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By Thomas T., Read

IN this survey of the progressive development (of education for the mineral industries throughout the United States, the review of .the history of each school has usually been completed wherever it is first mentioned, but the history of the schools in the cities of the eastern seaboard was not carried beyond 1870. It is necessary now to cover what happened during the period of approximately the last quarter of the nineteenth century in several of the schools in the east. Philadelphia Of Philadelphia, it has been related in chapter 4 that the Polytechnic College of Pennsylvania began offering a curriculum leading to the B.S. in mining in 1853; that the school did not prosper, and finally closed about 1890. The establishment of a Department of Mining, Arts, and Manufactures at the University of Pennsylvania in 1855-56 was also mentioned, but its history was not carried beyond 1860. In 1859 J. Peter Lesley was appointed professor of mining in the University of Pennsylvania. The son of a cabinetmaker, born in Philadelphia Sept. 17, 1819, he had taken his A.B. degree at the University of Pennsylvania in 1838 and then secured a position on the Geological Survey of Pennsylvania under H. D. Rogers. When the Survey was discontinued, in 1841, he went to Princeton to study theology, was ordained a Presbyterian minister and followed that career until 1852, when the Pennsylvania, Geological Survey was again started and he rejoined its staff. He published "A Manual of Coal and its Topography" in 1856, and studied at the École des Mines, Paris, in 1856-57. He published an 800-page "Iron Manufactures Guide" the year that he was appointed to the staff at the University of Pennsylvania. In 1863-64 a College of Agriculture, Mines, Arts and the Mechanic Arts was established, but it was not a separate school

Jan 1, 1941

By D. W. McGlashan, K. N. Mcleod

IN the use of free bubbles with precise temperature control and continuous pH measurement, the contact angle apparatus differs from all previous equipment. Experimental procedures differ sharply from the captive bubble method1,2 of introducing the gaseous phase in the three-phase system. When freed from the tube and captured by a solid surface, a bubble more closely conforms to the spherical ideal set up by the usual mathematical analysis of surface free energy or surface tensional relationships of the forces involved. The assembled equipment, Fig. 1, departs from the usual contact angle apparatus in providing: 1) water circulation for fixing temperature, 2) instruments to measure and record pH during testing, and 3) a system for producing and using free bubbles. The apparatus allows testing over a broad range of closely controlled conditions, and the use of free bubbles gives contact angles independent of operator manipulation, which was unavoidable in the older captive bubble method. A bubble released below the specimen rises through the liquid and contacts the mineral. If the mineral is gas-avid the bubble adheres, developing a finite contact angle. Reaction cells (1), 2x33/8x5 3/16 in. ID, are of pyrex glass 5 mm thick. To prevent optical distortion, the sides are optical flats and are planed parallel to within five wave lengths of light over the entire surface. Special cement is required to withstand chemical attack and thermal shock. The cell is placed in a thermal jacket (2) made of welded aluminum. A water seal for the optical ports is made by using O-rings tightened against the flats of the cell by fine-threaded and adjustable ports, Fig. 2. In-flow water is discharged downward from a manifold located near the bottom of the cell jacket. Water overflows the weirs at each end of the cell jacket, discharging from both sides to a collecting manifold (24). A hose (26) leads the overflow water to the thermal-conditioner well (4), which is recessed to accommodate a reaction cell and two beakers (150 ml). Both the thermal jacket and the thermal-conditioner well are insulated to minimize the effects of temperature differentials. Water, discharging from the thermal-conditioner well, returns to a thermostat bath and pump (3), from which it is pumped to the thermal jacket. The thermostat bath permits temperatures to be adjusted from 1" or 2°C to 80°C and will maintain the selected temperature within 0.2ºC. An electrode support (22) groups the four electrodes (8) so that they fit conveniently into the reaction cell, Fig. 2. This assembly holds the glass electrode, the calomel electrode, the temperature-

Jan 1, 1957

By Evan Evans

WITH the expiration on April 30, 1941, of the agreement between the anthracite operators and the United Mine Workers of America, a new agreement was entered into, providing for a general wage increase of 7 1/2 per cent effective May 1, to be brought to a total of 10 per cent on Oct. 1. Contract rates were increased from the rates established under the agreement of September 1923, and hourly rates were raised above the agreement of May 1936 as modified from the eight-to seven-hour day in May 1937. The new rates are to be in force for the duration of the agreement, ending April 30, 1943.

