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By V. R. Garfias

EVEN before the arrival of Cortes in 1519, the history of Mexico was closely linked to that of its mineral production; the mining activities of the Aztecs being thus described by Clavigero, one of the early historians: In the mountains of Anahuac there abound in veins all kinds of metals, and infinite variety of other fossiliferous products. The Aztecs obtained gold from the countries of the Cohuijques, of the Mixtecas, of the Zapotecas and from various other places. They gathered that precious metal usually in grain, from the sands of the rivers, keeping a certain portion for the crown. They obtained silver from the mines of Taxco, of Tzumpango and others; however, this metal was not as esteemed by them as by other neighboring nations. They had two kinds of copper; one hard, which they used instead of iron to make sickles, lances and all kinds of rural and military instruments and another, soft, with which they made kettles, goblets and other receptacles. This metal abounds mainly in the province of Zacatula and in that of Cohuijques, which at present is in the kingdom of Michoacan. They obtained tin from the mines of Taxco and lead from those of Izmiquilpan, located in the country of the Otomiea. From the tin they made money, and the lead, we know they sold in the market places, but we ignore the uses to which they applied it. They also had mines of iron in Tlaxcala, in Taxco and in other places; but they either had not discovered them, or did not know how to make use of the metal they contained. In Chilapa there were mines of mercury, and in other places there were mines of sulphur, alum, vitriol, cinnabar, cohre and of a white earth which they esteemed highly. As regards mercury and vitriol, we do not know of what use they were to them; the other metals they used in paintings and dyes. There were then great abundance of amber and asphalt-bitu- men of Judea--on the coast of the seas and many cities of that territory paid tribute of one and the other to the kingdom of Mexico. They mounted the amber in gold, and it was only used as ornament and display by them. With the asphalt they made certain perfumes. The following extracts dealing with pre-Colonial gold are taken from the famous "Cartas de Relación" to Charles V, in which Cortea described the progress of the Conquest: . . . here there came two chiefs who owned lands in the valley; one four leagues down the valley and the other two leagues up the valley and they gave me some gold necklaces of little value and seven or eight girls. . . . . . . that day I left the City of Churultecal and traveled four leagues to some villages of the City of Cuasucingo where the natives received me very well and gave me women and pieces of gold. . . .

Jan 1, 1937

PLANS are underway for the annual meeting of AIME, to be held in New York, February 17 to 21. The technical program includes meetings of all divisions of all three branches, Mining, Metals, and Petroleum. The bulk of the technical sessions will be held at the Statler Hotel, and the annual banquet will be held at the Waldorf-Astoria, Wednesday evening, February 20. The technical program of the Mining Branch activities is included in this issue. While it is not complete in every detail, it shows general interest groupings as well as subjects to be discussed. The program for each division is shown separately to facilitate following the activities of these special interest groups. Then, after a full scale and possibly somewhat strenuous technical meeting, a post-meeting feature will appeal to many of the members. A restful cruise to Bermuda and Nassau is offered at special rates to AIME members and friends. The schedule is a 3:00 pm departure from New York on the Queen of Bermuda on Saturday, February 23; arrival at Bermuda at 7:00 am Monday, February 25; arrival at Nassau at noon, Wednesday, February 27; and the trip ending again in New York at 9:00 am, Saturday, March 1. Rates begin at $202.10 per person, with higher rates depending upon accomodations desired. The base rate includes outside room with private bath and all meals, as well as Federal, Bermuda and Nassau taxes. Reservations for the trip should be made immediately through Leon V. Arnold, 36 Washington Square West, New York 11, who is in charge of arrangements.

Jan 1, 1952

By James W. Malcomson

The Tigre Mining Co. of Mexico, owned by the Lucky Tiger Combination Gold Mining Co. of Kansas City, decided early in 1910 to enlarge its mill, which consisted of a concentrator milling 3,000 tons of ore per month. The enlarged plant was designed to crush and concentrate 6,000 of ore and to cyanide 7,500 tons per month. The extra tonnage cyanided was to be obtained from tailings which were stored below the old mill. Power was supplied to the old mill from four boilers; a 150-h-p. Corliss engine and two Weber 60-h-p. gas-engines using producer-gas made from charcoal. The total horse-power required, including 60 h-p. used for machine-drills in the mine, was approximately 275. Cord-wood cost $4.32 per cord, 8 by 4 by 3 ft., and charcoal $15 per ton. The fuel supply in the surrounding country was approaching exhaustion; more than 150 mules and 50 men were engaged in cutting and transporting this fuel, and the unsettled political conditions in Sonora were such that it would be practically impossible to keep an organization of this kind together. The price of fuel was steadily rising and at times it became almost impossible to get sufficient fuel to operate. It was estimated that the enlarged plant, together with the mine, would require 750 h-p., as follows: Horse-Power. Old mill, which was left unchanged,..............180 New concentrator,.......................90 Cyanide-plant,........................380 Mine and other requirements,................. 100 Total,........•..................750 In a study of the best manner to obtain power the following alternative propositions were considered:

