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By Joseph L. Gillson

BRAZIL has had an industry based on ocean beach deposits of heavy minerals containing monazite, zircon, rutile, and ilmenite for well over 40 years, but except at the very earliest period, prior to 1906, and again during World War 11, has this industry been at all comparable in size with similar operations in other countries. Limiting factors have been neither a lack of reserves nor lack of markets (except for zircon). Although poor local transportation and shipping facilities have handicapped the development in Brazil, these conditions were perhaps equally bad (when mining operations started) in the Indian State of Travancore, and in New South Wales and Queensland, Australia, in which states the principal production of beach deposits of heavy minerals has occurred. The outstanding restraints on the Brazilian industry have been the lower quality of the Brazilian minerals, the relative small size of individual deposits that were known until recently, the lack of interest of Brazilian investors in mining ventures, and the unfavorable climate for investment of foreign capital under Brazilian mining law. The lower quality of the minerals is indicated by the fact that the Brazilian monazite carries only 5 to 6 pct Tho2*, and the ilmenite 561/2 pct TiO2, whereas the corresponding Travancore minerals carry 9 pct Tho, and 60 pct TiO, respectively. The Brazilian zircon is a dirty brown color (which can be removed readily) as compared with the gleaming whiteness of the Australian zircon. An inadequate market for the abundant zircon that will be available in any operation in Brazil is certainly a heavy restraint, since otherwise it could be an important byproduct. The oxide of zirconia, baddeleyite, that has come from Brazil is from other sources.' Since the Brazilian beach sands carry only a little rutile, that mineral has not been available as a valuable byproduct to help finance the operations. Substantial tonnages of rutile have been exported from Brazil. The sources of this mineral are stream placers and residual deposits over gneisses in the States of Goyaz, Minas Geraes, Ceara, etc. (Leonardos,' and Chambers". With these handicaps, Brazilian production from beach sands has been marginal, and there has been only one consistent producer. This is a company, originally French, which was called Companie de Franco-BrazilliCne, but, with the downfall of France in 1940, became Brazilian under the name Monazita e Ilmenita do Brasil ("Mibra"). This company has operated several deposits in the vicinity of Guara-pary, in the State of Espirito Santo. Its office and plant has been at Guarapary. Recently a company called, "Fomil" (Fomento Monazita-Ilmenita) started operations. This company was organized by the Foote Mineral Co. of Philadelphia, and such share as a foreign company can hold under Brazilian law has now been acquired by the Lindsay Light and Chemical Co. of Chicago. When the writer went to Brazil in the fall of 1940, he found that no general survey of the beaches had been made except for a thorough study of part of the area by Abreu.4 The paper by Miranda6 had not then been written. The federal Geological Survey and Department of Mines knew only of the existence of the deposits in Espirito Santo south of Vitoria, and had a hazy idea that others might be found north of Vitoria. One deposit in Bala was known in Rio, but the larger one at Guaratiba was not known, although a Frenchman had prospected

Jan 1, 1951

By Joseph L. Gillson

BRAZIL has had an industry based on ocean beach deposits of heavy minerals containing monazite, zircon, rutile, and ilmenite for well over 40 years, but except at the very earliest period, prior to 1906, and again during World War 11, has this industry been at all comparable in size with similar operations in other countries. Limiting factors have been neither a lack of reserves nor lack of markets (except for zircon). Although poor local transportation and shipping facilities have handicapped the development in Brazil, these conditions were perhaps equally bad (when mining operations started) in the Indian State of Travancore, and in New South Wales and Queensland, Australia, in which states the principal production of beach deposits of heavy minerals has occurred. The outstanding restraints on the Brazilian industry have been the lower quality of the Brazilian minerals, the relative small size of individual deposits that were known until recently, the lack of interest of Brazilian investors in mining ventures, and the unfavorable climate for investment of foreign capital under Brazilian mining law. The lower quality of the minerals is indicated by the fact that the Brazilian monazite carries only 5 to 6 pct Tho2*, and the ilmenite 561/2 pct TiO2, whereas the corresponding Travancore minerals carry 9 pct Tho, and 60 pct TiO, respectively. The Brazilian zircon is a dirty brown color (which can be removed readily) as compared with the gleaming whiteness of the Australian zircon. An inadequate market for the abundant zircon that will be available in any operation in Brazil is certainly a heavy restraint, since otherwise it could be an important byproduct. The oxide of zirconia, baddeleyite, that has come from Brazil is from other sources.' Since the Brazilian beach sands carry only a little rutile, that mineral has not been available as a valuable byproduct to help finance the operations. Substantial tonnages of rutile have been exported from Brazil. The sources of this mineral are stream placers and residual deposits over gneisses in the States of Goyaz, Minas Geraes, Ceara, etc. (Leonardos,' and Chambers". With these handicaps, Brazilian production from beach sands has been marginal, and there has been only one consistent producer. This is a company, originally French, which was called Companie de Franco-BrazilliCne, but, with the downfall of France in 1940, became Brazilian under the name Monazita e Ilmenita do Brasil ("Mibra"). This company has operated several deposits in the vicinity of Guara-pary, in the State of Espirito Santo. Its office and plant has been at Guarapary. Recently a company called, "Fomil" (Fomento Monazita-Ilmenita) started operations. This company was organized by the Foote Mineral Co. of Philadelphia, and such share as a foreign company can hold under Brazilian law has now been acquired by the Lindsay Light and Chemical Co. of Chicago. When the writer went to Brazil in the fall of 1940, he found that no general survey of the beaches had been made except for a thorough study of part of the area by Abreu.4 The paper by Miranda6 had not then been written. The federal Geological Survey and Department of Mines knew only of the existence of the deposits in Espirito Santo south of Vitoria, and had a hazy idea that others might be found north of Vitoria. One deposit in Bala was known in Rio, but the larger one at Guaratiba was not known, although a Frenchman had prospected

