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By John L. Ham, Robert M. Parke

The melting point of molybdenum is 2625° + 50°C. Heretofore the metal has been considered too refractory to be melted in commercial quantities; hence, it has been formed into rod, wire, and sheet by the methods of powder metallurgy, wherein the temperatures do not exceed 90 per cent of the melting temperature. The manipulation of liquid metals at temperatures of about 2000°C. and above presents some difficult problems in heat transfer, in purification, and in container materials. For metals melting at such high temperatures, it is generally regarded as expedient to circumvent the more common melting and casting process by resorting to powder metallurgy. This circumvention is not accomplished without some penalties, the more notable of which are the relatively high cost of the powder metallurgy method and particularly the size limitations of its product. In an effort to overcome the inherent disadvantages of the powder metallurgy method, especially in respect to the limit of size, a project was begun in 1943 at the Climax Molybdenum Co. laboratory to develop a method of melting and casting molybdenum capable of producing larger bodies of molybdenum than were then obtainable. Later, from Feb. I, 1944, to Aug. 31, 1945, the project was under the supervision of the National Research Committee, Division One. In peacetime, too, there are needs for molybdenurn, which make consideration of another process desirable; for example, large parts for heat engines generally, the omnipresent demand for metal of higher quality and lower cost, and the development of molybdenum-base alloys. This paper describes methods for melting and casting molybdenum, with details of the special process needed to make molybdenum castings ductile, and reports some of the properties of what may be regarded as a new, or at least modified, form of the metal. First Process for Melting and Casting Molybdenum The maintenance of a temperature greater than 2625°C. in a 'pace large enough to melt several pounds of molybdenum may involve the loss of heat at a Very considerable rate. For melting molybdenum, therefore, the source of heat must be of high potential and of fairly high power. Evidently, also, the source of heat must not impair the purity of the product. The electric arc operating in vacuum appeared to meet these requirements and was accordingly the first choice as a source of energy. A number of arc devices for melting molybdenum were examined, and several were tried. In the first experiment, a 20-kw., 60-cycle-per-second alternating-current arc was operated between two horizontal and opposed electrodes of molybdenum- In this arrangement the falling droplets of molybdenum solidified below the arc in an irregular mass. This experiment did not produce a useful casting, but the data obtained indicated that

Jan 1, 1947

By John L. Ham, Robert M. Parke

The melting point of molybdenum is 2625° + 50°C. Heretofore the metal has been considered too refractory to be melted in commercial quantities; hence, it has been formed into rod, wire, and sheet by the methods of powder metallurgy, wherein the temperatures do not exceed 90 per cent of the melting temperature. The manipulation of liquid metals at temperatures of about 2000°C. and above presents some difficult problems in heat transfer, in purification, and in container materials. For metals melting at such high temperatures, it is generally regarded as expedient to circumvent the more common melting and casting process by resorting to powder metallurgy. This circumvention is not accomplished without some penalties, the more notable of which are the relatively high cost of the powder metallurgy method and particularly the size limitations of its product. In an effort to overcome the inherent disadvantages of the powder metallurgy method, especially in respect to the limit of size, a project was begun in 1943 at the Climax Molybdenum Co. laboratory to develop a method of melting and casting molybdenum capable of producing larger bodies of molybdenum than were then obtainable. Later, from Feb. I, 1944, to Aug. 31, 1945, the project was under the supervision of the National Research Committee, Division One. In peacetime, too, there are needs for molybdenurn, which make consideration of another process desirable; for example, large parts for heat engines generally, the omnipresent demand for metal of higher quality and lower cost, and the development of molybdenum-base alloys. This paper describes methods for melting and casting molybdenum, with details of the special process needed to make molybdenum castings ductile, and reports some of the properties of what may be regarded as a new, or at least modified, form of the metal. First Process for Melting and Casting Molybdenum The maintenance of a temperature greater than 2625°C. in a 'pace large enough to melt several pounds of molybdenum may involve the loss of heat at a Very considerable rate. For melting molybdenum, therefore, the source of heat must be of high potential and of fairly high power. Evidently, also, the source of heat must not impair the purity of the product. The electric arc operating in vacuum appeared to meet these requirements and was accordingly the first choice as a source of energy. A number of arc devices for melting molybdenum were examined, and several were tried. In the first experiment, a 20-kw., 60-cycle-per-second alternating-current arc was operated between two horizontal and opposed electrodes of molybdenum- In this arrangement the falling droplets of molybdenum solidified below the arc in an irregular mass. This experiment did not produce a useful casting, but the data obtained indicated that

