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By Donald E. Meyer

High current-low voltage EB-gun evaporation in an oil-free ultra-high vacuum system was found to be necessary, though not sufficient, for stability (300°C, 106 v per on) of aluminium gate MOSFET's and MOS capacitors not stabilized by a phosphorous glaze. five characteristics of the equipment used: 1) Vacuum purification of the aluminum charge, 2) Ionization of the evaporant by the electron beam, 3) X-ray formation, 4) Residual gases during evaporation, and 5) Metal film structure were studied as Possibly significant in MOS fabrication. EVAPORATION of contact metals common to the semiconductor industry historically has been accomplished with oil diffusion pump systems and various resistance heated evaporant sources as dictated by the type of metal evaporated. To meet a need for greater reliability of semiconductor devices, other metallization methods were developed. A good example would be application of the moly-gold contact system to integrated circuits with deposition by RF or triode sputtering.' More recently, fabrication of stable metal-oxide-silicon devices and circuits has put new demands on metallization. The purity of the thin metal films composing MOS structures is critical, particularly at the metal-oxide interface, and ultra-high vacuum metallization using sputter-ion pumping and electron beam gun (EB-gun) evaporation are well suited for the task. At this laboratory aluminum has been the most common contact-gate metal for both MOS capacitors and MOSFET's. In the earliest work with MOS capacitors, aluminum was evaporated from wetted tungsten filaments using both diffusion pump and ion pump vacuum systems. In spite of clean oxide techniques these capacitors were unstable under bias-tempera-ture stressing. Only after a switch to EB evaporation of aluminum were stable capacitors produced. Using the same techniques it was possible to make MOSFET's with equivalent stability. Stability data for a discrete MOSFET is shown in Fig. 1. This is a "clean" oxide gate (no phosphorus stabilization or no etch back of a thicker gate) having a thickness of lOOO? thermally grown on the (111) plane. Gate length after diffusion was 0.24 mils, and the devices were hermetically sealed. Stressing conditions were 300°C and 106 v per cm applied alternately as a positive and negative field for 10 min, 50 min, and 4 hr for a total stress time of 10 hr. An initial shift in turn-on voltage of 0.1 v was detected for 10 min of positive bias. All evidence at this laboratory indicated that while EB-gun evaporation of ultra-high purity aluminum was not sufficient for 300°C stability, it did seem to be necessary. There may well then be something inherent in the EB-gun deposition used which enhanced stability, and probably no single factor existed but rather a series of factors. It is the purpose of this paper to report on some of the investigations carried out to learn more about EB-gun evaporation in ultra-high vacuum systems. EXPERIMENTAL DESCRIPTION The EB-gun was self accelerated, had a maximum power rating of 10 kw, and used a water-cooled copper crucible able to hold a 20-g aluminum charge. The electron beam was bent 180 deg and focused by an electromagnet which also provided movement of the beam across the crucible. Normal power conditions in this work were 9 kv and 300 to 600 mamp. The gun can be described as high-cur rent/low-voltage and was quite different in its mechanism of operation from EB-guns with much higher acceleration potentials. An oil-free vacuum system capable of 5 x 10- l0torr, a quartz crystal rate and thickness monitor and a quadruple mass spectrometer completed the evaporation system, Fig. 2. A typical evaporation cycle consisted of a 3 to 4 hr pumpdown to the upper l0-9 range and evaporation at l0? per sec with the pressure in the bell jar not rising above 1 x 10"7 torr. Thickness control was 5 pct or less and could be automatically monitored and controlled. Five phenomena associated with the EB evaporation and considered as possible contributors to Ma performance included a purification effect, ionization of evaporating aluminum, X-rays, constitution of vacuum ambient during evaporation, and film structure dependence upon evaporation rate. These phenomena are now discussed. Vacuum Purification. The design of the EB-gun permitted purification of the aluminum charge by vacuum outgassing. Particular features included an efficiently water-cooled copper hearth with a capacity of over 20 g of aluminum and the capability for sweeping the beam across the charge. Such capacity meant that aluminum had to be added only after about every fifth evaporation. A new charge was not required each evaporation as is necessary with filament evaporation. An oxide "scum" which appeared on the charge could be completely cleared from the top hemisphere of the charge by sweeping with the beam prior to opening the shutter. An indication of the purifying effect was obtained by a series of analytical measurements on incoming aluminum, after melting but with little vacuum out-gassing, after 30 min outgassing, and the evaporated film itself. Either a solids (spark source) mass spectrometer or an emission spectrometer were used for analyzing the aluminum charge. Analysis of the evapo-

