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By John W. Burd

A system is described for the simultaneous deposition of epitaxial layers on as many as eight substrates. A high degree of uniformity of both physical and electrical characteristics is achieved in the films. Variation of film thicknesses is consistently less than ±10pct within a wafer and from wafer to wafer within a run with the variation typically on the order of 55 pct. Composition variation of GaAs1-x PX layers within a wafer and from wafer to wafer within a run is consistently less than 51 pct. Electrical evaluation of the films by several techniques indicates excellent doping uniformity within a wafer and from wafer to wafer within a run. Mobilities for lightly doped GaAs films at 300°K are consistently >6000 cm2 v-1 sec-1 and mobilities > 7000 cm2 v- 1 sec-1 are regularly attainable. Techniques for the preparation of material with carrier concentrations from 1 x 1015cm-3 to 1 x 1019 cm-3 n-type and 5 x 1016 to 5 x 1018 cm-3 p-type are discussed. METHODS for the preparation of 111-V compounds by vapor phase reactions have been extensively reported in the literature.1-6 Almost all of the apparatus described for these various methods are suitable for processing one or at the most a very limited number of wafers simultaneously. With the recent rapid advances in the use of vapor grown GaAs for microwave oscillators and GaAs1-xPx as visible light emitters the requirements for these materials are steadily increasing. In order to satisfy these requirements it is necessary to move from a laboratory scale apparatus to one which is capable of processing a large number of wafers simultaneously. Desirable features would be a high degree of uniformity among the wafers and good reproducibility from run to run. The apparatus to be described fulfills these requirements very well. DISCUSSION The various methods reported in the literature can be classified under three headings: 1) closed tube, 2) open tube, and 3) the close-spaced method. Of these three the open-tube method is the most amenable for scale-up to a manufacturing process. It is the most versatile and the various operating conditions can be more precisely controlled than with the other two methods. A number of chemical reactions may be used to achieve vapor-phase growth of 111-V compounds. Sev-era1 of the more generally used reactions are shown in Fig. 1. All of these reactions have the following points in common: 1) generation of a volatile group III(Ga) species by the reaction of the transport agent (halide or HC1) with either Ga or GaAs, 2) introduction of the Group V(As and/or PI component, 3) a method of adding dopant, if desired, and 4) a region in which deposition from the vapor will occur and form as a single crystal epitaxial film on the substrates. The laboratory scale reactors permit the hot re-actant gases to flow into the relatively cooler deposition zone and pass successively over the several substrates which are arrayed along the long axis of the tube parallel to the gas flow. With this arrangement the composition of the reactant stream is continually changing as solid material is deposited on each successive substrate. As a result of this changing gas composition the reaction driving force also changes from substrate to substrate and the degree of uniformity of layer thickness, doping level, and so forth, is poor. This effect can be partially overcome by imposing a controlled temperature gradient along the deposition region to compensate for change in gas composition. However, even when this is done variations in layer thickness on the order of 30 to 40 pct are common and as high as 50 pct are frequently experienced between adjacent wafers in the tube. To expand this arrangement to a large number of wafers would only increase the nonuniformity from the first to last wafer in the line. From the above discussion the two undesirable features of changing gas composition and temperature gradient become evident. A reactor system which eliminates or minimizes these undesirable features is one in which the apparatus is mounted vertically as shown schematically in Fig. 2. The vertical mounting permits the disposition of a number of substrates on a suitable support so that all wafers are at the same vertical height in the furnace and hence at essentially the same temperature. By using only a single row of wafers the reactant gas mixture passes over only one substrate in its path through the reactor. Thus the two undesirable features of changing gas composition and temperature gradient are minimized. An additional design feature which further minimizes temperature variations is rotation of the substrate holder. Rotation serves to integrate any radial temperature gradient existing around the resistance heated furnace. A photograph of a reactor assembly at the completion of a run is shown in Fig. 3. MATERIAL PREPARATION Apparatus. Although any of the several chemical systems shown in Fig. 1 are adaptable for use in this apparatus the one generally used is System 2, the hydride synthesis system. This system has been de-

Jan 1, 1970

By T. F. Archbold, W. H. King

THE diffusivities of gold in polycrystalline copper have been determined in the temperature range from 700° to 1000°C by the utilization of the neutron-activation method. Martin, Johnson, and ~saro' used this method for their investigation of the diffusion of gold into copper at 375° and 550°C for 59 days in order to circumvent the experimental difficulties imposed by the 2.7-day half-life of Au-198. They employed the conventional technique of depositing Au-198 on copper specimens for short-time dif-

Jan 1, 1965

By Howard N. Eavenson

The mines of the United States Coal & Coke Co. are located in the Pocahontas coal field, in McDowell County, West Virginia. Twelve plants have been opened and equipped, of which, by reason of the present business depression, only nine are now in operation. These twelve plants serve eighteen mines; some of the plants having several openings, in either the same seam or in different seams, tributary to the same tipple. Only nine of these mines are now being worked at the plants in operation. Construction work was begun in 1902, and coal from the first three plants started was shipped in December of that year. An additional plant was opened in 1903, two in 1904, two in 1905, two in 1907 and the last two in 1908. On Jan. 1, 1915, the plants have been in operation an average period of 8.8 years. The rules of the company, which have been in operation since work was first begun, are similar to those in use by the H. C. Frick Coke Co. at its mines in Pennsylvania, in which " Safety First" was incorporated as early as 1907; and it has always been the policy of both companies to look carefully after the safety of their employees. Although the field is an extension of the old Pocahontas field, the mines, located upon a new branch railroad, are away by themselves, and, as is usual in such cases, the class of labor attracted at first was temporary in character. The rapid development of the mines required the employment of many new men and officials each year; and, while the accident record from 1904 to 1909 was as good as the average of the field, it was felt to be not as good as it could be made, and a determined campaign was inaugurated for preventing accidents of all kinds. Fig. 1 shows the tonnage of coal produced per fatality, both total and for inside accidents only, at our mines; the tonnage per fatality of all West Virginia mines, and of those in the Pocahontas field. The purpose of this paper is not one of congratulation on the results so far accomplished, since the operating officials are not at all satisfied that the maximum is in sight, to say nothing of its having been reached; but to describe the organization and methods that have produced these

