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By C. G. Dunn

This note describes a method for revealing micro-structures in tantalum through an {hkl} effect which was found during a study involving amorphous and crystalline tantalum oxides. Three steps are involved. First, an amorphous film of Ta2O5 is formed anodically1 on the surfaces of the tantalum. The amount needed depents on the thickness of the substrate tantalum; 1600Å of oxide, however, is generally satisfactory in the 1/2 -mil (12 µ) to 3-mil thickness range. The film at this point is uniform in color. Second, the anodized specimen is heated to 800°C in. vacuo during a period of a few minutes and held at temperature for 5 min. During such a treatment some oxygen leaves the oxide through dissolution into the substrate tantalum (e.g., at 10-8 Torr oxide films thinner than about 800 completely disappear on 5-mil strip). Considerable crystallization of the amorphous oxide also occurs adjacent to the metal/oxide interface but not throughout the oxide thickness. The thickness of oxide needed as a residue is not too critical; values between 500 and 1000Å (optical estimate') may be most useful. (The presence of a residual oxide layer after the heat treatment usually is not apparent; in fact, in most instances the surfaces have a metallic appearance. This can be the case also for thicker residual films needed in the detection of a crystalline oxide phase by surface X-ray diffraction—e.g., if the initial oxide film is 3000Å thick, enough crystalline oxide is formed for X-ray detection.) The third step eliminates the metallic appearance at the surface and reveals (or produces) a varied colored film of tantalum oxide. Two methods can be used and both will be illustrated. If the specimen is dipped in 48 pct HF for a few seconds, the tantalum is found to be covered with a multicolored oxide. Moreover the colors correlate with the grain structure of the substrate tantalum through an orientation dependence of the type illustrated in Fig. 1, where results of an orientation analysis by the Laue X-ray method have been plotted. Other film conditions would have provided a different set of colors for the same orientations. Any such correlation, however, provides a basis for a qualitative assessment of the distribution of orientations in a large sample. The cold-rolled structure of tantalum foil produced by a recrystallization anneal and a cold-rolling reduction of 95 pct is not easily obtained by usual metal-lographic methods.' The structure, however, is easily revealed by the present technique, Fig. 2. The alternative third step is to reanodize the specimen. The optical nature of the final anodic film depends on the presence of the crystalline oxide phase; color variations indicate optical thickness variations in the film. As the reanodization voltage is increased from zero, straw and light brown colors appear (as usual), followed now by variations in color from grain to grain depending on {hkl} orientation. Suitable end points, which are determined by voltage and time, are easily established. Fig. 3, for example, shows the grain structure developed in 5-mil tantalum strip during a 30-min re-crystallization and grap-growth anneal at 1800°C. An anodic film of 1600Å thickness was added prior to the special 800°C anneal. Reanodization was done at constant current density (near 0.2 ma per sq cm) in an aqueous solution of H3PO4 (0.01 pct) and was terminated after the initial brown colors were replaced by a deep blue at approximately 30 v. Although good grain contrast can be obtained with bright field illumination, even greater contrast for black and white micrographs may be obtained with polarized light, as in Fig. 3.

Jan 1, 1967

By John C. Branner

Within a couple of years I have received many inquiries in regard to the manganese-mines of Brazil. These inquiries were doubtless directed to mc because I had lived and traveled in Brazil for more than eight years, and was therefore supposed to be pretty well acquainted with its geology and mineral resources. Somewhat to my chagrin, I not only knew nothing of manganese-mines in that country, but I had never before heard of the mineral having been found here in quantity, and I did not even know in what State the mines were located. The present summer found me in Brazil again, trying to finish up some of my early geological investigations along the northeast coast, and I have used the occasion to find out something about the manganese-deposits. Very little is known of these mines, even in Brazil. While at Pernambuco I was told that they were in the distant interior of the State of Bahia. In August I reached Bahia, and there I found out, concerning the mines and their geology, enough to be worth telling for the benefit of those interested in the mining or using of this mineral. Thus far, all the manganese-ore shipped from this State has come from two mines, the principal one of which is known as the Pedras Pretas mine. This was the first mine opened, is the best developed, and was the original discovery; the second one is on an adjoining tract, and the general geology and natural conditions are about the same in both. The Pedras Pretas mine is on the Nazareth-Amargosa railway, twenty-six kilometers west of the town of Nazareth, which is on tide-water, at the head of navigation, and is reached from the city of Bahia by a small side-wheel steamer that runs across the bay of Bahia and up the Rio Jaguaripe

