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By R. O. Williams

A recent article by Chernock, Singer, Mueller, and Beck 1 which supports the use of the integral of I sin $ d$ for comparing fiber texture data does not settle what happens to I sin ø as ø approaches zero, where I is the diffraction intensity for poles oriented 0 deg from the fiber axis. They indicate that they believe that it should approach some constant value (that is, I increases without bound) and the fact that in reality it does not was a result of the diffraction

Jan 1, 1960

By F. D. DeVaney

Metallurgists and coal-washing engineers have used heavy liquids for years in studying the characteristics of ores and coal. By such means true separations can be made between the various specific-gravity increments in the materials examined. To use of heavy liquids has permitted determination of the possible grades of tailings and concentrates by specific-gravity methods on any particular size, and therefore the size to which the ore must be crushed to free the valuable material. The simplicity of float-and-sink separation and the high degree of efficiency attained in the laboratory are factors that commend the method for commercial concentrations.

Jan 1, 1940

By F. D. DeVaney

Metallurgists and coal-washing engineers have used heavy liquids for years in studying the characteristics of ores and coal. By such means true separations can be made between the various specific-gravity increments in the materials examined. To use of heavy liquids has permitted determination of the possible grades of tailings and concentrates by specific-gravity methods on any particular size, and therefore the size to which the ore must be crushed to free the valuable material. The simplicity of float-and-sink separation and the high degree of efficiency attained in the laboratory are factors that commend the method for commercial concentrations.

Jan 1, 1940

By Lynn B. Hales

Everywhere you turn today there are articles on artificial intelligence and the rapid emergence of expert systems. Expert systems form a class of software that has developed as a result of the large research effort to develop computers and software that think intelligently. By definition, an expert system is a computer program that contains the knowledge component of an expert skill, can offer intelligent advice and justify its line of reasoning. Expert systems can advise people on what actions to take and when, assist in the diagnosis of the physical condition of a human patient or piece of equipment, or even take actions without human guidance, as in process control applications. Expert systems can also explain the line of reasoning behind a particular piece of advice or query for information from the user. Expert systems can be used as advisors to newcomers in any field in which mastery is attained by many years of experience. They often can provide expertise more uniformly and rapidly than human experts. Expert systems can also provide a means of documenting expert knowledge and procedures and provide a common repository for a changing knowledge base. The expert system can represent the best expertise available, thought out in the absence of pressure situations. Each of these attributes or characteristics should be helpful in improving typical concentrator control systems.

Jan 1, 1987

By Edward S. Cook

For several years past, dating particularly from the days of serious "ore-dirt" complications at the Warwick furnace, I have been desirous of providing some safe, quick and easy method of relieving the tuyeres of slag, when the cinder- and iron-notches are chilled through loss of heat in the clucible or when, from dropping or jumping of stock, the molten slag is forcibly driven into the bellyand leg-pipes. Various methods were proposed, but objections of one kind or another always presented themselves, and the subject was postponed to a more convenient season. In the summer of 1887, while running on anthracite alone, 1 found the various expedients in use to be so utterly valueless, that the importance of a practicable tuyere slagging-valve impressed me more forcibly than ever. The holes left in the cast-iron jacket at one side of the bottom of the water-blocks were found to be of no value whatever. The swinging or hinged cap on the elbow of the belly-pipe, while convenient to permit the removal of lag after the belly-pipe was partially or wholly filled, could not be adapted to discharge the slag before solidifying, except at great risk to the men and loss of time just when the constant running of the engine and the keeping of blast on the furnace was of the utmost importance. By removing keys from the caps and holding them in place with props, the slag could be discharged through the tuyeres and belly-pipes, with the engine running, by knocking the props away at a given signal. This method is extremely hazardous to life and limb, and I have always hesitated to make use of it. When the furnace is in such condition as to require the adoption of some method of the kind, the stoppage of the engine, cooling the blast and the contents of the crucible, always aggravates the trouble. When the caps are blown open and the slag is discharged by removal of the props, it is necessary to stop the engine to replace them. An hour or more will elapse before this can be done, as the slag must be partly removed before the tuyeres can be approached by ordinary mortals, and the caps handled and fastened in place again. Any movement of the stock is liable to burn the workman, as he stands, securing the cap in front or at one side of the open belly-pipe.

