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By John J. Reed

The mines of southeast Missouri's Lead Belt have been in operation since 1864, almost 100 years. During this period about 10 pct of the total ore available has been left in place as pillars, and this now represents the best ore reserve left to the older mines. St. Joseph Lead Co. has been investigating various plans of pillar recovery for several years. The example to be described is only one possible approach under a specific set of conditions. Conditions vary greatly in the different areas within the Lead Belt, and the same approach would be entirely in- adequate in certain other areas, but there are important sections where this system is clearly applicable.

Jan 7, 1959

By Fred C. Bond

IN crushing and grinding the larger particles are more exposed to the work input. They absorb most of the work and protect the smaller neighboring particles from destructive contact with the crushing surfaces or grinding media. The importance of this exposure differential upon the reduction efficiency and product size distribution has long been recognized. Unfortunately, there has heretofore been no direct method of evaluating it, and such indirect methods as observing the slope of the plotted product size distribution line have been used as an indication. In this presentation the Third Theory of Comminution1 has been used, together with the exponential formula for size distribution, to evaluate the exposure ratio and exposure constant and to illustrate examples of their utility in crushing and grinding applications.

Jan 12, 1957

By Thomas Fraser

BECAUSE of the present interest in the subject of sulfur in coal and its removal, such information as is available in the coal-washing literature on the various factors that determine the adaptability of a coal for wash- FIG. I.-COAL-WASHING TABLES OF ONE-FOURTH COMMERCIAL SIZE. ing have been collected and are presented here together with some observations based on results of experimental work carried out in the coal-washing laboratory of the mining department of the University of Illinois, and investigative work at Illinois washeries in connection with the work on reduction of the sulfur content of coal, being carried on at the Urbana Station of the.U. S. Bureau of mines. This investigative

Jan 9, 1919

By R. Hadfield

Since the writer has been intimately connected with the development of manganese steel for many yearsm some remarks upon the early work wutg regard to the rolling and forging of the material might be of interest…

Jan 1, 1915

By Thomas Fraser

Because of the present interest in the subject of sulfur in coal and its removal, such information as is available in the coal-washing literature on the various factors that determine the adaptability of a coal for wash- ing have been collected and are presented here together with some observations based on results of experimental work carried out in the coal-washing laboratory of the mining department of the University of Illinois, and investigative work at Illinois nrasheries in connection with the work on reduction of the sulfur content of coal, being carried on at the Urbana Station of the U. S. Bureau of Mines. This investigative

Jan 1, 1920

This is a brief account of the history of unit operation in the Salt Creek field, Wyoming, from the time of the agreement to prorate production in March, 1921, to the present. An attempt has been made to evaluate the savings in development and production costs resulting from the unit plans adopted. Summarized, these savings have amounted to $11,650,000. No effort has been made to estimate any increase in ultimate recovery, for it is believed that unit operation can be justified on saving in development and production costs alone. It would require nearly 20,000,000 barrels of additional oil to be produced in order to return the amount saved by not drilling unnecessary wells. Four horizons are affected by unit or near-unit programs, as follows: The principal operator is under contract with six companies to operate 10,400 acres. This includes all of the productive area of the First Wall

Jan 1, 1930

By K. E. Niermeyer, J. A. Bratt, B. A. Fahm, B. A. Kennedy

The instrumentation, monitoring, and prediction of a major slope failure at the Chuquicamata mine are described. In December 1967, preexisting tension cracks on the south end of the east wall of the mine began to open. Various forms of instru¬mentation were installed for continuous monitoring. These systems included tension crack stakes, crack extensometers, linear extensometers, tape and transit lines, sliding wire contacts, and a seismograph. From the information obtained, the failure date was accurately predicted some five weeks before failure, enabling the mine to reroute truck and rail access; hence, causing a minimal mine shutdown of 21/2 days and preventing any injuries to person or damage to equipment. The shape and form of the sliding mass are analyzed, as are possible modes of failure.

