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By Jeffrey L. Thompson, Kenneth A. Gutschick, Robert C. Freas, Robert S. Boynton

Lime, the "versatile chemical," is, generally speaking, a calcined or burned form of limestone commonly known as quicklime, calcium oxide or calcia, or, when water is added, calcium hydroxide or slaked lime. Almost 40 different lime products are available, a fact which has contributed to the rather loose use of the term lime as well as to much confusion and misunderstanding. The term is frequently, albeit erroneously, used to denote almost any kind of calcareous material or finely ground form of limestone or dolomite. Lime is usually made from high-calcium or high-magnesium limestone, generally having a minimum of 97% combined carbonate content. Normally, high-calcium limes contain less than 5% MgO. When the lime is produced from a high-magnesium limestone, the product is referred to as dolomitic lime. Calcination, or the production of lime, has its origins in the earliest days of alchemy, with the general reaction class having been identified in an Arabic text printed in 1000 A.D. It was much later, however, in the mid-1700s to the mid-1800s before this basic reaction became understood from a scientific perspective. The production of lime has been so basic and simple that its underlying scientific principles have over the years received only intermittent investigation. Rather, much of the thought and inquiry has been directed toward the development of kilns. Thus, it has only been in the last 15 to 20 years that lime has received any concentrated scientific investigation relative to the thermodynamics and kinetics of the calcination and hydration reactions. Calcination refers to a broad class of reactions, of which the lime/limestone reaction is just one, wherein a substance is heated to less than its melting point, resulting in a weight gain or weight loss. In the calcination of limestone to produce lime, the basic chemical reaction is as follows: [CaCO3 (limestone) + heat (1000° to 1300°C)= 100 CaO (quicklime) + CO2 T 5644 or CaCO3 • MgCO3 (limestone) 10084 + heat (900°C to 1200°C) CaO • MgO (quicklime) + 2CO2 T 56 4088] While there is nearly universal agreement about the equilibrium conditions related to the limestone/lime reaction above, there have been numerous and varied calcination models developed for the reaction. Recent investigations have resulted in the development of the model shown in Fig. 1. From this model it can be seen that calcination is a function of both temperature and CO2 pressure. It does not, however, provide any indication of the rate at which the reaction takes place. Calcination is strongly time variant with different limestones. In a very broad sense this relates to the fact that the calcination reaction starts on the exterior surface of the limestone and then proceeds toward the center. As the calcination reaction takes place, the CO2 released at the reaction interface must make its way through the lime to the exterior surface. Therefore, because calcination is limited by gas diffusion to the surface of the partially calcined limestone, natural impurities in the stone, differences in crystallinity, grain boundary chemistry, density variations, and imperfections in the atomic lattice all play a significant role in

Jan 1, 1983

A. L. FIELD, Cleveland, Ohio (written discussion*.-)In equation 2, B is used to denote the ratio of bases (lime plus magnesia ) to acids (alumina plus silica) it being stated that this ratio gives more concordant results than the ratio either of bases to silica, or of lime to silica. I find, however, that, by making use of the ratio between true CaO (CaO by analysis minus sulfur calculated to CaS) to acids, equation 2 may he modified to agree with the observed facts within an average error of 0.0041 per cent. sulfur instead of 0.0045 per cent. The revised equation is s = 0.072 + 0.01835 - 0.00061 (t - 1400) - 0.0403B where B is the ratio of true CaO to Al2O3 Plus Si02, and the other symbols have the same significance as before. I would not appear to stress too much this slightly better agreement of the revised equation with the observed sulfur. Yet I believe that the use of this ratio of true CaO to acids is to be preferred, if for no other reason than the fact that it is more in harmony with the previous findings of the Bureau of Mines with regard to the effect of magnesia and other impurities on slag viscosity.1

