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By J. H. Frye, C. P. Sun

A Frimary substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced, solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver alloys.1-5 It has been shown that at least four factors are involved: (1) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2,4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work-hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. Calculation of Rates as Work- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

By A. Blake Caldwell

In 1936 the Ertsberg story began and its development is a classic example of the courage it takes to discover one mining prospect and bring it into production. Truly, the finding and working of this mine is a modern exception to the overwhelming odds every modern prospector must surmount to be successful. Today, it takes lots of time, plenty of money and the tenacity of a bulldog to whip the laws of nature. Ertsberg ("ore mountain" in Dutch) is literally an elliptically shaped plug of magnetite which erosion has exposed for 560 ft above ground level. The deposit has been likened to an ice cream cone with the outcrop the ice cream, which is above ground, and with the cone buried below the surface. Assaying about 2.5% Cu, the 33 million tons of ore also carry 0.025 oz Au and 0.265 oz Ag per ton.

Jan 1, 1970

By H. Foster Bain

[Secretary's NoTE.—This paper, presented in oral abstract at the San Francisco meeting, was not at first supposed by Mr. Rain to be required for publication in the Transactions; and the excursion to Japan, in which he took part, immediately after the San Francisco meeting, delayed his presentation of the manuscript. After his return to San Francisco, Mr. Bain, in view of the importance of his paper and its discussion, kindly furnished it in full. The delay in its publication (since it was received in April last) has been due, partly to the circumstance that other contributions had meanwhile acquired the " right of way," and partly to the consideration that, the situation contemplated in Mr. Bain's paper having remained practically unchanged, the paper and its discussion would not lose force or timeliness by this lapse of time.—J. S. ] No acute observer of public affairs can have failed to observe a growing disposition on the part of the public to change emphasis in government from political equality to social justice. When our own government was founded it was felt to be sufficient to secure to each individual the fullest possible freedom of opportunity, and such a scheme was excellently adapted to the rapid development of a large territory having a small population. As the number of people in a given area increases, there are more points of contact and conflict; each must move in a smaller orbit, and there must be more regula-

Jan 1, 1913

By A. A. Smith, J. S. Smart, A. J. Phillips

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By A. J. Phillips, A. A. Smith, J. S. Smart

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By Phillip J. Maddex, Ole Skaarup

The quite diverse backgrounds of the authors and their mutual interest in reducing transportation costs has produced some interesting innovations. A few words about their background will tell the reason for this joint paper. . . One is a shipping executive with a background of shipowning, ship management, ship and cargo brokerage and chartering, and most facets of the steamship industry, both American and International. The other is a chemical engineer, thoroughly brought up in the American chemical and mineral industries, with several top managerial positions behind him. They began cooperating when U.S. Borax was contemplating a change in its export shipping program and studying the freight cost for shipping borax from The mines in the Californian desert to Europe, and eastern U. S. markets. In the 20 Mule Team days, borax was exported in 50 pound bags. In 1960 it was still shipped in 50 pound hags. Three main products were shipped: two were anhydrous, and all three were sensitive to impurities. The products were bagged at the plant in the Mohave Desert, and shipped about 150 miles by rail to the port in Los Angeles. From Los Angeles, shipment was made by Conference steamship lines at Conference rates. Anyone who has shipped bagged material to Europe by steamer knows that the tab is anywhere from $20 to $30 or more per ton.