Jan 1, 1972

By R. B. Sudderth

The recovery of copper by various combinations of processes centered around liquid ion exchange has certainly been accepted as a technically superior entity when compared to the widely applied classical method of cementation. While the technical aspect of liquid ion exchange processes has received much attention and acclaim through actual operating data, in particular the ease of handling solutions, percentage recovery, reduction of pollution, etc., the corresponding economic data has either gone unpublished or has been held confidential. Much of this economic data has now been made available for publication; and with this data, we at General Mills Chemicals, Inc., will attempt to present an accurate economic analysis of some liquid ion exchange plants and an economic comparison between these plants and the typical cementation facility.

Jan 1, 1974

By Vito J. Colangelo

The primary object of this study was to determine the effect of ferrite and its orientation upon the mechanical properties of a precipitation -hardening stainless steel with particular attention to the short-transverse properties. The investigation consisted of Jour major parts : the preliminary investigation of billet properties, the effect of forging reduction and ferrite content upon mechanical properties, the effect of notch orientation upon impact strength, and the relationship of heat composition to ferrite content. Low ductility and impact strength in the short transverse direction were found to he associated with the orientation and shape of- the ferrite plates. It was also determined that impact strength varied with notch orientation. The test values obtained with the notch perpendicular to the plane of the ferrite plate were lower than those obtained in the notch-parallel condition. The over-all investigation showed that high ferrite contents in general had a deleterious effect upon mechanical properties and that the ferrite content could he minimized by exercising rigorous control of the heat composition. A careful balance of elements, nitrogen in particular, must he maintained in order to reduce the formation of ferrite. THE precipitation-hardening stainless steels were developed to fulfill a need for high-strength corrosion-resistant alloys. In the annealed condition they are soft and ductile and possess many of the desirable characteristics of the austenitic stainless steels. In the hardened condition, the alloys exhibit the high strength and hardness of the martensitic stainless steels. The alloy under consideration in this investigation has a nominal composition as follows: C Mn Si Cr Ni Mo N 0.13 0.95 0.25 15.50 4.30 2.75 0.10 The hardening mechanism is identical to that of other hardenable steels in that it depends upon the transformation of austenite to martensite. This alloy because of its annealed structure and its ability to be hardened combines the desirable forming and corrosion properties of the austenitic grades with the high hardness and strength levels attainable with the hardenable grades. The reason for this apparent duplicity of proper- ties can be explained by considering a basic metallurgical difference between the hardenable stainless steels and those of the austenitic group. Both types are austenitic at 1800°F but, while the martensitic grades transform to martensite upon rapid cooling to room temperature, the austenitic grades remain austenitic even when cooled to temperatures below room temperature. The major difference then is in the degree of austenite stability. This stability can quantitatively be described by the Ms temperature. The Ms is defined as that temperature at which austenite begins to transform to martensite. The austenitic grades for example may be cooled to -300°F without producing significant quantities of martensite. The hardenable stainless steels on the other hand have an Ms temperature in the vicinity of 400" to 700°F. In cooling to room temperature, these alloys traverse the entire Ms-Mf range and show almost complete transformation to martensite. The semiaustenitic stainless steel, however, occupies an intermediate position with respect to its austenite stability. The analysis is so balanced that the Ills temperature lies at or slightly above room temperature. The resulting alloy retains much of its austenite at room temperature and yet responds to hardening heat treatments. Achieving this delicate balance of elements is therefore of great importance. Slight imbalances of the equivalent Cr-Ni ratios frequently result in the presence of 6 ferrite. It is the effects of this ferrit with which we are concerned, more specifically the effect of the quantity and ferrite orientation upon mechanical properties, particularly ductility. PROCEDURE A) Preliminary Investigation of Billet and Forging Properties. In order to determine the effect of ferrite on billet properties, billet stock from three heats with various ferrite contents was utilized. Tensile specimens were obtained in the transverse and longitudinal directions from this material and heat-treated as shown in Tables I and 11. Forgings were made from these same heats, the purpose being to determine what effect, if any, the ferrite might have upon the mechanical properties. These forgings were made in such a manner as to elongate the ferrite in the longitudinal and transverse directions. The method of forging was as follows. A section was cut from a 6-in.-sq billet of Heat A and flat-forged to 1-1/2 in. thick. Working was done from one direction only with no edging passes as shown

