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By A. U. Seybolt, V. A. Phillips

Binary iron alloys containing 1 pct of Al, Cr, Mn, Mo, Si, Ti, or V, and 0.4 pct C, 1 pct Cr steels with and without 1.2 pct A1 or 2.0 pct Ti additions, were ion-nilrided at 550° to 600° in N-H mixtures. Nitriding increased the inicrohardne ss of all the binary alloys except those containing manganese or molybdenutn, and also hardened the heat-treated steels if aluminum or titanium urns present. Transmission electron microscopy revealed particle formation in all casts where hardening occurred. Electron diffraction gare positive identifications for ALN, CrN, and a, Si3N4 in the binary alloys, and AlN and CrN in the aluminum- cold chromium-bearing steels, respectil&apos;uly. Cubic VN with a, = 4.13A was tentatively identified. Particles, apparently of CrN, also formed in the base steel but did not increase the hardness very much. Chromium and vanadium formed nitride platelets on {001}° matrix planes, while titanium gave clusters <15A diam. Aluminum nitride precipitated at grain and subgrain boundaries, and within the grains. Silicon gave profuse precipitates of several Morphologies at grain boundaries and cubical particles within the grains. No effect of the alloy carbides on nitride precipitation was observed in the heat-treated steels. THE nitriding of steel has been a well-established commercial process for about 40 years, but in spite of this comparatively long period of use there have been few studies aimed at understanding the process. Most studies, like the early but very competent work of Jones and organ&apos; and nones.&apos; were concerned with establishing the pertinent engineering variables of steel composition, gas composition, temperature, and time. As far as the present authors are aware, there have been no studies of the composition, size, shape, or distribution of the nitrides formed in the nitriding of steel. Noren and Kindbom3 did, however, examine a few nitrided steels by surface replica electron microscopy, and were able to show the presence of car-bonitrides and AlN and TiN nitrides. pitsch4,5 and Hrivnak6 examined nitrided pure iron by transmission electron microscopy. Baird7 found manganese nitrides in Fe-1.6 pct Mn when nitrided at 650°C, using the same technique. In the present work, emphasis was placed on transmission electron microscopy because of its inherently better resolution, using principally binary alloys of iron containing 1 pct of alloying element. In addition, a few simple 0.4 pct C steel compositions were examined to investigate possible carbonitride formation. It was not anticipated that all of the added elements would form nitrides under the conditions used, but it was considered desirable to obtain direct experimental evidence on this point. It would be considerably easier to ascertain the presence of alloy nitrides by examining appropriate binary alloys in preference to relatively complex steels. The work reported here could have been done using orthodox ammonia-nitriding procedures, but an operating ion-nitriding equipment was available, and was therefore used for specimen preparation. EXPERIMENTAL DETAILS 1) Materials. Binary alloys were made up from vacuum-melted electrolytic iron with 1 wt pct additions of Cr, Ti, V, Al, Mn, Mo, and Si of about 99.9 pct purity. In addition, three steels were similarly made up—a basis steel with 1 wt pct Cr and 0.4 wt pct C and two steels with further additions of 1.2 wt pct A1 or 2.0 wt pct Ti, respectively. The materials were vacuum-melted and cast as 11-lb heats into tapered square molds of about 2 by 2 in. average cross section. The castings were forged and hot-rolled to 11/4 in. rounds. Discs of 4 in. thickness by about 1 in. diam were machined from the rods. Some of these discs were hot-forged and hot-rolled to about 0.020 in. thick, sand-blasted, and then cold-rolled to about 0.003 in. thick. At this point, the surface was cleaned by light etching with HC1, then washed, dried, and vapor-degreased prior to nitriding. 2) Ion-Nitriding Procedure. The type of ion-nitriding equipment used here is similar to that described by Jones and Martin.8 Briefly, a mixture of nitrogen and hydrogen at 5 mm total pressure is placed in a vacuum chamber with a dc potential of 450 to 500 v applied between the work (cathode) and the grounded metal vacuum enclosure (anode). Nitrogen ions are accelerated to the work where a thin layer of Fe4N forms on the surface and thus sets up a nitrogen concentration gradient. This causes nitrogen atoms to diffuse into the surface layers of the alloy forming a finely divided dispersion of alloy nitrides, causing hardening of the surface. In the work to be reported here. the nitriding was carried out at 550° to 600°C to be consistent with commercial nitriding practice. The temperatures cited are those measured by a thermocouple located under a platform on which the work was sitting. Except where otherwise stated, the mixture used in nitriding the binary alloys contained -2.0 pct N, balance hydrogen. The nitrogen concentration in the nitriding gas mixture used for the binary alloys was purposely kept lower than normally used in nitriding steels. 10 to 20 pct, in order to minimize Fe4N formation. In this way only the alloy nitrides would be present as a second phase. However, in the case of steels which would contain a- carbide phase along with as