Jan 1, 1970

By A. G. Jordan, W. Jeitschko, Paul A. Beck

The occurrence qf the V phase structure /Zr,Co,Ge, type) in ternary syste7ns (titanium, zivconium, niobium, lanta1urn) -(nickel, cobalt, iron)-(silicon, germanium) was incestigated. Nine V silicides and four V gertrlanides were found and their lattice constants are reporled. The lattice constants of twenty-one preri-ously identified E phases (TiNiSi type) are given. The average atomic volumes of these phases are discussed in relation to similar binary phases. ThE occurrence of a phase Ti4Ni4Si7 was first reported by Westbrook. DiCerbo, and peat' who gave it the name "V phase". They also reported the existence of an E phase TiNiSi. Subsequently a systematic study was undertaken in this laboratory to explore the occurrence of E' and V phases3 in related ternary systems. In the meantime the crystal structure of the E phase TiNiSi 4 and of the V phase Zr4CO4Ge 75,6 was determined. In the present paper the details of the V phase investigation and the lattice constants of the E and V phases are presented. V PHASES Alloy specimens of approximately 10 to 15 g were prepared by arc melting under argon (99.996 pct Ar) atmosphere. The starting materials were all of purity higher than 99.9 pct, with the exception of cobalt. which contained 0.14 pct Fe as the only major impurity. The weight losses were in all cases less than 2 pct, in most cases less than 1 pct. The samples were encapsulated in fused silica tubes with sufficient argon to yield about 1 atm pressure at the annealing temperature. After the homogenization anneal. Table I. the specimens were water-quenched. A representative portion of each specimen was then examined metallographically (etchant: 20 pct HNO,. 10 pct HF. 25 pct glycerine, 45 pct H20). Only minor amounts of second- and third-phase particles were observed in the specimens listed in Table I, with the exception of alloys Zr4Fe4Si7 and Ta,Fe,Si,. which contained an estimated 10 pct by volume of foreign phases. X-ray powder photographs were taken with a Seeman-Bohlin type focusing camera and Fe-KO radiation. Of the thirty possible combinations of elements in the ternary systems (titanium, zirconium. vanadium. niobium. tantalum)-(iron. cobalt, nickel)-(silicon. germanium) thirteen V phases could be identified. In the remaining seventeen ternary systems and also in the systems Cr-Ni-Si and (M0.W)-(Ni.Co)-Si no V phase was found at the composition 4:4:7 after annealing at temperatures between 900" and 1200'C. For the determination of the lattice constants of the V phases Debye-Scherrer photographs were taken using the asymmetric film arrangement and CrKcr radiation (ka1, = 2.28962A). Using the positional parameters, as determined6 for Zr,Co,Ge,. Table 11. intensity calculations were carried out for each of the V phases with the aid of a computer program.: Thus unequivocal indexing of the diffraction patterns was greatly facilitated. The lattice constants. Table I. were then computed by a least-squares fit of the high-angle lines with f (0) = cos2 Q as extrapolation function. Only few. if any. very weak impurity lines were observed, with the exception of the three iron alloys Zr,Fe,Si7. Zr4Fe,Ge7. and Ta,Fe,Si7. The agreement

Jan 1, 1970

By Ruder, W. E.

CONSIDERABLE interest has been shown lately in various types of furnaces for the production of high, temperatures, both for laboratory purposes and for small industrial uses. Dr. J. A. Harker1 described certain modifications of the Arsem graphite resistance helix for high-temperature work at the National Physical Laboratory. Dr. Northrup ,also has developed two interesting forms of high-temperature furnaces. In 1911, Messrs. Winne and Dantsizen2 described two forms, of resistance furnaces using ductile molybdenum or tungsten as resistors. Since the discovery, by this laboratory, of methods for producing these metals in ductile form, their use as resistance elements in the research laboratory of the General Electric Co. has grown to such an extent that they are now almost indispensable. These furnaces are used here for alloy research, annealing, heat-treating, and practically all f the thermal processes requiring temperatures above 900° C. Various types of furnaces have been developed to meet the general needs of laboratory work, and it is the purpose of this paper briefly to describe some of these furnaces. A tubular furnace wound with a metallic resistor is the simplest type to construct, and almost every laboratory has made such furnaces. The only essential difference between a furnace wound with platinum or base metal and one wound with tungsten or molybdenum is that the coils of the latter must be heated in a neutral or reducing atmosphere. It has long been our custom here to build our resistance furnaces with a metallic casing from which the tube could be easily removed for rewinding. The heat-insulating material-usually calcined magnesia, alumina, silica, or silex, depending upon the nature of the resistor-is used in powdered form so that it can he readily removed and replaced. In order to adapt this method to tungsten or molybdenum windings, it