Jan 1, 1947

By W. Rostoker

Single isothermal sections were constructed for the titonium-rich corners of the systems Ti-Fe-O, Ti-Cr-O, and Ti-Ni-0 with a view to locating the shape and disposition of the ternary intermediate-phase fields for the compounds isomorphous with Fe3W3C. IN a previous note,' it was reported that a group of ternary intermediate phases existed which occurred in the general composition range Ti,X,O-Ti&O where X was one of the following elements: copper, nickel, cobalt, iron, or manganese. In two instances, binary intermediate phases occurred (Ti²Cu and Ti²Ni) which appeared to be isomorphous. The X-ray diffraction patterns of the phases could be indexed on a cubic lattice whose cell edge was of the order of 11 kX. Karlsson2 stated that the line extinctions and line intensities indicated that these phases were isomorphous with Fe³W³C and therefore belonged to the space group Oh. This author also noted that no unique phase of this type occurred at the composition Ti,Cr,O. This latter statement was accepted as true at the time the previous technical note was written.' However, work continued along these lines and that reported here has shown that a phase isomorphous with Fe³W³C does exist in the vicinity of the composition Ti³Cr³O but not at or near Ti4 Cr²O. The lattice parameter of this phase was found to be 13.01 kX. Metallographic examination of both as-cast and annealed specimens of these supposed ternary oxide phases disclosed structures which were far from single phase in many instances. It was considered a point of some interest to locate more positively the composition coordinates of the single-phase fields. To this end, single isothermal sections for the systems Ti-Fe-O (1000°C), Ti-Cr-0 (1000°C), and Ti-Ni-0 (900"C) were constructed. Phase relationships were studied by both X-ray diffraction and metallotrra~hic methods. Allovs were prepared as 10 g buttons by melting in a noncon-sumable electrode, water-cooled copper crucible arc-melting furnace using a helium atmosphere. Oxygen was introduced quantitatively by the use of weighed amounts of TiO² or TiO. Iodide titanium and the purest available alloying metals were used. All results are discussed in terms of the nominal composition of the melts. Previous experience with making oxygen-rich alloys had shown that oxygen losses were not significant if a homogeneous melt was produced. Weight-loss measurements were used to check loss in metallics during melting. Anneals were conducted in evacuated Vycor bulbs, and annealing times ranged from 24 hr at 1000 °C to 48 hr at 900°C. To achieve equilibrium in certain sluggish alloys, seven-day anneals were used. Debye-Scherrer powder patterns were taken in a 14 cm diam camera using filtered CuK radiation (K² = 1.541232 kX; K., = 1.53739 kX). Specimens were prepared by crushing and screening previously annealed buttons. In general, the X-ray diffraction results were used to identify the major phases, while the metallographic examinations were more useful in indicating the number of phases present. By the use of the combined results and general fundamental rules governing ternary equilibrium, it was possible to construct isothermal sections in good detail. In some instances where auxiliary lattice-parameter data were available, it was possible to lay down tie lines and to locate more positively corners of three-phase fields. Isothermal Section of the System Ti-Fe-O at 1000°C The binary systems Ti-O³ and Ti-Fe4 have been published. Binary phases, TiO, TiFe, and TiFe2, are likely to be encountered in the titanium-rich corner of the system. The structures are NaCl (Bl), CsCl (B2), and MgZn, (C14) types, respectively. Although preliminary X-ray diffraction studies indicated the presence of a ternary phase in the composition range Ti,Fe,O-TiJ?e,O, metallographic examination of two specimens at these compositions revealed the presence of other phases. Thirty-eight alloys were used to delineate the phase boundaries of the isothermal section illustrated in Fig. 1. The five almost single-phase ter-

Jan 1, 1956

By H. I. Aaronson, S. Toney

When the component grains of .ferritic hicrystals of an Fe-1.55 pct Si alloy are disoriented through an angle "6 " about a conzmon [ll0] axis, the tendency for preferential growth of austenite crystals along the grain boundary during transformation at elevated temperatures is small when 11 deg, but increases rapidly at larger angles. This type of orientation-dependence indicates that grain boundary diffdsion promotes preferential growth along large-angle boundaries. Morphological differences between austenite crystals formed at small-angle [1101 and [loo] boundaries suggest that precipitate morphology can be dependent on the dislocation structure of the boundary. ThE morphology of precipitate crystals nucleated at a grain boundary can be significantly affected by the structure of the boundary.' The limited amount of experimental evidence available in the literature indicates that the morphological effects of boundaries made up of arrays of dislocations, such as subbound-aries and small-angle grain boundaries, are different from those of boundaries having essentially disordered structures, i.e., large-angle grain boundaries. On the basis of indirect evidence, it has been concluded that large-angle grain boundaries give rise to the formation of grain boundary allotriomorphs (crystals which nucleate at grain boundaries, and grow preferentially and more or less smoothly along them)2 in the proeutectoid ferrite and the proeutec-toid cementite reactions in plain-carbon steels, and apparently also in many non-ferrous alloys.' At small-angle grain boundaries in a plain carbon steel, on the other hand, ferrite crystals were found to take the form of primary side plates. Similarly, Guinie, loys. Primary sideplates formed at a subboundary with a constant orientation tend to be parallel to only one, or occasionally two matrix habit planes, and a marked change in the orientation of the boundary is accompanied by a change in the habit plane. Previous studies on the morphological effects of grain boundary structure were performed on poly-crystalline aggregates. Information on the disorien-tation of the pairs of grains forming the boundaries at which the various morphologies appeared in these specimens was largely either qualitative or semi-quantitative. Precipitate morphologies accordingly could not be accurately and systematically correlated with grain boundary structure, and thus theories which have been proposed for the various morphological effects could not be satisfactorily tested. This investigation was undertaken in an attempt to remedy these deficiencies by studying the morphological effects of grain boundary structure with a method in which the boundaries are formed by matrix grains whose disorientations are known and controlled with reasonable accuracy. EXPERIMENTAL PROCEDURE The crystallographic requirements of this study were fulfilled by means of oriented bicrystals of silicon-iron. Disorientation of the component ferrite crystals was carried out about common, major crystallographic axes through angles ranging from 1/2 to 44 deg. The silicon content was low enough SO that the bicrystals could be partially transformed to austenite by heating to elevated temperatures. The silicon-iron used had the following initial composition: 1.55 pct Si, 0.04 pct C, 0.0031 pct N, 0.17 pct Mn, 0.020 pct S, and 0.002 pct P. The alloy was obtained in the form of 0.036-in. sheet. The procedures employed to prepare seed crystals in strips of this sheet, to reorient the seeds, and to grow them into bicrystals are essentially those described by Dunn and Nonken and aynes." The characteristics of the bicrystals are given in Table I. The "bicrystal type" indicates the crystallographic plane parallel to the broad faces of the strip in both grains and the crystallographic direction which was parallel to the long edges of the strip in both grains prior to disorientation. The angular disorientation of the grains, 8, which was performed about the direction normal to the plane of the broad faces of the strip, was measured between the [ 00l] directions. Orientation of the grain boundary, , was taken as the angle between the plane of the grain boundary and a plane containing the axis of disorienta-

