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By M. N., Short

TIE Pioneer mining district, better known as the Superior district, from its principal town, is located in Pinal County in south-central Arizona about 80 miles east of Phoenix and 22 miles west of Miami. The region embraces a confused series of mountain ranges of moderate FIG. I.----SUPERIOR, LOOKING NORTH FROM SOUTH BANK OF QUEEN CREEK. MAGMA MINE IS INDICATED BY WASTE DUMP IN GULCH TO RIGHT OF CENTER. height but precipitous slopes, between which lie irregular valleys filled with alluvial detritus. The average elevation is about 2800 ft. in the valleys and the summits of the ranges reach 2000 ft. above this. Superior is situated on the north bank of Queen Creek where it emerges from one of those ranges into a more or less basin-shaped valley. The drainage of Queen Creek is to the southwest and the flood waters spread out and lose themselves in the desert northeast of Florence, the county seat of Pinal County.

Jan 2, 1926

Asarco's Sacaton unit, located near Casa Grande 45 miles southeast of Phoenix, Arizona, was brought into production in February 1974. Ore reserves are estimated at about 48 million tons at 0. 95% copper. Mineralization of the orebody comprises both sulfides and oxides, with minor amounts of gold and silver. Preproduction stripping of 40 million tons of overburden was accomplished in less than two years. Mining is done at the rate of 9,000 stpd ore with a waste-to-ore ratio of 4.6 to 1. 0. The mine is developed on 40 ft benches, and by 1979 underground block caving methods will be phased into the operation at a depth of 1900 ft. Ore is mined in the pit two shifts per day, seven days per week, and is hauled with 85 ton trucks to the primary crushing plant. Trucks dump their loads into a 165 st capacity pocket equipped with a chain curtain which controls the ore flow to the 6 ft 6 in. wide by 24 ft long (2. 0 m by 7.3 m) vibrating feeder grizzly. Grizzly bars are inclined at a 5º slope on the first half of the 0 feeder and 10 on the last half. Grizzly bars have 6 in. (13 mm) spacings which pass 60 to 70% of the mine-run ore. Grizzly oversize drops into a 48 in. by 60 in. (1. 22 m by 1.52 m) primary jaw crusher. Both the grizzly undersize and crusher discharge are collected on a 42 in. (1.07 m) conveyor belt operating 398 fpm (121 mpm) for transport to the 4,750 live st intermediate storage area ahead of the fine crushing plant. Capacity of the Sacaton primary crushing plant is a nominal 1150 stph (1043 mtph). It operates fourteen shifts per week with an effective crushing time of four hours per shift. An economical open-air design was used, but an enclosed operator control room is located on the upper level where the dump truck, feeder, and crusher can be observed. Oversize rocks are removed from the feeder or crusher by the 10-ton bridge crane. Direct operating costs for this well-designed primary crushing plant, including labor, power, supplies, and maintenance, are only 3.5 cents per short ton. An interesting feature of the Sacaton orebody is that the non-sulfide copper minerals, which are less prevalent than the sulfides, occur intimately with the sulfide minerals; for this reason, all ores as mined are treated in a flotation circuit using sulfidizing methods for oxide recovery.