Jan 1, 1900

POSITIONS VACANT (Under this heading will be published notes sent to the Secretary of the Institute by members or other persons.) Opening for man as head of laboratory of large brass manufacturing plant in Ohio; must also be competent to manage foundry making brass castings, following practice of malleable iron castings and insulating materials. Good opportunity for right man. No. 36. Professorship in Mining at a Western university; requires man competent to give instruction in ore dressing, in metal and coal mining, and in zinc smelting, and capable of gaining confidence of mining interests. Salary $2,200 to $3,000. No. 37. ENGINEERS AVAILABLE (Under this heading will be published notes sent to the Secretary of - the Institute by members or other persons introduced by members.) Member, graduate engineer, aged 44, with over 20 years' experience in connection with large coal and coke operations in different parts of the country, desires position as general superintendent of large coal company, or will take an interest with the management in a smaller company. No. 206.

Jan 6, 1915

By Thomas N. Williamson, Victor Zeni

A 6-ft diam core drilling machine has successfully completed seven mine shafts in Virginia and West Virginia to depths as great as 465 ft. There is no practical depth limitation to this new system-a potential method in formations not easily penetrated with other large-scale drilling programs-and higher penetration rates and larger diameters are possible in some formations already being drilled successfully by other methods. The core barrel on the machine is fitted with rolling cutters such as those used on oil field rotary bits, so that less torque is required than with other large- scale drilling systems. The core is made with a wider kerf than is achieved with other coring methods, providing more working room for core drilling.

Jan 4, 1957

By R. M. Hays

Prior to use of this model siphon finisher, the only means of evaluating metallurgical performance of the siphon finisher was by pilot plant studies. These are costly and require large quantities of material. A model siphon finisher and a test procedure which permits the evaluation of siphon finisher metallurgical performance has been developed. Metallurgical results between the model siphon finisher and pilot plant or commercial units show fairly good correlation. The upgrading of magnetic taconite concentrates by hydraulic concentration has been practiced for several years. In the 1940's, Braund1 used a multistage upflow classifier to upgrade magnetized magnetic concentrates. In present taconite plants, the SiphonSizer, marketed by Dorr-Oliver, Inc., has been particularly suitable for upgrading magnetic concentrates. When the hydraulic SiphonSizer is used to upgrade the concentrates in the finishing portion of the overall flowscheme, the unit will be called a siphon finisher to distinguish this application from classification. Prior to this work the only means of evaluating the metallurgical performance of the siphon finisher was by pilot plant studies which are costly and require large quantities of material. Therefore, it was desirable to develop a model siphon finisher and a test procedure which would simulate siphon finisher performance and require only small samples of material. This model would permit the evaluation of small samples such as drill core samples and be useful in evaluation of commercial siphon finisher design and performance. THE SIPHON FINISHER The siphon finisher, as shown in Fig. 1, is a tank equipped with a system of water jets which distribute the hydraulic water uniformly across the bottom of the vessel with an energy release for agitation in the teeter bed. The feed to the siphon finisher is intre duced through a feed well in the center of the unit. The silica and middling particles overflow a peripheral weir into the overflow launder. The magnetite fraction is discharged by a siphon or a modulated discharge valve. The siphon or the discharge valve is usually operated automatically by a float assembly which is responsive to the depth of the teeter bed. Various interface sensing devices have also been

Jan 1, 1968

By Richard P. Rothwell

REVOLING slime-tables with stationary sprays and oscillating brushes have for many years been a favorite apparatus used for working slimes in German dressing-works, often displacing Rittinger tables and the many variations of Cornish buddles. The difficulty of building these tables larger than 5 1/2 meters (17 feet) in diameter, increasing the cost and making them unwieldy, rendered it necessary also to concentrate the slimes in several operations, because the travel over so short a length of hearth would not suffice for close concentration. A preliminary sizing is effected in a system of spitzkasten. Herr C. Linkenbach, general manager of the Ems Lead and Silver Works, Germany, devised a buddle, in 1878, which has since worked well and found much favor in Germany, and has been in one instance copied here, at Colorado Springs, without any credit having been given to the original inventor. Linkenbach's plan has been to reverse the functions of the table and the washing apparatus of the old German revolving table. He makes the tables stationary and rotates the washing apparatus,, thus enabling him to save in power, and, within certain limits, to increase the dimensions of the table, without in any way affecting its durability or materially increasing its cost. In its earlier form, the buddle was single, and that type is still

