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By Everett G. Trostel

AMERICAN industry in 1943 emerged from the construction phase into the production phase, and American military operations passed from preparation into full action in the many theaters of the global war. The increased pace of industrial and military operations has resulted in a tremendous demand for petroleum and its products.

Jan 1, 1944

By Persifor Frazer

The mines which I am about to describe are all situated in the northern part of the States of Nuevo Leon and Coahuila, Mexico, between the twenty-sixth and twenty-seventh degrees of latitude. They might be grouped, orographically, into four classes: 1. Those in the Sierra de la Ygnana chain; 2. Those in the Sierra de Gomez chain; 3. Those in the Cerro Mercado; 4. Those in the Sierra de San Marcos chain. (See large map.) The first two of these may be further arranged in one geographical district, to which the name, "the Villaldatna. district," may be applied, and the last may be ascribed to the geographical district of " Monclova." Geologically described, the country rock, in which four of the six mines occnr, is a limestone, concerning which a few words will be said further on, to wit.: The Arroyo (gulch), the Montanos and the Pinitos (pines), in the Villaldama district, and La Paloma (the dove), or Iron Mine, in the Monclova district. The San Rafael appears to lie in granite, or a heavy-bedded gneiss, presenting most of the characteristics of the latter, though the contact plane of the limestone is not far off. It is certainly worthy of attention that the ore occurs in that portion of the crystalline rock, which is nearest to the limestone, and it has been thought by some observers to be a true contact vein. It is well known that veins of this character are very often distinguished for constancy and richness. Although the undersigned cannot entirely free himself from the impression that this proximity of different formations has had an important influence in the origin of the part of the vein on which this mine is situated; still he was unable to establish it actually at the contact of the limestone and granite, but rather a short distance within the latter. Two openings of the Riojas vein were respectively in limestone and in rotten whitish granite, but this fact, if established (as by the correspondence of the strike line of the vein in direction with that of a line joining the

Jan 1, 1884

By W. W. Wirth

RESEARCH looking toward the reduction of the cost of roof support by substitution of longer-life materials for wooden timber is fully justified by the fact that roof support is an important element of all production costs. Permanent or semipermanent roof support will reduce the expense of timber-maintenance crews during steady operations, but even more markedly during idle periods. The management, therefore, is faced with the important problem of timber renewals, which in times of regular operation are frequently obscured by more urgent problems of production. Increased use of timber in the Anthracite Region of Pennsylvania is caused mainly by increased percentage of coal obtained from robbing areas, which requires more timber for safety than develop-ment work, and maintenance of long haulageways through crushed ground despite the fact that less coal is transported over them. The timber reserve in the immediate vicinity of the mines has been depleted to such an extent that it is necessary to secure 70 per cent of the timber requirements from distant sources. Originally, mine timbering in this region was done by largely utilizing round props or legs with round collars. The whole cross section of the tree from which timber was cut was utilized by forming the joints between the legs and the collars with saw and adze, using plank or round saplings for lagging behind the legs and over the collars to prevent material falling between them. The Mine Inspectors' report of 1898 records an important digression from the use of round timber, when two tunnels at the Babylon colliery, near Pittston, Pa., were timbered with 12 by 12-in. square timber sets with mud sills, through quicksand for distances of 425 and 160 ft., respectively. The timbers were lagged with 3-in. plank to control sand.

Jan 1, 1940

By George A. Komadina

From its modest beginning in 1957 with one mill grinding section handling 3000 tpd Pima has steadily expanded. In July 1966, work was completed that allowed the concentrator to treat in excess of 18,000 tpd. Almost immediately Pima embarked on another expansion program that will increase plant capacity to 30,000 tpd during the summer of 1967. This repeated expansion has corresponded with the development of additional low-grade ore deposits and with the improved operating economics realized by handling larger masses of material. Early in the life of Pima it was known that a mineralized area was present on the flanks of the high-grade orebody which systematic drilling had shown to be a low-grade copper orebody. Many months of engineering studies revealed that this was sufficient to allow Pima to compete with other large scale, low-grade copper operations in the Southwest.