Jan 1, 1942

By L. A. Creglow

IN common with many other companies engaged in the mining and processing of ores, research has always been an important activity of the United States Smelting Refining and Mining Company. Much of this research has been carried on at the various plants of the Company by the operating staffs, and over the years has been an essential factor in developing new methods and improving existing methods of operation. In 1917 arrangements were made with the Massachusetts Institute of Technology under which the Company had the exclusive use of one or two small laboratories in the then newly constructed MIT buildings and the use of the metallurgical laboratories, subject of course to the Institute's needs. After about two years this work was temporarily discontinued but was resumed in 1920 under the direction of G. H. Clevenger, consulting metallurgist for the Company, who recently retired. Becoming cramped for space, the laboratory was moved to a location near MIT on Amherst Street, Cambridge, in 1924. Establishment of a general research laboratory in metropolitan Boston naturally followed from the fact that the head office of the Company was located there and that the library facilities available for all types of research were, and are, unsurpassed. The disadvantages in carrying on research at great distances from the operating units of the Company were always apparent, but with widely scattered plants this disadvantage could not he overcome. With

Jan 1, 1948

By Cecil H. Desch

THE progress of metallurgical practice and the demands made by the engineering industry on our foundries and mills have made the crystalline structure of metals a subject of far more than academic interest. Metals and alloys are made up of crystals. Even if we accept the view, so ably maintained by some metallurgists, that the crystals are separated from one another by an amorphous layer, it remains true that all but a very minute fraction of any metallic mass is crystalline. The conditions which affect the growth of crystals are therefore of importance in metallurgy. It is not only castings whose properties depend on the arrangement of their crystals, for the more we learn of the behavior of forged, rolled and drawn metals, the more certain it becomes that it is profoundly influenced by the size and arrangement of the crystals in the original ingot, deter- mining a structure which may persist in a modified form through a long series of mechanical operations and annealings. This is mainly due to the concentration of much of the impurities in the last portions of the liquid to freeze, so that the boundaries between single crystals or groups of crystals are marked out by a zone of segregated material, differing in properties from the mass, and offering a barrier to diffusion and equalization of composition throughout the whole. The importance of this fact has been fully recognized by steel manufacturers, who have to deal with ingots which are sometimes very large, and are cast at a high temperature, containing impurities which have a marked effect on the properties even when present in very small quantity. For this reason the Iron and Steel Institute has set up a committee to examine the whole question of the heterogeneity of steel ingots,(l)f and a report has been issued, containing an account of the structure of 16 ingots, ranging in weight from 15 cwt. to 172 tons, each of which was sectioned and examined by chemical analysis and by etching. A valuable body of data concerning segregation has thus been collected. The work of the committee is being prosecuted with great activity, and at the same time researches are in progress to determine the physical

