Chairman ERLE V. DAVELER, Vice-chairman WILDER JUDSON R. M. ROOSEVELT G. B. WATERHOUSE Finance H. G. MOULTON, Chairman HENRY KRUMB PAUL D. MERICA H. T. HAMILTON, Consultant Admissions W. B. HEROY, Chairman GEORGE D. BARRON, Vice-chairman H. T. HAMILTON PHILIP KRAFT W. A. SINSHEIMER

Jan 1, 1937

By Earnest R. Woakes

Those engaged in pumping from shafts, or other mining works, may be intereited in the following suggestion of what is believed to be a novel method of raising moderate quantities of water against a considerable head. It is admitted that the ordinary Cornish pump, as generally used in mines, is hard to beat, on account of both its extreme simplicity and its easy adaptation to the requirements of mining; its great drawback, however, being the enormous weight of heavy rods and successive plungers that have to be kept in motion, not to mention the necessary " balance-" and " angle-bobs," with all their accompanying friction and wear and tear. It is contended that the following method would, to a great extent, overcome these drawbacks ; though, no doubt, many old miners may say it would also introduce new ones. Possibly, this may be the case. It is only desired that this pump may be judged upon its merits. The chief novelty of the method consists in employing the almost unlimited pressure obtainable from a high column of water, augmented, if necessary, by a hydraulic ram or press at the top, to work a small-diameter piston or plunger at the bottom of a shaft or well. This high-pressure plunger, indicated at E, in Fig. 1, transmits power direct to a larger-diameter plunger, F, constituting, together with the ordinary H-piece, valves, and wind-bore, the actual pump, which raises the water, by column C, to the adit-level or other discharge, placed as far as possible below the head of the high-pressure column A and ram W. It will thus be seen, that it is only necessary to maintain a prmsnre on the small piston, E, equal to that on the larger one, F, by means of the small but high column of water, A, in order to cause F to descend, and thus force the water up through C. The up-stroke is accomplished by a small water-wheel, or other engine, connected to the light rod or wire rope B, this having only to raise the weight of the actual plungers and fill the H-piece with water from the tank or

Jan 1, 1892

By O. W. Ellis

THE question of the influence of gases upon the properties of copper has received the attention of a number of investigators, among whom Sieverts,1 Iwasé,2 Lobley and Jepson3 stand preeminent. SOLUBILITY OF . GASES IN. COPPER Sieverts and Iwasé concerned themselves with the solubility of a variety of gases in the metal in the solid and liquid states. They determined the absorption coefficients of these gases and in all cases found a sharp change in solubility at the melting point of the metal. In this respect they disagree with Lobley and Jepson, who have based their opinions upon the appearance of small ingots of the metal which had been fused in an atmosphere of one or other of three gases and had then been rapidly cooled, while surrounded by gas, to the freezing point (rate-possibly 30° to 60° C. per sec.). The ingots that had been fused and cooled under nitrogen and carbon monoxide were free from blowholes and it was assumed that these gases were not absorbed in amounts much in excess of those which would dissolve in the solid metal; the ingots similarly treated under hydrogen were full of blowholes and it was assumed in this case that gas was ejected on solidification of the copper. The effect of varying the rate of freezing upon the character of the test ingots was not examined by these investigators; otherwise, it is felt, their views might have been subject to modification. Sieverts' most important contribution is that the solubility of a gas in any metal is proportional to the square root of its pressure or concentration. Knowing then the absorption coefficients of the various gases in copper, it should be possible to determine the analysis of the

Jan 1, 1928

By P. Barnes

(Read at the Wilkes-Barre Meeting, May, 1877.) THE tabular statement accompanying this note shows the money cost in each of the three departments of manufacture, of 17 leading items, and also the proportion (expressed in a decimal fraction) which each of these items bears to the total cost. The statement can hardly be taken for more than an average illustration of the clear showing of ratios and of results which may be made by such an arrangement, for not only will these items vary from month to month in any given works, but the methods themselves of manufacture differ widely in different works. It is obvious that such a statement, however useful it may be, must be submitted with but exceedingly little explanation or discussion, or with none at all, for the reason that to enter at any satisfac-

Jan 1, 1878

By WILLIAM WATERS

L HISTORY. THE Pierrefitte mines, situated in the South of France, in the district of the Hautes-Pyrenees, owe their name to the fact that the first mining operations of any extent, and of comparatively recent date, were carried out in the neighborhood of the vil¬lage of Pierrefitte, which is a branch terminus of the Midi railway. The Pierrefitte mines, however, embrace a wide extent of country and several different concessions, on most of which comparatively little exploration-work has been done. The portion of the property presently to be described is a zone running roughly E-W., over a distance of about 5 miles from the valley of Cauterets to the valley of Estaing, the ridge dividing these valleys being a spur of the main chain of the Pyrenees, and running more or less at right angles to it. According to local tradition, which various indications tend to confirm, these mines are of ancient date, the first workings being attributed to the Romans, who are supposed to have sought not only the lead but also the silver which is contained in the ore. Old slags have been found in the neighborhood which might well have been produced from the cupellation of lead-ores. These old workings, while of considerable extent at times, do not seem to have extended beyond a depth of 100 ft., even this depth being somewhat exceptional. The old notarial records of the district show that mines were known to exist, and that they were even worked, in the sixteenth century, but since the mines were abandoned (by the Romans or others) considerably prior to this period, very little