Jan 2, 1918

By John Hillman

Reconstruction of the British mining industry began shortly after nationalization in 1947 and continued until well into the 1950s with the support of the government. This support diminished as plentiful supplies of cheap oil from the Middle East made many coal mines uneconomic. The planned rundown which followed was foreshadowed in the 1965 White Paper which outlined financial measures to speed the closure of uneconomic collieries. The decline appeared likely to continue into the 21st century as the role of coal in UK energy requirements became less and less significant. This policy was well on course in 1973 when the oil crisis led to a complete reappraisal of the position. A government examination in 1974 of the coal industry then supported the National Coal Board's general strategy of major capital investment as set out in its 'Plan for Coal'. The plan was aimed at halting the intended decline in the industry's capacity and restoring it to 120 million tons of deep mined output in 1985. The plan proposed action along the following lines: Increase output by major investment in construction at existing collieries with sufficient reserves to give 13 million tons per annum extra output.

Jan 1, 1980

By Norman L. Newbern, Robert E. Green

An investigation of the effect of size on the deformation properties of metal single crystals made it desirable to grow from the melt cylindrical aluminum single crystals possessing exactly the same crystallographic orientation but varying in diameter. Methods for the growth of rather large (up to 3 in. diam) aluminum single crystals in molds of the desired shape are well known. However, when one applies the same techniques to the growth of smaller (less than 1/8-in. diam) specimens many additional problems arise. Two of the major problems are the construction of the molds to be used and the removal of the thin specimens from these molds without deformation after growth has been completed. Also the problem of the constraint forces exerted by the mold on the specimen is much more pronounced for the smaller specimens. The technique described herein is a zone-melting method in which no mold is used since the surface tension of the molten metal and its oxide is sufficient to retain the melt. The specimen is suspended vertically in a manner similar to that of Keck and Golay.2 However, while Keck and Golay supported the specimen from both ends, the method used here supports the specimen only at the upper end. The surface tension of the molten aluminum and aluminum oxide contains the melt and suspends a length of newly grown crystal that has already passed through the molten zone until the weight of the newly grown crystal is equal to the component of surface tension holding the specimen together in the molten region. When the weight of the newly grown crystal is equal to the component of surface tension holding the specimen together the specimen pulls in two in the molten zone. The length of crystal which can be grown before this separation occurs varies with the diameter of the specimen and the size of the molten zone. In order to prevent the specimen from pulling in two a tube of glycerine is placed beneath the furnace in such a manner that the newly grown crystal passes into the glycerine which provides sufficient buoyancy to allow aluminum single crystals in wire form to be grown to lengths determined only by the length of the tube containing the glycerine. A schematic diagram of the experimental arrangement is shown in Fig. 1. The furnace used is constructed as follows. High-resistance nichrome wire is coiled on a 3/8-in. diam fused quartz tube. The distance between the windings is much less over a length of about 3/8 in. at the center so as to develop a hot spot. This core is located in the center of a 4-in. diam steel cylinder 5 in. in height and insulated from it by Kayolite. The temperature of the furnace is controlled by means of a thermocouple located near the central hot spot and a Minneapolis-Honeywell temperature controller. Temperature ins,ide the furnace is measured with a thermocouple and a standard potentiometer in the usual manner. By the above method it is possible to grow high-purity (99.99 pct Al) aluminum single-crystal wires over a range of sizes. Crystals varying from 1/8 to 1/64-in. diam were grown by the authors. Since the tube containing the glycerine cannot contain a crystal longer than approximately 3 ft, the growth of crystals longer than this presents another problem. It was found that one could cut the newly grown crystal without deformation in the region between furnace and glycerine tube try means of a cutting torch and then by moving the glycerine tube slightly aside continue