Jan 1, 1927

By Sanford Belden

My topic, Recent Developments in the Design of Electric Mine Locomotives and Mining Machinery, does not require me to go into a general review of electricity as applied to the mining industry. Interesting as that subject always is, what I might say in regard to it, by way of introduction, would be unnecessary use of your time, since such facts are familiar to all. First, we will consider the recent development of the electric mine locomotive. We may well pause for a moment to reflect upon its importance to the coal-mining industry of to-day. With the dawn of the electrical age its advent was inevitable. Our practical interest is aroused not so much by the first crude effort as by the great efficiency attained during the 30 or more years since the electric locomotive made its first appearance. To judge accurately what it means to coal mining, and through coal mining to the industrial field at large, we would have to know how many of these locomotives are in use throughout the country and their aggregate daily performance, and then compare the results with what could be expected with other forms of power. Such data are lacking, but it requires no statistician to make it evident that the electric mining machine is a tremendous factor in modern progress, and that without it the work of the world could never have reached its present magnitude. Not only has the electric mine locomotive served its own special branch of usefulness, but incidentally it has solved in the main the whole problem of electric transportation. It is but a step from the triumph of a 25-ton locomotive leading a long train of loaded coal cars from a mine to the electrification of common carriers. We may or may not be near any great change in this respect. Economical reasons may hold it back for an indefinite period. But the fact remains that in the development of our mine locomotives we have met this larger emergency, in mechanical type and efficiency, whenever it may come.

Jan 6, 1914

By Dudley L. Davis, E. C. Peterson

Introduction The Darwin District is 30 miles east of Olancha which is 220 miles north from Los z4ngeles via U. S. Highway No. 6. The ore deposits occur in the Darwin hills that have been elevated above the Darwin plateau by typical basin and range-type faults. Some of these faults have been active quite recently as shown by the displacemerit of Quaternary (?) basalt flows and the rejuvenation of erosion in Darwin wash. The ore bodies occur as fissure fillings and replacement of favorable beddings in a thick series of Paleozoic limestones, dolomites, shales and quartzites. Rich oxidized lead-silver ores were dis'Overed in the early seventies. BY 1875, Darwin had a population Of about 5000, and by 1880 several small mills and smelters had been built. Early exhaustion of surface ores, the isolated location of the district, and fluctuation Of metal prices caused intermittent operations until World War 11. The district production is estimated at about $3,000,000 prior to 1900 and perhaps $4,000,000 between 1900 and 1945 when Anaconda purchased the major producing mines. 'or the Past two Years, daily production has averaged 75 tons of direct shipping and 150 tons of milling-grade ore. At present, 300 tons of mixed oxide and sulphide ore are treated by flotation, the oxidized lead minerals being activated by addition of sodium sulphide after galena and sphalerite have been recovered from the circuit. Extraction averages 85 pct of the lead, 80 pct of the silver, and about 33 Pct Of the zinc in a bulk concentrate. The mill is designed so that minor changes permit selective flotation of pyritic lead-zinc ores encountered at depth. General Geology The oldest rocks in the Darwin hills are a series of Paleozoic limestones, dolomites, shales and quartzites probably pennsyl-vanian in age. These rocks have been intruded on the Rest by the Coso granite batholith and on the east by a granodiorite stock. Numerous sills and dikes grading from orthoclase granite to gabbro are exposed in the underground workings. The sedimentary rocks have been considerably folded and faulted, the most prominent structure being a northwest pitching anticlinal fold, the crest of which lies just west of the ridge line of the Darwin hills, The east limb of this fold has been intruded by the granodiorite stock and east of the stock the sediments show several closely spaced anticlines and synclines. The minor flexures on the west flank of the major fold are structurally important in localizing the ore in the Defiance and Essex mines of the Darwin group. There are three principal systems of faulting and fissuring, most of which are post-intrusive and premineral in age, with minor amounts of postmineral movement. The Darwin tear fault is the largest, most persistent fault in the district. It strikes N 60 to 75°W, dips steeply south and is traceable for about 10 miles. It is a normal

