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By R. B. Schluter, M. M. Fine

Processes for manufacturing prereduced pellets have heretofore required temperatures of 2100°F or higher. Sulfides will accelerate the liquid-phase sintering of metallic iron, yet do not deter the reduction of iron oxides. The sulfides may be introduced as gases to the kiln atmosphere or as solids in the re-ductants. The net result is that well metallized iron pellets with good crushing strength can now be produced at a little over 1800°F. One of the most persistent topics at technical gatherings and in the recent scientific press has been the reduction of iron ore. In May 1960, a symposium on the subject was sponsored by the Electrochemical Society. The proceedings, comprising two dozen papers, were later published.' More recently, in November 1966, a similar gathering took place at Michigan Technological University, Houghton, Mich. The latest meeting was the International Congress on Production and Utilization of Reduced Materials at Evian, France, in May 1967. If the volume of literature, symposia and conferences is a measure of industry concern, then the current interest in reduction must be at a high level. Barrett,2 one of the early pioneers, stated some years ago that "The history of sponge iron has been so discouraging that many men in the iron and steel industry are violently opposed to giving it any further consideration." In spite of the "violent opposition" noted by Barrett, research people in and out of the industry continue to be attracted by the elusive prospect of uncovering a simple, viable means of direct reduction. Wild,3 one of the speakers at Evian, listed no less than 48 direct reduction processes (laboratory, pilot plant and commercial). Some of these were of historical interest only, but many others had resulted from developments within this decade. The previous big thrust into direct reduction occurred under the artificial impetus of a wartime economy (World War 11) and was largely an effort to provide more melting stock without coke ovens and blast furnaces. The present-day inquiry is proceeding at a more leisurely pace and the emphasis is different. For one thing, there is much less anxiety to circumvent the blast furnace. On the contrary, a whole new research endeavor has grown from the discovery that metallized burdens are exceptionally productive.4 Although the search for a melting stock

Jan 1, 1970

By S. A. Braley

DRAINAGE of acid mine water into surface streams of coal mining areas is one of the most serious problems of stream pollution, since there is no known method that completely prevents its forming and no economically feasible treatment after it has formed. The mine acid problem differs from other pollution hazards because acid production does not end with cessation of mining but actually becomes more evident when pumping is stopped. The acid problem in the Pennsylvania, Ohio, West Virginia, and Kentucky bituminous coal areas of the U. S. began with the first operation in 1761, and the volume of acid discharge today is largely the cumulative result of years of mining. Provided they lie above the drainage area, the oldest mines, now long abandoned, are almost without exception producing acid in the same manner as those now operating or recently abandoned. It is well to consider some of the many procedures that have been used to determine the composition

Jan 1, 1957

By Robert H. Richards

The extent to which sizing by sieves should be carried, as a preliminary to the separation, by jigging, of minerals of different specific gravities, has been a matter of controversy for many years. The subject has been investigated by several authorities, yet the ground does not seem to have been completely covered, nor are the questions involved entirely settled. For my present purpose I shall refer to but three investigators—Rittinger, Munroe, and Hoppe. In seeking additional light, I have gone over part of the old ground which has been considered satisfactorily settled; and since these preliminary tests have thrown light on some points, they have been included in this paper. In the investigations here described, I have confined myself, for several reasons, wholly to small sizes—grains of 0.1 inch in diameter and less. Rittinger's work was mainly done upon larger sizes, and there is much need among millmen of information concerning the smaller sizes. Moreover, these sizes brought the investigation within the means at my disposal. The laws that have been claimed as the laws of jigging by the several authorities are: 1. The law of equal-settling particles. 2. The lam of interstitial currents. 3. The law of acceleration. 4. The law of suction. The first of these has been considered by investigators, generally, to be the most important of all, and the larger part of the work of jigging is thought to be governed by it. But that it does not cover the whole of jigging is clear to all; and to account for the increased efficiency which we may call the extra jigging-catch, the other three laws have been advanced. The investigation described in this paper was undertaken to determine, as far as possible, to what extent each of the four laws con-

Jan 1, 1895

By Walter C. Smith, O. J. Seeds

METALLIC bismuth was known in the Middle Ages and the name is supposed to come from the German Wismut. The origin of the German name is uncertain. References to bismuth are found in the writings of Valentine, Paracelsus, and Agricola between 1450 and 1550. Early specimens of bismuth were very impure and often were confused with antimony, tin, and zinc. About the middle of the eighteenth century, J. H. Pott, C. J. Geoffroy, and Torbern Bergman succeeded in producing fairly pure bismuth and showed it to be an elementary metal similar in many respects to lead. H. S. Washington has estimated that bismuth occurs in the earth's crust about as abundantly as tungsten and silver; i.e., to the extent of 10-6 or 10-7 pct. It is found as native metal, both alone and associated with tin, copper, and other metals, and in a large variety of ores. The important ores are the sulfide (bismuthinite), the oxide (bismite), and the carbonates (bismutite and bismutosphaerite) . Other occurrences of bismuth are in the vanadate (pucherite), the selenide (guanajuatite), the telluride (tetradymite), and in many complex sulfides, arsenides, and antimonides. Bismuth minerals have been found in many parts of the world but very few of the bismuth deposits have been of economic value, the oxide ores from parts of China being the exception. The major portion of the bismuth production of today is the so-called by- product bismuth. Bismuth often occurs in ores mined and treated primarily for other metals, and during the treatment of these ores

