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By C. L. Dake

Discussion of the paper of. C. L. DAKE, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 103, July, 1915, pp. 1429 to 1436. A. C. LAWSON, Berkeley, Cal.-It appears that our bog-iron ores are due in a large measure to the activity of certain iron bacteria, and a paper dealing with this subject that makes no reference to that particular agency strikes me as rather curious. C. L. DANE, Rolla, Mo.-Mr. Lawson's criticism that this paper makes no reference to the activity, of iron bacteria is scarcely true. On p. 1430 I stated: "Certain bacteria precipitate iron by building the hydrated oxide into their body cells," and again, "There are many other means by which, under special conditions, iron may be precipitated in nature. Oxidation, evaporation of CO2, and iron bacteria have been held to be the most important." Thus the activity of bacteria receives as extended mention as the action of any other agency in precipitation of iron. The paper makes no pretense of covering exhaustively the origin of bog ores, but, as its original title suggested, refers to Some Principles Controlling the Formation and Distribution of Bog Iron Ores. Mr. Lawson seems to have entirely missed the main thesis of the paper, which attempts to establish some relation between glaciation and abundance of bog ores now forming. Unfortunately, I have no immediate access to the literature of the subject, but my best recollection is that the data regarding iron bacteria throw no light whatever on the cause of bog ores being so much in ore abundant within the limits of the glaciated regions, and being reported much less frequently from the tropics. This lack of data is suggested in the following (p. 1434): "It has already been shown that bacteria aid in the precipitation of iron. Whether tropical conditions increase or decrease the activity of such bacteria is unknown."

Jan 12, 1915

By AIME

J. B. Haffner, or "Barney" as he is known to his wide circle of friends, was born at Landskrona, Sweden, on Christmas Day, 1886. He attended grade and preparatory schools there and then went to the Royal Technical Institute at Stockholm from which he graduated as a mining engineer in 1910. During these school years he gained practical experience in his summer vacations by working in various mines in Sweden and other European countries. Upon graduation he set forth for the land of opportunity, the United States. Upon arrival in this country he found people everywhere talking about the fabulous gold fields in Alaska and thereupon set sail for Nome, to take part in placer gold mining operations. Returning to the States, Barney worked in Illinois coal mines for a time and then carried on some construction work in Oklahoma. In 1913 he accepted employment with the Ray Consolidated Copper Co. in Arizona and soon found himself in positions of responsibility in the operating and

Jan 1, 1948

By J. T. Eash, E. M. Wise

MANY of the platinum metal alloys are hot-forged in the early stages of reduction from ingot and substantial quantities of platinum alloys are commercially employed at very high temperatures in ammonia oxidation units, orifices for forming glass rods and fibers and as cathodes in long-life thermionic amplifiers. They are used also for electrical heating resistors, safety blowout disks, thermocouples and crucibles. The tensile properties at elevated temperatures are important in many of these situations but data on the subject are limited. Creep data also are important, but will not be covered at this time. SCOPE AND CONCLUSIONS Tensile tests were carried out at room temperature and elevated temperatures up to 11000 C. on previously well annealed samples of platinum, palladium and several of their important alloys with compositions shown in Table 1. The results are presented graphically in Figs. 1 to 4. The tensile strengths of platinum and the platinum-base alloys (with the exception of the 10 per cent rhodium-platinum alloy) at 1100° C. are from 16.6 to 18.8 per cent of the strengths of the same alloys (well annealed) at room temperature. The strength ratio of the 10 per cent rhodium-platinum alloy is 22.3 per cent, which is appreciably higher than that of the- other materials tested. The tensile strengths of palladium and the palladium alloy at 1100° C. are from 10 to 11.2 per cent of the room-temperature values. The elongations of platinum and its alloys tend to increase at tempera¬tures above 600° to 800° C., while the two samples of pure palladium show a maximum at 600° C.