Jan 1, 1962

By Henry M. Howe

Henry M. Howe, Bedford Hills, N. Y. (communication to the Secretary.)*—Mr. Johnson's explanation, that the rounding of the graphite masses in oxygen-bearing cast iron is due to their being in part reprecipitated after re-solution in forming carbonic oxide temporarily with.that oxygen, is certainly most attractive and suggestive. It remains to be shown whether this rounding occurs also when the solidification is too rapid to permit this process to go on. J. E. Johnson might easily test this by casting a single ladleful of his oxygenated iron in masses of varying size. If this present hypothesis is true, then the rounding ought to increase progressively with the size of the casting, and with the distance from the outside, that is to say with the time available for re-solution and reprecipitation. I question whether a like benefit is to be expected even on this hypothesis, from the oxygenation of steel. The spheroidizing of graphite does good because graphite itself is so weak. But the constituent which can be spheroidized in steel is its cementite, which is a source of strength. Lamellar pearlite, in which this cementite in effect forms long den-drites, is far stronger than divorced pearlite, in which these dendrites have been broken up into spheroids. Even the surfaces of contact between ferrite and cementite are probably sources of strength because of the amorphous iron which probably fills them.

Jan 1, 1917

By Richard P. Rothwell

THOUGH coal has been mined in this country for more than a century, no systematic effort was ever successfully made to ascertain the total amount produced. The production of the Cumberland Basin, Md., and the shipments from the anthracite fields of Pennsylvania, have been placed upon record, thanks to the intelligence sand foresight of Mr. C. Slack in the former case, and to the late Mr. B. Bannan in the latter. For some of the years between 1822 and 1842, the production of the Richmond Basin was reported by Mr. R. C. Taylor, but since that date till the author undertook this work it was impossible to obtain any statement of the production of this field. A few of the newer fields, such as that of Mt. Diablo, Cal., have been fully reported, and a few of the newer States have also had this service performed by some intelligent private individuals.; but no statistics of coal production have ever been collected either by the State or General Government, if we except the returns for the years 1869-70 of the census report. During the year 1875, by great exertions, I succeeded in obtaining, and July 3d, 1875, gave in the Engineering and Mining Journal what, "though not an accurate statement of our coal production," was " by far the most full and reliable that had ever been published." Though that report showed the production of bituminous coal to be 23,630,094 gross tons, or about six million tons more than had ever before been reported, it was in reality two and a half million tons below the actual output. The more full returns I obtained for 1875 gave many figures for 1874

Jan 1, 1877

By C. W. Hill, G. P. Luckey

In a previous article1 preliminary experiments were described, indicating the possibilities of a quantitative spectroscopic method for the determination of small amounts of lead in copper, which would be accurate and rapid, and could be carried out in the refining plant by one not skilled in chemical analysis. The present paper deals with the development of the method in the factory, giving the details of apparatus and its standardization, and presenting a comparison of the accuracy of the method with that of the standard electrolytic determination. (For variations and other applications of the method, the reader is referred to the first article.) A carefully weighed sample (0.4 gm.) of the copper to be tested is placed in a cavity in a graphite positive electrode. An arc capable of

