Search Documents

By John W. Sweeney

Shales and clays from Illinois were sampled, tested, and evaluated to determine feasibility of producing lightweight aggregate by rotary-kiln methods. Sampling procedures and the 1 ,,,y of the Pennsylvanian shale units are discussed. Chemical, X-ray spectrographic and X-ray petrographic analyses were run on the samples to determine if a correlation existed between chemical mineralogic composition and expansion. Preliminary expansion testing was conducted in a muffle furnace. Rotary-kiln tests were conducted in a 16- inch by 14-foot rotary kiln. The weight of the aggregate ranged from 27 to 59 pounds per cubic foot. Concrete cubes employing the aggregate were tested to determine the qualities of the concrete. Compressive strength of the concrete using the 7-bag of cement cement per cubic yard mix, after autoclave curing for 6 hours, ranged from 2,950 to 6,750 psi. No correlation was found between the chemical, X-ray spectrographic, and X-ray and petrographic analyses and expansion, Sixteen samples made suitable lightweight aggregates in the laboratory rotary kiln. The expansion temperature range of eight of the samples was extremely narrow, and difficulties would probably be encountered in processing these materials commercially.

Jan 1, 1965

By James R. Boyle

The mining methods and practices used at the Young zinc mine, American Zinc Co. of Tennessee, have resulted in a low-cost, high-yield operation. Zinc ore (sphalerite) occurs in limestone-dolomite beds of the Kingsport Formation and is mined by modified room and pillar method. Utilizing trackless mining equipment which incorporates a high degree of flexibility, this operation has had a steady increase in productivity.

Jan 1, 1965

By R. W. Stahl

Gas accumulation and dust suspension are the major safety hazards in coal stockpiling and reclaiming operations. This report presents a schedule of safety precautions and plant design features devised by the Bureau of Mines to reduce danger from these and other sources.

Jan 1, 1965

By John I. Sharpe

Masses of pyritic copper and zinc ores are entrapped along the contact zone between two volcanic groups in the Matagami area. The upper limits of the sulphide concentrations tend to form concordant contacts against lava or cherty tuffite units of the younger group; the lower extremities tend to either follow transverse structures or merge with zones of dispersed sulphides. The sulphides are deformed and intruded by folded dykes. Close relations between metallization boundaries and volcanic lithology and stratigraphy, and a preliminary investigation of the fabrics and crystallization temperatures of the sulphide masses, suggest that the copper and zinc (but; not necessarily all the iron sulphides) were emplaced at h1gh temperatures during volcanism in near-surface lithological-stratigraphic traps. Introduction T HE Matagami area is centered 120 miles north of the Val d'Or and Noranda camps in north-western Quebec. For the present purpose, it is considered to comprise a 155-square-mile area in Isle-Dieu, Galinee and Daniel townships which encompasses the main sulphide masses. Airborne geophysical surveys within this area in 1956 led to the discovery of a large sulphide body -the.

Jan 1, 1965

By N. Albon, J. F. Miller, R. W. Coutant

The deposition of nickel from nickel carbonyl onto amorphous substrates has been studied, with attention being paid to the specific effects of the physical and chemical nature of the substrate and to the effect of oxygen on the crystal morphology. With substrates having microscratches or etch lines, nu-cleation was observed to occur preferentially at these surface features. Flame polishing of the substrate surfaces was found to remove any regularity in preferred nucleation sites. Nucleation was observed to occur less readily on substrates having relatively low surface energies, e.g., Teflon and carbon, than on materials having relatively high surface energies such as fused silica. At low oxygen concentrations [Ni(CO)4/O2 > 54 x 1031, apparently pure and well-formed nickel crystals were observed to nucleate and grow irrespective of the presence of oxygen. At higher concentrations of oxygen, a secondary growth process, dependent upon oxygen concentration and resulting in a gradual change in crystal morphology, was observed. It is concluded that the influence of oxygen on the nucleation and growth of nickel is determined by the relative kinetics of the various possible reactions, and that under the experimental conditions employed the 0-Ni interaction occurs at some nucleation or prenuclea-tion stage. THE purpose of the research on crystal nucleation in chemical vapor deposition as described in this paper has been twofold: 1) to examine some effects arising from the use of amorphous substrates, and 2) to study the specific effects of oxygen on the nucleation and growth of nickel in a nickel carbonyl-carbon monoxide system. The nickel-nickel carbonyl system was chosen for study for several reasons: 1) nickel films are of potential interest in electronic technology, and 2) the deposition can be carried out at moderate temperatures, thus making possible detailed study of the processes occurring and the use of a variety of substrate materials (including some which melt at relatively low temperatures). Fairly well-characterized chemical kinetics and a broad background of information are available on the py-rolysis reactions and on the mechanisms of Ni-O interactions. NUCLEATION AND GROWTH THEORY The theoretical background for the analysis of nucleation and growth by vapor deposition for a one-component system (physical vapor deposition) and the problems encountered therein have been reviewed by Hirth and pound.' More recently Mande12 has indicated the difficulties of applying such theory to chemical systems. One of the major problems involved is the possible multiplicity of chemical reactions and deposition routes. For example, those reactions which are probably of significance in a discussion of the pyrolytic deposition of nickel from nickel carbonyl under the conditions of the present experimental work are illustrated in Fig. 1. As is true with most cases of chemical deposition, many of the quantitative data necessary for a complete analysis of the system are either not available or not directly measurable. However, with the present system, sufficient data are available for a discussion of nucleation and growth on a qualitative basis. Classically, the rate of nucleation of a monatomic species being deposited from a vapor phase is given by

