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By James Fisher

THE copper mines of the Keweenaw Peninsula in northern Michigan have long been of interest in connection with deep earth-temperature measurements. The extraordinary low geothermal gradient of 1° F. in 223.7 ft. announced by Agassiz1 as a result of measurements dating from 1886, although later" stated as in error, served to focus attention on this region as one offering, because of the great depth of the mines, unusual opportunity along this line. Lane,3 Van Orstrand4 and others have made valuable contributions to this study. Fresh opportunities afforded by the constant deepening of the mines, improvements in the accuracy and reliability of temperature-measuring instruments together with increasing knowledge of the heat conductivities and specific heats of the rocks, led the Michigan College of Mining and Technology in cooperation with some of the mining companies to renew work on this problem. It is planned eventually to complete a survey which will make use of the favorable opportunities for deep rock-tempera-ture measurements presented in these mines. This survey should include the determination of a depth-temperature gradient in both conglomerate and amygdaloid mines, and also the variations in temperature at the same depth in different geological formations. The first problem has a direct bearing on the question of providing equipment for necessary ventilation with increased depth. The second may show that a relation exists between the natural rock temperature and the mineral content of the formation.

Jan 1, 1932

By Wendell E. Dunn

INTRODUCTION The early history of the chloride process has been recorded in a chapter of a Bureau of Mines bulletin (9 by one of the inventors of a chloride process, Stewart Croasdale, who is famous for the Pohle- Croasdale Process. The earliest use of chlorine in metallurgy was in 1557 by Bartholome Medina. But apparently even earlier there was knowledge that salt could be used in gold and silver extraction because a treatise, de la Pyrotechnica, published in 1540 in Venice, asserted that silver could be obtained from its ores by a wet salt process. In 1609 a priest, Alonzo Barba, invented a process using a copper vessel and boiling a solution of salt to extract silver chloride ores. The copper vessel was, of course, one of the reactants. This led to the Kronke process introduced in Chile in 1860 which substituted cuprous chloride for the kettle. A major step was taken in Europe in the late 1700's to chloridize roasted silver ores in combination with amalgamation using iron to reduce the silver chloride. By 1843 the Augustan process was introduced. Ores were roasted with salt and leached with a saturated salt solution. The silver chlorides passed into solution from which silver was precipitated by copper. In 1848 sodium or calcium thiosulfate solution of silver chloride was suggested by Dr. John Percy, and the idea was applied in 1856 by Von Patera in Bohemia.

Jan 1, 1983

The Library of .the above-named Societies is open from 9 A.M. to 9 P.M. on all week-days; except holidays, from September 1 to June 30, and from 9 A.M. to 6 P.M. during July and August. The Library contains about 55,000 volumes, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library can render valuable service through correspondence; letters requesting information will receive special attention. The Library is prepared to furnish references and copies of articles on mining and metallurgical subjects; to determine the existence of mining-maps, and to furnish general information as to the geology and mineral resources of all countries. All communications should be made as definite as possible so that the information received may he what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable shape. The members of the Institute can be of service to the Library by forwarding copies of mining-reports, maps privately issued, and similar material, which will be classified, indexed, and made available to other members. Suggestions for additions to the Library, either by purchase or personal solicitation as gifts, will be welcomed. It is hoped that members while in the city will use the Library freely, and assurance is given that most careful service will be rendered to them.

Jan 6, 1913

By Jamie Deuel

The a ad on Connection" For the purpose of this paper, we will concentrate on the ubquitous radon gas as the principle, low-level radiation effect from uranium tailings piles. Standards are also proposed for gamma radiations but, by most accounts, this is much less of a low level problem than is radon. I am also aware of some just completed research at Oak Ridge National Laboratories that suggest polonium may be a major concern in tailings, but those data are preliminary at this time. What is radon gas? In the first place it is not a gas in the accepted sense in that it has no driving pressure head. It might prove a more convenient description to call it radon vapor. Radon vapor, then, is 7-1/2 times heavier than air. Radiologically, it is an alpha emitter which means it spontaneously gives off high ionizing potential but low penetrating power particles. In fact, the alpha particle has such low penetrating power that this sheet of paper will completely shield a person. The problem, though, is breathing the radon decay products, called radon daughters. If radon daughter products are ingested into the lungs, their alpha emissions may cause cancer. The principle carcinoma associated with breathing radon, or more basically, associated with radiological effects is oat cell car- cinoma of the undifferentiated mall cell type. Radon has a 3.8 day half life which means in less than four days half of its initial radioactivity has decayed away. In less than a month it essentially becomes inert or non-radioactive. The Tailings Situation The NRC, in its April 1979 Generic Environmental Impact Statement