Jan 1, 1970

By H. Doi, Y. Fujiwara, K. Miyake

In order to throw light on the mechanism of plastic deformation of WC-Co alloys, compressive tests of WC-(7 to 43) vol pct Co alloys have been carried out at room temperature, and stress-micro strain relation has been investigated in detail. The analysis of the factors affecting the yield stresses reveals that the yield stresses can be predicted by modified Oro-wan's theory if one properly estimates the planar in-terfiarticle spacings. Conzpressive straining of some of the alloys by 0.066 to 0.17pct increases the decrements by a factor of as much as 3.4 to 14, whereas the corresponding increase in the electrical resistivities is less than 10 pct. The analysis of the decrement data in terms of -Gramto and Lücke theory shows that the marked increase is attributed to increased dislocation darnping itt the binder (cobalt) phase. By cornbilling the decrement data and the conzjwession duta, one obtains the relation between flow stress in shear (?t) and increase in dislocation density (p): At = const . v6 . This is interHeted to mean that the mechanism of strain hardening of CirC-Co alloys is essentially sarne as the one for dispersion strengthened alloys. The possible effect of bridge formations between the carbide particles has also been examined. OWING to the combination of hardness, strength, and other physical and chemical properties, WC-Co alloys have opened the way for unique fields of applications, the recent ones being, for instance, anvils for super-high-pressure generation apparatuses. In such applications, the alloys are frequently subjected to very high compressive stresses: these stresses may cause the alloys to deform plastically and eventually to fail. However, much remains obscure regarding the nature of the plasticity of the alloys. Evidently, the alloys owe their high strength to the hard carbide particles which frequently occupy as much as 80 to 90 pct in volume fraction, whereas the ductility required for practical applications is provided by the small amount of the binder phase between the carbide particles. When the volume fraction of the carbide phase is not very large, deformation behavior of the alloys may be described by some of the current dispersion strengthening theories. However, greatly increasing the carbide phase is thought to lead to some carbide skeleton structure or bridge formations owing to the increased chances for direct contacts between the carbide particles;1,2 this may appreciably affect the plasticity of the alloys. Regarding the effect of formation of the carbide skeleton structure, it is interesting to note the work by Ivensen et al.3 on compression tests of the alloys containing somewhat large carbide particles; they observe extensive generation of slip bands in the carbide particles after application of some preliminary compressive stresses. They interpret the results in terms of plastic deformatiot: of the carbide particles which are supposed to have formed a skeleton structure; the binder phase plays only a passive role, at least in the early stages of the deformation. That carbide crystals exhibit microplasticity at room temperature is apparent from the work of Takahashi and Freise4 and French and Thomas5 on indentation of WC single crystals. On the other hand, Dawihl and coworkers6-10 maintain that even when volume fraction of the carbide phase is very large (for instance, more than 90 pet), a very thin binder layer generally exists between the carbide particles. They interpret the results of the extensive mechanical tests in terms of the plasticity of such a layer. Gurland and Bardzil11 point out that decrease in ductility of the alloys with increase in the carbide phase is caused by the effect of plastic constraint exerted by the dispersed carbide particles. Drucker12 further develops this concept from a continuum-mechanics approach on an assumption that a continuous thin binder layer separates the carbide particles. A common feature of the studies reported so far on the plasticity of the alloys is that the information deduced is invariably qualitative in nature. Thus, very few systematic experiments for obtaining reliable and sufficiently detailed stress-strain curves of the alloys varying widely in the microstructural features have been carried out. In particular, it may be of special interest to investigate in detail the early stages of the plastic deformation of the alloys in order to shed light on the strengthening mechanism. However, such work appears to be extremely rare. Doi et al.13 recently reported a first brief account of the results of some quantitative analysis of the plasticity of the alloys in terms of dislocation theory. Their experiment was rather limited in the composition range covered (volume fraction occupied by the carbide phase: 79 to 83 pct), and thus they could not necessarily elucidate the controlling mechanism of plastic deformation of the alloys of a more general composition range. Consequently, in the present investigation, deformation behavior and some other physical properties of the alloys were investigated and discussed in more detail over a much wider composition range. SPECIMEN PREPARATION WC-Co alloys used in this experiment were prepared in cylindrical or rectangular form by sintering in vacuo compressed mixtures of tungsten carbide and cobalt

Jan 1, 1970

By M. Ghiani, P. Carbini, R. Ciccu, C. Del Fà

"This paper is concerned with the problems inherent in the efficient and economical processing of the fine fractions of a coal from the Sulcis basin (Sardinia, Italy) whose characteristics are typical of low-rank coals occurring in the Mediterranean region. Three different techniques, based upon surface properties, are examined. Flotation can be very efficient from both a technical and economic point of view, provided care is taken in the modulation of the flotation pulp. Interesting results have been obtained with oil agglomeration and this method could be economically feasible. Finally, electrical separation has proven a viable technique, although it entails preliminary drying.Besides discussing the problems encountered in the experimental research, some significant results of general validity are also given. They demonstrate that cleaned products can be obtained with fairly interesting recoveries, thus opening the way to advanced research aimed at setting up the most suitable technique for industrial application. IntroductionAs a result of the oil crisis, which caused a major upset in world energy supplies, the last ten years have seen a revolution in the energy policies adopted.In particular, the status of coal, which seemed destined to decline in view of the availability of liquid fuel, has had to be re-examined. The need to meet energy demands under improved reliability conditions and controlled prices through a broader and more flexible diversification of sources of supply has evoked, especially in highly industrialized countries, a renewed interest in coal. The result has been a consistent increase in demand and production as well as investments in new mines and the reinforcement of the infrastructure.This turn of events has also lead to a re-evaluation of young low-rank coals, hitherto considered uneconomical and thus neglected, because of their low heat value. In fact these coals, which have a high ash content, may also be relatively highly contaminated with sulphur. The above drawbacks, which still today preclude the widespread use of these coals, are bound to create even greater problems in the future as increasingly restrictive environmental control imposes, without exception, recourse to cleaner fuels."

Jan 1, 1986

By D. François-Bongareon

"In previous publications by the author, significant advances and generalizations of the theory of sampling of broken ores, prompted and confirmed by experimental results, have been presented. This paper shows how to implement these theoretical results in practice. The models to be used are reviewed, with a description of the various sampling parameters involved. Then the methodology for the experimental assessment of those parameters, including segregation factors, is described in simple and practical terms, along with the use of handy sampling protocol charts. Finally, the particularly important case of processing data from a sample-tree experiment is detailed, and examples of applications covering all situations and types of experiments are provided.IntroductionThe reliability of a sample of crushed material , i.e. the expected (average) deviation between its true grade and the true grade of the lot it comes from, mostly depends upon six factors:• the size (mass) of the sample (and to a minor extent, for small lots, the size of the lot);• the size of the rock particles (degree of comminution)• the nature of the mineralization at microscopic scale (i.e., within even the smallest particles);• the geological nature of the mineralization and mineral of interest;• the grade of the lot in the mineral of interest; and• in some cases, the state of segregation of the lot.In practice, one should first disregard segregation problems, and assess sample variability in the segregation-free case. Once the numerical parameters governing this variability have been assessed, then segregation factors can be assessed in turn. In the case of laboratory standard sample preparation procedures, segregation can usually be disregarded altogether."