Jan 1, 1914

The co-operation of the members of the Institute is earnestly sought by the Committee on Nominations, recently appointed by the Board of . Directors, in its work of formulating a ticket for officers and places falling vacant in the Board of Directors in February, 1916. The Committee must present the official ticket of nominations to the Board of Directors at its October meeting. Members are, therefore, urged to send promptly their nominations for officers and Directors in order that the Committee may have an opportunity to give them full consideration. The officers to be elected at the annual meeting in February, 1916, are: One officer, known as Director and President. Two officers, known as Director and Vice-President. Five officers, known as Director; The attention of members is called to Articles V and VII of the Constitution, and to By-Law XIII, which reads as follows: "The geographical districts to be considered by the Committee on Nominations shall he as follows, until otherwise ordered by the Board. District No. 1. New England, New York, and New Jersey, excepting New York City and district., which is provided for in the Constitution. (N. B.-New York City and district is designated District 0.) District No. 2. Pennsylvania. District No. 3. Ohio, Indiana, Illinois, Iowa, and Missouri. District No. 4. Minnesota, Wisconsin, and Michigan. District No. 5. Montana, North and South Dakota, Wyoming, Nebraska, Kansas, Washington, Oregon, Idaho, and Alaska. District No. 6. California and Nevada. District No. 7. Utah, Colorado, Arizona, and New Mexico. District No. 8. Louisiana and Texas. District No. 9. Other Southern States and District of Columbia. District No. 10. Mexico. District No. 11. Canada."

Jan 7, 1915

(Under this heading will he published notes sent to the Secretary of the Institute by members or other persons introduced by members.) No. 488.-Mining engineer, member, technical graduate, married, age 38, desires position of superintendent or assistant superintendent. Has had 15 years' practical experience as miner, millman, machinist, surveyor, engineer, foreman, and superintendent in the West, Southwest, and Mexico. Speaks Spanish. Now employed as superintendent of copper property in Southwest. Can give the best of references. Minimum salary $250. Available now. No. 491.-Mining engineer, member, married, age 43, desires to connect with some-good coal company as superintendent or manager. Is thoroughly conversant with flat and pitching systems of coal mining. Has had 23 years experience from the bottom up; 7 years experience as superintendent and manager. Good organizer. Has handled all classes of labor acid has always made good. Available now. No. 492.-Metallurgist and chemical engineer, member, with 8 years executive experience in research and technical direction of all departments of nom-ferrous metallurgical manufacturing, is open for change in position. Specialist in raw materials-and supplies, reclamation of wastes, and standardized control of processes. No. 493.-Member, age 37, technical education, married. Seventeen years' experience as superintendent, engineer, chemist, and assayer, exploration engineer in United States, Central and South America, Siberia and India. Especially in iron, manganese, copper, and rare metals. Desires to make a change. No. 494. Electrometallurgical engineer, member, age 30, A. M. and Ch. E. degrees, thoroughly trained in electrochemistry, metallurgy and electrometallurgy. Three years in charge of experimental work on and operations of electric furnaces. Desires responsible position in investigative or executive work with commensurate salary.

Jan 11, 1918

By G. H. Billings

The following data were collected some years since in the course of a series of experiments with oil as a substitute for coal in puddling, the earlier form of the Archer apparatus being employed. While I am not at liberty to give the name of the works at which the tests were made, I can personally warrant the accuracy of the record, and feel justified, therefore, in making this contribution to a discussion in which all trustworthy figures are likely to be helpful. Oil in Puddling. Starting with everything cold, we used 3518 pounds of oil to get the furnace in condition to charge a heat. After charging, we ran until we took out 13,340 pounds of puddled-blooms, using 8437 pounds, or 1333 gal1ons of oil. At 49 cents per gallon, the cost for oil per gross ton of blooms was $10.91; with coal at $4.871/2, and a consumption of 1.5 tons per ton of blooms (the usual quantity is ton for ton), the cost for coal is $7.31. The quantity of oil consumed in heating the furnace to the proper temperature and to make the bottom, is not included in the oil consumption stated. The quantity used was 3518 pounds of oil. Usually, the furnace need only be lighted, but in this case it had been repaired, and it was necessary to make a new .bottom. This required the quantity of oil necessary to make three heats of blooms, or 2109 pounds. Deducting this from the 3518 pounds leaves 1409 pounds of oil as the quantity consumed every week in lighting up.