Jan 1, 1915

By T. Sterry Hunt

The deposit of rock-salt which is known to exist along the eastern shore of Lake Huron, in the province of Ontario, has lately been more completely explored than before, by a boring with a diamond drill, put down by Henry Attrill, Esq., of New York City, and the results obtained are so important in every way that I make no apology for presenting them to the Institute of Mining Engineers. I may be permitted to preface an account of this remarkable exploration, and of its results, with a historical sketch of the discovery and development of this salt-region. It was in December, 1865, that a boring was begun near the town of Goderich, in the hope of finding petroleum. In this the adventurers were disappointed, but, after passing through about 800 feet of limestone, they encountered a series of variegated marls, in which, at a, depth of 964 feet from the surface, a bed of rock-salt, 30 feet in thickness, was met with in May, 1866. The boring was carried to a depth of 1010 feet, ending in hard rock, and yielded, by pumping, a very pure saturated brine when examined by me in August of the same year. In the report of the Geological Survey of Canada for 1863-66, published early in 1867, I described this salt-well, with many geological details, and gave an analysis of the brine. In the next three years a considerable number of wells was sunk in and around Goderich, and numerous trials were made in various other parts of the region. Salt was found at Kincardine, thirty miles north-northeast from Goderich, at a depth of about 900 feet, and also at Clinton, thirteen miles southeast, at 1180 feet. Records of these wells, with analyses of the brine from them, were given by myself in a subsequent report of the Geological Survey, 1866-69, published in 1870 (pp. 211-244), together with accounts of various unsuccessful borings in the neighborhood, analyses of the brines from the various wells (including one analysis by Dr. Goessmann), with many details of the salt-manufacture at Goderich, at Syracuse, New York, and at Saginaw, Michigan. The geological character of the region was there discussed at length, and it was shown that the salt here occurs in the Onondaga or Salina formation, which

By Harry M. Mikami

Chromite is the only ore mineral of metallic chromium and chromium compounds and chemicals. Because of this fact, chromite and chrome ore are used synonymously in trade literature. In commercial market quotations, chrome ore is the term commonly used. Chromite per se, because of properties imparted by its chromium content, is used in refractories and in special purpose molding sands for metal casting. There are many other minerals containing some, generally minor, amounts of chromium, but none are commercial sources of the element (Thayer, 1956). Chromium and chromite have many diverse uses that, directly and indirectly, critically affect vast segments of our modern industrial system. Most important are probably the metallurgical applications wherein chromium is a component of heat-, abrasion-, corrosion-and oxidation-resistant and high-strength alloys of many types. Stainless steels are the largest volume category of chrome-bearing alloys. Chromium chemicals are used in leather tanning, in pigments, dyes and mordants, printing, chemical process industries, photography, pharmaceuticals, metal plating, pure chromium metal production, and for many other purposes. Chromite is a necessary constituent in basic refractories indispensable for the production of steel, copper, cement, and glass. Under present conditions, the US and North America, with the possible exception of Cuba, have no commercial ore reserves. There are chromite deposits, as will be described, but they would be used only under highly abnormal conditions if all outside sources were cut off for an extended period. All chromite used in the US is imported from the eastern hemisphere in which are contained the principal world reserves. The main suppliers in 1980 were the Republic of South Africa (43%), the USSR (21% ), the Philippines (12%), Albania (11 %), Turkey (8%), and others (5%). The strategic nature of chromite is obvious. End Uses-Grades and Specifications As noted before, the three principal uses for chromite are metallurgical, refractories, and chemical with a fourth minor use as foundry molding sand. For metallurgical applications chrome ore is first reduced in electric carbon arc furnaces to various types of ferrochromium alloys. There are high, medium, and low carbon ferrochromiums with carbon ranging from 0.01 up to 10%. Chromium itself ranges from 50 to 73 %. Ferrosilicon chromium and ferrochromium-silicon grades have chromium from 33 to 67% and silicon from 3 to about 48%. Since iron is reduced with chromium, the Cr:Fe ratio of the ore will determine the ultimate grade of the ferrochromium whereas carbon and silicon can be controlled during processing. MgO, A12O3, CaO, and excess SiO2, are removed in slag. A small amount of pure chromium metal is prepared by alumino-thermic and electrolytic processes from essentially iron-free chrome components that have been made via the chemical route. The higher grades of ferrochromium with chromium in the 66 to 73% range can only be made from ores with not only high chromium content, but low iron, i.e., high Cr:Fe ratio. These ores, conventionally termed metallurgical grade, have Cr2O3 contents of 45 to 56% with Cr: Fe ratios of 2.5 to 4.3. A standard composition is generally 48% Cr2O3 and 3:1 Cr:Fe ratio. Very high grade ores are often blended with lower grades even with the high iron chemical grade. For some ferrochromiums, additions of high alumina refractory grade are used as slag conditioners to facilitate smelting while still contributing chromium values. A lower grade ferrochromium, the high carbon charge chrome, has become the predominant grade in use today for making chromium-bearing steel alloys. This