Jan 1, 1965

To enable ammonium nitrate-fuel oil (AN-FO) to be used on an equal weight basis with nitroglycerine explosives, smaller diameter bore holes became necessary with consequent modifications to drill steel and burden on holes. Detonation of AN-FO in small diameter holes proved successful both with and without primer charges but some alterations were required to adapt anoloders to the smaller holes.Important factors in training all operators in the new charging method were the retention of improved fragmentation, avoidance of excessive overbreak and keeping wall rock dilution to an absolute minimum. The successful storage of ammonium nitrate in climatic conditions with daily temperature fluctuations above and below the critical 90°F has been achieved.INTRODUCTIONTechnical aspects of ammonium nitrate-fuel oil (AN-Fa) blasting agent are well covered in recent literature. This paper deals primarily with the manner of its introduction as the principal explosive underground at Great Boulder Gold Mines Ltd. and with the many problems encountered in the process. Following reasonably successful experimental firings in June 1962', using granular ammonium nitrate and an anoloder, permission was granted by theWestern Australian Mines Department to carry out test work in selected areas of the mine. The permit allowed for fuse firing only, and for a mixture of AN-Fa containing between 5t and 6 per cent fuel oil, with an adequate primer.The use of AN-Fa on an equal weight basis with nitroglycerine explosives, involved smaller diameter holes with alteration to ground burden and modification to drill steel.Initial tests indicated that it was apparent that AN-Fa could not replace gelignite on an equal weight basis if the...

Jan 1, 1965

By Clark F. Grain

The monoclinic to tetragonal inversion of zirconium dioxide was studied by single-crystal X-ray methods, high-temperature X-ray diffractometry, and differential thermal analysis. The unusual features of the inversion, such as no definite transition Lperature, hysteresis, and athermal kinetics, were confirmed for powders who mean crystallite size was greater than 1,000 A. Samples of mean crystallite size below 1,000 A displayed classical kinetics, obeying a logarithmic rate law. A detailed mechanism based on Ubbelohde's theory of continuous phase transformations was proposed which is consistent with all the experimental facts.

Jan 1, 1965

By Wilbur I. Duvall

A linear array of shot and gage holes 30 feet deep in a granite outcrop was used to compare the size and shape of radial strain pulses produced in the rock when short cylindrical charges of cast composition B were detonated axially or at one end. The axially detonated charges produced radial strain pulses that had shorter rise times and larger peak strain than the strain pulses produced by end detonated charges.

Jan 1, 1965

By Matthew Blecha

The Tribag copper deposit is one of the rare examples of mineralized breccias in the Canadian Shield. The breccia is a pipe-like body, and consists of granitic, diabasic and volcanic fragments embedded in a vuggy, quartz-carbonate matrix. The mineralization is essentially chalcopyrite and pyrite, with minor molybdenite, sphalerite, galena and other sulphides. The main ore zone is saddle-like in shape, and is enveloped in a zone of chloritization, sericitization and clay-mineral alteration. It is suggested that the breccia is of the diatreme type. Introduction T HIS paper is based on eighteen months of field work, including surface and underground geological mapping and core logging, and on the survey of relevant literature. No significant amount of laboratory work has been done as yet. Location and Access The Tribag Batchawana property is located 40 miles north of Sault Ste. Marie, Ontario, about 10 miles east of Lake Superior. A 17-mile, all-weather road connects the property to the Trans-Canada highway to the south, and 4 miles of a 12-mile road remain to be completed to link it to the Algoma Central Railway to the northeast.