Jan 1, 1889

ZAY JEFFRIES, who has been awarded the Douglas medal, established in 1922 by a group of the friends of the late James Douglas for distin-guished achievement in non-ferrous metallurgy, is one of the most notable graduates of the South Dakota School of Mines where he took his B. S. degree in 1910. The following year he was manager of the Ideal Mining Co., at Custer, and in 1911 he became instructor in metallurgy at the Case School of Applied Science, Cleve-land, where he remained until 1917, and in 1918 he took his D. Sc. degree at Harvard. During all this period he was engaged in experi-mental and consulting work for the Electric Railway Improvement Co., t h e Cleveland Steel Tool Co., the W. S. Tyler Co., the Lincoln Electric Co., the Aluminum Castings Co., and the Cleveland wire di-vision of the General Elec-tric Co. He is now en-gaged in general consulting work, especially for the Aluminum Co. of America, the General Electric Co., and the National Tube Co. He has contributed to the Transactions papers on the determination of grain size in metals (with A. H. Kline and E. B. Zimmer) LIV, 594; grain growth phenomena in metals, LVI, 571; the tungsten-molyb-denum equilibrium diagram and system of crystalliza-tion, LVI, 600; grain size inheritance in iron and carbon steel, LVIII, - 669; effect of temperature, de-formation and grain size on the mechanical properties of metals, LX, 474; metallography of tungsten, LX, 588; physical changes in iron and steel below the thermal critical range, LXIII, and LXVII, 56; and the trend in the science of metals, LXX, 303. In addition to participating freely in the discussion of other papers before the Institute he has found time to contribute notable papers to the Institute of Metals (Great Brit-ain), the principal technical journals, and to write a book on "The Science of Metals" in collaboration with R. S. Archer.

Jan 2, 1927

By J. Leja, N. Sheikh

The stability of lead ethyl xanthate precipitate in aqueous environment of different pH (4.5 to 10.5) and at temperatures 25°C-60°C was investigated. Dissolution leads to a wide variation of pH, xanthate, and lead ions concentration in solution and to a deposition of solid products of reactions. X-ray diffraction patterns of these solids enabled identification of Pb(OH)3, PbCO3, and PbS as constituents of the remaining undecomposed Pb(EtX)1, together with some unidentified compounds (which give rise to intensive peaks with d values of 2.82A and 1.71A, and numerous peaks of lesser intensity).

Jan 1, 1974

Jan 1, 1931

By R. C. Stevens

INTRODUCTION Idarado Mining Company, a subsidiary of Newrnont Mining Corporation, is situated high in the San Juan Mountains in southwestern Colorado. Portals, offices and surface plants are located near the towns of Ouray and Telluride at elevations ranging from 9,000 to 12,000 feet. The Ouray portion of the development was initiated in 1943. Upon completion in 1945 of a 250-ton mill, processing of development ores containing copper, lead and zinc was undertaken; thus, serving as a pilot testing unit for larger scale milling operations. These facilities were subsequently enlarged and utilized until 1956. Meanwhile, in 1953 Idarado had acquired The Telluride Mines Company, 62 miles distant by highway; however, only six miles via a network of tunnels which eventually linked the two workings. Extensive underground development and increased ore production necessitated reconstruction and expansion of the milling plant. The facility was designed to accomodate processing of 1700 tons of ore daily. This goal was achieved and it represents the current daily output. MINERALOGY The veins are a compound fissure which have undergone several stages of mineralization. The first stage is represented by complex ores of copper, lead and zinc in a quartz gangue. Precious

Jan 1, 1970

By O. E. Kiessling

THIS announcement of the topics relating to production control, which the Committee hopes to have discussed at the February meeting, supplements the preliminary announcement published in the November number of MINING AND METALLURGY. In the previous article, the writer indicated the kaleide-scopic nature of the questions involved in obtaining better coordination in industry, and that, as a matter of practical expediency, the discussion in February would be limited to the more obvious difficulties in industry which need attention and to those questions which the Committee thinks would be of greatest interest to members of the Institute. But while practical considerations necessitate limiting the program, free discussion of all phases of the subject is urged by 'the Committee. In a preliminary consideration of the production control problem, there loom up two questions which have to be faced: (1) First, there is the question of the extra industrial capacity necessary to meet demand during the ordinary fluctuations of business, commonly characterized as `the "business cycle." Anyone who tries to formulate a program pertaining to productive capacity must decide whether he wishes to discuss the control of business cycles. While this question may eventually lend itself to treatment, the Committee does not feel that it can be considered at present with much profit. (2) The second question arises from the existence of over-stimulated capacity above and beyond peak demands in boom times. Discussion of this topic, it is felt, would be most fruitful. How to prevent capacity from being over-stimulated to an extent beyond any hope of possible demand is a

Jan 1, 1929

By Norman Maxwell

There was more activity in crude production in northwestern Pennsylvania in 1935 than for several years before, resulting in an increased oil production and also in the number of wells completed. Crude -production approximated 16 million barrels for the state, an increase of about one million barrels over 1934. Demand, indicated by refiners' runs to stills, increased proportionally, leaving stocks of available crude at the end of the year at the lowest point since the middle of 1934, when they reached an all-time low. The price of crude varied during the year from a low of $2.02 to a high of $2.27 at the end of the year for Middle district oil. The price of Bradford and southwest Pcnnsylvania oil changed accordingly. The average for the year would be a lower price than in 1934. A summary of the production data for the year 1935 is given in Table 1. In making up this table, 1935 figures were simply added to the table published by S. H. Cathcart last year1. A list of important wildcats is given in Table 2. Bradford Field Approximately 10,000 acres of the proven producing area of the Bradford field is in Cattaraugus County, New York, and it is possible, by differences, to distinguish the Pennsylvania production from the New York portion. The listed production for the Bradford field includes only that portion of the field situated in Pennsylvania, but also includes production from a small pool, locally known as the Mt. Jewett-Kanesholm pool, where the Bradford sand is being developed and flooded in precisply the same manner as that of the Bradford field itself. The Mt. Jewett-Kanesholm pool is not, strictly speaking, an extension of the Bradford field, but inasmuch as it is so closely allied with the Bradford field-—that is, the sand is the same and the production methods are the same—the production and drilling figures include this area.