Jan 1, 1953

By A. Martens

When I was honored with an invitation from the American Institute of Mining Engineers to present a paper at the Chicago meeting on the microstructure of iron, I hesitated about accepting, as the short interval that would remain at my disposal, after other pressing matters had received attention, could not but seriously affect the work of preparing such a paper. Unfortunately my fears have been realized and my work is neither completed, nor yet as comprehensive as I should desire. Mindful of my promise, however, and recognizing that 1 have reached a point where the results of my researches may prove suggestive, I am led to present them now, trusting that this brief explanation map secure indulgence for whatever deficiencies the paper may disclose. So far as my knowledge of published memoirs and treatises extends, microscopy cannot yet be said to possess a really firm foundation. In few cases only has any systematic development of the methods of investigation been undertaken, and broad gaps remain to be filled. It is not yet possible, therefore, to give a complete survey of the field, or, indeed, to supply a text-book on microscopic metallography. As Mr. F. Osmond, of Paris, a distinguished member of our profession, has undertaken to prepare for the Chicago meeting a historic review of the work actually accomplished I need not touch on that branch of the subject; but before entering upon my special theme, it may not be out of place for me to introduce certain explanations, as furnishing reasons for the course 1 have hitherto pursued, and to offer some suggestions for the further development of the methods of microscopic investigation. In microscopic metallography, the examination has to be conducted principally with incident light. Objectives of low power, in which the distance between the front lens and the abject is considerable, are adapted for directly incident light, and in such cases the relatively great depth of the image renders it possible to examine

Jan 1, 1894

By M. G. Corson

Until recently, the characteristics of cast copper have seldom been studied and such study as has been made has been inadequate. The prevailing idea seems to be that since pure copper is infrequently used in the cast stlate, there is no reason for trying to establish precise data regarding the properties of the metal in that condition. On the other hand, wrought copper either in the shape of sheets or wire rarely fails in service, except as a result of the action of reducing gases at the annealing temperatures, so there is little incentive to study the properties of the cast shapes —cakes, bars, ingots and billets—for the sake of tracing the causes of failures of the wrought metal to the cast stock. However, about a decade ago, wirebars of American origin often cracked badly while being hot-rolled in mills in Germany. This Icd to four investigations: by E. Seidl and E. Schieboldll by P. Siebe12 by 0. Bauer and G. Sachs,3 and by G. Welter.4 These authors came to the conclusion that failures in hot-rolling were due essentially to the presence of a wide zone of columnar crystals between t'he thin layer of fine crystal5 near the surfaces of the bars and the large but more nearly equiaxed grains of the central core. This macrostructural defect was explained in turn by the probable upward deviation in the temperature of the metal while it was being poured into the molds of the castling machine. More recently, cast shapes of copper were investigated by X. 1'. Allenh and by C. Blazey. Allen examined vertically cast wirebars and hori-zontally cast wedge cakes of electrolytic tough-pitch copper, but only for the distribution of densities; i.e., porosity. Blazey was interested mainly in the mechanism of the variations in electrical conductivity due to cold-work and anneal, but gave introductively an account of the composi-tion and average densities of the tough-pitch horizontally cast Wirebars used. As far as the present writer can tell, no investigation mas under-taken for the sake of presenting a picture of the distribution of mechanical characteristics in the wirebars of copper, or otherwise.

Jan 1, 1938

By M. G. Corson

Until recently, the characteristics of cast copper have seldom been studied and such study as has been made has been inadequate. The prevailing idea seems to be that since pure copper is infrequently used in the cast stlate, there is no reason for trying to establish precise data regarding the properties of the metal in that condition. On the other hand, wrought copper either in the shape of sheets or wire rarely fails in service, except as a result of the action of reducing gases at the annealing temperatures, so there is little incentive to study the properties of the cast shapes —cakes, bars, ingots and billets—for the sake of tracing the causes of failures of the wrought metal to the cast stock. However, about a decade ago, wirebars of American origin often cracked badly while being hot-rolled in mills in Germany. This Icd to four investigations: by E. Seidl and E. Schieboldll by P. Siebe12 by 0. Bauer and G. Sachs,3 and by G. Welter.4 These authors came to the conclusion that failures in hot-rolling were due essentially to the presence of a wide zone of columnar crystals between t'he thin layer of fine crystal5 near the surfaces of the bars and the large but more nearly equiaxed grains of the central core. This macrostructural defect was explained in turn by the probable upward deviation in the temperature of the metal while it was being poured into the molds of the castling machine. More recently, cast shapes of copper were investigated by X. 1'. Allenh and by C. Blazey. Allen examined vertically cast wirebars and hori-zontally cast wedge cakes of electrolytic tough-pitch copper, but only for the distribution of densities; i.e., porosity. Blazey was interested mainly in the mechanism of the variations in electrical conductivity due to cold-work and anneal, but gave introductively an account of the composi-tion and average densities of the tough-pitch horizontally cast Wirebars used. As far as the present writer can tell, no investigation mas under-taken for the sake of presenting a picture of the distribution of mechanical characteristics in the wirebars of copper, or otherwise.