Jan 1, 1965

By W. S. Landers

This report presents a detailed study of low temperature, entrained-bed carbonization of an Australian coking coal. The coal studied was high-volatile B bituminous from the Foybrook mine, an open-cut operation in the Liddell seam, New South Wales, Australia. Carbonization was conducted in an 8-inch diameter, continuous vertical reactor at several temperatures from 960° to 1,300° F. It was demonstrated that this bituminous coal can be carbonized within this temperature range to produce tar and a nonagglomerated char, without prior oxidation or char recirculation. Carbonization rates from 138 to 287 lb/hr (as-carbonized basis) were investigated. It was found that the carbonization temperature and the air-to-coal ratio must exceed minimum values to insure continuous operation. At the higher air-to-coal ratios employed, all or most of the carbonization heat was provided by internal combustion with air in the reactor. At the lower air-to-coa1 ratios, part of the heat for carbonization was supplied externally. On the moisture-and ash-free basis, the yield of tar plus light oil ranged from about 26 to 44 gallons per ton, and the char yield ranged from approximately 1,160 to 1,370 pounds per ton. The heat in the gas ranged from about 900 to 3,000 Btu/lb of moisture-and ash-free coal. Carbonization product yields correlated well with air-to-coal ratio and carbonization temperatures. The volatile matter in the char was found to be temperature dependent. At 1,300° F carbonization, the volatile matter in the char was 8.7 percent (dry basis), whereas at 9600 F carbonization, the residual volatile matter was about 16 to 18 percent (dry basis).

Jan 1, 1965

By Zoltan Hajnal

Magnetic studies have been carried out on 88 surface and 157 underground samples from the Coronation Mine area of northern Saskatchewan. The intensity of the surface samples was compared to trace element determinations from the same locality. A good correlation was found between the titaniferous constituent of the rocks and the intensity of magnetization. From the direction of the remanent magnetism, two virtual geomagnetic poles were determined -latitude 12° 54' North, longitude 158" 17' West; and latitude 23" 42' North, longitude 163° 45' West. The sulphide ore specimens showed anisotropic susceptibility characteristics. A relationship was found between the measured maximum susceptibility values of the ore specimens and the direction of the tectonic forces which are considered to have formed the structure at the Coronation mine. Introduction T HIS paper summarizes the results of a study of the magnetic properties of samples from well-known Precambrian formations. The observed data give information for an interpretation of the magnetic field conditions in Precambrian times. The high magnetic intensity values indicate the importance of the study

Jan 1, 1965

By Rex B. McLellan, M. L. Rudee, T. Ishibachi

A modelfor dilute quasi-regular interstitial solid solutions is proposed in which the solute atoms can occupy both the octahedral and tetrahedral interstices in the bee solvent lattice. The distribution function, according to which the solute atoms are apportioned between the two kinds of sites, is calculated. The partial thermodynamic functions of the solution are calculated from the distribution function. It is shown that such a solution model can explain the deviation from linearity of the Arrhenius plot of the temperature variation of the diffusivity of carbon through a iron. The published difiusivity data is analyzed to obtain numerical values for the distribution function. Finally it is shown from the numerical values of the distribution function that the possibility of dual-site occupancy will have a negligible effect on the solution thermodynamics for this system. DeSPITE the large amount of experimental data available on the thermodynamics and diffusion kinetics of dilute solid solutions of carbon in a iron, many of the elementary properties of these solutions are not understood due to real or apparent discrepancies in the experimental data. Basically there is a lack of agreement between the solubility and diffusion data obtained by anelastic damping techniques and by bulk chemical thermodynamic methods. SPecifically the heat of solution of cementite in ferrite estimated from thermodynamic measurement1, 2 is about twice as high as that determined from anelastic damping measurements.3 Furthermore the diffusion coefficient D of carbon in a iron in the range -40" to about 150°C (covering about ten orders of magnitude) determined from anelastic damping techniques is such that an Arrhenius plot of In D vs 1/T is linear. However in the range of about 300o to 850°C where mass flow measurements of D have been made (covering about four orders of magnitude), although the data merges with the low-temperature data, the Arrhenius plot departs from linearity. The object of this paper is to present a more refined model of dilute ferrite solutions in which the solute atoms can occupy two kinds of interstitial sites. The experimental data is analyzed in the light of this model and it is believed that thereby some of the anomalies can be resolved. snoek4 explained the room-temperature internal-friction peak (usually referred to as the Snoek peak) in iron as the stress-induced ordering of interstitial carbon and nitrogen atoms occupying the octahedral (0, 0, 1/2) interstices in the bee lattice. From the consideration of a hard-sphere lattice model the (0, 1/4, 1/4) tetrahedral interstices are larger than the octahedrons but their symmetry would not produce the strain dipole necessary to give rise to the Snoek peak. Thus the presence of the Snoek peak is direct evidence that the octahedrons are occupied. Since the publication of Snoek's explanation, most workers have assumed that all of the carbon and nitrogen in the a solid solution was located in the octahedral sites. This assumption of universal octahedral occupancy has been implicit in the theory of wert5 for interstitial

