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By R. A. Vandermeer, J. C. Ogle

The preferred crystallographic orientations (texture) developed in randomly oriented, poly crystalline niobium during rolling were studied by means of X-ray diflraction techniques. The evolution of texture at both the surface and center regions of the rolled strip was carefully examined as a function of increasing defamation throughout the range 43 to 99.5 pct reduction in thickness. Certain aspects of the center texture development in niobium are in agreement with the predictions of a theory by Dillamore and Roberts, but others cannot be explained by the theory in its present form. Above 87 pct reduction by rolling, a distinctly different texture appeared in the surface layers which was unlike the center texture. The present results are compared with previous results obtained from other bcc metals and alloys. RANDOMLY oriented, poly crystalline metal aggregates when plastically deformed to a sufficiently large extent develop preferred orientations or textures. In a recent review article, Dillamore and Roberts1 pointed out that the nature of the developed texture may be influenced by a large number of variables. These include both material variables such as crystal structure and composition and treatment variables such as stress system, amount of deformation, deformation temperature, strain rate, prior thermal-mechanical history, and so forth. From a practical point of view, the control of preferred orientation may often be important for the successful fabrication of metals into usable components. During the past few decades many experiments have been devoted to the study of deformation textures. This work, however, has been confined in large part to metals and alloys that have an fcc crystal lattice. By comparison, bcc metals and alloys have received much less attention, and consequently our understanding of preferred orientations in these materials is only shallow. This state of affairs worsens when it is realized that almost all of our present howledge about this class of materials derives from studies on irons and steels.' The bcc refractory metals, which are relative newcomers to the industrial world, have, on the other hand, been given at best only passing glances in the area of texture development. Our understanding of the evolution of preferred orientations in bcc metals can only remain fairly limited until systematic studies of metals and alloys other than the irons and steels have been carried out and the influence of the many variables has been determined. To that end a program was initiated to investigate in detail texture development in niobium. The present paper reports some of the results of this study. Textures were determined at both the center and surface of strips rolled variously to as much as 99.5 pct reduction in thickness at subzero temperatures. Emphasis in this paper is on texture description and on texture evolution during rolling to progressively heavier deformation. EXPERIMENTAL PROCEDURE The niobium was purchased from the Wah Chang Corp. as a 3-in.-diam electron-beam-melted billet. Chemical analysis indicated the impurities to be less than 300 ppm Ta, 40 ppm C, 10 ppm H, 170 ppm 0, and 110 ppm N. All other impurities were below the limits of detection by spectrochemical analysis. This large-grained billet was fabricated into specimen stock so that a fine-grained randomly oriented grain structure resulted. This was accomplished in three deformation steps alternated with recrystalli-zation anneals of 1 hr at 1200°C in a vacuum of low 10"6 Torr range after each deformation step. The first step was to alternately compress the billet 10 to 20 pct in each of three orthogonal directions. The second step was to compress in only two directions 90 deg apart to produce a 2-in.-sq bar. The final step was to roll this bar 50 pct to give a 1-in. by 2-in. cross section. After the final anneal, metallo-graphic examination showed the material to have an average grain size equivalent to ASTM No. 5 at 100 times (i.e., 0.065 in. diam). Specimens cut from the center and edges of this bar gave no indication of detectable preferred orientation when examined by X-ray diffraction. Samples 1.5 in. long, either 0.625 or 0.750 in. wide, and approximately 0.400 in. thick were machined from this fabricated ingot. The surfaces corresponding to the rolling planes were ground so as to be parallel. The samples were chemically polished in a solution of 60 pct nitric acid and 40 pct hydrofluoric acid (48 pct solution) prior to rolling to remove any cold work introduced in the machining operations. Rolling was accomplished with a 2-high hand-operated laboratory rolling mill that had 2.72-in.-diam rolls. Prior to operation, the rolls were polished with 600 grit paper, cleaned with acetone, and then soaked in a container of liquid nitrogen for several hours. The samples were also soaked in liquid nitrogen prior to rolling and were recooled between each pass. While some slight heating of the samples occurred during rolling, this procedure maintained the sample temperature well below 0°C at all times. The samples were rolled unidirectionally, and the rolling plane surfaces were not inverted during any phase of the operation. The draft per pass averaged between 0.010 to 0.012 in. After 96 or 97 pct reduction the draft was reduced to 0.001 to 0.002 in. per pass. Samples were rolled to various reductions in thickness between 43 and 99.5 pct.