Jan 11, 1967

By Reginald E. Hore

Since the discovery of silver at Cobalt, Ontario, in August, 1903, more than 100,000,000 oz. of silver have been produced by the mines in the Nipissing district, and there is reason to believe that at least as much more will be produced in the nex five years. The estimated value of the aggregate output o ore to the end of 1910 is $48,327,280. The ore yielded 93,977,833, oz. of silver and was mined at a net profit of abou $16,000,000. For 1910 the production was 30,558,825 oz., valued at $15,436,894, and yielding a profit of about $9,000.000. The details of the production of the Cobalt district for the years 1904 to 1909, inclusive, as reported by the Ontario Bureau of Mines, are given in Table I. The shipments from Cobalt are in the form of smelting-ore, concentrates from milling-ore, and bullion. The smelting-ore is largely high grade, averaging about 3,000 oz. per ton A smaller return is from what is called low-grade ore and which

Jan 1, 1912

G. M. TAYLOR,* Colorado Springs, Co1o.-I do not think the plan outlined in this paper would work at Cripple Creek. Most of our men have had a pretty good education. The Cripple Creek district is a lessee district-I do not think there is one mine operating in Cripple Creek to-day that does not have the leasing system. We have as many men leasing on our property as we have mining and every plan who is working for wages is looking for n lease-everyman has mined for him- self, he has been his on7n boss on n lease, either on our own property or

Jan 1, 1919

By T. Lane Carter

It is a curious fact that while in our Transactions there are papers dealing with mining-districts in all parts of the world, in Europe, Asia, Africa, and Australia, there is not one which describes the mining possibilities of Nicaragua, our near neighbor. To be most interested in distant objects, like the moon, and to neglect what lies at our feet, appears to be a trait of human nature. The neglect of Nicaragua is not confined to the American Institute of Mining Engineers. In no other transactions am I able to find papers dealing with mining in Nicaragua, some parts of which are as much in need of discovery and research as the North Pole. I hope this paper will be the precursor of many others to be printed in our Transaclions, dealing not only with the miniilg possibilities of Nicaragua, but with the whole of Central America, where there are vast areas a,waiting skill and capital for their development. Much of this capital and skill should come from the United States in the future, although it is probable that European capitalists, when they appreciate fully the possibilities, will investigate more and more the mining-resources of Nicaragua and ot'her Central American republics. Fig. 1 is a sketch-map of Nicaragua showing the principal mining-districts. 11. History. Mining in Nicaragua did not begin yesterday. It was commenced by civilized man when the Spanish conquerors pene-' trated into the interior and forced the natives to procure the precious metal for them. It is strange that the Spaniards did not find more gold, and work on a scale as extensive as in Colombia and other parts of South America. Probably in Nicaragua the Indians covered up most of the rich prospects

Jan 1, 1911

By John S. Johnson, Thomas Fraser

SIZING is the process of separating mixed particles into groups of particles all of the same size, or into groups in which all particles L range between certain definite maximum and minimum sizes. In coal preparation, sizing is generally accomplished by passing the coal over screens. Separation by differential settling in air or water currents has been adapted to the special field of separating very fine sizes, and these processes are in commercial use to a relatively small extent in the coal industry. Separation with screens is a very old industrial practice. Agricola 1 described the use of screens for ore treatment in the middle ages. In the literature of the British coal industry references were made to the screening of coal as early as 1589, but the practice of extensive sizing for the market did not become general until the last half of the nineteenth century. In America, the practice of sizing developed first in the Pennsylvania anthracite region, beginning with the use of rakes2 in the mine working places to recover coarse coal. This mining procedure left the fines in the mine. Preparation outside the mine started with the installation of stationary cast-iron plates with 4 to 6-in. square holes. The run-of-mine coal was dumped upon the platforms, the large pieces of rock were picked out by hand, and the large lumps of coal were broken with hammers. The term "breaker," which still applies to the anthracite-preparation plant, originated with this practice, but the term is no longer descriptive of the entire function of the plant. In 1884, the first power-operated anthracite coal breaker3 was erected by Gideon Bart at his colliery at Wolf Creek near Minersville, Pa. This plant utilized a system of rolls for breaking the coal and revolving screens for sizing. The plant was driven by a steam engine. It could handle