Jan 1, 1938

By W. A. Stickney, J. W. Town

Tests demonstrated that aqueous solutions of sodiu~n sulfide would dissolve over 95 pct of the cinnabal- in 5 pct Hg flrotation concentrates and 60 to 90 pct of the cinnabav in low-grade ol-es. Double-leach tests showed that potassiutn sulfide would dissolve 90 pct of the avsenic sulfide in Hg-As satnples and only 1 to 10 pct of the Hg; the sodium sulfide would then dissolve 80 to 90 pct of the rernaining Hg and 30 to 70 pct of the vemaining As. 1 HIS paper describes the extraction, by alkaline sulfide solutions, of mercury from cinnabar-bear ing ores and flotation concentrates. Leaching time and solution temperature had minor effects on mercury extraction when compared to the effects of reagent quantity and ore type and grade. Cinnabar, although readily soluble in sodium sulfide, was only partially soluble in potassium sulfide and essentially insoluble in ammonium sulfide. A double leach process was developed to extract selectively the arsenic from Hg-As products with K2S and to treat the residue with sodium sulfide-hydroxide solutions to extract the mercury.' Mercury was then recovered from the pregnant solutions either by precipitation with metallic aluminum or by electrodeposition. The solubility of HgS in alkaline sulfide solutions was first reported by Volhard in 1878.' The first reported commercial application was made in 1915 when Thornhill applied the method to the treatment of an amalgamation tailing.3 Mullhollen, in 1911. described the chemical reaction of HgS with Na,S and alkaline hydrate to be:4 Most investigators have reported using a 4-pct sodium sulfide and a 1-pct sodium hydroxide soluti~n.3-4 An increase in temperature or excessive dilution of the solution causes the reaction to be reversed. Church Holmes described a similar process used for the extraction of antimony from silver concentrates at the Sunshine Mining Company's mill at Kellogg. Idaho.5 More recently. Erspamer and Wells reported the results of leaching studies on a Hg-Sb ore from Alaska.6 EXPERIMENTAL PROCEDURE Leaching tests were made on samples of mercury ore from eight deposits in Oregon, Washington, and Idaho. In addition. tests were made on flotation concentrates from seven of the samples as well as a flotation concentrate from an operating mill. Since previous investigators reported reagent requirements greatly in excess of that required by the equation HgS + Na2S = HgS . Na2S, initial studies were made on chemically pure HgS. Results showed that the reaction actually required about 1 g of Na,S per g of HgS in an aqueous solution rather than 0.338 g of Na,S as indicated by the equation. To check further the matter of reagent requirements, Na2S and HgS were mixed together in equal mole ratios. Water was then added, a drop at a time, until the components reacted; X-ray diffraction analyses showed no HgS nor Na,S present. The yellow hydrate compound which formed would not redissolve until about three additional mole equivalents of Na,S were added to the solution. This indicated that a stable solution would require at least 4 moles of Na2S for each mole of HgS. While these implications may be valid for pure HgS, the possibility of entirely different results caused by the existence of other elements present in ores and concentrates was recognized. Consequently, experiments of the same order were made on samples of a flotation concentrate from a producing mill. The concentrate, containing about 18 pct

Jan 1, 1962

By C. M. St. John

INTRODUCTION The stress redistribution accompanying the excavation of a deep tunnel may induce failure of the rock. The role of the support system is to control the extent of the failed region and hence to limit closure of the tunnel within an allowable amount. In such circumstances, the design of the support system is generally based on the Ground Reaction Curve (GRC). The GRC is the relationship between the support pressure and the induced displacement at the tunnel wall for a circular tunnel under hydrostatic loading. In the calculation of the GRC (see Brown et al. (1983) for an exhaustive list of reference), the rock is generally treated as an elastoplastic material characterized by cohesive-frictional yield strength and by dilatancy during plastic deformation. A recent analytical development (Detournay, 1983) has allowed the generalization of the GRC concept for some cases of non-hydrostatic in-situ stress fields (Detournay and Fairhurst, 1982). As an application of that development, this paper describes design charts that provide powerful means of performing parametric analysis for tunnels subject to non-hydrostatic loading. BACKGROUND The in-situ stress in a plane perpendicular to the tunnel axis can be decomposed into mean and deviatoric components, Po and So (see Fig. 1). Since it is assumed that the rock is characterized by a Mohr-Coulomb yield strength, the deviatoric invariant So must be less than the limiting value Sl0 given by

