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By J. H. Smith, H. W. Paxton

ALTHOUGH many structural and kinetic investigations have been made for alloys of iron and nickel, only meager data exist from thermodynamic investigations. The purpose of this note is to estimate the free energy of the Fe-Ni solid solutions from thermodynamic data available for ternary alloys containing iron and nickel. The lack of a description of the thermodynamic behavior for the Fe-Ni system has required the structural and kinetic analyses of the system to assume some form of solution behavior, usually regular, e.g., the mar-tensite transformation analysis of Kaufman and Cohen, 1 consistent with the limited thermodynamic data. Indications that this system could exhibit ideal solution departures might have been suggested by the large deviations from additivity rules observed in the density and lattice-parameter measurements of Jette and Foote2 who interpreted this in terms of possible solute-solvent interactions. Later Turkdogan et al. 3 and more recently Ward and wright 4 found a minimum in the graphite solubility in liquid Fe-Ni solutions near the concentration of FeNi3 with deviations from linearity persisting at all concentrations. This was interpreted by Ward and wright4 to indicate negative heats of solution and was suggestive of short-range ordering. The infinitely dilute activity coefficient of carbon (?oC) was also observed by smith5 to pass through a maximum near the FeNi3 concentration in Fe-Ni solid solutions. Recent investigations of the liquid solutions over the entire concentration range by Zellars et a1.' and Speiser et a1.," using vapor-pressure determinations, revealed both negative departures from Raoult's law and a nonregular solution behavior. The solid alloys have been studied by Oriani 8 and Kubaschew-ski and von Goldbeck6 employing gaseous H2/H2O equilibria with Fe and FeO. Both investigations were in substantial agreement, indicating very small departures from ideality. However, Oriani observed the formation of Fe3O4 (instead of FeO) at XFe= 0.441 which severed the equilibrium and precluded experimental investigation of the nickel-rich alloys. Heat-capacity and heat-content measurements have been evaluated by Montgomery10 and found generally unsatisfactory for gleaning thermodynamic information. This is due to the unknown final states of the alloys caused by the interference of the martensite transformation on cooling iron-rich concentrations and superlattice formation, magnetic transformation, and the varied heat treatments used by investigators of nickel-rich concentrations. As an alternative to the experimental difficulties, indirect estimates of the solid-solution behavior have been made by Fleischer and Elliott11 and Smith et a1.12 From their measurements of the solubility of Fe-Ni alloys in liquid lead, Fleischer and Elliott calculated the nickel activity (aNi) (and integrated for aFe) by assuming: 1) liquid lead has no solubility in solid Fe-Ni alloys, 2) Henry's law is obeyed throughout the liquid lead-rich phase (0— 12 at. pct Nil, and 3) Henry's law constant is independent of relative iron and nickel concentrations. The estimate of Smith et a1.12 was obtained

Jan 1, 1964

By F. W. Newhall, L. N. Plein

During the latter part of the year 1931, the Republic mine of the Republic Steel Corporation, at Republic, about 4 miles south of Brownsville, Pa., was mining coal along four rib or fracture lines. One of these lines, the west butt rib line, was retreating towards a concrete-lined air shaft, 320 ft. deep, which had been sunk in 1911 for ventilation purposes. With the normal rate of mining at that time, it was expected that this rib line would pass the shaft in three or four months and the shaft would then be abandoned and allowed to cave. Realizing the opportunity presented for the study of an unusual case of ground movement, the question of conducting the study was presented by the junior author to thechairman of the Institute's committee on Ground Movement and Subsidence, Mr. George S. Rice, who presented the matter to Mr. G. H. Morse, General Manager of the Northern Mines, Republic Steel Corporation, and he agreed to cooperate with the Bureau of Mines in making the study, the results of which arc presented in this paper. Acknowledgments are due to Mr. Morse for his full cooperation in this work and to Mr. G. S. Rice and Mr. J. W. Paul, both of the U. S. Bureau of Mines, for their advice and guidance during the course of the work. The authors are indebted to Mr. B. F. Herbert, mining engineer, Northern Coal Mines, Republic Steel Corporation, who assisted in all the surveys, and Mr. W. H. Smith, draftsman, U. S. Bureau of Mines, who prepared all illustrations for publication. Geologic Conditions The shaft is at Merrittstown, which is about one mile northwest of Republic. The topography in the immediate vicinity of Merrittstown consists of rolling country dissected by the meanders of Dunlap Creek and its tributaries. The surface slopes of the hills are gentle and their average gradient is less than 6º. The area at the point where the study was made lies on a hillside sloping towards the southwest, the gradient, varying from 1º to 14º. Fig. 1 shows contour lines at 5-ft. intervals on

Jan 1, 1936

By L. N. Plein, F. W. Newhall

During the latter part of the year 1931, the Republic mine of the Republic Steel Corporation, at Republic, about 4 miles south of Brownsville, Pa., was mining coal along four rib or fracture lines. One of these lines, the west butt rib line, was retreating towards a concrete-lined air shaft, 320 ft. deep, which had been sunk in 1911 for ventilation purposes. With the normal rate of mining at that time, it was expected that this rib line would pass the shaft in three or four months and the shaft would then be abandoned and allowed to cave. Realizing the opportunity presented for the study of an unusual case of ground movement, the question of conducting the study was presented by the junior author to thechairman of the Institute's committee on Ground Movement and Subsidence, Mr. George S. Rice, who presented the matter to Mr. G. H. Morse, General Manager of the Northern Mines, Republic Steel Corporation, and he agreed to cooperate with the Bureau of Mines in making the study, the results of which arc presented in this paper. Acknowledgments are due to Mr. Morse for his full cooperation in this work and to Mr. G. S. Rice and Mr. J. W. Paul, both of the U. S. Bureau of Mines, for their advice and guidance during the course of the work. The authors are indebted to Mr. B. F. Herbert, mining engineer, Northern Coal Mines, Republic Steel Corporation, who assisted in all the surveys, and Mr. W. H. Smith, draftsman, U. S. Bureau of Mines, who prepared all illustrations for publication. Geologic Conditions The shaft is at Merrittstown, which is about one mile northwest of Republic. The topography in the immediate vicinity of Merrittstown consists of rolling country dissected by the meanders of Dunlap Creek and its tributaries. The surface slopes of the hills are gentle and their average gradient is less than 6º. The area at the point where the study was made lies on a hillside sloping towards the southwest, the gradient, varying from 1º to 14º. Fig. 1 shows contour lines at 5-ft. intervals on