Jan 1, 1951

By H. J. Levinstein, W. H. Robinson

A method of chemically polishing silver for metal-lographic examination has been developed. The samples are prepared by polishing on 0, 2/0, and 3/0 paper. They are then polished on 600 micro-cut paper, followed by a final mechanical polish on a cloth containing 5µ diamond paste. The samples are then chemically polished in a solution of 100 cc of saturated chromic acid and 5 cc of a 5 pct HC1 solution. The chemical polishing is performed by swabbing with a cotton ball saturated with the solution. During the chemical polishing, the sample is rinsed frequently in running water. Polishing in this manner for 5 min is sufficient to remove the strained material from the previous polishing operations. The amount of material removed is approximately 4µ/min. The surface obtained is flat and free of pits. Fig. 1 is an interference micrograph of a silver surface polished by this technique. If the solution employed is of improper HC1 content, an interference color film will form on the sample. This film can be removed either by swabbing with a cotton ball saturated with ortho-

Jan 1, 1962

By A. D. Rich

The term "bleaching clay" or "bleaching earth," as used in the oil industries, refers to clays that in their natural state, or after chemical or physical activation, have the capacity for adsorbing coloring matter from oil. There are three common types of bleaching clays: fuller's earth, activated clays, and activated bauxite. Fuller's earth, or naturally active clay, is prepared from bentonites (see Chap. 5) that possess natural activity. It is not activated commercially; in fact, earths of this type ordinarily do not respond satisfactorily to acid activation. Fuller's earth is prepared in pulverized as well as granular form for use in the contacting and percolation processes, respectively. Acid-activated clays also are of bentonitic origin. The basic raw clay, however, is of a type that has a very low natural activity but is highly activable by treatment with mineral acid. Commercial acid-activated clays generally possess several times the decolorizing power (bleaching efficiency) of the best quality of fuller's earth. The former are prepared commercially only in the pulverized grade because of the difficulties in obtaining a satisfactory granular product, and hence are used only in the contact process. Activated bauxite is made by heat-treating bauxite ore, which in its natural state has very little natural activity. The commercial product is prepared in granular form for use in the percolation process on petroleum oils. For the most part, bleaching clay is used commercially in the decolorization of animal, vegetable and petroleum oils, fats and waxes. It is applied in two ways: (1) by the percolation method and (2) by the contacting method. Percolation refers to the passage of oil through a bed of granular clay whereas contacting refers to direct agitation of oil and pulverized clay followed by removal of the clay from the oil by filtration. In either case, the decolorizing effect is obtained by intimate contact between the liquid oil and the solid adsorbent. Petroleum oils are treated commercially by either the percolation or the contact process. Animal and vegetable oils are treated by the contact process only. Composition The raw clays from which both fuller's earth and acid-activated clays are prepared are composed of hydrous aluminum silicates containing varying quantities of magnesium, iron, calcium and other elements. These raw materials are usually nonswelling bentonites derived from volcanic ash or lava by weathering and hydrothermal chemical reactions. The bentonites have as their chief mineral constituent montmorillonite, which has the formula [(OH)4Si6A14O20•nH2O], according to Grim. (See Chap. 5, ref. 6, p. 91.) The underlying reasons are not fully known for the natural activity of the fuller's earth type of clay and its usual failure to further activate with mineral acid in contrast to the natural inactivity of the activatable type of clay. However, it may be said that the bentonites that are responsive to the acid-activation treatment generally have not undergone any drastic metamorphism. The chemical composition is not a reliable means of discrimination between a nonactive, a naturally active, and a nonactive but activable clay, therefore it is not possible to forecast the ultimate quality of a clay on the basis of the raw-clay analysis alone. Table 1 gives typical analyses of representative clays of the foregoing classifications.