Jan 1, 1983

By S. Shapiro, G. Krauss

RECENT investigations1 3 of the products of marten-sitic transformation in Fe-Ni and Fe-Ni-C alloys have made use of light microscopy to describe mar-tensitic fine structure. The application of conventional metallographic techniques to this problem was possible because of the similarity of distributions of parallel striations developed by etching polished surfaces to distributions of transformation twins which are positively identified in thin films by transmission electron microscopy. The surface striations frequently are not well-defined, and could also be due to, for example, rows of etch pits which are not resolved by the light microscope. This note describes the etching effects revealed by examination of surface replicas of mar-tensite in the electron microscope. The application of a replica technique both extends the observations of fine structure made with the light microscope and allows the results of conventional metallography to be used with more confidence. Samples of an Fe-33 wt pct Ni alloy were used for this study because of the detailed knowledge of the fine structure of martensite which has been developed'-4 for alloys of about this composition. Samples transformed to martensite at -120°C, and transformed samples heated to 340°C to effect a small amount of reversal of martensite to austenite, were examined. Surfaces were first prepared for replication by elec-tropolishing in a chromium oxide-acetic acid electrolyte at a current density of 0.1 amp per sq cm and a temperature of 15°C or a perchloric acid-acetic acid electrolyte at a current density of approximately 2 amps per sq cm and a temperature of 15°C. The polished surfaces were then etched for 4 to 7 sec by immersion in a solution of equal parts HC1, HNO,, and H20. Application of the etchant for this period of time produced discrete attack of certain features without loss of resolution due to overlapping of areas most susceptible to etching. The etched surfaces were replicated by 1) preshadowing with Pt-Pd alloy at an angle of 20 to 30 deg, 2) depositing a thin carbon film, and 3) stripping the film and shadowing material by immersion in a 5 pct nital solution. Two types of etching effects were observed by examination of the surface replicas in the electron microscope: l) continuous striations centered at the bottom of long grooves or the tops of pyramidal elevations on the sample surface, and 2) high densities of fine etch pits. Examples of both types of features are shown in Figs. 1 to 4. The striations are in each case continuous and have the same characteristic configurations as do transformation twins in martensite. Fig. 1 shows that the density of grooves decreases toward the edge of a martensite plate and Fig. 2 shows a region where the striations are of varying length. Similar examples of transformation twin arrangements determined by transmission electron microscopy of thinned foils of martensite have been shown in the literature,'~ and, based on these similarities, the striations and their associated grooves or mounds are considered to be evidence for the presence of transformation twins. The transf~rmation twins in martensite are on the order of l00 A thick, much too fine for resolution by the light microscope. It appears that orientation-dependent etching of the matrix martensite about the twins results in grooves or surface elevations which

Jan 1, 1967

By F. D. Rosi, C. A. Dube, B. H. Alexander

WHEN a deformed polpcrystalline metal is heated to a sufficiently high temperature, a recrystallized structure develops which consists of small, essentially stress-free grains. This transformation is referred to as primary recrystallization. Under certain conditions, on prolonged annealing of the specimens, a type of grain coarsening occurs in which a small number of grains commence to grow at various points by devouring the neighboring finegrained primary structure, which, in itself, exhibits a marked stability toward normal grain growth. This grain coarsening process has been referred to by Burgers' as "secondary recrystallization" or "exaggerated grain growth." Although much work has been done on recrystallization and growth processes, present knowledge of the factors which determine the occurrence and growth of secondary grains is inadequate for the advancement of a theory which accounts for the observed characteristics of this recrystallization phenomenon. In this respect, it would be important to make measurements of the velocity of growth of these large secondary grains. The early work of Feitnecht2 on aluminum showed that the size of secondary grains increased with temperature and time, suggesting that such measurements would be possible. More recently, Burgers1 found that the growth velocity of these grains in aluminum was constant over a large time interval, as is generally found for the growth velocity of primary grains in a uniformly deformed test piece.3-5 It is reasonable to expect that the determination of the activation energy of the secondary growth process might lead to a better understanding of the underlying atomic mechanism. This investigation, therefore, is one of a series primarily designed to measure the growth velocity of secondary grains at various temperatures for silver, copper, and aluminum. It is hoped that these studies along with those of orientation relationships, will establish a sound basis for theorizing as to the origin and nature of the secondary transformation. Experimental Procedure The metal used in the present investigation was high-purity silver (999.9 fine), which was supplied in the form of cold-rolled plates 0.250 in. thick. These plates were annealed at 500°C for 1 hr and then straight-rolled to a thickness of 0.04 in. in three reductions of approximately 45 pct, followed in each case by an anneal at 450°C for 1/2 hr. The 0.04 in. sheets were given a final reduction of approximately 50 pct, which resulted in a thickness of 0.02 in., thereby insuring two-dimensional crystal growth. Individual specimens of this material about 1x3 cm were used for all heat treatments, unless otherwise noted. The annealing was carried out under an atmosphere of argon in an Inconel tube furnace whose temperature was controlled to within -+2°C. Metallographic examination of the secondary transformation was accomplished by mechanically polishing the specimens on one side to approximately one half their thickness through 2/0 metallographic emery paper, and then electrolytically polishing in a solution of potassium ferrocyanide and sodium cyanide. With a current density of approximately 20 amp per sq dm, the time required to obtain a satisfactory surface varied from 3 to 5 min. Standard potassium bichromate was used to etch the electrolytically polished surfaces. A heavy etch with this solution produced a sharp contrast between the secondary grains and the fine-grained primary structure, darkening the latter while leaving the large secondary grains bright. All area measurements of the secondary crystals were made with a planimeter on enlarged tracings of the grains.