Jan 1, 1938

By T. A. Rickard

The province of Otago consists, roughly speaking, of the southern half of the South Island* of New Zealand. On three sides it is washed by the Pacific Ocean and on the north it abuts against Westland and Canterbury. It covers an area of over 20,000 square miles, and for the most part has an extremely broken surface; the narrow plains of the sea-board are bounded by the rounded foothills which in turn are overlooked by range after range of the snowy summits whose varied beauty has made the island known as the Switzerland of the southern hemisphere. The gold-fields are confined to the quartzose schists which, in a broad band, 70 to 75 miles wide, cross the district, extending in a northwesterly direction from the shore of the western ocean into the northern provinces. These quartzose schists are the characteristic rocks of Otago, and to their curious structure are due the interesting differences exhibited by the mining districts in the modes of occurrence of the gold. These rocks, which are almost unbroken over their full extent, have been divided by the Provincial Geologist, F. W. Hutton, into two series of beds, named respectively the Wanaka and Kakanui formations. The only reason given for this division is the desire " to divide such an enormous thickness of rocks in order that the map might display somewhat of the geological structure of the district." As Hutton and others have pointed out, there is in fact no dividing line. The changes noticeable in the ascending series of schists are very gradual, and are due to the slowly decreasing effects of metamorphism. Hutton estimates the thickness of the Wanaka series at as much as 50,000 feet, and the

Jan 1, 1893

By Michel T. Halbouty

The area for which oil and gas developments in South Texas are reported for 1940 in this paper covers the same counties that were included in the reports for 1938 and 1939, with the addition of LaSalle County. LaSalle County is includcd in the Laredo district of South Texas, which totals seven counties for that district. The Corpus Christi district remains the same, with nine counties. The two districts together comprise what is known as the South Texas area for this report. Continued exploration along established trends and beyond proven field limits during 1940 provided South Texas with new fields and new producing levels at a rate of discovery fairly comparable with the high records set during recent years. The wells drilled in the counties within this district (including LaSalle) numbered 1656, approximately 8 per cent below the 1801 figure of last year. However, rank wildcats totaIed 336, an increase of 17.5 per cent compared to the 286 drilled in 1939. Therefore, since new field discoveries numbered 25 in 1940 against 29 in 1939, the rate of new field discoveries in 1940, based upon rank wildcats drilled, was I/I3.4 while that of 1939 was I/9.86, which shows a decrease of about 25 per cent in the rate of new fields. The rank wildcat tests in 1940 gave the following results: 18 produced oil, 4 produced distillate with gas, 3 produced. only gas, and 3r1 were dry holes (Table 5). Of the 1320 tests drilled in already proven fields or as extensions to pro+en areas (representing a decline of 12.8 per cent from last year's total of 1515 tests), 1048 produced oil or distillate, 60 produced gas and 212 were dry holes (Table 4). Of the producers, 50 found new sands or crude-in-distillate-sands in existing fields. Among the several fields subjected to extensive development were: Colorado, Jim Hogg County; East White Point, San Patricio and Nueces County; Rincon and Sun, Starr County; Glen, Webb and Zapata Counties; Wade City and Orange Grove, Jim Wells County; Stratton and South Clara Driscoll, Nueces County, and Aransas Pass, San Patricio and Aransas Counties. The development of important crude reserves on structures formerly considered primarily distillate fields has probably been the most important phase of the year's operations in South Texas. The Rincon, Stratton, Agua Dulce, Wade City, Odem and Robston fields provided the new crude sand discoveries. At some places crude production was opened by exploratory wells that found new sand horizons; in others by flank wells that found already discovered distillate sands sufficiently low to provide crude production. Rincon, Starr County, with its multiple sands, is now believed to be one of South Texas' largest crude-oil reserves. Offshore drilling showed important results during the year, including the discovery of two new submerged fields and the extension of the East White Point field into offshore Nueces County. The new marine fields are: East Flour Bluff) 76

Jan 1, 1941

By Michel T. Halbouty

The area for which oil and gas developments in South Texas are reported for 1940 in this paper covers the same counties that were included in the reports for 1938 and 1939, with the addition of LaSalle County. LaSalle County is includcd in the Laredo district of South Texas, which totals seven counties for that district. The Corpus Christi district remains the same, with nine counties. The two districts together comprise what is known as the South Texas area for this report. Continued exploration along established trends and beyond proven field limits during 1940 provided South Texas with new fields and new producing levels at a rate of discovery fairly comparable with the high records set during recent years. The wells drilled in the counties within this district (including LaSalle) numbered 1656, approximately 8 per cent below the 1801 figure of last year. However, rank wildcats totaIed 336, an increase of 17.5 per cent compared to the 286 drilled in 1939. Therefore, since new field discoveries numbered 25 in 1940 against 29 in 1939, the rate of new field discoveries in 1940, based upon rank wildcats drilled, was I/I3.4 while that of 1939 was I/9.86, which shows a decrease of about 25 per cent in the rate of new fields. The rank wildcat tests in 1940 gave the following results: 18 produced oil, 4 produced distillate with gas, 3 produced. only gas, and 3r1 were dry holes (Table 5). Of the 1320 tests drilled in already proven fields or as extensions to pro+en areas (representing a decline of 12.8 per cent from last year's total of 1515 tests), 1048 produced oil or distillate, 60 produced gas and 212 were dry holes (Table 4). Of the producers, 50 found new sands or crude-in-distillate-sands in existing fields. Among the several fields subjected to extensive development were: Colorado, Jim Hogg County; East White Point, San Patricio and Nueces County; Rincon and Sun, Starr County; Glen, Webb and Zapata Counties; Wade City and Orange Grove, Jim Wells County; Stratton and South Clara Driscoll, Nueces County, and Aransas Pass, San Patricio and Aransas Counties. The development of important crude reserves on structures formerly considered primarily distillate fields has probably been the most important phase of the year's operations in South Texas. The Rincon, Stratton, Agua Dulce, Wade City, Odem and Robston fields provided the new crude sand discoveries. At some places crude production was opened by exploratory wells that found new sand horizons; in others by flank wells that found already discovered distillate sands sufficiently low to provide crude production. Rincon, Starr County, with its multiple sands, is now believed to be one of South Texas' largest crude-oil reserves. Offshore drilling showed important results during the year, including the discovery of two new submerged fields and the extension of the East White Point field into offshore Nueces County. The new marine fields are: East Flour Bluff) 76

