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By Charles Wurms, Robert Steinitz

DURING an investigation to determine the compatibility of several metals with tungsten, the degree of reaction between tungsten and lead was determined. A literature survey showed considerable disagreement between the results of various earlier investigators. Information presented by M. Hansen1 states that, according to S. Inouye,2 tungsten has very poor resistance against attack by molten lead, even at the low temperature near the melting point of lead. A phase diagram in the same reference indicates a solubility of 30 wt pct W in molten lead at 1300°C. Contrary evidence was shown by Parkman and shepard3 in their investigation of materials for use in heat transfer systems containing liquid lead alloys; they performed experiments at 980°C for times up to 50 hr without noticing any appreciable attack on the tungsten. Tungsten sheet was immersed in molten lead contained in Vycor tubes evacuated to at least 10-4 mm Hg. R. Bernard4 and R. I. Jaffee5 also indicate that no reaction occurs between molten lead and tungsten. However, no experimental data were included in these reports. In order to settle the question of the solubility of tungsten in molten lead, tungsten powder with an average Fisher subsieve particle size of 6µ was pressed in a double-acting die at 6 tsi to small compacts. They were then sintered in an atmosphere of hydrogen for 2 hr at 1700°C, resulting in a sintered density of 64 pct of theoretical with final dimensions of 0.260 in. in height and 0.245 in. in diameter. For all tests, the tungsten pellets were immersed in molten lead. Table I is a summary of the experimental procedures showing atmospheres, temperatures, and times. The first experiments were performed at 650°C; at this temperature, the liquid lead should wet the porous tungsten better than at its melting point, and penetrate into the pores. The lead was heated in a graphite crucible with a graphite cover. No protective atmosphere was used, as it was expected that the formation of CO would be sufficient to prevent oxidation. This, however, proved to be wrong, and all tungsten samples showed a slight oxide film after treatment. The tungsten samples were immersed in the molten lead for times of 5 min, 10 min, 1/2 hr, 1 hr, and 2 hr. After this time, the melt was poured into a form and the

Jan 1, 1962

By Sanai Nakabe

Japanese wartime economy demanded domestic cobalt production. This paper describes a process operated for two years at the Besshi mine and smelter on extremely low grade (0.1 pct Co) pyrite concentrates obtained from copper ore. 'The steps in the process were roasting, leaching, precipitation, reduction fusion to crude cobalt, and finally refining by electrolysis to 99+ pct. COBALT ore deposits in Japan are all small and of poor grade. In the past, a small amount of cobalt has been produced from the best portions of a few of these deposits, and very little production is expected in the future. In addition to these lean cobalt ores, cobalt is present in the cupriferous pyrite which is fairly abundant although of low grade, as is shown in Table I. Considerable cobalt is expected from these deposits because of their extent. Cobalt cannot be exclusively recovered economically from ore of this type; however, if means could be devised to recover it as a byproduct of copper production, a fairly large production at reasonable cost could be expected from Japanese sources. It was along this line that the research work was done. Selection of Suitable Process The process for extracting cobalt differs from ore to ore according to their composition. The difficulty in cobalt metallurgy arises from the fact that chemically cobalt resembles many such common metals as Mn, Fe, Ni, Cu, and Zn, associated with it in the ores. In the present case the most serious difficulties were: 1—Extremely low grade ore, 0.1 pct Co. 2—The large proportion of iron accompanying cobalt and its close similarity in chemical behavior. 3—The fairly large proportion of zinc and manganese and their chemical similarity to cobalt. The recovery of cobalt oxide as a byproduct of the hydrometallurgy of copper had been attempted in Japan but was stopped after a short period because it proved uneconomical. The literature disclosed no method for the recovery of cobalt from cobaltiferous copper pyrite and it was therefore necessary to devise a new process. The following basic principles were considered in selecting the process: 1—A major alteration in copper production methods should not be necessary. 2—The first step should be the extraction of cobalt leaving the large quantity of iron unaffected. For this purpose wet metallurgy would be preferred.