Jan 1, 1969

By R. R. Jones, R. W. Kraft

Zn-Mg2Znn eutectic alloys nzay freeze willr either rodlike or lanzellar rnorphology. Alloys with slighlly more than /he eutectic arrzount of rnagnesillrn usually contain three-cnned dendrjles of MgzZnll in a eutec-lic ttlulris. All three morphologies haue the same cryslallographic orientution relationship: (0UOl) zn - 11 (111) Mg2Znll and (2310)Zn 11(101) Mg2Znll, but u3ith different prej-erred groulth direclions. The lurnellae lo rods transifion in con/rolled ingols qf euleclic cotnposition occurs because lhe large kinelic undercooling due to MgzZnll minirrzizes /he ejj-ecl of the solid-solid inlerface energy. The eutectic morphology is influenced by the presence of lhree-nned dendrites 0-f MgzZn11 which may conlrol /he rricroslrccture by acting as nuclealion sites. In recent years there has been much interest in eutectic solidification and several theories have been proposed. One of the confusing factors is the existence of various morphologies in which the solidified phases may form. The lamellar microstructure seems to be most common in metal eutectics, and it has been claimed' that all regular eutectics should be lamellar if sufficiently pure. However, there still remain eutectic alloys which are not lamellar or which change their morphology as a function of growth conditions. The eutectic between zinc and the intermetallic phase Mg2Znll was chosen for this investigation because it has been found to solidify in more than one morphology. The diagram in anssen' locates the eutectic point at 3.0 wt pct Mg and 367°C. lliott gives 364°C as the eutectic temperature, leaving the phase compositions unaltered. Since the growth conditions determine the micro-structure of the solidified alloy, the factors controlling the transition from one morphology to another could be studied. The lamellae to rods transition is of particular interest. PROCEDURE Alloys were prepared from carefully weighed portions of 99.999 pct Zn and 99.97 pct Mg by melting in Pyrex containers under argon and casting into graphite boats. The resulting ingots were remelted under argon and solidified unidirectionally in a horizontal tube furnace at growth rates ranging from 2.0 to more than 50 cm per hr under a temperature gradient, measured over a 5-cm length, of 9" to 14°C per cm. The solid-liquid interface appeared to be planar at all growth rates although no attempt was made to confirm this by decantation or quenching. A few ingots were allowed to freeze uncontrolled. Most alloys were of the nominal eutectic composition, 3.0 wt pct Mg according to Hansen2 and lliott, but some contained as much as 3.35 wt pct Mg. Chemical analyses were not run since metallographic examination confirmed that the desired composition was achieved. Specimens were cut from the middle portion of the ingot normal to the growth axis, polished mechanically, and etched with 2 pct Nital. Suitable areas were selected for the determination of crystallographic orientation relationships by a tiontechniqueof described previously by one of the authors.4 The (2310) planes of zinc and the (8701, {944}? (1032) planes of Mg2Znll were found suitable for orientation determination; experimental error was on the order of 2 or 3 deg. RESULTS Three different morphologies were found in the unidirectionally solidified alloys: lamellar eutectic, rod-like eutectic, and a structure whose most predominant characteristic was the presence of three-vaned (cellular) dendrites of Mg2Znll. These dendrites were only found in alloys with more than the eutectic amount of magnesium. In some ingots fine hexagonal needles of Mg2Znll surrounding a core of MgZn2 were observed. They were probably due to incomplete alloying and seemed to have no effect on the eutectic morphology. In addition hexagonal spirals like those discussed by Fullman and wood5 and Hunt and acksonh ere observed in some ingots frozen without directional control. Both MgZZn,, and MgZnz were detected by X-ray diffraction in these alloys. Since the morphology could not be grown unidirectionally and no characteristic orientation relationship between the phases was found, further study was limited to the lamellar: rodlike, and three-vaned dendrite morphologies. Alloys of Eutectic Composition, No Dendrites. The mcrostructures of allovs with no three-vaned dendrites were either lamellar or rodlike depending on the growth rate. At rates below 10 cm per hr the morphology was lamellar, consisting of two sets of parallel plates intersecting at about 54 deg like the Mg-MgzSn eutectic described by raft.7 At growth rates faster than 14 cm per hr the microstructure showed rods of zinc in a matrix of MgnZnll, while intermediate rates yielded mixtures of rods and lamellae in small groups. The lamellar "grains" were often several millimeters in cross section, but contained small irregular areas which divided each grain into perfect islands 100 or 200 p in diam. Lamellae were parallel to each other throughout the grain in spite of these defects in the structure, Fig. 1. Rods, on the other hand, could only be produced in small groups arranged like fish scales and separated by irregular areas of appreciable thickness, Fig. 2. Alloys Not of Eutectic Composition, With Dendrites. In alloys with 3.1 to 3.35 wt pct ME,-. three-vaned dendrites bf MgzZnll were usually found surrounded by eutectic. At growth rates slower than about 10 cm per hr the dendrites were separated from each other by small areas of both lamellar and rod eutectic, Fig. 3.