Jan 1, 1936

By A. W. Gauger

It is with some trepidation that I approach my subject, for I know that I shall at once incur the suspicion of the mechanical engineer, with his concern for boiler tests and efficiencies; of the mining engineer, with his mechanization problems; and of the chemical engineer with his unit processes. Nevertheless, it must be recognized that the technology of fuels, the systematic body of knowledge relating to the production, processing and utilization of mineral fuels, has grown to such proportions and involves so many widely diverse applications of fundamental science and engineering that it behooves us to stop and consider just what its status is in relation to other technologies, as well as in relation to the present and future needs of the social order. The time has come when technologists, applied scientists and engineers must consider the possible effects that their achievements may have on Society. The development of a machine to - -replace -several hundred men is a fine achievement when considered solely from the point of view of creative endeavor. But what of the men who are displaced by the machine! Does not the responsibility for the development of this machine embrace as well the consequences of obsolescence and technological unemployment resulting from such development? I believe that it does and that we must recognize this fact in our practice of engineering and tech- nology as well as in the training of future engineers and technologists. Magnitude of the Fuels Industry Fuel technology is the body of knowledge that relates to the mineral fuels. The fuels industry is by far the most important of all Our mineral industries. The chart in Fig. I, reprinted from U. S. Bureau of Mines Information Circular No. 6643, indicates the compartive values of metals, fuels and other nonmetallic minerals for the year 1929. Of the grand total of 13¼ billions of dollars in value of minerals at the mines, the mineral fuels contributed 48 per cent. Coal, with 34.4 Per cent, exceeded the value of any other single mineral. In fact, the value of the production of the Pennsylvania anthracite mines alone anand exceeds the value of the gold production of the entire world. Petroleum and natural gas in 1929 contributed 14.3 per cent and 3.3 per cent, respectively, of the total value of world mineral production. So much for the world picture; let us now look at the situation in the United States. Over the 60-year period 1880 to '939, $46,409,727,000 of metal1ic products, $80,788,852,000 of fuels (coal, petroleum, natural gas, natural gasoline) and $27,871,-ooo,ooo of nonmetallic minerals other than fuels were produced. The mineral fuels have contributed 52.7 per cent of the entire mineral wealth produced over this period that has seen such tremendous industrial development in our Our As a matter of fact, our present industrial civilization has been made possible through the use of the

Jan 1, 1942

By A. W. Gauger

It is with some trepidation that I approach my subject, for I know that I shall at once incur the suspicion of the mechanical engineer, with his concern for boiler tests and efficiencies; of the mining engineer, with his mechanization problems; and of the chemical engineer with his unit processes. Nevertheless, it must be recognized that the technology of fuels, the systematic body of knowledge relating to the production, processing and utilization of mineral fuels, has grown to such proportions and involves so many widely diverse applications of fundamental science and engineering that it behooves us to stop and consider just what its status is in relation to other technologies, as well as in relation to the present and future needs of the social order. The time has come when technologists, applied scientists and engineers must consider the possible effects that their achievements may have on Society. The development of a machine to - -replace -several hundred men is a fine achievement when considered solely from the point of view of creative endeavor. But what of the men who are displaced by the machine! Does not the responsibility for the development of this machine embrace as well the consequences of obsolescence and technological unemployment resulting from such development? I believe that it does and that we must recognize this fact in our practice of engineering and tech- nology as well as in the training of future engineers and technologists. Magnitude of the Fuels Industry Fuel technology is the body of knowledge that relates to the mineral fuels. The fuels industry is by far the most important of all Our mineral industries. The chart in Fig. I, reprinted from U. S. Bureau of Mines Information Circular No. 6643, indicates the compartive values of metals, fuels and other nonmetallic minerals for the year 1929. Of the grand total of 13¼ billions of dollars in value of minerals at the mines, the mineral fuels contributed 48 per cent. Coal, with 34.4 Per cent, exceeded the value of any other single mineral. In fact, the value of the production of the Pennsylvania anthracite mines alone anand exceeds the value of the gold production of the entire world. Petroleum and natural gas in 1929 contributed 14.3 per cent and 3.3 per cent, respectively, of the total value of world mineral production. So much for the world picture; let us now look at the situation in the United States. Over the 60-year period 1880 to '939, $46,409,727,000 of metal1ic products, $80,788,852,000 of fuels (coal, petroleum, natural gas, natural gasoline) and $27,871,-ooo,ooo of nonmetallic minerals other than fuels were produced. The mineral fuels have contributed 52.7 per cent of the entire mineral wealth produced over this period that has seen such tremendous industrial development in our Our As a matter of fact, our present industrial civilization has been made possible through the use of the

Jan 1, 1942

By Richard D. Hagni

Although the ore microscopist routinely examines polished sections to determine the mineralogy and texture of ores, his importance to the solution of problems peripheral to geology is not always fully realized. The techniques which he uses can be applied with little modification to the solution of a wide variety of beneficiation problem. By extending his studies beyond those normally considered to be of interest to the geologist, he can include examinations of polished sections of selected mill products. This is a logical extension, because the minerals and textures in the polished sections of ores are the same as those in millproducts. The mill dressing engineer should be more aware of the types of beneficiation problem that can be solved by the ore microscopist and what the ore microscopist can do for him. A greater degree of cooperation between the ore microscopist and the mill dressing engineer can be of significant mutual benefit. Ore microscopy holds an advantage over chemical analysis, because the interrelations and combinations ofthe mineral constituents of an ore or mill product can be visually determined. This advantage provides solutions to many beneficiation problem. Locking is a type of beneficiation problem that is particularly amenable to ore microscopy. The percentage, type, and distribution of locked particles can be readily determined with the aid of an ore microscope and an estimate made of the extent of additional grinding required for liberation. The extent of intimately locked types, which no reasonable amount of grinding will liberate, can also be evaluated. Mineral coating conditions, free particles of a deleterious mineral, and free particles of a valuable mineral held in flocculated clusters of gangue are other features that can readily be observed. In some instances, visual examination may show that the problem is not one of locking. Photomicrographs illustrate the variety of beneficiation problems for which the ore microscope is applicable. These problems and their resolution demonstrate the importance of the instrument and show the value of close coordination between the mill dressing engineer and the ore microscopist.