Jan 1, 1962

By E. V. Watts

The D-7 zone of the Ventura Avenue field is of special interest because the initial reservoir pressure at 92.00 ft nearly equaled the pressure exerted by the overburden. While the phenomenon has been observed elsewhere in the world, there is no record of a previous case in California. Such high pressures have been attributed to sealing of the reservoir, followed either by emergence of the beds or by compaction of the sediments in various ways. Oil in the D-7 zone is undersaturated. At pressures above the bubble point, oil is recovered by the slight expansibility of the reservoir framework and its liquid contents. More than 40 pct as much oil probably will be recovered by this mechanism as will be recovered by internal gas drive after pressures pass below the bubble point. Operations are handicapped by sand and pipe troubles. Introduction The Ventura Avenue field has been under development since 1915. It has long been considered a "high-pressure" field, but interest was heightened by the extreme conditions encountered in the recent development of the so-called D-7 zone. The original reservoir pressure in this pool is estimated to have been 8300 psi at a depth of 9000 ft below sea level, or 9200± ft below the surface. A fluid pressure approaching that exerted by the overlying sediments has been encountered in other parts of the world, but never before in California to the degree observed in the D-7 pool. With few exceptions, the original pressure in California fields is about equivalent to the static head of water below the water table in the outcrop. Structure The Ventura anticline is a prominent feature of the Ventura basin, being traceable on the surface about 17 miles.' The Ventura Avenue field is at the apex of the anticline. It is about one mile wide and five miles long, the major axis lying in an east-west direction. The productive limits cover an area of about 2300 acres. The entire anticline has been severely folded and faulted. The productive portions in particular are broken up by three major thrust faults having a general east-west strike. The resultant four fault blocks are termed the A, B, C, and D blocks, respectively. Certain electric-log intervals are assigned numbers. Fig I is a diagrammatic north-south section of the field near the crest, looking west, and shows three of the four fault blocks. To the west, the upper fault divides into two branches, which define the B block. Wells penetrating a fault may duplicate over 1000 ft of formation. However, the greater fault movement is the strike shift, which is believed to exceed 2500 ft both between the A and C blocks and between the C and D blocks. The location of water is irregular and unpredictable. A few intermediate waters exist, while some strata have more than 2000 ft of productive closure.

Jan 1, 1948

By E. V. Watts

The D-7 zone of the Ventura Avenue field is of special interest because the initial reservoir pressure at 92.00 ft nearly equaled the pressure exerted by the overburden. While the phenomenon has been observed elsewhere in the world, there is no record of a previous case in California. Such high pressures have been attributed to sealing of the reservoir, followed either by emergence of the beds or by compaction of the sediments in various ways. Oil in the D-7 zone is undersaturated. At pressures above the bubble point, oil is recovered by the slight expansibility of the reservoir framework and its liquid contents. More than 40 pct as much oil probably will be recovered by this mechanism as will be recovered by internal gas drive after pressures pass below the bubble point. Operations are handicapped by sand and pipe troubles. Introduction The Ventura Avenue field has been under development since 1915. It has long been considered a "high-pressure" field, but interest was heightened by the extreme conditions encountered in the recent development of the so-called D-7 zone. The original reservoir pressure in this pool is estimated to have been 8300 psi at a depth of 9000 ft below sea level, or 9200± ft below the surface. A fluid pressure approaching that exerted by the overlying sediments has been encountered in other parts of the world, but never before in California to the degree observed in the D-7 pool. With few exceptions, the original pressure in California fields is about equivalent to the static head of water below the water table in the outcrop. Structure The Ventura anticline is a prominent feature of the Ventura basin, being traceable on the surface about 17 miles.' The Ventura Avenue field is at the apex of the anticline. It is about one mile wide and five miles long, the major axis lying in an east-west direction. The productive limits cover an area of about 2300 acres. The entire anticline has been severely folded and faulted. The productive portions in particular are broken up by three major thrust faults having a general east-west strike. The resultant four fault blocks are termed the A, B, C, and D blocks, respectively. Certain electric-log intervals are assigned numbers. Fig I is a diagrammatic north-south section of the field near the crest, looking west, and shows three of the four fault blocks. To the west, the upper fault divides into two branches, which define the B block. Wells penetrating a fault may duplicate over 1000 ft of formation. However, the greater fault movement is the strike shift, which is believed to exceed 2500 ft both between the A and C blocks and between the C and D blocks. The location of water is irregular and unpredictable. A few intermediate waters exist, while some strata have more than 2000 ft of productive closure.