Nov 1, 1908

I. MCLAUGHLIN, R. P.-Protecting California Oil Fields from Damage by Infiltrating Water. Discussed by M. E. Lombardi, A. F. L. Bell, A. C. McLaughlin, R. P. McLaughlin, William A. Williams, Mark L. Requa, C. D. Keen 2413 BEST, W. N.-Petroleum as Fuel Under Boilers and in Furnaces. Discussed by William A. Williams, Hennen Jennings, David T. Day, Mark L. Requa, A. F. L. Bell, W. N. Best 2420 JOHNSON, ROSWELL H.-Sliding Royalties for Oil and Gas Wells. Discussed by William A. Williams, A. C. McLaughlin, A. F. L. Bell, Roswell H. Johnson 2423 BELL, ARTHUR F. L.-Important Topping Plants of California. Discussed by William A. Williams, David T. Day, A. F. L. Bell 2426 LOMBARDI, M. E.-The Cost of Maintaining Production in California Oil Fields. Discussed by C. D. Keen, Mark L. Requa, H. M. Bacon, M. E. Lombardi 2427 HUNTLEY, L. G.-Oil, Gas, and Water Contents of Dakota Sand in Canada and United States, Discussed by E. W. Shaw 2428

Jan 12, 1915

By H. H. Klepfer, M. E. Snyder

UNTIL very recently, the commercial availability of the rare earths as metals has been very limited. Fabrication of mill products from these metals has not been studied in most cases. This note reports the results of the development of fabrication techniques for thulium. Thulium has a melting point of about 1550°C and a hexagonal close-packed crystal structure. It oxidizes in air to give a black oxide (TmzO,). The procedures for producing thin thulium foil were developed on one ingot weighing about 220 g and were subsequently applied in processing about a pound of metal to foil. Several alternates for the various fabrication steps were investigated and will be discussed. The metal fabricated was in the form of commercial chill-cast ingots 1 in. in diam and 2 in. long weighing approximately 220 g. Impurities in the ingots were reported by the vendor to be 4000 ppni tantalum, 2000 ppm calcium, 200 ppm nickel, 100 to 200 ppm iron, 100 ppm europium, and less than 100 ppm copper, lutetium, and ytterbium. In addition to these impurities, several salt-like inclusions as large as l/8 in. in diam were revealed along the center line of the one ingot sectioned. Preliminary tests indicated that small wafers cut from the as-cast ingot would not fabricate readily by rolling. Forging of copper-jacketed wafers was therefore attempted. At 1550"F forging was satisfactory but an apparent reaction of copper with thulium demanded investigation of lower temperatures. Therefore, the remainder of the test ingot was forged at 1450°F—with only minor cracking. All ingots forged were inserted into copper tubes of 1 in. 1D and 0.125-in. wall thickness. The jackets were sealed by flattening the ends of the tubes and welding under helium. Heating time at 1450°F was 30 min. Press forgings of 1/8 in. per pass were used, followed by 10 min reheats. When the ingots had been squared and reduced to 0.250 in. in thickness, the original copper jacket was stripped off and replaced by a new jacket in preparation for hot rolling. Hot rolling at 1450" F without edge cracking was readily accomplished after forging. Excellent results were obtained with 10 pct reductions of thickness followed by 5 to 10 min reheats. After reduction of thickness from 0.250 to 0.100 in. the copper jacket was removed. It was found, in fact, that hot rolling in air was possible. A tenacious black oxide similar to that seen on zirconium was formed during 3 min reheats at 1450°F. Reduction in air to 0.010 in. foil was possible taking 10 pct reductions per pass. The oxide coat formed during hot rolling in air could best be removed by sand blasting and pickling. Common pickling solutions containing polar solvents were found to attack the metal too rapidly and a concentrated nitric-hydrofluoric acid mixture attacked neither the oxide nor the metal. The most satisfactory pickling solution was 52 vol pct concentrated nitric acid-48 vol pct glacial acetic acid. After forging to 0.250 in., vacuum annealing and cold rolling was found to be another satisfactory alternate to hot rolling in copper jackets. After forging. a hardness of Rockwell B76 was found. Annealing in vacuum (2 X l0-5 mm of Hg) for 1 hr at 1200"F did not alter this value. Annealing at 1470"F for 1 hr brought the hardness down to R;]63. With cold rolling (5 pct per pass) the hardness returned to about R,1:76 after 20 pct reduction and edge cracking became noticeable. However, cold rolling to a total of 40 pct reduction in thickness (RI,,83) was possible before edge crack propagation became serious. Good surface finish was obtained, and the metal loss due to oxidation was minimized by cold rolling and vacuum annealing. Using this procedure the yield of 1.25 in. wide by 0.010 in. thick foil from a 1-in. diam ingot was about 40 pct.

Jan 1, 1961