Jan 1, 1883

By Ellsworth Daggett

THE system of pitwork used with the Cornish pumping engine, and which, for want of a better name, we may call the Cornish system of pitwork, consists essentially of a series of plunger-pumps, situated one below the other, in a shaft or incline, the plungers being operated by a rod called the pitman or pump-rod, which must, therefore, extend from the motor at the surface to the lowest pump. The subject will be best understood by reference to Fig. 1, in which k may be taken as typical of the ordinary plunger-pump, in which S is the suction pipe, u, the lower valve situated in the H piece T; v, the upper valve situated in the valve-box O; I, the mounting-pipe or column through which the water is carried to the surface; L, the plunger-barrel, and P, the plunger working through the stuffing-box, and actuated by the branch rod r, which is attached to the main pump-rod, R. The action of the pump is as follows : On the ascent of the plunger, acting now by suction, the water flows from the reservoir through the valve u, into the barrel, L. On the descent of the plunger, the water is forced up through the valve, v, which acts merely as a check valve, into the pipe, I, through which it is, at each successive down-stroke of the plunger, forced upward until it reaches the next reservoir, from which it is taken by another similar pump, and so on until it reaches the surface or drain-tunnel. The pump is obviously only single-acting, i. e., it acts only during one-half of its entire stroke. The weight of water raised during the up-stroke of the plunger is equal to the weight of a column of water whose base is the area of the plunger and whose height is the mean distance between the plunger-face and the surface of water in the lower reservoir, a distance not usually exceeding 12 or 15 feet, and which obviously cannot under the most favorable circumstances, exceed 25 or 30 feet. The water forced up during the down-stroke is equal to the weight of a column of water whose base equals the area of the plunger and whose height equals the length of the mounting column above the mean position of the plunger-face, say from 150 to 300 feet. Almost all of the useful work, therefore, is done on the de-