Jan 1, 1941

By N. A. Zeigler, T. D. Yensen

Aging is a term that connotes a slow change in properties under ordinary operating conditions. It can be accelerated by increasing the temperature and by mechanical straining. The magnetic properties of iron and some of its alloys have for many years been known to be subject to such a change. But the cause of the change was not recognized until a few years ago after mechanical age-hardening in non-ferrous alloys of the "duralumin" type had been definitely shown, by means of solid solubility curves, changes in electrical resistance and microanalysis, to be caused by slow precipitation of one or more constituents from the solid solution. The similarity between the solid solubility curves of such alloys (Fig. 1) and those for iron-nitrogen (Fig. 2) and iron-carbon alloys (Fig. 3) below the A1 transformation point suggested at once that magnetic aging of iron might be caused by a similar process; namely, by the slow precipitation of carbon and nitrogen in the form of Fe4N and Fe3C at ordinary temperatures because of a cooling rate that had been too rapid to permit complete precipitation according to equilibrium conditions. This suggestion has since been amply confirmed, particularly by the comprehensive work of Köster1 on the effect of nitrogen and carbon. Typical curves are shown in Fig. 4 for the relationship between aging temperature and coercive force. Previous to the establishment of the precipitation-hardening theory it was thought that the effect of nonmetallic elements like C, N, O, etc., on the magnetic properties of iron was greatest when these elements were retained in solid solution, atomically dispersed throughout the interstitial spaces of the iron lattice2. Based on the theory that magnetic properties are intimately connected with the regularity of the lattice, it now follows quite logically that a greater effect on this regularity may be obtained when the above impurities are precipitated as very fine particles of Fe3C, Fe4N, FeO, etc., more or less uniformly dispersed within the grains. But if this is the case, it follows also that there must exist a relationship between the size

Jan 1, 1935

By N. A. Zeigler, T. D. Yensen

Aging is a term that connotes a slow change in properties under ordinary operating conditions. It can be accelerated by increasing the temperature and by mechanical straining. The magnetic properties of iron and some of its alloys have for many years been known to be subject to such a change. But the cause of the change was not recognized until a few years ago after mechanical age-hardening in non-ferrous alloys of the "duralumin" type had been definitely shown, by means of solid solubility curves, changes in electrical resistance and microanalysis, to be caused by slow precipitation of one or more constituents from the solid solution. The similarity between the solid solubility curves of such alloys (Fig. 1) and those for iron-nitrogen (Fig. 2) and iron-carbon alloys (Fig. 3) below the A1 transformation point suggested at once that magnetic aging of iron might be caused by a similar process; namely, by the slow precipitation of carbon and nitrogen in the form of Fe4N and Fe3C at ordinary temperatures because of a cooling rate that had been too rapid to permit complete precipitation according to equilibrium conditions. This suggestion has since been amply confirmed, particularly by the comprehensive work of Köster1 on the effect of nitrogen and carbon. Typical curves are shown in Fig. 4 for the relationship between aging temperature and coercive force. Previous to the establishment of the precipitation-hardening theory it was thought that the effect of nonmetallic elements like C, N, O, etc., on the magnetic properties of iron was greatest when these elements were retained in solid solution, atomically dispersed throughout the interstitial spaces of the iron lattice2. Based on the theory that magnetic properties are intimately connected with the regularity of the lattice, it now follows quite logically that a greater effect on this regularity may be obtained when the above impurities are precipitated as very fine particles of Fe3C, Fe4N, FeO, etc., more or less uniformly dispersed within the grains. But if this is the case, it follows also that there must exist a relationship between the size

