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By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.' Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-' and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964

By GEO H. DEIKE

NOT much activity has been evident during the past year in the establishment of co-operative scholarships but the interest among the coal-mining companies is more pronounced than ever. This is apparent from the replies received to a letter sent out by the Committee on the Promotion of Student Interest in Coal Mining to over 120 coalmine operating officials. With that letter was forwarded a bulletin issued by the school of mineral industries of The Pennsylvania State College entitled ?Industrial Scholarships ? a Partnership of Industry and Education.? In that circular was outlined the need for trained men in the war and postwar world, and particularly as such demands pertain to the growth of the mineral industries.

Jan 1, 1943

By Philip E. LaMoreaux

Fluoride, generally less than 0.5 ppm, is present in ground water from rocks of Paleozoic age and older, in northern and eastern Alabama. Some of the water-bearing formations in the Coastal Plain area of the State yield water with as much as 6.8 ppm fluoride.

Jan 8, 1950

By Arthur Knapp

The petroleum industry is confronted with the problem of conservalion. This is not a simple problem in view of a wide difference of opinion among authorities as to whether conservation is necessary and the specific direction that it should take. Many writers accuse the petroleum industry of wasting the natural resources of the country. Others link the consuming public with the industry in this waste. Let us define our terms; agree, if possible, on where and when waste occurs in connection with either the recovery or use of petroleum and select such plans for conservation as appear most practical. A plan for conserv3tion which appears to be logical today may not meet the problem tomorrow. The conservation of petroleum is closely linked with the advancement of marly arts and sciences and as these advance, the plan of conservation has to change. The need for conservation does not necessarily rest upon the elimination of waste. There is not necessarily a fixed connection between waste and conservation. Conservation may be necessary or desirable although there is no waste. Definitions Waste: Useless or unnecessary expenditure. Conservation: The preservation of the natural resources for economical use. Both definitions contain adjectives the interpretation of which is extremely difficult. It is the determination of what expenditures are "unnecessary" or what uses are "economical" that will require study and agreement. If one lets his automobile engine run in cold weather in order to keep it hot, it is difficult to measure that necessity. If an automobile is driven two blocks, when the driver is physically capable of walking, what is the measure of necessity. This question is in the realm of one of the oldest of sociological problems, "What is a luxury?"—a problem which has not been solved. The history of society indicates that the measure of a man's wealth has been the measure of necessity. What he can afford to buy without stinting himself in some other direction, is not a luxury to him and, if it fulfills his desires, may be considered his necessity.

Jan 1, 1927

Jan 1, 1879

By D. F. Coolbaugh

Successful mine exploration requires sound planning and modern exploration techniques, but it also requires perseverance and the right timing. The La Caridad mineral area has been known for over 70 years, but as with many mines, it was not "discovered" until viewed under new economic conditions and exploration philosophies. Present exploration of the La Caridad area began in 1964 and was carried out under a joint Mexican Government-United Nations Project. Detailed exploration was begun by Asarco Mexicana S.A. in late 1968. The geology of the La Caridad deposits conforms, generally, to the "porphyry copper" deposits of Arizona. However, breccias and pegmatites play a very important part in the emplacement of mineralization.