Jan 1, 1965

By T. H. Courtney, G. W. Pearsall, J. Wulff

The mechanism, of the decrease in transition temperature of Nb3Sn was studied. Presintered Nb3Sn powder compacts were heated in a dynamic vacuum at elevated temperatures. Loss of tin resulted from these heat treatments and transition temperature as a function of tin loss was discontinuous at a critical value of tin loss. In general, decreases in transition temperature were correlated with deviations from AS a class, the A15 structure-type (also known as Cr3O or ß W) compounds have the highest superconducting transition temperatures.' In this class are stoichiometry and presence of vacancies in niobium sites. The effect of vacancy distribution on the physical properties of Nh3Sn is considered. It is concluded that the close-packed atomic A chain in the A3B A15 structure must be preserved both in coutinuity and direction if good superconducting properties are to he obtained. tempting to associate these high transition temperatures with the most unique crystallographic feature of the A3B structure: the three close-packed, orthogonal chains of A atoms.'0"' There are at least three principal mechanisms by which the perfection of these "A-atom chains" could be interrupted: changing stoichiometry, inducing disorder, or introducing vacancies. Departures from stoichiometry in either direction in V3Ga lower the transition temperature.7'8 In niobium-

Jan 1, 1965

By Stephan Stecura

Crystallographic modifications and kinetics of solid-state phase trans-formations were determined for five rare-earth" sesquioxides--La2O3, Nd2O3, Sm2O3, Eu2O3, and Gd2O3. Oxides used for crystal modification studies were prepared by thermal decomposition of the following high-purity salts of the five rare-earth elements--carbonates, chlorides, fluorides, nitrates, oxalates, and sulfates. X-ray diffraction patterns of the cubic and hexagonal oxides were indexed by a graphical method and patterns of the monoclinic oxides by Ito's method. The kinetics of crystallographic transformation were determined by high-temperature X-ray diffractometry. The kinetic data were interpreted using a shrinking sphere model. All of the transformations followed first order kinetics. Activation energies were calculated by application of the Arrhenius equation. These solid-state phase inversions were concluded to occur by a reconstructive transformation mechanism.

Jan 1, 1965

By R. R. Joseph, K. A. Gschneidner

The solid solubility of magnesium in the close-packed modifications of lanthanum, cerium, praseodymium, neodymium, gadolinium, dysprosium, and lutetium was determined from approximately 250°C to the eutectoid temperature by the X-ray parametric technique. The maximum solubility at the eutectoid temperature was found to be 9.4 at. pet in La, 8.2 in Ce, 9.2 in Pr, 8.2 in Nd, 14.1 in Gd, 13.5 in Dy, and 11.5 in Lu. The solubility when compared at a homologous temperature was found to increase in a smooth manner with decreasing size factor from lanthanum to lutetium. It was found that the apparent atomic radius of magnesium when dissolved in the lanthanide solvent was constant and could be accounted for by consideration of several models dealing with departures from Vegard's law. The eutectoid temperatures for the lanthanide-rich La-Mg, Ce-Mg, and Nd-Mg systems were found to be 544", 505°, and 551°c, respectively. A study of the solid solubility of magnesium in the lanthanide metals was initiated because the valency and electron egativity difference are essentially constant and favorable for solid-solution formation, and thus one could examine the effect of size on terminal solid solutions. The size factors based on metal radii range from 14.6 pet for lanthanum to 7.5 pet for lutetium. Since the electronegativity difference is small, 0.06 unit or less, application of the Hume-~othery' and Darken and Gurry2 criteria for solid-solution formation indicates that the solubility of magnesium would be expected to be small for lanthanum (between 5 and 10 at. pet) and to increase as we proceed along the lanthanide series. A search of the literature revealed no data on the solubility of magnesium in the lanthanide metals except for the solubility of magnesium in cerium at 450oCA typical phase diagram for the lanthanide-rich end of the lanthanide-magnesium phase diagram is shown in Fig. 1. EXPERIMENTAL PROCEDURES Preparation of Alloys. The lanthanide metals used in the preparation of alloys for this investigation were prepared from the corresponding fluoride by metallothermic reduction techniques previously described by Daane.4 The chemical analyses of the metals used are listed in Table I.