Jan 1, 1935

By K. M. Rolls, F. W. Reuter, J. Wulff

The superconducting behavior and microstructural characteristics of a nominal Nb-40 wt pct Ti-0.239 wt pct O alloy were studied as a function of ther mo -mechanical processing treatment. Critical current density us applied transverse magnetic field was obtained for 0.010-in.-diam wires at 4.2°Kin steady fields 14 to 110 kG. Both optical metallogvaphy and transmission electron microscopy were used to delineate the micros tructures of the same wires. It wan found that a 1-hr 500°C precipitation heat treatment after cold drawing to final size led to the highest critical current density. Heat treatment at 600°C also led to a high critical current density, but the precipitate differs in kind and form from that at 500°C. The resistire critical field was also found to be sensitive to precipitation heat treatment since the effective composition of the superconducting phase changes. This is discussed in terms of the oxygen in interstitial solid solution. Two types of high-field superconducting wire are at present used in the construction of high-field superconducting solenoids. These types are solid-solution alloy wire such as Nb-Zr and Nb-Ti and composites of the brittle inter metallic compound Nb3Sn. The latter generally have a high super cur rent-carry ing capacity which is difficult to vary if properly made. The supercur rent- carry ing capacity of the former can be varied drastically and often predictably by suitable thermomechanical processing treatments. In general, the critical current density Jc of the solid-solution type of alloy is increased by cold work and by additions of interstitial elements along with aging heat treatments. The imperfections which result are be-iieved to be responsible for the observed increase in Jc. In 1962 Kneip and coworkers1 found that the critical faurrent density of Nb-Zr alloys could be increased by proper heat treatment preceded and followed by cold work. Betterton and coworkers2 using a Nb-25 at. pct Zr alloy found that small additions of oxygen or carbon enhanced the effect of this heat treatment. They suggested that the interstitials present aided precipitation in the alloy, leading to a filamentary structure with superior properties. If the precipitation heat treatment was omitted, interstitial additions had a negligible effect on Jc. wong3 showed that higher heat-treatment temperatures lowered Jc. Walker and co-workers,4 who studied microstructure (by transmission electron microscopy) as well as superconductivity, found that the Jc anisotropy introduced by cold rolling was itself affected by heat treatment. They were unable to clarify the relation between microstructure and critical current density, although evidence of precipitation was indicated. More recent investigation of Nb-Zr alloys,5,6 besides showing that structural defects and fiber ing due to cold work and precipitation serve to raise Jc, also elucidate important optically observable microstructural changes which occur upon precipitation. In these reports, coarsening of the microstructural features was found to decrease Jc. Vetrano and Boom,7 who studied Ti-20.7 at. pct Nb, found that Jc was increased to a maximum by a 415°C, 3-hr heat treatment following quenching from 800°C and cold working. Heat treatments can also affect the resistive critical field Hr. Final-size heat treatments of Nb-Zr wire can lower Hr drastically if gross phase decomposition occurs5'* or moderately if the effects of cold work are eliminated without changing significantly the composition of the phase of interest.3,5,6,8 The percentage of oxygen which can be added to Nb-Zr alloys to enhance Jc is limited by the difficulty of subsequent cold drawing. Since Nb-Ti and Ta-Ti alloys in contrast can tolerate appreciably higher percentages of oxygen, it was decided to investigate the superconducting behavior of various alloys in these systems. The present paper describes the results of adding oxygen to a nominal 40 wt pct Nb alloy as a function of thermomechanical treatment. I) EXPERIMENTAL PROCEDURE A small alloy ingot was prepared from high-purity niobium, iodide, crystal-bar titanium, and Nb2O5 powder by arc melting on a water-cooled copper hearth in a gettered argon atmosphere. The ingot was turned and remelted fourteen times to insure homogeneity. After final melting and rapid cooling, it was machined round to 0.415 in. diam, jacketed in stainless steel, and cold-swaged to 0.117 in. diam. The jacket was removed and swaging continued to 0.051 in. diam followed by wire drawing in carbide dies to 0.010 in. diam. Although it was intended that about 1500 ppm O (by weight) be added, inert gas fusion analysis indicated a 2390 ppm 0 content, apparently due to additional oxygen pickup in the arc furnace. Even so, the alloy was sufficiently ductile to be cold-worked to greater than 99.9 pct reduction

Jan 1, 1967

By H. F. Haller

COLUMBIA-SOUTHERN'S Barberton limestone mine, 8 miles southwest of Akron, Ohio, is a million-ton-per-year producer from a depth of over 2200 ft in a district where other underground mining at this depth is unknown. Mining extracts 46 of the top 51 ft from a formation of Devonian limestone discovered by drilling in the 1890's. The same drilling revealed extensive salt deposits below the lime- stone, which led to the location of the chemical plant at Barberton as a division of the Pittsburgh Plate Glass Co. in 1899. Soda ash was the principal product of the plant, and as production increased the demand for limestone increased. Columbia's first attempt to secure a reliable all-weather source of stone was the development of a quarry at Zanesville, Ohio, in 1919. Zanesville production eliminated some of the stock- piling required by the use of Michigan stone, avail- able only during the lake shipping season. Stone from some Zanesville horizons, however, was found to be more suitable for cement production than for soda ash, and rail transportation remained an important factor. As demand continued to increase, plans were made to develop the Barberton deposit.