Jan 1, 1972

By E. Parthe, J. P. Pemsler

TWO references can be found in the literature concerning the ternary system uranium-tantalum -carbon. C. H. Schramm, P. Gordon, and A. R. Kaufmam reported in this Journal1 on the existence of the ternary carbide "UTa10C4." They also report a second face-centered-cubic carbide phase in the system U-Ta-C, which they denote as "white" phase. The publication includes a reproduction of a Debye-Scherrer powder photograph of "UTa10C4" and a list of the sin2 0 values of this compound. H. Nowotny, R. Kieffer, F. Benesovsky, and E. Laube2 report the complete solid solubility between TaC and UC with a B1 structure. Since the ternary phase "UTa10C4" lies very close to the binary system Ta-C, and the established phase Ta2C with a C27 structure had not been mentioned by Schramm et al., it was thought worthwhile to compare the patterns of "UTa10C4" with Ta2C. The strong lines of the given pattern were indexed on a hexagonal unit cell with the approximate cell parameters a = 3.09A and c = 4.93A. These are the values reported for Ta2C in the literature.3 The correspondence between reported and calculated sin2 8 values may be studied in columns 4 and 5 of Table I. The agreement is fair, but there remain weak lines which cannot be assigned to the hexagonal unit cell. The extinctions correspond to those of Ta2C, but a comparison of the calculated and observed intensities of the Ta2C lines (columns 2 and 3) with those of the corresponding lines of "UTa10C4" (column 6) show occasional deviations. To clarify this situation, four new samples were prepared. The compositions of these samples were chosen in such a way as to observe any existing ternary phase in the system TaC-UC-U-Ta. The samples were arc melted in an inert atmosphere and annealed at 1100°C for 36 to 72 hr. Compositions of the samples determined by chemical analysis are given along with the results of X-ray investigations in Table 11. The following conclusions may be drawn from these data: a) No ternary compounds occur in the section TaC-UC-U-Ta of the ternary system Ta-U-C. The "white" phase reported by Schramm et al. corresponds to a solid solution between TaC and UC. Only one three-phase field exists: C27-B1-A2. (Both tantalum and ? uranium have body-centered-cubic A2 structures.) The a uranium observed in sample 4 transformed from the high-temperature ? phase on cooling. b) The phase Ta2C with a C27 structure extends into the ternary system. "UTa10C4" is, therefore, a uranium-enriched Ta2C. Good agreement is ob-

Jan 1, 1960

By GEORGE A. KIERSCH

The awesome destructive power of known and projected weapons of war presages a new need for geologists and engineers, who may be called upon to locate vital industry underground, thereby protecting it from sky-borne destruction. The Corps of Engineers is now conducting special tests to establish design standards covering the general field of underground installations as well as surveys a of construction methods and the operational hazards connected with such plants. National planning must dictate a policy that is either tactical, where surface manufactured parts; are stored underground and during art emergency assembled, or operational with both the manufacturing and assemblage completed in subsurface plants. Both plans of operation require the use of subterranean plants. Relocation of vital plants underground will probably involve only a small percentage of the production capacity of this nation. The cost of rebuilding in new location will obviously limit its adoption

Jan 1, 1949

THE members arrived at Ticonderoga, N. Y., at noon, Tuesday, October 15th, and were received by Mr. Cyrus Butler, Chairman of the Local Committee of Arrangements. During the afternoon the works of the American Graphite Company and the Horicon Iron Company were visited under the guidance of Mr. Butler, President of both companies, and of Mr. William Hooper, Superintendent. An excursion was then made, in carriages, to old Fort Ticonderoga, on Lake Champlain, after which the party were driven to the Rogers Rock Hotel, on Lake George. The first session of the Institute was held in the parlor of time hotel on Tuesday evening. Mr. Eckley B. Coxe, President of the Institute, opened the proceedings with the following address: I shall ask your attention, this evening, to a few reflections upon the subject of mining engineering as a profession in the United States, its past, its present, and its future, and its duties and oppor¬tunities with reference to the proper development of our great min¬eral resources. Thirty years ago, there were scarcely any mining engineers in this country, and but few in England, and there were no institutions where young men could be educated for the profession in the Eng¬lish language. France and Germany have been able for about a century to boast of mining schools of a high character, that number among their graduates such men as Humboldt, Weisbach, Rittinger, Combes, and Gruner. Of the few we then had worthy of the name of "mining engi¬neer," some had studied in the continental academies, and others were graduates in the school of practical experience, and had learned their profession in mines and smelting-works. Their work con¬sisted principally in making surveys and maps of mines and mining properties, geological reports, and analyses of ores ; but the mining engineer whom we often meet with now, who has studied chemistry, physics, mineralogy, geology, mechanics, and drawing; who is more or less familiar with machinery and its construction, and with the practical management of mines or smelting-works, and who is an expert in some one branch of his profession, would have been very difficult if not impossible to find in the United States. The induce¬ments held out to ambitious and talented young men to enter the