Jan 1, 1993

By C. Alan Tapp

Introduction Mine sampling determines the practicality of any mining operation. Improper sampling can result in an incorrect appraisal of present production and future potential. Therefore, the mine department in charge of ore-reserve calculations and mine sampling should be overseen by competent and experienced professionals with technical backgrounds qualifying them to produce accurate results. Sampling is a process by which portions of an ore body are collected and analyzed to estimate the average mineral content of the entire ore body. It is incorrect to assume that a large number of samples eliminates any errors in the sampling method. To obtain unbiased samples, proper sample location with respect to rock type and mineralization is just as important. The sampling procedure must yield correct results for the type of mineral deposit, and careful consideration should be given to whether or not the sampling technique has been developed to an extent sufficient to eliminate as much human error and bias as possible. Only after the ore has been mined and milled is the sampling accuracy known. Sampling also provides information about the bulk composition of the ore for mineralogical and metallurgical tests that determine the economic ore-waste boundaries and the geologic trends for exploration. Actual mining plans can be developed from this information to maximize profits. Accurate sampling is critical, and thus must be approached in a scientific manner. Sampling Techniques Sampling practices and techniques are as varied as the mines in which they are used. The method(s) chosen must be tailored to suit the company and mining needs. For instance, tabular uranium deposits, vein gold deposits, and porphyry copper deposits pose special problems in conducting unbiased sampling. The mine geologist or engineer in charge must develop a sampling method, test it in a sample area, and then critically evaluate the results. If the results from the test area are accurate within the economic limits established by the company, they then may be adopted for general use in the mine. Four routine sampling methods are suitable for specific sampling objectives in the daily mine routine: (1) channel sampling, (2) chip sampling, (3) grab sampling, and (4) bulk sampling. The final sampling results depend upon how the four methods are combined to accurately determine the grade of the ore body. When used in conjunction with each other during different stages of mine development, the channel, chip, grab, and bulk sampling methods provide an in-house check or a comparison by which mining methods and sampling procedures can be evaluated. However, the most valid check is based upon the daily mill production. Channel Sampling Channel samples consist of cuttings collected from a groove cut into the rock about 102 mm (4 in.) wide and 19 mm (0.75 in.) deep. Various tools ranging from a 1.8-kg (4-lb) hammer and moil to a pneumatic chisel can be used to cut the sample. Accessibility and rock hardness determine the applicable sampling tools. Before attempting to take a sample, the rock surface must be cleaned thoroughly; the method of cleaning depends upon the amount of mine dust accumulated on the surface or the degree of alteration of the rock surface. Typical cleaning methods 'employ a wire brush, water, or chipping a fresh surface. Next, the sample outline is marked on the prepared surface, taking care to choose appropriate sample loca- tions. After determining the proper sample outline and length, the sample can be chiseled out, catching the rock fragments on a canvas tarpaulin on the floor, in a powder box, in a canvas bag to avoid contamination, or by some other suitable means to capture all of the sample. Vertical veins present a special problem because the drift's back usually is arched, not square. For example, Fig. 1 shows that if sample intervals are measured from A' to D', the length of the sample interval is greater than the true vein width, resulting in an incorrect calculation of the ore reserves. The correct method would collect three samples at A'-B', B'-C', and C'-D', using either actual measurements in the mine represented by A-B, B-C, and C-D or trigonometric calculations to determine the true ore thickness. Then, each sample can be weighted by grade and true thickness for the vein. Channel lengths usually are a maximum of 1.5 m (5 ft), and it is good practice to divide longer samples into smaller intervals according to structures, changes in rock types, or differences in rock hardnesses. The influence of those features on the mineralization then can be determined. Chip Sampling Chip sampling is a variation of channel sampling used when the rock is too hard to channel sample economically or when little variation in the mineral content indicates that this sampling method will yield results similar to those of channel sampling. Rather than cutting a channel in the rock, small chips are flaked off at regular intervals over the entire face or area being the mine. sampled. Care must be taken to assure that the sample is representative of variations in the rock hardness and type. hi^ method is fast and useful in preliminary evaluations, but it should not be used for quantitative ore-reserve calculations. Grab Sampling Grab sampling is a fast method for double checking either channel or chip-sampling procedures, and, in some instances, mine production can be estimated from carefully taken grab samples. Grab sampling takes equal amounts of material at selected intervals over a mine dump, a muck pile, or from an ore car to estimate its Channel Sampling mineral content. Generally, this method is not considered reliable. Many independent variables can affect this type of sampling process. Thus, if the ore occurs in the softer fraction and a proportional amount of the result-

Jan 1, 1982

By Richard R. Zupp, David A. Stevenson

An experimental method to determine the carbon activity in various solid solutions was developed. Samples of the solid solutions and an Fe-C reference sample were equilibrated with respect to carbon content by annealing them in a Hz-CHI gas mixture in a closed cell. The carbon content of each sample was determined, and the carbon activity was obtained from the carbon content of' the reference sample and well-established data for the dependence of the carbon activity on the carbon content in Fe-C alloys. The influence of vanadium on the activity of carbon in austenitic Fe-C-V alloys at 1000°C was determined by this technique. A general semiempirical correlation was developed to describe the dependence of the activity coefficient of- carbon on the composition of ternary austenitic iron-base alloys containing interstitial carbon and a substitutional solute. The correlation is particularly useful in predicting the partitioning of- carbon between various alloys. THE influence of substitutional solutes on the activity of interstitial solutes in metallic solid solutions is important in the theory of alloy phases. Solid solutions of particular interest are the fcc austenite phases of ternary Fe-C-Z systems, in which carbon is the interstitial solute and Z represents any substitutional solute. Carbon-activity data are also needed in these solid solutions to solve practical problems; the quantitative treatment of diffusion-controlled transformations' is an examvle. Experimental information is available for ternary austenitic solid solutions containing Mn,2 Si,2 and A16 as the substitutional solute. Because qualitative preliminary studies indicated that vanadium appreciably decreases the carbon activity,14 the present investigation was undertaken to determine the influence of vanadium on the activity of carbon in austenite. Although Flender and ever" measured carbon activity over a range of compositions in the Fe-C-V system, they were primarily interested in determining phase boundaries in the ternary system, so most of their measurements were outside the composition range for stability of single-phase austenite. Petrova and Shvartsman' also made limited measurements of the carbon activity in Fe-C-V alloys. The dependence of the carbon activity on the carbon content of an alloy may be determined by passing COCOz or H2-CH4 gas mixtures of carefully measured composition over the alloys, determining their equilibrium carbon content, and utilizing the relevant equilibrium relationships. smith16 used this technique with both CO-COZ and HZ-CH4 gas mixtures to determine the dependence of carbon activity on carbon content in pure Fe-C alloys. His data, which are in good agreement with those of some previous and subsequent investigators,6'17 but not with those of others,lfl'ao are usually considered to be the most reliable. Although the same method can be applied to Fe-C-Z alloys, it is difficult experimentally, because the appropriate gas mixtures are almost pure CO or Hz. A simpler technique is to simultaneously equilibrate the Fe-C-Z alloys and pure Fe-C alloys with the gas mixtures, and then use Smith's data to determine the carbon activity in the pure Fe-C alloy. A number of investigators have employed this technique. others Have used the partitioning of carbon at the interface of a diffusion couple prepared from an Fe-C alloy and a Fe-C-Z alloy. In the present study, a closed-cell method was developed by which carbon was selectively transferred via a gas medium between pure Fe-C alloys and Fe-C-V alloys which were not in physical contact. A similar method was developed independently by Heckler and winchel14 and used to study the Fe-C-Ni system. EXPERIMENTAL METHOD A schematic diagram of the experimental arrangement is shown in Fig. 1. In a typical experiment, a 5-g Fe-C sample was placed in one compartment of a quartz cell, and a 5-g Fe-V sample was placed in each of the other compartments. The cell was evacuated, outgassed, backfilled with approximately 125 Torr of hydrogen, and sealed. After being placed in a fur-