Jan 12, 1919

Executive Committee. ROBERT H. RICHARDS, Chairman. ALBERT SAUVEUR, Vice-Chairman. TIMOTHY W. SPRAGUE. HENRY A. WENTWORTH. AUGUSTUS H. EUSTIS, Secretary, 131 State St., Boston, Mass. The twelfth meeting of the Boston Section was held at the Engineers' Club, 2 Commonwealth Ave., Boston, on Monday evening, May 5, 1913, fifteen members and three guests being present. The meeting was called to order by Vice-Chairman Albert Sauveur, who introduced the speaker of the evening, Utley Wedge, of Ardmore, Pa. Mr. Wedge read his paper on the chloridizing roasting of copper ores, which he illustrated with a stereopticon, and which will be published in full by the Institute. After Mr. Wedge had closed his paper, which was received with great interest by all the members, the following discussion took place: Professor Hofman said that iron was formerly thought to ho essential to the Henderson process, but that it is not absolutely essential. Mr.Wedge said that, as far as he. knew, the presence of some sulphates was an abso¬lute necessity, and that line ores can be worked satisfactorily, although lime has an effect on the subsequent leaching. He added that the low fuel consumption of the latest Wedge furnace is a result of direct application of the combustion gases to the ore. Ten per cent. of fuel was needed with the muffle furnace. By direct firing he has been able to reduce the fuel needed to from 2 to 4 per cent. In the latest types of furnaces the gases from the upper hearth are not used. There is doubtless some temperature at which the loss. from copper chloride volatilization becomes serious, but in practice on Rio Tinto ores troublesome losses are not experienced. The copper apparently does not become volatile at. the temperatures where we would expect that it would. There are doubtless ores in which there would be serious danger from losses from this source. The latest furnaces do not use the high temperatures that were needed in the former single-hearth Wedge furnaces.

Jan 7, 1913

Last October a committee was appointed by The War Service Association of Manufacturers of Solder and Bearing Metals, Inc. to consider the report of the U. S. Bureau of Standards to the Conservation Division of the War Industries Board, a letter of the War Industries Board, and the discussions of this letter as reported at the meetings of association and to summarize the information thus obtained. The report of this committee has just been printed. The committee agrees with the Bureau of Standards that 99 per cent. tin can be used. It also finds that a very small amount of lead might increase the tendency of the bearing to crack and that lead has a hardening effect on babbitts up to a possible limit of 10 per cent. of lead. Still in the so-called genuine babbitts, in the presence of lead a certain proportion of low melting point eutectic is introduced which admits of the bearing being poured into thinner sections and is decidedly advantageous in the die-casting process in producing a much smoother casting. But the committee recommends that the Bureau of Standards thoroughly investigate this point. Lead-base babbitts, to give satisfactory service, must be carefully made of the proper raw materials. The bronze hearing that has been thoroughly tinned and containing the thinnest possible babbitt lining is now becoming recognized as the ideal bearing. The compositions, recommended by the committee are as follows:

Jan 2, 1919

By Hamilton Wingate

In his paper on the hydraulic mining of a low-grade gravel in California,* Mr. W. H. Radford expresses the hope that other members of the Institute will contribute, for the benefit of all, their experience in similar lines. In these notes 1 shall describe the conditions and results of the operation of the Gold Bug Mining Co., of Cleveland, O., at Georgetown, Eldorado county, Cal.

Jan 1, 1903

By G. R. Rigby

Used basic brick taken from copper anode furnaces, reverberatory furnace roofs, md copper converters have been examined by chemical analysis, petro-graphical examination, and X-ray diffraction tech-niques. In the anode furnace roof, brick absorb copper and copper oxides, whilst in the reverberatory roof, iron oxide with smaller amounts of alumina and silica are absorbed. Chemical reactions in the converter are most complex since the brick absorb both a copper-copper oxide slag and a fayalite-magnetite slag. CHANGES taking place in basic brick after use in copper smelting furnaces have received attention from C. Burton Clark and J. Spotts Mc Dowell,' who examined brick taken from copper converters, and by G. R. Rigby and B. G. Hamilton' who examined brick from copper anode furnaces. This paper describes the changes taking place in basic brick from all types of copper smelting furnaces and discusses the major reasons for lining wear. A) METHODS OF EXAMINING SAMPLES A variety of used brick have been taken from the following positions in various furnaces, a) roofs, reverberatory arches, and bottoms of copper anode furnaces, b) roofs of copper reverberatory furnaces and c) the tuyere line and end walls of copper converters. The method of examination was standard in that brick were first measured and the extent of wear-back computed. They were next sawn in two by a central cut vei-tical to the working face to enable the freshly cut surfaces to reveal any zonal changes and cracks, both of which usually ran parallel to the working face. Each well-defined zone was then sampled for a) chemical analyses, b) petrographical studies using transmitted and reflected light techniques under the microscope, and c) X-ray diffraction studies on powdered samples. From the data accumulated, changes taking place in a variety of