Jan 1, 1889

By G. A. Bezuidenhout, S. Bradshaw, W. Malan

"The purpose of the study was to investigate the feasibility of SiC reduction of low-grade concentrates from Lonmin’s Rowland and Easterns operations with respect to metal fall and PGM recovery. These concentrates are rich in SiO2 and MgO with low concentrations of chalcopyrite and Cr2O3. Pd is the most abundant of the PGMs. SiC reduction of samples was conducted at 1600? with 2.5-3.5 kg SiC per 100 kg concentrate.PGM recoveries for Easterns concentrate were better than for Rowland. More than 85% of the Ir and Pd and almost 60% of the Pt were recovered with 3.5 kg SiC per 100 kg concentrate. SEM of slag samples showed little entrainment of metallic prills compared to Rowland samples. This was attributed to the relatively higher melt viscosities of the Rowland concentrate. In order to decrease slag viscosity and to enhance PGM recovery, the FeO content of the Easterns concentrate was increased with the addition of 10 kg converter slag per 100 kg concentrate. Ir and Pd recoveries were increased to about 95%, while Pt recovery was around 70%. On the basis of these results an optimum feed ratio between Easterns and Rowland concentrates and converter slag is proposed. Carbothermic reduction of the optimum charge was also compared to SiC reduction. Carbothermic reduction yielded a marginally higher metal fall; however, the calculated gas emissions and energy requirements were higher than for SiC reduction."

Jan 1, 2015

By R. del Villar, A. R. Laplante

"This article presents four grinding simulation programs, written in Applesoft BASIC. The firs t two calculate residence time distributions (RT Ds) for open and closed loops mills. The third program calculates the select ion functions from the RTD, breakage function and particle size distribution (PSD) o f the feed and discharge. Two linear regression programs are also included to calculate the breakage function. These results are used in the fourth program to simulate continuous or batch grinding kinetics.The modelling approach presented is the size discrete, time continuous matrix formulation presented by Reid (1965) from concepts originally proposed by Epstein (1948). It is at the present time the most widely accepted phenomenological model of grinding kinetics and is standard textbook material (Austin et 01., 1982; Kelly and Spottiswood, 1982, p. 152). The concepts of RTDs and tracer testing originated from chemical engineering theory and practice, and are well presented in Leven spiel (2n d Ed . 1972 , Ch. 9) .Applesoft* was chosen because it is compatible with many micro computers. It is also one of the simplest and least powerful BASIC versions. Thus it can easily be adapted to other more complex BASIC versions.Open Loop Residence Time Distributions (Program RTDOPEN)As mixing, channelling, stagnation and short-circuiting all affect slurry motion in tumbling mills, transport characteristics are very complex an d cannot be derived from fundamental principles. Fortunately , as grinding follows first order kinetics, transport characteristics for the purpose of grinding simulation ca n be represented by the RTD of the slurry phase . It is normally determined using liquid tracers, as it has been demonstrated and is commonly accepted that in industrial ball mill s, the RTD of the so lid phase is particle size independent and equal to that of the liquid phase."

Jan 1, 1985

By Gary A. Kingston

Low-cost hydroelectric energy in the Pacific Nortnwest has been an important factor in the development of a ferroalloy industry. Eleven companies, employing approximately 1,000 persons, produce about 116,000 tons (1954-58 average) annually of ferrosilicon, ferrochromium, ferromanganese, ferrophosphorus, silicomanganese, and ferronickel. About 7,500 tons (1954-58 average) of these ferroalloys is consumed in the Pacific Northwest States of Washington and Oregon; the rest is used principally in other western and mid-western markets. In 1959, the Bureau of Mines began a study to determine the current status and to evaluate the potential of the ferroalloy industry in the Pacific Northwest. The Bureau gathered information from operating alloy plants in Oregon, Washington, Idaho, and Montana; from published materials; and from consumers of ferroalloys.