Jan 1, 1879

By F. Weinberg

The relative concentration of 1" at grain boundaries in controlled orientation bicrystals has been examined by autoradiographic techniques, and by activity measurements of grain boundary surfaces exposed by preferential ,melting. The autoradio-graphs indicate that thallium is concentrated at grain boundaries in as-grown bicrystals, but not in zcell-annealed bicrystals. They also indicate that the solute concentration and the distribution on as-grown bicrystal surfaces are markedly different than that of the bulk material. The boundary surface measurements are in agreement with the autovadiographic evidence. On the basis of these measurements, as-grown bicrystals containing approximately 100 ppm of Tl, solidified at rates between 5 and 30 cm per hr and with tilt boundaries greater than 10 deg, exhibited grain boundary segregation equivalent to roughly 10 atomic planes of pure solute. Higher solute concentrations (equivalent to 140 atomic planes of pure solute) were obtained in bicrystals solidified slowly (0.6 cm per hr); slightly higher values were obtained in specimens containing a large angle nantilt boundary. Annealing for various times over a range of temperatures eliminated grain boundary segregation within the experimental uncertainty of the results (equivalent to 1 atomic Plane of pure thallium at the boundary). The results for the as-grown bicrystals can be qualitatively accounted for by assuming the presence of a groove on the solid-1iq;id interface, at the grain boundary. SOLUTE segregation at grain boundaries may be considered in two parts, namely, nonequilibrium segregation associated with the solidification process, and equilibrium segregation in fully annealed materials.' There is much indirect evidence for nonequilibrium segregation, based on preferential etching at grain boundaries and the mechanical properties of as-cast alloys. In addition, some direct observations have been reported in which radioactive tracers were used as solute additions and segregation detected at the grain boundaries by autoradiographic techniques. However, there is little detailed quantitative data on solute concentrations related to grain boundaries, particularly for different freezing conditions and grain boundary configurations. Equilibrium segregation at grain boundaries has been considered both theoretically and experimentally. cean' has made an estimate of the maximum equilibrium solute concentration that might be expected at a grain boundary, based on the lattice distortions in the boundary region. He arrived at a concentration which was equivalent t a monatomic layer of pure solute. A similar value, based on thermodynamic arguments, was calculated by Cahn and Hilliard for the segregation of phosphorus in iron. Experimentally, much higher values of solute concentration at grain boundaries have been reported recently by both Inman and iler' for phosphorus in iron, and Ainslie et 1.' for sulfur in iron. They observed concentrations equivalent to as much as 20 to 100 atomic layers of pure solute at the grain boundaries. However, in both cases it was shown that the observed segregation was not due solely to equilibrium segregation at the grain boundary. In the former case, precipitation effectss due to trace impurities in the material were believed to account for the large amount of solute present at the grain boundary. In the latter case it was shown that a high density of dislocations in the boundary region could provide a large number of additional sites for solute atoms, other than at the grain boundary. Thomas and chalmera have reported on the equilibrium segregation of po210 in grain boundaries of Pb-5 pct Bi alloys. Using autoradiographic techniques, they observed a concentration of polonium along the boundary trace on the surface of annealed bicrystal specimens grown from the melt. The concentration only appeared after annealing, and varied with boundary angle, increasing as the boundary angle increased. Their conclusions have been questioned by Ward," who pointed out that the segregation they observed along the boundary trace was much too wide to be compatible with the usual concepts of the thickness of a grain boundary of several lattice spacings. Also, Maroun et al.,l1 with specimens similar to those of Thomas and Chalmers, found that segregation could only be detected on the specimen surface, suggesting that Thomas and Chalmers' results were associated with an oxidation effect of polonium, and not equilibrium segregation. Thomas and Chalmers replied12 that they did observed segregation at the grain boundary in the bulk material and suggested further experiments were necessary to resolve the difference. The purpose of the present investigation was to examine both nonequilibrium and equilibrium grain boundary segregation in melt grown bicrystal specimens as a function of boundary angle, growth rate, and solute concentration, and to de-

Jan 1, 1963

By L. L. Handy

The most common method of identifying hydrocarbon-bearing strata in a well that penetrates many different formations involves measurement and interpretation of the electrical properties of the formations as determined by electrical logs. Even though this method is used extensively, and even though in a great many instances it is capable of indicating presence of oil or gas, situations arise for which it is extremely difficult, if not impossible, to deduce the presence of hydrocarbons. These situations may involve the following. 1. A thin formation, bounded by highly resistive formations, in which it is impossible to obtain the actual resistivity of the uninvaded zone with existing logging devices. 2. A formation in which invasion has been so extensive that a value for the uninvaded zone resistivity cannot be obtained. 3. A very shaly formation in which the resistivity index, I, is lower than that usually associated with productive formations. 4. Laminated formations comprised of thin productive sands separated by thin shale streaks in which the individual sand and shale streaks are too thin to permit measurement of uninvaded-zone resistivity with existing logging devices. 5. Productive formations in which the water saturation is high. To extend the utility of electric log interpretation to identification of hydrocarbons in all types of formations, there is strong incentive to find a method not subject to these limitations. Some time ago, in connection with research on the wettability of reservoir rock, an investigation was conducted in which the resistivities of cores were measured shortly after they were removed from a core barrel, and again after they had been extracted and restored to their original oil and brine saturation.' The resistivities after extraction were generally lower. Other tests made on the cores indicated that they were more nearly water wet after they were extracted; thus, it was assumed that the observed changes in resistivities were due to a change in wettability of the cores. Other experiments'," have shown that resistivities of rock samples are sharply dependent on wettability. These experiments have shown that oil-wet samples are more resistive than water-wet samples. To obtain an understanding of how the wetting properties of the surfaces of core material affect electrical resistivity, a series of experiments was conducted. Two groups of core samples were prepared for testing. One group contained brine, but no residual oil. The other group was saturated with brine, flooded with oil to a low water saturation, then flooded with brine to a final residual oil saturation. Resistivity measurements were made on each group. Both groups were then flooded with the original brine to which a chemical had been added that renders sand and clay surfaces preferentially oil wet, a so-called reverse-wetting agent. very little change in resistivity was observed in cores containing only water. The group containing residual oil, however, showed resistivity increases of 100 to 200 per cent. These experiments showed that the resistivity of a core containing oil could be altered by changing wet-tability of the core. Moreover, the possibility was introduced that reverse-wetting agents might be employed as the basis for a logging method for identification of oil-bearing strata. Since behavior of a porous rock containing gas and water might be expected to be similar to that of a rock containing oil and water, such a method should also be applicable to identification of gas-bearing zones. In principle the wettability of the invaded zone could be reversed without altering conductivity of the interstitial water or the hydrocarbon saturation therein. Those strata showing significantly increased invaded-zone resistivities would, therefore, contain hydrocarbons; those with no significant change would be filled only with water. Addition of a reverse-wetting agent to a hydro carbon -bearing zone which is, by nature, already preferentially oil wet would not result in an enhancement of its resistivity. It is generally believed, however, that most hydrocarbon-bearing strata are preferentially water wet.