Jan 1, 1979

By William E. Harris

Time and experience have demonstrated that by means of the Waelz process zinc, lead, cadmium, arsenic, antimony, bismuth and tin can be volatilized satisfactorily. In this way difficult gold ores are being treated to allow for the recovery of the precious metal. Iron ore containing zinc is being treated to remove the zinc and recover the iron. In Germany, thallium is being recovered in commercial quantities from the zinc oxide fume; indium, germanium and gallium are also concentrated to a degree warranting recovery, even though these rare metals are only recognizable in the ore by means of the spectroscope. The physical, chemical or mineralogical condition of the raw material affects very little the applicability of the process. The name Waelz is derived from the German word Waelzen, meaning a "trundling motion," which very aptly describes the movement of the charge through the slowly rotating kiln. The recovery of zinc and lead by volatilization in a rotary kiln has its origin in a process patented in 1910 by Edward Dedolph, of British Columbia. The Dedolph patent was taken over by the Metallgesell-schaft of Frankfurt-on-Main, Germany, which in cooperation with the Griesheim-Elektron, now a part of a large industrial combine, introduced certain improvements (Ohlmer, Specketer patents), but without bringing the process to a state suitable for large-scale operations. The war temporarily stopped all work on the process, and it was not until after the war that the Krupp Grusonwerk, of Magdeburg-Buckau, Germany, quite independently of the Metallgesellschaft, instituted research work in this field of metallurgy, which in 1923 led to the Waelz process proper. The Krupp Grusonwerk and the Metallgesellschaft A.G. later on collaborated, and by their joint efforts further developed and perfected the Waelz process, which they are marketing together as "Waelz-Gemeinschaft." The process is capable of treating a varied type of material; for instance, oxidized and sulphide zinc ores, calamine (zinc carbonate ore) waste dumps, jig tailings, jig slimes, table concentrate slimes, brass ashes, zinc-bearing iron ores (where the iron sinter is the real objective and the zinc oxide a by-product), electrolytic-zinc leach residues, zinc muffle residues and works sweepings, lead-furnace slags, tin ores and slags, anti-

Jan 1, 1937

By Walter Herd

Fox the past eight years No. 2 mine of the Cumberland Railway & Coal Co., Springhill, Nova Scotia-a subsidiary of the Dominion Coal Co., Ltd.-has had an unenviable reputation for bumps. As the workings extended in certain directions under a greater cover, these bumps increased in severity and it became apparent that some change in the system of extraction was necessary if the mine was to continue to operate. In September, 1924, following several fatalities resulting from bumps, the Mines Department of Nova Scotia requested from the U. S. Bureau of Mines the services of George S. Rice, Chief Mining Engineer of the Bureau, to report on the conditions then prevalent in No. 2 mine, Springhill. This request was promptly and courteously granted. Mr. Rice made a full investigation and a comprehensive and helpful report, which is embodied in the 1924 Annual Report of the Department of -Public Works and Mines, Nova Scotia. Prior to 1925, the room and pillar method was employed and in January of that year (there being a cessation of work from March to August due to labor troubles) longwall retreating on the west side, on a limited scale, and in a small section on the east side of the mine was started. The major portion of the east side was not operated on this system till August, 1926, as there was developed a considerable area ready for pillar extraction between an arbitrary boundary and a point up to which bumps of any consequence, had not been experienced. In the interval development work for longwall retreating below the 5900-ft. level was vigorously- pushed. This longwall retreating system was suggested by Mr. Rice as a possible remedy and was heartily endorsed by the company officials. This paper describes the conditions and happenings subsequent to Mr. Rice's report and more especially the results with the longwall retreating system of mining under the peculiar circumstances pertaining to mining. No. 2 Seam, Springhill, at depth, and records the 'conclusions which experience with several severe bumps under this mode of extraction would suggest. Except where necessary to make the paper intelligible as an entity any duplication of Mr. Rice's report will be avoided.

Jan 1, 1929

By P. W. Ramsey, E. J. Boyle, E. A. Anderson

ONLY a few zinc-rich alloys are in commercial use today, and these depend largely upon solid solution effects for their desirable properties. Typical examples are rolled alloys containing about I per cent of copper, with or without additions of elements such as magnesium,1 and die-casting alloys containing about 4 per cent of aluminum with small amounts of magnesium and sometimes copper.2 A number of elements are capable of forming alloys with zinc, which do not enter into solid solution except in limited degree. The present paper considers one such system, zinc-titanium, in which alloys having potentially useful properties in the rolled form were found. ZINC-TITANIUM SYSTEM The zinc-rich portion of the zinc-titanium diagram, as determined by standard methods in this laboratory,3 is shown in Fig. I. The portion of the diagram of significance in the present work extends from 0 to about 0.5 per cent titanium. Gebhardt4 places the eutectic at 0.45 per cent, but the evidence in favor of the composition given in Fig. I is considerable. The solid solubility of titanium in zinc is very low indeed and possibly places these alloys in a somewhat different category from the commercial alloys previously mentioned. ALLOY PREPARATION All of the alloys used in this work were prepared with titanium metal of 98.9 per cent purity. In most cases high-purity zinc (99.99 per cent) was used but sufficient work was done later to show that zinc of about high-grade composition would yield approximately equal results. Best practice in alloy manufacture seemed to be to prepare a zinc-titanium hardener by adding about 4 per cent of titanium metal to molten zinc and holding under a boric acid cover, with frequent stirrings, at 750°C. until the titanium had dissolved. The desired titanium content could readily be obtained in the final alloy by adding the calculated amount of this hardener. The alloys proved to be quite stable in composition, unless overheated, and, with reasonable temperature control, required no cover or flux to prevent loss of titanium content by oxidation. HOT-ROLLING TESTS Three alloys containing, by analysis, 0.05, 0.12, and 0.23 per cent titanium were selected for preliminary study. Slab cross sections revealed a marked grain refinement* (Fig. 2) in the two alloys of highest titanium content. Cast unalloyed zinc has a columnar grain structure similar to that shown for the alloy of lowest titanium content but without the scatter of small equiaxed grains at the center.