Jan 1, 1962

By D H. Bell

Slab-buckle failures in coal sequences involve thin slab deformation in strata dipping parallel to the footwall, and are a consequence of both unloading and the weak nature of the thinly bedded rock mass. Methods of modelling and predicting such occurrences include: +        a conceptual model using a base friction table, +        a mathematical model using the Euler solution for column and beam bending (after Goodman, 1980), and +        computer analysis techniques such as UDEC (Universal Distinct Element Code after Cundall and Hart, 1993).   Slab-buckle failures have the potential to seriously disrupt production because of their volume and rapidity, and to endanger both equipment and personnel working on the pit floor.   In July 2004 a large slab-buckle failure occurred overnight after a new batter and bench had been formed at the Malvern Hills Opencast Mine in inland Canterbury. This involved the entire length of the pit (85m along strike) when a 2m thick intact slab with a total volume of ~3500m3 translated down dip 6.2m on the base of a thin coal seam to form a pronounced buckle at the toe. The coal measures consist of finely laminated mudrocks with multiple coal seams of varying thickness dipping ~45¦ to the southeast, and the opencast mine had been designed with footwall batters formed parallel to bedding with a vertical bench separation of 15m.   Back analysis of the Malvern Hills failure was necessary to investigate the controls on footwall instability, and for future mine design. An engineering geological model was created and samples of the slab material and failure surface were collected and tested to establish the required parameters for use in the Euler solution for column and beam bending. Back analysis using the Euler solution provided unrealistic results that overestimated the overall length of a stable slope by more than 10 times.   No further large scale slab-buckle failures have developed at the mine site, in part because of the slow rate of coal extraction, but precautionary drainage of the footwall slopes has been undertaken to improve overall batter stability. The location of the slab-buckle failure on a critically positioned pre-sheared thin coal seam with full hydrostatic head is considered the most probable cause of the July 2004 failure, rather than inherent instability of the generic bench and batter arrangement adopted. The use of a precedent-based engineering geology approach to future mine design is considered the most appropriate solution in the circumstances.

Jan 1, 2007

Design and test a high-production coal mining machine that generates less respirable dust. Background Current coal cutting systems generate excessive amounts of airborne respirable dust and fines during the mining process. Dust control technologies, including dust dilution by ventilation and suppression by water sprays, are not always able to reduce dust levels sufficiently. The U.S. Bureau of Mines (USBM) has designed a cutting system that reduces respirable dust generated by the cutting action of the drum. This cutting system, based on geometric principles developed in the 1500's, makes use of a constant depth, linear cut to remove coal at deeper cut depths and at lower rotary speeds than a conventional rotary drum. A comparison of the linear and rotary cut paths is shown in figure 1. Approach A full-scale prototype of the linear cutting concept was valuated under laboratory conditions to determine its performance relative to standard rotary drums. Results of these evaluations show production of fewer fines, or more uniform product size, a significant reduction in the amount of airborne dust, and reduced torque and power requirements (figure 2). On the basis of these results, a contract effort was undertaken by McCracken and Associates of Bristol, TN, to design a linear cutting head for underground testing.