Jan 1, 1948

By G. Carman Ridland

In conjunction with a geological investigation of the silver-bearing veins at Contact Lake, Northwest Territories, Canada, a survey was made with a Geiger-Miiller counter of the gamma-ray emissions from the rocks in the vicinity of the mine workings. Discontinuous pitchblende veins have been encountered occasionally in the silver-bearing fissures, and the geophysical survey was undertaken with the hope that abnormally high gamma-ray intensities, if detected, might lead to larger and more continuous pitchblende discoveries. Before the instrument was used at Contact Lake, preliminary tests were made, first with laboratory specimens at Princeton University, and later over known pitchblende deposits at the Eldorado property, LaBine Point, N.W.T. The Geiger-Müller counter, as adapted for field use, is described; the technique of transporting and operating the instrument is outlined; and the general precautions to be observed are discussed. The results obtained at Great Bear Lake show that the instrument is capable of detecting not only a pitchblende ore shoot in a shear zone, but also the mildly radioactive "host rock" at a considerable distance from the ore body. Hence, use of the Geiger-Müller counter is urged, not just for the detailed search for an ore body in a shear zone, but for the detection of possible radioactive "host rocks" in large-scale reconnaissance surveys of unexplored regions made by prospectors and members of federal geological survey parties. Location.—Along the rocky eastern shores of Great Bear Lake, in the Northwest Territories of Canada, lies one of the world's great radium-producing areas. The Eldorado mine, owned and operated by the Eldorado Gold Mines, Ltd., is at LaBine Point; while the Contact Lake mine, operated by Bear Exploration and Radium, Ltd. (B.E.A.R.), lies 9 miles to the southeast of LaBine Point and 2 miles south of Echo Bay, an indentation in the eastern shore line of Great Bear Lake. Geology.—The Eldorado company obtains its radium by the mining of the mineral pitchblende, which is found associated with a complex variety of metallic and nonmetallic minerals1 in quartz-carbonate veins occurring in metamorphosed pre-Cambrian sediment aries. Most of the pitchblende is intimately associated with a brown quartz and belongs to an early hydrothermal stage of mineralization during which safflorite-rammelsbergite and minor cobalt-nickel minerals were also deposited. Some pitchblende occurs with a group of minerals belonging to a later stage of mineralization in which the gangue is mainly dolomite and sometimes ferruginous rhodochrosite. Associated with this group are native silver and lead-zinc-copper sulphide minerals. The Contact Lake property owes its existence to the mining of rich, native silver ore shoots, which are

Jan 1, 1946

By G. Carman Ridland

In conjunction with a geological investigation of the silver-bearing veins at Contact Lake, Northwest Territories, Canada, a survey was made with a Geiger-Miiller counter of the gamma-ray emissions from the rocks in the vicinity of the mine workings. Discontinuous pitchblende veins have been encountered occasionally in the silver-bearing fissures, and the geophysical survey was undertaken with the hope that abnormally high gamma-ray intensities, if detected, might lead to larger and more continuous pitchblende discoveries. Before the instrument was used at Contact Lake, preliminary tests were made, first with laboratory specimens at Princeton University, and later over known pitchblende deposits at the Eldorado property, LaBine Point, N.W.T. The Geiger-Müller counter, as adapted for field use, is described; the technique of transporting and operating the instrument is outlined; and the general precautions to be observed are discussed. The results obtained at Great Bear Lake show that the instrument is capable of detecting not only a pitchblende ore shoot in a shear zone, but also the mildly radioactive "host rock" at a considerable distance from the ore body. Hence, use of the Geiger-Müller counter is urged, not just for the detailed search for an ore body in a shear zone, but for the detection of possible radioactive "host rocks" in large-scale reconnaissance surveys of unexplored regions made by prospectors and members of federal geological survey parties. Location.—Along the rocky eastern shores of Great Bear Lake, in the Northwest Territories of Canada, lies one of the world's great radium-producing areas. The Eldorado mine, owned and operated by the Eldorado Gold Mines, Ltd., is at LaBine Point; while the Contact Lake mine, operated by Bear Exploration and Radium, Ltd. (B.E.A.R.), lies 9 miles to the southeast of LaBine Point and 2 miles south of Echo Bay, an indentation in the eastern shore line of Great Bear Lake. Geology.—The Eldorado company obtains its radium by the mining of the mineral pitchblende, which is found associated with a complex variety of metallic and nonmetallic minerals1 in quartz-carbonate veins occurring in metamorphosed pre-Cambrian sediment aries. Most of the pitchblende is intimately associated with a brown quartz and belongs to an early hydrothermal stage of mineralization during which safflorite-rammelsbergite and minor cobalt-nickel minerals were also deposited. Some pitchblende occurs with a group of minerals belonging to a later stage of mineralization in which the gangue is mainly dolomite and sometimes ferruginous rhodochrosite. Associated with this group are native silver and lead-zinc-copper sulphide minerals. The Contact Lake property owes its existence to the mining of rich, native silver ore shoots, which are