Jan 1, 1984

By M. F. Fogler

An attempt to duplicate Rawdon and Mutchler's experiments showing a reversal of hardness with continued rolling gave negative results, indicating that the phenomenon is not general but depends, probably, on local conditions of rolling. IN A recent paper, Rawdon and Mutchler1 gave some exceptionally interesting results on the Brinell and scratch hardness of severely cold-worked metals. In their work, they found that, on continued cold rolling, the metal hardened up to a particular point and then reversed and became softer; this was true for both Brinell and scratch hardness values. The generally reported behavior2 of metals, with respect to Brinell tests on cold-worked material, is that the metals harden up to a certain point and then, on further cold rolling, no change in Brinell hardness occurs. Jeffries and Archer3 state that there is little difference between the scratch hardness of annealed and cold-worked metals; the work of Faust and Tammann4 also indicated no difference between-the hardness of annealed and cold-worked copper. Rawdon and Mutchler found, when they plotted the reduction ratio (initial thickness divided by thickness after rolling) against the hardness value for the cold-rolled material, that the hardness number increased up to a reduction ratio of about 3 and then decreased and became even smaller than that for the annealed metal. This behavior was reported for both scratch and Brinell hardness; Figs. 1 and 2 show their results for Brinell hardness on the metals for which they published data. This is an exceptionally interesting phenomenon, if it occurs under all conditions of rolling, and would have an important bearing on the practice of cold

Jan 1, 1925

By Emil Gathmann

(San Francisco Meeting, September, 1915) THROUGH wide experience at numerous mills in the United States I have found that there is a decided difference of opinion among the producers of steel as to what constitutes commercially sound steel. Some metallurgists insist upon having, for certain grades of steel, a so-called "open steel," -i.e., one which contains numerous blowholes of varying sizes, and consequently but little volume of true pipe, although a central intermittent shrinkage cavity often extends well down into the ingot: Such blowholes and pipe are expected to weld up during rolling or forging, because their surfaces are not oxidized. Even if this be admitted, included slag particles and a high degree of segregation are bound to be present in the product of such ingots. Blowholes are the result of an oxidized heat, and all heats, unless made or finished in the electric furnace, are oxidized more or less. Subsequent deoxidation, or rather degasification, either in the ladle or in the mold, or in both, is necessary to reduce or prevent blowholes. As is well known, a greater yield of billets or sheets is secured from the ingot by allowing the formation of blowholes, but this is undoubtedly obtained at the expense of the quality of the product. Decided segregation of carbon, phosphorus, and sulphur, as well as small included slag particles, undoubtedly exists throughout the greater portion of all so-called open steel, and cannot be removed by cropping. The first requisite for sound, homogeneous steel ingots and blooms is therefore, in my opinion, so to treat the steel in the furnace, ladle, and mold that "piping" steel is produced. The line of demarcation between harmful and so-called "harmless" blowholes is practically impossible to define. Is it not, therefore, the better and safer practice to use means for the elimination of blowholes and correspondingly reduce the segregation and allow the formation of a well-defined shrinkage cavity or pipe .at the upper end of the ingot? With the relatively cheap deoxidizers available at the present time, e.g., ferro-silicon, aluminum and titanium,

Jan 8, 1915

By William E. Ford, Edward Salisbury Dana

239, Contact-Gwiorneters. - The interfacial angles of crystals are measured by means of instruments which are called goniometers. The simplest form is the contact- or hand-goniometer one form of which is represented in Fig. 377. This contact-goniometer consists of a card on which is printed a semi- circular arc graduated to half degrees at the center of which is fastened a celluloid arm which may be turned to any desired position. The method of use of the goniometer is illustrated in Fig. 377. The bottom of the card and