Jan 1, 1995

By Constanza Bujes, Mark Jones, Graham Crook, Yansan Jamyanbaatar, Sedat Esen

Tracking ore characteristics such as grade and hardness from its original position into the material handling and processing stages remains one of the key challenges in open pit mining of hard rock deposits. The most efficient technique for rock fragmentation and separation of ore from waste is blasting, which induces changes in the grade distribution by displacing the in-situ ore into a diggable muck pile. Material movement defines the post-blast grade distribution, which is key to optimising the value of the ore and accounting for ore loss and dilution. Techniques to directly measure the displacement in open pit mining have been implemented routinely and have provided calibration and validation data for blast models to build upon. The JK Value-Based Ore Control blast movement model (JKVBOC) is the latest development of a series of research studies into blast movement and ore control at the Sustainable Minerals Institute of the University of Queensland. The blast model discretises the bench into blocks, defines the initial velocity of each block based on the blast design, confinement and explosive properties, and simulates the displacement using a physics engine. Calibration and validation of the model has been performed in open pit hard rock mines in Australasia in diverse confinement conditions. This paper describes the calibration and validation of the blast movement model against direct measurements of blast movement and final muck pile shape for a case study where the displacement of multiple shots was modelled for an open pit mine, with an analysis of the implications for ore loss and dilution. A key finding in this study is the need for further integration of this technology into the existing systems for ore control, and the potential for applications in tracking ore characteristics other than grade into process control.

By J. Bensabat, B. Figueiredo, A. Niemi, J. Rutqvist, C. F. Tsang

"A hydro-mechanical model was developed to study the interaction between mechanical deformation and fluid flow in the fault zones during CO2 injection and storage at the Heletz site which was chosen as a test site for CO2 injection experiments in the framework of the EU-MUSTANG project. The potential reservoir for CO2 storage at the Heletz site consists of three sand layers separated by lowpermeability shale layers. The potential consequences caused by fault reactivation, focusing on the shortterm integrity of CO2 storage, are evaluated. The difference in the results obtained by considering the three-layer as an equivalent layer storage formation is analyzed.INTRODUCTIONLarge-scale storage of CO2 in deep underground reservoirs may cause considerable pore-pressure perturbation as well as flux migration and concern has been raised over whether shear slip displacements may be induced in nearby faults, as a consequence of their reactivation. A state-of-the-art review can be found in Rutqvist (2012), which describes the various possible effects resulting from CO2 injection into a deep sedimentary basin, including those involved in reservoir stress–strain changes, micro-seismicity, caprock sealing performance, and potential fault reactivation. Moreover, several studies have recently shown how CO2 injection may produce seismic events both on major faults (i.e., large faults with large initial shear offset) (Cappa & Rutqvist, 2011a, b, 2012), and on minor faults that might have gone undetected during the site characterization, e.g., faults less than 1 km long and without detected initial offset (Mazzoldi et al., 2012).The present paper is concerned with the Heletz formation which was chosen as a test site for CO2 injection experiments in the framework of the EU-MUSTANG project. The Heletz site located at the southern Mediterranean coastal plain of Israel and the structure is an anticline fold with a crest of about 4 km by 2 km. The structure is gently dipping to the east, truncated by a pinch-out line to the west and subdivided into a number of blocks by transversal normal faults with small displacements. The water table is located at 300 m below the land surface. An areal sketch of the site with the elevation of the caprock and the location of the borehole that has been chosen for the CO2 injection experiment is presented in Figure 1."

Jan 1, 2015

By William Vietti

WEST TEXAS and New Mexico has been overshadowed by the develop-ment in East Texas to such an extent that the area has been placed on a settled production basis by most of the operators. Considerable develop-ment work on both proven and unproven acreage remains to be carried on, but the incentive, a ready and profitable market, has been lacking. The main characteristics of the fields in this area are so well known that they are not described again in this paper, which thus resolves itself into a statistical review of the more important production features of the area. Proration has been in effect during the year and has been rigorously applied with the full cooperation of all producers. Proration in West Texas and New Mexico is based in the more pro-ductive fields on a potential and acreage distrbution of the allowance to the individual wells or acreage units. Potentials are determined generally by a short production test of from 1 to 4 hr.; and the hourly rate is multiplied by 24 to obtain the 24-hr. production or rated potential of the separate wells. The potential values thus set up have been questioned by many production men who are not willing to concede that the instantaneous (hourly) capacity of a well to produce is its potential capacity for a day with all other wells in the pool producing at their capacity. However, the potential of a well determined as above remains its chief rating as a measure of the permeability in place and as an indication of the possible reserve feeding that well. , The acreage factor has made it unnecessary to overdevelop properties in order to obtain an allowance proportionate to neighbors who are willing to drill an excessive number of wells on a piece of acreage in the hopes of a quick drainage and a corresponding profit. Proration has resulted in an orderly development of many of the pools in this area on the base as out-lined above, resulting in more reasonable spacing of wells and the more even withdrawal of oil and the ensuing expectation of high recoveries.