Jan 1, 1919

By B. B. Wood, M. J. Rzasa, E. W. Hough

An apparatus for the determination of fluid-fluid interfacial tension by the pendant drop method has been constructed. The apparatus is refined beyond those previously described in that the samples are introduced into an evacuated windowed cell without contacting air or mercury. Interfacial tension data are reported for the water-methane system between 74 and 280°F and 15 and 15,000 psi. The variation of wettability of the stainless-steel dropper tip with pressure and temperature was observed incidentally to the measurements. INTRODUCTION The most refined previous apparatus --for the determination of fluid-fluid interfacial tension at reservoir conditions was built by Hauser and Michaels.' These authors used the pendant drop method, previously investigated by Andreas, Hauser, and Tucker.' Recently, Fordham3 has made the pendant drop method an absolute one by numerical integration of the differential equation of drop shape. It is necessary to know the difference in density of the two fluids and the acceleration due to gravity in order to evaluate the interfacial tension from measurements of drop dimensions. Contact angle is not involved in the measurements by this method. Some precise tests of the method have been made at atmospheric pressure and 77°F by Douglas," who found agreement with established values to within about 0.1 per cent for water and air, cyclohexane and air, benzene and air, and benzene and water. No values of interfacial tension from the recent pendant drop apparatusJ have been published by Hauser and Michaels. However, values for the water-benzene and water-decane systems are given in Michaels' thesis5 or Dressures from 15 .to 10,000 psi and temperatures from 73 to 268ºF. Some determinations on gas-oil and gas-water systems in the range of 15 to 4,000 psi and 78 to 178°F have been made by Hozott,' by the drop-volume method. The capillary rise method has been used to investigate the interfacial tension in gas-oil systems at 88°F to several thousand psi by Swartz.7 Other determinations in gas-oil systems at pressures under 1,000 psia have been made by Jones: and Beecher and Parkhurst.9 The scarcity of data for pressures above 5.000 psi is apparent. APPARATUS An assembly drawing of the working section of the interfacial tenqion apparatus is given in Fig. 2. 'The endanant drop (A) is housed in a pressure chamber having glass windows (B). An agitator (6) is provided. The metal parts of the apparatus coming into contact with the sample are made of AISI: Type 316 steel. Drain grooves are provided around the whdows so that the sample in contact with the O-rings is not returned to the working section when the pressure is reduced. A schematic arrangement of the apparatus is given in Fig. 3. The working section containing the pendant drop (A) is filled by samples from bombs (B) with the aid of the vacuum system (C). The O-ring sealed pistons (D) used to separate the sample from the hydraulic fluid are shown together with the pressure production and measurement system (E). A front view of the apparatus is shown in Fig. 1. Most of the hydraulic system is at the top of the panel. The pump and displacement piston are at the lower right. The Variacs for the air bath heaters. the camera. and the vacuum gauge are a1so visible on the panel. The working section together with a window closure and a drop-forming tip closure are shown in Fig. 9. The carbon arc light source with filter is visible in the upper part of the picture. Two sides of the air bath with the impeller and a part of the convection shield can also be seen. The assembled air bath is shown in Fig. 10.

Jan 1, 1951

By E. W. Hough, B. B. Wood, M. J. Rzasa

An apparatus for the determination of fluid-fluid interfacial tension by the pendant drop method has been constructed. The apparatus is refined beyond those previously described in that the samples are introduced into an evacuated windowed cell without contacting air or mercury. Interfacial tension data are reported for the water-methane system between 74 and 280°F and 15 and 15,000 psi. The variation of wettability of the stainless-steel dropper tip with pressure and temperature was observed incidentally to the measurements. INTRODUCTION The most refined previous apparatus --for the determination of fluid-fluid interfacial tension at reservoir conditions was built by Hauser and Michaels.' These authors used the pendant drop method, previously investigated by Andreas, Hauser, and Tucker.' Recently, Fordham3 has made the pendant drop method an absolute one by numerical integration of the differential equation of drop shape. It is necessary to know the difference in density of the two fluids and the acceleration due to gravity in order to evaluate the interfacial tension from measurements of drop dimensions. Contact angle is not involved in the measurements by this method. Some precise tests of the method have been made at atmospheric pressure and 77°F by Douglas," who found agreement with established values to within about 0.1 per cent for water and air, cyclohexane and air, benzene and air, and benzene and water. No values of interfacial tension from the recent pendant drop apparatusJ have been published by Hauser and Michaels. However, values for the water-benzene and water-decane systems are given in Michaels' thesis5 or Dressures from 15 .to 10,000 psi and temperatures from 73 to 268ºF. Some determinations on gas-oil and gas-water systems in the range of 15 to 4,000 psi and 78 to 178°F have been made by Hozott,' by the drop-volume method. The capillary rise method has been used to investigate the interfacial tension in gas-oil systems at 88°F to several thousand psi by Swartz.7 Other determinations in gas-oil systems at pressures under 1,000 psia have been made by Jones: and Beecher and Parkhurst.9 The scarcity of data for pressures above 5.000 psi is apparent. APPARATUS An assembly drawing of the working section of the interfacial tenqion apparatus is given in Fig. 2. 'The endanant drop (A) is housed in a pressure chamber having glass windows (B). An agitator (6) is provided. The metal parts of the apparatus coming into contact with the sample are made of AISI: Type 316 steel. Drain grooves are provided around the whdows so that the sample in contact with the O-rings is not returned to the working section when the pressure is reduced. A schematic arrangement of the apparatus is given in Fig. 3. The working section containing the pendant drop (A) is filled by samples from bombs (B) with the aid of the vacuum system (C). The O-ring sealed pistons (D) used to separate the sample from the hydraulic fluid are shown together with the pressure production and measurement system (E). A front view of the apparatus is shown in Fig. 1. Most of the hydraulic system is at the top of the panel. The pump and displacement piston are at the lower right. The Variacs for the air bath heaters. the camera. and the vacuum gauge are a1so visible on the panel. The working section together with a window closure and a drop-forming tip closure are shown in Fig. 9. The carbon arc light source with filter is visible in the upper part of the picture. Two sides of the air bath with the impeller and a part of the convection shield can also be seen. The assembled air bath is shown in Fig. 10.