Jan 1, 1962

By AIME AIME

COAL occupied a large place in the technical sessions of the Institute at its annual meeting for in addition to three sessions specifically de- voted to coal the two sessions on mine ventilation and the two on ground movement and subsidence, which are reported under their own headings, were primarily concerned with coal. The first session on coal was a joint one with the Iron and Steel Division, on Wednesday afternoon, with F. H. Crockard and J. R. Campbell presiding as joint chairmen and the latter actually officiating. The principal topic of discussion was G. S. Scott's paper "Evaluation of Coal for the Making of Blast- Furnace Coke," which has been published as T. P. 159. The author made a brief statement of its con- tents to start the discussion and the chairman, after briefly reviewing it himself, called on C. A. Meissner to start the discussion. He briefly reviewed the economic factors in the use of coal for coke-making, saying that not only .does the removal of 1 per cent of ash from the coal reduce the cost of pig iron 12 or 13c. per ton, but it also permits coke of satisfactory structures to be made from a coal which otherwise could not be used. He stressed the importance of uniformity in blast-furnace fuel and discussed the benefit of mixing different coals as raw material for the coke oven and cited experience with Illinois coals.

Jan 1, 1929

By Augustus Locke

Jan 1, 1923

By Augustus Locke

Jan 1, 1923

By E. V. Kleber, V. F. Novy, R. C. Vickery

The constitutional diagram has been determined for the system gadolinium-nickel. Nine intermetallic compounds have been found at compositions corresponding to the following gadolinium-nickel ratios: 3:1, 3:2, 1:1, 1:2, 1:3, 2:7, 1:4, 1:5, 2:17. The GdNi and GdNi5 compounds have congruent melting points of 1300' and 1500°C, respectively while the remaining compounds melt in-congruently. Eutectics exist at 15 wt pct Ni, 31 1/2 wt pct Ni and 87 wt pct Ni with melting points of 6703 8803 and 1220°C, respectively. IN a continuing investigation of the properties of rare earth alloys, a study has been made of the gadolinium-nickel system. Previous work encompassed the iron containing alloys and a subsequent paper will deal with the constitution of the gadolinium-cobalt system. Vogel,1 examined alloys of nickel with lanthanum and cerium. R3Ni, RNi, RNi2, RNi3, RNi4, and RNi5 compounds were found. Endter and Klemm,2 Fulling et al.3 Heumann,4 and Nowotny5 found the 1:2 compositions of this series to exist in a C-15 (face-centered cubic) structure, and the 1:5 compositions in a hexagonal system. Jepson and Duwez6 more recently examined these 1:2 and 1:5 compositions and generally confirmed earlier data while Wernick and Geller7 most recently have given additional data on the GdNi5 compound. Comparisons with our results will be made in the appropriate section of this report. EXPERIMENTAL Methods of alloy preparation, annealing procedures, and experimental techniques have been given in our earlier paper.8 Chemical analyses of the alloy samples were made by dissolving the specimen in nitric acid, precipitating the gadolinium as hydroxide and the nickel with dimethylglyoxime. Both precipitates were ignited to oxide and weighed. RESULTS Microstructure— Metallography of alloy specimens in this series has been conducted on both arc-melted and annealed materials. Etchants used have been 5 pct nital with approximately 10 pct distilled water added, for high gadolinium samples; Carapella's ferric chloride solution for intermediate compositions; and Marble's (copper sulfate) reagent for high nickel content alloys. Because of difficulties encountered in the grinding and polishing of specimens containing 40 to 75 wt pct Ni, no photomicrographs were made of such specimens. The microstructure of an arc-melted 5.3 wt pct Ni alloy is shown in Fig. 1. Light etching primary grains of gadolinium are embedded in an eutectic matrix. The microstructure of an alloy of 9.55 wt pct Ni alloy, Fig. 2, annealed 50 hr at 700°C, consists almost entirely of the intermetallic compound Gd3Ni. The structure of an arc metal alloy of approximately 19 pct Ni, Fig. 3, consists of grains of the compound GdNi embedded in the Gd3Ni2-Gd3Ni eutectic. The arc-cast structure of the 38.7 wt pct Ni alloy is shown in Fig. 4. Large primary grains of a compound rest in a matrix structure of coarse GdNi-GdNiz eutectic. Because of the occurrence of several peritectic compounds in the central region of the diagram, identification of the primary structure in this alloy is not certain. As has been indicated above, microstructures of alloy specimens containing between ca 40 and 75 wt pct Ni have not been photographed. These specimens were highly brittle, and macro- and micro-cracking were impossible to control in the grinding and polishing procedures. Prolonged annealing did not alleviate this condition. Visual observations in small specimens did, however, provide evidence for a multiplicity of phases and peritectic dissociations of compounds although rationalization of structures was not possible.