Jan 1, 1944

By S. F. Reiter

The paper presents isothermal recrystallization curves for 0.08 and 0.15 pct C steel at subcritical temperatures following small amounts of plastic deformation. The effects of deformation, temperature, and aging on nucleation and growth rates ore described. The free energy of activation for grain boundary migration in steel is given. SEVERAL excellent reviews of the literature have appeared concerning the recrystallization of metals.'-' The present investigation follows the approach advanced by Mehl, Stanley, and Anderson,6-7 in which the rate of recrystallization was analyzed in terms of N, the rate of nucleation, and G, the rate of growth of recrystallization nuclei. Two lots of low carbon, capped steel of the analysis given in Table I were studied. Each lot consisted of a 150 lb coil which had been hot rolled to 0.083 in. and then cold rolled to 0.042 in. at the mill. Strips 0.930 in. wide were sheared perpendicular to the rolling direction. Both steels were normalized before studying their recrystallization characteristics. The strips were cleaned, painted with a magnesia-acetone paste, and made into packs of equal weight, wrapped in 0.002 in. copper foil. The packs were placed in a salt bath at 900°C for 30 min and air cooled. A relief anneal followed in a second salt bath for 15 min at 650°C. The relief anneal was found necessary from early tests in which a longer incubation period and slower rate of recrystallization were observed in relief-annealed lot A steel than in similar material which was strained and recrystallized directly after being normalized. This effect, which indicates the presence of transformation and/or cooling stresses in steel air cooled from above the A, temperature, has also been observed by Samuels8 and Masing.9 Figs. 1 and 2 show the microstructure of lot A and B materials and illustrate the rather uniform No. 8 ASTM grain size produced by this heat treatment. Winlock and Leiter10 observed that strip specimens which had their sharp edges removed elongated more uniformly than those which were not polished. Similarly, when the sheared edges were removed on a belt grinder, it was found in the present investigation that such samples recrystallized more uniformly than did unpolished strips. Therefore, all strips were carefully rounded prior to their extension. The approximate strain limits for the production of large recrystallized grains are from 6 to 12 pct extension." It was found that for the purpose of this investigation, 8 and 9 pct elongation were suitable deformations. The strain rate employed was 0.01 in. per in. per min and produced a yield point elongation of 4 pct. Winlock and Leiter found that mild steel of No. 8 ASTM grain size gave the same yield point elongation when extended at 0.012 in. per in. per min. All of the lot A and B strips extended in tension developed a straight, stretcher strain line at each grip when the upper yield point was reached. The lines were parallel and made an angle of 55" with the edge of the strip. They approached each other with increasing strain and met near the center of the sample at the end of the yield point elongation. Immediately thereafter, a small drop in load was observed and then the load increased in a regular manner with increasing extension. The grips were initially 8 in. apart. After extension, the 6 in. gage length was carefully cut into 1 in. samples. The remainder of the strip was discarded. After a flash pickle in hot 50-50 hydrochloric acid, six samples, each of which had been taken from a different strip, were placed in a basket and submerged in a lead pot for isothermal recrystallization. Although no recovery effect was observed, strain aging did occur after extension. Therefore, samples were always recrystallized within 24 hr after their cold deformation. After recrystallization, the samples were etched with a solution comprised of one part by volume of nitric acid with three parts of water. Bromide printing paper was exposed directly at low magnifications and later used with a mask to measure the desired quantities. First, the average diameter of the largest grain visible in each sample was determined using dividers. Next, the number of recrystallized grains per unit area was counted and recorded as n. Then, for each sample, the combined area of the recrystallized grains was measured by transcribing the grain outlines to standard graph paper. Many determinations of the area of the recrystallized grains were repeated five times and indicated a standard error that was not greater than 25 pct. The average area for six samples was divided by the area of the mask to yield the percentage recrystallized. Recrystallization of 0.08 Pct C Steel The progress of recrystallization at 670°C after 8 pct elongation of lot A steel is shown in Fig. 3, a through f. The shapes of the growing crystals are approximately equiaxed, as is assumed in the

Jan 1, 1953

By L. W. Sink, B. H. Kear, S. M. Copley, M. F. Hornbecker

IT is well known that under appropriate conditions of chill casting, many metals and alloys develop a columnar grain structure having a high degree of preferred orientation.' In cubic materials, this principle has been employed to produce shaped castings with a unidirectional cube oriented columnar grain structure as well as shaped single crystals with a cube axis parallel to the growth ais.' "he purpose of this note is to describe how this same principle can be enlployed to produce wires, rods, or more complex crystal Shapes with a variety of conlpositions in cube or random orientations by a single casting operation. The procedure for directional solidification of in Fig. 2. Examination under crossed polarizers indicated that the striations were a second phase (presumably the B19 phase) which frequently forms initially at primary grain boundaries and then grows toward the interior as thin ribbons. X-ray studies on filings of this alloy reannealed at 1300°C for 15 min indicated a strong pattern of the fcc phase together with a substantial pattern of the B19 phase. The un-annealed filings, however, showed only the pattern of a cold-worked, fcc structure. In these two-phase alloys it appears, therefore, that the B19 phase is transformed into a disordered fcc structure by cold-working. The mechanical properties of these alloys would be of some interest since a fcc structure might be expected to possess greater ductility than the or-thorhombic B19 structure from which it forms. The author wishes to thank Mr. Harvey Yakowitz and Mr. Richard Manuszewski for obtaining the photomicrograph in Fig. 2. This research was partially supported by Research Grant DE-02455 from the National Institute of Dental Research. columnar grained ingots involves pouring a melt into a preheated mold having a water-cooled copper chill at its base? and controlling the temperature gradient in the mold so as to maintain columnar grain growth from end to end of the ingot.4 This is illustrated schematically in Fig. l(a). It should be noted that the longitudinal temperature gradient promoting unidirectional columnar grain growth is maintained by heat loss primarily through the solidifying ingot to the chill, so that both the temperature gradient and the growth rate diminish with increasing distance from the chill. As the distance from the chill increases? the columnar structure coarsens, and the perfection in preferred orientation tends to increase progressively. Using this same procedure of gradient solidification, Fig. l(b) shows a simple scheme for producing a batch of crystals having the same cube orientation rather than an assemblage of columnar grains. Wires and rods are produced by cementing ceramic tubes to the wall of the mold. The steep temperature gradient produced in the central chamber is controlled by the mold heater to produce favorable conditions for crystal growth. Clearly the success of the operation lies in the selection of individual growing columnar grains by some kind of orifice at the base of each channel in the mold. Using simple constrictions, experience with nickel-base alloys has shown that 4 -in.-diam holes at a distance of -1 in. from the chill yield crystals within 7 deg of (100); closer control of orientation is possible by placing the crystal selector farther away from the chill.