Jan 1, 1960

By Klaus M. Zeitler

INTRODUCTION One cannot discuss the subject of "Raising Capital in the 1990s" without having a crystal ball and a reliable fortune teller. This discusses "Raising Capital for the 1990sW, which is what Metal1 Mining Corporation did in 1987. We raised (3166 million in an IPO (initial public offering) that was originally planned for only some (375 million. Why did we raise this money? How did we do it, and why was this IPO so successful? The answer to the first question requires a description of the promoter and principal shareholder of Metal1 Mining Corporation, Metallgesellschaft AG. This West Germany company was founded over 100 years ago in Frankfurt as a trading house for non-ferrous metals. It has developed into one of the world's leading firms in the non-ferrous metals industry. The company's worldwide activities in all areas of that business include mining, smelting and refining, the trading of ore, base and precious metals, the production of semi-fabricated and finished metal products, and the provision of engineering, construction and transportation services. Metallgesellschaft AG has also diversified into many other areas, the most significant of which are manufacturing, the production of chemicals, the development and application of technical and chemical processes, the planning and construction of industrial plants, and activities associated with finance, insurance, shipping and freight forwarding, and the provision of barter and countertrade services. The company maintains a network of more than 100 offices around the world; it employs some 25,000 people in its worldwide activities. [Selected financial data, as of September 30, 1987: (MetaUgesellschafl AG) Working Capital DM 8%.6 million CDNS 672.8 million Long Term Debt DM 568.0 million CDNS 426.2 million Sales DM 14.9 billion CDNS 11.2 billion Net Income DM 87.7 million CDN$ 65.8 million Market Capitalization at April 27, 1987: (Metallgesellschafi AG) Outstanding Shares ~,6oo,o0o DM 1,875 million CDNS 1,407 million] For the fiscal year ended September 30, 1987, Metallgesellschaft AG had, on a consolidated basis, net sales of DM13.3 billion, net income of DM100 million and total assets of about DM7.0 billion. Metallgesellschaft AG established the American Metal Company, a predecessor of AMAX Inc. one of the largest ventures undertaken by Metallgesellschaft AG then was the acquisition, through the American Metal Company, of a majority share in the Mexican Penoles mine, a large lead and silver deposit. METALLGESELLSCHAFT AG Figure 1 depicts an overview of Metallgesellschaft AG before and at the time the initial public offering of Metall Mining Corporation's shares took place. It shows that mining was far from the centre of Metallgesellschaft's activities. Therefore, it could not expect to receive an extraordinary amount of board attention. Thus, mining investments not only had to compare well with other mining opportunities, but were in fierce competition with projects from other divisions. In addition, mining was sub-divided into two separate departments -- domestic and international. These two departments had different management styles and diverging interests which resulted in a minimum co-operation between them. The domestic mining department was primarily interested in the survival of the local mines. These mines were characterized by rising operating costs and declining ore grades. It took a special commitment and continued ingenuity to develop and adjust to local conditions, and modern mining and processing technology, in order to remain competitive, or at least survive within the international mining industry. Local management

Jan 1, 1990

By H. F. Mills

THE Iron King mine is 12 miles east of Prescott Arizona, in low foothills of the Agua Fria mining district. It was operated in 1906 and 1907, using gravity methods of concentration, mostly on oxide ores. In 1923 and 1924 shipments of sulphide ores were made to the Humboldt smelter. It remained inactive and stripped until 1936, when it was unwatered and sampled to the 400-ft level, the bottom at that time. In 1937 the Iron King Mining Co. purchased the mine and shipped oxide ores. During 1938 a bulk flotation plant of 140 tons daily capacity was erected. The mill has been enlarged and operations have been continuous since the mill first started. In July 1942, the Shattuck Denn Mining Corporation purchased the physical assets from the Iron King Mining Co., and since that time it has operated as the Iron King Branch of the Shattuck Denn Mining Corporation. Economic metals recovered are gold, zinc, silver, lead, a little copper, and fluxing pyrite. The ore occurs as a series of northward-dipping shoots arranged in echelon pattern, the series extending over a length of 3500 ft. Strike lengths of shoots vary from 60 to 600 ft, and widths from 3 ft to as much as 14 ft. The ore occurs in a sheared zone in pre-Cambrian chloritic schist. This schist belt is about 6 miles wide, and the ore zone is about 4 miles from the pre-Cambrian granites to the west. No intrusive rocks have been found in the mine, nor is there evidence of any on surface that might indicate a genetic connection with the ore occurrence (Fig I). The schists strike N23°E and dip 75° to the northwest, which might indicate an overturned thrusting from the granites. In the upper levels, the echelon pattern in which the ore occurs was quite regular, no disturbance of the enclosing schist, or of any faulting that might contribute to the formation of the ore pattern was noted. There is a possibility that the ore zone may be on the axis of an isoclinal fold. Another interesting feature is the more or less typical zoning of minerals along the strike in each of the ore shoots (Fig 2). The north end of each shoot is enclosed by schist, while the south ends usually extend out at full width beyond the economic mining limits in a pyrite-quartz low-grade material. The plane of demarcation between ore and schist is very sharp, with little or no impregnation of sulphide in the schist, especially on the footwall side. The footwall schists are usually firm and strong, and vary from dioritic phases to fine-grained, lighter colored bands, almost silky in texture. The hanging wall for a width of 50 to 8o ft consists of alternating sheetings of chloritic and pyritic schists. The mine is now partly developed to the 92o-ft level, with some diamond drilling from the 1150-ft station of No. 6 shaft. Economically there has been little change in nature or grade of ore from the top of the sulphides, about 200 ft below surface, to the bottom levels. There have been a few echelons in depth, just as there are in plan, and while a few shoots have had