Jan 1, 1962

By H. M. Chance

The Taviche district is about 12 miles from the town of Ocotlan in the State of Oaxaca, and about 250 miles south of the City of Mexico. Its altitude rises to something more than 5,000 ft.; and although within the tropics (latitude about 17° N.) the climate is mild and salubrious, neither excessively hot in summer nor cold in winter. The phrase, "perpetual spring," which has been applied to it, aptly describes the weather during my stay. Sugar-plantations, bananas and other tropical and semitropical fruits flourish in the valleys, while the hills

Jan 1, 1905

The Joint Economic Committee's subcommittee on international payments and exchange has recommended that, following international monetary reforms, the law which prohibits private possession of gold by American citizens be repealed. The subcommittee recommendation called for reforms to enhance the role of special drawing rights in international monetary affairs and downgrade the role of gold. Special drawing rights, also known as "paper gold", are on artificial reserve with the International Monetary Fund (IMF) which distributes them to member nations in proportion to their economic importance in the world economy. The special drawing rights are then used to settle debts between nations in the same manner as gold or currency. The subcommittee said that under the reforms now being discussed special drawing rights would be acceptable in lieu of gold among the member countries of the IMF.

Jan 1, 1973

Planning for a surface coal mine includes selecting the best means and equipment for uncovering the coal, loading it, and transporting it to the preparation plant. The machines and methods that will ensure optimum production will depend upon the location and characteristics of the seam to be mined. Stripping Techniques The choice of stripping units is influenced primarily by the system of mining, such as contour or out-crop mining as contrasted to mining in a region of rolling terrain with relatively flat upland surfaces. Factors such as the life of the mining operations production requirements, types of overburden, local and regional dip of coal, and land reclamation are other important considerations.

Jan 10, 1967

By J. D. Miller Discussion by N. P. Finkelstein, M. C. Fuerstenau

The point designating 10 -4 nole/per liter sulfonate addition in Fig. 1 has been presented incorrectly. This figure, with the corrected scale, is shown at right. N. P. Finkelstein (National Institute for Metallurgy, Johannesburg, South Africa) - The qualitative conclusion the authors of this paper have reached in evaluating the influence of hydrocarbon chain length on collector effectiveness agrees with conclusions in several published reports. However, in two other