Jan 1, 1879

By R. W. Fountain, J. Chipman

THE solubility of nitrogen in iron and steel has been of considerable interest due to the role of nitrogen in strain-aging and in quench-aging. It is generally considered that quench-aging is the result of precipitation of carbide and nitride particles from supersaturated solid solution, while strain-aging results from the segregation of carbon and nitrogen atoms to dislocations.1-9 The rate of strain-aging is controlled primarily by the amount of carbon and nitrogen in solution and the temperature. In experiments on strain-aging of pure iron with only carbon or nitrogen as impurities, Fast" has shown that even after 40 hr at 50°C carbon did not give any strain-aging while

Jan 1, 1959

By Edward Wisser

THE Pachuca silver district, situated about 100 kilometers northeast of Mexico City (Fig. 1), covers roughly the southeastern half of the Sierra de Pachuca. The latter is a mountain range with northwest trend, and forms a part of the northeastern rim of the topographic basin known FIG. 1.-LOCATION OF PACHUCA DISTRICT AND OTHER MINING CAMPS. as the Valley of Mexico. The length of the Sierra proper is about 50 km., its greatest width about 9 km., and it rises to a maximum of 600 meters above the general level of the basin floor. The Pachuca district consists of two contiguous subdistricts, the Pachuca area and the Real del Monte area. The center of the Real del

Jan 1, 1936

By Wm. Terry Siemers, Frank E. Kottlowski, George S. Austin

The value of industrial rocks and minerals produced in New Mexico in 1978 exceeded $227 million. The state ranked first in the nation in production of potash and perlite and was a leader in pumice production. Other commodities with sizable production in New Mexico include barite, caliche, clay, dimension stone, fuorspar, gypsum, humate, limestone, mica, salt, sand and gravel, scoria, and silica sand. Non-metallic resources are distributed throughout the state, but development and exploitation is concentrated in western and southeastern New Mexico. The value of industrial rocks and minerals within the state grew about 9% to more than $227 million in 1978. Continued growth, however, depends on continued demand, exploration, and development.

Jan 1, 1982

By Reed S. C. Rogers, Robin P. Gardner, Kuruvilla Verghese

The development and use of short-lived radioactive tracer methods for the onstream determination of residence time distributions in large-scale ball mills is described. Tests are reported on a pilot-plant ball mill with 0.43 m diameter and 0.86 m length and on an industrial mill with 1.83 m diameter and 2.74 m length. Tests with different tracer feed sizes indicate that the residence time distributions on both mills are independent of charge particle size. Similar tests are planned for a large ball mill of 4.57 m diameter and 9.30 m length. No safety problems were encountered in these tests and none are anticipated in tests of the larger mill.

Jan 1, 1981

By George F. Beardsley

The silver-fields of Zeehan and Dundas are located on the "West Coast" of Tasmania, 30 miles from the port of Strahan on the Macquarie Harbor. This harbor is 17 miles long, from 4 to 5 miles wide, and completely landlocked. Its only drawback is a shallow bar with 9 feet of water on it. The hills on the western side of the harbor vary from 200 to 300 feet in height, and are all composed of quartzite or a quartz grit. From 15 to 20 miles back from the eastern shore of the harbor is a conglomerate-capped range of mountains, rising to the height of 4700 feet. The immediate eastern

Jan 1, 1893

By Horace V. Winchell

The St. Helens mining-district, indicated in sketch-map, Fig. 1, is chiefly in Townships 9 and 10 North, Ranges 5 and 6 East of the Willamette meridian, in Skamania county, Wash. There is no railroad or even a wagon-road at present connecting it with any base of supplies; access is usually by wagon-road for about 50 miles from the town of Castle Rock to Spirit lake, and from that point by pony-trail from 6 to 10 miles farther. History. Nearly 20 years ago two German farmers, totally inexperienced in prospecting, penetrated this region upon a hunting-and fishing-trip. Their attention was drawn to numerous joints and crevices filled with black, glistening tourmaline, and con-