Jan 1, 1970

By J. F. Gormley

Drill pipe, and the connections used to join the pipe together, have had a long history of development and improvement. With the growing use of high tensile-strength pipe, the rotary shouldered connections used to join the lengths of drill pipe have become more critical. Fatigue-type failures of rotary-shouldered connections, or tool joints, have become a cause of much conern to operators and manufacturers. Most fatigue tests on tool joints have been made on the basis of bending moment applied vs number of cycles, rather than on the basis of stress vs cycles. A desire to learn more about the nature of stress in a tool joint due to bending caused a rather intensive experimental study to determine what actually happens to cause fatigue failure. It was known that a tool joint with insufficient make-up torque was subject to early fatigue failure. Therefore, the establishment of the relationship between make-up torque and allowable bending moment would enable a testing engineer to better correlate the results of various tests. The problem of calculating the stress in a tool joint due to an applied bending moment was complicated by: the effect of unknown stress concentrations; the applicability of the well known formula S = Mc/I; and the question of whether to use the combined cross section of the pin and box in calculating the moment of inertia I. TEST EQUIPMENT The test equipment consisted of the following. 1. A lathe modified to act as a fatigue machine for full-size tool joint or drill-collar specimens. 2. An adapter plate bolted to the headstock of the lathe and into which a short adapter was screwed. 3. Tool-joint pins on sections of drill collars bucked into the adapter. 4. A hydraulic load cylinder which rested on the bed of the lathe and applied bending moments to the joints. 5. Paper-backed strain gauges (FAP-12-12, 1/8-in. gauge length and A-5-1, 1/2-in. gauge length). 6. Eastman 910 contact cement for bonding gauges to joint and Epoxylite 222 waterproofing. 7. A 12-position switchbox, SR-4 bridge balancing unit connected to an SR-4 strain indicator to read the gauge output. 8. A four-channel Sanborn recorder, Model 150, was used as the readout instrument for part of the testing. The fatigue machine was well suited as a loading device. Because of the long lever arm available, the change of moment with distance was small; consequently, the vertical shear stress was small, less than 300 psi. Some difficulty was experienced with the hydraulic load cylinder at high bending moments due to leakage. The strain gauge equipment was simple and quite reliable. A 41/2-in. extra hole (E. H.) joint with "as machined" threads and shoulders and a 2 7/8-in. internal flush (I. F.) joint with copper-plated threads and shoulders were selected for testing because of their common usage in the field. In addition, the 4 1/2-in. E. H. was suitable because it had an inside diameter large enough to permit the insertion and accurate positioning of strain gauges without using special jigs, while the 2 7/8-in. I. F. joint required much lower bending loads to cause separation of the shoulders of the joint when made up to the recommended torque. The joints were made to standard API specifications, except for very small bevels on the box and pin shoulders and cylindrical stress-relief grooves added to the pins. Larger bevels would have

By Robert D. Pehlke, Robert G. Blossey

The solubility of nitrogen in liquid cobalt and a number of dilute cobalt alloys Was measured in the temperature range 1550" to 1700°C at nitrogen pressures to 1 atm. At 1600°C and 1 atm nitrogen pressure, the solubility in pure cobalt is 0.0047 wt pct [3.8 cu cm (stp) per 100 g Co]. The standard free- energy change for the solution reaction 1/2 N,(g) = gout pct in Co) is iF - 10,000 + 5.24 T cal per g atom N. The alloying elements Cv, Cu, Mo, Nb, Tu, W, and V increase the nitrogen solubility, while Al, Fe, Ni, and Si decrease the nitrogen solubility. THE solubility of nitrogen in cobalt was studied previously by Sieverts, Busch and Dodd,2 and Schenck, Frohberg, and Graf.3 Sieverts investigated the solution below the melting point of cobalt, and Busch and Dodd worked with the liquid metal; however, neither study found any solubility for nitrogen in cobalt. Schenck et al, reported a solubility of 0.005 wt pct N in cobalt at 1600°C. Seagle et al. 4 reported residual nitrogen in cobalt after electron-beam melting, although no reasons were ventured for the presence of this interstitial impurity. This investigation was undertaken to clarify these inconsistencies, and to provide additional data on atomic interactions in dilute metallic solution. EXPERIMENTAL PROCEDURE This study was well-suited to the Sieverts' method, which has not changed significantly since its introduction by Sieverts. 5 The apparatus was of the same design as that described by Humbert and Elliott, 6 with a reaction bulb similar to that reported by Weinstein and Elliott. 7 The buret was not water-jacketed, but the measured gas volumes were corrected for small changes in room temperature. The melt temperature was measured by a disappear ing-filament optical pyrometer sighted through a prism onto the melt surface. Temperature calibration was made based on a measurement of the melting point of pure cobalt taken as 1495°C. The difference between the reciprocal of the observed and the true temperatures was assumed to be a constant, neglecting the changes in emissivity with small additions of alloying elements. The total error in gas-volume measurement caused by accuracy limitations in reading the mercury level in the buret, variation in ambient temperature, and variation in melt temperature was about 0.5 cu cm. This represents approximately 10 pct of the total solubility, and is a larger relative error than in previous studies6-' because of the small nitrogen solubilities encountered in the present investigation. The source and purity of the materials used are listed in Table IA. Recrystallized alumina crucibles were used throughout the investigation. Examination of the crucibles after solidification of the melts showed no reaction or penetration. Alloying of the cobalt melt was accomplished with the dropping technique described by Humbert. 6 The investigation was started using cobalt from African Metals Corp. in shot form, but this material was not of sufficient purity and did not yield consistent solubility results. Sherritt Gordon Mines Ltd. cobalt was then used throughout the investigation. In experiments involving alloying elements which could react with oxygen dissolved in the melt, the cobalt was further refined by annealing at 1400°C in a dry-hydrogen atmosphere. This treatment, described by Woolley and Pehlke, 8 markedly reduced the oxygen content. The oxygen and nitrogen analyses of the cobalt used in this study are presented in Table IB. RESULTS Hot Volume. The hot volume was measured prior to each run and was 50 to 55 cu cm (stp) at 1600°C. It increased linearly with increasing pressure and decreasing melt temperature. Pure Cobalt. Measurements of the solubility of nitrogen in pure cobalt and the temperature coefficient of solubility are summarized in Table 11. At 1600°C and 1 atm nitrogen pressure, the solubility was found

Jan 1, 1967

By J. H. Rushton, L. H. Mahony

Principles of fluid motion and turbulence which have been found to be of use in mixing and agitation problems are discussed, as well as suggested applications in extractive-metallurgy processes. Various types of impellers are described, together with other conditions that affect flow pattern and turbulence. The choice of equipment for particular requirements is considered, and equations for power input are given. Modern heavy-duty mixing and agitation equipment can take an increasingly important part in such extractive-metallurgy processes as solids handling, crystallizing and leaching, chemical operations, and flotation. Application of mixing and fluid-mechanics principles to extraction methods can lead to greater process rates and a resultant saving in time and money. MIXERS are being applied with increasing frequency to problems in the metallurgical industries. The increase represents in part the modernization of mechanical equipment used through the application of unitized drives, modern electric motors and speed reducers, and recently developed materials of construction. Some applications have resulted from process changes and the use of techniques for operations similar to those that have been demonstrated and proven in the chemical industry. Still more applications are being developed through the use of fluid-dynamics principles not previously recognized as applicable to these operations. It is the purpose of this paper to describe those principles of fluid motion and turbulence which have been found to be of use in mixing and agitation problems, and to suggest applications for them in the extractive-metallurgy processes. Modern mixing equipment has been designed to provide the fluid motion consistent with that best suited to different operations.' When properly applied, these more efficient fluid-handling mixers result in lower process-production costs. Metallurgical operations usually involve large amounts of solids. The characteristics of the ore control the process and only enough liquid is added to provide sufficient fluidity for handling and processing. The reactive part of the ore, the mineral value to be extracted, is likely to be low in percentage, and the quantity of reagent required is similarly low, but excessive dilution makes additional reagent necessary and therefore is undesirable. Thus, the primary problems in minerals processing are to handle as high a concentration of solids as possible and to distribute reagents uniformly. These pulps, or slurries, are in a range of solids concentration where hindered settling rates apply, and care must be taken to agitate and mix sufficiently to maintain suspension and flow throughout the equipment. Such slurries have high densities which are the weighted average of the components and viscosities that are spoken of as "effective viscosities" but are difficult to evaluate. It is convenient to separate metallurgical operations involving mixers and agitators into three categories: solids handling, mechanical or physical operations, and chemical operations. In each of these categories fluid motion is required to maintain suspension, to distribute surface-active agents, to blend components and reactants, and to induce high rates of chemical reaction. After a discussion of some basic principles of mixing and agitation, examples of application to the three categories will follow. Fluid Motion The fundamental problems of mixing and agitation of liquids have to do with the mechanics of fluid streams and the means by which they are