Jan 1, 1969

By M. C. Lavine, H. C. Gatos, R. S. Mroczkowski

The structure of GaAs-Ge heterojunctions prepared by a back-melting process was studied by X-rav diffraction, melallographic, and electron-micro-analyzer techniques. The boundary region between the GaAs and the germanium was found to consist of a four-layered band. A discontinuity between the two inner bands was brought about by solidification occurring simultaneously from the GaAs and the germanium side. The junction material OH either side of the central discotinuity was found to have grown as a single Crystal with the orientation of the parent substrate. It was found essential to determine the GaAs-Ge phase diagram. This was accomplished by a series of alloys containing 0 to 40 wt pet GaAs. Over this range the diagram is a simple eutectic with the eutectic point at 74 wt pet Ge and 845 C. The limiting- solubility of Coils in germanium was found to bc less than 5 wt pet. The Kossel divergent-beam X-ray technique was used to study orientation relationships across the boundary lager. A great deal of effort has been recently expended on the electrical properties of heterojunctions. Little attention, however, has been given to the metallurgical variables which may be of importance in the formation of the junctions. The present work was undertaken to investigate some of the more pertinent metallurgical aspects of interface-alloyed GaAs-Ge heterojunctions. Such parameters as solidification processes, composition gradients, orientation effects, and the accommodation of crystal structures have been the objects of study in this program. EXPERIMENTAL PROCEDURES Phase Diagram. The phase diagram of the GaAs-Ge pseudobinary system was determined by means of cooling curves. A Bridgeman furnace was employed with the center section maintained at 1200°C and the upper section at 800°C. Melts varying from 0 to 40 at. pct in GaAs content were used. Each charge was incapsulated under a two-thirds atmosphere of argon in a carbon-coated quartz tube. Five min in the furnace hot zone provided rapid melting and homogenization. The capsule was then removed to the cooler portion of the furnace. Cooling times were of the order of 3 min. The resulting homogeneous microstructure indicated that equilibrium conditions were obtained by this procedure. Formation of Heterojunctions. Rectangular parallelepiped single-crystal samples were cut with the large faces of either the (l00), (110), or (111) orientation. The remaining four surfaces were also cut to specific orientations to permit accurate relative orientation of the GaAs-Ge pairs. The

Jan 1, 1965

Discussion of the paper of M. B. YUNG, presented at the Pittsburgh meeting; October, 1914, and printed in Bulletin No. 93, September, 1914, pp. 2451 to 2458. T. T. READ, New York, N. Y.-I might .point out that this paper of Mr. Yung's is on a field that is comparatively little known. It is not as well known as the Kochiu tin field, of Yunnan, which is probably the third . in tin output of the world. This field under discussion is considerably further west and the tin which is produced here is, according to Mr. Yung, of somewhat higher grade than the Yunnan tin, and is used by the refiners at Hong Kong to improve the grade of the Yunnan tin. Most of you know that the tin from the Yunnan is shipped to Hong Kong, where it is refined and shipped to Europe. Mr. Yung points out that the Fu Chuan deposits are entirely alluvial and not found in any veins. They .differ in that from the Kochiu deposits, which Leclere says are "nullement alluvionels; leur origéne filonienne est de plus evidentes." Granite is the country rock here; doubtless the tin occurred in veins in the granite, and the deposits have resulted from the disintegration of the granite. This is a country of strong erosive agencies. The country is semi-tropical, and the rainfall is heavy, so that one would naturally expect deep surface erosion of this kind.