Jan 1, 1965

By R. R. Klimpel Discussion by C. C. Harris, L. G. Austin

C. C. Harris (Columbia University) — The authors ' have presented relationships for the random division of a magnitude into r + l parts taking account of the order of selection. Interpreting their model in comminution terms, their Eqs. 7, 9 and 11 refer to the one-dimensional case; that is, to the subdivision of a long thin rod at random. It is assumed that the fragments may be indefinitely small. Real materials, however, are limited in the degree of subdivision which can be attained through the intervention of practical restrictions. One in fine grinding is the depletion of microflaws as material becomes finer. Another is the

Jan 1, 1969

By Howard M. Wells

The investment worth of a mineral deposit can only be realistically evaluated in relation to specified engineering design criteria which fully detail the proposed method of exploitation. The operational design of a mine falls essentially within the technical discipline of the mining engineer, under the constraint that the technical design should be aimed at optimizing the financial attractiveness of the project. In the case of a marginally viable proposition it becomes vitally necessary to identify the best set of design parameters which together will add up to an optimum investment proposal. This paper examines some fundamental logic of optimization for a "wasting asset" type of investment such as a mine, with special reference to the rate of annual production and the strategy of selective mining.

Jan 1, 1979

By R. E. Collom

VARIOUS chapters already written in the history of development of the North Dome of Kettleman Hills are monotonously identical in the one underlying theme of conservation of oil and gas. Discovered on Oct. 4, 1928, by Milham Exploration Co. with its wildcat Elliot No. 1, the field has been subjected to practically every modern form of produc-tion restraint in the name of conservation. The record thus far developed shows that conservation was had for a time, at a price; and that unitiza-tion must he blessed by single ownership or 100 per cent participation to be effective. In fact, incomplete unitization places a heavy handicap upon its participants in the competitive development that follows.

Jan 1, 1937

By Andres M. Liebenthal, Jan M. Mutmansky

This paper is concerned with the layout of a conveyor and beneficiation plant system involving several mines and a single point of delivery. The objective of the procedure is to locate the conveyor lines and beneficiation plants in an optimal manner considering the economics of scale inherent in both the transportation and beneficiation processes. Upon completion of the mining plan, the layout of the conveyor network is achieved through the principle of Steiner minimal trees. The optimal number and location of beneficiation plants for this layout are then determined using a sequential economic analysis based upon the flow of material from the individual sources to the ultimate destination. The practical aspects of the method and the advantages and disadvantages of its use are discussed to link the model to a practical problem.

Jan 1, 1976

By E. P. Pfleider

IT is generally believed that the amount of diamond drilling will increase appreciably in the next decade, as the search for minerals throughout the world becomes more difficult and intense. An attendant problem may be one of short diamond supply, resulting in higher bit and drilling cost. With this background, the U. S. Bureau of Mines1 and the School of Mines at the University of Minnesota2 have established comprehensive research programs in diamond drilling. One of the several aims is the design of a more efficient bit, which would lower diamond consumption and increase rate of advance, both essential in reducing drilling costs.