Jan 1, 1969

By G. H., Wigton

THE present milling operations of the Chief Consolidated Mining Co. consist- of flotation of oxidized minerals from siliceous ores of the Tintic Mining district, Utah. As the lead, silver, and gold minerals that give the ores economic value are almost entirely oxidized; their successful flotation has necessitated the solution of many new problems. Laboratory effort resulted in the selection of a, natural float for the oxidized minerals. 'By "natural float," I mean that no reagent was added to produce a sulfide film on the osidized minerals before or while subjecting them to flotation operations. As compared to methods involving sulfide filming, the natural float was selected because it promised successful treatment of a larger variety, of ores without change in quantity or kind of reagents, as well as a better economic balance between metal recovery and concentration ratio. In explanation, I can, state that with sulfide filming, the efficiency of the method decreases rapidly with increase of hydrated, iron osides in the ore, whereas with the natural float the same effect has not been noted. Evidence shows that although sulfidizing can produce greater metal recoveries, it yields a concentrate so much lower in grade that no advantage results.

Jan 1, 1928

By K. L. Sehgal

Minerals are the basis of modern civilization: their exploitation and effective utilization are a yard- stick for measuring the comparative prosperity of different nations. This is particularly true in India where industrialization is just beginning to pick up speed. Production targets for our Fourth Five Year Plan (1966-71) are far ahead of the figures for, say, 1950 (the year we won independence) and show the extent of the expansion. Many problems remain to be solved, not least of which is the shortage of raw materials. India is no novice at utilizing minerals. Archaeological ruins at Harappa and at other historical places in the country show evidence of the fact that the ancient Indians not only knew the art of winning minerals from the ground over 6000 years ago-they were also well acquainted with metallurgy. Some of the present sites of mineral exploitation are the same as those our ancestors worked for many centuries.

Jan 9, 1965

By L. O. Bieber, L. H. Martin

DIFFERENT MELTS OF THE same type of nickel and high-nickel alloys, while having almost identical mechanical properties at room temperature, may have widely varying hot malleability. Either the upper limit or burning temperature may vary or a variation in malleability may occur within the temperature limits normally encountered during hot working. Melts which have reduced hot malleability of the latter type, are said to have a "hot short" range. Examination of melting records and chemical analysis of these heats fails in most cases to show the reasons for these variations. In May, 1930, an investigation was started to determine if a quick and accurate method of hot-malleability testing could be developed which would predict the ability of the metal to withstand hot forging and hot rolling by standard mill practices. The results obtained were so satisfactory that from that time on, all melts of nickel and high-nickel alloys produced in the International Nickel Company's Huntington, W. Va. Works have been tested when hot malleabilty was an important factor. To date, over 63,000 commercial melts of Monelt † nickel, Inconel† and other high-nickel alloys have been tested and the test data compared with processing results. As the result of experience gained in over sixteen years, two standard methods of hot malleability testing have been adopted.

Jan 1, 1948

By E. H. Dix, F. Keller

The use of magnesium as an alloying element in aluminum alloys has been limited, in general, to comparatively small quantities. In duralumin-type, strong aluminum alloys, magnesium is present to the extent of 35 to 3/4 per cent. and various grades of Magnalite and the "Y" alloy of the National Physical Laboratory of England contain up to 1 1/2 per cent. In this country small quantities of aluminum alloy sheet containing 4 per cent. magnesium are produced commercially. All commercial aluminum contains sufficient silicon to convert a portion of the magnesium added to the compound Mg2Si. It is well known that the solubility of both magnesium and magnesium-silicide decrease with decrease in temperature. It is, therefore, impossible to separate the age-hardening effect of the magnesium-silicide from that of magnesium, except by the use of aluminum of such high purity that the silicon content is negligible. The present paper is the fifth l, 2, 3, 4 of a series from the laboratories of the Aluminum Co. of America reporting the results of investigations of the equilibrium relations in aluminum-rich alloys made from the high-purity aluminum manufactured by this company. 5 Previous Investigations A number of investigations have been made of the constitution of the complete aluminum-magnesium system and several determinations made