Jan 1, 1978

E. Windsor Richards, London, England:—In reading this paper the most interesting point to me mas the question of the maximum percentage of phosphorus allowable in the steel rail. Mr. Colby said, and we will all agree with him, that the engineer knew, and even a steel-rail maker grants that phosphorus is the most undesirable constituent of steel. We in England have been for a long time considering a specification for the supply of steel rails. This matter has been taken up by the Institution of Civil Engineers, the Mechanical Engineers, the Iron and Steel Institute, the Institute of Naval Architects, and the Electrical Engineers. Committees have been formed,and the whole matter has received most careful attention. They arrived at last at an analysis which I will read: " The carbon is to be from 0.35 to 0.5 per cent.; the manganese from 0.7 to 1.0 per cent.; the silicon, not to exceed 0.10 per cent.; phosphorus, 0.07; and sulphur, 0.07 per cent." As to the phosphorus, which is the most important point of all in the analysis, we have for many years, and indeed until very lately, always agreed to supply steel which would not contain above 0.06 per cent. of phosphorus. Iron-ores are not quite as good now as they were formerly, and the manufacturers at the meetings of the committees referred to, tried to obtain an increase in the allowance of phosphorus. They asked the Sub-committee to agree to 0.08 per cent. of phosphorus. They tried all they possibly could to obtain that; but they failed. English engineers in Great George Street and all over England, representing the important Associa tions I have mentioned, would only agree to 0.07 per cent. and that is the maximum allowance of phosphorus. Mr. Colby is an able advocate, but with all his ability he would not have been able to persuade the English engineers to agree to 0.08 per cent.

Jan 1, 1907

Jan 1, 1879

Jan 1, 1967

By Donald J. Knight

HEAT Treatment at 1500' F of a mild steel containing 0.1 pct C, in an atmosphere which is oxidizing to both carbon and iron, results in the progressive oxidation of the metal surface with little or no change in the carbon content of the underlying metal. Further heat treatment of the scaled metal in either a neutral atmosphere or in a vacuum may or may not result in the decarburization of the metal depending upon the physical nature of the scale. It is apparent that if a continuous layer of oxide is present on the steel surface, the reaction OScale + Cmetal Cogas cannot progress since the SO formed gas would be unable to leave the oxide/metal interface. Thus, in order for the reaction to progress, the oxide must be cracked or porous. Vacuum heat treatment at 1500" F of samples with a thick continuous oxide scale showed no decarburization of the steel. However, when cracks were introduced mechanically into the scale prior to the vacuum heat treatment notable decarburization of the metal resulted and a structure as shown by Fig. 1 obtained, i.e., reduction of the crack walls to ferrite. With reference to the diagram of Fig. 2, it would appear that a mechanism of the following type takes place. Carbon atoms arriving at an oxide/metal/void interface, such as 'A', Fig. 2(a), can combine with oxygen atoms from the scale and leave the reaction site as Cogas thereby reducing the oxide to metal. On a greatly magnified scale, Fig. 2(b),this will appear as a ferrite projection along the crack wall. Carbon atoms entering this projection can react with oxygen atoms at point 'C', which is a new interface, and so on leading to a progressive growth of the ferrite along the crack wall and to the surface, Figs. 2 (c) and 1. It would appear that the only means by which thickening of the ferrite film can take place is by a diffusion of oxygen through the ferrite film to react with carbon at the newly formed ferrite/ void interface. Since the diffusion rate of carbon is reportedly much greater than that of oxygen, and since there is a low probability factor of oxygen and carbon atoms arriving simultaneously at the same site on the ferritehoid interface, there will be a tendency for more rapid lengthening than thickening of the ferrite layer, as is observed.

Jan 1, 1962

Alfred C. Young† (communication to the Secretary): Before the appearance of Mr. Scott's paper in these Transactions we were not specially interested in the investigation which he has started; but at his request we have endeavored to collect from musty records and the recollection of our old friends a brief chronicle of the progress made by this house. As 3000 instruments were manufactured by us before any descriptive record was kept, and 2000 more before the record contained more than a statement whether the instrument was a transit or a level, and sometimes its size, we approach the task with timidity, trusting that the reader will bear the difficulties in mind, particularly as the writer's predecessors, from whom, no doubt, the information desired could have been obtained, have passed away. Instruments for surveying were manufactured by David Rittenhouse, of Philadelphia, as early as 1760; but it was not until late in the first quarter of this century that there was any American market for an instrument outside of the ordinary surveyor's compass. With the advent of canals and railroads, and the more extensive development of the Pennsylvania coalfields, arose a demand for surveying-instruments to meet problems in engineering beyond the limited field of the compass. On May 1, 1820, in which year the practical mining of anthracite coal in Pennsylvania began, William J. Young, who had served his apprenticeship with one Thomas Whitney,