Jan 2, 1953

By Rudolph G. Wuerker

Charles T. Holland (Head, Dept. of Mining Engineeri*, Virginia Polytechnical Inst., Blacksburg, Va.) Mr. Wuerker has presented a very interesting discussion of the use of triaxial test methods for investigating the strength properties of rocks. Such methods, no doubt, eventually will develop considerable information of interest to those concerned with the design of mine layouts, particularly in the field of pillar design. From his discussion of my recent article, "Cause and Occurrence of Coal Mine Bumps" (Holland Mining Engineering 1958, p. 933-1002), it is evident that in one place at least I did not make my meaning clear to him and perhaps others. To clear the matter up I think it best to quote from the article, somewhat more fully than did Mr. Wuerker, as follows: "4) In actual operations — because rocksare not perfectly elastic, homogeneous, nor isotropic and because local yield does occur — the maximum stress as demonstrated by Phillips (Ref. 22, pp. 64, 65) and indicated by much experience in mining, does not occur at the walls of the opening but at a short distance inside the pillar. Furthermore, the maximum stress does not reach as great a value as theoretical considerations and laboratory experimental methods indicate.* Actual distance inside the pillar, measured from the wall, at which the maximum stress exists, has not been determined. Observations in many mines, however, indicate that this distance could have a mini-value of one to six or eight times the bed thickness and that it is probably affected by width and height of the opening, depth of cover, and relative values of the elasticity and plasticity of materials comprising the roof, floor, and coal seam. The actual value of the stress produced probably lies between the theoretical maximum and the average stress concentration that would be produced if the weight of the strata above the unsupported opening were evenly distributed over the pillars for a distance equal to the opening width." The footnote reference in the above quotation referred to the following: "*For example, the Pocahontas No. 4 coal bed in southern West Virginia is mined under cover up to 1800 ft thick. Development openings are driven 18 to 20 ft wide, and the bed is about 6 ft thick. According to the work of Panek, the tangential wall stress at mid-bed height under these conditions would reach values between 4000 and 5000 psi. Actual tests of 3-in. cubes of this coal show its compressive strength would be much less than this, perhaps as low as 400 psi. Yet the pillars usually show no evidence of failure in these headings. In this same bed at a depth of 800 ft, the author has seen an opening 225 ft between supports lying between two old groves approximately 1100 ft apart. According to the theoretical considerations, the stress in the pillar walls would have been about 18,000 psi, yet the pillar showed little or no evidence of weight. In view of these observations, it is clear that the wall stress does not attain the maximum values indicated by theory." (Underlining added to original wording.) By referring to Fig. 2A of my paper it will be noted that theoretically the maximum pillar stress would occur at the pillar wall, i.e., at the passageway surface of the pillar. Obviously this cannot be correct in the cases of stress ranging from 4000 to 18000 psi since the coal at the surface of the pillar is under no constraint and cannot have a strength much greater than 400 or 500 psi. Hence, my conclusion that the maximum stress does not occur at the wall but back in the pillar some distance from the wall. Since these stresses are pushed back in the pillar from the wall, it is also obvious that the loads transferred to the pillar from the opening will be spread over a greater area and hence Pillar stresses will not rise to the values postulated by theory and photoelastic experiment. Further since to visual inspection the coal along the pillar wall did not appear to be failed the conclusion was reached that the stress shift was caused by local elastic or plastic yield and by difference in the elastic modulus of the rocks composing the mine floor, mine roof, and coal bed. Later on under the heading "Strength of Mine Pillars" (pages 1000-1002) the effects of constraint is briefly described. Also a formula taking into account constraint is developed relating pillar strength to the uniaxial strength of coal and the L/T ratio of the pillar. Since my paper was written, reports of experiments conducted in South Africa (Denkhaus, et. al., 1959), in Sweden (Hast 19581, and in Canada (McInnes, et.al., 1959) reveal that the conclusion expressed relative to the existence of a low stress area existing around the edges of pillars and solid faces as described above is generally correct. But it seems possible that where the wall stress developed is less than the unconfined strength of the rock composing the pillar and where the roof, floor, and pillar