Jan 1, 1967

By M. P. Tixier

In several log interpretation methods, water saturation is evaluated by use of the ratio of the readings of a short spacing resistivity device and a long spacing resistivity device plus information on the mud filtrate and connate water resistivities, which is often derivable from the SP. These methods are valid over a certain range of conditions, usually specified by moderate invasion and R.. greater than R,. Since these methods involve no explicit evaluation of the formation factor, F, the saturafiion so found may be used in the standard Archie equation to derive a computed formation factor which, as a check, may be compared with the formation factor known from other independent measurements. Discrepancies in the two values of formation factor generally indicate that the ratio method is not within its range of applicability. If the computed F is too low, the corresponding S, is too low; if the computed F is too great, the corresponding S, is too great. By means of this "porosity balance" check, and some knowledge of the probable conditions of invasion, the interpretation can often be improved. The poqosity balance check is discussed for the cases of the Induction-Electrical Log Interpretation Method, the Rocky Mountain Method, and the R.,/R, Method. For the first method, a discussion is also given for the case of shaly sands. INTRODUCTION Al though many logging tools are available to obtain a practical value of porosity, the only logging method reflecting the water saturation is electrical logging. Water saturation is commonly computed from electrical log data by means of the basic Archie formula, Where F is the formation factor, R, the resistivity of the formation water, and R, the true resistivity of the formation. One difficulty in this procedure is a possible error in the evaluation of R, from the logs— for example, in the case of very deep invasion. There is no possibility, inherent in the procedure, which would provide a check of the accuracy of R, and, hence, of the computed saturation. Other approaches have been proposed which are based essentially on the ratio of the readings made with two dzerent devices: one device, with a short radius of investigation, provides a value close to the resistivity of the invaded zone; the second device, with a long radius of investigation, gives a value close to the true resistivity of the bed. By these methods, the determination of saturation is made independently of any direct knowledge of the formation factor. Therefore, if the formation factor (or porosity) is known from other sources (core analysis, neutron log, MicroLog . . .), it becomes possible to take advantage of this additional information in order to check the value of saturation derived from these latter methods. Inasmuch as this proposed check procedure relies on a knowledge of the value of formation factor or porosity, it has been deemed appropriate to call this verification a porosity balance. The purpose of this paper is to discuss the principle and the application of the porosity balance, depending on the method of interpretation being used. Basis of the Method There are in existence three interpretation methods by means of which the water saturation can bc found without a knowledge of the formation factor (or porosity). As just stated, they are based on the fact that the ratio of the two resistivities (one measuring the resistivity close to the hole, the other measuring the resistivity far from the hole) is independent of the formation factor since it affects the two resistivity measurements in the same way. Chronologically, the resistivity ratio methods are: (1) the Rocky Mountain Method, which has been used since 1943 and was explained in a paper in 1949;' (2) the R../R, Method or Shaly Sand Method, presented in 1954, which permits the calculation of the water saturation in both clean and shaly sands2; and (3) the Induction-Electrical Log Method, presented in 1957 for the interpretation of the induction-electrical log combination." Each method requires certain definite conditions in order for the interpretation to be reliable. The porosity balance method will let us know whether these conditions are fulfilled. In clean formations we know that the fundamental Archie relation (Eq. 1) must always be verified. This relation can be rewritten:

By E. R. Parker, R. H. Thielemann

The conventional short-time tensile test provides a reliable means of predicting the sustained load-carrying capacity of steels only when the temperature is such that continuous plastic flow does not occur. At elevated temperatures, stresses considerably less than the short-time rupture value may produce continuous flow, with fracture occurring only after long periods of time. The amount of flow or creep accompanying failure varies for different steels, and depends, to a large extent, on the temperature and the duration of the test. Service records of cracking stills, steam superheaters and high-temperature boilers have shown that brittle fractures sometimes occur with little or no warning. In installations of this type, localized stresses are often encountered, and steels must be capable of withstanding a certain amount of deformation without fracture. The sustained-load rupture test determines the expected life and corresponding ductility of steels at various stresses and temperatures. It also yields additional information regarding the effect of micro-structure and metallurgical stability on the high-temperature properties. Present Status of Sustained-load Rupture Test The sustained-load rupture test conducted at elevated temperatures is not entirely new. Dr. Zay Jeffriesl presented in 1919 the results of a large number of rupture tests made on copper, iron and tungsten. These tests were made with various strain rates and at temperatures ranging from the boiling point of liquid air to 1000° C. At that time he observed the interesting phenomenon characteristic of metals, that a temperature exists below which a metal is ductile and breaks with a transcrystalline fracture (through the grain) and above which the metal is brittle and breaks with an intergranular fracture (through the grain boundaries). He observed that this temperature varied with the testing speed, and that a minimum temperature, slightly above the recrystallization temperature, existed at which the cohesion of the grains themselves was