Jan 1, 1936

By Norman Maxwell

There was more activity in crude production in northwestern Pennsylvania in 1935 than for several years before, resulting in an increased oil production and also in the number of wells completed. Crude -production approximated 16 million barrels for the state, an increase of about one million barrels over 1934. Demand, indicated by refiners' runs to stills, increased proportionally, leaving stocks of available crude at the end of the year at the lowest point since the middle of 1934, when they reached an all-time low. The price of crude varied during the year from a low of $2.02 to a high of $2.27 at the end of the year for Middle district oil. The price of Bradford and southwest Pcnnsylvania oil changed accordingly. The average for the year would be a lower price than in 1934. A summary of the production data for the year 1935 is given in Table 1. In making up this table, 1935 figures were simply added to the table published by S. H. Cathcart last year1. A list of important wildcats is given in Table 2. Bradford Field Approximately 10,000 acres of the proven producing area of the Bradford field is in Cattaraugus County, New York, and it is possible, by differences, to distinguish the Pennsylvania production from the New York portion. The listed production for the Bradford field includes only that portion of the field situated in Pennsylvania, but also includes production from a small pool, locally known as the Mt. Jewett-Kanesholm pool, where the Bradford sand is being developed and flooded in precisply the same manner as that of the Bradford field itself. The Mt. Jewett-Kanesholm pool is not, strictly speaking, an extension of the Bradford field, but inasmuch as it is so closely allied with the Bradford field-—that is, the sand is the same and the production methods are the same—the production and drilling figures include this area.

Jan 1, 1936

By M. L. Fuller

MOST commercial alloys undergo changes in phase composition after casting. This is a natural result of the fact that the alloys are not in a state of phase equilibrium as cast and phase changes will therefore take place, with more or less rapidity, in an attempt to attain equilibrium. The practical aspect of aging in zinc-alloy die castings concerns the changes in physical properties and in dimensions that may accompany aging phase changes. Harmful alterations have been reduced to a minimum and zinc-alloy die castings are being produced today that are so stable with respect to dimensions and physical properties that they are entirely suitable for most practical purposes1. In the first paper' of this series, and in this paper, aging phase changes of zinc alloy die castings have been investigated and the possible influence of these changes on dimensional changes of the castings has been evalu-ated and compared with the dimensional changes actually experienced. The change of dimensions has been selected for practical comparison in these papers because the effect of phase changes on the dimensions of a casting is directly calculable; from X-ray crystal-analysis data of the phase structure. The die-casting alloys considered contain, in addition to zinc, 4 per cent of aluminum, about 0.03 per cent magnesium, and from 0 to 3 per cent of copper. It was shown in the former paper that the eutectoidal decomposition of the beta aluminum-zinc phase, while intrinsically capable of causing a considerable shrinkage, can have very little effect on the observed shrinkage of die castings because it takes place within a few days of aging, whereas the observed shrinkage continues for five weeks. It was therefore concluded that the other existing phase change,