Jan 1, 1961

By M. J. Spendlove, H. W. St. Clair

The problem frequently arises, particularly in refining metals or smelting scrap metals, of separating metals in the metallie state. Many metals may be separated by taking advantage of their difference in vapor pressure. Such separations can be made at atmospheric pressure, but the separations are much more selective and can be carried out at considerably lower temperatures if the distillation is done at pressures of a few millimeters or less in an evacuated enclosure. Until recently, this has not been considered feasible as a metallurgical operation, but the recent improvemcnts that have been made in vacuum technology have broadened the applicability of vacuum processes and have prompted re-examination of low-pressurc distillation of metals as a practicable process. The distillation of zinc from lead is one separation that has already been reduced to practice.l This paper is the first of a series of studies being made on separation of nonferrous metals by distillation at low pressures. Although these experiments were confined to the separation of zinc from aluminum, the significance of the results is by no means confined to these two metals. The purpose has been to investigate a metallurgical technique rather than merely to devise a means of separating specific metals. The experimental work on distillation of zinc from zine-aluminum alloys at reduced pressure grew out of earlier work on distillation at atmospheric pressure.2 The earlier work indicated that it would not be practicable to decrease the zinc in the alloy much below 10 pct owing to the high temperature required. Therefore attention was turned to distillation ah low pressures, at which lower temperatures are required. After preliminary tests were made in a small, evacuated tube furnace, a larger furnace having a capacity of 100 to 150 Ib of metal per charge was constructed. Distillation tests were first made on pure zinc and then on aluminum-zinc alloys of various composition. Particular attention was given to the limit to which zinc could be reduced in the residual metal. Data were also taken on the rate of evaporation, and heat balances were made for both the crucible and the condenser. Distillation Furnace The vacuum-distillation unit is illustrated schematically in Fig 1. The major components are the induction furnace, the condenser, the vacuum system, and the power-conversion unit. Power is supplied to the induction furnace from a 50-kw 3000-cycle motor-driven alternator. The pressure in the furnace is reduced by a vacuum pump having a nominal pumping speed of 10 liters per sec. When in operation, the metal vapors travel upward from the furnace to the water-cooled condenser where they are collected in amounts of 50 to 100 lb. The condenser is removed with aid of an electric hoist. When the system is under vacuum, the condenser is made self-sealing by a rubber gasket between the smooth-faced, water-cooled flanges at the top of the furnace and the bottom of the condenser. The pressure of the atmosphere is more than sufficient to insure sealing. At the conclusion of an experiment, the residual metal can be removed from the furnace by removing the condenser and tilting the furnace with the electric hoist. The metal was cast into the molds carried on a mold truck. A photograph of the furnace and auxiliary equipment is shown in Fig 2. The details of the vacuum furnace are illustrated in Fig 3. The furnace proper is made vacuum-tight with rubber gaskets placed at each end of a fused quartz cylinder. A clamping plate at the bottom and a ring at the top are made to squeeze the rubber between the metal and the end of the quartz tube. A large graphite crucible placed inside the quartz cylinder is thermally insulated and physically supported by refractory insulating bricks. A thermocouple in a quartz protection tube is located at the bottom of the crucible: the leads pass through a rubber seal in the bottom plate. The supporting structure for the furnace is an angle iron frame with transite board sides. The condenser is made in the form of a water jacketed cylinder with an opening to the vacuum line at the top. The bottom has a projecting skirt inside the machined flange to provide additional cooling for the rubber gasket. Condenser sleeves are made in the form of two semicylindrical pieces of sheet metal that fit snugly inside the cooling jacket. The split sleeve facilitates removal of the condensate. Measurement of Temperatare and Pressure The metal temperature was measured by a platinum-platinilm rhodium thermocouple inserted in a well extending up into the bottom of the graphite crucible. During rapid evaporation there is a wide difference in temperature between the surface and the main body of metal in the crucible because of the large amount of heat that must be conducted to the surface to supply the heat of evaporation. The heat of