Jan 1, 1933

By Virgil A. Marple

It was the purpose of this contract to conduct research in several different areas of instrumentation used to determine the quantity of respirable dust in the mining atmosphere. One area of research was in evaluation of instruments including several respirable dust monitors, several types of photometers, and a QCM cascade impactor. An instrument evaluation chamber was developed to aid in evaluating the instruments in a dust atmosphere. Another area of research was investigations into new instrumentation concepts, such as a virtual impactor/photometer instrument, a new optical device which can be used as either an optical particle counter or photometer, a new personal respirable sampler, which employs an impactor instead of a cyclone as a preclassifier, and the development of a new cascade impactor, which deposits the particles uniformly on the impaction plate. Another area of research included the use of many of these instruments in two field studies, including a silica sand plant and a tungsten mine.

Jan 1, 1981

By John W. Reddy

The C&NW Ore Dock at Escanaba, Michigan, is a major terminal on Lake Michigan for iron ore pellets arriving from the Marquette Iron Range located 112 km (70 miles) to the north. In an average year, the terminal handles in excess of 8 000 000 Mg (LT) of iron ore pellets consigned to a number of major steel companies. It is important to the steel companies for both cost control and operating efficiency that each cargo be sampled as accurately as possible in order to determine the physical and chemical properties of the pellets. This paper describes the equipment and operating procedures of the sampling facility and Presents some sampling data.

Jan 1, 1985

By P. R. Goad

"Kidd Creek is a large volcanogenic base metal sulphide deposit, located near the west end of the Abitibi greenstone belt, 27 km north of Timmins, Ontario. The rhyolite geology is characterized by a NNE-striking and steeply east-dipping package of rhyolite volcaniclastics upon which has been imposed a strong ESE-striking and north-dipping structural fabric . Massive rhyolite units with grey-black. chloritic cores and yellow, sericitic margins intrude as dykes into the stratigraphic footwall and as sills higher in the stratigraphy. Massive rhyolite units positioned near the top of the felsic pile exhibit an extensive marginal development of hydraulic fracturing and are termed crackle-brecciated rhyolite.The stringer sulphide zone is positioned in a lobate blanket of crackle-brecciated rhyolite at the top of the felsic pile. The stringer sulphide zone is characterized by a mature chemical alteration, being specifically depleted in alkalis and enriched in iron-rich chlorite. with accompanying silica, sericite and carbonate alteration. A suite of trace elements characterizes this mature alteration. The massive rhyolite units, which intrude lower in the rhyolite volcaniclastics, exhibit a core of weak chlorite alteration and strong marginal sericite alteration. Tight or unfractured massive rhyolite units are essentially devoid of sulphide mineralization and exhibit a suite of trace elements characteristic of this immature alteration. It is interpreted that the massive rhyolite units intruded into an already evolving system and ""choked-off"" active conduits carrying hydrothermal fluids and subsequently acquired an immature alteration signature. Rhyolite units positioned higher in the pile developed intense hydraulic fracturing and a mature alteration coincident with the formation of the stringer sulphide zone. In summary, a model, based strictly upon the rhyolite geology, is reviewed to assist in the exploration for volcanogenic base metal sulphide deposits."