Jan 1, 1946

By W. R. Seyfried

THE -problem of extracting alumina from clay and low-grade bauxites has been the subject of considerable interest for some time. The basic reason, of course, lies in the fact that known reserves of high-grade bauxite are not inexhaustible and that the present commercial process cannot successfully cope with low-grade bauxites or clay. Ultimately it may be necessary to use these poorer raw materials for all commercial operations, An unprecedented demand for aluminum during the war emergency and the constantly threatened shortage of imported bauxite caused the United States Government to take an active role in this problem. Through the National Academy of Sciences, the War Production Board and the Defense Plant Corporation, it investigated processes and finally selected four to be used in the construction and operation of four experimental plants. Each plant was to be designed in such a way as to facilitate its incorporation into a larger commercial plant should the need arise. The Chemical Construction Corporation process, or "Chemico" ammonium sulphate process as it is better known, was one of the four selected. The extensive literature and patents on record before the war generally follow one of two process-types depending upon the extracting reagent used. One group uses an acid reagent, the other an alkali. The Chemico process uses an acid reagent. For those interested in other processes described in literature, there is a short bibliography at the end of this paper, The basic steps of all acid extraction processes are: (I) to make the aluminum silicates acid soluble, (2) to separate the released alumina from impurities and insoluble gangue, and (3) to recover the reaent for re-use. THE PROCESS AS PLANNED In April 1941, a group of chemists and engineers of the Chemical Construction Corp, became interested in the problem of extracting alumina from clays and low-grade bauxites and, under the leadership of Mr. Blakeslee Barnes, Vice President and General Manager of the Company, first drafted a process in July of that year-five months prior to Pearl Harbor. The work continued in our research laboratories and with a small pilot plant, By June 1943, the work had progressed to a point where it was possible to apply for a patent on the process which was U.S. patent 2,405,426, granted August 6, 1946. Immediately prior to the development of the Salem plant, the process was envisaged to be as follows: I. The first step was to make the aluminum silicates acid soluble. It was planned: (a) Clay or low-grade bauxite would be roasted at 700 to 800°C (1292° to 1492°F). (b) The roasted ore would then be leached .with hot aqueous ammonium bisulphate to form a slurry. In this way the

Jan 1, 1948

By K. P. Gupta, P. C. Panigrahy

The stabilization of the R, a-Mn, and 0-Mn phases have been studied in the Mn-Ti-Fe and Mn-Ti-Co systems. Iron and cobalt both appear to stabilize the (Mn-Ti) R phase to almost the sarne extent. The R-phase region was found to extend from the lowest e/a to slightly beyond the maximunz e/a limit known for this phase. But, while iron appears to stabilize the a-Mn phase, cobalt tends to stabilize the p-Mn phase. In the two systems manganese appears to get replaced by iron and cobalt in each of the mentioned phases. The instability of the a-Mn phase in the Mn-Ti-Co system and the /3 -Mn phase in the Mn-Ti-Fe system cannot be explained on the basis of adverse size effects because atomic diameters for both iron and cobalt (C.N. 12 at. diam) are ziery similnr and not much different from manganese which they replace. Qualitatively, the reason for the stability of the a-Mn and the p-Mn phases can be traced to the more favorable e/a ratio prevailing in the respective systems and to a competing tendency between the two phases. In transition metal alloy systems the o, p,P, R, a- Mn,' and p-Mn2 phases have been claimed as electron compounds. A large volume of work has been done to establish the criterion for the formation of the o phase but until very recently practically no systematic work was done on the a-Mn and the /3-Mn phases. A recent investigation on the P-Mn phase3 indicates the e/a criterion for p-Mn phase stabilization. Since the R phase was first known to appear only in certain ternary systems1 no detailed work was then possible for this phase. The R phase has been recently discovered as a binary intermetallic compound in the Mn-Ti~ and Mn-si~-' binary systems. The existence of binary R phases opens up the possibilities of studying the effect of alloying elements on the stabilization of the R phase. Of the two binary systems possessing an R phase, the Mn-Ti system appears to be more interesting because at a suitable high temperature it is possible to find the three electron compounds, the a-Mn, p-Mn, and R phases, side by side and it is possible to study the effect of a third transition element on these three electron compounds. For the present investigation iron and cobalt, so called B elements for the formation of electron compounds, have been used as the third element to study the stabilization of the a-Mn, P-Mn, and R phases. EXPERIMENTAL PROCEDURE The alloys were prepared by using 99.9 pct pure electrolytic Fe and Mn, 99.5 pct Co, and crystal bar titanium, supplied by Semi Elements Inc., New York and Gallard Schelsinger Mfg. Co., New York. Weighed amounts of the components were melted in recrystal-lized alumina crucibles in an inert atmosphere (argon) high-frequency induction melting unit. Titanium was made into fine chips for easy dissolution and a special charging procedure was adopted to avoid contacts of titanium chips with the alumina crucibles. Up to 20 at. pct Ti, the maximum titanium content in the investigated alloys, there was no visible sign of reaction of titanium with the alumina crucibles. With a careful control of melting time and temperature the losses were minimized and were always found to be below 0.1 pct. Because of such small and almost constant weight losses, the alloys were not finally analyzed. The alloys were wrapped in molybdenum foil and annealed in evacuated and sealed silica capsules at 1000" * 2°C for 72 hr and subsequently quenched in cold tap water. Annealed samples were examined metallographically and by X-ray diffraction. For all high manganese alloys oxalic acid solutions of various concentrations and 1.0 pct HN03 solution were found suitable as etching reagents. Best contrast between the a-Mn and the R phases could be obtained by using freshly prepared 60 pct glycerine + 20 pct HN03 + 20 pct HF solution. For high iron and cobalt containing alloys, especially for alloys containing the a-Fe, y-Fe, and P-Co phases, 15 cc HNOJ + 60 cc HC1 + 15 cc acetic acid + 15 cc water solution was found to be the best etching reagent. All X-ray diffraction work was carried out (using specimens prepared from annealed powders) with a 114.6 mm diam Debye-Scherrer camera using unfiltered FeK radiation at 25 kv and 10 ma. All calculations for X-ray diffraction work were carried out using an IBM 7044 digital computer RESULTS AND DISCUSSION The two ternary systems, MnTiFe and MnTiCo, were investigated near the manganese rich end, Figs. 1 and 2, and show some common features. In both alloy systems large extensions of narrow R phase regions occur at almost constant titanium contents. At titanium contents higher than that of the single phase R-phase alloys, the same unidentified X phase was found in both ternary systems. The extensions of the X phase close to the Mn-Ti binary indicate that this phase could be the TiMns phase. Too few X phase diffraction lines were present in the diffraction patterns to make positive identification of the X phase. In contrast to this similarity the two systems show opposite behavior in the extensions of the a-Mn and 8-Mn phase regions; while iron tends to stabilize the a-Mn phase, cobalt