Jan 1, 1950

By H. H. Kaveler, Z. Z. Hunter

Variation of the horizontal permeability (parallel to the bedding plane) in the vertical section of reservoir rocks has long been observed as a characteristic of a normally heterogeneous system which reservoir rock represent. The use of a recently developed water injection profile device offered opportunity to measure with a high degree of reliability the rate of inflow of water into Burbank sandstone in wells previously cored. Water injection profiles were not correlative with core permeability profiles in such wells. Apparently the vertical permeability substantially influences the flow between strata in a formation in a manner as to void the usual conclusions that have been drawn from consideration of the horizontal permeability measurements alone. The results obtained in comparing water injection profiles with horizontal permeability profiles suggest that many of the usual production operations based upon "selective" behavior or treatment of rock exposed in well bores need to he re-valuated and re-examined. INTRODUCTION Petroleum reservoir rock are heterogeneous systems. Heterogeneity exists in respect to lithologic character insofar as such rock are composed of distinguishable solid phases. Heterogeneity also exists in respect to certain properties, such as porosity and permeability, that vary due to variation of the physi-cal structure of the rock. Except in exceptional cases, both the horizontal permeability (measured parallel to the bedding planes) and the vertical permeability (measured perpendirularly to the bedding planes) exhibit significant variation in any common source of supply. The variation in horizontal permeability. as reflected by con. analyses. has drawn the greatest attention of petroleum technologists probably out of the general notion that the mass movement of fluids in a reservoir is predimonantly in the horizontal direction. Furthermore, in the usual case, the rock permeability measured in the horizontal direction is greater than that in the vertical. The variation of horizontal permeability of reservoir rock has been the basis for developing a number of operating practices and procedures intended to improve the petroleum production operation. Many such procedures are referred to as "selective" in the sense that the practice is intended to control the flow to a more. or less. permeable interval within the common source of Supply. It is often said that such practices are "tailored" to the permeability profile. The practices referred to involve, among others, the following: selective perforation of casing; selective shooting, acidizing and plugging: plugging back to intervals of low permeability; and, regulation of flow to prevent coning of water or gas, or irregular encroachment of water or gas. Certain expressed notions involving a concept of "by-passing," or "trappingl" that are held to be particularly harmful in causing the avoidable loss of recoverable petroleum have grown from observed variations in the horizontal permeability. Oftentimes estimates of the reserve of a common source of supply are tempered by conclusions relating variation in horizontal permeability to recover-ability of the oil-in-place. Certain conclusions attributed to the significance of the variation of the horizontal Permeabilitv often extend to the design and operation of pressure-maintenance projects involving both water flooding and gas-injection. Many advocate increasing the number of injection wells, advocate maintaining uniform and equidistant input-output well patterns, or advocate so-called "dispersed" gas-drive techniques rather than gas-cap injection because the permeability profile of cored wells is supposed to indicate that "by-passing" or "trapping" would otherwise exist. It is important, therefore, to have an opportunity to test whether the variation in the horizontal permeability found through core analyses of a typical reservoir rock is sufficient to establish the paths of fluid flow in a reservoir. It is particularly important to have an opportunity to determine whether flow at the sand face of a well conforms to the permeability profile as established by core analyses. In that manner, the merit of certain 50-called "selective" operating procedures and other notions may be evaluated. The purpose of this paper is to compare horizontal permeability profiles of wells in the Bartlesville (Bur-bank) sandstone with water injection profiles, for the purpose of showing that there is no correlation between the horizontal permeability of a core and the water intake characteristics of a typical sandstone. GENERAL CHARACTERISTICS OF BARTLESVILLE (BURBANK) SANDSTONE The Bartlesville sandstones of Northeastern Oklahoma are off-shore bar deposits.' Although other reservoirs had different processes associated with their deposition or with the formation of their porous, permeable structure, the l!artlesville sandstones on which these field Fields were made are, in every respect. typical petroleum reservoir rock. The permeability of the Bartlesville sandstones shows a typical variation in both the horizontal and vertical direction. Furthermore, the permeability profile logs of wells in any pool are not correlative, even as between wells as close as 660 ft and 330 ft apart.'. The same condition exists in such sand-tones as the Jones Sand at Shuler' and is the ordinary and usual characteristic of reservoir rock. THE FIELD DATA The data reported herein are those obtained from coring of nine wells on the center of ten-acre locations for the purpose of providing water-injection wells in the Bartlesville (Burbank)

Jan 1, 1952

By Steven T. Mitchell

The introduction of Vertical Crater Retreat (VCR) Stoping at the Homestake Mine in Lead, SD, constitutes a major advance in Homestake Mining Company's efforts to improve productivity and reduce costs through under- ground mine mechanization. The work to date indicates that Vertical Crater Retreat Stoping is one of the safest methods of underground hardrock mining today, and is competitive with all other forms of stoping in terms of cost and productivity. Homestake anticipates that VCR stoping will account for approximately 35% of the total mine production in 1981.

Jan 1, 1981

By R. S. Schechter, T. R. Guilinger, P. Bobeck, J. G. Price, L. W. Lake

This paper presents the results of an experimental study on the rate of uranium and molybdenum extraction from a flow reactor. Specific variables tested are fluid throughput and flow rate, lixiviant cation, and injected pH and carbonate concentration. The ore tested was from the Felder mine in southern Texas. It contained substantial quantities of marcasite and molybdenum disulfide that competed with the uranium ore for oxidant. Flow studies showed the oxidation of molybdenum disulfide under field conditions is mass transfer controlled, whereas the uranium oxidation is limited by surface reaction rate. The rate of uranium oxidation decreased with decreasing pH. The total carbonate levels, on the other hand, were unimportant. Ammonium carbonate appears to greatly decrease, if not completely halt, the reaction of marcasite with the oxygen. This effect was not found using either sodium or potassium carbonate.