Jan 1, 1922

By L. D. Anderson

WHEN, after years of troublous experiences in roasting sulfide ores with heavy dust and fume losses resulting from the equipment and methods first available, there appeared on the scene of metallurgy that revolutionary process known as sintering, it was felt that at last there had been found the ideal method for preparing sulfide ores for blastfurnace reduction. Not only were the sulfides roasted but also the fine oxidized ores were bound together with them in strong porous cellular masses which were in the best possible condition for reduction. With the experiences gained in the manipulation of the Huntington-Heberlein, Carmichael-Bradford, and Dwight & Lloyd processes there developed a refinement of detail which brought the whole plan of roasting by sintering to a high plane of perfection. But that metallurgy is never stationary is revealed by the fact that changes in milling practice, particularly the development of flotation, have introduced a new set of problems in sintering itself. Inasmuch as it is felt that these problems have not yet been solved in an entirely satisfactory manner this paper is written to record the present practice of the Salt Lake Valley smelters with the hope that there will be brought forth such discussios as may perhaps lead to still better practice. By far the greater proportion of the sulfides smelted today are flotation concentrates. Usually they are high grade, sometimes as high as 70 per cent. and more in lead. They are extremely fine, many mills grinding the ore so that from 60 to 80 per cent. will pass through screens of 200 mesh. The physical condition in which many of these concentrates reach the smelters is disconcerting to the metallurgists. Some are of about the consistency of putty. Others are of a sticky, slimy nature. Others again, dried to the limit, are veritable powders. Remembering that the down-draft sintering charge for the best results must be porous enough to let air be drawn through it reasonably well, must be thoroughly mixed, and must have some coarse material in it to segregate out and form a layer on the grates, it will be understood that the advent of this extremely fine material has made necessary still further elaboration in the equipment and processes of preparing sulfides for the blast furnaces,

Jan 1, 1929

By John W. Tieman

Coal is a term applied to vegetable matter (trees, grasses, etc.) which was subjected to heat and pressure through geologic ages. This resulted in a change in both the physical and chemical properties. Because its chemical composition is variable, geologists classify coal as a heterogeneous mineral rather than a homogeneous mineral. Peat represents the initial, unconsolidated stage in the development of coal. This coalification continues with time and the application of temperature and pressure to lignite, subbituminous, bituminous, and anthracite toward the theoretical graphite end member. PHYSICAL PROPERTIES OF COAL The physical properties are concerned with the characteristics of coal in its natural state, or prior to its end use as a fuel. For example, the hardness and grindability of coal determine the maintenance cost for coal mining, handling, and pulverizing equipment; the specific gravity of coal and its associated minerals determines the coal preparation technique used in a cleaning plant as well as the capacity of coal bins, boats and size of cargo, and other coal storage facilities. The physical properties are, of course, dependent on the chemical constituents of coal, and all properties are interrelated. Specific Gravity The specific gravity (sp gr) of a solid is the ratio of the weight of a cubic foot of the solid to the weight of a cubic foot of water. The specific gravity of pure coal has been reported to range between 1.23 to 1.72 and increases with the change in rank from lignite to anthracite. This means that it is 1.23 to 1.72 times heavier than water.

Jan 1, 1981

Recent start-up of a new 3450 t/d (3800 stpd) copper-zinc concentrator complex in northern Manitoba, Canada, is expected to open new reserves and dramatically cut transportation costs for Hudson Bay Mining and Smelting Co.'s Snow Lake operations. The new $C33-million mill is located in Stall Lake, Manitoba, and includes a new crushing and grinding facility and two flotation circuits for the production of 23-25% copper and 55% zinc concentrates. A small amount of lead concentrate will also be recovered. The plant will produce some 145 000 t/y (160,000 stpy) of concentrates, to be shipped by rail to the firm's Flin Flon copper smelter and zinc refinery complex, located 177 km (110 miles) to the west on the Saskatchewan-Manitoba border.

Jan 9, 1979

By Charles H. Moore

In the study of the properties of rutile pigments it became apparent several years ago that certain physical and optical properties could not be determined on particles of pigmentary size. Since reflected light is the dominant type which reaches the eye from small particles, the true color of pure rutile was not known. Most rutile pigments are acicular in habit, elongated parallel to the "c" axis. It was considered important to know the nature and tone of light transmitted, for example, by a basal plate. Further, as shown by spectrophotometric curves, there is a very strong absorption of light of 4000 k as measured on particles with random orientation. It would be interesting to see whether this absorption position varied with predetermined and selected orientations. Also, since the behavior of titanium pigments in a vehicle is important, a knowledge of the surface wettability of single crystals by various media should prove very fruitful. Finally, the optical properties of rutile are such that it should show, in a single pure crystal, greater fire and brilliance than the diamond. Mineralogists had long speculated that this would be the case and curiosity was strong to produce a single crystal large enough to cut.