Jan 12, 1954

By P. Beardmore, B. W. Howlett, B. D. Lichter, M. B. Bever

The heats of formation at 273°K of the compounds Mg2Ge, Mg2sn, and Mg2b, the heats of fusion and melting points of Mg2Sn and Mg2Pb, and the heats of solution of magnesium, germanium, and lead in liquid tin have been measured. The excess free energies of the liquid alloys and the free energies of formation of magnesium-Group IVB compounds at their melting points and their standard free energies of formation at 298°K have been calculated. The stability and bonding of the compounds are discussed with reference to these properties. Some thermodynatnic aspects of the liquid phases in the systems Mg-Sn and Mg-Pb are also considered. THE compounds of magnesium with the Group TVB elements, silicon, germanium, tin, and lead, have often been considered to constitute a nearly ideal homologous series. In particular, their thermodynamic stability has been assumed to decrease with increasing atomic number of the Group IVB element.' The binary-phase diagrams of the magnesium-Group IVB elements given by Hansen and Anderko2 have the same form. Each system has a single con-gruently melting compound of limited homogeneity range. The structures of these compounds, which have the formula Mg2X, are anti-isomorphous with the calcium fluoride structure. A recent investigation has found evidence of a second compound in the system Mg-Pb.3 The solid compounds Mg2Si, Mg2Ge, and Mg,Sn are semiconductors, while the conductivity of Mg2Pb approaches that of a metallic conductor. This difference suggests that other properties may also show a discontinuity. The investigation reported here is concerned with the thermodynamic properties of magnesium-IVB compounds and particularly their variations with the period of the Group IVB element. The heats of formation at 273°K of the compounds MgzGe, Mg2Sn, and Mg2Pb and the heats of fusion and melting points of Mg2Sn and Mg2Pb have been measured. The results, combined with published data, are interpreted in relation to the stability and the bonding characteristics of the compounds. Some thermodynamic aspects of the liquid phases in the systems Mg-Sn and Mg-Pb are also considered. In the course of the investigation the heats of solution of magnesium, germanium, and lead in liquid tin have been determined. 1) EXPERIMENTAL PROCEDURES 1.1) Samples. Samples of the compounds Mg2Ge, Mg2Sn, and Mg2Pb, supplied by Professor P. Aigrain, Compagnie Générale de Télégraphie Sans Fils, were used in measuring heats of formation, heats of fusion, and melting points. Samples of Mg2Sn and Mg2Pb, supplied by Dr. V. B. Kurfman, Dow Metal Products Co., samples of Mg2Sn, prepared at the Air Force Cambridge Research Laboratories, and samples of MgzPb, prepared in this laboratory, were used for additional measurements of the heats of fusion and the melting points. The samples were stored in evacuated Pyrex capsules or under nonreacting liquids. 1.2) Heats of Formation. The heats of formation at 273°Kof the compounds Mg2Ge, Mg2Sn, and Mg,Pb were measured by tin-solution calorimetry. In this method, samples of the compound and of a mixture of the constituent elements are added alternately from 0°C to a tin-rich bath. The difference between the heat effects, corrected for the change in composition of the bath, is the heat of formation of the compound. Details of the method have been given elsewhere. 4 The bath was maintained at 350°C for the dissolution of the compounds MgzSn and Mg2Pb. Since at this temperature the dissolution of Mg2Ge was too slow, a bath temperature of 400" or 450°C was used with this compound. At least three calorimetric runs, each of approximately six additions, were made with each compound. 1.3) Heats of Solution. The determination of the heats of solution of magnesium, germanium, and lead in tin was included in this investigation because they were not well-established at the time this work was started. To obtain the heat of solution, the difference

Jan 1, 1967

By George A. Komadina

The Pima mine lies 20 miles southwest of Tucson, Ariz., and 45 miles north of the Mexican border. It is located on a hillside overlooking Tucson, which allows for gravity flow generally through the plant. In April 1965, an expansion was authorized by the mine's board of directors. This will triple the mine's output to 18,000 tpd. At this rate, it is estimated that there is sufficient ore to last 20 years.

Jan 6, 1965

By H. B. Probst

Mechanical twins were produced in zone-refined tungsten single crystals by explosive working at room temperature. These twins are parallel to (112) planes and have irregular boundaries rather than the classical plane twin boundaries. These boundaries aye grooved surfaces in which the grooves themselves are parallel to a <111> direction and the sides of the grooves appear to be par-allel to (110) planes. TWINS were produced in tungsten single crystals by explosive working at room temperature. These twins differ in character from any previously reported for tungsten; however, they are similar to those found in molybdenum after compression at -196°C.1 Deformation twins "resembling Neumann bands in ingot iron" have been observed in tungsten by Bech-told and Shewmon.2 This observation was made with sintered polycrystalline tungsten pulled in tension to fracture at 100°C and using a strain rate of 2.8 x 10-4 sec-1. More recently Schadler3 found deformation twins in zone-refined tungsten single crystals pulled in tension at -196"&apos; and -253°C. These tests were conducted using a strain rate of 3.3 x l0-4 sec-1, and the twin bands were found to be parallel to a (112) plane. Deformation twins in tungsten&apos;s sister metal, molybdenum, were observed by Cahn.4 These twins were produced by compressing small (0.7 mm) vapor-deproducedposited molybdenum single crystals at -183°C. The compression was performed &apos;by impact." By the use of precession X-ray techniques, Cahn was able to identify the twin plane as {112} and the shear direction as <1ll>. Mueller and Parker1 produced deformation twins in polycrystalline electron-beam-melted molybdenum by compression at -196°C. Their "loading rate" was 5000 psi per min which, judging from their stress-strain curve, corresponds to a strain rate of approximately 0.3 x 10-4 sec-1. These twin bands were found to be parallel to (1 12) planes; however, they differed in appearance from previously observed twins. In place of straight and parallel twin boundaries they were found to be irregular, jagged, and sawtoothed. The sides of the saw teeth were identified as (110) planes and irrational planes of a (111) zone. The twins observed in the present work in tungsten single crystals are similar in appearance to those of Mueller and Parker in polycrystalline molybdenum. The starting material used in this investigation was 3/16-in. diam commercial tungsten rod produced by powder-metallurgy techniques. This material was converted to a single crystal by the electron-bombardment floating-zone technique.= The process was carried out in a vacuum of 10-5 mm of Hg using a traversing speed of 4 mm per min. Segments (=2 in. long and 3/16 in. in diam) of two crystals (A and B) produced in this manner were studied. Crystal A received one zoning pass, while crystal B received two passes. The two crystals were explosively worked at Bat-telle Memorial Institute in the following manner. A 1/2-in.-thick layer of plastic was applied to the crystals to serve as a buffer in an attempt to prevent cracking. The composite, crystal and buffer, was then wrapped with 1/8-in.-thick DuPont sheet explosive EL506A2 and detonated in water at room temperature. Metallographic samples of the worked crystals were prepared, and back-reflection Laue X-ray patterns were obtained using unfiltered molybdenum radiation. RESULTS AND DISCUSSION Blasting the crystals as described above failed to prevent cracking. The crystals fractured into several fragments about 3/16 to 1/2 in. long; however, the fragments were of sufficient size to be useful for the subsequent study. The diamond pyramid hardness of the crystals after blasting was in the range 430 to 450 as compared with 340 for the as-melted material, which shows a definite hardening resulting from plastic deformation. These hardness values were obtained using a 1000-g load and taking readings only in sound portions of the crystals free of cracks. The crystals exhibited profuse twinning as shown in Fig. 1. No such structure is present in the as-melted condition. Most of these twins have jagged twin boundaries and are similar in appearance to those found in molybdenum by Mueller and Parker. The twins in both crystals were found to be parallel to {112} planes. This identification was made by using the conventional two-trace method. Subsequent efforts to describe these twins more fully were carried out on crystal A. If the longitudinal axis of crystal A is placed in the (001)-(011)-(Il l) basic triangle of the standard cubic stereographic projection, as in Fig. 2, then the two sets of twins shown in Fig. 1 are parallel to the (112) and (121) planes. Fig. 3 shows a schematic representation of a twin with jagged boundaries. This type of twin with a <111>