Jan 1, 1986

By J. Alfred Berger, O. M. Katz

Selected samples of hydrided Zr-Hf alloys were rapidly quenched to voom temperature and exrtrnined metallographically, by X-ray diffraction, and through micro hardness studies to confirm high-temperutuve data Confirming experiments sllowed that there were five phases in this Lernary system: 1) hextrgonal with lattice parameters similar to that of the initia1 Zr-Hf alloy but slightly enlarged due to dissolved hydrogen; 2) fee with properties of a brittle, intermediate, hydride compound; 3) fct with c/a crvoltnd 1.07 and which appeared as a neetilelike precipitale; 4) hexagonal, designated ?, with c/a ratio of 2.37; and 5) orthorhombic, designated X, with a = 4.67, b = 4.49, and c = 5.093 and whose tnicro-st?ruct~ival nppetrl-nnce depcncled o/i, heat lvecrt~r~ent. The tetragonrrl phase never crppeal-erl witkorct the cubic hydricle. Abpecrrtrnce of 0 and A also tlependet on the hafnium content of the zirconium. A previous paper' on the Zr-Hf-H system described the thermochemical data obtained with a high-vacuum, high-sensitivity mirrogravimetric apparatus. This data presented a fairly complete picture of the phase relationships at elevated temperatures. However, it could not establish the actual crystal structures, lattice parameters, or metallographic disposition of the hydride phases. The present complementary study utilizes X-ray powder patterns along with light and electron microscopy to characterize completely the five hydrided phases found in Zr-Hf-H alloys quenched to room temperature. Crystallographic features of the zr-Hf,2,4 zr-H,5-7 and Hf-H8 systems have been summarized in Table I. Designations of a, ß, and ? were retained in the Zr-Hf-H system for the phase regions through which the pressure-composition isotherms always sloped. However, it was not firmly agreed that these were single-phase regions.' In fact, the region designated y always contained a cubic as well as a tetragonal phase after quenching to -196°C. MATERIALS Preparation of the high-purity Zr-Hf alloys has been described.' The four zirconium alloys which were hydrided contained 37 wt pct Hf (23 at. pct), 51 wt pct Hf (37 at. pct), 73 wt pct Hf (58 at. pct), and 91 wt pct Hf (82 at. pct), respectively. These were designated B-2, B-4, B-6, and B-8. Photomicrographs of the initial alloys showed the material to be quite clean as would be expected from the precautions exercised in producing them. However, there were a number of annealing twins but no other subgrain structure. In addition to the four original alloys, fifteen hydrided samples were observed at room temperature. Hydrogen compositions are given at the top of Tables I1 to V. APPARATUS The phases present at elevated temperatures were studied by quenching hydrided samples to room temperature by two different methods, both under vacuum: 1) fast cooling of the sample tubes of the microgravimetric apparatus1'9 with flowing air and 2) rapid quenching into liquid nitrogen. The cooling rate for 1) was 750° to 250°C in 30 sec. Since the microbalance chamber was not designed to permit very rapid cooling of a hydride sample, all liquid-nitrogen quenching was done in an auxiliary experiment. The auxiliary quenching apparatus consisted of a small-bore, high-temperature furnace, a sealed SiO2 tube containing the sample, and a dewar quenching flask filled with liquid nitrogen. The hydrided sample, previously quenched in the microgravimetric reaction chamber, was placed in a platinum boat in a vacuum-degassed SiO2 tube. A zirconium wire getter and degassed SiO2 rod, to reduce the internal volume, were also in the tube. After sealing the tube under vacuum the zirconium getter was heated to absorb the last traces of gas. Only the sample was heated at the reaction temperature for the desired length of time, and then the tube dropped through the opposite end of the furnace into the dewar. A quenching rate of 200" to 400° C per sec was estimated. Analyses of samples after the auxiliary experiment also showed practically no increase in oxygen or nitrogen content from heating in the SiO2 tube. All of the samples were examined at room temperature by the X-ray powder method. The majority of the powder patterns were obtained with double nickel-filtered CuKa radiation after 8- and 16-hr exposures in an 11.48-cm-diam camera. Cobalt and chromium radiation were also used to spread out the high d value end of the Pattern. Such patterns readily identified the minor phases. NO oxide or nitride lines were found. Where sharp back-reflection lines existed it was possible to reduce the

Jan 1, 1965