Jan 1, 1901

NEW MEMBERS The following list comprises the names of those persons who became members during the period of Oct. 10, 1917, to Nov. 10, 1917. ABEY, HIROSHI Min. & Met. Engr.. Mitsubishi Co., Tokio, Japan. BARNETT, WALTER W., Assayer & Chem., Seoul Min. Co., Tul Mi Chung, Chosen, Korea. BATES, WILLIAM S Min. Engr., Anaconda Copper Min. Co., Butte, Mont. BENDELARI, ARTHUR E Mgr. of Mines, Eagle Picher Lead Co., Picher, Okla. BERKEFELD, PAUL C Mining Engr., 2901 Piedmont Ave., Berkeley, Cal. BILLINGS, It. S Mgr., Sheep Trail Pyramid Mines Co., Kingman, Ariz. BILLWILLER, C. J., JR Mgr. Nitrate Agencies, Ltd., Iquique, Chile. BLUM, EDWARD H., Engr., Asst., to Pres., The Atlantic Refining Co., 3144 Passyunk Ave., Philadelphia, Pa. BORDEN, GAIL, Vice-Pres. & Treas., American Safety Explosive Co., 50 East 42d St., New York, N. Y. BRESLIN, THOMAS F Min. Engr., Cebu, Cebu, P. I. BURKE, JAMES M., Efficiency Engr., Calumet & Hecla Mining Co., Calumet, Mich. CANTON, WILLIAM R Met., Nevada Consolidated Copper Co., McGill, Nev.

Jan 12, 1917

By Rossier W. Raymond

John Birkinbine was born Nov. 16, 1844, at Reading, Pa., the eldest son of H. P. M. Birkinbine, widely known as a hydraulic engineer. The family removed subsequently to Philadelphia, where, as a young man he established with his father the office now, continued by his sons, after more than 60 years. His education was received at public schools, the Friends' High School in Philadelphia, the Hill School at Pottstown, Pa., and the Polytechnic College of Pennsylvania, where his studies were interrupted in 1863-4 by service in the Union Army, which included participation in the battles at and around Gettysburg. Later, he devoted two years to work in a machine shop; and subsequently he became associated with the late P. L. Weimer, under the firm name of Weimer & Birkinbine, operating the Weimer Machine Works at Lebanon, Pa. Much of his work was in mining, metallurgy, and blast-furnace construction. As manager for the South Mountain Mining & Iron Co. he carried on experiments with various fuels for iron-ore smelting while maintaining the furnace in constant operation. The carefully recorded results obtained were widely published, and are referred to in text-books by other metallurgists as most complete. From his Philidelphia office he was sent to nearly every State, and to Canada and Mexico, for examinations, reports, constructions or im-provements in iron-ore mines, blast furnaces, iron works, water supplies, hydraulic development, irrigation projects, etc., and his engineering knowledge was requisitioned by several Eukopean corporations. A number of business trips were made to Mexico, beginning with a visit to the Cerro de Mercado at Durango,,before railroads were established in that. portion of Mexico, to make a critical examination and report on this "Iron Mountain." Later visits covered other localities and engineering problems, familiarizing him with the major part of the iron industry in Mexico. The late disturbed political conditions in that Republic have retarded the probable enlargement, modernization, and improvement of much of the iron and steel industry of Mexico, upon which he investigated and . reported for various capitalists on both continents. One interesting subject included in these reports was a proposed electric furnace, to be operated by energy from water power.