Jan 1, 1970

By Lyall Zickrick

As a result of the studies on recrystallization and crystal growth made in this laboratory, certain theories have been developed. These are expressed briefly in a paper by Dean and Hudson.1 One of the principal points brought out in that paper is that in the deformation of a crystal, the energy supplied is distributed to the atoms of the lattice, probably by the forced formation of molecules. It is found that a Maxwellian distribution of the energy among these atoms will account for the grain growth at various temperatures. According to such a distribution the number of atoms with energy above a certain critical value, E, necessary for recrystallization at the absolute temperature T is given by n Ne(-E/kT) where N is the total number of atoms. It is apparent that if this line of reasoning is correct, a metal which has been cold-worked and reheated to a temperature below that of complete annealing will have the atoms with the higher energy recrystallized, that is, reduced to normal energy and there will remain only atoms below a certain energy. If this metal is again cold-worked the peak in the number-energy distribution curve will be displaced toward the regions of lower energies, that is, higher temperature of recrystallization. By a repetition of this process the position of this maximum and hence the recrystallization temperature of the metal could be raised considerably. In order to' check this theory, experiments have been made on copper wire. The wire was drawn from 1/4-in. rod to 22 B & S gage and then sample lots were annealed at 400 and 220° C., respectively. The wire annealed at 400° C. gave an elongation of 34 per cent., whereas that annealed at 220° C. gave only 23 per cent. These wires were then drawn by identical practice to 34 B & S gage and the elongation determined after an anneal of 3 mm. in an oil bath held at various temperatures.

Jan 1, 1927

By H. H. Stoek

Danville, the county seat of Montour county, Pa., was one of the earliest and best-known centers of the iron intlustry in the State. It is situated on the north bank of the north branch of the Sosquehanna river, twelve miles east of the confluence of the north and west branches of that river at Northurnberlttnd. The ore-belt, extending for a distance of twelve miles along the north bank, has been developed in a number of places, but nowhere so extensively as in the immediate vicinity of Danville. Hence, a description of the mines in that locality will suffice, as typical of the workings of the entire section. Geology. The Montour ridge consists of an anticlinal fold extending from the source of Wapwollopen creek on the east to the west branch of the Susquehanna, which it reaches at the mouth of Chilisquaque creek. According to the reports of the First Geological Survey of Pennsylvania, the length of the ridge is nearly twenty-seven miles, with an average breadth of three-fourths of a mile, and a maximum elevation of six hundred feet in the vicinity of Danville, where it also attains its greatest width. Just north of Danville the Mahoning creek cuts through it, exposing the iron-ore on the hill-side, where advantage has been taken of this to work the beds on the southern slope of the ridge by means of drifts. The sections given in Fig. 1 are taken from the reports of the First Geological Survey of Pennsylvania, made in 1858, by H. D Rogers, whose description of the Moatour ridge was so complete and accurate that the entire report was reprinted as an appendix to Vol. G 7 of the Second Geological Survey. The approximate crosssection shows that near Danville the top of the ridge is of Clinton vol, xx.—24

Jan 1, 1892

By J. H. Wernick, J. E. Kunzler

HIGHLY pure metals are needed for low-temperature electron transport studies in progress. Recent improvements in purification techniques, such as zone refining, have made it possible to obtain metals with improved purity. For some metals, the improvement has been to the extent that ordinary analytical techniques are inadequate and special methods are needed.1 For other metals purification is more difficult, so that simple but rapid analytical methods are desirable as an aid in evaluating the effectiveness of purification procedures. Furthermore, it is desirable to be able to determine the impurity level of the sample or ingot with the minimum of physical disturbance of the material. In order to aid in the preparation of purer metals, techniques involving the measurement of electrical resistance at liquid-helium temperatures have been devised for studying impurity distributions in zone-refined ingots and other bulk samples without destroying the ingot or its geometry. The method yields information on the variations in purity along the length of the ingot or sample and provides a measure of the overall purity of the material. Compared with ordinary analytical methods, the resistivity method is rapid, sensitive, and does not require significant physical disturbance of samples with reasonable shapes. It has the disadvantage that resistance measurements are not specific, i.e., they do not identify the impurity. However, this disadvantage is offset by the advantage of being able to establish a measure of the overall purity so far as electrically active" impurities are concerned. METHOD AND ITS BASIS The method is based on the well-known fact that the resistivity, at Liquid helium temperatures, of a reasonably pure metal containing no regions with additional phases decreases with increasing chemical purity or a decrease in the number of physical defects. It is convenient to separate the total resistivity into three parts: where is the resistivity due to the scattering of the conduction electrons by the lattice vibrations or phonons, p is the contribution due to physical defects, and originates from the effect of chemical impurities in the metal. Insofar as Matthiessen's rule is obeyed,2 pphys and pchem are independent of temperature. Except possiblyin the very purest metals, ptherm is negligible at liquid helium temperatures and For zone-refined metals, which normally are well annealed and consist of large grains, at the chemical purity levels thus far attained the available data indicate that pphys is negligibly small or at least constant throughout the ingot. Assuming that the effect of physical defects is negligible for isotropic metals, This assumption appears consistent with most of