Jan 1, 1939

By R. H. Thielemann, E. R. Parker

The conventional short-time tensile test provides a reliable means of predicting the sustained load-carrying capacity of steels only when the temperature is such that continuous plastic flow does not occur. At elevated temperatures, stresses considerably less than the short-time rupture value may produce continuous flow, with fracture occurring only after long periods of time. The amount of flow or creep accompanying failure varies for different steels, and depends, to a large extent, on the temperature and the duration of the test. Service records of cracking stills, steam superheaters and high-temperature boilers have shown that brittle fractures sometimes occur with little or no warning. In installations of this type, localized stresses are often encountered, and steels must be capable of withstanding a certain amount of deformation without fracture. The sustained-load rupture test determines the expected life and corresponding ductility of steels at various stresses and temperatures. It also yields additional information regarding the effect of micro-structure and metallurgical stability on the high-temperature properties. Present Status of Sustained-load Rupture Test The sustained-load rupture test conducted at elevated temperatures is not entirely new. Dr. Zay Jeffriesl presented in 1919 the results of a large number of rupture tests made on copper, iron and tungsten. These tests were made with various strain rates and at temperatures ranging from the boiling point of liquid air to 1000° C. At that time he observed the interesting phenomenon characteristic of metals, that a temperature exists below which a metal is ductile and breaks with a transcrystalline fracture (through the grain) and above which the metal is brittle and breaks with an intergranular fracture (through the grain boundaries). He observed that this temperature varied with the testing speed, and that a minimum temperature, slightly above the recrystallization temperature, existed at which the cohesion of the grains themselves was

Jan 1, 1939

By Richard H. Spencer, Warren G. Bender

Since the passage of the Coal Mine Health and Safety Act of 1969, the Bureau of Mines has made many advances in mine communications. These efforts have resulted in the following developments and demonstrations: • Surface-to-surface electromagnetic transmission of baseband voice signals through overburdens as deep as 600 feet. This transmission was achieved with equipment from the Interim Mine Rescue and Survival System Program, and demonstrated that baseband voice communications could be obtained through these overburdens in the absence of mine-generated noise; that is, when the mine power system was shut off. However, during mine operational conditions, the mine-generated noise proved to be so large that effective baseband voice communications to the desired depths could not be effected. • The development of beacon transmitters for locating trapped miners. This work was again the outgrowth of the Interim Mine Rescue and Survival System. Extensions of this work have led to reliable detection and location of trapped miners to depths of 1000 feet. The system, which makes use of a loop antenna deployed where the trapped miner is located, uses low-duty-cycle, tone-burst transmission. Portable tuned receivers and loop antennas are used on the surface to determine the location of the trapped miner. An extension of this work has led to a call-alert paging system concept, wherein a transmitter, similar to that used in the trapped miner system, is used to audibly and/or visually alert key mine personnel carrying pocket receivers that they are wanted at the nearest mine telephone. In addition, a roof-bolt paging system has been developed, wherein commercial paging and mine carrier phone equipment are used in conjunction with a long-wire "roof bolt" antenna to page individuals and relay to them short voice messages.

Jan 7, 1975

By R. Lovat, J. A. Hunter

"The design, development, and verification of the Lovat 7.6metre diameter full-face tunnel-boring machine is reviewed. Programmatic and technical challenges are outlined with a review of the specifications and the design to meet these requirements. Subsystem designs are presented for the waste material removal, ventilation, cutter head, structural support, advance technique, water removal, and interfaces with the Donkin-Morien Mine. The techniques used to verify that the design meets the requirements is by testing in the Lovat factory and in the field. Certification of the machine for use in a methane environment is discussed.IntroductionStudies have concluded that the average annual worldwide tunnel construction is 500 kilometres at an estimated average co st of $3,400 U.S . per linear metre. The total market value of the tunnelling industry is estimated as approximately $1.7 billion U.S. per annum. Of this, the current market for tunnelboring machine excavation is approximately $270 million U.S. per annum worldwide with a further potential of $250 million if more contractors are convinced that Tunnel-Boring Machines (TBM) are more suitable than conventional techniques. The worldwide civil tunnelling market has the potential to double each year in the next 5 to 15 years. Growth has been identified in the energy and mineral resources sectors of the economies of many nations and a significant volume of machine tunnelling studies and trials are presently underway for the extraction of coal, uranium , heavy oil or oil sand fuels, metallic and non-metallic industrial minerals and base metal or rare earth ores. Further tunnel projects for regional transportation, waterpower, irrigation , high density urban transportation, storm water sewers and water supply purposes are continually being implemented with new concepts like military security facilities and underground storage schemes being considered.Lo vat Tunnel Equipment of Rexdale, Ontario, the only Canadian manufacturer of TBMs was incorporated in 1973 to manufacture so ft ground tunnel-boring machines to satisfy this growing market demand. Lovat has produced an average of 5 machines per annum during the period 1972 - 1982 and has established an international reputation for competitive costs, quality of construction, after-sales service, and reliability. As of June 1982 Lovat TBM's have been used to tunnel over 240 km in projects throughout the world."