Jan 1, 1929

By F. Keller, E. H. Dix

The use of magnesium as an alloying element in aluminum alloys has been limited, in general, to comparatively small quantities. In duralumin-type, strong aluminum alloys, magnesium is present to the extent of 35 to 3/4 per cent. and various grades of Magnalite and the "Y" alloy of the National Physical Laboratory of England contain up to 1 1/2 per cent. In this country small quantities of aluminum alloy sheet containing 4 per cent. magnesium are produced commercially. All commercial aluminum contains sufficient silicon to convert a portion of the magnesium added to the compound Mg2Si. It is well known that the solubility of both magnesium and magnesium-silicide decrease with decrease in temperature. It is, therefore, impossible to separate the age-hardening effect of the magnesium-silicide from that of magnesium, except by the use of aluminum of such high purity that the silicon content is negligible. The present paper is the fifth l, 2, 3, 4 of a series from the laboratories of the Aluminum Co. of America reporting the results of investigations of the equilibrium relations in aluminum-rich alloys made from the high-purity aluminum manufactured by this company. 5 Previous Investigations A number of investigations have been made of the constitution of the complete aluminum-magnesium system and several determinations made

Jan 1, 1929

By A. D. Zunkel, A. H. Larson

Equilibrium antimony contents of pb-sb alloys in contact with PbO-Sb2O3 slags containing less than 45 mole pct Sb203 uleve determined at 650', 700°, and 750°C in an inert atmosphere. In this ten~pevature range, the antimony contmzt of the alloy increased with increasing temperature at all slag compositions. The PbO-Sb203 phase diagram below 28 mole pct Sb2O3 was determined by thermal analysis and by application of a log sbZ4/y$b0 us plot determined from the equilibrium-activity data. The resulting phase diagram showed a eutectic at a temperature of 604°C and a comfiosition of 21.6 mole pct Sb2O, with a maximum terminal solid solubility of Sb203 in PbO of 5.6 mole pct. These results are compared with existing data in the literature. In the past three decades, only a small amount of experimental work has been done on the slag-metal equilibria in the Pb-PbO-SbaO3 or the analogous arsenic and tin systems. These systems are important in commercial lead-refining processes such as softening and dross fuming since it is impurities such as antimony, arsenic, and tin in lead bullion and Sb2O3, As2O3, and SnOz in lead drosses which must be re-

Jan 1, 1968

By Stanley Lefond

Industrial Minerals, often called the Cinderella Minerals or the Building Blocks of industry continued their growth patterns through 1973, although profits were slightly lower due to the cost-price squeeze. Most of the individual reports which follow indicate growth rates of 3-15%. Surprisingly such commodities as sulfur held firm in spite of the over supply in the Canadian gas fields; cement was in short supply while the asbestos industry reported a worldwide shortage of group 4 and 5 fibers. Talc and perlite production set new records. In synopsis, 1973 was a productive year for industrial minerals. However 1974 onward appears to be one of contradiction. The unsettled conditions of world economics, the energy shortage, compounded by the Arabs oil embargo have created great problems for all industries. The high energy consuming segments of the Industrial Minerals field will be under intense pressures. On the other hand limestone, lime and perhaps trona, nahcolite might be consumed in ever increasing tonnages in SO2 removal systems connected with smelters and coal-fired power stations. The effects of the proposed changes in the staking, claiming and exploitation of federal lands by the BLM may also have serious repercussions not only to the industrial minerals field but to the entire mining industry. 1974-1975 will certainly be ear-marked as a year of frustrations and difficult decisions.

Jan 2, 1974

By J. S. Koehler, F. Seitz

THE dislocation theory of plastic flow originated in 1928, when Prandtl1 suggested that the internal damping of metals of plastic origin might arise from the motion of a crystalline imperfection. Following this, Dehlinger2 employed a similar imperfection in a theory of recrystallization. The first detailed theoretical discussions were those of E. Orowan3 and G. I. Taylor4 in 1934. The resulting theory was gen- eralized by J. M. Burgers5 in 1939. Mott and Nabarro, in England, and Seitz and Read,6 in the United States, started an extensive examination of the atomic theory of dislocations in the period between 1939 and 1941. However, this development was arrested by the mar and was not taken up again until after 1945. Since 1946, the field has been the object of very intense activity, particularly in the United States and England. Dislocations are beautiful and intricate imperfections; they are sufficiently complicated to account for the great variety of phenomena encountered in the field of plastic flow. Above all, the dislocation concept enables us to understand how a metal or other plastic solid can deform inelastically under very small stresses at temperatures far below the melting point. Suppose we attempt to shear a perfect crystal plastically. This can be done by sliding one entire atomic plane simultaneously through one atomic distance with' respect to the near-