Jan 1, 1955

By L. D. Jaffe, J. H. Hollomon

THE effect of tempering temperature and time upon the properties of quenched steel is clearly a subject of great practical importance, as well as of considerable theoretical interest. It would be very desirable to be able to predict the properties of a quenched steel when given any selected tempering cycle, with a minimum of experimental work upon that heat or even type of steel. Two problems are involved: one consists of relating the structure obtained to the physical properties, and will not be discussed here; the other, with which this paper deals, involves the relations of time, temperature and composition with the structure obtained on tempering. Indentation hardness is perhaps the most convenient quantitative measure of the tempered structure, or of what might be called the "degree of tempering." Undoubtedly, it is not an exact measure, and in some cases (as when temper-brittleness occurs) pieces of the same quenched and tempered steel may have widely differing properties at the same hardness. However, hardness has the advantage of being simple to determine and is certainly the most widely used indication of the degree of tempering. Moreover, for fully quenched steels that are not temper-brittle and do not contain retained austenite when quenched, it appears that, in general, if the hardness of the steel is the same, the tensile and impact properties will also be identical, whether a high or a low tempering temperature is used. The tempering charts available in the metallurgical literature usually give the hardness as a function of tempering temperature for only one tempering time. However, in practice, tempering times frequently vary, and a method of converting tempering curves for one time to tempering curves for some other time would be very valuable. It is also advantageous, in determining the tempering treatment necessary for a given part, not to have to temper samples at several temperatures for the time used for the commercial tempering operation. A more satisfactory procedure would be to employ times of the order of 10 to 30 min., rather than 5 or 10 hr., and if possible to use only one temperature. Furthermore, it is frequently desirable, for reasons such as temper-brittleness,* to obtain a given hardness with short times at relatively high temperatures, and it would be convenient to be able to compute without tests the time required to produce this hardness. Remarkably few quantitative studies of the hardness of quenched steel tempered over wide ranges of temperature and time

Jan 1, 1945

By Reynold Q. Shotts

The small domestic underfeed stoker as now designed is unusually sensitive to the coking and plastic properties of coals, and when the attempt is made to burn the high rank coking and caking coals of the Appalachian fields, serious trouble may occur. Part of the trouble may be caused by the ash content and clinkering characteristics of the particular coal in use, but more often it is the result of an excessive ac-in of coke in the form of ''trees,, or masses in the fuel bed. Often the zone of burning becomes so restricted that the fire goes out, and in extreme cases the fire may be lifted completely out of the fuel bed and away from the air ports. Even if the fire is preserved, excessive coking may cause response to subsequent heat demand to be slow and irregular. Coke trees seem to grow most readily during periods of hold-fire operation, so that in order to preserve the fire in mild weather it is often necessary to set the timer for such a long operating period each hour that much unneeded and unwanted heat is developed, causing discomfort. During demand periods the fire may pick up so slowly that the intense burning which develops just before stoker cut-off causes a serious overshooting of the thermostat. Stoker coal performance tests which have been made in a number of labora- tories1,2,3,4,5 are one method of approach to the problem Of selecting stoker coals- As yet these tests have not been standardized and they are expensive and time-consuming. The value of the results probably increases with the length of the test. Sherman and co-workers at Battelle Memorial Institute believe that even a one-week test is not too reliable a trial2 and it is quite likely that Others will agree. A great advantage of such tests is that characteristics of coals, other than the tendency to form coke masses, may be evaluated from them. The selection of stoker coals would be greatly facilitated if there existed some simp1e measure Of the tendency Of a a to form coke in a fuel bed. Although possessing all Of the disadvantages Of any small-scale laboratory test, the test for the free-swelling index of coal has been found useful for evaluating the probable effects Of swelling properties upon combustion.7 Ostborg, Limbacherand Sherman, have shown that the test can Predict, roughly, the tendency Of coke to accumulate in the fuel bed Of a domestic stoker. They also gave instances of its value in predicting combustion behavior in some large installations. The use of the test for free-swelling index has become well established and has been adopted as a standard by the American Society for Testing Materials.8 When domestic stoker coal investigations began at the State Mine Experiment Station in the summer of 1944, it was decided

Jan 1, 1949

By Luther W. Lennox

The purpose of this article is not to compare one type of grinding machinery with another and to conclude from a series of tests that one particular machine is superior to all others. Neither is the reader asked to tire himself with the details of many tests to prove the statements herein made. The Chilean mill stands today almost an outcast from the milling world. It ranks with the applicant for a job who has been given a trial along with others and condemned because he was not able to perform the definite task assigned as well as the others, and was forever eliminated. The judges did not tarry long enough to try this aspirant in a field of a slightly different nature. Even though it has been condemned, the writer contends that the published records will indicate that the trials were never shifted into the field of greatest efficiency for the . Chilean mill. Those of us who cling to this outcast as a fine grinder in our milling operations do not wish, naturally, to be condemned also, with the machine, and yet we feel that we are classed as behind the times, at least in this phase of our milling judgment. Hence there is considerable personal feeling in our efforts. During the last few years there have been published several papers on the relative merits of the various grinding machines. In two of these articles a comparison was made between Chilean mills and cylindrical grinders. In each case the Chilean mill came out second best from about all standpoints. The outstanding feature in these comparisons would seem to be the decided attempt to keep all conditions the same, so that each machine could be judged on its merit. As Mr. David Cole states,1 "We are inclined to regard a direct comparison of grinders arranged side by side, and making a product that affords as nearly as possible the same screen measure, as the Supreme Court in these grinding matters." The writer agrees that this is the very best method for true comparison between machines. The results in the two detailed tests should give the relative merits of the two grinders in doing the work assigned. And they probably do. The conclusion drawn in each case was adverse to the Chilean mill as a fine-grinding machine. However, the duty placed upon the machines was that of converting material that had already been