Jan 1, 1969

By O. D. Gonzalez

Existing measurements for the steady-state permeation of hydrogen in a iron above 100°C have been examined for contribution of determinate errors. The analysis leads to a recommended equation for the permeability of hydrogen in a iron: o= (2.9 ±0.5) x 10-3 exp - (8400 ± 400)/RT cu cm (ntp H2) cm-1 sec-1 atm-1/2 THE permeability of a iron to hydrogen has been the subject of numerous investigations over the past 40 years, and at present there are thirteen sets of published results for the rate of steady-state permeation of hydrogen in a iron above 100°C. The numerical values in each set of results are entirely self-consis-tent, but the spread among the sets is too large to be attributed solely to experimental error, i.e., to error other than in the specimen itself. Several reasons have been advanced to explain the disparities, but to date the relative importance of experimental inaccuracy to the spread remains uncertain. The purpose of this report is to examine in detail the sources of determinate errors inherent in the experiments and to assess as far as possible the contribution of the errors to the results. The ultimate goal is the selection of values for the permeability and heat of permeation most nearly representative of hydrogen in a iron. The analysis is limited to those experiments in which the permeation rate was observed at steady state—a condition in which traps for hydrogen within the metal are filled to a fixed level15 so that the trapping mechanism is not reflected in the rate of passage of the gas. Furthermore only data are examined in which surface processes are judged to have little or no influence on the flow. It is hoped with these restrictions to obtain values of the permeability and the heat of permeation which will be as closely related as possible to the mechanism of lattice diffusion. I) DEFINITION OF TERMS; UNITS In this report the data for permeation are given in terms of a coefficient oj permeability, ?, which is defined by the equation: jt=?A/?x{p1/2-po1/2) [1] where jt is the total flow of gas normal to the surface of a membrane of planar geometry, e.g., a disc, of area A and thickness ?x; pi and po are the pressures in the input and output sides, respectively. For flow radial to the walls of a membrane of cylindrical geometry, e.g., a tube, the corresponding equation is: where 1 is the length of the cylinder, and ri and ro are the inner and outer radii, respectively. The flux normal to the surface is given by Fick&apos;s law: j= -D(dc/dx) [3] At steady state the concentration gradient will be constant, and integration of Eq. [3] gives for the total flow through a disc of area A and thickness Ax: h =-DA(co - ci) [4] where c, and ci are the concentrations of solute at the output and input surfaces, respectively. When surface control is absent, co and ci are given by Sievert&apos;s law c = Kp1/2, and substitution therewith into Eq. [4] gives directly Eq. [I] where ? = DK. Integration of Fick&apos;s Eq. [3] in cylindrical coordinates will give Eq. [2] where again ? = DK and is thus shown to be independent of geometry (provided that surface control is negligible). The coefficient of permeability, or simply the permeability,* must be expressed in proper units. In *The term permeability will refer in this report always to the coefficient defined above; permeation will be used to specify the general phenomenon of gas passage through a membrane. this report ? will be expressed in the units of cu cm (ntp H2) cm-1 sec-1 atm-1/2. The variations of D and K with temperature are given by D = Do exp(-Ea/RT) and K = KO exp(-?Hs/RT) where E, is the activation energy for diffusion and AH, the heat of solution, each usually expressed in calories per mole of solute. The variation of permeability with temperature will thus be given (for conditions where surface control is negligible) by ? = ?o exp(-?Hp/RT) where ?0 = DoKo and ?Hp = Ea + ?Hs. The units of ?0 are the same as those of 6, and??Hp will be expressed in calories per mole H. 11) SUMMARY OF PERMEABILITY RESULTS Table I gives the values reported to date for the permeability of H2 in a iron in terms of ?o and ?Hp. Except where noted the parameters listed were taken directly from the numbers reported by the various investigators with only a change in units. The temperature limits within which the listed ?o and ?Hp hold are given in column 7; the limits marked in parentheses in this column indicate the entire temperature range covered in each investigation. The listed values of ?o and ?Hp are those giving a linear plot of ln? against T-1 at the higher temperatures in each set of measurements, and thus presumably represent the case for which surface control was negligible. Column 6 gives values of 9 at a representative tem-