Jan 1, 1954

From the beginning to the end, the attendance and enthusiasm of the 119th meeting, which was held in New York, Feb. 17 to 20 surpassed all expectations. Besides the ten technical sessions, one of which was in conjunction with the American Institute of Electrical Engineering and one a session of the National Research Council, there were two memorial meetings, one for Dr. Raymond and one for the members who died in service; two joint sessions with the Canadian Mining Institute; and a meeting devoted to pictures of copper mining, milling, and smelting. Of the 732 persons registered, 119 registered in the Institute of Metals Division. Monday's sessions were devoted to the problems of industrial organization, the Institute of Metals Division, and to petroleum and gas. Among the special features of these sessions were the topical discussions on housing and. Americanization. Americanization, too, was the topic for discussion by the Woman's Auxiliary Wednesday morning. On Tuesday, nearly 100-members of the Canadian Mining Institute were present to discuss the possibility of bringing about uniform mining laws for the United States, Canada, and Mexico, to obviate the maintaining separate legal departments and managerial forces for the several countries; and to avoid the confusion which, it is said, has led to a duplication of effort and has sometimes created a barrier to international cooperation in mining. Among the Canadian delegation were D. B.

Jan 3, 1919

By Henry Rawdon

ONE of the most vital problems in the manufacture of steel at present is the occurrence of the defects that have been popularly termed "snow flakes," "flakes," or "scabs." Particularly is this the problem of many manufacturers who during the past 2 yr. have undertaken large-scale production for the first time. A study of the microstructure of such defective material throws considerable light upon the nature of these defects and is essential before measures may be taken for the elimination of the defects. Flakes do not appear to be found in the plain carbon steels; they have been found, however, in abundance in some of the simple alloy steels that are being used in such vast quantities; viz., nickel steel of the approximate composition, 0.40 carbon and 3.5 per cent. nickel, and in the chrome-nickel type. The present article summarizes the characteristic features of defective steel of the flaky type as they have been found by laboratory study of numerous specimens, and it aims to show the conditions within the metal that are favorable to the occurrence of this type of defect without entering into the details of mill practice (size of ingot, design of molds, rate of cooling, distribution of cooling stresses, etc.), all of which conditions appear to play a role in the production of these defects.

Jan 2, 1919

By Sidney H. Loram

As the work carried on by this Company, of which the writer has been in charge for the past two years, is somewhat unique, the following account of it may be of interest, and, on that account, is offered to the Institute without any attempt to claim this practice as the best. Mines. The mines supplying ore to the Company arc situated in three groups: the Guanaco field,.about 80 miles N.E. of the port of Taltal (lat. 25" S., long. 70" 30' W. of Greenwich); the Sierra Overa, about 63 miles S.W. of Taltal; and Paranao, about 42 miles due N. of Taltal (12 miles N. of the small town of Paposo, once famous for its copper-output). Guanaco. This field lies in the center of an absolutely waterless mountainous desert, where not a sign of vegetation can be found for miles. The dryness is such that ivory and horn crack and open, while raw-hide must be used in place of leather, which -would become worthless in a very short time. Water is brought about 21 miles by piping from the Cordillera, but only in small quantities, and costs in the Guanaco $7 (= $1.78 gold) per cubic meter. All supplies and food are sent from the port of Taltal, which in turn draws its supplies from the south of Chile, the

Jan 1, 1900

By F. J. Norton

THE object of this investigation was to make a comprehensive study of the degassing of molybdenum in order to determine how rigorous a treatment was necessary to completely remove sorbed gases from molybdenum electrodes in vacuum tubes. Some work has also been done with tungsten, nickel and carbon. As a logical development of this work it has been shown that the gas is present throughout the body of the metal and a study has been made of the solubility of nitrogen in molybdenum and tungsten and the rate of diffusion of nitrogen through molybdenum has been calculated. Tests were made on molybdenum from all the commercial sources and no difference was discovered in the nature of the gases present, the amounts or the ease of removal. The reason for this was apparent when a study was made of the manner in which gases are absorbed by gas-free molybdenum. It is necessary to heat molybdenum to 1760° C. in a vacuum of the order of 0.001 micron for a time which varies lineally with the thickness, in order to obtain a condition in which no further gas is evolved by the sample. A sample so degassed can be handled and subsequently assembled in a tube and then degassed readily. The gases obtained from molybdenum are carbon monoxide and nitrogen, the nitrogen being the more difficult to remove.