Jan 1, 1965

By C. O. Hawk

A PART of the Bureau of Mines effort to improve the conversion of coal to liquid fuels, batch autoclave tests were made on the hydrogenation of bituminous coal by a dry method, which featured charging the autoclave with dry ingredients only-coal, catalyst, and hydrogen. This innovation, which omitted the liquid vehicle used in earlier work, limited the products to those made from the coal charged. The effects of the common process variables (catalyst, hydrogen pressure, temperature, and residence time) were studied. Tin catalysts showed the highest activity in the widest variety of forms and were the easiest to disperse; dry mixing in the autoclave during the heating-up period usually sufficed. Ammonium molybdate, on the other hand, was inactive when dry mixed, but it compared favorably with the best catalysts known when applied by impregnating the coal with a solution of a molybdenum compound. As a group, metal naphthenates were the most effective; in fact, molybdenum naphthenate was the most active catalyst the Bureau tests disclosed. One-hundredth of a percent of molybdenum in this form (calculated as the metal in weight-percent of maf coal) induced 90-percent conversion of coal. However, because of their high cost, naphthenates have as yet only technical significance in coal hydrogenation. Long residence time and high reaction temperatures tend to increase the amount of thermal decomposition products formed (light hydrocarbon gases and/or char). High hydrogen pressure favors the production of liquids.

Jan 1, 1965

By K. C. Dean

This report is the first of a series concerned with processes for producing magnesium. These reports will evaluate metallothermic, carbothermic , and electrolytic production methods, and will furnish a cost basis for comparing the processes. Areas deemed most promising for future research will be delineated for each procedure. This report presents briefly the history of the metallothermic process, and describes the operations of the Defense Plant Corp. (DPC) plants that employed the process. A hypothetical plant designed to produce 12,000 tons of magnesium per year, using ferrosilicon as a reductant, is described, and raw materials, energy, and major equipment requirements are estimated. Several process modifications are suggested for future research.

Jan 1, 1965

By James A. Deane

Strip mine reclamation Fs the process of restoring the land affected by the mining process to its most productive use. This can be timber production, pasture, crop land, wildlife and/or recreational use. The mining companies must determine, through the advice of their technicians, what the most advantageous use of the land will be. If the Company does not own the surface, the owner or owners must be contacted to determine their desires as to how the land should be reclaimed. Many times, in making the plans to restore an area with vegetative cover, the watershed and the quality of the water in the area is overlooked. The water itself must be an integral part of the reclamation plan. Many lakes and/or pits can be created with proper planning. In areas in the Midwest, where lakes are a scarcity, these strip mine lakes can become storage reservoirs for large amounts of water, They can help control runoff and low flow augmentation. The strip mining operation will affect the watershed regardless of whether a reclamation plan in made or not. It is up to the reclamation technician to see that the plan benefits the watershed instead of affecting it adversely. This can be done during the operation by intercepting the water before Pt enters the active pit. Diversion ditches above the highwall will handle the runoff water from the watershed. Water that does gain entry into the pit should be removed as quickly as possible. If the rules and regulations adopted by the Ohio River Valley Sanitation Commission in Resolution 5-60 are followed, water encountered during the operation can be handled with little or no adverse effect to the receiving watershed.

Jan 1, 1965

By J S. Kermeen

This paper deals with drilling and blasting techniques at the Phoenix mine, near Grand F1nks, B.C., which is now operated by The Granby Mining Company Ltd. The difficulties of open-pit mining through former underground workings are unique to this operation. Rock types are related to drilling conditions, and the methods used, or contemplated, to overcome the several difficulties are outlined. The equipment used is also mentioned. Finally, blasting techniques and costs are reviewed. Introduction T HE Granby Mining Company operates on open-pit copper mine and concentrator at the site of the original Phoenix mine, near Grand Forks in south-central British Columbia. The pit is a side-hill cut measuring approximately 1,000 by 2,000 ft., and covering a vertical range of from 4,550 to 4,950 feet above sea level. The mill is currently operating at 1,900 tons per day. A 4.5 to 1.0 waste to ore ratio necessitates the removal of some 15,000 tons of ore and waste per working day. Mining conditions at Phoenix are extraordinary in that all the ore zones currently being