Jan 1, 1949

By Ernest F. Burchard

The Pao deposits of iron ore are in the State of Bolivar, Venezuela, near Upata, about 30 miles south of the Orinoco River and 90 miles east of Ciudad Bolivar. They were discovered 4 or 5 years ago and have not yet been developed to the stage of mining. In March-April, 1929, the writer devoted a week to the examination of these deposits. The maps, drill records and chemical analyses presented herewith were derived from original sources, and the field photographs were made by the writer. The petrographic and metallographic data are from notes by C. S. Ross and M. N. Short, of the U. S. Geological Survey, who have kindly collaborated in these special phases of the study. The Iron Obebodies Topography and Accessibility The deposits are in a region of low mountains representing northern outliers of the Guayanan Highlands. These mountains reach altitudes of 1800 to more than 2000 ft. above sea level, as determined by aneroid barometer. The iron ore is found on mountain crests that reach altitudes of 1915 to 1930 ft., and may be followed down precipitous slopes for 200 • to 300 ft. or more. The greatest vertical range in outcrop is nearly 400 ft., and drilling has indicated that the ore extends to this depth below the surface in one place, at least. The superior hardness of the iron ore accounts for the preservation of the local mountain crests with the intermediate valleys eroded in softer granitic rock. The deposits of iron ore are reached by a private road for automobiles branching northeast from the Ciudad Bolivar-Upata road, a distance of about 12 miles. This road was used in 1928-29 by trucks for transportation of food and camp supplies, gasoline, drilling equipment, etc., but was not suitable for the transportation of iron ore. Between Ciudad Bolivar and the iron-ore area the western two-thirds of the automobile road passes through nearly level, open country known as the savanna, largely used for grazing cattle. About 96 km. (60 miles) east of Ciudad Bolivar at

Jan 1, 1931

By H.A. Schwartz

From time to time, one of the authors has had occasion to investigate the graphitizing reaction and has published the results mainly as discussion' of the work of other investigators. In view, therefore, of the diversity of both observations and interpretation, it seemed well to attempt, a revision of the entire subject in the Research Laboratory of the National Malleable Castings Co. The work consisted of a careful study of a single, impure, iron-carbon alloy. The material, which may be considered typical low-carbon white cast iron of the malleable industry, was an air-furnace iron of the following composit,ion: carbon 2.30 per cent., silicon 1.20 per cent., manganese 0.29 per cent., phosphorus 0.156 per cent., sulfur 0.048 per cent. The freezing range extended from 1213' to 1132' C., the latter figure agreeing with Gontermann's data.2 We have attempted to define the equilibrium diagram of this alloy, in the stable condition as related to the mctastable diagr,aui,- from a temperature somewhat below the euteetic freezing point to a temperature l>clow Arl and for a graphitic-carbon content from practically notliing to the original total rarbon of the specimen (see Fig. 6). More csp~c~ially we desired to locate the line in the stable diagra~n corrcspo~idi~lg to thc Ac, line of the metastable syst,ern, which is designated by analogy, thc At, line (t, from tcrnpcr carbon); also to dctermirle the locat'ion of A tm witah respect, to Acm t,o~vard their lowcr extremities at Arl in ordei to determine whether or not graphitization is completed by th~ separation of an iron-carbon entectoid analogous to pearlite in the iron-cementite system. This would involvc furthcr a colnparison of thc locations of Ihc stablc and met.astable 41 points. As the carbon concelltrations of thc solid solutions of the two syste~~ls are probably not, identical, an explanation of t>lieir differences and of thc,

Jan 1, 1923

By H. A. Schwartz

From time to time, one of the authors has had occasion to investigate the graphitizing reaction and has published the results mainly as discussion' of the work of other investigators. In view, therefore, of the diversity of both observations and interpretation, it seemed well to attempt, a revision of the entire subject in the Research Laboratory of the National Malleable Castings Co. The work consisted of a careful study of a single, impure, iron-carbon alloy. The material, which may be considered typical low-carbon white cast iron of the malleable industry, was an air-furnace iron of the following composit,ion: carbon 2.30 per cent., silicon 1.20 per cent., manganese 0.29 per cent., phosphorus 0.156 per cent., sulfur 0.048 per cent. The freezing range extended from 1213' to 1132' C., the latter figure agreeing with Gontermann's data.2 We have attempted to define the equilibrium diagram of this alloy, in the stable condition as related to the mctastable diagr,aui,- from a temperature somewhat below the euteetic freezing point to a temperature l>clow Arl and for a graphitic-carbon content from practically notliing to the original total rarbon of the specimen (see Fig. 6). More csp~c~ially we desired to locate the line in the stable diagra~n corrcspo~idi~lg to thc Ac, line of the metastable syst,ern, which is designated by analogy, thc At, line (t, from tcrnpcr carbon); also to dctermirle the locat'ion of A tm witah respect, to Acm t,o~vard their lowcr extremities at Arl in ordei to determine whether or not graphitization is completed by th~ separation of an iron-carbon entectoid analogous to pearlite in the iron-cementite system. This would involvc furthcr a colnparison of thc locations of Ihc stablc and met.astable 41 points. As the carbon concelltrations of thc solid solutions of the two syste~~ls are probably not, identical, an explanation of t>lieir differences and of thc,