Jan 1, 1949

Charles Catlett, Staunton, Virginia (communication to the Secretary*): I have had occasion to examine a few of the irondeposits in the immediate section of which Mr. Watson speaks, but have not had an opportunity to visit any of the well-known manganese-deposits. I find the former can be very safely read in light of the information which it is possible to get from the same measnres farther. north, where they are less completely decomposed. In the same way all of his conclusions in regard to the geology of the manganese-deposits bear out their occurrence in Virginia, when we allow for the far more complete decomposition in the section he has so carefully studied. Judging from the same measures farther north, I think he will be safe in agreeing even further with Penrose as to the origin of these ores. Some years ago I carried on prospecting work in these measures in Virginia, in which the iron-ore and manganese-ore were followed down to undecomposed material, and in which their occurrence along a definite line of stratification, and apparently a part of the original bedding, was plainly shown. This is unusual, however, even in the section of which I speak. At Crimora, Virginia, the decomposition is quite complete; at the same time the results of some hydraulic work, which has been done there, disclosed, at the time of my last visit, the manganese interbedded in the residual clay along a definite and distinct plane parallel to the bedding of the underlying quartzite, and which, as is shown at other points, corresponds with the plane of the original material. In view of the phosphorus reported by Mr. Watson as existing in the Cartersville ores, and the not uncommonly prohibitive amount in southern ores, I am interested to know whether

Jan 1, 1904

By Henry G. Morris

The use of compressed air for the transmission of power has reached so great a development that we find numerous large establishments devoted to the manufacture of machinery for its production and application, and special periodicals published for the dissemination of information on the subject. Moreover, its employment is so general in mining operations that no apology is needed for the presentation to the Institute of such a paper as the present. The admirable articles of Mr. E. A. Rix, published in Conzpressed Air, show a wide range in the mechanical efficiency of air-compressors, varying, under different conditions, from 15 to 60 per cent.; and it is evident that any

Jan 1, 1902

By William P. Blake

(Canal Zone Meeting, November, 1910.) A DEPOSIT of manganese-ore near Tucson, Ariz., merits notice by reason of the peculiar form in which it occurs, and as a striking. example of ore-deposition by vadose upward capillary flow of metal-bearing solutions with concentration at the surface of the country-rock. This deposit occurs at the northern end of the Coyote mountains, about 40 miles west of Tucson, upon the outcropping beds of porphyritic rock, which appear to be partly-metamorphosed strata of volcanic tufa, probably of late Secondary or of Tertiary age. The strata dip northward at a low angle, and present a series of basset-edges in parallel lines of outcrop, east and west, facing the south and extending over many acres. Successive groups of these outcrops, from 5 to 20 ft. in breadth, are coated with oxides of manganese in lustrous black films and crusts, shining in the sunlight like polished ebony, and covering the whole surface of the rock above the soil. Seen at a little distance, these croppings look like solid ledges of massive and pure ore; but closer inspection and a few blows of the hammer reveal their true nature as a superficial coating allied in origin to the blackened shining surface of rocks exposed in desert-regions, familiarly known as " desert paint" or "desert varnish,"' similar to the phenomena described by me in a former paper, but much thicker and heavier. * By reason of the death of the distinguished author, this communication, probably his last communication to technical literature, is published without revision of the proofs by him. A term first given y G. K. Gilbert. See Rocks, Rock-Weathering, and Soil; by George P. Merrill, p. 256 (New York, 1897). Superficial Blackening and Discoloration of Rocks, Especially in Desert Regions, Trans., xxxv., 371 (1905).

Sep 1, 1910

By Frederick Beckett

WIDESPREAD experimentation has been conducted in recent years to devise a means of preventing intergranular corrosion in austenitic chromium-nickel steels of the 18 per cent chromium-8 per cent nickel type. Additions of titanium to these steels have been used commercially to overcome this difficulty, as advocated by Krupp of Germany, and the latest literature reference concerning improved details of this method is the article by Bain, Aborn and Rutherford.1 Extensive work by the present authors has shown columbium also to be a particularly valuable agent for inhibiting intergranular corrosion. This paper does not deal with steels that are largely or wholly aus-tenitic ; it is limited to a discussion of the results obtained through the use of titanium and columbium in plain high-chromium steels. For many years titanium has been used commercially by some steelmakers as a cleanser, and to a lesser extent as a hardener, but then in greater per-centages. The results of the work to be described disclose that titanium and columbium in proper proportions act as effective softeners in the high-chromium steels. It is well known that chromium intensifies the hardening effect of carbon in steel; it imparts pronounced air-hardening properties within a rather wide range of chromium content; it provides increased ductility in steels of given strength and hardness; and it enhances resistance to corrosion and oxidation at elevated temperatures to a marked degree. However, in applications requiring a combination of some of these valu-able properties great hardness is frequently a detriment rather than a merit. When the objective is a soft and ductile steel having optimum corrosion resistance, the producer strives for a carbon content as low as commercially practicable.