Jan 1, 1916

By M. P. Tixier, M. Gondouin, G. L. Simard

In the quantitative interpretation of the SP logs, the electrochemical component is generally taken equal to — K log Rm /Rw where K has the theoretical value corresponding to solutions of pure sodium chloride. This method may be misleading when relatively large quantities of salts other than NaCl are present in form-rrtion waters—as is generally the case for low salinities —or in gyp-base muds. In such cases recourse is made in the field to changing the K value or to adding a correction term to the equation on the basis of local experience. An investigation has been made in the laboratory of the influence of HCO3, SO4=, Ca++, and Mg++ on the amplitude of the SP deflection, which included in par-ricular determinations of the activity coefficients of Ca++ and Mg++. The theory, the experimental techniques and a tentative method for applying the results are described. So far, applications to actual field cases where chemical analyses of waters were available have provided an excellent confirmation of the proposed method. The case of the SP in very salty brines is also considered and it is shown that the use of activity data for sodium gives satisfactory results. HISTORICAL In early times of electrical logging, the SP curve was used exclusively as a tool for the location of permeable beds and the definition of their boundaries. Later, with the introduction of methods of quantitative analysis, attention was called to the possibility of deriving from the SP log some information on the formation water resistivity, which constitutes one essential element for the computation of water saturation from log data. The first laboratory experiments' in 1932 had shown that, as a result of electrochemical phenomena arising at the contact of the niud and the formation, the amplitude of the deflection of the SP curve was, at least partly, a function of the salt concentration of interstitial water and accordingly of its resistivity. It was indicated that the amplitude of the electrochemical component of the SP should be equal to K log R1/R2, R1 and R2 being the resistivities of the mud and of the formation water respectively. However, the exact value of the K coefficient was not determined at that time because the surface clay used for a laboratory model was far from an ideal shale membrane. Consequently, the way was not yet open towards quantitative interpretation. In the early forties, Tixier reported2, on the basis of field log observations, the following equation for the case of NaCl solutions, SP = -71 log f1c1/f2c2, c1 and c2 being the concentrations and f1, f2 the mean activity coefficients. The local variations observed in the empirical values of K, chiefly in the Rocky Mountains, led him to advance the opinion that, besides the relative amounts, the nature of the salts present in the solutions had a bearing on the magnitude of the SP. At about the same time Mounce and Rust- ad published laboratory results which emphasized the part played by the shale in the generation of the SP. On the basis of laboratory tests and theoretical considerations, Wyllie in 1948' published the following equation of the electrochemical SP for the case of NaCl solutions, SP= - 71 log (a1)m/(a2)m