Jan 1, 1953

By F. H. Ellinger

TI HE crystal structure of neodymium has been re-A ported by Quill1 and by Klemm and Bommer"s to be hexagonal-close-packed, Strukturbericht-type A3, with a, = 3.650.4, c, = 5.890.4, c/a = 1.614. Klemm and Bommer,% owever, pointed out that the observed intensities of the lines of the neodymium powder pattern agreed only in part with the intensities calculated for the type A3 structure, and that the neodymium powder pattern showed extra lines which could not be traced to impurities. They found that these extra lines could be accounted for by doubling the c-axis, but apparently they did not consider their evidence to be sufficiently conclusive to justify reporting the doubled c-axis. In the present work, the structure of neodymium was found to be double hexagonal-close-packed. The neodymium metal used in the present investigation was obtained through the courtesy of F. H. Spedding of the Ames Laboratory. Its major impurity was stated to be 0.03 pct Ca. The author's spectrographic analysis indicated high purity and carbon was determined to be less than 30 ppm. X-ray powder specimens were prepared from filings stress relieved in vacuum at 200°C for 50 hr. Powder photographs were taken in an 114.6 mm diam camera (Straumanis film mounting) at room temperature and in a 19 cm diam Unicam high temperature camera at elevated temperatures. Copper x-radia-tion was used for all the photographs. The powder pattern of neodymium was found to index to a hexagonal unit cell with dimensions, as determined from the high angle Ka doublets, of: a.= 3.655+0.001.4; c, = 11.796+0.004.4; and c/a = 3.227 at room temperature. The measured density of neodymium shows that this cell contains 4 atoms, the calculated density is accordingly D, = 7.02 g per cu cm. The diffraction data for the first 15 lines of the powder pattern are listed in Table I. In a double hexagonal-close-packed unit cell, the 4 atoms would be in the positions (0,0,0), (0,0,%), (1/3, 2/3, 1/4), and (2/3,1/3,%) of space group P 6,/mmc. On the basis of these positions, the relative intensities of the reflections were calculated using the expression: 1+cos2 20 I oc \Frp 1 ' sin2 0 cos 0 where F is the structure factor and p is the multi- plicity factor. Since absorption was not taken into consideration, comparison of observed and calculated intensities should be made only for neighboring reflections. Each atom has 12 neighbors, 6 in the basal plane at a distance of 3.655.4 and 3 above and 3 below at the closer distance of 3.626.4. These distances correspond to an average radius of the neodymium atom of 1.820.4. The description of this structure in terms of A, B, and C close-packed layers of atoms is ABAC ABAC. ...... The structure repeats every fourth layer and the stacking sequence of the second, third, and fourth layers corresponds to cubic-close-packing of atoms. A series of powder photographs taken at successively increasing temperatures up to 680a10"C revealed that the double hexagonal-close-packed structure is stable up to this temperature. Acknowledgments The authw wishes to thank W. H. Zachariasen and A. S. Coffinberry for their helpful comments on this work and also Marion Gibbs for measuring the diffraction films. This work was sponsored by the United States Atomic Energy Commission.

Jan 1, 1956

By R. P. Aikman, F. G. Miller, J. M. Podgursky

As part of a larger study of the mechanism of froth flotation of coal, the rates at which coal particles of various size and specific gravity react to froth flotation were investigated. Results of this study show that in flotation: I) recovery rate increases, but selectivity decreases with a decrease in particle size down to 100 mesh, and 2) recovery rate is constant for all sizes between 100M and 325M. n response to the growing demand for low-sulfur coking coal for iron making, the coal industry is continually striving to perfect methods for cleaning coal to acceptable ash and sulfur levels while maintaining maximum product yield. By present standards the industry has adequate processes for cleaning coarse coal, i.e., + 28 mesh, at almost any desired specific gravity. However, in the case of fine coal, i.e., —28 mesh, neither of the two existing processes - froth flotation or hydrocycloning — in its present state of development yields products that are comparable in ash and/or sulfur content to products normally obtained from coarse coal processes. The work outlined in this paper is part of a larger study directed toward maximum exploitation of froth flotation for fine coal processing. The concepts and data presented are now serving as a basis for designing fine-coal circuits in which improved efficiency is obtained by optimum use of froth flotation with other fine-coal processing methods. The paper includes: 1) A discussion of the value of a detailed wash-ability study as a method of assessing the problems associated with fine coal processing, 2) A general discussion of hydrocyclone principles, included to serve as a basis for understanding the mechanism of coal flotation, and 3) A detailed discussion of the mechanism of coal flotation, as well as the research leading to the optimum use of froth flotation in combination with other fine-coal cleaning methods to provide efficient fine-coal processing. Our study of the rates at which coal particles of various size and specific gravity react to flotation shows that in flotation: 1) recovery rate increases but selectivity decreases with a decrease in particle size down to 100 mesh, 2) recovery rate is constant for all sizes between 100 mesh and 325 mesh, and 3) the flotation process effectively rejects only those extremely fine particles which do not contain surface carbon. (Because of this feature, froth flotation is an excellent method for rejecting clays - the only extreme fines in - 325-mesh coal that are always carbon free.) Washability studies of flotation products are used to assess flotation efficiency. These studies show that: 1) the increase in percent sulfur in flotation products above the theoretical sulfur content as defined by the washability study is due almost entirely to flotation of fine high-specific-gravity particles that are part coal and part pyrite, and 2) in a given size range particle floatability decreases with an increase in particle specific gravity. Error curves are explained and are used to compare the mechanisms of coal flotation and hydrocycloning. These comparisons show that hydrocyclone performance is affected primarily by particle mass, i.e., particle specific gravity and size, whereas coal flotation performance is dependent on both the particle mass and the coal surface available for bubble attachment. Since the error curve is a basic tool for rating the efficiency of any coal processing system, it will be useful to quickly review the principles of error curve construction. RATING COAL-PROCESSING EFFICIENCY BY THE ERROR CURVE The organic component of coal is of lower specific gravity than its impurities, and the most effective principle for coal concentration is therefore separation on the basis of specific gravity. However, since there is no sharp dividing line between pure coal and pure ash components, specific gravity must be closely controlled if the product is to have acceptable quality at maximum yields. In turn, the basis for close control in any coal processing system is the reference standard provided by precise laboratory washability studies. In these studies, coal is carefully separated into a series of progressively higher specific gravity fractions to establish a relationship