Jan 1, 1952

By A. Bar-Or, G. Hirsch, P. Wynblatt

The rates of nucleation and growth at various temperatures in U-0.45, 1.1, and 1.35 at. pet Cr alloys were determined, providing a qliantitative proo-f that the transformation under study is controlled by nucleation and diffusional growth. The linear relationship, log NV US 1/T2, suggests that the nucleation of the alloys is probably controlled by the classical law of nuclei formation. The established linear relationship, log G us 1/T, in the three alloys suggests that growth in each alloy is controlled by bidimensional nuclei formation. It was established that both the rate of growth and the rale of nucleation are retarded by chromium. Using classical formulae, sApN and sApG (the ß/a apparent interphase energies) were calculated from the nucleation and growth results, respectively. It was found that their values are of the same order of magnitude. However, why sApN is unaffected by the addition of chromium, while sApG increases with it, needs further clarification. In the last few years, an appreciable amount of research has been conducted into the mechanism of the ß —a transformation in uranium and uranium alloys. Recently, Burke1 reviewed the published work concerned with this transformation. He concluded that in dilute uranium alloys it is firmly established that, at high temperatures in the a range, ß decomposes by a diffusional process. However, he based his conclusion either on experiments dealing with the over-all transformation,2 or on qualitative results.3 It was felt that a better insight into the mechanism of transformation could be gained from the quantitative measurements of growth and nucleation rates, which we aimed to carry out in the present work. In a previous work,4 we have shown that a rim of a grains is formed during isothermal transformation at the high a range. The thickening of this rim with time was used for measuring the rate of growth in U-0.45 at. pet Cr.5 This method was also used in the present work for two more alloys. For meas- uring the rate of nucleation, a method of quenching and macroetching was developed to allow differentiation between a grains formed during isothermal transformation at the upper a range and those formed after quenching, Fig. 1. EXPERIMENTAL WORK AND RESULTS The Rate of Nucleation. The measurement of the rate of nucleation was effected by counting the num-

Jan 1, 1965

By Pieter W. Greeff, Graeme W. Mitchell

INTRODUCTION This paper describes the underground environmental planning parameters developed for Pancontinental Mining Limited's Jabiluka uranium deposit. The deposit is located 230 km east of Darwin in the Alligator Rivers region of the Northern Territory, Australia. The deposit is situated within land subject to an Aboriginal land claim, adjacent to a National Park and within a proposed extension to that National Park, as well as being close to a long- established Aboriginal reserve. In addition, being the first large underground uranium mine planned in Australia, the environmental considerations, both on surface and underground are considerable. Pancontinental is committed to the highest practicable standard of environmental management in the operation of the mine. In addition, Government regulations and requirements are particularly stringent by world standards. The underground environmental problems are discussed later in the paper with emphasis placed upon radiation aspects, both gamma and radon daughters, and dust. Consideration has also been given to heat and humidity due to the location of the deposit in a sub-tropical region 12° south of the equator. The paper explains how these environmental factors influence the design and selection of stoping methods. GEOLOGY AND ORE RESERVES The Jabiluka Two orebody is completely overlain by flat-bedded Kombolgie Sandstone with a thin layer of surficial colluvial sands. The orebody occurs in an east-west striking folded succession of Lower Proterozoic metasedimentary rocks of the Cahill Formation. Uraninite and pitchblende constitute essentially all the uranium mineralisation and are contained in the four lithological series, as shown in Fig. 1. - ,Upper Graphite Series - Main Mine Series - Lower Mine Series 1 - Lower Mine Series 2 The succession at Jabiluka has been folded and forms an east-south-east striking, asymmetric syncline-anticline which dips south and plunges to the east. A major fault bisects Jabiluka Tw8 having a north-south trend and dipping about 80 to the west. A near vertical tourmaline granitic pegmatite dyke up to 30 m in thickness has intruded the Jabiluka Two orebody at the western end. Current drilled ore reserves for Jabiluka Two are 52.0 million tonnes at 0.39% U308. Included in these reserves are 1.1 million tonnes of gold ore at 10.7 g/tonne. A large proportion of the orebody can be mined in thick sections (over 80% of tonnage) either as single sections or by bulking a number of thin sections which are close together.

Jan 1, 1981

By John Jan

Iodine is a soft, lustrous, grayish-black non- metallic element with a density of 4.9. It is the least active of the four members of the halogen family. The other members are, in order of increasing activity, bromine, chlorine, and fluorine. Iodine is a solid at ordinary temperatures, while bromine is a liquid and chlorine and fluorine are gases. Iodine melts at 113°C and volatilizes at 184.4°C to a blue- violet gas with an irritating odor. It occurs in nature only as iodates and iodides or other combined forms. It was discovered by Bernard Courtois in France in 1811, who noticed its presence as an unknown substance in crude soda ash obtained from burning seaweed. Gay-Lussac recognized it as a new element and named it iode, from the Greek word "ioeides or iodes" for violet color (MacMillan, 1970). The world production is not known with any great certainty, but it is probably between 20 and 25 million lb per year, of which about 25% is consumed in the United States. Geology and Mineralogy Iodine compounds occur as a minor constituent as a mineral in the Chilean nitrate deposits and in solution in brines and sea- water. According to the U.S. Geological Survey, it is the 47th most abundant element in the earth's crust. The minerals lautarite, Ca (10,) (calcium iodate), and dietzeite, Ca, (10,) , (CrO,) , (calcium iodate-chromate) are found in Chilean nitrate deposits which are located in Antofagasta and Tarapach provinces on the eastern slope of the coast range in a desert area. Various brines contain iodine compounds. Seawater contains about 0.05 ppm of iodine and some seaweeds will extract and accumulate it up to 0.45% on a dry basis. Some coals in West Germany also contain iodine compounds. The known and potential sources of iodine reported in 1968 are given in [Table 1]. Iodine has been recovered from brines in Java, Indonesia, France, England, and the USSR. Iodine has also been recovered from seaweed in Ireland, Scotland, France, Japan, Norway, and the USSR. The indicated re- serves and future resources of iodine are large but have never been adequately measured. Analysis Iodine as the free element can be detected by the characteristic blue color it gives to a starch solution. Quantitatively it is determined as the free element by titration with standard thiosulfate solutions using starch as an indicator. Colorimetric methods are also applicable.