Jan 1, 1923

By John Mark Patek

Knowledge of the relative floatability of silicate minerals is increasing in importance as flotation is being applied to the concentration of nonsulfides. Many silicates are in themselves commercial products amenable to concentration by flotation. Moreover, the selective flotation of other nonsulfide minerals, such as cassiterite, depends largely upon the floatability of associated gangue silicates. Differences in floatability existing between the various silicates have not- been sufficiently appreciated; for example, the feldspars that differ greatly in floatability have generally been merely treated as "feldspar." It was the purpose of the work described in this paper to determine by experiment the differences in floatability between silicates; to investigate the causes for such differences, and to discover a means of predetermining approximate floatability without the necessity of experimentation. Determining Floatability The relative floatability of 20 silicates so selected as to represent all of the more common silicate types1 was obtained by flotation tests enumerated in Table 1. The mineral to be floated was crushed dry on a steel plate, and screened repeatedly during crushing through an 80-mesh screen in order to produce a sand with all grains as close to 80 mesh as possible. The sand was placed in dilute (6N) hydrochloric acid until free of soluble foreign material, and then washed with tap water about ten times in order to remove both acid and fines. The resultant product, which averaged 82 per cent plus 200 mesh, was floated in 50-gram charges in a 50-gram Denver celluloid flotation machine with 0.008 gram of terpineol, and from 0.01 to 0.05 gram of oleic acid in a solution acidified with sulfuric acid. The degree of separation of one mineral from another was determined by counting under a nlicroscope the grains of each mineral, both in the concentrate and in the tailings, and comparing their relative abundance in each. Unless the comparison showed a decided difference in amount,

Jan 1, 1935

By George A. Laird

THIs old and once famous district played, through its enormous production of silver and gold, an important part in the history of the State of San Luis Potosi. According to a pamphlet prepared under the direction of the Governor of the State, Sr. Don Blas Escontria, and presented to the visiting members of the Institute during the Mexican meeting of 1901, this district is situated 20 km. east of the city of San Luis Potosi, in a range of mountains of moderate height, extending 135 km. N. and S., and 16 km. E. and W.; and the mineralized area hitherto developed is about 600,000 sq. m. The history of the district, as given by the record dated 1778, and formerly kept in the Sail Francisco convent, says that it was discovered in 1575 by Sr. Don Pedro Irarte, and adds that the city of San Luis Rey de Francisco de1 Potosi received its name (in allusion to the famous Potosi mines in Bolivia) by reason of the remarkable productiveness of its gold- and silver-mines in the first period of their exploration, during which they paid to the Crown, as quintos (the fifth part of the product), $97,000,000, as appears from the accounts of the royal treasury. The amount of the quintos paid during the " bonanza period " of 80 years was $72,000,000. The larger sum first mentioned probably represents a longer series of years. But either will suffice to indicate the great wealth of the mines. In 1663, the decadence of the industry began with the caving-in of several mines, concerning which the record of 1778, already cited, says, in substance, that on Good Friday one of the owners in the enterprise, in view of the unfavorable prospect of a lawsuit in which he was engaged, set fire to the timbers supporting the underground galleries and workings of the Sail