Jan 1, 1968

By W. C. Winegard, C. Feng, C. Elbaum

SEVERAL investigations have been made concerning the effect of oxygen on the mechanical properties of titanium 1-6= In particular, the yield strength has received considerable attention. Finlay and snyder2 report a 0.2 pet strain offset yield strength if 49 kg per sq mm in titanium containing 0.1 pct 0 and 61 kg per sq mm in titanium with 0.2 Pct 0. These results are in good agreement with those of Jaffee, Odgen, and Maykuth3 who report values of yield strength

Jan 1, 1960

Prior to any detailed discussion, I'd like to say that Dr. Aplan has made direct hits on two important considerations: 1) The most demanding need in Fine Coal research is to develop improved methods of sulfur reduction. 2) The areas of particle (impurity) liberation and froth flotation hold real near-term promise as techniques for improved sulfur removal. Digressing for a moment, I thin kwe can all remember the time when the biggest problem facing coal research was simply defined - "No money!" In the mid 70's we suddenly found ourselves dealing with a product worth five to seven times the value it carried in the mid60's. All of a sudden, we're talking about a high-profile, high- value commodity. The coal industry still hasn't made the complete psychological adjustment - especially in the operating areas (prep plants included). We have a valuable material at hand which is, in' many cases still being processed as though it were a two or three dollar per ton item. Simply put, I think that while the industry has made some major strides during this transition, a stronger commitment of attitude (and finances) needs to be made toward deeper definition of beneficiation work. Back to specifics - Dr. Aplan has really highlighted three areas where strong research efforts are needed. 1) Liberation processes - not limited to mechanical comminution - must be more fully studied.The industry certainly needs a better handle on value returned (improved ability to beneficiate) for dollars spent on improved liberation. 2) Flotation processes probably hold the most promise for near- term improvement in fine coal beneficiation technology. Dr. Aplan’s.

Jan 1, 1979

By G. A. Hellstrand

IN 1915, H. A. Guess, Vice President of American Smelting & Refining Co., in charge of its Mining Department, learned that the Anglo-New-foundland Development Co., Ltd., a pulpwood and paper-mill enterprise, had found upon its large concession in Newfoundland, and had opened up by shaft to the third level and some drifting, a lenticular orebody indicat-ing about 100,000 tons, as an extremely fine-grained sulfide ore, averaging about 0.05 oz. Au, 4 oz. Ag, 1.5 per cent Cu, 10 per cent Pb, 18 per cent Zn; and that having sent parcels of this ore to Minerals Separation, Ltd., and various other metallurgical testing concerns without obtaining any success in commercial separations thereon, had discontinued work thereon and let the workings fill. Mr. Guess wrote to the general manager of that company and obtained a few hundred pounds of the typical ore, which he sent to his company's metallurgical testing laboratory at Flat River, Mo., outlining various flotation tests desired thereon, in an endeavor to obtain separation into a commercial lead concentrate and a zinc concentrate. But the art of flotation had not then progressed far enough to treat such ore, the galena and zinc blende being so fine grained that grinding to about 300 mesh was required to release the mineral particles in their gangue. Mr. Guess had flotation and other tests continued upon this ore from time to time with whatever new reagents and flotation devices were evolved as time went on, and finally, in 1925, he succeeded in effecting in his company's testing plant, then at Wallace, Idaho, separations into lead concentrates and zinc concentrates of satisfactory commercial grade. Mr. Guess then proceeded to unwater, examine and sample the property and made with the owners a partnership operating agreement upon the mine itself and a considerable area surrounding it, and in the early summer of 1926 began to prospect for additional orebodies, utilizing for such prospecting geophysical methods, under the direction of Hans Lundberg, methods which up to that time had been little used in mining in the western hemisphere.. This geophysical work found two large flat-lying orebodies of a type precisely similar to the smaller body of the original discovery. The larger orebody, some 3500 ft. west of the original

Jan 1, 1934

By T. Sterry Hunt

THE deposit of rock-salt which is known to exist along the eastern shore of Lake Huron, in the province of Ontario, has lately been more completely explored than before, by a boring with a diamond drill, put down by Henry Attrill, Esq., of New York City, and the results obtained are so important in every way that I make no apology for presenting them to the Institute of Mining Engineers. I may be permitted to preface an account of this remarkable exploration, and of its results, with a historical sketch of the discovery and development of this salt-region. It was in December, 1865, that a boring was begun near the town of Goderich, in the hope of finding petroleum. In this the adventurers were disappointed, but, after passing through about 800 feet of limestone, they encountered a series of variegated marls, in which, at a, depth of 964 feet from the surface, a bed of rock-salt, 30 feet in thickness, was met with in May, 1866. The boring was carried to a depth of 1010 feet, ending in hard rock, and yielded, by pumping, a very pure saturated brine when examined by me in August of the same year. In the report of the Geological Survey of Canada for 1863-66, published early in 1867, I described this salt-well, with many geological details, and gave an analysis of the brine. In the next three years a considerable number of wells was sunk in and around Goderich, and numerous trials were made in various other parts of the region. Salt was found at Kincardine, thirty miles north-northeast from Goderich, at a depth of about 900 feet, and also at Clinton, thirteen miles southeast, at 1180 feet. Records of these wells, with analyses of the brine from them, were given by myself in a subsequent report of the Geological Survey, 1866-69, published in 1870 (pp. 211-244), together with accounts of various unsuccessful borings in the neighborhood, analyses of the brines from the various wells (including one analysis by Dr. Goessmann), with many details of the salt-manufacture at Goderich, at Syracuse, New York, and at Saginaw, Michigan. The geological character of the region was there discussed at length, and it was shown that the salt here occurs in the Onondaga or Salina formation, which