Jan 1, 1975

By F. E. Bash

PREVIOUS to the war, this country depended on Europe for its supply of a number of alloys of great importance in the manufacture of electrical apparatus and equipment. When this source was cut off shortly after the beginning of hostilities and the small stocks in the United States were exhausted, either inferior substitutes had to be used or the manufacture of the apparatus suspended. Since electrical equipment was of primary importance in the prosecution of the war, the substitutes had to be used until the composition and processes of manufacture of the alloys could be determined. Included among these alloys was one generally known as manganin, which is composed chiefly of copper and manganese and which, beside having a low-temperature coefficient of resistance, has a low thermal electromotive force against copper. These qualities make it valuable for the manufacture of electrical instruments and machines in which it is used in the shape of wire, rod, and strip. As a result of these circumstances, an investigation was started to deter mine how manganin could be made on a commercial basis so that a product of uniform quality and the necessary electrical characteristics could be produced. The object was to procure an alloy with temperature coefficient of resistance not greater than T 1 X 10-5 per ° C. and a thermal e.m.f. against copper no greater than that of the imported material. It is characteristic of manganin that the temperature-resistance curve is not a straight line but has a peak, which varies in position with different samples; it is most desirable, however, to have it at a temperature of 25° C. if possible. The coefficients of manganin from all records available ranged from a large negative to a large positive value. The composition as reported by different authorities is given in Table 1. Prof. Matthew A. Hunter, of Rensselaer Polytechnic Institute, made up a number of small melts of manganin in a graphite crucible and the one that he reported as having the best coefficient gave the following analysis: Copper, 83.6 per cent.; nickel 2.5 per cent.; manganese,-13.6 per cent.; iron, 0.3 per cent. An analysis of a sample of German manganin gave the following: Copper, 82.6 per cent.; nickel, 3.8 per cent.; manganese, 12.8 per cent.; iron 0.7 per cent.

Jan 9, 1919

By Francis Foley

WITH the possible exception of high-speed tool steel, the service demanded of rock-drill steel is probably more precarious than that of any other tool steel. Unaided by the helpful influence of alloys and dependent solely on the efficiency of the heat treatment applied for its ability to stand up under the abuse to which it is necessarily subjected, rock-drill steel is worthy of intensive study. For its heat treatment the smith has his fire, an oil fire perhaps, and a quenching bath; he judges' the temperature by his eye. There are shops where excellent drills are produced by this method, but there are more where the product varies between very good and very bad. Pyrometers with specially designed equipment are used in but few cases. But the responsibility for rock-drill failures does not rest entirely on the smith. Little has been published concerning the efficiency of drill steel, though the Canadian Mining Journal' published the breakage record of a large number of hollow drill steels. This record indicates that most of the breaks occur during the early life of the steel and that as a given batch of steel is used, its percentage of breakage decreases. This fact, the article points out, is at variance with the much-talked-f theory concerning failure from crystallization and fatigue. It seems to point to the fact that the greater part of drill-steel failure from breakage is traceable to faulty manufacture, resulting in defects in the bore of the hollow steel from inclusions of slag or oxides, etc. As this defective material meets with early failure, it is weeded out. In addition, some breakage may be caused by a lack of proper condition with respect to heat treatment of the steel as furnished by the manufacturer. In the article mentioned, the breakage of 1 ¼ -in. (3.17 cm.) hollow steel is given as 4.62 per cent. for the early period of use, with a decrease to 3.35 per cent. and 2.67 per cent. With time in use. For 1-in. (2.5 cm.) hexagonal hollow steel, the figures for breakage are 0.18 per cent. and 0.06 per cent.; attention is called to the "enormous decrease in breakage by the use of smaller diameter drills." The figures are given as so many "drills sharpened," but there is no way of determining the percentage of