Jan 1, 1913

By J. E. Ryan

TRONA, Calif., is a miniature urban community of some 3500 people, located on the northwest shore of dry Searles Lake in the extreme northwest corner of San Bernardino County, approximately 186 miles north and east of Los Angeles. Since it is situated on the Mojave Desert, a typically desert climate prevails with wide variations in temperature between day and night, extreme daytime summer heat, and cool to cold winters. Rainfall averages somewhat less than 4 in. per year, and dust storms are common. The rate of evaporation, however, is great, amounting to 6 to 9 ft of water per year. The extremely low humidity makes the summer heat of 110°F tolerable with only a mild, temporary discomfort.

Jan 5, 1951

By S. Tiwary, S. Samanta, B. N. Pandey, N. C. Saxena, R. Sinha, B. P. Nandy, B. Singh

Subsidence investigations over one bord and pillar and one longwall caved panel at Dhemomain colliery showed that, although the width-depth ratio (0.82 and 0.83) and working and strata conditions were almost identical, the maximum subsidence over bord and pillar panel was 46.2 per cent of extraction thickness against only 6.9 per cent over longwall panel. The angle of draw was 13O to 210 and 66 to 95 per cent of the subsidence had taken place immediately after extraction. The subsidence profiles were not symmetrical and were of funnel like shape. There was wide variation in subsidence movements over caved faces in India mainly due to difference in the composition of supercumbent strata.

Jan 1, 1983

POSITIONS VACANT No. 228. Slate mining company desires men for the following positions: Superintendent to take full charge of underground work, quarrying and milling. Assistant or night superintendent. . Foreman for sinking a new shaft. No. 229. Chief engineer to take charge of drafting room, on furnaces and combustion apparatus. ENGINEERS AVAILABLE (Under this heading will be published notes sent to the Secretary of the Institute by members or other persons introduced by members.) Mining engineer and executive. Member. Columbia graduate. Age, 32. Married. 9 years' responsible work in mine examination and development. Experience in United States, Canada, Mexico and South America. Now superintendent large operating mine. Personal interview in New York. Available in August. No. 367.