Jan 1, 1983

By Allen F. Agnew

Detailed stratigraphic studies in the Wisconsin-Illinois-Iowa district have made it possible to map the folds and faults that controlled the deposition of the zinc-lead ore. Prospecting on the basis of this mapping and prospecting in lower zones that are potentially ore-bearing have led to discoveries of ore. GEOLOGIC studies for the Federal and State governments in the Wisconsin-Illinois-Iowa zinc-lead district were begun in 1835, and subsequent surveys were made in the three states at intervals until 1916, see Table I. The current study of the district, Fig. 1, by the U. S. Geological Survey was begun in 1942 in the hope that a systematic investigation would help increase production of zinc and lead, then in extremely short supply. Major emphasis of the USGS program was on detailed mapping of the geologic structure and ore deposits. Preliminary maps and reports covering localities of intensive mining activity have been published during the course of this study, Fig. 2. By 1950 the objectives of the study by the USGS were revised; 71/2-min quadrangles of relatively unprospected localities as well as intensively mined localities are now being mapped in Wisconsin. Since 1945 the investigation in Wisconsin has been made in cooperation with the Wisconsin Geological and Natural History Survey, and since 1951 the geologic mapping of areas of particular interest in Iowa has been performed in cooperation with the Iowa Geological Survey. At intervals since 1943 the Illinois State Geological Survey has mapped the geologic structure and ore deposits of localities in the Illinois part of the mining district, see Fig. 2. Geology was applied by mining company personnel as early as 1853, but only sporadically, with periods of greater application between 1890 and 1925. Much of the so-called geologic work was in reality mining engineering. Since 1946 the major mining companies in the district have employed geologists who have successfully applied geologic techniques in the search for ore. History of Mining Occurrence of galena in the district was known as early as 1658 or 1659, when French explorers heard of lead mines that were apparently in the vicinity of Dubuque, Iowa. In 1690 a trading post was established near Dubuque to obtain galena. The first significant attempt at mining by white men took place in 1788 when the Indians granted to Julien Dubuque mining rights for 20 miles along the west side of the Mississippi River, including the vicinity of Dubuque, Iowa. By 1805 lead was being mined near Galena, Ill. In 1819 permanent settlement of the region was begun, and most of the important lead-producing areas had been found by 1830, see Fig. 3. Lead production in the Wisconsin-Illinois-Iowa district between 1830 and 1871 far exceeded that of any other district in the U. S.' Smithsonite was first mined in 1859, and sphalerite was mined as early as 1867. After 1873 the production of sphalerite exceeded that of smithsonite. In 1873 annual zinc production from the district first equaled lead production, and from then until 1893 production of zinc and lead was roughly the same. Since 1893 the ratio of zinc to lead mined has generally ranged between 5:l and 20:l. In 1942 the Wisconsin-Illinois-Iowa zinc-lead district ranked 14th among zinc-producing districts of the U. S. From 1946 until February 1953 the dis-

Jan 1, 1956

By Edgar G. Hill

MUCH has been written and said recently about the methods used and materials and equipment employed in building the long tubes that criss-cross a great part of the [ ] united States, like the pattern of a spider's web. This paper will discuss the fundamentals of design of these lines from the economic as well as the engineering view-point, pointing out the effect of the volumes transported, and the load factor at which they are operated, on the unit costs of transportation, as well as the effects on costs of the character of the fluids the lines are called upon to handle. Generally speaking, crude-oil pipe lines carry oil from the producing fields to the [ ] refineries. Sometimes part of the journey is by pipe line to a coastal point and tank ships are employed for the rest of the trip. The main lines of directional flow of crude oil through pipe lines in the United States are shown on Fig. I, but this, of course, does not always show individual pipe lines. BASIC FORMULA FOR FLOW OF CRUDE OIL The laws governing the flow of crude oil through pipes are well known. The basic

Jan 1, 1942

By Horace Pops, Jorge E. Kittl

In a recent study' of the martensitic transformation of Cu-Zn ß-phase alloys, it was noted that the MS temperature at the surface was raised due to the loss of zinc by volatilization. It seems likely, therefore, that the MS temperature may serve as a guide for the measurement of composition. From a knowledge of the dependence of the transformation temperature on composition, 2 it should be possible to detect variations in zinc content which are less than 0.1 at. pct by measuring the MS temperature throughout the sample. It is unlikely that an electron microprobe analysis could detect accurately such small zinc losses because the presently accepted limits of accuracy of the micro-probe analysis in simple ternary systems are of the order of 2 to 5 pct of the amount present.3 In the present study, a composition gradient was produced by precipitating the a primary solid solution, and reheating for a very short time within the ß-phase field. The nominal composition, in atomic percent, of the ternary ß-phase alloy used, 64.2 Cu, 34 Zn, 1.8 Si, was selected because it had an MS temperature of +4°C, thereby simplifying the experi-