Jan 1, 1905

By O. N. Carlson, D. G. Alexander

THE hardness anisotropy of metals and alloys has been of increasing interest in recent years but silicon ferrite,1 niobium,2 and tungsten3,4 are the only bcc metals about which this type of information has been reported. This investigation was carried out on vanadium and chromium single crystals in an effort to determine to what degree the hardness variations observed in these metals are due to orientation effects and to compare their behavior with other bcc metals. In earlier work the authors had observed a small angular dependence in the Diamond Pyramid Hardness of single crystalline vanadium on the (100) plane but no anisotropic effects were noted on either the (110) or (111) planes. At the suggestion of R. G. wheeler5 it was decided to investigate this effect in greater detail using the more asymmetric Knoop indentor. The vanadium metal used in the study was prepared by the aluminothermic reduction of V2O5 followed by electron beam melting.6 The principal analyzed impurities were 230 ppm C, 230 ppm O, 65 ppm N, 90 pprn Al, Cr not detected, 50 ppm Fe, 60 ppm Ni, and 200 ppm Si. The chromium was an iodide-refined product obtained from the Chromalloy Corporation. Analysis of this material showed the following amounts of impurities present: 10 ppm C, 9 ppm O, 2 ppm N, 0.4 ppm H, 3 ppm Al, 2 ppm Ca, 2 ppm Cu, 20 ppm Fe, 1 ppm Mg, 0.3 ppm Mn, 1 ppm Mo, 3 ppm Ni, 10 ppm Si, and 1 ppm V. Single crystals of both metals about 1 cm in diam and 10 cm in length were grown by an arc-zone melt- ing technique.7 The chromium crystal was annealed at 1600°C for 6 hr in a purified argon atmosphere to remove any strains or inhomogeneities, but the vanadium was tested in the as-grown condition. The crystals were oriented by the Laue back-reflection method and then sectioned with a spark cutter into individual specimens with a (loo), (110), or (111) plane parallel to the crystal surface. They were mounted in Lucite and carefully ground to a flat surface. The vanadium specimens were then electropolished in a 6 pct perchloric acid-methanol mixture while the chromium specimens were mechanically polished on a Syntron vibratory polisher using an alumina abrasive. The orientation of each crystal was then rechecked by the back-reflection X-ray method. All of them were found to lie within 2 deg of the desired orientation with the exception of the (110)-Oriented chromium crystal which was within 4 deg. Microhardness impressions were taken at 10 deg intervals from the common (110) direction by rotating the crystal in the plane of the crystal surface. A Knoop indentor was used with a 400-g load on the vanadium crystals and an 800-g load on the chromium. The hardness values are averages of 6 impressions and standard deviations were calculated for each set of data. The values reported for the (111) plane of vanadium are based on from 10 to 15 measurements for each point. The microhardness results for vanadium and chromium are plotted as a function of the angular rotation of the long axis of a Knoop indentor from the (110)

Jan 1, 1970

By J. E. Hanlon, S. R. Butler, R. J. Wasilewski

It is known that stoichiometric NiTi transforms to a structure of lower symmetry near room temperature. The present investigation deals primarily with the changes in the electrical and magnetic properties which occur at the transformation. The effects of composition and various heat treatments on electrical properties are also discussed. In recent investigations by Purdy and Parr,' Wang et a1.,2 Dautovich and Purdy,~ Dautovich et a1.,4 and the authors, ~,' NiTi has been observed to undergo a martensitic phase transformation from the ordered CsCl (B2) structure to one of lower symmetry. The crystal structure of the low-temperature modification is still not completely worked out. This transformation occurs near room temperature for the stoichiometric composition. The thermodynamic, elastic, crystallographic, and microstructural characteristics of this transformation for some compositions have been previously reported.'-= In the present investigation, the changes in the electrical transport properties and magnetic susceptibility of NiTi when it undergoes the martensitic phase transformation have been measured. The approximate composition range covered is 48 to 52 pct Ti.* *All compositions are given in atomic percent._____________________ EXPERIMENTAL PROCEDURES AND RESULTS 1) Sample Preparation. The NiTi alloys were prepared from iodide titanium (>99.92 pct Ti) and vacuum-premelted carbonyl nickel (>99.95 pct Ni) by repeated arc melting under gettered argon and casting in a water-cooled copper mold. After the cast buttons were hot-forged at 800" to 950°C, the oxidized surface was removed by grinding and etching. Samples were cut from the worked polycrystalline buttons. After fabrication, the samples were annealed 1 hr at 900°C and water-quenched. The composition of the alloys was assumed to be the same as in the initial feed. This assumption was supported by material balance checks on 100-g arc-melted buttons which demonstrated quantitative recovery to within k0.02 pct. The oxygen content of the alloys was '150 ppma (weight) and the carbon content was 30 to 50 ppm. 2) Electrical Resistivity and Hall Effect. The electrical resistivity was measured over the composition range 48 to 52 pct Ti for temperatures varying from 4.2"K to 900°C. The high-temperature and many of the low-temperature experiments were carried out using conventional 4-probe dc techniques.7 The Hall coefficient and ac resistivity were measured at 20 cps using the apparatus shown schematically in Fig. 1. The equipment is basically an ac potentiometer: The resistive or Hall voltage of the sample is balanced by a comparison voltage provided by a dividing network across a standard series resistance. The off-balance signal is amplified by a Tektronix 122 amplifier and detected by a Princeton Applied Research (PAR) phase-sensitive detector. The precision of the resistivity and Hall coefficient measurements is i0.1 and i3 pct, respectively. The uncertainty in the data is increased by i2 pct from the precision limits because of uncertainty in dimensions and possible end effects. The temperature dependence of the electrical resistivity and Hall effect for a stoichiometric (50.0 pct Ti) NiTi sample are illustrated in Fig. 2. Above 75"C, this sample has essentially the B2 structure, while below about 0°C it is completely in the low-tempera-