Jan 1, 1947

By W. C. Ellis

IN an ingot of germanium solidified progressively from the bottom by a method' devised by J. H. Scaff and H. C. Theuerer, examination discloses ex- IH. C. Torrey and C. A. Whitmer, Crystal Rectifiers. p. 364. 1948. New York. McGraw-Hill Pub. Co. tensive twin relationships. A slice taken about midway in a cylindrical ingot approximately 3/4 in. in diameter and 1 1/2 in. in length, after etching and polishing to delineate different orientations, is shown in fig. la. The orientations of the regions designated with letters were determined by Laue X-ray back-reflection methods and plotted on stereograms. The orientation relationships of the designated components were determined by comparing the values for the nine angles between the three respective cube poles of each orientation with the values calculated in a formal treatment of octahedral multiple twinning in cubic crystals. Germanium, diamond cubic in structure, has the octahedral twinning habit. I am indebted to K. H. Storks for the calculation of the angular relationships of cube poles in octahedral twinning to four orders. The set of values for the nine angles is distinctive of the order of twinning. Confirmation for a multiple twin relationship is obtained from the determined indices of the mirror planes. These exist for all orders of twinning through the third and for some of the fourth." If the orientations are not those for twinning, then the nine angles for the cube poles do not correspond in value and distribution to those formally calculated. Since all nine angles must correspond in values and distribution of values to the calculated ones, the Laue method with a precision of one or two degrees is adequate to establish or deny with confidence the existence of multiple twins. Regions of the same orientation can also frequently be identified by the optical reflections. For example, the narrow twin bands in A at 2: 00 o'clock have orientation B1. The interesting twin relationships shown schematically in fig. lb were found for the section in fig. la. Most of this slice was made up of orientation, A, appearing in widely separated regions. Of the four possible first order twins of A, three were present in this slice and are designated by B with subscripts. Four second order twins of A are designated by C with subscripts. It is worth emphasizing that two of these, C, and C,, are second orders of A through the first order missing in this section. Two regions, designated by D with subscripts are third order twins of A. D2 is a sixth order twin of D,. All orientations found were ascribable to multiple twinning, as if the orientations in this section originated earlier in solidification from a single nucleus. The presence of extensive multiple twinning to- gether with the absence of other orientations appears to be a characteristic result in many instances of solidification of germanium. Fertile conditions for twinning probably exist in the array of atoms in the diamond cubic structure. The high order twins in the section shown, it is reasonable to presume, are the result of progressive octahedral twinning through several generations in the material freezing earlier. Some of these generations do not appear in this section, it is suggested, because their orientations with respect to the growth direction were unfavorable for survival. The extensive twinning is probably promoted during solidification by constraint imposed by volume increase, and to an irregular growth front. Twinning may also be due, in part, to the attempt of the solidifying region to attain the orientation most favorable to the growth direction (maximum thermal gradient). The nucleus for a twinned orientation could have its origin in a "stacking fault" on the close-packed octahedral plane. Further work is being done in which the course of twinning throughout an ingot is being studied. The results appear to be important in the general theory of solidification.

Jan 1, 1951

STANDING COMMITTEES Executive-SIDNEY J. JENNINGS, chairman. Membership-KARL EILERS; chairman. Finance-GEORGE D. BARRON, chairman. Library-E. GYBBON SPILSBURY, chairman. Papers and Publications-BRADLEY STOUGHTON, chairman. Nominations-R. V. NORRIS, chairman. Institute of Metals Division-WILLIAM M. CORSE, chairman; FRED L. WOLF, secretary, Ohio Brass Co. Mansfield, Ohio.

Jan 12, 1918

G. SHERBURNE LAGERS (written discussion*).-Mr. Kennedy's discussion1 of Mr. Matteson's paper takes the form of a criticism of my own comments2 on this paper. Mr. Kennedy is a respected authority on matters pertaining to the salt-dome oil fields, and his characterization of my "elaborate figures" as "worthless" is sufficiently candid and comprehensive to warrant a brief reply. My "voluminous figures" consisted simply of a rough estimate of the minimum quantity of salt in the Humble dome, and a calculation of the volume of sea water and of the volume of saturated brine which this salt would represent. Mr. Kennedy apparently interprets my remarks as opposing the idea that so large a volume of salt could have been deposited from sea water, for lie cites the area and thickness of European salt beds; but nothing was further from my intention. Given an arm of the sea, an arid climate, and evaporation under a hot sun, it is easy to conceive the formation: of almost any thickness of bedded salt. I cited the figures in connection with Harris' theory of the origin of salt domes, according to which the plugs were formed by the deposition of salt from ascending brine solutions, owing to the drop in temperature as they neared the surface. I pointed out the well-known fact that the solubility of salt is only slightly affected by temperature, and that a drop of 80° C. would cause the deposition of less than one-tenth of the salt in solution; hence that more than ten times the volume of salt actually forming the plug must have been involved. If ten times the salt actually in sight be computed in terms of brine and multiplied by 50 or 60 to take into account all of the known salt domes, the resulting figure is so enormous that I am not at all as sure as Mr. Kennedy seems to be that the porous stratified rocks of eastern Texas and western Louisiana could contain or furnish so great a volume of migratory brine.