Jan 1, 1985

By S. Budavari, F. M. C. C. Vieira

For several decades, the deep, gold-bearing reefs of the Witwatersrand basin have been mined predominantly according to layouts characterised by longwalls with strike pillars to provide regional support. During the past few years, a new generation of mining layouts has been introduced. These layouts are based on the concept of grid-type, scattered mining with dip pillars for regional support. As the extraction of the gold reefs extends to depths below 3500 m, the hazards associated with mining at these ultra-depths are expected to increase to unacceptable levels. Therefore, the question arises as to, which of the currently applied mining layouts is most acceptable for the economic and safe extraction of an ultra-deep orebody. The purpose of this paper is to describe a research investigation carried out to evaluate the degree of acceptability, from the rock engineering view point, of four currently used mining layouts for application at a depth-range of between 3500 and 5000 m. Pendant plusieurs décades, les filons d’or profonds du bassin du Witwatersrand ont été exploités d’une manière prédominante selon des dispositions caractérisées par des longues tailles avec des piliers directionnels pour donner un support local. Les dernières années ont vu la naissance d’une nouvelle génération de dispositions de mine. Ces dispositions sont basées sur le concept d’extraction type grille, éparpillée, avec des piliers au pendage pour le support local. Comme l’extraction des filons d’or va à des profondeurs en dessous de 3500m, il faut s’attendre à ce que les risques associés à l’exploitation à ces profondeurs extrêmes atteignent des niveaux inacceptables. Par conséquent, la question se pose de savoir laquelle des dispositions de mine couramment utilisées est la plus acceptable pour l’extraction rentable et sans danger d’un gisement ultra profond. Le but de l’étude présente est de décrire les recherches exécutées pour évaluer le degré d’acceptabilité, du point de vue d’ingénierie de roche, de quatre dispositions de mine couramment utilisées pour application à un rayon de profondeur entre 3500 et 5000m. Die tiefen, goldträchtigen Riffs des Witwatersrandbeckens wurden über einige Jahrzehnte hindurch vorwiegend nach jenen Layouts abgebaut, die von Langfrontstreben mit Schlagpfeilern charakterisiert waren, um regionale Unterstützung zu gewährleisten. Während der letzten Jahre wurde eine neue Generation von Grubenlayouts eingeführt. Diese Layouts basieren auf dem Konzept der Rasterfeld-Art, gestreuter Bergbau mit Neigungspfeilern für regionale Unterstützung. Es kann erwartet werden, daß auf Grund der Tatsache, daß sich die Extraktion der Goldriffs auf Tiefen unterhalb 3500 m verlagert, die Gefahren, die mit dem Bergbau an diesen Ultratiefen verbunden sind, sich auf ein nicht annehmbares Niveau erhöhen. Folglich erhebt sich die Frage, welche der gegenwärtig angewendete Abbaulayouts für die ökonomische und sichere Extraktion eines ultra-tiefen Erzkörpers am annehmbarsten ist. Zweck dieser Arbeit ist es, eine durchgeführte Untersuchung zu beschreiben, die vom Gesichtspunkt der Gesteinstechnik gesehen, vier gegenwärtig angewandte Abbaulayouts für den Einsatz in einem Tiefenbereich zwischen 3.500 und 5.000 m evaluiert.