Jan 1, 1936

By Eugene S. Meieran

The effects of methods of crystal growing, wafer sawing, polishing, routine handling, diffusion, and epitaxial growth on the defects in GaAs are reviewed and studied using reflection and transmission X-ray topographic techniques. In general, it was found that boat-grown crystals exhibited fewer defects than Czochralski crystals, although all crystals showed large numbers of precipitates visible when examined in the electron microscope. Mechanical surface treatments such as sawing and mechanical polishing introduce damage to a depth of about 5 µ, most of which can be removed by suitable chemical or chem-mechanical polishing. In addition, defects can be introduced through routine handling of wafers, for example with metallic tweezers. These defects can be quite severe, and have been observed 20 µ below the wafer surface. Defects can also be introduced through diffusion and epitaxial growth. These defects, which include precipitates, growth pyramids, stacking faults, dislocations, and so forth, can be detrimental to device fabrication. It is shown that wafers or films which appear defect-free optically can contain defects visible in the X-ray topographs. WHILE the use of GaAs in the semiconductor industry has increased very rapidly in the last few years, due mainly to the recent development of many important GaAs devices,1,2 the major limit to the production of commercial quantities of many GaAs devices remains a severe lack of suitable materials technology. This lack is apparent in two critical areas. First, production quantities of high-quality GaAs crystals, reproducibly doped and precipitate-free, simply are not available commercially, although some reasonable quality material is available on a limited first-come, first-serve basis. Second, in comparison to silicon technology, little is known about the effects of processing variables on the defects either present in as-grown GaAs or introduced through processing and handling of wafers. These areas are now receiving some attention from semiconductor device manufacturers, who are studying defects in GaAs in order to better understand how either to prevent their occurrence or to cope with their existence. Most investigations of the defects in GaAs have been made by optical microscopy3-5 or transmission electron microscopy techniques.'-' Recently, however, the imaging techniques of X-ray topography, electron mi-croprobe analysis, and scanning electron microscopy are being applied to the study of GaAs.9-14 In the case of X-ray topography, a one-to-one image is obtained that must be photographically enlarged. In compensa- tion, the defects within entire wafers may be imaged by simple scanning (Lang technique15) if the wafer is reasonably perfect, or by using the scan oscillation technique developed by Schwuttke16 if the wafer is warped or distorted. The purpose of this paper is to both review and extend the general application of X-ray topographic techniques to GaAs. Emphasis will be placed on the effects of growth and process variables on the quality and perfection of both bulk and epitaxial GaAs. Reference to optical or electron microscopy results will be made when useful. Since the effects on defects of a wide variety of processing variables such as crystal growing, sawing, polishing, diffusion, and epitaxial growth will be somewhat superficially reviewed, a fairly extensive bibliography of the most important recent results in these areas is included. However, for completeness, important defects will be illustrated here, although such defects have been previously shown by others. While this paper is concerned with defects rather than with the physics of X-ray scattering, the mechanisms of contrast formation in the topographs will of necessity be briefly mentioned. EXPERIMENTAL GaAs crystals, both boat-grown18 and Czochralski-grown,'8 containing a variety of dopants of various concentrations, were purchased from outside vendors. Wafers were sliced from the crystals using a Hamco ID saw and were mechanically polished using 1 µ diamond paste. Chem-mechanical polishing was done in bromine-methanol as described by Sullivan and Kolb.18 Chemical polishing was done using a modified sulfuric-peroxide solution, 11 parts H2SO4, 1 part 30 pct H2O2, 1 part DI water.5 Zinc diffusion was carried out in a closed tube, using a 10 pct Zn-In source at 825°C for 1 hr. Oxide masking techniques were used to select the area to be diffused. Epitaxial wafers were either purchased or prepared here. All epitaxial runs prepared here were carried out using a Ga-GaAs-AsC13 source in a closed tube at a substrate temperature of 750°C. Wafers were chem-mechanically polished and gas-etched prior to deposition. The X-ray topographs were taken on a Krystallos Lang camera, operating in the transmission scanning geometry (Lang technique15) or in the reflection scanning geometry (modified Berg-Barrett technique20,21). MoKa, radiation was used for all transmission topographs using a Jarrell-Ash 100-µ spot focus. CuKal radiation was used for all reflection topographs using a General Electric CA-7 1-mm spot focus X- ray tube. Topographs were printed from an intermediate contrast inversion film, so the contrast shown in all figures here is the same as that of the original 50-µ-thick emulsion L4 Iiford nuclear plate used to record the topograph.

Jan 1, 1969

By S. G. Cupschalk, F. A. Dahlman, J. J. Wert

Studies have been undertaken to determine the indicidual effects of particle size, degree of long-range ovder, antiphase domain size, and root mean square stran on the microhardness and yield strength of ordered alloys. Dnta have been analyzed for Cu3Pt initzally ordered to a value of 0.82 and after deformations of 1 and 6 pct. It was observed that deformation fleatly reduced the degree of long-range order. Furtherrnore, wztkin this range of relatively small deforntntlons, the average particle size changed very little while the antiphase domain size was greatly reduced. Smultaneosly, the mcrohardness changed by a factor of two durzng the deforrtation process. PREVIOUS studies have reported some of the effects of cold work on the broadening of X-ray diffraction peaks. These investigations were performed on powder and wire samples representing both ordered and disordered states; i.e., the specimens were initially studied in a severly cold-worked condition. By comparing the difference in line shape between the annealed and cold-worked peaks, fundamental information was obtained concerning particle size, strain distribution in different crystallographic directions, degree of long-range order, and change in antiphase domain size. Considerable theoretical work has been done concerning the analysis of diffraction data obtained from cold-worked metals. Stokes' expressed the change in diffraction profiles in terms of Fourier coefficients. Much of the work in this area has been summarized by warren2 in an extensive review article concerning the analysis of plastic deformation by X-ray diffraction. Cohen and Bever3 applied these techniques in studying the effects of cold work on alloy systems exhibiting long-range order. They utilized the Fourier coefficients of fundamental peaks in conjunction with those of the superlattice peaks to determine the change in antiphase domain size. Little work of this nature has been reported for ordered systems that have undergone small degrees of plastic deformation. The purpose of this investiga-tion was to determine the effects of small deformations in such a material with respect to particle size, strain distribution in various crystallographic directions, antiphase domain size, degree of long-range order, and hardness. EXPERIMENTAL PROCEDURE CusPt was used for the initial investigation since the order-disorder transformation takes place with- out a change in crystal structure. The transformation is readily detectable via X-ray diffraction techniques due to the large difference in the scattering factors of copper and platinum. Additionally, the alloy is relatively low melting (approximately 1300°C) and is easily deformable in both the ordered and disordered states. 1) Specimen Preparation and Cold Working. A 100-g, 12-in. diam., cylindrical specimen of Cu3Pt was prepared by melting and casting 99.99 pct pure Cu and Pt i.n vacuo. Prior to any mechanical working, the material was homogenized in a vacuum for 60 hr at 100O0C, and surface defects were removed by machining to a depth of approximately 116 of an in. The material was then cold-rolled, with an intermediate anneal, into a strip approximately 12 in. wide by 14 in. thick. Straightening and flattening removed another 0.025 in. from the thickness. After a recrystallization treatment at 750°C for 30 min, the specimen was slow-cooled from 55OoC, at the rate of 6°C per hr, down to 150°C to induce superlattice formation. This treatment yielded an ASTM grain size of 7 and a degree of long-range order equal to 0.83 0.06. After obtaining X-ray and Knoop hardness data, the sample was cold-rolled approximately 0.75 pct in one pass through a hand-operated jewelers' mill. X-ray and hardness data were again obtained and the specimen was reduced an additional 5.41 pct in a single pass through the mill. 2) X-Ray Measurements. The specimen was examined in the ordered condition and after the two degrees of cold working previously mentioned using a General Electric XRD-5 unit equipped with a spectrometer and scintillation counter. Using Mo-Ka radiation with a zirconium filter, six orders of the 100 reflection were obtained. It was anticipated that point counting would be necessary for an accurate determination of the low-intensity peaks and tails: however, it was demonstrated that, by using a scanning speed of 0.2 deg per min and the appropriate time constant, the recorded data were sufficiently accurate. Thus, for ease of experimental procedure, all peaks were recorded on chart paper. Specimen position in the holder was considered to be insignificant after making a series of measurements of the same peak area in different positions with respect to the beam. Since peak overlapping did occur at high values of 20, it was necessary to separate the peaks graphically prior to analyzing the data in order to minimize this source of error. The peak tails were also carefully drawn to obtain the best possible data. Fourier coefficients of the line profiles were calculated on an IBM 7072 computer, and graphical meth-ods2j3 were employed in analyzing the results. For this type of calculation, in which the line profile is represented by intensities taken at set intervals, the intervals selected must be sufficiently small to give an accurate representation of the line profile. It was decided that for 20 = 0.02 deg the line profiles were