Jan 1, 1962

By T. H. Ramsey, Richard Shield

A process has been developed for fabricating thin-film resistors that are compatible with integrated circuits. Films are produced by evaporation of single refractory metals using an electron beam heating source. Resistor paths are then made using standard photoresist etching techniques. A low-temperature coefficient of resistance is obtained by control of nucleation during deposition of the film. One application of the process has been the development of a discrete resistor used for current setting in linear integrated circuits. Multiple thin-film resistors were formed on oxidized silicon substrates using molybdenum metal as a source. An evaporated protective layer of SiO2 over the resistor prevents resistance changes which might occur during subsequent high-temperature processing. Properties of a typical resistor are as follows: R = 15.7 ohm per sq, tolerance surface dimensions = 0.028 by 0.028 in., stable after 4000 hr at 0. 75 w without heat sink. THIN-FILM resistors have been investigated for many years with a large selection of usable resistors resulting from a wide variety of materials. Many of the processes necessitate a high degree of complexity but in nearly all cases the conclusions have been that the materials used in each case were acceptable provided the deposition process was reproducible and could be controlled sufficiently to give the required tolerances. It is our opinion that simplicity is still the key to thin-film resistor fabrication. In this regard, the single metal is obviously the simplest process to control, provided all the necessary properties can be obtained. The idea is not original in this laboratory by any means. Others have taken this approach.&apos; It has been demonstrated that a fairly wide range of resistivities can be obtained by careful control of deposition parameters for any given metal, and by selection of several single metals a very broad range of stable resistors can be obtained. The transition from one metal to the next is made when a film becomes too thin for adequate process control or long-term stability. A great deal of emphasis is once again being placed on the thin-film resistor. Although they have been thoroughly studied in the past, new applications have been found that require the properties obtainable only from thin-film resistors. Integrated circuits, in general, are advancing toward higher speeds and radiation environments which require replacement of the present diffused resistors. Linear circuits in particular are requiring high-power, high-precision resistors for the more advanced applications. The particular requirements of some linear circuits are such that a discrete resistor is required. The resistor described in this paper was developed as a 15.7-ohm precision discrete resistor for use in a current regulating circuit requiring a +2 pct end of life overall tolerance, a dissipation of 750 mw, and the ability to operate over a fairly broad temperature range (i.e., a low temperature coefficient of resistance, TCR). State-of-the-art integrated circuit and silicon processing technology lends itself well to the fabrication of thin-film resistors. Not only is the resistor thin film well-suited to integration on individual circuits, but the oxidized silicon surface provides one of

Jan 1, 1969

By Glenn S. Wyman

CHUQUICAMATA, located in northern Chile in the Province of Antofagasta, is on the western slope of the Andes at an elevation of 9500 ft. Because of its position on the eastern edge of the Atacama Desert, the climate is extremely arid with practically no precipitation, either rain or snow. All primary blasting in the open-pit mine at Chuquicamata is done by the churn drill, blasthole method. Since 1915, when the first tonnages of importance were removed from the open pit, there have been many changes in the blasting practice, but no clear-cut rules of method and procedure have been devised for application to the mine as a whole. One general fact stands out: both the ore and waste rock at Chuquicamata are difficult to break satisfactorily for the most efficient operation of power shovels. Numerous experiments have been made in an effort to improve the breakage and thereby increase the shovel efficiency. Holes of different diameter have been drilled, the length of toe and spacing of holes have been varied, and several types of explosives have been used. Early blasting was done by the tunnel method. The banks were high, generally 30 m, requiring the use of large charges of black powder, detonated by electric blasting caps. Large tonnages were broken at comparatively low cost, but the method left such a large proportion of oversize material for secondary blasting that satisfactory shovel operation was practically impossible. Railroad-type steam and electric shovels then in service proved unequal to the task of efficiently handling the large proportion of oversize material produced. The clean-up of high banks proved to be dangerous and expensive as large quantities of explosive were consumed in dressing these banks, and from time to time the shovels were damaged by rock slides. As early as 1923 the high benches were divided, and a standard height of 12 m was selected for the development of new benches. The recently acquired Bucyrus-Erie 550-B shovel, with its greater radius of operation compared to the Bucyrus-Erie 320-B formerly used for bench development, allowed the bench height to be increased to 16 m. Churn drill, blasthole shooting proved to be successful, and tunnel blasts were limited to certain locations where development existed or natural ground conditions made the method more attractive than the use of churn drill holes. Liquid oxygen explosive and black powder were used along with dynamite of various grades in blast-hole loading up to early 1937. Liquid oxygen and black powder were discontinued because they were more difficult to handle due to their sensitivity to fire or sparks in the extremely dry climate. At present ammonium nitrate dynamite is favored because of its superior handling qualities and its adaptability to the dry condition found in 90 pct of the mine. In wet holes, which are found only in the lowest bench of the pit and account for the remaining 10 pct of the ground to be broken, Nitramon in 8x24-in. cans, or ammonium nitrate dynamite packed in 8x24-in. paper cartridges, is being used. This latter explosive, which is protected by a special antiwetting agent that makes the cartridges resistant to water for about 24 hr, currently is considered the best available for the work and is preferred over Nitramon. Early churn drill hole shots detonated by electric blasting caps, one in each hole, gave trouble because of misfires caused by the improper balance of resistance in the electrical circuits. Primarily, it was of vital importance to effect an absolute balance of resistance in these circuits, the undertaking and completion of which invariably caused delays in the shooting schedule. Misfires resulting from the improper balance of electrical circuits, or from any other cause, were extremely hazardous, since holes had to be unloaded or fired by the insertion of another detonator. The advent of cordeau, later followed by primacord, corrected this particular difficulty and therefore reduced the possibility of missed holes. After much experimentation, the blasting practice evolved into single row, multihole shots, with the holes spaced 4.5 to 5 m center to center in a row 7.5 to 8 m back from the toe. Sucti shots were fired from either end by electric blasting caps attached to the main trunk lines of cordeau or primacord. The detonating speed of cordeau or primacord gave the practical effect of firing all holes instantaneously. Double row and multirow blasts, fired instantaneously with cordeau or primacord, proved to be unsatisfactory in the type of rock found at Chuquica-