Jan 8, 1918

By J. H. Scaff, H. C. Theuerer

Germanium may be reversibly converted from n to p type by heat treatment. Data for the conversion and the associated changes in resistreatment.tivity are given and the results are interpreted in terms of changes in the donor-acceptor balance. MEANS for controlling the electrical properties of germanium in a predictable manner are of interest because of the increasing utilization of this element as the semiconducting material in electrical devices. Since both the mechanism and the magnitude of the electrical conductivity depend upon the kind and quantity of impurities present, the conductivity usually is adjusted by first carefully purifying the germanium, and then, by standard alloying procedures, adding the elements desired. The elements usually added are from the third or fifth periodic groups depending upon whether p- or n-type germanium is desired. However, in the development of germanium rectifiers during the war, it was found that it was possible also to modify reversibly the conductivity of germanium and even to produce conversion from n to p type by heat treatment.1,5 Since then a detailed study of this effect has been made. The data are presented in this paper and an explanation is offered for the effects observed. Preparation and Experimental Procedure The method used in preparing the germanium ingots for this investigation has been previously described.' The method consists essentially of (1) reduction of GeO2* and (2) preparation of a 50-g ingot from the reduced material. Graphite containers are used in both steps. In the first step the GeO2 is reduced in hydrogen at 650 °C to form a sponge germanium which, to assure complete reduction and to obtain massive materials, is fused subsequently in the reduction furnace by gradually raising the temperature to 1000°C. The button of germanium thus obtained corresponds to a yield of 99.8 pct. The final ingot is prepared by fusion of the germanium button in a helium atmosphere. A cylindrical crucible in a vertical silica tube furnace is employed and the crucible is heated by an external induction coil. The ingot is solidified from the bottom upward by raising the induction coil at a constant rate with power to the coil kept at a fixed value. In such ingots, segregation is normal and most of the impurities are concentrated in the last region of the ingot to freeze. It follows then that the major portion of the ingot is purer than it would have been if freezing had occurred in a random fashion. Moreover the orderly advance of the freezing surface during solidification establishes in the ingot a succession of surfaces of constant composition, if it is assumed that the liquid is homogeneous and that diffusion in the solid is negligible. Therefore, some information on the distribution of impurities in the ingot may be acquired by determining the shape of the solid-liquid interface at different stages of solidification. This is of importance because the concentration of impurities will be seen to affect the response of germanium to heat treatment. Such information is difficult to acquire by direct means, for the impurities responsible for the electrical properties of germanium prepared in this way are present

Jan 1, 1952

Executive JOHN R. SUMAN, Chairman PAUL D. MERICA, Vice-Chairman CHESTER A. FULTON W. M. PEIRCE H. Y. WALKER Finance H. T. HAMIL'T'ON, Chairman ERLE V. DAVELER HENRY KRUMB Admissions FELIX E. WORMSER, Chairman GEORGE D. BARRON, Vice-Chairman PHILIP KRAFT EDWARD MEAGHER CLYDE E. WILLIAMS

Jan 1, 1941

By W. M. Corse

I bring this investigation to your attention to emphasize the needless waste attendent upon the use of tin plate with an unnecessarily heavy tin coating. With our present knowledge, we are unable commercially to produce coatings as light as the lower weights used in this test. If, however, future research should develop means to this end, the resultant product would meet all practical requirements, and a very considerable saving in pig tin would result. DISCUSSION G. H. Clamer.-—The National Canners' Association is studying the action of fruit juices, etc., on solders. Of course these tests will take quite a long time, and we hope by that time the war will be over and there will be no need for conserving tin for war purposes. Germany for a great many years has prohibited the use of more than 37 per cent. of lead in alloys used in contact with food products. The eutectic composition is 37 per cent. of lead and 63 per cent. of tin; alloys containing more than that percentage of lead have some free lead. J. W. Richards,' South Bethlehem, Pa.—A great deal of conservation can result from the packing of dry foods in cartons and in fiber packages instead of using sheet tin. Many of the boxes used for packing things other than food are frequently made of sheet tin because it prints and lithographs well; these could be made of sheet iron coated with copper or some other substitute metal which prints equally well. The Aluminum Bronze Industry W. M. CORSE,† Mansfield, Ohio.—The conservation of tin, in view of the shipping situation, is one of great importance. Several methods of conservation can be employed: 1. Reduction of the amount of tin in an alloy or compound. 2. Substitution of an entirely different metal or compound for tin. 3. A combination of the first and second methods. The second method is the one that I wish to discuss. Metallic aluminum, has been known for a long time, and its use in copper alloys was discovered about 1855 by Lord Percy. The high cost of production of metallic aluminum retarded its commercial development, and it was not until the discovery of the electrochemical processes for its production that it came to be known as a common metal. I have been particularly interested, for the past few years, in working with the alloy known as aluminum bronze, which is usually composed of approximately 90 parts of copper and 10 parts of aluminum, by weight.