Jan 1, 1959

By J. M. Hodge, M. A. Orehoski

The relationship between hardenability based on a 50 per cent martensite criterion, and that based on higher percentages of martensite in a number of low-alloy steels was discussed in a previous paper by the authors.' It was found that the differences between the hardenability values based on the 50 per cent martensite and full martensite criterions increased as the hardenability increased and that, in the steels of higher hardenability, these differ-

Jan 1, 1947

By M. A. Orehoski, J. M. Hodge

The relationship between hardenability based on a 50 per cent martensite criterion, and that based on higher percentages of martensite in a number of low-alloy steels was discussed in a previous paper by the authors.' It was found that the differences between the hardenability values based on the 50 per cent martensite and full martensite criterions increased as the hardenability increased and that, in the steels of higher hardenability, these differ-

Jan 1, 1947

By U. N. Bhrany, N. Arbiter

F. C. Bond (Consulting Engineer, Processing Machin-Dept., AllisChalmers Manufacturing Co., Milwaukee) This is a very comprehensive paper. It deals with 1) size distribution functions, 2) energy-particle size relationships, and 3) criteria for grinding efficiency. The method of analysis used consists of tracing the increase and decrease of successive Tyler scale screen fractions as grinding progresses. The treatment is based upon the assumption that the work done in grinding is concentrated entirely upon the coarse size fractions in the mill. It is postulated that when a feed consisting entirely of particles of one size fraction is batch ground that finer fractions increase at a constant rate as grinding progresses, until finally each in turn begins to be ground and to decrease in amount. It is shown that under these conditions the empirical Gates-Gaudin-Schuhmann log-log size distribution plot can be logically explained. It is difficult to imagine any condition of ball mill operation, or any probability analysis, which would result in no grinding contacts on the finer particles present. However, the authors' postulate must be accepted if their conclusions are to be sustained. They conclude that the equation expressing the for mation rate of each size fraction can be resolved into the G.-G.-S. size distribution equation, and that the curvilinear portion of the log-logsize distribution line represents the only particle sizes which are being ground as well as produced. The author's statement that the G.-G.-S. Eq. 4 applies only to the finer portion of the size distribution while the Rosin-Rammler Eq. 6 applies over the whole size distribution range certainly supports the view that an exponential equation of the Rosin-Rammler type corresponds more closely to actual size distribution than does the power law G.-G.-S. equation. However, the G.-G.-S. equation is used to derive Eq. 8 and Eq. 9, which state that the energy required to grind a ton through a particular mesh varies inversely as the particle size to the exponent -a , whic h is the slope of the extended G.-G.-S straight line. This is stated to apply to both batch and continuous grinding. The G.-G.-S. slope exponent thus becomes very important in all crushing and grinding analyses by this method. The authors include some data which can be used to test their conclusions, as described below: We will consider grinding a feed composed of 14 mesh (1190u) to -200 mesh (74u). The average of 17 Allis-Chalmers grindability tests on quartz gives a work index (Wi) of 12.77. The -200 mesh product should have 80 pct passing 41.6u or P = 41.6. The equivalent 80 pct passing size of the 14 mesh feed particles is considered to be the particle diameter, as is true for spherical particles. Thus F is 1190u. In the work index equation 10 wi 10 wi 127.7 127.7 P f 41.6 1190 = 16.1 kw-hrperton. In Table I the ball mill exponent for quartz is 1.0 and from Eqs. 9 and 10: w=kw-hr/ton =Constan/(do/di) = 16.1 ton so that (1190) Constant/ Constant and the Constant equals 259. The tons per horsepower-hour value is 0.0464, in agreement with Table IV. The exponents for other minerals are listed in Tabl e 11. In Table IIA, the kilowatt hours per ton required to grind these minerals between the same sizes as the quartz, both by the authors' method and the work index equation, are listed. According to the authors kw-hrperton = 259/(16.1)".