Jan 1, 1943

By E. W. Dewing

The nature of solid solutions of sodium in non-paphitic carbon at temperatures near 1000°C has been investigated by an electrolytic technique. The activity coefficient is found to vary strongly with the heat-treatment temperature of the carbon, and an analysis of the energy terms involved suggests that this is due to variations in the Fermi level. The diffusion coefficient for sodium is in the range implying that the sodium atoms (or ions) are not bound to specific sites on the carbon, in agreement with lack of evidence for specific compounds in the activity -composition curves. In the light of These results phenomena occurring in aluminum reduction cell linings are dis-cussed. It is concluded that sodium migrates by diffusion through the carbon lallice and not the pores, and that A14C9 is formed within the lining hy The excess of NaF invariably found in used linings is formed by this reaction and by air oxidation: There has recently been much interest in the swelling of carbon which occurs when it is made cathodic in an aluminum electrolysis cell, and there is general agreement that the phenomenon is due to the penetration of sodium atoms, derived from the reaction on the carbon lattice. (NaF and AlF3 are constituents of the fused-salt electrolyte.) The low-temperature lamellar compounds of potassium with graphite are well-known, and one compound between sodium and graphite has been reported.4 There is, however, virtually no information on the basic chemistry of the interaction of sodium with nongraphitic carbon at high temperatures, although Dell3 has made some fundamental studies of rates of penetration. At the time the present work was carried out these were not available. Rapoport and samoilenkol had measured rates of physical expansion in a dilatometer, using the fractional increase in length of a carbon specimen after electrolysis in a cryolite bath for 2 hr as an index of susceptibility to cathodic swelling. Work here with a similar apparatus showed that expansion (of a 1.5-in.-diam cylindrical specimen) ceased in less than 20 hr, and that the final expansion was much more reproducible than the value at some intermediate time. This suggested that an equilibrium was being set up, and that a thermodynamic approach was required. The results obtained are not as accurate as had been hoped, but they are the only ones of their type available and have enabled useful conclusions to be drawn. The experimental work was divided into two parts: an investigation of the activity-concentration diagram for sodium in carbon, and a rough determination of the diffusion rate. For the former, most of the experiments were made with petroleum coke even though this is not a form of carbon used in cell linings. It has the advantages, however, that it is a homogeneous material, that it is low in ash, and that its structure is reasonably well understood. Anthracites and coal cokes gave results of the same type as obtained with petroleum coke, but the reprodu-cibility from specimen to specimen was extremely poor. EXPERIMENTAL 1) The Activity-Composition Diagram for Sodium in Carbon. The petroleum coke was ground, pressed at 40,000 psi into plates 19 by 9 by 2 mm without added binder, and heat-treated. The sodium activities were established by an electrolytic technique. The carbon was made anodic in a cryolite bath with an aluminum cathode, and a controlled potential, E, applied so that the sodium activity at the anode was given by ln Na = 1n asa - EF/RT [21 where as, is the sodium activity generated by Reaction [I]. The relative activity is sufficient for many purposes and is simply given by The value of Na not at present known, but when the thermodynamics of the Na-A1 system have been worked out it can be derived from the equilibrium

Jan 1, 1963

By F. Keller, J. D. Edwards

THE anodic treatment of aluminum presents problems of scientific as well as of commercial interest.1-3 Of particular interest is the fact that, during the anodic oxidation process, the oxide continues to form at the metal-oxide interface under any oxide previously formed. This has led to speculation as to the mechanism involved in the formation of the relatively thick oxide coatings that are used commercially for decorative or protective purposes. Furthermore, the ability of certain types of oxide coatings to adsorb dyes and other substances has stimulated research to determine the actual structure of these adsorptive coatings. It has been found that anodic oxide coatings on aluminum are composed essentially of aluminum oxide. They are formed by the action of oxygen ions penetrating to the metal surface during the electrolytic oxidation treatment. These coatings can be formed in a number of different electrolytes, as for example, those which contain sulphuric acid, chromic acid, oxalic acid, or boric acid. These are the commonest and most useful electrolytes employed commercially. Except for certain specific conditions of formation, the coatings in general have been found to be amorphous alumina, as far as can be determined by X-ray or electron-diffraction methods. Anodic oxidation processes can be arranged in three rather general classes if they are grouped in relation to the solvent action of the electrolyte on the coating.4 In the first class, the electrolyte has little or no solvent action on the coating that is formed. In general, coatings produced under such circumstances are nonporous and non- adsorptive. In the second class, the electrolyte exerts an appreciable solvent action on the coating. These coatings are porous and adsorptive. Finally, for the third class, the electrolyte tends to dissolve the coating about as rapidly as it is formed. This action produces electrolytic brightening or anodic polishing of the aluminum surface and at most leaves only a very thin film of oxide. The nonporous and nonadsorptive type of oxide film is represented by the coatings that are formed when solutions of boric acid are employed as the electrolyte. It is especially significant that these impervious films are formed in electrolytes that exert little or no solvent action on the coating. Where a boric acid electrolyte is used, the coating tends to form rapidly, with the result that the flow of current is soon reduced to substantially zero. This indicates that the growth of the coating has stopped. As a rule, the thickness of the coating is roughly proportional to the voltage employed for formation and the coatings of this type are exceedingly thin. In an electrolyte of this type, the coating has a high resistance when the aluminum is made anode; consequently, any current that may flow (leakage current) is very