Jan 1, 1984

By C. E. Turner, J. R. Elenbaas, R. D. Grimm, J. A. Vary, D. L. Katz

A technique is presented by which well samples and core plugs of dolomite formations are classified by microscopic examination into seven different porosity grades. Quantitative values of porosity and permeability are determined for each grade by a statistical correlation of the core plug test data with the porosity grading system. These quantitative values are applied directly to the grades exhibited in the well samples for the purpose of estimating the reservoir void space for wells that were not cored. The procedure is described for estimating the gas reserves per unit area lor the South Hugoton gas field. but a reserve estimate for the field is not given. INTRODUCTION The miscroscopic examination of well sample; and the graphic recording of their lithologic qualities and other distinguishing characteristics of various geologic formations drilled is both a science and an art of long standing and wide application. Usually the primary objective of a geologist who "sits on the well" and examines the samples are: to identify the formation being drilled, determine the total depth, casing point. and completion interval. In most cases the porosity is described. if done at all, in general terms. such as: trace, scattered, fine, poor, fair, medium. good, excellent, or in some other relative terms. In fields where various geologists have examined samples and recorded observations on many wells considerable variations in lithologic terms and porosity descriptions occur unless there is primary effort to establish uniformity of logging observations and standards of recording observable porosity. When an estimate of the pore volume of a reservoir is made a geologic concept of the processes that control the magnitudes of porosity and permeability is developed by microscopic examination of well samples. The characeristics and appearances are then mentally related to rather general quantitative units of porosity based on physical core data from the same reservoir or on such data or experience in other reservoirs that have similar qualities. The reliability of such estimates depends largely on the variations of the lithology of the formations, the geometric properties of its void system. the extent of comparisons of sample appearances with porosity data, as well as the uniform recording of all relevant characteristics. This statement is particularly significant for dolo-mitized limestone formations of substantial thicknesses and heterogeneity such as the Permian Dolomites of the Hugoton gas field. Jn this field, as well as in most of the Permian Dolomite fields, the producing formations are of relatively great thicknesses in which the porosity and permeability of the reservoir varies substantially in all directions, depending on the crystalline structure. degree and kind of impurities, kind of fossils anti cementation thereof, degree of dissolution. and fracturing. The variations of the lithologic texture of the dolomites and post deposition alterations have resulted in porosities and permeabilities of such magnitudes that only a part of the gross thickness can be counted as "pay." At the time of this study insufficient gas production had been experienced to apply the pressure decline production method in the South Hugoton Field and the electric logs are not definitive enough. The problem of estimating gas reserves in the south part of the Hugoton Field is primarily one of determining the pay thickness and porosity from well samples and core data. The area studied embraced all that part of the field lying south of an east-west line through Guvmon, Okla., anti containing approximately 1.000,000 acres. This paper describes a technique of correlation of physical core data with well samples so that quantitative values of pay thickness, porosity. Permeability, and connate water may be assigned to well samples that are representative of a given interval, and thereby permitting the estimation of gas reserves lor a given unit area. The procedure was developed by a uniform microscopic qualitative porosity grading of the dolo. mite core plugs.. and relating these grades to the respective physical core data on a statistical basis The well sample-were also graded in a Similar manner in order that the quantitative values established lor the core plugs could be applied to the well Sample for wells that were not cored. GRADING OF DOLOMITE A group of experienced geologists was given the assignment of examining the samples on all wells in South Hugoton in order that they could log their observations in a uniform and standardized manner and grade the observed porosity so that it could be related quantitatively to the core data. The group initiated the study 011 chips from cores which bad been tested for porosity and permeability. This study continued until all of the geologists developed a common knowledge of lithologic terms and of the characteristic appearances of the samples and their relations to measured porosity. The characteristic appearances of the dolomite samples under twelve-power magnification as related to their qualitative porosities afforded a classification of the dolomite into :even grades of porosity, ranging from dolomite of no-visible porosity under twelve-power magnification to dolomite of excellent porosity. The assigned grade for a specific 10-ft interval is a weighted average of all visible grades of porosity exhibited by the cuttings representing that interval. The porosity characteristics were recorded by a color graph adjacent to the lithology column in conjunction with a numerical system for further definition of relative porosity as shown in Fig. 1. The three vertical lines to the right of the lithology column each represent 33 1/3 per cent. which lines were used to record the percentage of the samples, for any particular interval. that showed porosity under the microscope. The colors were used to denote actual pore size. i.e., orange. blue and I-ed for pore diameter of one-fourth or less. one-fourth to one-Ilalf. and greater than one-half millimeter, respectively. The area colored 1)). one or more colors represents the percentages of the samples exhibiting pores of the respective size or sizes. The numerals from one to six inclusive shown on the log in

Jan 1, 1952

The reduction in the number and duration of machinery and equipment failures is an important source of economical efficiency enhancement in the Polish coal mining industry.Non-dismantling methods have been thus developed to evaluate the technical state of machines. Among these viroacoustical methods are the most effectively employed. Two-directional organisation of the testing can be chosen, such as periodical and continuous inspection. The monitoring methods for ball bearing, rope tension uniformity, longwall shearers, main fans and shafts installations etc. Instrumentation for monitoring measurements are either of intrinsically - safe or explosion - proof construction, which enables using them in a gas-hazard atmosphere. The development of these procedures has led to the trials to insert the diagnostic methods into the organisational scheme of a coal mine.

Jan 1, 1991

By A. Dell’Era, E. Ciro, C. Lupi

The paper explores the recovery of indium via electrowinning from sulfate baths, focusing on the impact of different cathodic supports (AISI 316L and nickel) on process parameters such as electrolyte composition, current density, and temperature. The study compares productivity, morphology, and structure of indium deposits on both cathodes, finding that nickel cathodes generally yield better results.

Nov 1, 2023

By N. A. D. Parlee

The diffusion rate of hydrogen in liquid iron has been measured by a gas-liquid metal diffusion cell technique. The diffusion cell was formed by immersing an alumina tube containing hydrogen gas at 1 atm in a bath of stagnant liquid iron. The change in the composition of the melt in the cell was determined by measuring the rate of absorption of the gas in the cell. The appropriate solution to Fick's second law was used to examine the data and calculate diffusivi-ties. The absorption of hydrogen in stagnant pure liquid iron has been found to be diffusion-controlled. The results show that the chemical diffusion coefficient, D, of hydrogen in pure iron in the range of 1547" to 1726°C can be represented by the following Arrhenius relation: D(sq cnz per sec) = 3.2 x X exp(- 3300 i 1800/RT) where the uncertainty in the activation energy corresponds to the YO pct confidence level. Oxygen in the melt (above 0.015 pct 2) increased the apparent rate of absorption of hydrogen. The importance of diffusion data on liquid metals for predicting the rates of certain metallurgical processes has been recognized for a long time. Moreover, these data are much needed to test and develop theory for diffusion in liquid metals. Despite this practical and theoretical interest, however, relatively little reliable information about diffusion in liquid metals is available in the literature. This is particularly true for gas components such as hydrogen, oxygen, and nitrogen in liquid metals, where almost no data on chemical diffusion coefficients are to be found. This is probably due to a multitude of experimental difficulties particularly associated with high-temperature melts. In an effort to fill this gap in information, a research program was undertaken to study the diffusivities and rates of solution of gases in liquid metals. This paper presents the results of a study of the diffusion of hydrogen in liquid iron. EXPERIMENTAL METHOD Two methods for the study of the kinetics of dissolution of gases in liquid metals are being employed in this laboratory. Both involve the measurement of the volume of gas absorbed by the melt as a function of time and as such both avoid the uncertainties involved in chemical analyses of quenched samples for relatively small amounts of gas. In the first method, the gas dissolves in an inductively stirred melt and, in the absence of a slow surface reaction, the results are often interpreted in terms of mass transport across a liquid "boundary layer" between the homogeneous gas phase and well-stirred part of the melt. Other interpretations of the results of such experiments have also been described in the literature.1'5 In the second method a gas-liquid metal diffusion cell is used.' The gas dissolves in a cylindrical column of stagnant liquid metal and, in the absence of a slow surface reaction, the results are interpreted in terms of a non-steady-state diffusion solution to Fick's second law. The weakness of the first method is that while it gives information on the mechanism of absorption by stirred melts it yields an overall rate constant which even in the simplest cases depends on the nature and the thickness of the "mass transport layer" or "boundary layer". It yields no values of diffusion coefficients. The second method was used in this research because in many cases it is possible to determine the diffusion coefficient of the gas component in the liquid metal. In this research it has been utilized to measure diffusion coefficients of hydrogen in liquid iron. The apparatus used was essentially the same as that described by Mizikar, Grace, and par lee but certain modifications have been introduced to meet the elevated temperatures and special conditions of this research. Fig. 1 is a schematic drawing of the apparatus and Table I gives the identification of various parts in this figure. The diffusion cell, shown in detail in Fig. 2, was formed by immersing an impervious alumina tube (hereafter called absorption tube) in a bath of pure liquid iron contained in an alumina crucible. Two types of tubes were used, Morganite triangle RR and McDanel AP35. The crucible was contained in a vertical impervious alumina combustion tube (32 mm ID by 914 mm long) which was closed at both ends by water-cooled brass heads employing O-ring compression seals, Fig. 1. A protection tube enclosing a Pt, 5 pct Rh-Pt, 20 pct Rh thermocouple was introduced through the lower end of the combustion tube