Jan 1, 1919

By T. L. Chu, G. A. Gruber

Silica films hare been rleposited 011 silicon substmtes at 400° to 600°C by a chemical-transport technique using hydrogen fluoride as the transport agent ill a closed system. This transport takes place from a source materia1 1071: temperature to substrates at higher temperatures, as indicated by the thermochemistry of the transport reaction. The experimental variables of- the transport process, such as the substrate temperature, the pressure pi the transport agent, and so forth, have been studied. The rate -determining step of the transport process appears to he the ),ale of chemical reaction in the source region. The transported films are similar to thermally grown silica films in physical proper-ties with the exception of 'some what higher dissolrrtion rates. SILICA films deposited on suitable substrates serve many purposes in electronic devices. They are used for the fabrication of tunneling devices, the surface passivation of devices, and the shielding of devices from nuclear radiation: and as selective masks against the diffusion of specific impurities into semiconductors. Doped silica films can also be used as sources for the diffusion of impurities into semiconductors. Several oxidation and deposition techniques for the preparation of silica films have been developed to meet the requirements of these applications. The therma1 oxidation of silicon by oxygen or steam at temperatures above 900 C is commonly used in silicon technology. The deposition techniques are perhaps more advantageous since they usually require lower temperatures and are not limited to silicon substrates. Silica films have been deposited on silicon and other substrates by reactive sputtering and chemical reactions. The sputtering of silicon in an oxygen atmosphere is capable of depositing good-quality silica films on silicon' and gallium arenide. Many chemical reactions are known to yield silica at room temperature or higher. These reactions may involve intermediate steps. However, the final step yielding silica should take place predominately on the substrate surface in order to produce adherent films. When silica is formed in the gas phase by volume reactions, no adherent deposit can be obtained. Generally, the experimental conditions of a reaction can be varied so that the surface reaction predominates over the volume reaction. The chemical reactions which have been used successfully for the deposition of silica films are briefly as follows. The pyrolysis of alkoxysilanes in an inert atmosphere or under reduced pressure has been employed to deposit silica films on germanium3 and silicon4 at 650" to 750°C in a flow system. The deposition of silica films from alkoxysilanes has also been achieved at nearly room temperature by a low-pressure plasma. Device quality silica films have been deposited on germanium and gallium arsenide by the deposition of an amorphous thin silicon film followed by oxidation at 600" to 700" . Silica films for high-temperature capacitors have been produced by the hydrolysis of silicon tetrabromide at 950°C in argon and hydrogen atmospheres.7 We have developed a chemical-transport technique for the deposition of silica films on semiconductor substrates at relatively low temperatures. The thermochemistry of the transport reaction, the experimental variables of the transport process, and the properties of the transported silica films are described in this paper. THERMOCHEMICAL CONSDERATIONS The transport of solid substances by chemical reactions in the presence of a temperature gradient has been used for the preparation of films and crystals of many electronic materials. In this technique, a gaseous reagent is chosen so that it reacts reversibly with the solid substance under consideration to form volatile products. Since the equilibrium constants of most reactions are temperature-dependent, the transport of these products to regions of suitable temperature in the reaction system would cause the reverse reaction to take place. depositing the original solid. When the equilibrium is shifted toward the formation of the solid as the temperature is decreased, the solid is transported from a high-temperature zone to a lower-temperature region, and vice versa. This chemical-transport technique can be carried out in a closed or gas-flow system. In a closed system, chemical equilibrium is presumably established in the different temperature regions of the system, and the transport agent regenerated in the deposition region repeats the transport process in a cyclic manner. The local chemical equilibrium may not be approached in a flow system: however, this system offers a greater degree of flexibility. Silica reacts reversibly with hydrogen fluoride and this reaction was chosen for the transport process. The over-all reaction between silica and hydrogen fluoride may be written as: SiO2(s) + 4HF(g-) = SiF4Ur) + 2H2O(^)

Jan 1, 1965

By L. S. Castleman, R. K. Hotzler

We are currently studying the effects on recrys-tallization of impurities diffused into dispersion-hardened alloys. Our interest in this phenomenon was originally aroused by the observation that the recrystallization temperature range of tungsten "doped" with alumina and silica, or with thoria, is lowered drastically if nickel is plated onto the tungsten prior to heat treatment.' In this note, we report a similar effect that sulfur has on the recrystallization behavior of thoriated nickel. The experimental procedure for this exploratory phase of the investigation has consisted simply in heating commercially obtained stress-relieved samples of thoriated nickel for varying temperatures and times in sealed capsules containing air and small quantities of sulfur. The samples contain 2.4 vol pct thoria and initially less than 18 ppm S by weight; they are prepared either from 0.5-in.-ciiam rod stock or from 0.092-in. sheet and are in the "as-received" (stress-relieved) condition prior to exposure. In an atmosphere free of sulfur, such samples do not show evidence of recrystallization after being annealed for 1 hr at a temperature of 2500°F (1372C).2 The photomicrograph in Fig. 1 shows the microstructure of one of our samples annealed for 75 hr at 1000° C (1832°F) in a sulfur-free capsule. The grain structure is hardly evident (if at all) at 465 times magnification. In contrast, the photomicrograph of Fig. 2 shows the recrystallization that has taken place in a sample exposed to sulfur for 5 hr at 1000°C (1832°F). A nickel sulfide phase is visible at the grain boundaries of the light-appearing grains. We have also observed recrystallization to occur in a sample annealed at 600°C (1112°F) for 25 hr. This temperature is below the 637°C (1178°F) eutectic in the Ni-S system. In the latter case, no nickel sulfide phase is evident in the microstructure. Moreover, we have noticed the occur-