Jan 1, 1877

By B. B. Zavoico

After showing continued and very satisfactory progress until the close of 1931, the oil industry of the Soviet, Union experienced very great difficulties, and since 1932 has not only failed to complete its assigned quotas but has fallen farther and farther behind them, and in fact during 1932 and 1933 Russian production has been below production in 1931. In 1934 the total crude oil production of 169,200,000 bbl. exceeded that of the former peak year, 1931, when 156,100,000 bbl. were produced. The production during 1934 amounted to 78.65 per cent of the plan. The failure to complete the plan has been due to the inability of the oil trusts to develop new fields; the fields that have been producing since 1917 still account for between 75 to 80 per cent of total production. The failure of the Soviet Government to develop new fields has been due to unsatisfactory organization of the geological work, to the extremely slow drilling of wells and their exploitation, and to the very much delayed development of the few areas that have been discovered. The official overestimation of the proven reserves of the country has undoubtedly been an important factor in giving the Soviet industry too much confidence when actually such reserves have been small. The official Soviet estimate of proven reserves of Russia is now placed at 21,000,000,000, bbl., while in fact such reserves, if estimated on a conservative basis, do not exceed 4,200,000,000 bbl., as will be shown later in this review. The refinery branch of the industry also showed unsatisfactory results with a recovery of gasoline, both straight-run and cracked, of only some 16 per cent of the total runs to stills. In fact, the showing of the refineries has been so unsatisfactory that the exports of gasoline have been greatly curtailed from 1933 to 1934, dropping to 10,000,000 bbl. in 1934 from 12,230,000 bbl. in 1933. With the indicated increase in domestic demand, together with but slightly increased refining capacity, the volume of available gasoline for export probably will be reduced to about 6,000,000 bbl. during 1935. The geographic distribution of constructed refineries has been unsatisfactory and the crude oils from Baku had to be transported by tankers

Jan 1, 1935

By Rees D. Rawlings, C. W. A. Newey

The aging characteristics of an Fe-11 at. pct Mo alloy have been studied by means of light metallography together with density, Young&apos;s modulus, and hardness measurements. The results were consistent with the precipitation of a single intermetallic compound during aging; overaging was slow relative to that in other iron-based binary alloys. The solution treatment temperature had a small effect on the rate of hardening whereas deformation prior to aging had a marked effect on both the rate of hardening and the peak hardness. The density data indicate that the compound precipitated is Fe3MO2 and not the Laves phase Fe2Mo. Analysis of the modulus and density results gave values for the time exponent for precipitate growth of approximately 1.0 and 1.5 for the alloy aged with and without prior deformation, respectively. DETAILED studies of precipitation hardening in bcc matrices have been confined largely to the effects of carbides and nitrides. In view of this and the growing technological interest in intermetallic compound strengthening, e.g., in maraging steels, a study of precipitation in iron-based alloys with a low interstitial content has been undertaken. This paper is concerned with the aging behavior of an Fe-11 at. pct Mo alloy; the mechanical behavior of the alloy will be reported later. The early work of sykes on Fe-Mo alloys showed that precipitation of the intermetallic compound was accompanied by an increase in hardness and a decrease in volume of the material. More recent surveys of the strengthening associated with precipitation have been made3-5 and, in particular, Elsen and wassermann4 showed that deformation prior to aging increased the rate of hardening. These latter workers also followed the precipitation process by means of dilatometry, electrical resistivity, and lattice parameter measurements. Their results confirmed that there is a decrease in volume on aging. Except for the work of Hornbogen on an Fe-20 at. pct Mo alloy, neither clustering nor the precipitation of a nonequilibrium phase has been observed in Fe-Mo alloys. Studies of alloys of lower molybdenum content475 indicate that the equilibrium intermetallic compound is precipitated during aging. However, there is some doubt concerning the nature of the equilibrium precipitate phase. According to the phase diagram constructed by Hansen,8 the phase should be precipitated. This phase has a rhombohedra1 crystal structure which is characterized by the formula Fe706,&apos; although the composition of the molybdenum-rich boundary corresponds approximately to Fe3Mo2. The version of the diagram proposed by Sinha, Buckley, and Hume-Rother indicates that the A phase, a Laves phase Fe2Mo, should be precipitated. Their observation of a Laves phase supports the earlier findings of Bechtoldt and Vacher,13 although, in a recent study of the system by means of diffusion couples, Rawlings and Newey did not detect the phase. The work presented here describes the effect of solution-treatment temperature, aging temperature, and prior deformation on the aging characteristics of the alloy as revealed by light metallography together with hardness, density, and Young&apos;s modulus measurements. In addition the density data are used in an attempt to determine the compound precipitated during aging. EXPERIMENTAL PROCEDURE A 29-kg ingot of the alloy was cast at R.A.R.D.E., Fort Halstead, from deoxidized, Japanese electrolytic iron and sintered molybdenum. The ingot was homogenized for 6 hr at 1473°K and then worked, with intermediate anneals, into 6- and 16-mm-diam rods and 6-mm plate. Chemical analysis of the alloy gave, wt pct: Mo, 17.5 (11 at. pct); C, 0.003; Si, 0.002; S, 0.005; P, <0.002; and02, 0.0098. Solution treatments were carried out under a dynamic argon atmosphere in a vertical, "crusilite" element, furnace which had a facility for rapid quenching into iced water. Except for the study of the effect of solution treatment temperature, all specimens were solution-treated at 1573" * 2°K for 1 hr. Salt baths were used for the aging treatments. Specimens for hardness, density, and Young&apos;s modulus measurements were produced, after heat treatment, from the stock rod or bar using a precision silicon carbide slitting wheel. As described later, the quenching treatment produced local plastic strain in the stock material; consequently, care was taken to ensure that the specimens were not prepared from these regions. Those specimens used in the studies of the effects of prior deformation on the aging behavior were strained in compression in a Denison universal testing machine. Specimens for light metallographic observations were mechanically polished on successively finer grades of diamond paste down to and then etched in either alcoholic ferric chloride or in a 2 pct nital solution. Vickers diamond pyramid hardness data were obtained using a 30-kg load. At least five impressions were averaged for each determination. Density measurements were made using a displacement technique in which each specimen was weighed in air and in dibromoethane at 296°K. The specimens were cylindrical and weighed 3 to 4 g; all weighings were made on a balance reading to 1 x 10"5 g. For each specimen the mean value of five weighings was used to calculate the density. The density of the dibromoethane was determined using the displacement procedure and a standard nickel specimen. The error in an absolute density value was estimated to be HI.01 pct. To obtain the density as a function of aging time a single specimen was used and the density meas-