Jan 4, 1915

By N. F. Fiore, M. C. Mangalick

DISLOCATION damping in single crystals is orientation dependent.&apos; If dislocations are distributed uniformly over all the slip systems in a crystal, and if each dislocation contributes identically to the damping process, then a damping loss or decrement 6 arises. In fact, however, for a crystal of axial direction (hkl), dislocations on certain slip systems are oriented to make a larger contribution to the damping loss than are dislocations on other slip systems. Thus the measuring damping, 6 (hkl) is proportional to an orientation factor (hkl), which weights the ability of each slip system in the crystal to contribute to the total damping. If it is assumed that dislocations are distributed uniformly on all slip systems, then for a given orientation of an fcc crystal this factor is determined2,3 by the three nonzero elastic constants Cll, C12, and C44 and the density p. In this communication measured values of elastic constants for two Fe-18Cr-Ni alloys are reported, and the dislocation damping results on two different orientations of each alloy are analyzed for orientation dependence. Elastic constants were determined by measuring the ultrasonic velocities of one longitudinal and two shear waves in (110) direction of the fcc crystals.4 Variation of velocities with the change in orientation is very small for (110) orientation,3 and so this direction is ideal for orientation factor and comparative damping measurements. Experimental Procedures. The nominal compositions of the alloys studied are given in Table I. These alloys were vacuum-melted and vacuum-cast from high-purity materials at U.S. Steel Applied Research Laboratories. The single crystals were grown by the modified Bridgeman technique. The specimens were homogenized at 1350°C for 20 hr, cut to shape and size with a spark cutter, and then annealed at 1100°C for 20 hr prior to use. In the KHz frequency range, the Marx composite piezoelectric oscillator was used to obtain the damping. The ultrasonic pulse technique was used to measure the ultrasonic velocities and the attenuation in the MHz frequency range. M.c.mANGALICK,-- StudentMemberAIME,formerly Research Assistant, University of Notre Dame, is now with Casting Laboratory, Chase Brass and Copper Co., Cleveland, Ohio. N. F. FIORE, Associate Member AIME, is Assistant Professor, Department of Metallurgical Engineering and Materials Science. University of Notre Dame, Notre Dame, Ind. This communication is part of a Ph.D. thesis presented by M. C. MANGALICK to the Graduate School of the University of Notre Dame. Manuscript submitted May 20. 1968. IMD Elastic Constants. Table I gives the values of the ultrasonic velocities. Values of C11, C12, and C44 calculated from these velocities are also given in Table I, and it is evident that there is very little variation in C11, C12, and C44 with nickel content. This slight variation may be attributed to inaccuracies in velocity measurements and practical differences in the orientations of the specimens. For example, in B the time interval for vl was 2.4 ± 0.05 sec giving an error in v1 of 0.235 x or 0.005 in. per sec. The elastic constants obtained by pulse technique were tested by calculating E<110>, Young&apos;s modulus for the (110) direction, from the equation: This value was compared with the value computed from the resonance bar measurements in which where fr is the resonance frequency and I, is the length of the specimen. In all cases, the values calculated from the ultrasonic velocity measurements

Jan 1, 1969

R. B. BRINSMADE, Ixmiquilpan, Hgo, Mexico* (written discussion). As the discussion of Mr. Graton&apos;s paper by Messrs. Norris, Patterson, and Crane has been from the standpoint of the mineral land-value owners, a few remarks in the interest of the "under dog"-the average taxpayer and citizen-may prove timely. In my discussion of Doctor Raymond&apos;s Paper1 and of the papers of Messrs. Gibson2 and Godson, 3 have endeavored to demonstrate, from both political economy and history, that our existing system of unrestricted private ownership of land is incompatible with equality of economic opportunity and, therefore, subversive of our democratic political institutions. In Mr. Graton&apos;s paper, the same land problem is important, though camouflaged by the failure of the Federal income tax laws to distinguish between land and capital, in the requirements for valuation, or between earned and unearned incomes in the levying of taxes. I disagree with Mr. Graton&apos;s statement, on p. 2967, as follows: The immense majority of mining ventures are failures. A multitude of disappointments is relieved by occasional success. Were it not for the chance of great rewards, all the vitally necessary but mainly unremunerative work of exploration would not be undertaken. In contrast with nearly all other fields of endeavor, it is altogether unlikely that, on the whole, the gains in the successful mining ventures suffice to offset the losses in the unsuccessful.

Jan 3, 1920

The following communication has just reached the Institute, from the office of the Provincial Geologist, Department of Lands,-Forests and Mines, Ontario, Canada: During the autumn of 1917 gold was discovered in unsurveyed territory south of Lake Abitibi in northeastern Ontario. This area lies about 70 miles almost directly east of the well known Porcupine area. During the coming summer, the Ontario Bureau of Mines is to make a geological survey of this new gold area. Following the custom of Ontario, this area is being divided into townships, 6 miles square. These townships have recently been given the following names in honor of men well known in the mining and geological world. In alphabetical order the names are as follows: Frecheville-Prof. Wm. Frecheville, Professor of Mining in the Royal School of Mines, London; Past President of the Institution of Mining and Metallurgy. Garrison-Mr. F. Lynwood Garrison, Mining Engineer, Philadelphia, Pa. Harker-Dr. Alfred Harker, F. R. S., immediate Past President of the Geological Society of London.