By J. E. Johnson

(Cleveland Meeting, October, 11,1912.) THE subject of blast-furnace slag is one which has had much consideration, particularly from the scientific standpoint, and several years ago technical literature contained many learned discussions on the oxygen-ratio of the acids and the bases, all on the assumption that acids and bases must be present in a ratio depending on molecular weight and chemical valency. Much work has also been done, sometimes in conjunction with the former, on the total heat and the temperature of initial fusion or softening of various slags. A wider knowledge of the blast-furnace now enables us to say that for practical purposes this work has been of almost no value. It is now generally admitted that on the physical side the important point of a given slag is neither its total heat of fusion nor its softening-point, but its free-running temperature, since this is the critical temperature of the furnace. This temperature bears no definite relation to the softening-temperature, as determined by Seger cones, for instance, because some slags melt relatively like ice, with a very short viscous-range, while others melt relatively like tar, with a very long viscous-range. In one the difference between the softening- and the free-running temperature may be very small, as little as 100° F., while in another this difference may easily be 200° or 300°. The importance of this difference is so great in practice as to destroy completely the value of exhaustive investigations, even such as those of 0. Boudouard, published a few years ago.1 * Presented also at the Joint Meeting of the Institute with Section IIIa, Metallurgy and Mining, of the Eighth International Congress of Applied Chemistry, New York, September, 1912. 1 It may not be amiss at this point to call attention to the excellent suggestion of Woolsey McA. Johnson, made several years ago, for determining the temperature at which different slags have the same practical fusibility. This suggestion

Oct 1, 1912

By A. R. Jr. Amos

LOG washers have been used for many years in the washing of clay iron ores, phosphate rock and manganese ores, but not until the past 15 years have they been employed to any extent in the preparation of aggregate materials and fluxing stone. For a machine of such importance where tenacious clay or soft rock must be eliminated, there are few data generally available. The purpose of this paper is to set forth the results obtained from several operations, together with a few suggestions for planning a specific installation. Where the material to be washed out consists of loose surface soil, silt, or small amounts of quickly soluble clay, there is little competition with other forms of washers, because greater power and maintenance are required for the operation of log washers, but where the foreign matter is a stiff clay, such as occurs with high-calcium limestones and in marginal gravel deposits, the ability of other kinds of washers to eliminate com-pletely the hard clay balls is at least uncertain. Then the log washer comes into its own field, for with the breaking and churning action of the logs it will clean out the toughest clay. Even with material from the hydraulic dredge, if it contains tough clay, the log washer is desirable unless the gravel is subjected to a costly soaking and rehandling process. Recently there has been a considerable development in other types of machines to accomplish these results but it is not within the scope of this paper to make comparisons between competitive types, but to present the best obtainable data on log washers only. From the primitive design that gave it its name, a long log hewn from a tree, with paddles forged to shape from strap iron and attached by lag screws, the log washer has gradually been developed to the present all-steel type. As now manufactured, the log washer consists essentially of two built-up logs on which are mounted a series of paddles, carried by shafts fitted at the ends of the logs on bearings fastened outside the enclosing steel box, or trough, which is set at an angle of about 5° to 10° and into which the material is fed. Stuffing boxes at the places where the shafts pass through the box at the lower end are equipped with water-

Jan 1, 1936

By V. Lessels, D. J. Buckwalter, D. H. Rose

At White Pine Copper Co.'s operation in the Upper Peninsula of Michigan, the company has been losing more than four lbs of copper in each ton of sand tailings. With an average rate of 12,000 tpd of sand going to the tailing pond daily, the company has been losing more than 14 million lbs of the red metal annually. With an eye aimed toward lessening this loss, White Pine engineers in 1959 initiated a study on techniques for recovering this "lost" copper from the sands. Inasmuch as the flotation operation was considered to be optimized, a logical approach seemed to be leaching. For various reasons ammonia, ferric chloride, acid, and biological leaching were ruled out as impracticable. This led to a consideration of cyanide leaching as practiced in the precious metals industry.