Jan 1, 1969

By Charles Kumke

THE "slot" system of mining in use at the Golden Queen mine, Mojave, Calif., does not involve any new mining methods. It is, how-ever, a, new combination and adaptation of several stoping systems in common practice. The first plans for stoping operations at the Golden Queen mine called for ordinary shrinkage stopes. The hanging wall of the vein, where exposed, is a very hard felsite with a dip varying from 50° to 70°. The vein itself is quartz, shattered and fractured enough to make it easy to drill and blast to a clean hanging wall. There is no well defined footwall. The footwall limits had to be determined by assays as the metal content faded out into the felsite. Two shrinkage stopes, each approximately 200 ft. long, were laid out and started on the 200-ft. level. One of these stopes, varying in width from 8 to 18 ft., was carried on up to the top limits of the ore, approxi-mately 120 ft., without a break in the operation. The shrinkage system proved entirely satisfactory and low costs resulted from-this operation. In the final drawing of this stope, two timbermen followed down on the ore, scaling the hanging wall clean of small fragments and placing an occasional long stull from foot to hanging wall where it was deemed necessary. Few such stulls; however, were required. The hanging wall stood up very well until the stope was entirely emptied of ore. Waste fill was then put into the stope by the glory-hole method, through a waste raise that had previously been run to surface from the middle of the stope. The second shrinkage stope ran into difficulties about 35 ft. above the sill floor. Up to this point the maximum width of the ore had been about 15 ft. The ore suddenly widened into the footwall to a distance of 40 ft. in the north end of the stope. In extending the stoping operations over this width, it was soon found that the vein material would not arch and support itself. Drilling in this end of the stope was then entirely too hazardous, and all operations were stopped. The ore was drawn through the chutes below as rapidly as possible and as soon as the stope was entirely

Jan 1, 1937

By Charles A. Kumke

The (&apos;slot" system of mining in use at the Golden Queen mine, Mojave, Calif., does not involve any new mining methods. It is, however, a new combination and adaptation of several stoping systems in common practice. The first plans for stoping operations at the Golden Queen mine called for ordinary shrinkage stopes. The hanging wall of the vein, where exposed, is a very hard felsite with a dip varying from 50° to 70°. The vein itself is quartz, shattered and fractured enough to make it easy to drill and blast to a clean hanging wall. There is no well defined footwall. The footwall limits had to be determined by assays as the metal content faded out into the felsite. Two shrinkage stopes, each approximately 200 ft. long, were laid out and started on the 200-ft. level. One of these stopes, varying in width from 8 to 18 ft., was carried on up to the top limits of the ore, approximately 120 ft., without a break in the operation. The shrinkage system proved entirely satisfactory and low costs resulted from this operation. In the final drawing of this stope, two timbermen followed down on the ore, scaling the hanging wall clean of small fragments and placing an occasional long stull from foot to hanging wall where it was deemed necessary. Few such stulls, however, were required. The hanging wall stood up very well until the stope was entirely emptied of ore. Waste fill was then put into the stope by the glory-hole method, through a waste raise that had previously been run to surface from the middle of the stope. The second shrinkage stope ran into difficulties about 35 ft. above the sill floor. Up to this point the maximum width of the ore had been about 15 ft. The ore suddenly widened into the footwall to a distance of 40 ft. in the north end of the stope. In extending the stoping operations over this, width, it was soon found that the vein material would not arch and support itself. Drilling in this end of the stope was then entirely too hazardous, and all operations were stopped. The ore was drawn through the chutes below as rapidly as possible and as soon as the stope was entirely