Jan 1, 1944

By Augustus Locke

I WISH to urge on this Committee the task of evaluating mining geology. -My motive is as follows: It, is a. duty of the Institute from time to5 time, to establish the social perspective of the professions grouped within it, not simply to promote their use, but to determine with engineering definiteness their true powers and functions. This becomes the delegated duty, therefore, of this committee in respect to geology. Be- cause my own subject is mining, I shall confine my remarks to mining geology. But I believe that the evaluation should be made to include all of that geology termed economic. The perspective for such evaluation is shown in the nature of the public support given to geology. The federal Geological Survey, the leading organization on the economic side, is actuated by the zeal of a small group of devoted professionals who consider its work valuable, ' It proceeds, however, on a starvation ration of appropriations, and that implies that neither the corporations, the voters nor the vote getters consider it important. Altogether, in' the public consciousness, geology is negligible. That, at the same moment, .the profession should act with full confidence, while everyone else should act' with opposite motives, is not fitting. For us, as a committee, to remain incurious regarding such a disparity of beliefs is quite impossible.

Jan 1, 1931

By Alexander Field

The hot-rolling properties of a series of high-sulfur steels are described. From a consideration of the sulfur, manganese, and zirconium contents of these steels, it is shown that zirconium reacts with the sulfur content of molten steel in accordance with the equation Zr + 2S = ZrS2. Zirconium disulfide appears in the finished state as gray-colored inclusions, similar to manganese sulfide in plastic behavior and general appearance. Zirconium completes its act of deoxidation before proceeding to combine with sulfur and indirectly increases the effective sulfur-combining power of any manganese which may be present. IN A previous paper,1 the experimental methods used and some of the results obtained in an extensive investigation of steels containing zirconium were described. The present paper considers in greater detail one of the most interesting of these effects, namely, the elimination of "red shortness" and the occurrence in steel of a compound of zirconium and sulfur. A consideration of the actual percentages of zirconium, manganese, and sulfur in numerous steels in the light of behavior during rolling has led to new conclusions of the most practical import regarding the reciprocal relationships of these elements. The microscopic examination of high-sulfur steels containing zirconium has also been productive of interesting results. Before discussing the experimental data in question, it may be stated, briefly, that the reaction between zirconium and sulfur in molten steel may he represented by the simple equation, Zr + 2S = ZrS2, and that the zirconium sulfide thus formed occurs in the finished steel in the form of gray-colored inclusions, closely resembling manganese sulfide and, like the latter, exhibiting plasticity at rolling temperatures. Molten steel containing zirconium retains such a negligibly small amount of oxygen in solution that the foregoing reaction goes to completion.