Jan 1, 1920

By C. E. Schwab

A lead-zinc orebody, in fairly strong quartzite and with a dip of 35" to 60°, is block-caved by use of scrams in a stair-step pattern up the ore footwall. Scram linings to handle coarse muck and permit the use of folding scrapers are developed by the use of end-grain wooden blocks to reduce maintenance and keep operating cost to a minimum. THE Bunker Hill mine, since its discovery in 1885, has steadily produced a high grade of lead-silver-zinc ore. By the end of 1952 over 21,000,000 tons of this high-grade ore had been produced by square-set mining, and reserves in the mine continue to be very satisfactory both as to quantity and grade. For many years prior to 1941, mine production and mill capacity had been 1200 tons of feed per day. Closely adjacent to the mill, and stored behind dikes, coarse jig tailings had been impounded during the time preceding the advent of fine grinding and selective flotation. When manpower became short in 1941 and sink-and-float preconcentration was proved successful, mill capacity was increased to 1800 tons per day to treat these jig tailings economically. By 1946, because the supply of jig tailings was limited, underground exploration was started to discover and prove ore reserves of low-grade material which could be mined by an appropriate bulk mining method. During the years of square-set mining many possible areas of low-grade mineralization had been observed. One chosen for the first exploration work was sufficiently remote from active mining areas so that subsidence, if an ore-body were proved, would cause no problem. Also, old adits and workings were still open and in good enough condition so that exploration in the mineralized zone could be started with a minimum of preparatory work. In 1948 an orebody was proved of sufficient tonnage, of a grade about 2 pct Zn, 0.5 oz Ag, and 1.0 pct Pb. It was decided to use block-caving, the only appropriate mining method by which this grade of ore could be economically recovered. Exploration for additional reserves in other areas of the mine is continuing, but ultimate results are not known at this time. With more sink-and-float capacity, larger ball mills, and more flotation machines, mill capacity was increased to 3000 tons per day, permitting the mining of ore in the square-set area at a maximum rate not usually achieved, because of the scarcity of labor. Increased mill capacity also permits block caving and the mining of jig tailings at variable rates to keep mill feed up to 3000 tons per day. Fortunately the three types of feed are amenable to the same mill circuit and reagents for recovery of Pb and Zn. For example, during the first 10 months of 1952 square sets produced 827 tons per day, block-caving 1421 tons per day, and jig tailings 643 tons per day, an average daily production of 2891 tons for all three products. Exploration had proved the existence of an ore-body 1000 ft long and 165 ft wide in horizontal section, see Fig. 1. Company engineers were concerned only with the vertical extension, about 300 ft, from an old level to the surface. Much of this almost outcropped, Fig. 2. The ore lies in the hanging wall of a major fault of the Bunker Hill mine, standing at 65" in one end of the zone and separated from the fault by a wedge of waste, see Fig. 3. This wedge pinches out near the center of the zone, at which point the ore dips 45", lying nearly on the fault, Fig. 4. The remaining portion lies on the fault and conforms to the fault dip of 35", Fig. 5. Open-pit mining for the top of the ore was considered, but since the ore zone dipped into and under the mountains, adverse waste-to-ore ratios precluded use of this method. The ore occurs in massive quartzite of sufficient strength to support untimbered drifts, crosscuts, and raises. Zones of weakness in the quartzite are bedding, jointing, and small faults or slips. The mineralization, which occurs as small stringers of sphalerite and galena as well as pyrite, creates another line of weakness. The mineral veins or veinlets in themselves are high-grade. Their size and regularity and the amount of barren quartzite by which they are separated determined the limits of mineable ore, which are all assay limits except for the one determined by the major fault. Block 1 Without any background of caving in this type of quartzite, engineers selected the first block on the very steep end of the zone. Compelling reasons prompted this decision. The steep portion of the ore in Block 1 was of the lowest grade, so that if difficulties were encountered no very valuable ore would be lost, while the experience gained might be applied in mining the remaining blocks. A block 200x200 ft was laid out, with four scrams spaced 50 ft apart for drawing and placed at a right angle to the strike. Finger raises were placed in a 25-ft interval grid pattern, with flat undercutting done by crosscuts at the undercut level 25 ft above