Jan 1, 1968

By H. W. Mossman

Three aspects of magnetite smelting are discussed. The first is the working out of equilibrium conditions for eliminating sulfur. The second is the influence of magnetite solubility on the difficulty of tapping the reverb matte. The third is an approximation of the equilibrium conditions in the reverb gases which govern whether magnetite is mode or reduced in the reverb slag by these gases and by any iron sulfide in the slag. MAGNETITE has had a varied history in the Hurley Smelter since its start in 1939. Magnetite determinations on the smelter products are made regularly only on the monthly composite samples. Variations on the monthly averages are shown in Table I. Magnetite which drops from the slag and matte in the reverb has some slight bottom buildup which comes and goes, but no substantial accumulation from this source has been found at the end of a normal nine months' furnace campaign. However, there has been some low grade magnetite bearing material mixed with considerable A1,0,, which has slid down from the bottom of the sloping flue between the reverberatory furnace and the waste heat boilers. This accretion has required drilling and blasting near the skimming end of the furnace. The magnetite has interfered with tapping at times. When the smelter was first started, tapping trouble from magnetite was extremely severe. Increasing the reverberatory furnace temperature by putting in an air preheater and a Dutch oven has helped greatly, although there still is occasional tapping trouble. When the present series of physical chemistry articles on copper smelting started coming out in 1950, they were read with interest, but no immediate application was seen for them. Results of some laboratory work in 1952 aroused a much stronger interest in this physical chemistry. A series of melts was made on some converter slags, which had magnetite in very large grain sizes, with the object of reducing the grain sizes in the slag, as it was known that it was easier to handle in the reverb in that condition. Anything done in the tests greatly reduced the grain sizes—even in the controls, where nothing was done except melt the slag and cast it. There was more magnetite in the slags after the tests than before, and with wide variations. There were no obvious reasons lor much of what happened in these tests. Much of the base material published in English in this field was made available for study. Recalculations were made on many of the type problems, and part of the data was reduced to local temperatures and compositions. Explanations were found for what happened in the 1952 series of tests on converter slags, and the same principles turned out to be a description of much of what magnetite does in the reverb. This article is to present the results of that study, from the viewpoint of applying the technical material in definite numerical form to the operating conditions in both the converters and the reverberatory furnaces at the Hurley smelter. Table I. Magnetite Variations on Monthly Averages, 1939 to 1955 Pet Magnetite Lowest Highest Average Converter slag 13.6 43.3 25.4 Roverb slaa 2.7 20.9 8.7 Matte 28 15.9 98 In general it was found that magnetite is made or reduced in both the converters and the rever-beratory furnace, depending on variations of temperature, matte composition, and reverb gas composition occurring in ordinary plant operation. Within reasonable limits, the field conditions for formation or reduction can be predicted, and probably can be set up and maintained. Converter conditions affecting magnetite formation can be put into numerical values better than for the reverb from purely technical calculations. The converter can be operated so as to keep the magnetite in the slag down to between 12 and 14 pct and still give satisfactory life for the converter brick. This depends upon having converter flux available which will make a slag with a good separation without raising the temperature too high. In the Hurley reverb and others with similar conditions, it is likely that a compromise of conditions will give a reasonably good control of combustion and still keep the magnetite from building up on the bottom. This discussion consists of three main parts. The first is the working out of the equilibrium conditions in the converter for determining in which direction the reaction 3 Fe,,O, (s) + FeS (1) F? 10 FeO (1) + SO, will go under actual converter operating conditions. The second deals with the influence of the solubility of magnetite in the slag and matte in the reverb on the difficulty of tapping matte. The third is an approximation of the equilibrium conditions in the

Jan 1, 1957

By A. B. Young

IT is the he object of this paper to describe a Cottrell treater that was placed in operation, in April, 1919, at the Tooele plant of the International Smelting Co., for the purpose of recovering solids from the gases from the McDougall roasting furnaces. Fundamentally, the treater is simply a flue containing rows of vertical plates, forming the grounded electrode, alternated with rows of small horizontal pipes, forming the negative electrode, with proper provision underneath for taking away collected dust. There are advantages in construction over the more cumbersome types, both the vertical-tube and the vertical-box, particularly in the elimination of heavy supporting columns and massive foundations, giving a much lower first cost. There are no right-angle turns to interfere with gas distribution; consequently there is greater efficiency, or, in other words, a greater volume of gas per minute can be effectively treated. Another advantage of the horizontal installation over the vertical is that the principle of the selective precipitation of the various components of the dust and fume as they pass along the electric field may be utilized. Since the treater has been placed in operation, the results have been quite satisfactory and, in many ways, particularly in regard to the volume of gas that may be treated, have greatly exceeded expectations.