Jan 1, 1932

When Ponce de León landed in Florida in 1573 he was told of an Indian chief that possessed much gold. In 1576 Diego Meruelo obtained some of it from the Indians, and in 1579 Álvarez de Pineda reported that the natives wore ornaments of gold, which they obtained from the rivers. These statements all refer to the southern Appalachian region. The name is recorded in 1527; when Pamphilo Narváez landed at Tampa he heard that there was much gold to be obtained in a region named Apalache. * In 1564 René Laudonnière describes the methods used by the natives to win gold in the Apalatcy mountains.† However, no serious mining operations were undertaken until long afterward; the mining of gold in the Southern States may be said to have had its beginning when a nugget was found at the Reed mine, in North Carolina, in 1799. This nugget, which was of "the size of a small smoothing iron", was kept for several years before the finder learned what it was, but later more lumps, one weighing 28 pounds, were found in the same locality, and eager digging ensued. ‡ Thomas Jefferson, in his `Notes on Virginia', mentions the finding of a quartz specimen, not a nugget as is generally stated, that contained 17 pennyweights of gold; this was found on the Rappahannock river in 1782. §

Jan 1, 1932

By J. M. Pilcher

The application of oil to coal for-the reduction of dust has greatly increased the consumers' satisfaction with solid fuels, especially those for domestic use. The combination of oil-treated coal and automatic firing by a small stoker has made possible clean, automatic heating with bituminous coal. This, with the added pressure of competition by other fuels, has caused a rapid development of oil treating practice. A variety of materials derived" from petroleum oils is available from which one may choose for treating a par-ticular coal. Until recently, however, little information had been published to guide the choice. It is most im-portant that the proper type and amount of oil be used in order that all coals marketed as "dustless" will be reason-ably dustless, and thereby maintain a good reputation for oil-treatment. During the past two and one-half years, an investigation of a number of the problems related to the treatment of coal with oil has been conducted at Battelle Memorial Institute. This project was jointly sponsored by Bituminous Coal Research. Inc., Standard Oil Company of New Jersey, Sun Oil Company, and Viking Manufacturing Company. A progress report giving the principal results of the work of the first year was presented before the American Society of Mechanical Engineers in December 1937.1 The present paper is a summary of the entire inves-tigation.

Jan 1, 1939

By P. K. Strangway, H. U. Ross

Briquets consisting of pure artificial magnetite, pure artificial hematite, and mixtures of the two were reduced by hydrogen in a loss-in-weight furnace at temperatures in the range 500° to 1000° . The rate of reduction of the pure hematite briquets increased continuously with increased temperature. In contrast, the pure nmgnetite briquets exhibited a pronounced rate ninimutn at about 700°C. Metallographic studies of partially reduced briquets rerlealed that, at this temperature, the he.matite samples reduced in a topo-chemical manner while the magnetite ones reduced uniformly throughout, and after partial reduction their cross sections contained a mixture of iron and unreacted wustite grains. No iron shells could be detected on the surfices of any of these uwstite grains. X-ray diffraction investigations indicated that these grains had a rzinimum lattice parameter when they had been formed at the rate rninimum temperature. Also, it was found that an activation energy of 41,000 cal per mole zoas required for reduction when only these wustite grains were present. Thus, it is suggested that the overall reduction rate of the rnagnetile su?nples at temperatures in the range influenced by the rate nzinirnum phenomenon was limited by the rate qf iron ion diffusion in the unreacted wustite grains. THE rate minimum phenomenon, which has often been observed when reducing iron oxides at a temperature of about 700°C, is one of the most interesting, yet unresolved, problems in the field of reduction kinetics. Basic principles of chemical kinetics and 'In some instance, a second rate minimum has been observed at about 900°C. Since most investigators are in agreement that this minimum is directly related to the transformation from a to y iron (which takes place at 911°C) and since it was not encountered during the present reduction tests, it will not be referred to in this vaver. fundamental laws of diffusion all agree that, as the temperature is increased, the rate of reduction should also increase. However, with certain ores, it has been found that their reduction rate actually decreases with an increase in temperature up to some value X where a minimum reduction rate is reached. With further temperature increases beyond X the rate becomes more rapid again. Temperature X is usually referred to as the "rate minimum temperature", while the overall type of behavior constitutes the "rate minimum phenomenon". This phenomenon has been reported by numerous investigators. They have found rate minima during the reduction of both artifiial' and natural374 magnetites and artificia15j6 and natural5" hematites. Rate minima have been observed when reducing high-purity material2 or low-grade ores,3'4 when studying particles in the micronsize range5 or relatively large agglomerates,g10 and during reduction with either hydrogen7 or carbon monoxide.11"2 Previously, this phenomenon has been attributed to many factors; these include sintering and recrystallization of the iron formed during reduction374 changes in microporosity of the ore upon redction,"" formation of dense iron shells around retained wustite grains,11716 and chem-isorption,17 to name only a few. However, most investigators who have reported a rate minimum merely speculated as to what seemed to influence it and they did not examine the fundamental causes. Consequently, the present experimental study was initiated in order to evaluate the basic factors which could be associated with this phenomenon. MATERIALS AND METHODS The experimental techniques, followed during this investigation, are similar to those which have been described previously.18 The chemically pure magnetic powder was prepared by partially reducing Fisher reagent-grade hematite with a gaseous mixture of carbon monoxide and carbon dioxide in a rotating-drum furnace. Three-quarter-inch diam cylindrical briquets which weighed about 12 g were formed from this magnetite powder and pure hematite powder. All of the briquets were sintered while they were slowly raised through the 1200°C hot zone of a vertical tube furnace. An argon stream was continually flushed through this furnace in order to prevent oxidation of the magnetite briquets, while in the case of the pure hematite briquets sintering was carried out in air. The sintered hematite briquets had a density of 5.06 g per cu cm while the density of the sintered magnetite briquets was 4.27 g per cu cm. The sintered briquets were reduced by purified hydrogen in a loss-in-weight furnace at temperatures in the range 500" to 1000°C. In all instances, the critical reducing gas velocity was exceeded and, in order to ensure that the results were reproducible, duplicate briquets of each type were reduced under each set of experimental conditions. A continuous record of the weight loss during reduction was obtained with the aid of a Statham transducer. The present experimental setup was capable of detecting a change in weight as small as 10 mg. Since a weight loss of over 2 g usually occurred during each reduction test, an accuracy of better than 0.5 pct of the total weight loss could be achieved. RESULTS AND DISCUSSION Reducibility Tests. In the first set of experiments, pure hematite and pure magnetite briquets were used.