Jan 6, 1921

By T. J. Woodside

Prior to 1927 the lead blast furnace charge at El Paso consisted principally of direct-smelting carbonate ores, very low in zinc, and the resulting slag seldom carried more than 4.0 pct. With the exhaustion of the mines in Northern Mexico which supplied these ores, they were supplanted with a much smaller tonnage of sulphide concentrates containing appreciable amounts of zinc, and the zinc content of the slag rose to 10.0 pct. The Anaconda Company's slag fuming plant at East Helena, Montana, had then been in successful operation for several years, and it was immediately recognized that, while at that time the production of high zinc slag was small, if the grade held, a plant for the recovery of zinc from the accumulated slag might some day be practical. The grade not only held but became increasingly higher so that by 1946 suffcient slag had been accumulated to warrant the construction of a fuming plant regardless of future slag production from the blast furnaces, and with the removal of Government restrictions on construction at the end of the war the project was undertaken. The general design of the plant follows that at Bunker Hill, with waste heat boiler, unit coal pulverizers and even more extensive instrumentation and automatic control. The area around the lead blast furnaces is rather congested, being cut off from the nearest feasible site for the fuming plant by the copper plant, so that the most practical route for hot slag transfer is through the converter aisle. For this reason and also to make use of the existing converter cranes to serve the fuming furnace, an unused reverberatory at the north end of the converter building was dismantled and the fuming furnace and boiler located in its place. A flue at right angles to the furnace and boiler runs northward to the U-tube coolers and baghouse (Fig 1). From the bag-house a steel flue runs eastward to an existing and long unused 300 ft con- Crete stack. The coal handling system and de-leading plant lie north of the furnace and east of the cooling tubes and baghouse. The furnace is conventional, 8 X 21 X 33 ft high inside and completely water jacketed (Fig 2). There are 21

Jan 1, 1950

By Jerome Alexander

It is an outstanding fact of Nature that many of the practical properties of substances are dependent, not on their ultimate chemical composition, but on the kind and degree of aggregation of their constituent particles. Thus, a granite boulder is unmoved by wind or water, but if reduced to a fine dust it will be blown about by the wind and washed away by the rain. Carbon in one crystalline state of aggregation (diamond) is the hardest known substance, whereas in another crystalline state (graphite) it is so soft that it is used as a lubricant. Laying too much stress on the mere chemical analysis of substances is apt to obscure the fact that the nature of the aggregation of their particles is always a factor of importance, and sometimes the most important factor. Colloid chemistry deals with matter in a very fine state of subdivision; its sphere begins with particles just a little smaller than a wave length of light and extends down until they blend into molecular dimensions. With particles of this size, such phenomena as surface tension and adsorption, which depend on the development of free surface, become enormously magnified. Thus a cube of 1 cm. edge has a surface of only 6 sq. cm.; but if it is reduced to colloidal dimensions by being cut up into cubes each having an edge of 0.01 µ (0.00003 mm.), it will yield one million, million, million (1,000,000,000,000,000,O~) such cubes, having a combined area of 600 sq. m., or 21,274 sq. ft. The tiny force with which a drop of rain clings to the window pane becomes a factor to be reckoned with, if the surface involved is increased millions of times. From the colloid-chemical viewpoint, metals and alloys may be regarded as jellies or sponge-like structures,. the viscosity or stiffness of which at ordinary temperatures is exceedingly great; and like all jellies their properties are dependent on the composition and degree of dispersion of their constituent phases. These, in turn, depend on chemical composition, mutual solubility, speed of chilling, subsequent mechanical and heat treatment, etc. In fact, in preparing metals and alloys for practical use, we remove undesirable constituents (as in the conversion of pig iron into steel), add desirable constituents (as in

Jan 1, 1919

By B. D. Cullity

GOLD and beryllium form an intermediate phase composed of the two metals in equal atomic proportions and having the formula AuBe. According to Winkler,1 this phase probably exists in two modifications: beta, stable below about 600°C, and alpha, stable between 600°C and the melting point, about 740°C. Only the low- temperature beta form will be considered in this paper. EXPERIMENTAL PROCEDURE The gold used had a fineness of 999.75 to 999.85, balance mainly silver, and the beryllium purity was better than 99.8 pct. AuBe was prepared by melting the constituents in a beryllia crucible in an evacuated induction furnace. After melting and thorough mixing, the alloy was allowed to solidify in the crucible. No difficulty was encountered in obtaining a homogeneous ingot. Both chemical analysis and microscopic examination of the ingot showed that the alloy was essentially one phase, containing 50 at. pct gold. The alloy was quite brittle and powder samples could easily be pre- pared by grinding in an agate mortar. The X-ray diffraction patterns were made with CuK-alpha radiation in a Debye-Scherrer powder camera 57.3 mm in diameter. The film was placed unsymmetrically in the camera in order to afford a basis for am-shrinkage corrections. A sample homogenized at 5o0°C gave the same diffraction pattern as a sample taken from the as-melted ingot. GENERAL RESULTS The diffraction pattern of AuBe was readily indexed on the basis of a simple cubic lattice with ao = 4.659 ± 0.001kX. If the unit cell is assumed to contain four AuBe "molecules," the calculated X-ray density is 13.46 grams per cc as compared with the measured density of 13.55 gm per cc. The only missing reflections in the dsraction pattern are (100) and (220) (see Table I). Since these missing reflections are not those characteristic of body or face centering, the lattice of AuBe must be simple cubic. To locate the positions of the atoms within the unit cell, two possibilities had to be considered: I. The structure was disordered and there were eight positions to be filled by an "average" gold-beryllium atom. That the structure was disordered seemed unlikely since the lattice parameter did not vary with composition in alloys containing some- what more and somewhat less than 50 at. pct gold, indicating a fixed composition for AuBe.