Jan 8, 1920

By R. Jr. Schuhmann

PROBLEMS in expressing, interpreting, and using size-distribution data recur in many phases of mineral dressing; therefore it is desirable that size analyses be ex-pressed in such a form, either numerically or graphically, that comparisons can be made readily. The size distribution of comminuted material is a result of a specific physical operation on the material and therefore should be governed by some definite physical principle, or cause-effect relation. Although this principle has not been dis-covered, it has been found that the size distribution of comminuted, homogeneous solids may be expressed by relatively simple mathematical equations. Two equa-tions in particular, proposed by Gaudin1 and by Rosin and Rammler,2 respectively, have stood out, both having wide demon-strated ranges of application. The form and the method of application of the two appear almost irreconcilably different on the surface, but, as will be shown, they are asymptotic in the fine sizes when expressed in the same units. This paper gives the results of a further study of the Gaudin and Rosin-Rammler relations, made with the object of develop-ing a form of size-distribution equation that will be more usable and more signifi-cant-particularly in comminution studies, both for interpreting the nature of size distribution and for evaluating surface. The work is summarized in the following:

Jan 1, 1940

By Elwood G. Haney, R. N. Parkins

Stress corrosion cracking of two heats of 18 pct Ni maraging steel in rod form immersed in an aqueous solution of 0.6N NaCl at pH 2.2 has been studied on un-notched specimens stressed in a hard tensilf machite. Austenitizing temperature in the range 1830 to 1400 F has been shown to have a marked influence on the propensity to crack, the loulest austenitizing- temperature producing the greatest resistance to failure. In the nzosl susceptible conditions, the cracks followed the original austenile grain boundaries; but when tlze steels zcere heal treated to inproze their resistance to stress corrosion, the cracks becatne appreciably less branched and slzouqed significant tendencies to become trans granular. Electron metallography of the steels indicated the presence of snzall particles, possibly of titanium carbide, along- the prior austenite grain boundaries and these particles u:ere more readily detectable in the structures that were most susceptible to cracking. Crack propagation rates, which appeared to be dependent upon applied stress and structure, were usually in tlze reg-ion of 0.5 mm per hr and may, therefore, be e.xplained on tlze basis of a purely electrochetnical ,nechanism. However, there is some ezliderzce from fractography that crack extension may be assisted by ttlechanical processes. Anodic stit)zulation reduced the tiwe to fracture, although cathodic currents of small magnitudes delayed cracking-; further increase in cathodic current resulted in a sharp drop i,n fracture litne, possibly due to the onset of hydrogen ewbrittlement. THE use of the high strength maraging steels, with their attractive fracture toughness characteristics, is restricted because of their susceptibility to stress corrosion cracking in chloride solutions. Although this limitation has resulted in investigations of the stress corrosion susceptibilities of these steels, there have been few systematic studies aimed at defining the various parameters that determine the level of susceptibility. It is the case that the usual tests have been performed with the object of defining some stress or time limit, on unnotched or precracked specimens, within which failure was not observed,' but while such results may be of some use in design considerations, they are necessarily concerned only with the steels as they currently exist and not with their improvement to render them more resistant to stress corrosion failure. This omission may be considered unfortunate because the indications are that stress corrosion in maraging steels shows dependence on structure in following an intergranular path, and since experience with other systems of intergranular stress corrosion crack- ing is that susceptibility may be varied by modifying heat treatments, a similar effect may be expected with maraging steels. It is sometimes from such observations that a fuller understanding of the mechanism of stress corrosion crack propagation begins to emerge, leading in time to the development of more resistant grades of material. The present work was undertaken to study only one aspect of the influence of heat treatment upon the cracking propensities of the 18 pct Ni maraging steel, namely the effect of austenitizing temperature, although certain ancillary measurements and experiments have been undertaken. EXPERIMENTAL TECHNIQUES Most of the measurements were made on a steel, A, having the analysis shown below, although a few results were obtained on a steel, B, having a slightly different composition. Both steels were supplied in the austenitized condition, A as 3/8-in-diam rod and B as 1/2-in.-diam rod. Cylindrical tensile test pieces were machined from the rods: the overal length was 2 1/2 in., the gage length 1 in. and the diameter 0.128 to 0.136 in. The stress corrosion tests were carried out with the specimens strained in tension in a hard beam testing machine, the necessary total strain being applied to the specimen over a period of about 30 sec, after which the moving crosshead was locked in position and the load allowed to relax as crack propagation proceeded; the load relaxation was recorded. The load was applied after the specimen had been brought into contact with the corrosive solution, the latter being contained in a polyethylene dish having a central hole through which the specimen passed, leakage being prevented by the application of a film of rubber cement. The specimen was in contact with the solution for over half of its gage length and the solution was exposed to the air during testing. The solution was prepared from distilled and deionized water to which NaCl was added, 0.6N, and the pH adjusted to 2.2 by HCl additions. The composition of the solution