Jan 1, 1933

Abbey, Robert Graham, District Mgr.. The W. W. Sly Mfg. Co., 50 Church St.. New York, N. Y. '21 Abbott, A. N., Mines Supt., Mazapil Copper Co., LtdConcepcion del Oro, Zac., Mexico. '28 *Abbott, Argyle Campbell, Dev. Dept., E. I. du Pont de Nemours & Co., Wilmington, Del. '29 Abbott, Clarence E., V.P., Charge of Raw Materials, Tenn. Coal, Iron & R. R. Co., 1242 Brown-Marx Bldg.. Birmingham, Ala. '04 Abbott, Louis Benjamin, Chief Engr., Elkhorn Div., Consolidation Coal Co., Jenkins, Ky. '16 Abeel, George H., Jr., Cons. Min. Engr Box 427, Santa Monica, Cal. '18 Abel, Albert E., Asst. to Pres., Valley Mould & Iron Corp Hubbard, Ohio. '19 Abel, Raymond L., Asst. Prof., Dept. of Pet. Refin., Univ. of Pittsburgh Pittsburgh. Pa. '28 Abeel, Leo M., Research Engr., Sullivan Concentrator Chapman Camp, B. C., Canada. '31

Jan 1, 1929

By K. G. Wikle, W. W. Beaver

A general survey of the mechanical properties of commercially pure beryllium fabricated from powder by vacuum hot pressing and other consolidation methods is presented. The effect of fabrication method, grain size, strain rate, and directionality upon both room and elevated temperature tensile properties is reported. BERYLLIUM metal, in spite of its rather restricted use, has been the object of attention for many researchers in the past half century. However, such work was performed on special experimental lots of metal made in small quantities by a variety of reduction methods. Not until 1946 was there a substantial production of beryllium metal, and not until 1950 was there a steady production of a commercially standard beryllium in the United States. This output was both the result of a requirement of the Atomic Energy Commission for a high grade beryllium of consistent quality and the development of a powder metallurgy process, by the Brush Beryllium Co., known originally as Process Q, which yielded a fine grained beryllium suitable for fabrication. Because this powder metallurgy product, known as QMV, superceded other types of metal made previously and represents the great majority of beryllium in use today, it seems worthwhile to present the results of studies on the mechanical properties of this metal as currently made. To the design engineer and the metallurgist, beryllium has extremely interesting properties. It is as light as magnesium alloys while having a stiffness modulus 40 pct greater than steel and a strength-weight ratio superior to titanium and aluminum alloys and aircraft steels. The melting point is high, 1287°C (2348°F), and it has good corrosion resistance both in air and water. Also, it is highly transparent to X-rays and has good heat and electrical conductivity (electric conductivity is greater than 40 pct of Cu). To the atomic energy program beryllium is considered a valuable material because of its low neutron-capture cross section and high neutron-scattering cross section which make it a good moderator and reflector for the lower velocity neutrons. A major technical difficulty limiting the use of beryllium, especially in structural applications, has been its notch sensitivity and consequent room temperature brittleness. Kaufmann, Gordon, and Lillie1 have reported their work on the mechanical properties of beryllium performed from 1946 to 1950. They studied the room and elevated temperature properties of cast and extruded beryllium and extruded electrolytic flake, Table I. Cast and extruded alloys of 85 to 99 pct Be were tested also. They found that extruded metal developed good strength and appreciable ductility in the extrusion direction and that thermal treatment and alloying provided little improvement in mechanical properties. They concluded that preferred orientation and fine grain size were the means of obtaining optimum tensile properties in beryllium. Other investigators have measured and commented on one of the most striking mechanical properties of beryllium, namely, its abnormally low Poisson's ratio.2 Udy, Shaw, and Boulger3 presented the latest published survey on properties of beryllium but their information is based only on published data available before April 1949 and cites little information on metal fabricated by powder metallurgy