Jan 2, 1924

By T. D. McKinley

Theory, operational characteristics, and indicated precision and accuracy of analytical methods based on vacuum extraction, equilibrium pressure, and combustion approaches are reviewed. At the present time vacuum extraction at 1400°C and the equilibrium pressure method are recommended for determination of hydrogen in titanium and titanium-rich alloys. UNTIL a few years ago the role of hydrogen in titanium was an unknown factor with regard to its effect on the physical and mechanical properties of the metal. However, following the work of Jaffee and othersa-" it is now generally acknowledged that hydrogen has a degrading effect on titanium and its alloys. The chief manifestations are a decrease in impact strength in -systems and delayed cracking in a-ß systems. Since hydrogen does have a de- grading effect on titanium it is essential to control it within tolerable limits. It then follows that procedures for quantitative estimation of hydrogen are a primary requirement for the industry. For greatest benefit these methods should be simple, rapid, and precise. In addition to having these virtues, methods must be easy to duplicate in both equipment and technique to gain widespread use. After inherent accuracy has been established, the, required precision to make a method acceptable is dependent largely on the nature of the work at hand. Ability to obtain a representative sample has a pro-

Jan 1, 1959

By R. L. Templin

THE increasing use of aluminum and its alloys in commercial fields has demanded a better understanding of their machining properties. This fact is exemplified by problems that have arisen in the automotive and airplane industries, but many in other fields might be cited. As pure aluminum and its alloys in their various commercial conditions show appreciable differences in their machining properties, it is not surprising that quite divergent solutions have been offered for the machining problems encountered. However, if the fundamental requirements of the most suitable cutting tools for these metals are understood, these machining problems lend themselves more readily to satisfactory solutions. Since the machining of free cutting brass and mild steel is understood by most persons accustomed to working these metals, it may serve our purpose better to first make a general comparison of the tools more commonly used in machining these metals with the tools most suitable for machining aluminum, then proceed to a more specific discussion of the individual stools.

Jan 1, 1927

By G. F. Comstock

In the literature of metallography there is a large amount of material describing the various non-metallic inclusions found in iron and steel, and the appearance of sulfides, silicates, oxides, or alumina in steel under the microscope is fairly well known. The inclusions found in non-ferrous metals are, however, not so well known, at least judging from published writings, and the author has been interested in examining small castings of copper, brass, or bronze with certain inclusions purposely mixed with the metal, to see what was the characteristic appearance of each kind of inclusion, and if they could be readily distinguished from one another. The method employed in most cases consisted in overheating and oxidizing a small charge of copper, then cooling it somewhat, and adding a suitable amount of the element whose oxide it was desired to observe. This element was stirred in well and given time to react with the oxygen in the copper, then the melt was poured in a sand mold in the form of a cylinder about 21/2 in. (63 mm.) in each dimension, with a sprue about 11/2 in. (38 mm.) in diameter and 3 in. (76 mm.) high on top of the cylinder, the sprue forming the only riser. Samples for examination were cut sometimes from the center of the casting, and sometimes from the sprue or riser. A few of these samples were cast in chill molds. The appearance of sulfides was studied in an alloy containing 10 per cent, each of tin and lead, with which a flux of plaster of Paris was used. The appearance of foundry sand was studied in several alloys, one of them having sand stirred into the metal intentionally, and others having cut into the molds badly when poured, so that the castings were spoiled by included sand. As all this work was done on alloys having copper as the chief ingredient, the natural starting point was copper oxide, the appearance of which in a micro-section is well known. Cuprous oxide is soluble in molten copper, but separates out in freezing and forms a eutectic containing 3.5 per cent. Cu20, or 0.39 per cent. oxygen. If there is less

Jan 1, 1919

By J. Chipman, N. J. Grant, H. L. Bishop

Lime and dicalcium-silicate crucibles were equilibrated with molten iron and liquid slags containing iron oxide and small amounts of sulfur. The oxygen content of metal, iron oxide activities, and desulfurization values of the slags were determined in the temperature range 1530 to 1700°C. The influence of magnesia in the slag and the temperature dependence of the solubility of lime in liquid iron oxide and the ferric oxide content were established. The temperature contour of the liquidus surface of iron-silicate slags saturated with lime and dicalcium silicate was also established at 1600°C. THE importance of the role that slag composition plays in the refining of steel has been known for many years. Numerous studies have been made using actual plant data in order to establish the relationship between the composition of the slag and metal during the refining of a heat of liquid steel. These results rarely represent equilibrium conditions since completion of the various chemical reactions involved in steelmaking is seldom realized. In order to establish quantitatively the equilibrium conditions existing between the slag and metal, several laboratory studies have been conducted in the past 20 years to determine the reactions important in slag control. These investigations have included studies of simple liquid basic and acid slags as well as more complex slag systems which approach those commonly found during the refining of a heat of steel. Since most of the previous studies of simple basic iron-oxide slags equilibriated with molten iron were made in magnesia crucibles, it was not possible to establish the distribution of sulfur and oxygen between molten iron and slags consisting only of the three essential components, lime, silica, and iron oxide. This investigation was undertaken to establish the equilibrium conditions for simple lime-iron oxide and lime-silica-iron oxide slags. Accordingly, it was expedient to prepare crucibles both of lime and dicalcium silicate to establish the equilibrium conditions between molten iron and iron-oxide slags saturated with the refractory materials and free from other components. The only other studies of the equilibrium between molten iron and lime-saturated slags are those of Fischer and vom Ende, 1, 2 in which the solubility of oxygen was determined in an air atmosphere. The