Jan 1, 1969

By H. W. Graham

[ ] Even though we have a small audience, I am sure there are some here who are interested in sponge iron. It is a large subject, with a lot of economic interest, and one that will continue to grow in importance as the years go by and as the conditions that urge action in that direction increase. The authors have chosen to deal in this paper with one particular narrow phase of a long program of work by the Bureau of Mines. Before asking for any general discussion, I would myself like to ask Mr. Buehl if he would tell us just a little bit about the mechanism of discharge and the form in which the material was discharged; that is, when dolomite is added, what happens to the dolomite? R. C. Buehl (author's reply)-You are interested in the equipment that was used? H. W. GRAHAM-No, just the product. R. C. Buehl-The product was in granular form, of a shape very similar to that of the ore used. Using minus 10-mesh ore, the product is essentially minus 10-mesh, mixed with the coal and dolomite. It is then passed through a belt type of magnetic separator, which picks up the magnetic iron and allows the dolomite and coal to fall off. If the coal is sufficiently valuable, it can be separated from the dolomite and, provided the coal has a sufficiently low ash content, it can be reused. For instance, if a low-ash reducing agent like petroleum coke is used, it can be reused until all the carbon is consumed. H. W. Graham-That clears the point for me. I was not quite sure whether the experi-

Jan 1, 1947

By William Fink

THE investigation of aluminum alloy systems prior to 1923 was severely handicapped by the low purity of the best aluminum available. However, by that time, the electrolytic purification of aluminum had been developed by the Aluminum Company of America,(1)? and in May, 1923, there was initiated, under the direction of E. H. Dix, Jr.,(2) a program for the investigation of the aluminum-alloy systems using the purest electrolytically refined aluminum. Up to the present time 15 papers (a) have been published, most of which are on the binary aluminum systems. Work is now in progress on the ternary systems, and it seems probable that most of the future work will be on ternary systems. Therefore this survey of the binary aluminum systems investigated up to the present time (the sixteenth paper of the series) concludes the first phase of this program. Certain qualitative relations between corresponding portions of the various binary diagrams as well as between different parts of the same diagram were noted some time ago by R. S. Archer.(4) In the present . paper these relations and others are considered quantitatively by the application of well-known thermodynamic equations or by newly discovered empirical relations No attempt will be made here to present the history of the develop-ment of the thermodynamic equations defining equilibrium or their application to metallic systems, although a list of references is given at the end of this paper for those who are interested in this phase of the

Jan 1, 1934

By R. P. Agarwala, M. S. Anand

Using residual activity technique, the diffusion of palladium, silver, cadmium, indium, and tin in alunzinum has been studied in the temperature range of 400" to 630°C. The diffusivities (in units of square centimeters per second) have been expressed as: IMPURITY diffusion in aluminum,1-9 silverand lead5 for cases of low solid solubility of the impurity in the host metal has yielded frequency factors in the range of l0-6 to l0-9 sq cm per sec whereas the activation energy is practically half the self-diffusion activation energy value. From the observed values of frequency factor, activation energy, and entropy of activation, it has been suggested' that these solutes are not diffusing by vacancy or interstitial mechanisms but by a mechanism which should be consistent with such low values of the diffusion parameters (Do and Q). However in spite of extensive work on these types of systems, the mechanism of diffusion is still not well understood. The present investigation on the diffusion of palladium, silver, cadmium, indium, and tin in aluminum has been carried out to throw further light on the diffusion mechanism in systems, where the solid solubility is very low (except for the case of silver). The results are discussed on the basis of solid solubility and the structural changes involved owing to the presence of the solutes in aluminum solid solution. An attempt has also been made to apply the existing theories of charge5-8 and size8 difference between the solute and the solvent. EXPERIMENTAL PROCEDURE Specimens (1/2 in. diam by 3/8 in. high) were machined out of pure aluminum (99.995 wt pct) rod obtained from Johnson Mattheys. They were sealed under vacuum in quartz tubes and annealed at 620° C for several hours; the grains thus developed were sufficiently large to eliminate the possibility of diffusion along the grain boundaries. The flat ends were prepared carefully after polishing as described previously,10 Radioactive nitrates of cadmium, indium, and tin and chloride of palladium containing, respectively, cd115, 1n114, sn113, and pd103 were dissolved in distilled water and mixed with 30 pct acetone. By means of a micropipet a drop of this solution was placed on a smoothly polished and lightly etched surface of the specimen. Due care was taken to see that the solution spread uniformly on the surface of specimen without trickling down its sides. Radioactive silver was elec-trodeposited using a AgCN-KCN bath. The amount of sample deposited in all the cases was not more than 0.1 µ thick. The samples were then sealed in quartz tubes in vacuum. The cadmium samples were sealed in a purified argon atmosphere to avoid evaporation. The samples were then diffusion-annealed. The temperature of annealing varied between 400° and 630°C and was controlled to ±5°C. On heating to -400°C,the deposits of cadmium, indium, and tin, which were of the order of 0.1 p in thickness, were converted to their respective oxides. The contribution of oxygen present in the lattice of aluminum due to these oxides has been calculated and found to be less than 10 ppm in all cases. Oxide method has already been used by other workers11'12 in diffusion studies without any controversy on the issue. However, in some of these investigations, metallic deposition was also tried. The diffusivities calculated from these measurements were found to agree very well with the diffusivities obtained by using the oxide method. Thus it is assumed that the measured diffusivities represent true diffusion coefficients. Since palladous chloride decomposes at about 500°C, the deposited samples which were to be diffusion-annealed below 500°C were heated in vacuum for a very short time at 500°C to allow the decomposition of palladous chloride to palladium metal. Time taken in decomposition of nitrates to oxides and chloride to metal was negligibly small as compared to the period of the diffusion anneals. The residual activity technique13 was used to study the diffusion profiles where thin layers from the specimen surface were removed by grinding it parallel to a flat surface on a 600-grade carborundum paper. The specimen was washed, dried, and weighed, the differ -ence of the weight being the measure of the thickness of the layer removed. After each such abrasion and weighing, the total residual activity on the surface of the specimens was measured by counting 0.656, 0.94,