Jan 1, 1958

Jan 1, 1944

Jan 1, 1944

By J. W. Putman, N. J. Grant, D. S. Bloom

SEVERAL recent determinations of the melting S point of pure chromium have been reported which give values of 1845°C1; 1895°C,² 1930°C,³ 1860°C,' and 1890°C.5 because of this wide spread of values, it appeared desirable to make one additional attempt to obtain a more accurate, reliable figure. bloom and Grantx recently reported a phase transformation in chromium:.--- it was desired to check this, too, in the course of checking the melting point. To accomplish this, a much higher purity chromium was required. Electrolytic chromium containing about 0.5 pct 0 was crushed to a finer size and was then annealed in highly purified, dried hydrogen at 1375°C for 100 hr. This treatment produced chromium with about 0.008 pct 0, 0.002 pct N, and negligible carbon. The balance of the impurities was 0.3 pct Fe, 0.03 pct Si, 0.004 pct S, and less than 0.001 pct Mo. This chromium was melted in a stabilized zirconia crucible under pre-purified argon, using induction heating. Temperature measurements were made with annealed wolfram-molybdenum thermocouples and a Leeds and Northrup Speedomax Recording Potentiometer. The thermocouples were annealed for 1 min in hydrogen at a temperature of about 2400°C. Each leg of the thermocouple was immersed in an ice-water mixture using mechanical connectors to the lead wires. The thermocouple tip was immersed in the molten chromium in a zirconia protection tube which introduces an error of about 3°C as a temperature drop through the walls of the tube. The weight of chromium was about 183 g. The dimensions of the melt in the crucible were about 1.25 in. diam x 2 in. high. The tip of the thermocouple was held about ½ in. from the bottom of the crucible. Two new thermocouples were used with the above set-up giving the results shown in Table I. Since this chromium is purer than that used by Greenaway, Johnstone and McQuillan,' by Carlile et al.,4 and other investigators,²,3 it is believed to be the more accurate. Thermocouple aging effects which are believed responsible for the high value of 1930°C³ were avoided in this work. This value of 1903°C is correct to about ±10°C. The right hand column lists the temperature of the a ? ß transformation on heating and the ß ? a on cooling.3 A sample curve is shown in Fig. 1. The value so determined is 1840°C + 15°C. Fig. 1 gives adequate evidence that there is a transformation in chromium at high temperatures.' References 'H. T. Greenaway, S. T. M. Johnstone, and M. K. McQuillan: High Temperature Thermal Analysis USing the Tungsten-Molybdenum Thermocouple. Journal Inst. Metals (November 1951) 19, p. 109. ²J. W. Putman, R. D. Potter, and N. J. Grant: The Ternary System Chromium-Molybdenum-Iron. Trans. A.S.M. (1951) 43, p. 824. ³D. S. Bloom and N. J. Grant: Chromium-Nickel Phase Diagram. Trans. AIME (1951) 191, p. 1009; Journal of Metals (November 1951). ' S. J. Carlile, J. W. Christian, and W. Hume-Rothery: The Equilibrium Diagram of the System Chromium-Manganese. Journal Inst. Metals (1949) 76, p. 169. 5G. Grube and R. Knabe: Ztsch. Elektrochemie (1936) 42, p. 793.

Jan 1, 1953

By R. D. Pehke, J. F. Elliott

The solubility of nitrogen in liquid pure iron has been measured as a function of pressure and temperature. Sieverts' Law is obeyed at all pressures up to 1 atm and the temperature coefficient of solubility is 8 x 106 %/°C. The solubility of nitrogen in liquid iron alloys has been studied by the Sieverts' method and by the sampling method. The solubility is decreased by Al, C, Co Cu, Ni, 0. Si atzd Sn, and it is increased by Cr, Cb, Mn, Mo, Ta, W, and V. Interaction coefficients eN, for the effect of these elements on nitrogen dissolved in liquid iron, are reported. 1 HE effect of nitrogen upon the properties of steel may be desirable or not, depending upon the composition, processing treatment, and the use of the product. To understand the behavior of nitrogen in the various steelmaking processes, it is necessary to have reliable fundamental data pertaining to the solubilities, rates of solution, and chemical reactions of nitrogen in steel, particularly in the liquid state. In an effort to extend our knowledge in these areas, an investigation of the thermodynamics and kinetics of the solubility of nitrogen in liquid iron alloys was undertaken. The thermodynamic aspects of the study are presented in this paper. The solubility of nitrogen in liquid pure iron has received the attention of several investigators whose results are summarized in Table I. Reasonable agreement among the more recent researches1-l8 is found for the solubility of approximately 0.044 wt pct at 1600°C and 1-atm pressure of N,, for the temperature coefficient of solubility being small but positive, and for adherence to Sieverts' law for pressures up to 1 atm. The solubility of nitrogen in a number of binary liquid iron alloys has been studied: Fe-A1,3 Fe-As,16 Fe-C,3, 71 18, 19, 20 Fe-Cr ,5,7, 10, 11, 15 21 Fe-Co,'4, '6 Fe-Cu,'6 Fe-Mn,10, 11, 18 Fe-Mo,13, 16 Fe-Ni,10, 11, 13, 15, 16 Fe-O,16, 17, l9 Fe-p,7 Fe-S,l6 Fe-Sb,16 Fe-Se,lg Fe-Si,4) 97 '77 187 19>2° Fe-Sn,16 and Fe-v.51 '3 A few ternary systems have been studied, most of which were reviewed by ~angenberg" who applied the methods suggested by WagnerPz3 Chipman,24 Darken and G~rry, and Morris and Buehl26 for predicting solubilities in multicomponent alloys. Langenberg22 and Humbert and Elliott15 compared the solubilities computed from simple binary alloy systems with experimental measurements of nitrogen solubilities in liquid iron containing two or more alloying elements. The interaction coefficients for nitrogen in