Jan 1, 1969

By R. P. Laforce, ZJ. R. Low, A. M. Turkalo, D. F. Stein

The interaction of the crlloying eletnenls, nickel and chromium, with the impurity elements, antimony, pIzosphorus, tin, and arsenic, to producse reversible temper brittleness in a series of high-purity steels containing 0.40 wt pct C has been investigated. The alloyed steels contained approximately 3.5 pcl Ni, 1.7 pct Cr, and 0.05 to 0.08 pct of the particular irnpurity to be investigated. Susceptibility to teirlper embrittlement was measured by comparing the notched-bar transition temperature of each steel after quenching from the final temper and after very slow cooling (step cooling;) following the final temper. A plain carbon steel without alloying elements, bu/ ud/h 0.08 pel Sh, does not embrittle when step-cooled through the emzbrittling range of temperatures. The same embrittling treatment, applied to a steel with about the same antinzony content but with nickel and chvonziunz added, causes a 700°C increase in transition temperature. If chromium or nickel is the only alloying element, the increase in transition temperature is only 50%, again with antimony present. A carbon-free iron containing nickel, chromium, and antimony shou~s a 200°C shift in transition temperature for the same thermal treatment. Specific alloy-impurily interactions are also observed for the other impurity elements, phosphorus, tin, and arsenic. Additional investigations involving electron microscopy, trzicrohard-ness tests of vain boundaries, minor additions of zirconiutn and the rare earth and noble metals, nzainly with negative results, are also described. HE particular type of embrittlement investigated is that which is encountered in alloy steels tempered in the temperature range from about 350" to 525'C or slowly cooled through this range of temperatures when tempered above this range. This type of embrittlement is sometimes called reversible temper brittleness to distinguish it from the embrittlement indicated by a minimum in the room-temperature V -notch Charpy energy vs tempering-temperature curve encountered in the range 28 0" to 350°C. Temper brittle-ness seriously restricts the use of many alloy steels since it precludes tempering or use in the embrittling range of temperatures and may significantly raise the ductile-brittle transition temperature of heavy-section forgings and castings tempered above the embrittling range, since such sections cannot be sufficiently rapidly cooled after tempering to avoid embrittlement. The very voluminous literature of temper brittle-ness up to about 1960 has been reviewed by woodfine' and LOW.' Of particular significance to the present investigation was the demonstration by Balajiva, Cook, and worn3 that high-purity Ni-Cr steel does not exhibit temper brittleness and the subsequent detailed and systematic study by Steven and Balajiva~ of the effect of impurity additions on the susceptibility to embrittlement of Ni-Cr steels. Steven and Balajiva showed that, of the impurities which may be found in commercial steels, Sb, As, P, Sn, Mn, and Si could all produce temper brittleness in a high-purity Ni-Cr steel. The principal purpose of the present investigation was to study the effects of particular alloy-impurity combinations on susceptibility to temper embrittlement. The steels used were high-purity 0.30 to 0.40 wt pct C steels containing 3.5 wt pct Ni and 1.7 wt pct Cr, separately or in combination. The susceptibility of these steels was then determined when approximately 500 ppm by weight of antimony, arsenic, phosphorus, or tin were added as an impurity. The melting, casting, and forging practices used in the preparation of the materials investigated are described in Appendix A. Table A-I in this appendix shows the analysis of all steels to be discussed. The steels were produced as 20- or 2-lb heats. The smaller heats were used after it had been demonstrated (see Appendix B) that a small, round, notched test specimen could be used to measure the shift in the ductile-brittle transition temperature caused by temper brittleness with about the same result as that obtained by Charpy testing. HEAT TREATMENT Unless otherwise noted, all steels were tested for embrittlement in the tempered martensitic condition. A typical heat treatment for a 0.40 C, 3.5 Ni, 1.7 Cr steel was: 1 hr at 870"C, in argon, quench into oil at 100"C, quench into liquid nitrogen, temper 1 hr at 625"C, and water-quench. The warm oil quench was used where quench-cracking was encountered; otherwise the initial quench was into room-temperature oil or water. For other compositions austenitizing temperatures were 50°C above Acs with the remainder of the thermal cycle the same. Steels in this condition, with no further heat treatment, are designated as non-embrittled. The above quenching and tempering cycle for the 0.40 pct C steels resulted in as-quenched hardnesses of 48 to 53 RC and as-tempered hardnesses of 24 to 31 Rc except in the case of the plain nickel or plain carbon steels. In these, the as-tempered hardness was as low as 80 to 90 Rg. No attempt was made to adjust the tempering temperature to obtain the same hardness in ali steels since it was felt that a uniform thermal cycle was more important than exactly equivalent hardness values. Pro- the standard quench and temper described above, the standard embrittling treatment was "step-cooling". For this the thermal cycle was: 593"C, 1 hr; furnace-cool to 538"C, hold 15 hr; cool to 524"C, hold 24 hr; cool to 496"C, hold 48 hr; cool to 468'C, hold 72