Jan 8, 1917

By B. F. Oliver, C. W. Haworth

Pure tin and Sn-0.5pct Pb ingots have been frozen unidirectionally from the base. For quiescent melts that were initially undercooled, a transition from lower eqlciaxed structure to an upper columnar structure is found in the alloy ingots. Columnar to equi-axed back to columnar transitions are observed in superheated alloy ingots, but no such equiaxed band is observed impure tin. The reproducible equiaxed band is associated with a thermal undercooling followed by a recalescence. This undercooling is <5"C, whereas the critical (maximum obtainable) under-cooling for both the pure tin and the alloys used is -20°C. A similar undercooling is observed at the same position in the pure tin ingots, although in this case no clear transition in structure can be seen. The structure of the pure tin ingots is either entirely columnar or mixed columnar-equiaxed. A consideration of the detailed thermal history of the ingots indicates that the ingot macrostructures are determined by the occurrence of a local therlnal undercooling in conjunction with nuclei multiplication and transport mechanisrris. GENERALLY it is found that a pure metal ingot solidifies so as to produce an entirely columnar structure. Frequently an alloy ingot is found to have a columnar outer zone and an equiaxed central portion. Early systematic work to examine the factors controlling the formation of the equiaxed structure was reported by Northcott&apos; who showed that, for copper alloys frozen unidirectionally with a given ingot practice, the alloying element influenced the length of columnar crystals and the extent of the equiaxed structure. Northcott showed that alloys with a wider freezing range more readily produced the equiaxed structure. The nucleation process can be important in producing equiaxed structures; frequently an alloy which readily solidifies with an entirely columnar structure will produce an entirely equiaxed structure when a nucleating agent is added to the melt.&apos; The formation of the equiaxed structure was attributed by Winegard and chalmers3 to the presence of constitutional supercooling; that is, a region of liquid in front of the growing solid could have a temperature below its equilibrium liquidus temperature. Thus, with a small enough temperature gradient in the liquid, it was suggested that the presence of constitutional supercooling may be sufficient to bring about the nuclea-tion necessary for the formation of an equiaxed structure. Although this explanation is plausible, and may be relevant in many ingots, Walker has described an experiment&apos; for which constitutional supercooling seems to be an unlikely cause of nucleation. A Ni-20 pct Cu alloy, repeatedly undercooled more than 50"C, was crystallized and found to show the typical colum-nar-equiaxed structure. The separation between the liquidus and the solidus for the alloy is 40°C. Thus, in this experiment the nucleation required for the formation of the equiaxed structure must have come about in some other way than by the nucleation catalysis constitutional supercooling hypothesis. Chalmers has suggested more recently5 that nuclei (in a typical ingot) are present immediately after pouring and are prevented from redissolving by the constitutional supercooling effect. More recently Uhlman, Seward, Jackson, and ~unt&apos; have shown direct evidence using ice and organic materials that freeze dendritically that the "remelt mechanism" may be an extremely effective crystal multiplication process during the freezing of ingots under conditions involving dendritic growth. JSlia" experimentally demonstrated the detachment of dendrite arms. chernov14 has analyzed the dendrite arm detachment process as a coarsening phenomena driven by the minimization of interphase area. Katta-mis and ~lemings" working with undercooled steel melts give evidence supporting this mechanism. Mechanisms of dendrite arm detachment such as those assisted by convection are believed to be the origin of the macrostructures obtained in this study. This study makes no attempt to distinguish the relative contributions of these mechanisms. The object of the present work was to obtain accurate temperature measurements during the solidification of an ingot and to correlate these measurements with the formation of equiaxed grains in the resulting ingot structures. Similar previous work is very limited. The measurements carried out by Northcott are neither sufficiently extensive nor sufficiently accurate for any interpretation. Plaskett and winegard7 carried out experiments on A1-Mg alloys in which they observed values of the temperature gradient, G, in the liquid and rate of freezing, R (for a given alloy solute content Co), at the transition from a columnar to an equiaxed structure. They reported that equiaxed crystals were produced at values of G/G approximately proportional to the solidus composition. Similar experiments using Pb-Sn alloys carried out by £111011" showed a linear relation between G/R and the solidus composition. However, the thermocouples were in the mold wall rather than in the melt and, in one case, ingot surfaces were examined. There is ambiguity in the meaning of the values of G and R measured in all these experiments. APPARATUS AND EXPERIMENTAL PROCEDURE Alloys were prepared by induction melting 99.999 pct Sn and 99.999 pct Pb to form a Sn-0.5 wt pct Pb alloy in air in a graphite crucible and casting into a cylindrical graphite mold 6 in. long, 1 in. in diarn , and with a & in. wall thickness. This mold was mounted on a copper base through which cooling water could be

Jan 1, 1968

By W. L. Staker

The Bureau of Mines investigated selective extraction of Au and Ag from a low-grade Au ore containing Hg. Gold and silver were extracted from the ore in cyanide slurries, and Hg extraction was suppressed with sodium or calcium sulfide. Maximum Au extraction and minimum Hg extraction were obtained using solutions containing 0.34 lb NaCN/ton of solution. Increasing the cyanide concentration increased Hg extraction without increasing Au extraction. Mercury extraction from the ore was suppressed with 0.5 to 2.9 lb CaS/lb Hg in the ore. Gold-to-mercury ratios of 100:l to 400:l were obtained in the leach solution, and on the activated carbon in a CIP circuit.

Jan 1, 1984