Jan 1, 1959

By Robert Rhea Goodrich

This research was done partly in the non-ferrous laboratory of the Department of Metallurgy of Columbia University, under the direction of Dr. Edward I?. Kern, and completed elsewhere. Acknowledgment is due to Prof. Arthur L. Walker, Dr. Edward F. Kern and Dr. William Campbell of the Department of Metallurgy, for their kind advice and for the inspiration derived from their instruction. This report is given under the following heads: Petrographic Description (Microscopic Study); Sampling and Preparing Ore for Treatment; Chemical Analysis; Treatment of Ore. Petrogeaphic DescRiption Texture: variable. Fine to medium mixed aggregate. Original Structure: Obscurc. Secondary structure: Fractured; healed. Mineralogy (Minerds are grouped for interpretation purposes and are arranged, in each group in approximate order of abundance)

Jan 1, 1916

By R. W. Raymond

THE absence of a convenient glossary of terns connected with mining and metallurgy has long been felt by the general public. It is to meet this want, not to furnish a technical manual for experts, that the following glossary has been prepared. It originated in an attempt on my part to revise for publication the manuscript of a compilation prepared from the appendix of Yale's work on Mining Titles and one or two other sources, to serve as an appendix to a new work on mining law, about to be published by Mr. H. N. Copp, of Washington, D. C. This revision soon assumed, contrary to my original intention, the proportions of a reconstruction ; and with the consent of Mr. Copp, and for the purpose of receiving from my fellow-members valuable aid, I presented my still incomplete work as a paper at the Lake Superior meeting of the Institute, inviting from any quarter suggestions of new terms or better definitions to be incorporated in the glossary before its final publication. This invitation was so widely and generously responded to, that I cannot undertake to make in this place' individual acknowledgments to those members of the Institute, and professional colleagues outside of it, who hays favored me with ' assistance and advice. The labor bestowed upon this paper since its presentation, at the Lake Superior meeting has considerably exceeded that of its first preparation, as

Jan 1, 1881

By J. Ruzicka

IN creep testing, material is subjected to a constant load, preferably at a constant temperature, and its rate of deformation is measured. The method of loading can be of various types but in this paper only creep testing under tensile load will be considered. The ordinary tensile test is essentially a comparison test in conditions that frequently bear little or no relation to those under which the test material is to be used in service. The purpose of creep tests is to measure the strength of the test material at slow rates of deformation that more nearly approach the rates realized in service. One purpose of this paper is to illustrate that the creep test, in addi-tion to its value as a service test, is superior to the ordinary tensile test as a sensitive tool for the comparison of certain metals in investigative testing. The other purpose is to describe equipment having distinctive features of design that make it especially suitable for such tests. Representative data obtained with this equipment on a group of rolled zinc-base materials are given. These data are compared with those from practical comparison tests of the creep type on weatherstrip fabri-cated from the same group of materials. The comparison illustrates the value of the fast creep test and of the equipment.