Jan 1, 1953

By Glenn S. Wyman

CHUQUICAMATA, located in northern Chile in the Province of Antofagasta, is on the western slope of the Andes at an elevation of 9500 ft. Because of its position on the eastern edge of the Atacama Desert, the climate is extremely arid with practically no precipitation, either rain or snow. All primary blasting in the open-pit mine at Chuquicamata is done by the churn drill, blasthole method. Since 1915, when the first tonnages of importance were removed from the open pit, there have been many changes in the blasting practice, but no clear-cut rules of method and procedure have been devised for application to the mine as a whole. One general fact stands out: both the ore and waste rock at Chuquicamata are difficult to break satisfactorily for the most efficient operation of power shovels. Numerous experiments have been made in an effort to improve the breakage and thereby increase the shovel efficiency. Holes of different diameter have been drilled, the length of toe and spacing of holes have been varied, and several types of explosives have been used. Early blasting was done by the tunnel method. The banks were high, generally 30 m, requiring the use of large charges of black powder, detonated by electric blasting caps. Large tonnages were broken at comparatively low cost, but the method left such a large proportion of oversize material for secondary blasting that satisfactory shovel operation was practically impossible. Railroad-type steam and electric shovels then in service proved unequal to the task of efficiently handling the large proportion of oversize material produced. The clean-up of high banks proved to be dangerous and expensive as large quantities of explosive were consumed in dressing these banks, and from time to time the shovels were damaged by rock slides. As early as 1923 the high benches were divided, and a standard height of 12 m was selected for the development of new benches. The recently acquired Bucyrus-Erie 550-B shovel, with its greater radius of operation compared to the Bucyrus-Erie 320-B formerly used for bench development, allowed the bench height to be increased to 16 m. Churn drill, blasthole shooting proved to be successful, and tunnel blasts were limited to certain locations where development existed or natural ground conditions made the method more attractive than the use of churn drill holes. Liquid oxygen explosive and black powder were used along with dynamite of various grades in blast-hole loading up to early 1937. Liquid oxygen and black powder were discontinued because they were more difficult to handle due to their sensitivity to fire or sparks in the extremely dry climate. At present ammonium nitrate dynamite is favored because of its superior handling qualities and its adaptability to the dry condition found in 90 pct of the mine. In wet holes, which are found only in the lowest bench of the pit and account for the remaining 10 pct of the ground to be broken, Nitramon in 8x24-in. cans, or ammonium nitrate dynamite packed in 8x24-in. paper cartridges, is being used. This latter explosive, which is protected by a special antiwetting agent that makes the cartridges resistant to water for about 24 hr, currently is considered the best available for the work and is preferred over Nitramon. Early churn drill hole shots detonated by electric blasting caps, one in each hole, gave trouble because of misfires caused by the improper balance of resistance in the electrical circuits. Primarily, it was of vital importance to effect an absolute balance of resistance in these circuits, the undertaking and completion of which invariably caused delays in the shooting schedule. Misfires resulting from the improper balance of electrical circuits, or from any other cause, were extremely hazardous, since holes had to be unloaded or fired by the insertion of another detonator. The advent of cordeau, later followed by primacord, corrected this particular difficulty and therefore reduced the possibility of missed holes. After much experimentation, the blasting practice evolved into single row, multihole shots, with the holes spaced 4.5 to 5 m center to center in a row 7.5 to 8 m back from the toe. Sucti shots were fired from either end by electric blasting caps attached to the main trunk lines of cordeau or primacord. The detonating speed of cordeau or primacord gave the practical effect of firing all holes instantaneously. Double row and multirow blasts, fired instantaneously with cordeau or primacord, proved to be unsatisfactory in the type of rock found at Chuquica-

Jan 1, 1953