Jan 1, 1968

By D. J. Schmatz, H. I. Aaronson, H. A. Domian

Diffusion kinetics in disordered hcp Cd-Mg alloys have been investigated by means of the Kirkendall effect and concentration-penetration curves determined with an electron-microprobe analyzer. Self-diffusion coefficients of both species were determined at the three marker compositions obtained, averaging 27.6, 46. 7, and 78.1 at. pct Mg, by means of the Darken analysis. These coefficients were then corrected for the unequal and concentration-dependent partial molar volumes of the two elements with the Balluffi analysis, and for the vacancy flux effect by the Manning analysis. The latter correction reduced the Balluffi correction produced larger changes in the self-diffusiv-ities; neither, however, produced statistically significant changes in the Do's or the H'S. The most striking result of this investigation is that at all three compositions and at all temperatures studied both the uncorrected and corrected self-difjusivities of magnesium are higher than those of cadmium. The Cd-Mg system is the first one found in which the higher melting, lower vapor pressure element diffuses more rapidly. Both an empirical correlation due to Toth and Searcy and considerations of the atomic mechanism of diffusion indicate that this anomaly is probably due to a comparatively low value of the activation energy required for a magnesium atom and a vacancy to exchange sites, perhaps occasioned by the higher compressibility of magnesium atoms. KIRKENDALL effect studies have been previously reported for only two hcp solid solutions: the E phase of the Zn-Cu system1 and the a phase of the Cd-Hg system.' In neither investigation were the marker-movement studies supplemented with the concentration-penetration curve determinations necessary to evaluate self-diffusivities by means of the atano and the Darken analyses. The present program was undertaken to obtain both types of data on a hexagonal solid solution in order to provide more detailed information relevant to the mechanism of diffusion in this type of lattice. The Cd-Mg system was chosen for this study because the disordered solid solution extends across the entire phase diagram at temperatures above 253"c5 and the substantial difference in the melting points of the component pure metals promised that marker movements would occur at reasonably rapid rates should the diffusivities of the two species be as unequal as might be anticipated. The experimental convenience of the relatively low melting points of cad-miun and magnesium and the availability of extensive and accurate activity data6 (required for application of the Darken analysis) were additional reasons for selecting this alloy system. Since the anisotropy of diffusion is not large in either pure cadmium7 or pure magnesium,' the diffusion couples were prepared from polycrystalline components. The presence of a well-defined texture in the couples—the c axis of individual crystals tended to be normal to the diffusion direction— however, provides a fair degree of crystallographic definition to the data obtained. The principal (and entirely unexpected) finding of this investigation, that magnesium, the high-melting low-vapor pressure element, diffuses more rapidly than cadmium, in contradiction to a broad range of results in fcc and bcc alloys, as well as in the previously studied hcp alloys,172 makes the self-diffusivity determinations of immediate interest in understanding the origin of this anomalous result. EXPERIMENTAL PROCEDURE The cadmium (Belmont Smelting and Refining Co.) and magnesium (Dow Chemical Co.) used in this study were both of 99.99 pct purity. Alloys containing 51.0 and 65.6 at. pct Mg were prepared from these materials by melting under a MgC12-base flux in a high-purity graphite crucible. These alloys were subsequently hot-worked and then homogenized in a helium atmosphere at temperatures close to their solidus points. Sandwich-type diffusion couples of the type g/d/g were prepared from the pure metals by solid-state diffusion. Two-piece alloy couples of Mg/65.5 at. pct Mg (Mg/gCd) and Cd/51.0 at. pct Mg (Cd/CdMg) were welded by a liquation technique. The individual components of both types of couple were initially cylinders 1.27 cm in diam and in length; the ends of these cylinders were machined accurately flat and parallel. For both welding techniques, the pure cadmium cylinders and the alloys were chemically polished in a mixture of 40 pct ethyl alcohol, 40 pct hydrogen peroxide (30 pct conc), and 20 pct nitric acid,g while those of pure magnesium were polished in a solution of 10 pct nitric acid in ethyl alcohol.' Immediately afterwards, both metals were rinsed in freshly distilled acetone, and then in similarly purified methanol.' The Mg/Cd/g couples were assembled in a carefully cleaned stainless-steel welding fixture, in which a screw operating through a self-centering arrangement permitted a controlled pressure to be exerted upon a couple prior to welding.'' Tungsten marker wires 0.005 cm in diam were placed at the d:g interfaces of some of these couples, and imbedded in the couples during the application of pressure. As soon as a couple had been assembled, the welding fixture was inserted into a Pyrex capsule containing a packet of zirconium chips at each end. The capsule