Jan 1, 2003

By Dale A. Vaughan, Oliver M. Stewart, Charles M. Schwartz

A. U. Seybolt (General Electric Research Laboratory)—The authors should be commended for adding some important information to our knowledge of the solubility of interstitial elements in metals. It is becoming increasingly evident that the effect of even traces of such elements have very far-reaching effects upon the mechanical properties of the body centered cubic metals. Those who have worked in this area know that the accurate determination of the small solid solubility limits in systems of the type reported by the authors is a quite difficult task, and it is therefore not surprising that frequently the results of different workers are not in agreement. It is instructive, and usually helpful, to plot the solubility results on log weight or atomic percent -1/T coordinates to find out if a straight line is obtained. A straight line is expected because in systems displaying solubilities of the order of 1 to 3 at. pet or less, Henry's law is usually obeyed—or at least well enough obeyed so that the deviation from linearity is not very appreciable. If Henry's law is obeyed, one canthen use the Van't Hoff Equation in the form In N = ?H/RT + C, where N is mole fraction, at. pet, or wt pet for small values, and AH is the partial molal heat of solution of the solute. R and T have the usual significance, and C is an integration constant. If one plots the reported nitrogen solubility values as indicated above, the three points fall reasonably well on a straight line. The oxygen values for the two upper temperatures fall very closely to the nitrogen values as shown in the authors' Fig. 15. However, the value at 500°C departs widely from the straight line established by the data at 1500" and 1000°C. It is, of course, true that one cannot place too much emphasis on the significance of a line established by only three points, but in the absence of reasons for anticipating deviations, data exhibiting wide departures from linearity should at least be examined closely. Fig. 16 shows the log at. pct -1/T plots for the authors Ta-O and Ta-Ndata including a solid circle point at 500°C and 1.8 at. pet for Ta-O, which is simply extrapolated from the two higher temperature points. In addition, the data of R. P. Elliott9 for Nb-O are shown. These points were picked off his curve and are not very exact, but as can be seen they line up well on a straight line. It is interesting, and probably significant, that the slope of Elliott's results is not far from those of Vaughn, et al. This is probably to be expected because one would anticipate that the partial molal heats of solution of oxyten in these two very similar metals should be not too far apart. AH for Ta-O is about -1900 cal per mol, while for Nb-O it is near -2300 cal per mol. Hence, this lends some support to the thesis that the point at 500°C for Ta-O is much too high. The data of Gebhardt and Preisedanz10 are also plotted, and it is seen that their data while lying on a linear plot, have an appreciably steeper slope. The possible reasons for this will not be discussed here except to point out that their pressure-composition data show anomalies which suggest that they may have been dealing with a different equilibrium from that being discussed. There is another consideration which would also suggest that the solubility at 500°C is lower than shown. The solubility values were obtained by the classic method of first establishing a lattice parameter-composition curve. This the authors did, and there is probably little doubt that it is quite accurate. Such a plot is generally almost error-free because it has a self-correcting feature in that any deviation from linearity makes a data point immediately suspect, and subject to confirmation. Unfortunately, this is not true with respect to the actual solubility values. These are obtained ordinarily by taking an alloy containing more solute than is soluble at some temperature and then thermally

Jan 1, 1962

By R. Bakish, M. A. Badiali, N. W. Kirshenbaum

One pound of ultra pul-e molybdenum has been produced containing both metallic and nonmetallic impuvities close to or less than the limits of detection. various purification methods were investigated; althouglz the use of move than one purification step was consideved, it was found that a single, caefully-controlled sublimation of MoCl5 yielded a highly puvified product without prior treatment or recourse to repeated sublimation. Hydrogen reduction of MoC1, to metal was attempted at atmospheric pressure; however, reduced pressure was necessary to obtain substantial yields. The tubular deposits of metal were consolidated into bulk fovm by electron beam melting undev high vacuum yielding a very low gas content. Boblems involved in monitoring the puvity of these materials and analytical results obtained are also presented. THE pronounced effect of even trace amounts of impurities upon fundamental properties of materials is well known to metallurgists and solid-state physicists. Consequently, groups interested in basic studies of metals have in recent years immensely stimulated the preparation and production of numerous ultra-pure metals. Increased demand by scientists for these high purity materials has necessitated development of facilities to prepare them in significant quantities; the procedures reported here were devised to produce significant quantities of ultra-pure molybdenum. Previous work performed in the field of vapor phase purification and hydrogen reduction of several other refractory metal chlorides had demonstrated valuable techniques applicable to molybdenum.' Various purification and reduction steps were individually investigated. Those procedures which showed the most favorable results with respect both to attainment of high purity and to ease of operation were then incorporated in the process utilized to produce the metal.' STARTING MATERIALS It is well known that because of differences in volatility, chlorides may be separated by fractional distillation. It was presumed that distillation of molybdenum pentachloride offered a simple and straightforward method of purification due to its relatively low boiling point. Alternatively, sublimation of the solid chloride also appeared feasible since MoC15 has both a reasonably narrow temperature range in which it exists as a liquid (a property typical of refractory metal chlorides) and a low enthalpy of sublimation. Pertinent thermochemical data of MoC15 are given in Table I. It should be noted that this compound must be handled with care as it is extremely hygroscopic. Anhydrous MoC15 was obtained from the A Metal Climax Co. METHODS OF PURIFYING MOLYBDENUM PENTACHLORIDE Distillation. It was expected that distillation methods, while affording an efficient purification, would prove simple to control and would have a higher production rate than sublimation processes. Also considered was the possibility of effecting a high degree of purification by using both these volatilization methods in conjunction—possibly a distillation followed by sublimation of the solidified condensate. Distillation of MoC15 was investigated using a single stage distillation column packed with chemically resistant glass beads. Heating coils were wound around the column and collection tube (condenser). As-received MoCl5 was charged into a flask connected with the column using a side loading arm under an argon flow. After the column and condenser were brought to about 270" and 210°C, respectively, the apparatus was lowered until the flask was fully immersed in a constant temperature fused salt bath maintained at about 285 °C. Distillation was continued for about 10 or 15 min until 50 to 70 g of distillate had been collected. Analyses of these distillations indicated that several elements, e.g., Cu, Fe, Ni, Cr, and Mg, were lowered in quantity although not all were removed to the same extent. The occurrence of Na, B, Si, and A1 in the distillates appeared to be due to contamination, possibly from corrosion of the pyrex glass. An improved distillation system of larger capacity and longer distilling column was built. Improvements were effected in lowering the amounts of such impurities as B, Mn, Ni, Na, Mg, Cr, Cu, and Fe. These studies were pursued concomitantly with efforts to purify by sublimation; it was subsequently found that although improvements in purity were obtained by distillation, sublimation processes were simpler to control and effected a high degree of purity.