Jan 8, 1967

By A. K. Gangopadhyay, J. J. Moore

The effect of grinding media composition, mineral type, and slurry environment on the wear rate of various grinding media (balls) are discussed. Sufficient wear data have been obtained and correlated. Modes of wear were determined from examination of the ball surfaces using scanning electron microscopy. Five modes of wear have been identified to be operative under certain slurry conditions for the various ball compositions studied.

Jan 1, 1986

By W. C. McClain

In the design of underground excavations, rock mechanics considerations are nearly always based on an elastic behavior of rock. Most rocks do exhibit a certain amount of elasticity, and the application of principles and concepts of elasticity to rock mechanics problems has been largely responsible for progress in the field over the past 10 or 15 years. No doubt the theory of elasticity will remain the most useful analytical tool available for both the design of underground openings and the interpretation of phenomenological data.

Jan 1, 1967

By T. B. Counselman

WHEN one thinks of Minnesota iron ore, one thinks of big open pits, where high- grade ore is simply scooped up with a power shovel, loaded into cars, and hauled away for shipment to the blast furnace. On the western end of the Mesabi range, however, are large tonnages of iron ore which contain too much silica to be used directly in the blast furnace, and these ores must first be concentrated to a purer form. The Mesabi range is about 100 miles long and a maximum of 3 miles wide. The iron formation, which in its unaltered form is called taconite: consists of a banded iron- bearing chert. Where the high-grade ore bodies occur, these have resulted from folding and cracking with sub- sequent leaching out of the silica, leaving the iron oxide behind. The big open pits and the underground mines are situated in these concentrations.

Jan 1, 1941

By O. Bergmann, R. E. Lueders, R. R. Ellefson, H. M. Brennecke, D. S. Davies

A new hydrometallurgical process has been developed to recover copper from sulfide ores. Copper is leached in a staged reactor system utilizing nitric and sulfuric acids at 105OC. Iron is removed from the pregnant liquor as a jarosite, and cathode copper is electrowon directly from the purified pregnant liquor. The spent electrolyte is recycled. Nitrogen oxides evolved from the leach are reconverted to nitric acid and are also recycled. Sulfur is rejected as So, jarosite, and gypsum. The process is highly versatile and can recover precious metals, molybdenum, and zinc when these elements are present. Continuous, integrated, semi-pilot plant operations using chalcopyrite ores demonstrated 99% copper leaching and production of cathode grade copper. Economic evaluation shows that the process is competitive with pyrometallurgical and other hydrometallurgical processes.