Jan 1, 1961

By R. W. Raymond

The sudden death of Dr. Drown, on Nov. 17, 1904, brought to multitudes the pang of personal loss. Of all those who, as students at Lafayette College, the Massachusetts Institute of Technology and Lehigh University, were brought under his influence, not one can have forgotten him, and all will now acknowledge, with an unfading gratitude, what they owe in professional equipment to his wise, clear, skillful guidance, and in character to his sympathetic, stimulating personality. Outside of this wide circle, the experts of both hemispheres will lament the departure of one who, in his department of scientific investigation, both knew what work was needed, arid how to do it so that it needed not to be done again. The older members of the Amierican Institute of Mining Engineers will remember with gratitude the part he took, as Secretary from 1873 to 1884, in promoting the interest of that organization, and in shaping the plan and policy which it has followed with such noteworthy success. And, in addition to all these (though partly included among them), there are a host of friends, who can scarcely think of the public loss by reason of their own. Thomas Messenger Drown was born March 19,1842, at Philadelphia, Pa. His parents were natives of New England; and he was the youngest of their three sons. He received his preliminary education in the public schools and the High School of Philadelphia, from which he was graduated in 1859. Be-

Jan 1, 1906

Commonwealth of Pennsylvania, Department of Internal Affairs, Topographic and Geologic Survey, Harrisburg, Pa George H. Ashley, State Geologist All available printed Bulletins may be obtained through the Commonwealth of Pennsylvania, Division of Documents. Where a price has been set on the publication, checks should be made out to the Commonwealth of Pennsylvania. A Syllabus of Pennsylvania Geology and Mineral Resources has recently been published by the Survey as Bulletin G1, and consists of a general survey of the state An appendix of this bulletin also gives a complete bibliography of Survey publications It will be sent upon request. The State Geological Survey has gone through several phases and reorganizations, publications of three of them being numerous and important A fire, in 1927, destroyed supplies of many of the papers of the present Survey. Available bulletins of the present Survey are: Bulletin M6: Bituminous coal fields of Pennsylvania, in 4 parts available as follows: pt 1, General description of coal, 50 cents; 3, Bituminous coal resources, 25 cents, 4, Analyses of bituminous coals, 25 cents Bulletin M10, Fire clays of Pennsylvania; Mll, Molding sands of Pennsylvania; M12, Anthracite culm and silt (1928); M13, Feldspar in Pennsylvania; M14, Magnetite deposits of French Creek (1931); County Report C1, Adams County, pt 1, Geology and geography (in press), County Report C2, Geology and mineral resources of Greene County (in press); Topographic and Geologic Atlas A5, New Castle Quadrangle (1929), $1; Topographic and Geologic Atlas A27, Pittsburgh Quadrangle (1929), $1; Topographic and Geologic Atlas A168, Lancaster Quadrangle (1930), $1. The present Survey has also issued a number of short mimeo¬graphed bulletins any of which will be sent upon request Briefly they are: No. 15, Mineral resources of Pennsylvania; 20, Iron ores; 28, Magnesite; 40, White clay deposits, Monroe County; 45, White clay deposits, central Pennsylvania; 47, Manganese, Eastern Pennsylvania, 48, Pyrite from bituminous coal mines; 59, Bog