Jan 1, 1955

By E. L. Bruce

The district of Patricia, in the province of Ontario, lies northwest of the Albany River and extends northward to Hudson Bay. Formerly this was the unorganized district of Keewatin, the southern part of which was divided in 1912 between the provinces of Manitoba and Ontario. The interprovincial boundary now runs north from Lake of the Woods for 275 miles and thence northeast 375 miles to Hudson Bay. This district is comparable in size to all the older part of Ontario south of the Canadian Pacific Railway east of Lake Huron—thus it is roughly one-third of the whole of the present provincial area. The central part of this great triangle is one of the least accessible parts of Canada. From it streams flow southward to the English River, southeastward to the Albany, northward to Hudson Bay and the Hayes River, and westward to Lake Winnipeg. None of the streams is large and canoe travel is not easy. The only industry it has ever had is the trade in furs. Until the development of the airplane on a commercial basis, the only means of travel was by canoe or dog-train. There is not a mile of railway in the whole district. The two areas to be dealt with lie in the southwestern part of Patricia. Red Lake is 50 miles east of the Manitoba boundary and 75 miles north of the transcontinental railway from Cochrane to Winnipeg. Woman Lake is 50 miles farther east and slightly farther north. The late Dr. D. B. Dowling, of the Geological Survey of Canada, visited Red Lake and spent some time there during his exploration survey from Lac Seul to Berens River in 1893. He also visited the Woman Lake basin during the same journey, but his examination of it was much less detailed, the great area covered by him during the one field season making it impossible to make more than a hurried reconnaissance. Some prospecting in the Red Lake district followed Dowling's exploration, but the distance from railway was too great for any systematic work to be done. In 1922, following the usual plan, the Ontario Department of Mines made a geological reconnaissance of the English River, following :in instrumental survey of that river and its lakes by the Department of Lands. A side trip was taken to examine the rocks of Red Lake described

Jan 1, 1928

By P. F. Kinyoun

MANY interesting new features are embodied in the latest extension to the open-hearth department of the Bethlehem Steel Co., at Lackawanna, N. Y. Automatic control of the important factors in furnace operation-fuel, air, draft, pressure, slag composition, and of the temperature in various regions of the furnace-has been carried out to a remarkable degree; the human factor is minimized, and the chances for mishaps and irregularities in operation are greatly reduced.

Jan 1, 1937

By F. B. Plummer

PROGRESS during 1940 in oil-production technology has been confined largely to a steady advancement in practices inaugurated in previous years, rather than the introduction of any new startling process or technique. The usual changes, improvements and additions in production equipment have been introduced. An increased attention to, and interest in, research has been noteworthy, resulting in improved efficiency in operation of oil wells. control, utilization of reservoir energies and reduction of production costs.