Jan 1, 1982

By P. R. Swann, R. M. Fisher, W. R. Duff

Observations by transmission electron microscoPy of the microstructures in quenched Fe-A1 alloys provide the basis for revision of the Fe-A1 phase diagram. The diagram is characterized by first-order transitions between the disordered ferromagnetic a! solid solution and the two ordered phases FeAl and Fe3Al. However, second-order transitions showing corre-luted fluctuations in the degree of order near the critical temperature occur between the paramagnetic a! and FeAl and the FeAl and FeAl phases. ELUCIDATION of the true nature of the Fe-A1 equilibrium diagram has proven to be an extremely challenging problem as evidenced by the fact that six quite different versions of the iron-rich portions have been published since 1958.&apos;-6 The most recent diagram shown in Fig. 1 was proposed by Rimlinger6 based on X-ray diffraction analysis and dilatometry. He shows the single-phase fields of the ordered phases of the types FeAl(L20) and Fe3A1(D03) and the disordered bcc Fe-A1 solid solution, a, separated from one another in every case by large two-phase regions. Thus, he implies that in Fe-A1 alloys ordering always occurs via a classical phase transition. In contrast to this view, theoretical studies3&apos;" have concluded that the transitions a — FeAl and FeAl — Fe3A1 should be second- or higher-order in character. A further revision of the Fe-A1 diagram of state is presented in Fig. 2 based on our previous8,9 and current observations by transmission electron microscopy of the microstructures found in quenched specimens. The average quenching rate was 50,000°C per sec and although this was sufficiently rapid to prevent Fe3A1-type ordering below -550°C it was not sufficient to suppress ordering of the type FeAl in the temperature range -650" to 800°C. However, ordering during the quench is easily recognized since the FeAl phase formed during holding at temperature rapidly develops large antiphase domains whereas FeAl formed during quenching has a very fine domain size, -50Å diam. Each symbol in Fig. 2 indicates the result of a micro-structural examination of specimens heat-treated (-1 hr) until equilibrium was established. The results will be discussed in the order of the points, A - Dl marked on both diagrams with reference to the phase fields, critical temperature, and "transition" ranges, respectively. The dark-field micrograph corresponding to point A is shown in Fig. 3 and was obtained using a 111 reflection of the Fe3A1 structure which reveals both a&apos;/4<111> and a&apos;/2<100> antiphase domain boundaries.10 The structure observed in this specimen is typical of single-phase Fe3A1 and shows no evidence for FeAl or any other additional phase. The dark-field micrograph shown in Fig. 4 corresponds to point B on the two diagrams. It was taken with a 100 FeAl reflection which reveals a/2(111) domains and exhibits the typical structure of single-

Jan 1, 1970

Jan 1, 1916

By R. J. Hopkins, L. B. Haney

On the basis of limited experimental work conducted at the Port Pirie smelter, it would appear that, by increasing the specific surface of sinter, and possibly that of coke as well, a marked increase in the rate and degree of sinter reduction in the furnace shaft can be achieved. Fusion-point tests have shown that this increased reduction means a much higher sinter fusion point and narrower plastic zone, while the more efficient utilization of coke in the furnace is inherent in the intensification of reduction by the provision of a more reactive sinter surface. Investigations aimed at increasing the ability to operate the blast furnace with a higher lead tenor of sinter reducing fuel cost proportionately, and at eliminating the loss in reduction potential in coke entering the furnace, as shown by the presence of appreciable proportions of CO in the top gases, are reported. Several lines for future investigations that could result in improved smelting methods are proposed. A SOMEWHAT informal presentation of ideas on lead blast-furnace smelting will be given in this paper. These ideas have been developed during observations of furnace behavior at Port Pirie and earlier at Mt. Isa, and have been guided by the results of laboratory experiments at Port Pirie. The authors do not intend to propound any particularly new theories, but present their ideas as a basis for discussion which may help toward a better understanding and improved control of blast-furnace operation. Performance variations of considerable magnitude occur from time to time at most lead blast-furnace plants. While Port Pirie is fortunate in having a very regular supply of high grade concentrates, it is no exception in this respect. Such irregularities are of considerable economic importance and they constitute a challenge to present-day metallurgists in their efforts to obtain an ever greater degree of control over furnace operation. In operating as Port Pirie does with a relatively high lead charge, it has been recognized for a long time that shaft conditions are ,of the greatest importance. A practical, or engineering, attack on the problem of accretions consisted of changes in furnace design, e.g., by widening the shaft to 10 ft above the bottom row of tuyeres, and by the provision of curved ends and vertical walls.&apos; That this attack has had a great measure of success is shown by the fact that barring down of these wide furnaces is rarely necessary, shaft conditions have greatly improved, and sensitivity to charge variations has been markedly reduced. These modifications, followed by some metallurgical changes (chiefly the incorporation of pig iron into the furnace charge in 1948), have brought furnace operation to a point where some variables which were previously masked can now be studied. Accordingly, over different periods of time during the last five years, such variables as could be given numerical values have been recorded and subjected to statistical examination. The objectives of this work were: 1—to reveal the true importance of the different variables and 2—to show the proportion of total furnace variation which is unexplained and therefore referable to causes not measured at present? e.g., shaft accretions, sinter structure, coke structure, and others. Statistical Study of Variables In this work factors relating to furnace speed and lead reduction have been examined: 1—slag com-

Jan 1, 1955

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Jan 1, 1928