Jan 1, 1961

By Roy C. Kirkman

Dear Editor: It is with great pleasure that I read Mr. Howard M. Wells article in the December 1978 issue of MINING ENGINEERING entitled: "Optimization of Mining Engineering Design in Mineral Valuation." Mr. Wells very adequately presents the case and point that there are a great number of variables which must be analyzed during an economic evaluation of an FUND RESOURCE, such as copper or uranium. I wish to take this opportunity to suggest that, given today's economic climate, decision making takes place under conditions of uncertainty and that this uncertainty justifies our need to examine each one of the parameters entered into the evaluation model. It is my contention that the influence of the tonnages and grades as well as their distributions, have the most profound effect upon the results of an evaluation. Everyone concerned with the evaluation of FUND RESOURCES realizes that as metal prices decline or stagnate with sharply rising direct operating costs, cutoff grades (Gc) must increase according to the equation below which Mr. Wells uses: Gc = Total Operating Cost/(Market Price X 20 X Recovery) However, historically, we have seen cutoffs move dramatically lower in both the copper and uranium industries for the past decade. Henceforth, this established the metals industry most important argument for processing greater tonnages of lower grade materials from disseminated deposits (refer to paper by Kirkman, Roy C.). These disseminated deposits, created by either concentration processes (uranium) or dispersion processes (copper, gold, molybdenum), have log-normal grade distributions (Fig 1). Gross profits are rising, but unit profits are falling. The industry has created longevity through economy of scale, i.e., mining vast tonnages of low grade. In order to develop the great tonnages necessary to prove economic viability, we must examine alternatives at the low-end of the tonnage grade relationship. Notice from [Fig. 2] that as we move further to the right away from line A-B drawn tangential to the average grade curve at 45°, total profits will increase (given fixed annual production capacity) and unit profits decrease. The theoretical optimum operating point is where: [ ] At this point my observation is that slight shifts in production capacity bring about greater changes in profitability due to greater grade changes. Therefore, the best financial risk evaluation is obtained by totally revising the mining engineers methods and fixing the financial parameters such as discount and interest rates. A 10% shift in either of these two parameters will not cause near the same variance in economic viability as will a change on the GRADE-TONNAGE curve [(Fig. 2)].

Jan 1, 1980

By W. L. Batt

MODERN war means mechanization, and mechanization means raw materials, especially minerals-and lots of them. Let me recall a few events of recent history-events that constitute mile- stones down the road to the war now blazing on three continents and threatening to spread still farther. In 1932, Japan took Manchuria, largely upon the excuse that she needed raw materials; in 1935, Italy invaded Ethiopia, largely upon the excuse that Mussolini's growing nation needed raw materials-in this case oil; from 1933 to 1935, Germany cried out for a greater share of the world's natural wealth, and since 1938 has invaded or occupied ten other countries, frequently upon the excuse that she needed-and had a right to-more raw materials.

Jan 1, 1940

By P. Barnes

(Read at the Wilkes-Barre Meeting, May, 1877.) THESE furnaces are of the ordinary Siemens type, and present no special peculiarities of construction. The bed of each is 8 feet by 20 feet clear inside of the walls and ports. The producers are placed at a distance of about 200 feet from the furnaces, and the gas is collected in an iron tube and led across the yard overhead. It then drops underground into the gas flue, and is distributed to the furnaces. A considerable weight of floor-plates over the valve-pits is included in account 39, but none of the general stock of floor-plates for the mill were charged to the furnaces. In Table No. 1 is shown the money cost of the furnaces as distributed to the several accounts named. In Table 2 is shown the proportion of each account due to each of the several items or classes of expenditure named.

Jan 1, 1878

By S. S. Solomons, V. H. Tillmann, L. Smaniotto

INTRODUCTION The Zinc Corporation, Limited and New Broken Hill Consolidated Limited (ZC/NBHC) mines are situated at Broken Hill, New South Wales, Australia (refer Fig. 1). Both companies are wholly owned subsidiaries of Australian Mining and Smelting Limited (AM&S). Annual production from both mines is 2.3 million tonnes of lead, silver and zinc ore mined by a variety of underground methods. From 1911 to 1968, conventional overhand cut and fill stoping (both open and square set timber) was used almost exclusively, though some trials with shrinkage and sublevel stoping were undertaken. The trial stopes used short holes in conparison with today's sublevel open stopes. Mechanised cut and fill methods with regular rockbolt support were introduced in the early 1960's and undercut and fill stoping replaced square set timber stoping for pillar extraction in the late 1960's. Since 1968, increasing emphasis has been placed on longhole open stoping (LHOS) although some areas of the orebodies are comrnrnitted to the abovemehtioned methods since existing stope development makes it impracticable to change. In 1979, approximately half the total production was mined by LHDS and it is expected that the LHOS proportion will increase in the future. A vertical crater retreat method of longhole mining has also been successfully introduced to replace the undercut and fill stoping of some pillars and it is expected that this stoping method will be used in some future primary ore extraction. This paper reviews the progress of LHOS technology at ZC/NBHC with emphasis on the stope planning and design process and the importance of rock mechanics applications. The objective has been to maximise the primary extraction of the orebody giving due consideration to stability and safety. This has led to the design of a novel sloped wall longhole stoping method which should eliminate the formation of pillars by mining the orebody in a "continuous" manner incorporating a sloped sand interface between the blocks of ore being mined and the previously mined sandfilled stope. The expected results include the complete extract of the orebody without the formation of pillars and with minimal dilution of ore with sandfill. The evolution of the method can be best illustrated by following the mining progress of the relatively new Southern 'B1 Lode orebody at the NBHC mine. GEOLOGY Southern '8' Lode is the southern extension of the 'Bt Lode orebody, which is currently being mined further to the north in ZC/NBHC (refer Fig. 2). The ore block being developed and stoped extends for a vertical height of 90 metres from No. 17 level down to approximately ten metres above No. 19 level. The ore minerals are sphalerite and galena with the zinc:lead ratio averaging approximately 3:l with a minor amount of silver associated with the galena. There is a sharp contact between the ore and the country rock on the footwall and keel, while the hanging wall gradates into medium and low grade material. The gangue is primarily quartz together with garnet, biotite, feldspar, gahnite, sericite and minor apatite. In various horizons within the orebody, grey feldspar, quartz and garnet pegmatites occur as stratiform layers. The ore and country rock are competent with some inconpetent boundaries.

Jan 1, 1981