Jan 1, 1947

By Stephen H. Stow

A relationship exists between the color and the chemical composition of the pebbles from the Bone Valley Phosphate Formation. Darker-colored pebbles are relatively high in iron oxide and relatively low in calcium phosphate when compared to lighter-colored samples; the brown color of the phosphate pebbles can be correlated with their iron content and the black and gray colors with their organic carbon content.1,3 It was anticipated that the darkness of a phosphate sample might be quantitatively measured by a simple reflectivity test and that the amount of reflected light could be correlated with the chemical composition of the rock, especially with the elements which cause the color and darkness of the Florida phosphates. Twenty-one samples of production grade phosphate rock from Hillsboro County, Fla., were studied. All samples were ground to -200 mesh for reflectivity tests and analyses. All analyses are accurate to well within ±2% of the reported value, except for aluminum and organic carbon, which are accurate to only ±15% of the reported amount. Reflectivity measurements were taken with a model 610 Photovoltmeter for tri-stimulus amber, blue and green, and white lights. Experimental procedures and data are available upon request. Results Table 1 contains linear correlation coefficients (LCC) for the element-reflectance relationships for the samples. The top portion of the table refers to the LCC between the percent of light reflected off the samples and the percent of a given element (or its oxide) as analyzed. In the lower portion of the table the LCC refers to the relationship between the same reflectance data and the chemical analyses which have been corrected on the basis of 0% acid insoluble material (chiefly quartz) in the phosphate rock. Each LCC presented in Table I is computed for the 14 coarser samples exclusive of the seven concentrates since the concentrate samples appear to have anomalous reflectivities upon comparison with the coarser grades. Only the most significant LCC for each element is presented in graphical form. Discussion of Data Iron: [Fig. 1] is a graph of the relationship between iron and reflectivity (LCC = - 0.98). A good correlation with Fe2O3, is expected due to the relationship between the tan (or brown) color and the abundance of iron oxide, the principal mode of occurrence of iron in Florida phosphates.8 Note the location of the seven triangles which repre-

Jan 1, 1972

By F. E. Bash

Previous to the war, this country depended on Europe for its supply of a number of alloys of great importance in the manufacture of electrical apparatus and equipment. When this source was cut off shortly after the beginning of hostilities and the small stocks in the United States were exhausted, either inferior substitutes had to be used or the manufacture of the apparatus suspended. Since electrical equipment was of primary importance in the prosecution of the war, the substitutes had to be used until the composition and processes of manufacture of the alloys could be determined. Included among these alloys was one generally known as manganin, which is composed chiefly of copper and manganese and which, beside having a low-temperature coefficient of resistance, has a low thermal electromotive force against copper. These qualities make it valuable for the manufacture of electrical instruments and machines in which it is used in the shape of wire, rod, and strip. As a result of these circumstances, an investigation was started to determine how manganin could be made on a commercial basis so that a product of uniform quality and the necessary electrical characteristics could be produced. The object was to procure an alloy with temperature coefficient of resistance not greater than 1 X 1X per " C. and a thermal e.m.f. against copper no greater than that of the imported material. It is characteristic of manganin that the temperature-resistance curve is not a straight line but has a peak, which varies in position with different samples; it is most desirable, however, to have it at a temperature of 25' C. if possible. The coefficients of manganin from all records available ranged from a large negative to a large positive value. The composition as reported by different authorities is given in Table I. Prof. Matthew A. Hunter, of Rensselaer Polytechnic Institute, made up a number of small melts of manganin in a graphite crucible and the one that he reported as having the best cocfficient gave the following analysis: Copper, 83.6 per cent.; nickel 2.5 per cent.; manganese, 13.6 per cent.; iron, 0.3 per cent. An analysis of a sample of German manganin gave the following: Copper, 82.6 per cent.; nickel, 3.8 pcr cent.; manganese, 12.8 per cent.; iron 0.7 per cent.

Jan 1, 1921

H. M. BOYLSTON, Cambridge, Mass.-I would first like to ask what machine Capt. Bellis used to make his tests on impact strength. I have made some tests with the Charpy impact machine, the specimen being supported at both ends and nicked in the middle, and, find that the results do not always agree with those obtained by the Izod and other machines. I would also like to ask what effect the composition and heat treatment of the tool steel had on the drilling of his rifle barrels, as compared, with the heat treatment of the steel itself? I notice that the analysis of the composition of steel used shows sulphur 0.050 and phosphorus 0.065; I should like to ask how those high limits of sulphur and phosphorus came to be allowed? I have some data which lead me to feel pretty certain that those high limits make for very unsafe steel in rifle barrels. It has never been explained to the satisfaction of all of us, why the manganese is so high: 1.22 per cent. I believe several reasons have been stated; among them, that it is high in order to compensate for the high sulphur, and also to increase the elastic limit and improve other physical properties of steel. Lastly, I wish to ask whether Capt. Bellis has tried any different methods of heat-treating his steel rifle barrels? Apparently these were all heat-treated before machining; has he had any experience with heat-treatment after machining, especially after drilling? Those questions may seem somewhat outside of the range of this -paper, but they are important, and if Captain Bellis can give us any information, it will be very helpful. Dr. J. A. MATHEWS,* Syracuse, N. Y.-The same subject was discussed here last year, and the earlier papers by Dr. Carle Hayward seem to indicate that nothing was gained by the length of time of 'tempering. (It should be borne in mind that his results were based upon electrical and magnetic measurements and not upon tensile tests.) That idea has been accepted as gospel by steel workers, until late years, and particu-larly in connection with alloy steels, on which there is no question that the effect of time of tempering is very marked.