Jan 1, 1937

By R. F. Domagala, M. Hansen, D. J. McPherson

Iodide zirconium was combined with calculated amounts of nitrided zirconium sponge and arc melted to prepare alloys in the 0 to 6 wt pct N region. Annealing treatments were carried out at 21 temperature levels. Metallographic examination of the heat-treated specimens permitted construction of the binary phase diagram from 0 to 6 pct N. Features of the diagram include the peritectic formation of both a and ß solid solutions. The maximum solubility of nitrogen is 0.8 pct in 8 zirconium and 4.8 pct in a zirconium. An X-ray study of nitrided materials was made in the range 6 to 13 wt pct N region because serious nitrogen losses were experienced when attempts were made to arc melt these high nitrogen alloys. PHASE relationships in the Zr-N system have been determined. Due to the inability to retain nitrogen in nitrogen-rich alloys subjected to arc melting, definitive work was possible only in the range 0 to 6 wt pct (0 to 30 atomic pct) N. Sufficient complementary X-ray work was done to permit construction of the binary phase diagram up to 13.3 wt pct (50 atomic pct) N (ZrN). Small ingots were prepared by arc melting master alloys with enough zirconium to produce an alloy of the desired composition. Following pretreatment, alloys were annealed at temperature levels between 600" and 2020°C. Determination of the phase boundaries was then accomplished by metallographic evaluation of specimens quenched from the various temperatures. Incipient melting techniques were used to corroborate solidus curves, and X-ray diffraction was employed to study the nitrogen-rich region of the a + ZrN phase field. Materials Westinghouse Grade 1 iodide zirconium crystal bar served as the base material for this investigation. The as-received bars were lightly sandblasted, pickled in a 20 pct HN0-5 pct HF aqueous solution, rinsed in water and acetone, and dried. They were rolled to about 1/32 in. strip and acid-pickled, followed by water and then acetone rinses. The material was sheared to approximately 1/4 in. squares, cleaned with acetone, and stored for use. Pure zirconium nitride is not commercially available, according to correspondence with possible suppliers. A literature survey indicated that nitrogen may be introduced into zirconium metal by passing nitrogen or ammonia gas over zirconium at an elevated temperature. After considerable experimentation, a train was devised whereby high quality nitrogen was passed through a series of bubblers to remove the last traces of oxygen, through an H,SO, bubbler and a cold trap to remove moisture, and finally over zirconium within a resistance furnace. Hand-picked Bureau of Mines magnesium-reduced zirconium sponge proved more amenable to nitriding than the crystal bar. The nitrogen used was extra pure gas purchased from Linde Air Products Co. The first two bubblers through which the gas was passed contained a solution suggested by L. F. Fieser" as being ideal for removing the last traces of oxygen from nitrogen. The solution contains 20 g KOH, 2 g sodium-anthraquinone ,9-sulphonate, and 15 g NaHSO, dissolved in 100 ml water. It is blood-red and turns brown when contaminated with oxygen. A saturated lead acetate solution, next in the series of bubblers, removed any H2S which might have formed in the 0, removal stage. An H,SO, bubbler and cold trap removed moisture before the nitrogen was passed over the zirconium. The zirconium was contained in a stainless steel screen within a Vycor or quartz tube in a resistance furnace. Unreacted nitrogen passed out of the system through a mercury bubbler. A nitriding run was performed in the following manner: Zirconium was placed in the screen within the furnace tube. The unit was assembled, suitably clamped off, and evacuated to remove the air and moisture within the tube and that trapped by the zirconium sponge. The unit was flushed with nitrogen and evacuated twice. After nitrogen was allowed to pass over the zirconium for about 30 min, the furnace was turned on; several hours were required to reach temperature. The reaction was allowed to continue at temperature for about 4 hr and the screen was then withdrawn from the hot zone of the furnace by means of a Nichrome or Kanthal rod. The screen and its contents were allowed to cool at the end of the tube and were then removed. At 800°C no more than about 5 pct N could be introduced into the sponge zirconium. This material was designated M-1 (master alloy No. 1) and reserved for the preparation of alloys in the dilute nitrogen region. A second set of experiments was conducted at 1000°C; no more than 7.2 pct N could be introduced into the zirconium at this temperature. Enough material (M-2) of this nitrogen content was prepared to produce a second set of alloys to complement the first and to provide alloys in the 0 to 6 wt pct N range. It was hoped that a diffusion anneal plus a re-nitriding might yield a material of higher nitrogen content. The material containing about 7 pct N was therefore given a homogenization treatment at 1000°C for 6 hr under an argon atmosphere. It was

Jan 1, 1957