Jan 1, 1941

By C. R. Fettke, Bela Hubbard

During the summer of 1916, while on a visit to the United States Agricultural Experiment Station at Mayaguez, Porto Rico, the writers were told by D. W. May, the director, that an occurrence of manganese ore had been reported from the mesa southeast of Mayaguez. A visit to the locality showed that the mesa is covered by a mantle of bright red soil resting upon serpentine. Here and there over its surface concretionary masses of limonite have been mashed out of this soil. These were apparently mistaken for manganese ore. On account of the similarity of this occurrence to the extensive iron deposits of northeastern Cuba, it was thought that a brief description based upon a two days'reconnaissance survey of the area mould be of scientific interest. Mayaguez is on the west coast of Porto Rico, at Mayaguez Bay, which is the third in importance of the harbors of the island. The city itself is about 3/4 mile inland on the low-lying plain at the mouth of the

Jan 1, 1920

After the close of the Revolution, settlers began to pour over the mountains, to settle in the western parts of Pennsylvania, of Virginia, to move down the Ohio into Kentucky, and in the late seventeen-eighties to settle on "the Indian side" of the river, now Ohio. With the growth of population the interest in coal increased and it was not long before the production of coal west of the mountains was larger than that east of them. Foreign nations, too, became interested in the young republic and in 1783, at the instance of the Swedish government S. A. Hermelin, an engineer, visited this country to investigate its iron industry. He made a very interesting report, not published until 1931, in which he gave many details of the iron plants in the eastern United States; apparently he was not west of the mountains, but was well informed about conditions there. He says, "that some coal near the first branches of the Schuylkill River has been mined and utilized by the blacksmiths," referring, of course, to anthracite; again that "coal mines have also been worked for several years near Pittsburg," and that "great supplies of iron ore are available at the Ohio Falls and further to the west, at Coney Creek, a part of the Green River, where there is also coal."' In 1788, Dr. Johann David Schoepf, who came to this country with the Hessian troops, visited Pittsburgh. He was an intelligent man and acquainted to some extent with minerals and methods of working them. In speaking of Coal Hill on the south side of the Monongahela he mentioned several strata of marble in the lower part and that

Jan 1, 1942

By C. S. Barrett, D. F. Clifton

THE transformation that occurs in lithium and its solid solutions containing magnesium1,2 is similar in many respects to other diffusionless transformations of the martensitic type. This general similarity makes it desirable to investigate the transformation curves in detail. The current interest in the phenomenon of stabilization in martensitic transformations has created a need for a careful appraisal of possible stabilization effects in both cooling and heating transformations in lithium alloys. The effect of prior heat treatment on the temperature at which transformation begins and the effect of various temperature cycles in partially transformed alloys also merit attention. Limited data on some of these features were presented previously,' but the present studies have been made with improved apparatus, in which erratic fluctuations were smaller than in the earlier work, and include many independent determinations of certain critical observations. Material and Methods Geiger counter X-ray spectrometers were used: a Norelco instrument, original model, and a General Electric XRD-3. The low-temperature specimen holder has been described elsewhere." Specimens 10 mm in diam and 1.5 mm thick were held in firm contact with a copper block which was attached to the lower end of a stainless steel tube that extended up to a reservoir of liquid nitrogen. A heating coil on the tube permitted a controlled temperature gradient along the tube, so that desired temperatures and rates of heating and cooling could be obtained by controlling the heating current. The specimen was surrounded by an atmosphere of evaporated nitrogen in an insulated chamber having double cellophane windows. The temperature of the specimen was read by a thermocouple imbedded in it close to the irradiated area; the specimen could be held at constant temperature within 1°C for long periods. The body-centered cubic 200 reflection near 8 = 26" was used as the index of the amount of b.c.c. material present; occasional checks were made using the most suitable line of the low-temperature phase, the close-packed hexagonal 110 line near 8 = 29". Copper radiation was used throughout. A continuous record was made of the reflected intensities on a strip chart recorder, both when the peak intensity of a line was being followed and when the lines were being scanned at constant temperature. On the continuous recordings of peak intensity, periodic checks were made on the background intensity between the lines, and on the setting of the spectrometer for maximum intensity. The lithium-base solid solution containing 12.4 atomic pct Mg (33.3 wt pct) that had been used previously' was chosen, as it had a transformation range at relatively high temperatures, so as to permit wide temperature cycling within the range. Just prior to use a pellet was cut from the ingot,

Jan 1, 1951

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