Jan 1, 1965

By J. Alfred Berger, O. M. Katz

The Zv-Hf-H ternary system was studied between 500° and 900°C at pressures less than 1 atm of hydrogen gas between 1 and 60 at. pct H. A new and unique microgravimentric apparatus was used. Cizanges of slope on pressure-hydrogen composition isothernis delineated phase boundaries. These boundaries separatecl the three regions, a, 0, and y—so designated to correspond to the regions of the Zr-H binary system—from the multiphased areas between them. A eutectoidal decomposition was found with the ß region phase or phases decornposing into a lamellar product on quenching to rool ter,zperatuve. Reproducible decomposition-pressure hysteresis occilrved lnainly at lower hydrogen cornpositions and at lower temperatures across multiplzase vegions between a and 0 and a and y. Tire effects of hqfniur7z on the hydriding charactevistics of zirconiurrz weYe as follows: 1) stabilization of the a and y vegions while destabilizing the 0 region; 2) a/?preciable elevation of the decomposition pressrkres in the multiphase region between the a and /3 field; 3) ~nouenzent of the eutectoid reaction to high te~nperatures; 4) reduction in the total qiiantity of hydrogen absorbed under one atmospheve of Hz p7-essure; and 5) introduction of a split deconzposilion at the eiitectoiclal poinl in pa?? of the ternavy. Assuru~ptions based on an ir-2terstitial vandonl-solulion rtioclel 0.f hydrogen in metals slzowed that the bindit~g energy between solute sites prednnzinatecl at low /i?!dvogen concentrations. However, at high hydrogen contents the entropy was the predorninatlt factor in determining the stability of the Zr-Hf-H al1o.s. This was interpreted to mean a scarcity of filrtlzer itltevslilinl solute sites caused by hydrogen-hydvogen intet-actions in the metal lattice. INTEREST in the reaction of hydrogen with metals has increased in the past few years for the following reasons: 1) the formation or use of high hydrogen potential environments in nuclear reactors; 2) the reaction of hydrogen with alloys in nuclear reactors with the accompanying deleterious effects on the mechanical and corrosion properties; 3) the theoretical implications of thermodynamic data on the theory and rules of alloy formation in the metal-hydrogen systems; 4) the use of hydrogen-containing fuels in rocket engines; 5) the need for a process of making fine metal powders of high-melting reactive metals; and 6) the beneficial impregnation of superconducting alloys with hydrogen. In nuclear pressurized-water reactors, the problem exists of limiting the hydrogen pickup of zirconium alloys which are utilized as fuel cladding, heat shields, and support members. In general, zirconium alloys have good mechanical and corrosion-resistant properties in high-temperature water. However, hydrogen is absorbed from the corrosion reaction between metal and water, greatly accelerating the formation of the corrosion product ZrOz as well as mechanically embrittling the underlying metal. In addition, recent observations1 at zirconium to hafnium welds showed that secondary elements in zirconium can have an appreciable, and somewhat unexpected, effect on hydrogen absorption. This paper lists the thermochemical data in the range 500" to 900°C for the equilibrium reaction of four high-purity Zr-Hf alloys with hydrogen. Phase boundaries and thermodynamic functions are determined while the structural data will be presented in a future paper. In general, the Zr-Hf-H system approximates the well-known, eutectoidal, Zr-H diagram2,3 with modifications introduced through the behavior of hafnium.4,5 The Hf-H system,' published while this work was in progress, provided a consistent trend with the Zr-Hf-H data. PREPARATION OF Zr-Hf ALLOYS Table I presents a complete flow chart of the preparation procedure. The zirconium and hafnium crystal bars were completely immersed in high-purity kerosene and slowly cut into thin wafers. Wafers were then cold-sheared into approximately 1-g pieces, thoroughly cleaned, weighed, and inserted into the furnace. The alloys, B-2, B-4, B-6, and B-8, were then nonconsumable arc-melted under 500 mm of purified argon. Additional purification of the argon was accomplished by melting a large titanium button each time an alloy was re-melted or a different alloy melted. Each alloy button, which weighed 25 g, was remelted four times in an approach to complete homogeneity. Material losses were less than 0.02 wt pct. Alloy buttons were alternately cold-rolled and vacuum-annealed into 10- and 20-mil sheets. Table I1 gives the composition of the four alloys used. Very little elemental segregation existed be-

Jan 1, 1965