Jan 1, 1954

By R. F. Dickerson, D. A. Vaughan, A. F. Gerds

ALTHOUGH the metallurgy of uranium has been under intensive study since the early 1940's, no systematic effort has been made to identify the non-metallic inclusions in uranium. Uranium carbide (UC), which is probably the most common inclusion found in graphite-melted metal, has been tentatively identified by previous investigators, but the other nonmetallic inclusions have received little attention. Since metallography is a valuable tool in metallurgical studies, the metallographic identification of the nonmetallic inclusions in uranium is important. Such an investigation has been completed and the identification of slag-type inclusions and of uranium monocarbide, uranium hydride, uranium dioxide, uranium monoxide, and uranium mononitride is described. Metallographic Preporation It is often possible to prepare specimens for metal-lographic examination equally well by several methods. The specimens which were examined in this work were prepared by one of two acceptable methods. For the convenience of the reader, both methods will be discussed in detail and will be referred to simply as Method I or Method II in the subsequent sections. For both Methods I and 11, specimens for microscopic examination usually were mounted either in bakelite or in Paraplex room temperature mounting plastic. Method I—Specimens were ground in a spray of water on a revolving disk covered successively with 120-, 240-, and 600-grit silicon carbide papers. It was necessary to perform the final grinding operation carefully on worn 600-grit paper to keep the scratches as fine as possible. After washing and drying, the specimens were polished for 3 to 4 min on a slow speed wheel (250 rpm) covered with a medium nap cloth. Diamet Hyprez Blue diamond polishing paste, Grade 00, 0 to 2 µ, was used as abrasive with kerosene as lubricant on the wheel. Specimens were washed thoroughly in alcohol and final polished electrolytically in an electrolyte composed of 1 part stock solution (118 g CrO, dissolved in 100 cm3 H2O) with 4 parts of glacial acetic acid. A stainless steel cathode was used. At an open circuit potential of 40 v dc, a polishing time of 2 sec retained inclusions well with the bath at room temperature. If additional etching was required to sharpen the interface between the metal and the inclusions, an electrolyte composed of 1 part stock solution (100 g CrO3 and 100 cm8 H20) and 18 parts glacial acetic acid was used at room temperature. Best results were obtained by etching for from 10 to 15 sec at 20 v dc in the open circuit. Surfaces obtained by this method are suitable for microscopic examination. However, if desired, they may be etched further with other chemicals. Method 11—Rough grinding was done on a wet 180- or 240-grit continuous grinding belt. The specimen was then ground by hand successively on 240-, 400-, and 600-grit silicon carbide papers in a stream of water. Final polishing was accomplished on a 4 in. high speed wheel (3400 rpm) covered with Forstmann's cloth. Linde B levigated alumina, suspended in a 1 volume pet chromic acid solution, was the abrasive. Specimens usually were polished in 5 min or less by this technique. Often the inclusions present in the metal were identified in the mechanically polished condition. When etching was required to outline inclusions more sharply, one of the two following methods was used. In the first method, the specimen is etched lightly while electropolishing in the chromic-acetic acid solution described above (1 part of stock solution to 4 parts of acetic acid). The electrolyte was refrigerated in a dry ice-ethyl alcohol bath and specimens were etched at 60 v dc on the open circuit for 2 or 3 cycles of 3 to 4 sec each. The second technique utilizes electrolytical etching at about 10 v dc (open circuit) in a 10 pet citric acid solution at room temperature. X-Ray Diffraction Technique The major problem in the identification of inclusions in metals by X-ray diffraction techniques is the extraction of a sufficient amount of each type of inclusion to obtain an X-ray diffraction pattern. In the present study, X-ray diffraction patterns were obtained from individual inclusions of the order of 10 µ diam. The polished and etched samples shown in the micrographs were examined at a magnification of X54 or XI00 with a binocular microscope. This allowed sufficient working distance to extract the inclusions with a needle probe for powder X-ray diffraction analysis. Friable inclusions such as MgF2, CaF2, UO2, and UH3 could be freed from the metal by probing the as-polished and etched surface. The fine particles then were picked up on the end of a Vistanex-coated glass rod (0.002 in. diam) which was held in a brass adapter made to fit the powder X-ray diffraction camera. The end of the glass rod was centered in the path of the X-ray beam. In the case of the UC, UO, and UN inclusions which are smaller in size, more metallic in appearance, and less friable than the other inclusions, it was necessary to etch the inclusion in relief before extraction. UN inclusions etched sufficiently in relief in the electrolytic polishing solution described in Methods I and II by increasing the polishing time. UN inclusions were relief etched by extending the

Jan 1, 1957

By L. T. Larson, M. L. Picklesimer

The relationship between the apparent angle of rotation of monochromatic plane polarized light and the tilt of the basal pole from the surface normal has been experimentally determined for zirconium over the wavelength range of 500 to 655 mp. This relationship allows the determination of the spatial orientation of the basal pole of an individual grain in a polycvystal-ling zivrconium specimen to within ±3 deg by three simple tneasurements with a polarized-light metallurgical microscope. The method of measurement is discussed in detail. THE optical anisotropy of materials having noncubic crystal structures has long been used to reveal features by polarized-light microscopy. Petrographers have used measurements of certain optical properties to identify and classify transparent or translucent minerals. More recent work (i.e., Cameron1) has extended such measurements to opaque minerals in reflected light. Few attempts have been made to make similar measurements on noncubic metals. Couling and pearsall2 have reported that a sensitive tint plate can be used in a polarized-light metallurgical microscope to determine the position of the basal-plane trace in a grain of polycrystalline magnesium. Reed-Hill3 has reported that the same technique can be used for zirconium. We have found that the precision of measurement can be increased to about ±0.5 deg by using a Nakamura plate4,5 to determine the exact extinction position after the sensitive tint plate has been used to locate approximately the basal-plane trace. This report describes a method for measurement of another optical property, the apparent angle of rotation. This measurement permits determination of the angle between the basal pole of a grain of a hcp metal and the normal to the surface of the specimen. When the two measurements are combined, the orientation of the basal pole in space can be determined from three simple measurements on a single surface. One to two hundred such determinations will permit plotting of a basal-pole figure for the polycrystalline material with reasonable accuracy. When normally incident, monochromatic, plane-polarized light is reflected from the surface of an optically anisotropic material, the light may be converted to elliptically polarized light, the plane of vibration may be rotated, or both may occur. The el- lipticity, the angle of rotation, and the reflectivity can be related to the indices of refraction and the absorption coefficients of the material.6,7 Ellipticity values can be determined with an elliptical compensator, but not with the ease and precision desirable for the present purposes. Measurement of the angle of rotation requires only the determination of the angle from the crossed position (90 deg to the polarizer) that the analyzer must be rotated to obtain extinction when the trace of the optical axis in the surface is at 45 deg to the vibration direction of the polarizer. The angle of rotation of the analyzer is approximately 6/5 that of the true angle of rotation of the light as reflected from the specimen because there is a small amount of additional rotation produced during the passage of the reflected light through the mirror of the microscope. Since we are presently interested only in determining the tilt of the basal pole, the angle of rotation of the analyzer (the apparent angle of rotation of the light, i.e., uncorrected) can be used. Precision of the measurement can be increased substantially by the use of a Nakamura plate4,5 in determining the extinction position. In an optically uniaxial material (hcp or tetragonal crystal structure) the angle of rotation depends only on the optical properties of the material and the orientation of the optical axis of the grain relative to the plane of incidence of the plane-polarized light.7,8 Thus, in a metal such as zirconium, the apparent angle of rotation at the 45-deg position in any given wavelength of light is a direct measure of the tilt of the basal pole from the normal to the surface. If the optical properties vary with wavelength, the apparent angle of rotation for any given tilt of the basal pole will vary. None of the required information exists in the literature for zirconium nor for any other non-cubic metal. MEASUREMENTS ON SINGLE-CRYSTAL ZIRCONIUM A single-crystal sphere of zirconium 9/16 in. in diam was spark-cut from a single-crystal rod grown from iodide bar by an electron-beam zone-melting process.9 The damaged surface was removed by chemical polishing in a 45/45/10 mixture (by vol) of water, concentrated HNO3, and HF (48 pct) and then electropolishing at 50 v in a bath1' of methyl alcohol and perchloric acid (95/5 by vol) at -70-C. The single-crystal sphere was mounted in a five-axis goniometer stage having a removable eucentric X-ray diffraction goniometer head for the two inner orientation axes. The basal pole of the single-crysta sphere was aligned parallel to a third axis of the goniometer stage by using the sensitive tint method to determine the basal-plane trace at several rotational positions of the sphere. The alignment was then checked by removing the sphere and eucentric gonio-

Jan 1, 1967