Jan 1, 1970

By Michel G. Drouet

Dross, a major by-product of all processes involving molten aluminum, forms at the surface of the molten metal as the latter reacts with the furnace atmosphere. It generally represents 1 to 5 wt% of the melt, depending on the process, and contains on average about 50% free aluminum dispersed in an oxide layer. Since aluminum production is highly energy-intensive, dross recycling is very attractive from both the energy and the economic standpoints. The conventional recycling process using salt rotary furnaces is thermally inefficient and environmentally non-acceptable because of the production of salt slags. Hydro-Quebec has developed and patented a new salt-free technology using a rotary furnace heated by an electric arc between two graphite electrodes, called DROSCAR®. A 600-kW pilot plant in operation at LTEE is in use to demonstrate the process. This process provides aluminum recovery rates over 90%, using a highly energy efficient, environmentally sound production method. In 1994, 400 tonnes of aluminum dross were treated in this facility and several tests on various types of dross have also been conducted in early 1995. A report on the results will be presented.

Jan 1, 1995

By E. Miller, R. Geffken, K. L. Komarek

The thermodynamzc properties oJ liquid Cd-Sb alloys were investigated using the cell arrangement measurments were obtained every 2°C at a heating and cooling rate of 12°C per hr and at equilibrium every 2O0C frorn 500°C down through the stable liquidus. The S-shaped asCd US composition curve was used in the cotnposition regzon near Cd,Sb, to calculate a tempeerture-dependent inleraction coefficient from quasichemical theory. Rapid changes in a scd were observed at a transition temperature varying from 400" to 465°C depending on con/kosition. It could not be determined if the changes in aScd were discontinuous, but tlze composition dependeke of the magnitude of the change is indicative of a second-order phase transformation in the liquid. The values of the experimental changes in ASCd are in agreement with calculations from the slope of the transition temperature, using the concept that a second-ovdev phase transition occurs in liquid Cd-Sb alloys. II is suggested that the transformalion is associated with the formation of Cd4Sb3 molecules in the liquid. ThE structure of liquid alloys is the subject of many investigations. X-ray, resistivity, and thermody-namic data have been interpreted as indicating varying degrees of short-range order in the liquid in alloy systems forming inter metallic compounds. In general, the melting process is not a transition from an ordered to a completely disordered state, but some degree of order is retained in the liquid. Maximum ordering in the liquid state occurs close to the melting temperature of the compound and the arrangement of atoms becomes more random at higher temperatures. Of special interest in this respect is the Cd-Sb system. It is one of the few metallic systems which form both stable and metastable compounds when liquid alloys are cooled at normal rates. The stable system exhibits an intermetallic compound, CdSb, melting at 459"c.l A second compound, CdrSbs, has also been reported,&apos; melting close to this temperature. The metastable system has one compound, CdsSbz, melting at 420"c.I Resistivity measurements on liquid Cd-Sb alloys close to the liquidus temperatures have been interpreted in terms of a complex ordering behavior which changes rapidly with increasing temperature.3 The resistivity-composition curve is characterized by two maxima corresponding in composition to CdSb and CdsSbz. The resistivity-temperature plots show sharp breaks for alloys in the composition range of 45 to 70 at. pct Cd on cooling through a transition temperature close to the stable liquidus. Fisher and phillips4 investigated the influence of temperature and composition on the viscosity of liquid CdSb alloys. The viscosity