Jan 1, 1967

By R. Grierson, L. J. Bonis

The high-temperature Strength oF TD nickel has been observed to be dependent upon the previons thermal and mechanical history of the material. Variations in both the level and the anisotropy of strength have been observed. 01 this paper- these variations are correlated with the storing of annealing resistant elastic strain energy in the matrix of the TD nickel. An x-vay line -broadening tecknique is used to measure the maLrTis elastie strain. THE inclusion of a finely dispersed second phase into a ductile matrix has long been recognized as an extremely effective method of strengthening the matrix both at high and at low homologous temperatures. It has been found, however, that the factors which determine the high-temperature strength are not the same as those which are important at low temperatures. Below 0.5 Tm the size and distribution of the second phase particles are of prime importance in determining the strength,')' while above this temperature the strength is mainly dependent upon the previous thermal and mechanical history of the alloy,3-7 This paper is primarily concerned with explaining the response of the high-temperature mechanical strength of one of these alloys (DuPont's TD nickel) to various thermo-mechanical treatments. It will be shown that this response is not associated with the occurrence of any form of dislocation substructure within the matrix of the alloy. It has been found, however, that a correlation does exist between the elastic strain level in the matrix and the previous thermomechanical history of the alloy and that the observed changes in elastic strain level parallel the measured changes in high-temperature strength. It therefore must be concluded that variations in high-temperature strength are a direct result of the variations in elastic strain level. MATERIAL TD nickel contains approximately 2 vol pct of Tho2 in an unalloyed nickel matrix. It is formed, as a powder, by a chemical technique and this powder is compacted to form ingots which are then extruded to give 21/2-in.-diam rod. Rod of smaller diameter is prepared from the as-extruded rod by swaging. In the studies reported in this paper, 1/2-in.-diam rod was used. This rod received an anneal of 1 hr at 1100°C prior to being used in any of these studies. EXPERIMENTAL TECHNIQUES Two methods were used to examine the structure of the nickel matrix of the TD nickel. These were: 1) transmission electron microscopy; 2) the analysis of the position and profile of X-ray diffraction lines obtained using the nickel matrix as the diffracting media. To prepare thin foils for electron-microscopical examination, slices of TD nickel approximately 0.050 in. thick were cut from the as-received 1/2-in.-diam rod. These were then chemically polished down to 0.045 in., rolled to 0.009 in., given a predetermined heat treatment, and thinned, using a modified Bollman technique, to provide the foils for observation. All observations were carried out at 100 kv, using a Hitachi HU-11 electron microscope. Specimens of the undeformed rod were prepared by grinding down the 0.050-in.-thick slices to approximately 0.015 in. and then thinning chemically and electrolytically to give the thin foils. The X-ray specimens were prepared by rolling 0.375-in.-thick rectangular blocks down to 0.075 in. The surfaces of the rolled material were ground flat, chemically polished to remove the layer disturbed by the grinding, and given a predetermined anneal in an inert atmosphere. They were then ground lightly to check their flatness and given a final chemical polish prior to being examined. The X-ray diffraction line profiles were measured using an automated Picker biplane diffractometer. A special specimen holder was built to allow a more accurate and reproducible positioning of the specimen. The line profiles were determined by carrying out intensity measurements at intervals of either 1/30 deg or 1/60 deg over a range of 3 deg on either side of the nickel peaks of interest. A piece of pure nickel which had been recrystallized to give a large grain size was used as a standard to give the X-ray line profile generated by a strain-free matrix. The analysis of the X-ray diffraction line profiles is a modification of that due initially to Warren and Aver-bach8and has been described elsewhere.3 This analysis gives a measurement of two parameters associated with the structure of the nickel matrix. These parameters are: 1) the size of the coherently diffracting domains within the nickel matrix; 2) the magnitude of the elastic strains in these domains. Both of these parameters are first determined in terms of a Fourier series. These series are obtained from other Fourier series which describe the measured profile of the X-ray diffraction lines. Thus, for both the coherently diffracting domain size and the elastic strain level, it is possible to plot Ft (the Fourier coefficient) against t (the term in the Fourier series), where t can be expressed in terms of a distance L and the Fourier coefficient Ft(S) (associated with elastic strain level) can be expressed in terms of the root mean square strain (e2)1/2. Thus a plot of (F 2)1/2 vs L can be obtained. Plots of this type are shown graphically in Figs. 6 and 8. Interpretation