Jan 4, 1918

By P. W. Davies, B. Wilshire

PREVIOUS investigations on the effect of stress changes on the high-temperature creep and fracture behavior of metals have been confined mainly to the testing of complex alloys.172 Most of these alloys are structurally unstable during creep because of such effects as recrystallization, overaging, and so forth, so that the results are of limited application. The only pure metals on which observations have been made appear to be lead3,4 and aluminum5 tested under conditions which allow rapid recovery to take place. The present work describes the effect of a single stress change on the creep and fracture properties of a metal in which recovery is very slow. A Ni 0.1 at. pct Pd alloy was used so that grain growth and recrystallization did not occur during creep testing. Specimens of this material were heat-treated to give a uniform grain size of 10 grains per mm. Creep tests were carried out at 500°C using Denison T.47 machines; details of the creep-testing procedure have been given elsewhere.' All specimens were tested at a constant initial stress of 5 tpsi which gives, in an uninterrupted test, a minimum creep rate of ~10-3 pct per rnin and a life of -7000 min. Specimens were loaded under these standard conditions and after 1500 min, when secondary creep was well-established, the stress was changed to either 8, 7, 6, 4, 2, or 0 tpsi for a period of 180 min. After this time the original load was reapplied and the tests continued to fracture. The results are shown in Fig. 1. No detectable creep occurred during the period of reduced load, even at 4 tpsi, and on reverting to 5 tpsi the creep rate returned to its original value immediately. Increasing the stress to 8, 7, or 6 tpsi resulted in an instantaneous extension followed by a period of transient creep leading to a new steady creep rate. On returning from these higher stresses, the resulting creep rate at 5 tpsi was very low compared with the original value. Furthermore, the higher the stress during the stress change, the lower was the final creep rate. It is significant that the rupture life is comparatively unaffected by any of these stress changes.

Jan 1, 1965

By P. D. Hunt, B. Tani, M. G. Chasanov, R. Schablaske

The Zn-Vphase diagram was studied by thermal. metallographic, X-ray, and sampling techniques. Three ternary phase equilibria were observed: Mutual solid solubilities in vanadium and zinc appear to be negligible. The liquidus line is retrograde from 670° to 756°C. 1 HE only information in the literature relating to the Zn-V system was a study of corrosion of vanadium by liquid zinc' and an examination of the effectiveness of zinc coatings in protecting vanadium-base alloys from oxidation at high temperatures.2 Establishment of the Zn-V phase diagram was undertaken as part of a study of transition metal solubilities in liquid metal solvents. Chemical, metallographic, thermal, and X-ray diffraction analyses were used to determine the diagram. MATERIALS AND EXPERIMENTAL PROCEDURES Vanadium (99.86 pct) in the form of powder and small chips was employed. Stick zinc (99.99 pct; major impurities: 10 to 15 ppm Pb and 20 ppm Cu) was used in the liquidus determinations and thermal analyses; zinc powder (98.80 pct) was used to prepare intermediate compositions. The liquidus lines were determined by chemical analysis of filtered samples of the saturated melts. The apparatus and sampling techniques were similar to those described by Martin, et al.3 The entire metal sample was dissolved to preclude analytical errors due to segregation on cooling. Vanadium was determined amperometrically, using iron (11) as the titrant,4 to an estimated accuracy of 1 pct. Standard techniques of thermal analysis were employed to examine alloy specimens contained in alumina crucibles under helium. Heating and cooling rates were about 1°C per min. At least five heating and cooling cycles over the range 420° to 700°C were performed for each of two Zn-15 pct V alloys. A Zn-0.2 pct V alloy was used in the determination of the eutectic temperature. The separation of intermediate phases from zinc-rich alloys was carried out by selective leaching with ammonium nitrate solutions. For further investigation of intermediate phases 1/4 in. diam powder compacts were prepared by pressing at 80,000 psi and were annealed in argon at 415" to 450°C for 10 days. Larger quantities of intermediate phases were prepared in sealed tantalum capsules heated in a rocking furnace. Temperatures were determined to an estimated accuracy of 0.5°C with a Pt/Pt-10 pct Rh thermo-