of some alloys increases sharply on supercooling below the stable liquidus. A maximum in the viscosity-composition curve occurs at the composition CdSb. The thermodynamic properties of liquid Cd-Sb alloys have been investigated by Seltz and ~e~itt&apos; and Elliott and chipmane by the electromotive-force method and their results are in good agreement. However, these investigations were carried out at temperatures well above the liquidus temperatures of the alloys, and the temperature coefficients of the electromotive force, dE/dT, were obtained from experimental points for each alloy at a few temperatures considerably above the liquidus temperature. Scheil and ~aach&apos; investigated the thermodynamic properties of this system by the dew point method in the temperature range from about 100°C above the stable liquidus down into the supercooled liquid region. They reported several anomalies, i.e., the activity of a melt on heating differed from that on cooling, and the activity increased sharply in the limited temperature interval immediately above the liquidus temperature of the stable alloy, followed by a sudden decrease below the liquidus. Values obtained on heating and cooling were not in agreement. A reinvesti-gation of a few alloys by Scheil and Kalkuhl&apos; by the electromotive-force method failed to confirm these observations. The authors concluded that the anomalies were due to inhomogeneities in the starting alloys and they discarded their previous results. The present investigation was undertaken in order to obtain thermodynamic data close to the liquidus temperature and in the supercooled region where the anomalies were originally reported, employing the electro motive-force method. This method is quite precise and will most easily permit observations of small changes in activity and partial molar entropy with temperature. Measurements were taken every few degrees so that the dE/dT values could be calculated over the entire temperature range and small changes in the thermodynamic properties close to the liquidus temperature could be observed. I) EXPERIMENTAL PROCEDURE Specimens were prepared from 99.999+ pct Cd and Sb (Cominco). Surface oxide was removed by scraping and then melting the metals under vacuum and filtering through Pyrex wool. Appropriate amounts of the metals were weighed on an analytical balance to k0.1 mg, sealed in double Pyrex capsules under vacuum,

Jan 1, 1968

By Peter Halbach

Hydrothermal activity is well known from many locations on most mid-ocean ridges, however no hydrothermally mineralized area had yet been found at the ultraslow spreading southwest Indian Ridge up to October 98 when the Japanese RV Yokosuka with the submersible Shinkai 6500 investigated this area. A massive sulfide field was discovered near 27º51S / 63º56 E in the 11th segment west of the Rodriguez Triple Junction. The Free University of Berlin had joined this cruise and taken over the responsibility for the study of the respective sulfide mineralizations. Hydrothermal minerals were sampled during two dives at water depth of about 2940 m close to the summit of an axial volcanic ridge called Mount Jourdanne. There massive sulfides occur on the seafloor as small smooth mounds with an average area of about 5 m2. Their surfaces are weathered and have a reddish to brownish colour. In addition to these mound-like structures, small tube-like chimneys were observed. These chimneys rise approximately 30 to 40 cm above the floor and are less than 10 cm in diameter. No indications of hydrothermal fauna could be detected. All the hydrothermal features are spatially related to faults and smaller fissures controlled by an E-W trending graben system crossing the summit region of the submarine volcano. Such tectonized areas are generally considered to be ideal for hydrothermal activity because they may have both a magmatic heat source in the deeper underground and pathways for fluid circulation, respectively.