Jan 1, 1937

By H. W. Reid

One of the outstanding features of the year was a further marked decline in the footage drilled. This is estimated at 169,000 ft., as against 218,000 ft. for the previous year, and 372,500 ft. in 1930. Owing to repair work and improved production methods, there was an increase of about 4.25 per cent in the amount of oil won, the production being estimated at 10,160,000 bbl., or an increase of 400,000 bbl. over 1931 and nearly 750,000 bbl. more than in 1930. (See Table 1.) At the end of November there were 28 rigs in operation. During the first 11 months of the year 54 new wells were started; the average depth of those completed was 2476 feet. Owing to the continued restriction of drilling programs there has been little of outstanding interest in the way of new plant or technique. The use of the acid bottle, for testing the verticality of wells while drilling, has increased considerably, and this is now in use in practically every well except the very shallowest. During the last six months of the year fairly extensive use has been made of electrical coring. The number of wells started in the Colony up to the end of November, 1932, was 1894. The average number of producing wells during the year was 789, or 41.7 per cent of the total. Of these, 214 were flowing wells, 473 pumping, 80 bailing or swabbing, and 22 were produced by air or gas-lift. Although the last category represents less than 3 per cent of the total, there has been a marked increase in the use of air or gas-lift as compared with 1931. During the year there were 16 companies engaged in producing oil, as compared with 14 in the two previous years. In addition to one small refinery which started to operate at the beginning of the year, the five existing refineries worked continuously. At the latter very little has taken place in the way of extensions, except at one in the Parry Lands—Pitch Lake—Point Fortin area, where extensive alterations and additions are in progress, including the building of a deep-water pipe-line pier. When this is completed there will be five loading terminals, all situated in the sheltered Gulf of Paria, or west, coast, capable of accommodating ocean-going tank steamers. There

Jan 1, 1933

By Charles A. Kumke

THE "slot" system of mining in use at the Golden Queen mine, Mojave, Calif., does not involve any new mining methods. It is, however, a new combination and adaptation of several stoping systems in common practice. The first plans for stoping operations at the Golden Queen mine called for ordinary shrinkage stopes. The hanging wall of the vein, where exposed, is a very hard felsite with a dip varying from 50º to 70º. The vein itself is quartz, shattered and fractured enough to make it easy to drill and blast to a clean hanging wall. There is no well defined footwall. The footwall limits had to be determined by assays as the metal content faded out into the felsite. Two shrinkage stopes, each approximately 200 ft. long, were laid out and started on the 200-ft. level. One of these stopes, varying in width from 8 to 18 ft., was carried on up to the top limits of the ore, approximately 120 ft., without a break in the operation. The shrinkage system proved entirely satisfactory and low costs resulted from this operation. In the final drawing of this stope, two timbermen followed down on the ore, scaling the hanging wall clean of small fragments and placing an occasional long stull from foot to hanging wall where it was deemed necessary. Few such stulls, however, were required. The hanging wall stood up very well until the stope was entirely emptied of ore. Waste fill was then put into the stope by the glory-hole method, through a waste raise that had previously been run to surface from the middle of the stope. The second shrinkage stope ran into difficulties about 35 ft. above the sill floor. Up to this point the maximum width of the ore had been about 15 ft. The ore suddenly widened into the footwall to a distance of 40 ft. in the north end of the stope. In extending the stoping operations over this width, it was soon found that the vein material would not arch and support itself. Drilling in this end of the stope was then entirely too hazardous, and all operations were stopped. The ore was drawn through the chutes below as rapidly as possible and as soon as the stope was entirely

Jan 1, 1937

By D. Walton

The effect of small solute additions of Cu on the activation energies for creep A1 single crystals were determined over the range from 78° to 850° K. Below 240°K and above 800°K activation energies were unchanged. Between 240°K and 400°K strain aging causes the creep rate to become vanishingly small and the flow stress was independent of the temperature. Between 500° and 50°K the activation energy was increased to 41,000 cal per mole. NUMEROUS investigationsL have shown that solid solution alloying invariably increases the flow stress. A typical example is documented in Fig. 1. Such increases in flow stress can arise from two general effects: Alloying can increase the long-range stress fields through which dislocations must move by causing appropriate clustering; modification of dislocation densities, and so forth. Alloying can also modify the short-range stress fields that determine the activation energies for thermally stimulated migration of dislocations, such as occurs in some solute atom pinning processes, and so forth. Actually both long- and short-range stress-field effects can occur simultaneously. It was the purpose of this investigation to evaluate the effect of alloying on the short-range stress fields by determining the effect of alloying on the activation energies for creep. The resulting observations also shed some light on the effect of long-range stress fields on dislocation processes. EXPERIMENTAL TECHNIQUE Single-crystal bars (6 in. long 3/8 in. wide and l/4 in. thick) of dilute solutions of Cu in A1 were seeded, so as to provide extensive single slip, with the pole of the tensile axis located in the standard stereographic projection as shown in Fig. 2. Each crystal was grown under an argon atmosphere in a graphite mold containing a large reservoir of molten alloy for the purpose of obtaining rather uniform composition of Cu along the length of the bar. The nominal compositions of the alloys which were produced from 99.99 pct Cu and high-purity A1 containing 0.001 pct Fe and 0.001 pct Si, are given in Table I. Strains, measured by linear variable transformers attached by quartz rods to a 3 in. gage section were sensitive to and the stresses were ap- plied by direct loading of the specimen. Temperatures were determined by thermocouples attached to the gage section of the specimens. Below 400°K the apparent activation energies for creep, Q, were determined by the effect of small, rapid changes in temperature of about + 10°K from T1 to T2 on the corresponding creep rates ?1 and ?2 during primary creep according to where R is the gas constant.&apos; Above 400°K, Q was evaluated from Eq. [1] for the secondary creep rate using temperature changes of about ±20K. A typical set of results is shown in Fig. 3. RESULTS AND DISCUSSION The previously obtained effect of temperature on the apparent activation energy for creep of single crystals of high-purity A12 is shown by the broken curve of Fig. 4. The datum points on the same graph illustrate the effect of dilute a solid solution alloying with Cu on the activation energy between 600" and 750°K. Each plotted point is the average of not less than five independent test values between 600° and 750°K and not less than three at other tempera-

Jan 1, 1962