Jan 1, 1968

By W. J. Helfrich, C. L. Sollenberger

Many present direct reduction processes utilize iron ore concentrates for the production of sponge iron and the sponge iron is usually preferred as an agglomerate. Pelletizing a high grade iron oxide concentrate prior to reduction is a simple approach to the high capacity production of a uniform and agglomerated sponge iron product. The present paper describes the effect of different atmospheres and physical characteristics on the reduction of pelletized iron oxide concentrates. The kinetics of iron oxide reduction have been I studied by numerous investigators1-4 and a rate equation for the hydrogen reduction of hematite and magnetite has been proposed. Mc Kewan' obtained kinetic data for the reduction of hematite spheres sintered at 13'70°C (2498'F'). The kinetics of magnetite reduction was studied by Quets. He compacted the oxide at a pressure of 1 ton per sq cm and sintered the specimens to densities of 95 to 96 pct of theoretical. These studies demonstrated that the reduction of iron oxide is a topochemical process and that the rate of reduction is proportional to the receding surface area of remaining iron oxide. Thus, the measurement of the kinetics of iron oxide reduction depends upon the development of a measurable and well defined interface between metal and reacting oxide. It is evident that the reduction rate will be constant only when the rate of formation of the reaction product layer is constant. It was recognized by Joseph' and Edstrom' that the physical character of the oxide will determine the configuration of the interface between oxide and metal. The reduction of oxides which exhibit few pores or no interconnected pores should proceed by topochemical processes. However, if a massive or dense crystalline ore cracks during the reduction of the oxide, thus allowing the reduction to Proceed away from a well defined oxide/metal interface, then the observed reduction rate will vary or change during reduction. From a process standpoint, it would be difficult to apply absolute reduction rates determined for crystalline or nonporous iron oxide to the direct reduction of a porous pellet of iron ore concentrate. Most present direct reduction processes are attempts to utilize iron ore concentraates in the production of sponge iron. The sponge iron is usually preferred in an agglomerated form for subsequent melting practices. Pelletizing a high grade iron oxide concentrate prior to reduction is a simple approach to the high capacity production of a uniform and agglomerated sponge iron product. One process for preparing such a product has already been de-scribed. This paper describes the effect of different atmospheres and physical characteristics on the reduction of pelletized iron oxide concentrates. ORE CONCENTRATES STUDIED A magnetite concentrate from Reserve Mining Co. and a hematite concentrate from U.S. Steel Corp. were used in preparing pellets for these experiments. A head analysis of these concentrates is given in Table I. To compare the reduction rates of pelletized concentrates, it was necessary that each pellet contain equal amounts of oxygen which could be removed by reduction, regardless of the oxidation state, i.e., Fez% or Fe304. Also, because of the difficulty in preparing spherical pellets of uniform size, weight, density, and porosity for experimental purposes, pellets of a cylindrical shape were formed in a press.

Jan 1, 1961