Jan 1, 2001

By Haijian Shi, Drew Pizzo

This article focuses on the appropriate application of subsurface investigation methods for transmission structures, which are typically designed to resist lateral rather than vertical loads. Currently, the three methods used most often for the subsurface investigation of transmission structures in the field are the Standard Penetration Test (SPT), the Cone Penetration Test (CPT), and the Flat Dilatometer Test (DMT). Each of these methods has advantages and disadvantages, and each is more applicable to some scenarios than to others. To gain a better understanding of these test methods and the implications of using them for various kinds of applications, a comparison study was conducted in the field in Maryland, for three boring locations. Each boring location was explored using each of the three tests as stated. The results of the tests and lessons learned are presented and compared, and these comparisons show that the three test methods agree on the majority of the findings. The results from each test method were also used to derive key parameters such as the soil friction angle for given foundation designs considered in order to establish a clear basis for comparison. Recommendations for performing transmission structure subsurface investigations are made in order to optimize the use of each method and thereby optimizing subsequent foundation designs. INTRODUCTION For overhead transmission structures, the most important structural requirement for determining the foundation design differs from the requirement for other structures such as buildings and bridges in accord with the conditions the transmission structures will need to withstand. In addition to the ability to bear a given vertical load consistent with its use, the foundation must bear lateral loads arising from wind and other weather conditions. The foundation types used most often for overhead transmission monopole structures include concrete drilled pier, vibratory caisson, and direct embedment. In order to determine an appropriate and even an optimum foundation design for any given set of conditions, an appropriate subsurface investigation method or approach is needed. Currently, the standard penetration test (SPT), the cone penetration test (CPT), and the flat dilatometer test (DMT) are the three most commonly used subsurface investigation methods.

Jan 1, 2018

By N. D. L. Burger

Underwind and overwind protection system concepts for mine hoist shafts were developed in conjunction with and for the Safety in Mines Research Advisory Committee (SIMRAC). End-of-wind operation of mine hoists is the most hazardous aspect of mine hoisting, carrying the highest risk of loss of life, injuries to workers and loss of production. Systems operating mechanically and with local actuation were developed. This was done in order to remove the increased risk associated with dependency on remote or external energy and information supply associated with most existing protection systems. The proposed underwind protection system concept absorbs the energy of motion of a conveyance overrunning the design lower limit of travel by drawing a metal strip through a set of rollers. This action causes dynamic cyclic plastic bending of the strip material that converts the kinetic and potential energy of the conveyance into strain energy of the metal. In the concept design a pair of steel wire rope slings attached to the strips catch the overrunning conveyance and transfer the retardation force. The proposed overwind protection system concept absorbs the energy of motion of a conveyance overrunning the design upper limit of travel by early detaching of the conveyance from the hoist rope. This detaching is carried out via an additional detaching hook activation mechanism fitted at a sufficient height below the spectacle plate to allow the conveyance to retard to standstill under gravity before it would crash into the spectacle plate. The conveyance so brought to rest is prevented from falling by means of jack catches on the conveyance interacting with a rack (toothed profile) fitted on the guide rails in the retardation zone. Scale models (1:10 scale) of both protection systems were designed to conform to established retardation standards. The retardation standards were limited by the requirement of passenger safety in retarding cages. The models were then built and tested in a1:10 scale shaft model. Retardation performance close to the required levels was achieved. The retardation distance required should allow such systems to be retrofitted in most existing shafts. Given the simplicity and robustness of the designs, further development was recommended because of their enhanced self-sufficiency and reduced risk of malfunction. Keywords: underwind, overwind, deceleration, mineshafts, hoisting.

Jan 1, 2004

By Rolando Campos

The CODELCO-CHILE Teniente Converter Technology, is presently being applied in four Chilean smelters (Caletones, Chuquicamata, Potrerillos and ENAMI-Ventanas). A Teniente Converter is due to be used at ENAMI-Hernan Videla Lira (Paipote) smelter in the near future. Also, a Teniente Converter is to be installed as part of a retrofit project for Nkana smelter of Zambia Consolidated Copper Mines Ltd. (ZCCM). The charge to be treated through this smelter will consist of a blend of concentrate arisings from the various concentrators within the ZCCM group. The present status on the application of the Teniente Converter Technology at Caletones smelter as well as its projected performance when used at Nkana smelter, are presented in this paper. The design operational basis, autogenous smelting throughputs, concentrate to matte ratios and benefits due to the use of technical oxygen, are presented and analysed.