Jan 1, 1963

By Y. C. Liu, W. R. Hibbard

An aluminum single crystal cold-rolled from (110) [1121 essentially retains its initial orientation after 99.6 pct reduction in thickness. The orientation of the recrys-tallized grains of this material can be described in terms of crystallographic rotations about principal poles of deformation texture. DURING the study of the recrystallization of a copper single crystal cold-rolled from a (110) [112] initial orientation, the orientation of the re-crystallized grains could be derived by a 30" rotation of the orientation of the cold-rolled matrix about its <111> poles.&apos; The present investigation was undertaken to extend the work done on copper&apos; to an aluminum crystal also cold-rolled from a (110) [112] initial orientation. Experimental Procedure The procedure of this experiment was similar to that reported for copper.&apos; An aluminum (99.998 pct) single crystal rod* 1 % in. in diameter was grown in back-reflection technique.&apos; The specimen (1.20x 1.004x0.6787 in. thick) was then rolled along the [112] direction. The final thickness was 0.0028 in., giving a reduction in thickness of about 99.6 pet. Specimens were cut from the rolled strip with scissors, and approximately in. of disturbed metal was removed with Tucker&apos;s reagent. The rolling edge remained intact. The specimens were sandwiched between two graphite plates and annealed in a lead or lead alloy bath which was electrically heated. Pole figures were constructed using the techniques previously described.&apos; Specimens were electrolytically polished4 and etched with 47 pct HNO8, 50 pct HC1, and 3 pct of 48 pct HF. The electrolytic polishing method and etching reagent employed for aluminum specimens were not entirely satisfactory and the microstruc-tures could not be studied in any detail. Results and Discussion The octahedral pole figure of cold-rolled aluminum strip is plotted in Fig. 1. The <111> poles spread in the transverse direction approximately 8" for the highest intensity areas. The spread in the transverse direction can be related to a rotation about two <110> directions lying in a plane containing the rolling direction and rolling plane normal. The two <110> directions and a scale of rotation for the <111> poles are shown in Fig. 2. The amount of rotation is consistent for three of the four <111> poles, about 35" to 40". The discrepancy for the fourth pole is believed to be due to limitations of the film technique. Alternate inter-

Jan 1, 1956

By K. H. G. Ashbee, J. W. Heavens

One consequence of the distribution in orientation of Bragg diffracting planes in an elastically bent foil is that simultaneous diffraction occurs from ±g pairs, where g is the reciprocal lattice vector to a diffracting plane. If such Bragg contour pairs are indexed, then the variation in orientation with respect to the incident electron beam is known. This note describes a construction by means of which Bragg contour pairs may be indexed by inspection. Referring to Fig. 1, the Ewald sphere radius is l/h, where is the wavelength of the electron beam, and the half spacing of first-order reciprocal lattice planes is l/d, where d is the corresponding spacing in direct space. The angle subtended by the zero and first-order planes at the center of the Ewald sphere is a = sin-&apos; Thus, to represent a pair of first-order Bragg contours on a stereographic projection, measure ±a from, and along the normal to, the zero-order plane. The traces of the required Bragg contours pass through these points and parallel to the zero-order trace. In practice, it is desirable to enlarge a stereographic projection of the zero-order planes before making the construction. As an example, a stereographic projection of first-order Bragg contours up to line 27 for an fcc crystal is given in Fig. 2; if required, higher-order contours can easily be added. Fig. 2 is, of course, a map of first-order Brillouin zone boundaries. One use of this construction is the measurement of large elastic fields in electron microscope specimens. Fig. 3(a) shows a pattern of Bragg contour pairs due to lattice distortions near a large precipitate. This particular example is of a T-phase precipitate in Hidu-minium 54 (A1 + 6 wt pct Cu, 0.5 wt pct Mn). Foil buckling is produced by annealing during observation and may be evidence for evaporation from the precipitate.&apos; Comparing Figs. 2 and 3(0), it is evident that the axis of high symmetry in Fig. 3(a) is [lll]. The strain in a bent foil is approxinlately t/2r, where / is the foil thickness and ? the radius to which the foil is bent. From the projections of grain boundaries and of helical dislocations, it was estimated that ( - 3000A, and values for ? were obtained from the