Jan 1, 1967

By F. M. d’Heurle

Films of molybdenum have been prepared by sputtering onto oxidized silicon substrates. The resistivity. lattice parameter, orientation, and grain size were studied as a function of substrate temperature and substrate bias. Under normal sputtering conditions, the resistivity of the films was found to be quite high (600 x 10 ohm-crn). However, with the use of the negative substrate bias of 100 v and a substrate temperature of 350°C, films weve produced with a resistivity of ahout twice that of bulk molybdenum. The lattice parameters measured in a direction nornzal to the surface of the films weve found to be gveatev than the bulk value. This was interpreted as being at least partly due to the presence of compressive stresses. The effects of annealing in an Ar-H atmosphere were studied in terms of diffraction line width, lattice parameter, and resistivity. BECAUSE of its relatively low bulk resistivity (5.6 x 106 ohm-cm)' molybdenum is potentially interesting as a thin-film conductor in integrated circuits. An additional feature which makes it attractive for this purpose is its low coefficient of expansion (5.6 x KT6 per "c),' which is fairly well matched to that of silicon (3.2 x 10 per c). It is possible to deposit molybdenum films by evaporation but generally films produced in this manner have a high resistivity. In order to achieve resistivities close to bulk value, Holmwood and Glang found it necessary to operate in a vacuum of about 107 Torr and to maintain the substrates at 600 C during film deposition. Sputtered molybdenum films have been examined by Belser et a1.7 and, recently, by Glang et al.' This paper describes the results of an attempt to extend some of that work and examine the effects of annealing and getter sputtering on the physical and structural properties of the films produced. SPUTTERING APPARATUS AND PROCEDURE The apparatus used for most of the film sputtering work described here consisted of two "fingers" serving as anode and cathode, respectively, which were mounted within an 18-in.-diam glass chamber. A liquid nitrogen-trapped 6-in. diffusion-pump system was used to achieve a vacuum of about 1 x 107 Torr within the chamber prior to sputtering. The essential features of the equipment are shown in Fig. 1. Cathode and anode fingers are stainless-steel tubes isolated from the top and bottom plates by Teflon collars. In order to limit the discharge to the space between anode and cathode, each finger is surrounded by an aluminum hield, at ground potential, having an internal diameter 18 in. larger than the outside diameter of the finger. The cathode and anode fingers are 6 and 4 in. in diam, respectively. A 116-in.-thick sheet of molybdenum is brazed with a 10 pct Pd, 58 pct Ag, 32 pct Cu alloy to a copper disc which is mounted by means of screws and a large 0 ring onto the lower end of the cathode finger. The disc is cooled during sputtering by water circulation inside the finger. The use of several feet of plastic tubing for the water input and outputg reduces leakage to ground to less than 1 ma when the cathode potential is raised to 5 kv. The upper end of the anode finger is terminated by a brazed-on copper block. A variety of specimen holders can be easily mounted on the upper face of this block. Substrate heating or cooling is achieved by use of an appropriate unit attached to the lower face of the same block. Heating is achieved by means of cartridge-type heaters and cooling by copper coils fed with forming gas under pressure. The inner chamber of the specimen finger constitutes a small vacuum chamber of its own which is evacuated by an auxiliary mechanical pump in order to limit heating element oxidation and heat transfer by convection currents. An advantage of the finger arrangement is the absence of cooling and heating coils and wires within the main chamber. The stain less-steel shutter is useful to establish a discharge for cleaning the cathode at the beginning of each sputtering run. Water cooling of the shutter reduces heating and the out-gassing of impurities which might condense on the nearby substrates. Unless otherwise specified, the substrates used in these experiments were 1-in.-diam oxidized silicon wafe:s, 0.007 in. thick, having an oxide thickness of 6000A. The substrate holders were large copper discs onto the surface of which a number of molybdenum discs, 116 in. thick and 78 in. in diam, were brazed. The wafers were clamped to the molybdenum discs

Jan 1, 1967

By John G. Cazort

In August 1957, a cutter suction dredge started the removal of overburden from a bauxite deposit near Paranam, Surinam (formerly Dutch Guiana), South America. This event marked the climax of a program of investigation, design and construction which lasted almost five years. Cutter-suction dredges are used predominantly for harbor and river work, and land reclamation. While they have been utilized to remove overburden from ore bodies, notably at Steep Rock, Ontario, and Black Lake, Quebec, the conditions under which one is being used for this purpose in Surinam are unusual. Paranam is a mining town built by Suriname Aluminum Company, a subsidiary of Aluminum Company of America. It is located on the Surinam River, about 30 miles from the Atlantic Ocean. The bauxite mining, drying and shiploading facilities have been in operation since 1941.