Jan 1, 1992

By J. E. Steiner, J. M. Hodge, M. A. Orehoski

Ingots of four steels (1045, 1080, Ni-Mo-V, and Ni-Cr-Mo-V) were cast at pressures varying from about 1 to 760 mm of mercury, so as to obtain a range of hydrogen contents in each steel. The susceptibility of these steels to flaking was evaluated by cooling hot-rolled blooms at a range of cooling rates, varying from water quenching to slag cooling, and studying the occurrence of flaking as a function of cooling rate. The steels exhibited differences in susceptibility to flaking, and a tlzreshold value for hydrogen content for each steel was found, below which the susceptibility was very low and above which the susceptibility increased markedly with increasing hydrogen content. Mechanical property evaluations, metallogvaplzic exantinations, and X-my diffraction determinations o,t retained austenite were made on samples from the blooms. A mechanism of flaking which is consistent with the observed behaviors, the effects of hvdrogen content, and the differences in susceptibility among the steels investigated is postulated, based on the results of mechanical property evaluations and metallographic and X-ray diffraction studies. ThE important role of hydrogen as a factor in the occurrence of "flakes" or "hair-line cracks" in steel has now been established by many investigations. These have included investigations by steel producers and forging manufacturers, to whom the prevention of flaking is a very real and serious problem, and many research studies aimed primarily at establishing the mechanism of this behavior Several investigators3 have reported that steels cast at reduced pressures (absolute pressures of about 1 mm) not only are low in hydrogen content but are essentially insensitive to the formation of flakes. These investigations have shown that a general relationship exists between hydrogen content and susceptibility to flaking. The difficulty of obtaining suitable samples of steels of a given composition with the desired range of hydrogen contents, particularly in the relatively large sections in which flaking most commonly occurs, has been the principal obstacle to quantitative evaluations of these relationships. Steels with intermediate hydrogen contents between 1 ppm, and the 4ppm or higher of air-cast steels are generally not available in commercially produced steels. Laboratory procedures, in which the hydrogen is introduced into solid steel samples by heating in a hydrogen atmosphere under pressure, generally involve a limitation in the size of the sample which can be treated, and thus are not representative of the behaviors in large sections. The availability of a facility at the South Chicago Works of U.S. Steel, in which several ingots could be cast from a single heat of steel at total air pressures ranging from 0.25 to 760 mm of Hg, has made it possible to overcome this obstacle and to obtain ingots of a given steel covering the intermediate range of hydrogen contents desired. These ingots, furthermore, are of a size suitable for the production of product with section sizes large enough to be representative of the products in which flaking most commonly occurs in commercial production. In these experiments, this facility was used to study the relationships between hydrogen content and the susceptibility to flaking of four steels, two plain carbon steels at 0.45 and 0.80 pct C and two low-carbon alloy steels representing a medium and a rather high hardenability level. These flaking studies were supplemented by evaluations of mechanical properties and by metallographic studies on samples from the blooms, in order to obtain pertinent information on the factors other than hydrogen content which influence the susceptibilities of these steels to flaking. Based on the results of these tests, a mechanism for the initiation and propagation of the flaking cracks, which is consistent with the observed behaviors, is postulated. MATERIALS AND EXPERIMENTAL WORK Steelmaking and Conversion. To provide material for the investigation, five 29- by 35-in., hot-topped, big-end-up ingots were cast from each of four 80-ton, basic electric-furnace heats of four different steels (a 1045 steel, a 1080 steel, a Ni-Mo-V steel, and a Ni-Cr-Mo-V steel). A double-slag practice was used on all steels and the two plain carbon steels were Si-A1 deoxidized with an addition of 2 lb of A1 per ton, while the Ni-Mo-V and Ni-Cr-Mo-V steels were deoxidized only with silicon and