Jan 1, 1951

By John G. Baragwanath

THE September issue of the Engineering and Mining Journal carried an item regarding the Cercapuquio Mining Co. which was mentioned as a large producer of lead, zinc, and cadmium, situated near Huancayo, Peru. The paragraph caught my eye because I had not heard of the property in thirty years and I recollect all too well the circumstances of its accouchement. In 1916 1 was making my headquarters in the town of Huancayo, then the terminus of the Central Railway of Peru, and was examining mines and prospects in that general area for Cerro de Pasco. In the course of my work I became acquainted with an engaging and energetic "practical" miner named Balarin, a Dalmatian living in Huan¬cayo, and made numerous trips in his excellent company. One day Balarin came to the down-at-heels hostelry where I stopped and told me that a Cholo prospector, a character by the name of Jose, had just reached town and claimed to have made a discovery in a little known locality called Cercapuquio. Lead-silver, Balarin said, and showed me a sample of galena about the size of his fist. "Fine," I remarked. "When do we leave?"

Jan 1, 1947

By H. E. Cline, D. F. Stein

A fine lamellar structure with interlamellar spacings ranging from 0.I to 3.7 was Woduced by high-speed directional solidification and used to study the interaction of dislocations with an array of bimetallic bound-am.es. The tensile flow properties were measured at elevated temperatures and the results interpreted in terms of an image force model. As the width of the plates decreases the strength increases according to a Hall-Petch relation, suggesting pile -ups. Considerable strengthening was also observed at elevated temperatures. In recent years composites containing a strong but brittle phase and a ductile but weak phase have been studied extensively in the search for a high-strength material with adequate ductility.' However, the strength of these composites has been limited to a volumetric average of the strengths of the component phases. In this paper we will show that a composite made by directional solidification of a Cu-Ag eutectic has strength properties that substantially exceed the strength of either of the metals in the composite, and an explanation for this increased strength will be presented. The Cu-Ag eutectic is a near ideal material to study for several reasons. The eutectic structure is made up of alternate plates of silver-rich and copper-rich phases with the same crystal structure.2'3 In addition, the mechanical and elastic properties of silver4 and copper5 are known over a wide range of temperatures and the eutectic microstructure is stable to nearly the melting point.6'7 Therefore, the properties of the eu-tectic are readily comparable to various theories involving the mechanical properties of copper and silver. The experiments consisted of producing directionally solidified Ag-Cu eutectic material, determining the structure and performing tensile tests at different temperatures and strain rates. EXPERIMENTAL A) Solidification and structure. A cylindrical ingot 2.2 cm in diam and 15 cm long was prepared from 99.999 pct pure materials and cast in argon. The ingot was placed in an alumina crucible and was direc-tionally solidified at 7 x 10"4 cm per sec in a Bridg-man apparatus in argon. Metallographic examination at both ends and along the length of the ingot showed a uniform structure that consisted of fine alternate plates of silver- and copper-rich phases. The plates were aligned parallel to the growth direction, as shown in the longitudinal section, Fig. 1, and were in small randomly oriented domains of parallel plates as viewed in a transverse section, Fig. 2. Four smaller ingots 0.175 in. in diam were solidified at speeds of 2Xlo-', 4.4 xlo-', 4.4 x 10-3, and4.4x10-4 cm per sec to produce a range of lamellar spacings. Replica electron micrographs were taken to resolve the individual plates as shown in Fig. 3. The copper-and silver-rich plates in the larger ingot were about