Jan 1, 1969

By M. E. Fine

IN the apparatus for measuring internal friction shown in fig. 1, a modification of that described by Kê,1,2 the parasitic energy loss or background is equivalent to a Q-1 of approximately 4x10-5. This low value of background was obtained by using a jeweler's collet of appropriate size for the upper support, eliminating lateral motion without immersing the bob in oil, and designing the bob to reduce air resistance. The pendulum is supported on the frame through a snug fitting, sliding rotary joint (fig. I-B). A slight twist of the top imparts essentially pure torsional motion to the pendulum. No evidence of energy loss in the sliding joint has been observed. In the bob (E) steel balls are used in the torsion arm, and the bottom is filled with lead giving a total weight of 94 g. A lighter bob may be used for small diameter specimens. Another bob was a solid disc with provision for adding discs to change the frequency. The oscillating image of the filament is recorded on a revolving drum camera (fig. 1-3) driven by a synchronous motor. This allows use of frequencies higher than can be measured visually on a glass scale. Samples varying in diameter from 0.020 to 0.075 in. have been measured, the frequencies have ranged from 1 to 12 cps, and the maximum strain varied from 0.5 to 10x10-5. With appropriate modification the sample may be placed in a thermostat. The apparatus may also be used to measure the shear modulus. In the examples of measurement given in table I the internal friction of Permendur and the 46.8 Ni-Fe alloy are due, for the most part, to magneto-mechanical hysteresis8 (elastic hysteresis accompanying stress-induced magnetostriction) which depends on strain amplitude and increases with annealing. The internal friction of most materials decreases with annealing. References IT. S. K6: Physics Review (1947) 71, 533. 2 T. S. Kê: Transactions AIME (1948) 176, 448; Metals Technology (June 1948) TP 23703. 3 R. Becker and W. Döring: Ferromagnetismus. 365 (1939). J. Springer.

Jan 1, 1951

By Charles E. Wait

HAVING had some experience in the use of gasoline-gas in a laboratory, I have been induced by frequent inquiry to present a few hints concerning it, which I hope may be of some value to those who are out of the reach of coal-gas, and who contemplate using this gas. While I will not delay to describe the method by which this gas is made, it may not be out of place to note that, unless frequent charges are put into the carburetter, the gas is variable in richness. This may be partially avoided, it is said, by repeatedly pumping from one cell in the carburetter to another. If a machine is in constant use for many months without re charging, the gas becomes rather poor for illuminating purposes ; but in this condition it may be burned in a Bunsen burner with advan tage. Could the gas be used always in this condition, no difficulty would be experienced, and it would be quite satisfactory for general laboratory purposes. Considerable annoyance, however, is experi enced whenever the machine is filled with gasoline. The Bunsen and other burners then produce a flame too smoky to be used with com fort, and, in fact, with most of them, a full supply of air; turned on at the base of the burner, will not suffice to completely burn off all the carbon. Finding it necessary to adopt some method by which I could get a flame free from unconsumed carbon, I adopted a plan which has in every way proved satisfactory. In addition to the pipe conveying the gas to the table, and ar ranged with a stopcock, there is brought to the table, within a fern inches of the gas-pipe, another pipe, conveying air direct from the pump. This pipe is also arranged with a stop-cock. The air- and gas-pipes are now connected with one pipe by a T joint; and to this last pipe is attached, by rubber tubing, the Bunsen or other burner. I have successfully used this simple system in connection with both small and large Bunsen burners, a burner with three tubes, arid a Fletcher burner; and recently I have added a new still to our equipment, and have been tising with it a Fletcher special high power burner No. 6, to which this system has been applied. With