Jan 1, 1969

By N. Arbiter, C. C. Harris

In 1961, a research program started at Columbia into the mechanical aspects of flotation,* and certain ends are now in view. The purpose of this note is to explain these tentative conclusions in the hope of stimulating discussion and eliciting new data, especially industrial data, with which to test the views expressed. The variables presently under consideration are impeller rotational speed, N, volumetric air rate, Q, and impeller diameter, D, the latter being the parameter chosen to designate cell size. The most favorable *The latest work 1 references all previous publications. chemical environment is not under discussion since the procedures for establishing it are better understood than those for optimizing N and Q by virtue of a longer history of more intensive investigation. THE GRADE AND RECOVERY SURFACES With a given ore, chemical treatment, and flotation machine, both grade, G, and recovery, R, are functions of N and Q. The GNQ and RNQ relationships are best viewed in terms of three-dimensional surfaces (Fig. 1) which are experimentally determinate.2 TO maintain grade at an acceptably high level, it is necessary for N and Q to lie within certain limits, and similarly with recovery. However, the ranges of N and Q for grade on the one hand and recovery on the other are rarely the same. Selecting the single N

Jan 1, 1970

By P. H. Dudley

THE piping and segregation of ingots of steel is a comprehensive subject, and must be studied in reference to the different grades of soft, medium, and hard steel, rather than to discuss it in a general manner, as though applicable to all grades. Rail steel, however, will receive the most consideration in this paper, for the wheel-loads of the motive pourer and rolling stock have doubled from 1890 to 1910. Steel rails and tires which were efficient under the light loads, became less serviceable under the double wheel-loads, quadrupled tonnage, and higher speeds. Bessemer Steel. Bessemer steel of froth 0.10 to 0.15 per cent. of carbon, for splice-bars, spikes, and tie-plates, rises in setting, and is cast in bottle-mouthed molds, which must be capped to prevent an over-flow from the top. This grade of steel rises in the molds and makes a longer ingot than the volume of molten steel when first teemed. The ingots which are allowed to cool and then cut open, show, particularly in the upper part, large occluded blow-holes, and when they are Dot oxidized or do not contain foreign matter, weld more or less completely when the steel is rolled or forged above 1,100° C., and it :is in this way that the blow-holes are closed it the low-carbon steels.

Jan 4, 1913