Jan 1, 1968

By N. F. Dyson, T. R. Scott

The iilzfluence of catalytic agents on the oxidation of ZnS has been studied under pressure leaching conditions, using a chemically prepared sample of ZnS which was substantially unreactive on heating at 113°C with dilute sulfuric acid and 250 psi oxygen. Nurnerous prospective catalysts were added at the ratio of 0.024 mole per mole ZnS in the above reaction but pvonounced catalytic activity was confined to copper, bismuth, rutheniuwl, molybdenum, and iron in order of. decreasing effectiveness. In the absence of acid, where sulfate was the sole product of oxidation, catalysis was exhibited by copper and ruthenium only. Parameters affecting the oxidation rate were catalyst concentration, temperature, time, oxygen pressure, and a7riount of acid, the first two being most important. The main product of oxidation in the acid reaction was sulfur, with trinor amounts of sulfate. An electrochemical (galvanic) mechanism has been suggested for the sulfuv-forming reaction, whereby the relatively inert ZnS is "activated" by incorporation of catalyst ions in the lattice and the same catalysts subsequently accelerate the reduction of dissolved oxygen at cathodic sites on the ZnS surface. Insufficient data was obtained to Provide a detailed mechanism for sulfate fornzation, which is favored at low acidities and probably proceeds th'rough intermediate transient species not identified in the preseni work. THE oxidation of zinc sulfide at elevated temperatures and pressures takes place according to the following simplified reactions: ZnS + io2 + H2SO4 — ZnSO4 + SG + HsO [i] ZnS + 20,-ZSO [21 In dilute acid both reactions occur but Reaction [I] is usually predominant, whereas in the absence of acid only Reaction [2] can be observed. Both proceed very slowly with chemically pure zinc sulfide but can be greatly accelerated by the addition of suitable catalysts, as suggested by jorling' in 1954. Nevertheless, an initial success in the pressure leaching of zinc concentrates was achieved by Forward and veltman2 without any deliberate addition of catalytic agents and it was only later that the catalytic role of iron, present in concentrates both as (ZnFe)S and as impurities, was recognized and eventually patented.3 It is now apparent that another catalyst, uiz., copper, may have also played a part in the successful extraction of zinc, since copper sulfate is almost universally used as an activator in the flotation of sphalerite and can be adsorbed on the mineral surface in sufficient amount The importance of catalysis in oxidation-reduction reactions such as those cited above has been emphasized by various writers and Halpern4 sums up the situation when he writes that "there is good reason to believe that such ions (e.g., Cu) may exert an important catalytic influence on the various homogeneous and heterogeneous reactions which occur during leaching, particularly of sulfides, thus affecting not only the leaching rates but also the nature of the final products." Nevertheless relatively little work has appeared on this topic, one of the main reasons being that sufficiently pure samples of sulfide minerals are difficult to prepare or obtain. When it is realized that 1 part Cu in 2000 parts of ZnS is sufficient to exert a pronounced catalytic effect, the magnitude of the purity problem is evident. An incentive to undertake the present work was that an adequate supply of "pure" zinc sulfide became available. When preliminary tests established that the material, despite its large surface area, was substantially unreactive under pressure leaching conditions, the inference was made that it was sufficiently free from catalytic impurities to be suitable for studies in which known amounts of potential catalytic agents could be added. The first objective in the following work was to identify those ions or compounds which accelerate the reaction rate and, for practical reasons, to determine the effects of parameters such as amgunt of catalyst, temperature, time, acid concentration, and oxygen pressure. The second and ultimately the more important objective was to make use of the experimental results to further our knowledge of the reaction mechanisms occurring under pressure leaching conditions. The fact that catalysts can dramatically increase the reaction rate suggests that physical factors such as absorption of gaseous oxygen, transport of reactants and products, and so forth, are not of major importance under the experimental conditions employed and an opportunity is thereby provided to concentrate on the heterogeneous reaction on the surface of the sulfide particles. As will appear in the sequel, the first of these objectives has been achieved in a semiquantitative fashion but a great deal still remains to be clarified in the field of reaction mechanisms. EXPERIMENTAL a) Materials. The white zinc sulfide used was a chemically prepared "Laboratory Reagent" material (B.D.H.) and X-ray diffraction tests showed it to contain both sphalerite and wurtzite. The specific surface area, measured by argon absorption at 77"K, varied between 3.9 and 4.6 sq m per g. Analysis gave 65.0 pct Zn (67.1 pct theory) and 31.9 pct S (32.9 pct theory). Other metallic sulfides (CdS, FeS, and so forth) used in the experiments were also chemical preparations of "Laboratory Reagent" grade. Samples of mar ma-