Jan 1, 1968

By N. A. Gokcen

THE data of Chaudron,1 Tonosaki,2 and Collins³ on the thermodynamic properties of MOO, disagree widely. These authors, by using essentially similar methods, studied the following reaction: 1/2MoO2(s) + H2(g) == i/2Mo(s) + Ph,o H2O(g),K = —----- [1] Ph2 Tonosaki used a vacuum system consisting of a furnace containing MOO, and a water saturator whose temperature was kept at 25 °C with a thermostat. After repeated evacuation, hydrogen was admitted slowly into the system. The experiments were based upon the fact that at a constant furnace temperature and constant partial pressure of water, the total pressure of gas mixture over MOO? + Mo is constant. Any attempt to vary the pressure by external forces would vary only the amounts of MoO2, and Mo, after which the pressure should return to the equilibrium value in accordance with the equilibrium constant of reaction 1. The actual value of K was determined from the total equilibrium pressure (sum of Ph2o + Ph2) at each temperature. The total pressure of gas was varied within the range of 80.2 to 125.4 mm Hg, within a temperature range of 645" to 823 °C. The results were summarized as log K = 0.9413 — 1444.6/T for reaction 1. The ratio of H2O/H2 was considered to be uniform in spite of the presence of a thermal gradient across the static gas phase. It was shown by Rosenqvist and Cox,' however, that in somewhat similar circumstances the error resulting from thermal diffusion may be large. Collins³ improved Tonosaki's method by attempting to avoid thermal diffusion errors. His equilibrium data were obtained at 700°, 800°, and 900° C, and the result for reaction 1 was expressed as log K = 1.258 — 1822/T. The purpose of this investigation was to study reaction 1, avoiding the thermal diffusion errors, and to obtain equilibrium data in a considerably wide temperature range for the reliable extrapolation of the resulting thermodynamic functions. Experimental Procedure The diagram of the apparatus is shown in Fig. 1. Tank hydrogen was passed through a tube containing platinized asbestos at 425 °C in order to convert a trace of oxygen into water vapor. The flow rate was carefully controlled with a capillary-type flow-meter B and a bubbling column D. The gas was then presaturated sufficiently at P and led into a condenser system immersed in a thermostat, controlled to within ±0.002C. The temperature of the thermostat was measured with a thermometer calibrated against a certified standard. The temperature of P was adjusted to avoid the condensation of unduly large amounts of water as judged from the rate of flow out of the capillary tube M. Argon was purified by passing it through magnesium chips kept at 630°C. After passing through the flowmeter B', it was mixed with moist hydrogen emerging from the thermostat. The resulting gas mixture was then led into the hot zone of the furnace through the heated glass tubing and the silica tube S, thus insuring the same ratio of PII2o/Ph2 from the condenser to the reaction chamber, thus avoiding thermal diffusion. The entire gas system was of all-glass construction, except at the magnesium train. The furnace comprised a glazed alumina tube over which a 15-in. platinum coil was wound. The lower end of the alumina tube was tightly closed with a brass bottom and a silicone rubber gasket, and the upper end with two glass disks, each with a hole of 1/16 in. in diameter, through which the gas mixture escaped into the atmosphere. A back-up coil of kanthal wire facilitated the temperature control of the furnace. A coil of annealed molybdenum strip of 99.99 pct purity, 0.005 in. thick and 0.050 in. wide, and weighing 17 g was hung in the furnace with a 0.010-in. platinum wire attached to one end of a sensitive analytical balance. The temperature of the furnace was measured with a Pt-Pt-10 pct Rh thermocouple checked against a standard. The experimental procedure consisted of heating the gas purification trains, adjusting the gas flow rates, attaining a constant thermostatic temperature, flushing the entire system for 2 hr while heating the furnace to well above the expected equilibrium temperature and then cooling it at a rate of 0.3°C per min during which time the change in the weight of molybdenum was observed on the balance. For a given thermostatic temperature, i.e., a constant Prr,o/Px,, molybdenum oxidized upon cooling slightly below the equilibrium temperature. The procedure was then repeated by heating the furnace and thus reaching a temperature slightly above the equilibrium value. The average of the two temperatures, differing by 2" to 3"C, was considered to be the true equilibrium temperature. In order to determine the stoichiometric composition of the oxide phase present in this investigation,