Jan 1, 1963

By William D. Klopp

A study was conducted of the tensile and creep properties of are-melted and electron-beam-melted tungsten over the temperature range 2250° to 4140°F. The tensile and creep strengths vary with pain size, the finer -grained materials being stronger. The activation energy for transient creep at 2250° to 3500°F is 95,000 cal per (g)(mole), while that for steady creep at 3300o to 4000°F is 141,000 cal per (g)(mole). At 2875o to 3300°F the apparent activation energy for steady creep decreased with decreasing temperature. It is suggested that cross slip is rate controlling during transient creep, while dislocation climb is rate controlling during steady creep above 3300° F. ALTHOUGH considerable data have been generated on the high-temperature tensile properties of powder-metallurgy tungsten,1 relative few data have been published on the properties of are-melted2 or electron-beam melted tungsten.3 Furthermore, the available data show a fairly large amount of scatter at high temperatures. The effects of structure and purity have not yet been defined, aside from observations that high-purity electron-beam (EB)-melted tungsten3 and single-crystal-plasma-flame tungsten4 are weaker than less pure powder-metallurgy tungsten. The creep behavior of powder-metallurgy tungsten has been studied, but no data are available on the creep behavior of tungsten consolidated by melting. Green5 found that powder-metallurgy tungsten exhibited linear creep at 4082° to 5072°F with an activation energy of 160,000 cal per (g) (mole). The similarity of this activation energy to that of 153,000 cal per (g)(mole) for volume self-diffusion6 suggests that recovery of strain hardening by dislocation climb is rate controlling in this temperature range. In studies at 4800°F, Sutherland and Klopp7 concluded that grain size significantly affected the creep behavior of commercial powder-metallurgy materials. This grain-size effect was suggested by sherby,8 although the opposite relation had been reported for aluminum.' The purpose of the present study was twofold: first, to provide baseline data on high-temperature tensile and creep properties of are-melted and EB-melted tungsten for concurrent tungsten alloy studies, and, second, to determine the phenomenolo-gical effects of structural and purity variables on the high - temperature mechanical properties of tungsten. EXPERIMENTAL The are-melted tungsten materials were prepared by melting sintered 1-1/4-in.-diam electrodes into 2-1/2-in.-diam by 5-in.-long ingots. The are-melting facility has been described previously.' Eight ingots were melted, machined, and hot-extruded at

Jan 1, 1965