Jan 1, 1969

By C. H. Li, R. J. Stokes, T. S. Liu

Poly crystalline silver chloride specimens having different micro structures were prepared by extruding monocrystals or precompressed powder at varying temperatures. Extrusion at high temperature (370°C) produced a Fully recrystallized equi-axed material which was brittle and fractured by simple cleavage below its transition temperature (60°C for notched specimens). Extrusion at low temperatures (down to -196°C) produced an extremely tough cold-worked material with grains elongated in the extrusion direction. This material fractured below its transition temperature (which varied from —20" to —200°C) by an intergranular mode. It is concluded that cold work increases the resistance to transgranular cleavage. Fracture is then de-flected to propagate intergranularly ouer surfaces making an angle with the tensile axis with a corresponding improvement in notch toughness. This deflection is greater for extruded powder than for extruded monocrystals because of the extremely elongated grain shape. PREVIOUS work1,' on the fracture properties of fully recrystallized silver chloride under notch impact conditions has indicated that the fracture behavior is rather invariant. Thus polycrystalline materials originating from a number of sources ranging from relatively pure Harshaw single crystals to commercial-purity powder and prepared by hot extrusion at 370°C all fracture by simple cleavage with a ductile-brittle transition at 60°C, see Fig. 1. This behavior is also typical for fully annealed single crystals and appears to be fundamental to silver chloride for the particular loading conditions and notch configuration adopted. One way in which this characteristic fracture behavior can be modified is by the dispersion of alumina particles in the silver chloride matrix.' Then, particularly when the alumina particles are in the shape of spheres, the duc tile-brittle transition is much less sharply defined and occurs over a range of temperature, the transition temperature is lowered considerably and the fracture mode changes from simple cleavage to a fibrous or shear mode. The reason for this change is believed to be partly due to the nucleation of cavities in the region of the dispersed alumina particles which influences the state of stress locally and the distribution of plastic constraint at the root of the notch. It is emphasized however that this is not the sole factor responsible for the increase in toughness. In extruded materials it is reasonable to expect that the resultant grain size, texture, and the residual cold work will be influenced by the presence of a dispersed phase. The present experiments were initially designed to determine the extent to which cold work influenced the fundamental ductile-brittle transition temperature and fracture mode of silver chloride. They were stimulated by the discovery that silver chloride could be extruded at temperatures as low as -25°C when commercial-purity powder was used and as low as -196°C when single crystals were used. This working temperature was far below that previously used (370°C) and it was found that such extruded material was exceedingly tough. The reasons for the enhanced toughness and its relation to the previous work on silver chloride-alumina compacts will be discussed. EXPERIMENTAL PROCEDURE Materials Used. Two forms of silver chloride were used in this study: i) silver chloride powder

Jan 1, 1964

By Frank Miller

THE lower cost of producing oil from naturally flowing wells compared with pro-duction costs accruing from artificial lifting methods has stimulated much research, with the joint purpose of extending the natural flowing life of wells and of increas-ing the productivity of small wells. The laboratory investigation described herein was made to determine the effect of a slotted liner on the pressure gradient in the vicinity of the wall of a flowing well. Flow restrictions caused by the liner induce energy losses between the oil-bearing for-mation and the inside of the liner, which may be reduced by improved liner design, and thereby the flow capacity of wells may be increased. These losses have been evalu-ated for rectangular slots of different sizes, and means are suggested for reducing them. The dearth of information concerning the nature of the flow of fluids from uncon-solidated sands through small openings in the walls of pipes-as represented by the flow of oil from an oil sand into a slotted liner-is acknowledged. Although the bene-fits to be realized by operators through the use of optimum liners is just beginning to be recognized generally, Coberly1 in 1937 pointed out that the functioning of screen casing is an important factor in the pro-duction of oil. From his study on the selection of size of oil strings for wells in California, Parks2 concluded, in part, that the perforated section of the oil string de-serves continued study, especially with respect to the selection of perforations. The growing use of gravel packing result-ing from certain research findings lends even more significance to the problem of selecting optimum liners, as the application of these methods usually requires slotted liners or other kinds of perforated liners. The present study was made to obtain further information for the guidance of engineers and operators in selecting slotted liners and to develop a laboratory method that may be used in analyzing possible pressure conditions surrounding most types of perforated casings used in producing oil wells, so that the present inadequate fund of knowledge on this important subject may be expanded.

Jan 1, 1940