Jan 1, 1933

By Donald T. Hawkins, Ralph Hultgren

The lorsion effusion method has been used to measure the vapor pressure of lead over pure lead and eight Pb-Sn alloys ranging from 9.1 to 87.9 at. pct Pb in the temperature range 950° to 1125°K. The resulting ?H°y 298 = 46,630 ± 200 cal per g-atow for pure lead is in excellent agreement with previous work. Deriued ?Gph values for the alloys were smoothed and correlated with previous heat of formation data to obtain entropies for the liquid alloys. values for the tin component were calculated by Gibbs-Duhem integmtion. Surfhce depletion of these liquid alloys was found to be absent, as shown by the fact that the measured pressure remained substantially constant with time in contrast with previous measurements on iron-rich solid Fe-Mn alloys. The activities and Gibbs (free) energies of the liquid Pb-Sn system are not well known although the heats of formation have been accurately determined by K1eppa.l Vapor pressure determinations of the activity of lead by Voronin and Evseev2 disagree with those of Predel.3 Elliott and chipman4 measured activities by the electromotive -force technique in the ternary Pb-Sn-Cd system. From the resulting values of the activity of cadmium, they were able to calculate the activities of lead and tin for the binary Pb-Sn system at the compositions xsn = 0.33 and 0.67. Atarashiya, Uta, Shimoji, and Niwa5 determined the activity of tin from Hz-H2O equilibrium measurements, but their results are subject to question due to uncertainty in the final state of their samples. To resolve these differences, measurements of the activity of lead were made using a torsion-effusion apparatus. Among other advantages, this apparatus rapidly detects errors caused by surface depletion, which tends to reduce the apparent vapor pressure of the more volatile component. If the measured torques remain nearly constant with time, only bulk depletion is occurring. This contrasts with the rapid decrease in torque found in solid Fe-Mn alloys at high temperatures and low manganese contents.6 EXPERIMENTAL 99.999+ pct Pb was obtained from the American Smelting and Refining Co. and 99.999 pct Sn from Vulcan Detinning Co. Eight Pb-Sn alloys were prepared by melting together weighed amounts of the pure metals in evacuated Pyrex tubes and quenching the melts in water. Loss of weight in preparation was less than 0.02 pct in all cases. The effusion cells were made from high-purity, nonporous graphite. Graphite was chosen because of its resistance to reaction with lead and tin and because it can be accurately machined with precision orifices. Two cells were used with overall dimensions as shown in Fig. 1. The orifices of cells 1 and 2 were, respectively, 1 and 1.5 mm in diam.