Jan 1, 1954

By L. J. E. Hofer

THIS BULLETIN analyzes and summarizes research at the Bureau of Mines dealing with the preparation, properties, and reactions of iron carbides in the period 1948-60, part of which was sponsored by Wright Air Development Laboratories. The objective was to develop better catalysts for the synthesis of methane and higher hydrocarbons from hydrogen and carbon monoxide. The investigations resulted in the first adequate characterization of epsilon iron carbide, which later proved to be an important intermediate in the tempering of martensite in steel. At temperatures near 170° C, the carbon in carbon monoxide reacts nearly quantitatively with finely divided alpha iron to form an iron carbide in which the metal atoms occupy the positions of the close packed hexagonal arrangement with lattice parameters of ao=2.754 A and co=4.349 A. The carbide has a composition within 2 atomic percent of that required for the formula Fe2C, a Curie point of about 370° C, a specific magnetization of 160.4 ergs per gauss-gram Fe at 50° C, and a ferromagnetic moment of 1.70 Bohr magnetons. Epsilon iron carbide can be converted to chi iron carbide by thermal treatment at 343° C for about 70 hours. The chi iron carbide so formed has a Curie point of 247° C, a specific magnetization of 142.5 ergs per gauss-gram Fe at 50° C, a ferromagnetic moment of 1.72 Bohr magnetons per iron atom, and a paramagnetic moment of 5.5 Bohr rnagnetons per iron atom. Direct synthesis of this carbide from carbon monoxide at 240° C indicates a composition within 7 atomic percent of that required for Fe2C. Chi iron carbide can be converted to cementite at 550° C in about 315 minutes. The theta iron carbide so prepared has a Curie point of 210° C, a specific magnetization of 147.3 ergs per gauss gram Fe at 50° C, a ferromagnetic moment of 1.72 Bohr magnetons per iron atom, and a paramagnetic moment of 3.9 Bohr magnetons per iron atom. Pure chi iron carbide reacts to form theta iron carbide by the elimination of free carbon. In the presence of an excess of free iron in intimate contact with the carbide, chi iron carbide reacts with the free iron to form theta iron carbide. The second reaction proceeds at an appreciable rate at 320° C and can be used to snythesize finely divided theta iron carbide with no free-carbon impurity at low temperatures. The ease of the reaction in the presence of free iron suggests that chi iron carbide is an intermediate in the tempering of epsilon iron carbide to theta iron carbide as it proceeds in steels. Experiments on carbon steel show that the magnetic moment of the iron atoms in martensite is about 2.2 Bohr magnetons per atom, a value approximately the same as that of the iron atoms in alpha iron. The Curie points of epsilon iron carbide, chi iron carbide, and theta iron carbide were found -in various specimens of tempered steel to be 10° to 20° C lower than normal values. This shift is probably the result of manganese in solid solution. Preparations of various compositions of epsilon iron carbonitrides show many effects of extensive isomorphism between epsilon iron carbide and epsilon iron nitride. The action of carbon monoxide on finely divided alpha iron at 400° C results in free carbon deposits containing filaments about 0.1 micron in diameter and several times as long. The filaments are characterized by nuclei of dense material located midway from each end of the filament. Although carbiding to near completion at 240° C over periods of about 300 hours produces a preparation containing no appreciable percentage of epsilon iron carbide, very brief periods of carbiding of the order of a minute result in the formation of detectable epsilon iron carbide even at temperatures as high as 325° C. The data indicate that epsilon iron carbide is an intermediate in the formation of chi iron carbide during its formation from carbon monoxide in the gas phase. Attempts to convert cementite to chi iron carbide by cold work increased the Curie point but did not change the X-ray powder diffraction pattern.

Jan 1, 1966

By Herty, C. H.

Present-day interest in the question of "dirty steel" has arisen primarily from the increasingly rigid specifications on various grades of steel and from the growing conviction that non-metallic inclusions are the source of many of the difficulties in meeting these specifications. The importance of inclusions has unquestionably been over-emphasized in many cases, but on the other hand many unpublished instances could be recorded where all evidence pointed to inclusions as the primary cause for the failure of steel in rolling or in service. The solution of the problem of dirty steel is not a matter of a few years. There are almost numberless types of inclusions. They segregate in steel ingots in an entirely different manner from other impurities, and, at best, only a start has been made in developing correct analytical methods for their determination. Most of the writers in the field have expressed opinions rather than given facts, and so many variables enter into the manufacture of steel that a study of plant conditions is difficult unless definite facts on certain phases of the inclusion problem are available. This statement is not intended to convey the idea that little work has been done on this problem. On the other hand, the number of investigations has been large, but in most cases too many variables have been present to allow definite conclusions to be drawn. In the body of the text, reference to previous investigations is made at suitable points. Rather than burden the reader with a lengthy review of the literature on the general subject of inclusions, reference to the particular works pertinent to the subject matter of the bulletin has been discussed. Three excellent bibliographies b on the subject have been lately published: one by the Committee on

Jan 1, 1957

By Thomas S. Jones

This report discusses processing and use of the principal forms of manganese. The focus is on trends in the United States in the 20th century and specifics of domestic manganese material flows as of about 1990. To protect proprietary data, quantitative assessments are limited to the iron and steel industry, which accounts for about 90% of consumption. Nonmetallurgical uses are considered qualitatively. Approximate disposition of a U.S. cumulative consumption during 1901-90 of an estimated 69 million st of manganese is estimated to be iron and steel slag, 69%; nonmetallurgical uses of a dissipative na¬ture, 10%; iron and steel scrap, 9%; National Defense Stockpile, 3%; unidentified and/or including items in service, 10%. In slag from iron blast furnaces and steelmaking, manganese is present as a minor, relatively im¬mobile component, which so far has been uneconomical to recover. Construction and road building are main applications for these slags. Steel slag contains the greater amount of manganese. Studies by others of global manganese fluxes and the effect of human activities on them also are discussed. One source concludes that the main effect of human activities, via deforestation and agricultural activities, has been to increase the rate of transport of manganese to the oceans.

Jan 1, 1994

This information circular describes research the Bureau of fines has conducted to improve technology for recovering precious metals from low-grade resources. Many of the reported findings are recent, and some of the work described is ongoing. Topics discussed include cyanidation of carbonaceous gold ores to enhance gold recovery, a new method for precipitating mercury during cyanide leaching of gold ores, a staged heap leaching process to generate suitable solutions for direct electrowinning of gold, the use of anion-exchange resins to recover gold from cyanide solutions, and precious metals recovery from electronic scrap.

Jan 1, 1986