Jan 10, 1960

For some time attempts have been made to improve drilling efficiency (and therefore reduce costs) by introducing certain reagents to the flushing medium. Much of this interest is the result of the Russian book, Hardness Reducers in Drilling, by Rehbinder, Schreiner, and Zhigach, published in 1944. Before embarking on full-scale drilling tests, it was decided to investigate the effects on the tensile strength; these results would help in the selection of the proper reagent and its optimum concentration. Selection of Tensile Strength Testing A drilling system basically performs two separate operations: 1) Breakage of rock. 2) Removal of the broken pieces of rock. Both affect drilling and drill performance but are distinct and separate phases of the process. Causing rock to break during drilling is a matter of generating sufficient stress with a drill bit to exceed the strength of the rock. This strength of the rock may be termed its drilling strength; it is not equivalent to any of the well-known strength parameters. Various criteria have been employed to measure the efficiency of a given drilling system or for comparing different systems and one of the most important criteria is "speed of drilling." Speed of drilling is a function of drilling strength of the rock. Many researchers have tried to correlate the speed of drilling with the strength properties of rock and compressive as well as tensile strength values have been found to give reasonable correlation." As the strength of rock drilled increases, speed decreases. As the Brazilian testing requires the least amount of core, this test was selected. Material Tested Broken Hill lode quartzite has been used in these tests. It is composed chiefly of quartz with varying amounts of sericite, pyrrhotite, chalcopyrite, galena, and garnet. The total porosity of this quartzite is about 11%.

Jan 1, 1973

By C. Richards Honeycutt, Frederick C. Langenberg, Guenter Pestel

Solidification in a moving electromagnetic field was successful in altering the as-cast grain structure of steel ingots. The equipment is described and exerimental results are presented for several different alloys. Conditions for optimum grain refinement are described and an empirical design constant presented. The effect of the grain refinement on hot workability is briefly discussed. T HE grain structure of a steel ingot teemed into a metal mold can be defined by macroscopic examination in semiquantitative terms. For example, the relative volume of obviously differing structures can be estimated with the classic definitions of chill, columnar, and equiaxed zones. Experimental evidence has proven that the grain structure of an ingot is affected by changes in such factors as teeming temperature, rate of teeming, degree of turbulence, size of ingot, mold characteristics (including preheat temperature, design and coating), and composition of the metal (especially as it affects the range of solidification). Significant advances have been made in fundamental solidification studies; but the principles which have been developed are difficult to apply tothe complex and changing phenomena that occur simultaneously during ingot solidification. In particular, many attempts have been made to refine the as-cast structure of ingots, with special emphasis on the columnar grains. The formation of large columnar grains is generally considered harmful to the further fabrication of an ingot. It may also result in undesired ani-sotropic properties. However, columnar grains are not undesirable in all grades, or product applications, and caution must be exercised to determine in which grades and applications columnar grains are not desired in the ingot. Although the literature on the refinement of as-cast ingot grain structures is too vast in general to review here, it is noteworthy that such methods are additions of artificial nuclei, mold vibration, mechanical stirring or ultrasonic agitation of the molten metal, and controlled cooling and reheating during solidification have been tried with varying degrees of success. However, it is doubtful that any method of refining the as-cast ingot grain structure has been completely successful on a commercial basis. The purpose of

Jan 1, 1962

By Frederick Becket

DOCTOR Albert Sauveur, distinguished scientist and Honorary Mem-ber of this Institute, predicted in the first Howe Memorial Lecture that the privilege of delivering this annual address would be considered a highly significant honor. The intervening years have well borne out Sauveur's prophecy. I wish to assure the American Institute of Mining and Metallurgical Engineers that I also deeply appreciate this honor, recognizing at the same time the present and even more the future respon-sibilities with which it is accompanied. Several of the previous lecturers had the good fortune to attend the classes of Professor Howe and to work in his laboratories. I was similarly favored, although in my instance and to my great regret the period was all too short. However, Howe's book, published in 1903, "Iron, Steel and Other Alloys," afforded me abundant opportunity to continue these studies. How well I remember the inspiration I derived from this famous book by Howe, the metallurgical master, pioneer, and educator! Remembering that Professor Howe contributed numerous papers to The Metallographist, a magazine supported from a technical point of view by the world's pioneers in metallography, I was curious a few days ago to learn the nature of Howe's early contributions to this magazine. The first paper by Howe in the first year of The Metallographist (1898) dealt with the allotropic theory; the second also treated of allotropy, and I quote the first sentence. of that paper: The allotropic theory of the hardening of steel may, like so many other important theories, have to be accepted or rejected not on direct proof or disproof, but on the accumulation of circumstantial evidence for or against it.

Jan 1, 1938