Jan 1, 1968

By Hansheinz Portisch, Harold Margolin

A surface expansion was found to occur sometime after etching in Ti-A1 alloys containing 9.5 to 12.5 wt pct Al. The structure formed, grew, and disappeared with tzrrze. The surface expansion was followed by microscope observations and interferometric and lattice parameter measurements. Activation energy measurements for the growth of the "expansion structure" and chemical analysis indicated that the phenomenon occurred as a result of hydrogen pzckup during etching. It is proposed that hydrogen initially enters octahedral sites of Ti3Al coherent with a Ti and later shifts to the tetrahedral sites. It is postulated that expansion occurs when hydrogen enters the tetrahedral sites. The expansion structure disappeared, it is proposed, because of diffusion of hydrogen from the surface into the body of the alloy and because of loss of coherency of Ti3Al. In examining Ti-A1 alloys, Ence and arolinl observed markings on the surface of specimens. These markings did not appear after electropolishing only, but rather appeared only after etching. The markings appeared to grow as a function of time after etching and later seemed to disappear. Although the markings had some similarity to precipitates, showing, frequently, a Widmanstatten type of arrangement, the observation that other microstructural markings continue to be seen within the new structure suggested that it was actually not a precipitate. The source of this structure was unknown and an attempt was made in the present investigation to develop some understanding of its nature. It has been labeled expansion structure. 1) EXPERIMENTAL PROCEDURE A) Alloys. Alloys in the range 6.5 to 14.5 wt. pct A1 were studied. Bars, 4 in. sq, forged from Bureau of Mines (73 Bhn) titanium consumably arc-melted 4-lb ingots,' as well as 50-g arc-melted buttons of desired aluminum contents were used. The 50-g buttons also used Bureau of Mines titanium (73 Bhn) and aluminum of 99.99 pct purity. Buttons containing up to 8.5 wt pct A1 were hot-rolled from a furnace at 900' . Those with higher aluminum contents were hand-forged on a titanium anvil, and heated with an oxygen-hydrogen torch in the region of 1200" to 1300°c. Frequent reheating kept the samples at the desired temperature range. After a reduction of about 30 pct, the samples were water-quenched. To eliminate any contamination picked up either during hot rolling or forging, at least 1 mil of the surface of the sample was taken off. B) Heat Treatment. Prior to heat treatment all alloys were vacuum-annealed to remove hydrogen. Samples were annealed at 900' until a vacuum of 10'5 mm Hg was established. After this treatment, the samples were wrapped in molybdenum sheet and heat-treated in argon-filled quartz capsules, which were broken under water or iced brine at the conclusion of the heat treatment. All heat treatments under dynamic vacuum were performed in a rapid-quench furnace. This consisted of a molybdenum-lined quartz tube attached to a vacuum system and through a stopcock to a beaker of water. At the completion of the heat treatment the vacuum stopcock was closed, the furnace shut off, and dropped below the quartz tube. Then immediately the inlet stopcock was opened and water admitted until the tube was filled. The steam formed was allowed to escape through the inlet stopcock. This method was used in heat treatments up to llOO°C. C) Metallography. Specimens for metallographic examination were ground, then electropolished using a Disa Electropol machine with a perchloric acid electr01te. Specimens were etched with R-etch.3 A standard etching time of 3 min was used, with the specimen being agitated during immersion. D) Sample Preparation for X-ray Analysis. Samples 0.2 to 0.5 mm in diam were produced from heat-treated rods which were turned to 2 mm diam on a lathe and then rotation-etched. An etchant consisting of 1 pt HF, 7 pt HN03, and 12 pt HzO was satisfactory. With the rod rotating in a vertical position at 50 to 100 rpm, a needle with uniform dimensions could be obtained. Care had to be taken to insure that the rod was at the center of rotation, otherwise cavitation developed. If a small unevenness developed, it was possible to grind it off with a fine emery paper. E) X-ray Diffraction. All X-ray work was done on a North American Phillips X-ray diffraction apparatus and a Jarrell Ash microfocus X-ray unit. The Phillips unit was used with a copper target and nickel filter. The Jarrell Ash unit was fitted with a cobalt target and iron filter. For the Phillips unit 35 kva and 20 ma were used, whereas for the microfocus unit with the 100-p fixed-focus gun 40 kv and 1.5 ma were used. It was found that alignment of cameras on the Jarre11 Ash unit was very critical. The X-ray beam contains an intense area which is not the beam center. The cameras were aligned with the intense region by monitoring the beam coming out of the camera with a Geiger counter. Adjustments were made until a maximum intensity was obtained. A Phillips diffractometer with a Brown chart recorder furnished some of the lattice parameter data. The divergence slit up to 80 deg 28 was I deg; above 80 deg, a 4-deg opening was used, while the scatter slit was1 deg and the receiving slit had a 0.003-in. opening. The general scanning rate was 1 deg per min, while peaks of special interest were rescanned at -j deg per min. For elevated-temperature X-ray diffraction a Uni-cam High Temperature Camera with a film diameter

Jan 1, 1969

ALABAMA America.-Foreman, J. T. Ashland.-Sturdevant, J, C. Altalla; Henderson, R. M. Bessemer.-Ball, E. M. Maschmeyer, W. L. McKenzie, W. C., Jr. Birmingham.-Abbott, C, E. Aldrich, T. H. Aldrich, T. H., Jr. Aufderhaar, H. C. Berg, H. A. Blair, C. S. Bush, M. W. Clark. G. H.

Jan 1, 1929