Jan 6, 1918

By John D. Roach

DURING an investigation of the yttrium-hydrogen system aimed at producing solid yttrium hydride specimens containing various amounts of hydrogen, it was observed that yttrium containing approximately 2 wt pct H exhibited a tendency to crack and crumble to a powder on standing in air at room temperature. It was also observed that longer hydriding times, at a given temperature, increased this susceptibility to powdering without an increase in hydrogen content, also that moisture in the air is necessary for the observed effects to occur. Even if cracking did not occur, there was a continual formation of a light gray powder on the as-treated surface of the hydrided yttrium and this reaction continues until the entire hydrided piece has been reduced to a powder. Storing the hydrided specimens in the absence of air or removing the surface either by machining or grinding were effective means of preventing this disintegration of hydrided yttrium. In an attempt to determine the reason for this powdering phenomenon, the surfaces of a number of as-hydrided yttrium specimens were examined by X-ray techniques. In all cases the X-ray pattern obtained showed the major phase to be yttrium hydride (YH2) as would be expected since the specimens contained 2 to 2.2 wt pct H. In some cases a trace of yttrium oxide was observed. There was also a third phase present on the surface of these hydrided specimens which could not immediately be identified. This unknown phase was a face-centered cubic material, NaC1-type structure, with a lattice parameter of 4.855 and a calculated density of 5.914 g per cc. Very slight hand polishing of the surface of the hydrided yttrium specimens completely removed both the unknown phase and the traces of oxide so that only the yttrium hydride pattern remained. Based on the X-ray patterns the quantity of the unknown phase on the surface of the hydrided yttrium appeared to be directly related to the susceptibility of the material to powdering. Work at the Denver Research Institute on the yttrium-nitrogen binary system showed that yttrium nitride (YN) is a face-centered cubic material with a lattice parameter of 4.878A and a density of 5.890 g per cc. They also noted that this compound rapidly disintegrated to a powder on standing in air. The unknown pattern observed in the above specimens corresponds very closely to that of the nitride—fcc structure, 4.885 parameter, and density of 5.914 g per cc. The presence of this thin film of nitride on the surface of the hydrided specimens probably accounts for the observed powder formation and crumbling. The nitride reacts with the water vapor in the air (verified by private communication from Dr. C. Huffine, General Electric Co.) to yield yttrium oxide and ammonia. Ammonia is readily detected when hydrided yttrium specimens were allowed to stand in bottled moist air. The powder formed on the surface of the hydrided specimens was shown by X-ray analysis to be yttrium oxide. This reaction appears to occur primarily at the grain boundaries since discrete particles of yttrium hydride separate from the specimens during this powdering process. The reaction of yttrium nitride with water vapor is believed to be as follows: 2YN + 3H2O - Y203 + 2NH3. Despite the fact that this nitride is present only as an extremely thin surface film, if the above reaction is not prevented by removing this film from the surface either by machining or grinding, the reaction continues until the entire hydrided piece has been reduced to a powder. To account for this continuation of the reaction, it is believed that the following reactionalsooccurs: 2YH2 + 2NH3 -2YN + 5H2. The nitride produced by the latter reaction reacts in turn with water vapor. The reaction therefore becomes autocatalytic and continues until the hydride has been consumed and the entire piece reduced to oxide powder. The amount of nitride required to initiate this reaction is quite small and this nitrogen contamination can occur from a number of sources—hydrogen gas employed, minute leak in the hydriding apparatus or even from degassing of the reaction vessel itself. Longer hydriding times increase the possibility of nitrogen contamination and this is especially true when a dynamic gas system is employed in the hydriding process. The production of stable, solid hydrided yttrium is dependent on the complete absence of nitrogen contamination during processing. If such contamination does occur, powdering of the hydrided product can be prevented by removing the nitride from the surface e.g. grinding or by preventing access of air to the pieces e.g. sealing in wax or plastic. The author wishes to express his appreciation to General Electric Co. for sponsoring this research and for permission to publish the results of work under Subcontract AT-93.

Jan 1, 1962