Jan 1, 1970

By C. W. Washburne

THE waters of many oil fields have been regarded as buried sea water which has been retained in the sediments since the time of their deposition. The preservation of connate water through geological time has seemed improbable to only a few geologists, but there is room for doubt that buried sea water could remain in the strata during their periods of deformation and during the many subsequent epochs of. the circulation of meteoric ground-water. Some have even suggested that the calcium chloride water in the deep mines of the Lake Superior region is ancient sea water buried in the Algonkian lavas, but it is hard to understand how such water could be derived from the highly sodic and sulphatic water of the sea. It would seem more plausible to connect the calcium chloride with the highly calcic magmas of the greenstones in which it is found. Chemical analyses of waters associated with oil differ widely from the composition of sea water, requiring extensive alteration of the latter, if the former is truly its derivative. The first notable difference is the general absence of sulphates from oil-field waters, but this has been explained satisfactorily through reduction by hydrocarbons and organic matter. Oil reduces sulphates with the production of hydrogen sulphide (or sulphur), water, and carbonates (or carbon dioxide). The second striking difference is in the high ratio of chlorine to sodium. An examination of the analyses of chloride waters from oil fields shows that they contain a large relative excess of chlorine over that in sea water. Moreover, there is difficulty in finding chemical reactions that are probable in nature, by which sea water could be converted into anything like the chloride waters of oil fields. In the latter a large part of the chlorine occurs as calcium acid magnesium chloride. This condition might be produced by the removal of sodium carbonate, which; however, cannot be precipitated in the presence of much calcium or, magnesium.