Jan 1, 1886

By Paul Weir

DURING the past decade, methods of producing bituminous coal in the State of Illinois, which ranks third in production among the states in which bituminous coal is mined, have undergone great changes. From less than one million tons in 1923, the strip-mine production has gradually increased to a high of 11,725,870 tons in 1937. From a negligible amount prior to 1927, the amount of coal mechanically loaded underground had increased to a high of 28,374,362 tons in 1937. The amount manually loaded in 1937 reached a low of 12,332,023 tons. In this same year, this state ranked first in strip-mine production, also in mechanically loaded production. For this reason a study of the influence of mechanization on location of production in Illinois may be helpful in anticipating what may happen in other producing states. The reason for the changes in methods lies in the differences in costs of production. The Bureau of Research and Statistics of the National Bituminous Coal Commission has made public the following costs of pro-duction by various methods in the State of Illinois (district 10) for the last nine months of 1937: all mines, $1.7602 per ton; strip mines, $1.4319; mechanical loading mines, $1.7457; hand loading mines, $2.1793; all underground mines, $1.8703. These are weighted averages for the entire district. Inasmuch as production in 1937 was reported from 58 counties scattered over two-thirds of the area of the state and from five different seams varying in thickness from less than 3 ft. to as much as 12 ft., it is apparent that the location of production must be influenced by the extent of mechanization possible in the various producing counties.

Jan 1, 1939

By Frederick C. Pearson, Albert Brown, Emil R. Ermert

EARLY in 1946 the Shen-Penn Production Co., a subsidiary of the Philadelphia and Reading Coal and Iron Co., was organized to operate the Shenandoah Stripping, one of the largest open-pit anthracite mines in the world. This mine is located in the Western Middle Field near Shenandoah, Schuylkill County, Pa., and involves the removal of approximately 60,400,000 cu yd of overburden to permit the recovery of 9,200,000 gross tons of rough cleaned coal from an area 8000 ft long and 2700 ft wide, with a maximum depth of 400 ft. Operations began in August 1946, and within the next few years 31,811,000 cu yd of overburden and 2,994,000 gross tons of rough cleaned coal had been removed. During the early days of open-pit mining operations, steam was the primary motive power. However, as the size of the equipment increased, so did the problems of fuel, water, labor, and maintenance. Because of its efficiency and convenience, electric power rapidly replaced steam. Later the modern diesel engine was developed, and today practically all stripping equipment is either electric, diesel-electric, or diesel-powered. In locations where electric power is not readily available or where operations are scattered over a large area, diesel power is favored. At Shenandoah operations are highly concentrated in a relatively small area, and this fact, coupled with the availability of ample electric energy, indicated the selection of electric-powered equipment. Since this was a new company, it was necessary to purchase every item, from the smallest tools to stripping shovels. Although the organization period was hampered by the postwar scarcity of materials, an excellent opportunity was afforded to set up a thoroughly modern plant. This paper will describe the power facilities, with particular emphasis on the more unusual features. The substation is a major item in a power distribution system, and a simple arrangement utilizing high quality equipment is an excellent investment. With this in mind, a 3000-kva unit type substation was selected and installed. This unit is made up of three sections, which are assembled simply by bolting together the various sections and connecting the power leads, see Fig. 1. The transformer proper, rated at 3000 kva, is oil-filled and nitrogen-sealed, having a 66,000-v Delta primary and 4160-v Wye secondary with a grounded neutral and 46-ohm ground resistor. The function of this resistor will be described later. Electrical energy is purchased from a public utility and is delivered to the main substation at 66,000 v over one or the other of two incoming lines. These lines terminate on a high voltage switching section on which high voltage fuses and Thyrite lightning arresters are installed. The outgoing feeder switching unit is made up of the following: 1-An auxiliary compartment consisting of potential and current transformers with necessary terminal blocks for connecting to power company metering equipment. 2-Another auxiliary compartment containing a control transformer, battery, and battery charger for the furnishing of power for tripping and reclosing of power circuit breakers. The assemblies in these auxiliary compartments are mounted on carriages that can be rolled in and out with ease. Potential transformers are readily accessible for inspection and fuse replacement. When withdrawn from the operating position they are completely de-energized and grounded. 3-Two feeder breaker compartments, each with a 1200-amp, 5000-v, solenoid-operated magneblast air circuit breaker, voltmeter, ammeter, overcurrent relays, and a ground relay. These power circuit breakers can be quickly and safely withdrawn or repaired. A built-in isolating mechanism is used for lowering the breaker to a transfer truck for repair or inspection or as a means of disconnecting the breaker from the source of power as an added precaution when working on power lines. Thus inspec-

Jan 1, 1952

By Rossiter W. Raymond

The 12th of April, 1877, witnessed the celebration, at Freiberg, Saxony, of an event profoundly important for the ancient mining industry of that district, and full of interest to mining engineers throughout the world—namely, the connection of the famous Roth-

Jan 1, 1879

By Edward L. Clark, Garrett A. Muilenburg

THE first record of the discovery of iron ore in Missouri was Marquette's observation in 1673 of brown iron ore, or limonite, in the Mississippi River bluffs just north of the mouth of Apple Creek in southeastern Perry County. There is no record of any attempt to mine or smelt Missouri iron ores until 1815, when the Ashebran furnace was erected at the Stouts Creek shut-in near Arcadia, Iron County. Some limonite was treated in this furnace, the first iron furnace west of Ohio, but most of the ore was hematite from Shepherd Mountain and adjacent deposits. Eight years later, in 1823, the Perry furnace five miles north of Caledonia, Washington County, was constructed to smelt limonite ore. It

Jan 1, 1955