Jan 1, 1968

By L. Zwell, H. A. Wriedt

In describing their procedure for measuring the lattice parameters of solid solutions, Abrahamson and Lopata report (p. 77) the final heat treatment of their alloy specimens as "700°C for 100 hr, followed by a furnace cool". The isothermal part of this treatment may be expected to precipitate solute in excess of the stable a solid-solution limit at 700°C; the subsequent slow cooling is likely to reduce the dissolved solute still further. Fig. 1 (upper) presents the data for titanium alloys so he;rt-treated and shows the lattice parameters of solid solutions containing up to 3.5 at. pct Ti; Fig. 17 (lower) shows 2 at. pct Ti as the solubility limit in a iron at 700°C. Figs. 1 and 17 are thus incompatible. The paper contains comparable incon~patibilities for zirconium alloys, for niobium alloys, and for tantalum alloys. The final heat treatment at 700°C may also be responsible for the anomalous "knee" in the lattice-parameter data for nickel alloys, Fig. 3. The "knee" composition is located near the 700°C limit of the stable a solid-solution field;37 alloys of the experimental composition range with more nickel than the "knee" composition are two-phase at 700 C and prolonged heat treatment of them at 700°C would tend to produce inhomogeneity rather than homogeneity. In Figs. 4 and 7, the composition ranges of the zirconium, hafnium, and niobium alloys examined terminate at alloy concentrations of 0.1 to 0.2 at. pct. These metals form very stable oxides and their partial removal from solid solution in iron by impurity oxygen may be expected. We believe that the authors should have reported the procedure by which they distinguished the amounts of alloying elements in solution and in oxide. The diagrams pertaining to copper in Figs. 3 and 18 (lower) are almost certainly incorrect. Three recent investigations of this system38-40 all substantially agree on the solubility of copper in a iron, finding it to be much larger than that reported by Abrahamson and Lopata. The change of the lattice parameter with composition reported by Abrahamson and Lopata is too large by a factor of three to five, as seen by comparison with the findings of other investigators.41738 Moreover, the authors violate, in Fig. 18, the accepted Fe-Cu constitution diagram37 by ignoring the eutectoid at about 850°C.

Jan 1, 1967

By V 7. 0 / 300 dpi

WHEN the copper smelters were built, in Montana, all of the refractory products which were used in their construction were shipped in from Eastern factories. It was apparent that if a material suitable for the manufacture of these products could be found within the State, a saving of freight could be effected and a new industry built up. Prospecting for such materials was started and experiments were made with samples from numerous deposits. Considerable effort and funds were expended in an attempt to manufacture silica brick from Dillon quartz, a light colored sandstone that is found near Dillon, Mont., on the Oregon Shortline railroad. As a brick material the Dillon quartz was a failure, but it has proved very satisfactory as a silica cement. It is now being used in laying silica brick and for reverberatory furnace bottoms. A bed of quartzite that is particularly suited to the manufacture of high-grade silica brick -was finally discovered at Browns Spur, 6 miles west of Anaconda. The material from this deposit is now being used in the manufacture of the Anaconda silica brick, which have gained a wide reputation for heat-resisting and lasting qualities. The analysis of all average sample of this quartz is: SiO2,, 96.7; Fe203, 0.3; Al203, 2.5; CaO, 0.3 per cent. The very low percentage of fluxing ingredients makes this a most refractory material. All of the Anaconda silica brick are hand molded. Various types of brick machines have been tried, but the hand-mold process proved the best suited to the manufacture of silica brick from this material. The silica is first put through a jaw crusher and is then clumped into wet pans, where 4 per cent. of lime paste is added, to produce a bond. Without the lime the. material would not be plastic enough to mold. After a few minutes&apos; grinding in the wet pans the material is conveyed to the molder, who forces it into the molds by hand. The brick are then dumped on pallets and placed in the drier, where they are left until dry enough to be set in the kilns. Some of the brick are re-pressed before being dried. They are burned about five days, in round down-draft kilns. It is not necessary to have as much heat in the kilns as the brick will be subjected

Jan 9, 1913

By Charles J. McMahon

In a recent paper, Floreen and Hayden report that additions of the noble metals iridium, rhodium, ruthenium, and platinum to Fe-C alloys containing 0.03 to 0.08 wt pct C act to significantly reduce the ductile-to-brittle transition temperature in a notched-bar impact test. They compare these results with the similar, well-known effects of nickel and manganese additions, and they note that this supports the hypothesis that addition of austenite stabilizers enhances notch toughness. Although not attempting to offer an explanation for this, they suggest that it might be found in an alteration of the bonding characteristics of the bcc lattice of iron by additions of elements which tend to stabilize the fcc lattice. While this suggestion appears to have some merit, it should perhaps be held in abeyance until two more likely possibilities have been explored. It is now fairly clear that the beneficial effect of manganese derives from its ability to promote a globular carbide morphology instead of the platelike form found in grain boundaries and pearlite patches in Fe-C al10~s.&apos; Previous work14 has also shown that cleavage fracture in Fe-C alloys of the type tested by Floreen and Hayden originates almost exclusively in the cracking of cementite platelets, and that the ductile-brittle transition temperature is very sensitive to the volume density and size of these carbides. Treatments which lead to development of nonlamellar carbides or fine dispersions of carbides, such as quenching and tempering or appropriate alloy additions, promote toughness by removing the primary mode of cleavage initiation. The effectiveness of manganese in this regard has long been known. Nickel appears to behave in a similar manner, though the effect is perhaps not as dramatic as with manganese.15 However, nickel additions do lead to a definite refinement of ferrite grain size following a given transformation heat treatment, and this in itself acts to greatly enhance notch toughness.&apos;&apos; (The grain sizes of the various heats tested by Floreen and Hayden were not reported, so it is not known how much influence this factor exerted in their results.) In conclusion, it is suggested that one should consider the well-established effects of alloying elements on carbide morphology and ferrite grain size before resorting to more complex possibilities, such as modification of interatomic bonding.

Jan 1, 1969