Jan 3, 1914

By Donald E. Meyer

High current-low voltage EB-gun evaporation in an oil-free ultra-high vacuum system was found to be necessary, though not sufficient, for stability (300°C, 106 v per on) of aluminium gate MOSFET's and MOS capacitors not stabilized by a phosphorous glaze. five characteristics of the equipment used: 1) Vacuum purification of the aluminum charge, 2) Ionization of the evaporant by the electron beam, 3) X-ray formation, 4) Residual gases during evaporation, and 5) Metal film structure were studied as Possibly significant in MOS fabrication. EVAPORATION of contact metals common to the semiconductor industry historically has been accomplished with oil diffusion pump systems and various resistance heated evaporant sources as dictated by the type of metal evaporated. To meet a need for greater reliability of semiconductor devices, other metallization methods were developed. A good example would be application of the moly-gold contact system to integrated circuits with deposition by RF or triode sputtering.' More recently, fabrication of stable metal-oxide-silicon devices and circuits has put new demands on metallization. The purity of the thin metal films composing MOS structures is critical, particularly at the metal-oxide interface, and ultra-high vacuum metallization using sputter-ion pumping and electron beam gun (EB-gun) evaporation are well suited for the task. At this laboratory aluminum has been the most common contact-gate metal for both MOS capacitors and MOSFET's. In the earliest work with MOS capacitors, aluminum was evaporated from wetted tungsten filaments using both diffusion pump and ion pump vacuum systems. In spite of clean oxide techniques these capacitors were unstable under bias-tempera-ture stressing. Only after a switch to EB evaporation of aluminum were stable capacitors produced. Using the same techniques it was possible to make MOSFET's with equivalent stability. Stability data for a discrete MOSFET is shown in Fig. 1. This is a "clean" oxide gate (no phosphorus stabilization or no etch back of a thicker gate) having a thickness of lOOO? thermally grown on the (111) plane. Gate length after diffusion was 0.24 mils, and the devices were hermetically sealed. Stressing conditions were 300°C and 106 v per cm applied alternately as a positive and negative field for 10 min, 50 min, and 4 hr for a total stress time of 10 hr. An initial shift in turn-on voltage of 0.1 v was detected for 10 min of positive bias. All evidence at this laboratory indicated that while EB-gun evaporation of ultra-high purity aluminum was not sufficient for 300°C stability, it did seem to be necessary. There may well then be something inherent in the EB-gun deposition used which enhanced stability, and probably no single factor existed but rather a series of factors. It is the purpose of this paper to report on some of the investigations carried out to learn more about EB-gun evaporation in ultra-high vacuum systems. EXPERIMENTAL DESCRIPTION The EB-gun was self accelerated, had a maximum power rating of 10 kw, and used a water-cooled copper crucible able to hold a 20-g aluminum charge. The electron beam was bent 180 deg and focused by an electromagnet which also provided movement of the beam across the crucible. Normal power conditions in this work were 9 kv and 300 to 600 mamp. The gun can be described as high-cur rent/low-voltage and was quite different in its mechanism of operation from EB-guns with much higher acceleration potentials. An oil-free vacuum system capable of 5 x 10- l0torr, a quartz crystal rate and thickness monitor and a quadruple mass spectrometer completed the evaporation system, Fig. 2. A typical evaporation cycle consisted of a 3 to 4 hr pumpdown to the upper l0-9 range and evaporation at l0? per sec with the pressure in the bell jar not rising above 1 x 10"7 torr. Thickness control was 5 pct or less and could be automatically monitored and controlled. Five phenomena associated with the EB evaporation and considered as possible contributors to Ma performance included a purification effect, ionization of evaporating aluminum, X-rays, constitution of vacuum ambient during evaporation, and film structure dependence upon evaporation rate. These phenomena are now discussed. Vacuum Purification. The design of the EB-gun permitted purification of the aluminum charge by vacuum outgassing. Particular features included an efficiently water-cooled copper hearth with a capacity of over 20 g of aluminum and the capability for sweeping the beam across the charge. Such capacity meant that aluminum had to be added only after about every fifth evaporation. A new charge was not required each evaporation as is necessary with filament evaporation. An oxide "scum" which appeared on the charge could be completely cleared from the top hemisphere of the charge by sweeping with the beam prior to opening the shutter. An indication of the purifying effect was obtained by a series of analytical measurements on incoming aluminum, after melting but with little vacuum out-gassing, after 30 min outgassing, and the evaporated film itself. Either a solids (spark source) mass spectrometer or an emission spectrometer were used for analyzing the aluminum charge. Analysis of the evapo-

Jan 1, 1970

By Dart Wantland, C. A. Heiland

There once was a little kid, whose lot was a very tough one until he grew up. His parents did not have much in common; from all indications, it is probable that the child was not wanted. His father Geology and his mother Physics separated shortly after his birth, which occurred during the World War amid a smoke screen of mathematics. He was kicked around a great deal. His parents could not agree on a name, and they finally christened him "Geophysics," for short. His relatives insisted that the name should be "Geophysical Prospecting," "Geophysical Exploration" or "Exploratory Geophysics"; though the youngster has grown up by now, this battle is still going on. His father did not think the child would amount to much until he began to show some unexpected talents, which were acquired, no doubt, from his mother Physics. His progress caused his father no little worry, and he began to wonder whether his offspring would help him in his business when he grew up or would set up shop in competition with the old man. His aunt Petroleum watched his growth with benevolent interest; his uncle Mining remained rather skeptical and cousin Civil Engineering not only assumed the attitude of the man from Missouri but was not much convinced even after he had been shown. Making a long story short, the kid decided that he had to stand on his own feet and get along as best he could. Having come from a good family he possessed some outstanding characteristics such as resourcefulness and a reasonable amount of business ability. He therefore decided that it would be to his advantage to follow in his father's and mother's footsteps as much as possible, and develop the good qualities of both. As a result, the youngster did fairly well for himself, and his relatives decided that it might be to their advantage to be on better terms with him. Father Geology had come to the conclusion that the boy could be very helpful to him and now wanted him to live in his house. His mother, who had brought him through the teething and measles stages, felt quite capable of bringing up the boy without the help of his father; and, as the fairer sex will do, would confide to a neighbor every now and then that his

Jan 1, 1940