Jan 1, 1964

By R. S. Dean

A large metallurgical experiment station at Salt Lake City to house the works of the Bureau of Mines in the intermountain area properly has long been projected. It finally became possible when a Public Works Allotment of $300,000 was set aside for building and equipment. With the new building assured, the Bureau of Mines decided to move the headquarters of its Metallurgical Division from Washington, D. C., to Salt Lake City, Utah. It was felt that this move would simplify they administrative work of the chief engineer of the division, as all stations devoted primarily to metallurgical work are west of the Mississippi. These include Rolla, Mo.; Minneapolis, Minn.; Pullman, Wash.; Reno, Nev.; Berkeley, Calif.; Boulder City, Nev.; and Tucson, Ariz. In addition to these stations will groups, of investigators working on metallurgical problem, are maintained at Pittsburgh, Pa., and College Park, Md. Salt Like City was clearly a more central point for the direction of this scattered work than Washington, D. C. The building (fig. 1, A and B) was designed from general plans worked out by the authors of this paper. Contraction was begun in March of 1939, and by the end of the year the Metallurgical Division had moved, into its now quarters.

Jan 1, 1940

By E. J. Schneider

In view of the current interest in the constituents of low-temperature tar, the Synthesis of three known xylenols and their hydroxyacetic acid derivatives has been undertaken by the U. S. Bureau of Mines. One of these xylenols, the 1,3,2 derivative first reported by Steinkopf and Höpner,4 has been described by Brown and Branting.5 The other two derivatives, the 1,3,5 first reported by Schütz6 and the 1,2,3 reported by Steinkopf and Höpner, have now been studied in greater detail. In the present work the synthesis of 1,2,3-xylenol and 1,3,5-xylenol was repeated, with some improvements in the former. The hydroxyacetic acid derivatives were also prepared, and it was found that while the melting point of the 1,2,3 derivative agreed with that of Steinkopf and Höpner. that of the 1,3,5 derivative was found to be 111° instead of 85 to 86° as reported by Schütz, by Steinkopf, and later by Bruckner. The discrepancy between the melting-point figures is doubtless due to differences in the purity of the xylenols used in the synthesis of the acids. Schütz obtained his 1,3,5 acid by recrystallizing an impure sample obtained from a mixture of xylenols. The difficulty of obtaining a pure acid by starting with a mixture is demonstrated by Bruckner, who despite painstaking efforts was unable to obtain the pure 162.5° melting 1,2,4 isomer from a mixture that persistently melted at 138° C. Steinkopf did not repeat Schütz&apos;s work but merely used the latter&apos;s figures in compiling a table. Bruckner, on the other hand. apparently also made the acid (by an improved method), and it is difficult to explain his checking Schütz&apos;s figure, unless it is that he, too used a symmetrical xylenol obtained from a tar and not prepared synthetically, as was the one reported in this paper.

Jan 1, 1929

By Richard S. Olsen

Prior work by the Bureau of Mines demonstrated a feed preparation method that eliminates the formation of slime during leaching of calcined kaolinitic clay and makes leached residues fast settling and easy to filter. Nitric acid leaching rates determined for calcined kaolinitic clay prepared by this method were found to correspond to a zero-order reaction model for both batch and continuous, stirred-tank leach-ing. A rate constant of 0.136 min-1 was determined. Separation of solid residues from the reacted slurry was examined, and filtration rates were determined. Permeabilities of the flocculated, leached residues were around 51 darcys, or 5.0 x 10-7 cm2 for laminar flow through 4-ft-deep beds.

Jan 1, 1983

By Walter Kawa

In connection with its research in producing synthetic liquid fuels from coal, the Federal Bureau of Mines studied reactions of iron and iron compounds with hydrogen and hydrogen sulfide in batch autoclaves. The Bureau hoped to gain indirect evidence regarding the chemical changes that iron catalysts undergo when they are used in the hydrogenation of coal. The information obtained may be helpful in identifying the active form or forms of iron catalysts. At 450° C., with hydrogen at hundreds of atmospheres and hydrogen sulfide at 1 or 2 atmospheres, the thermodynamically stable form of iron is ferrous sulfide in the case of the metal, magnetite, ferric oxide, ferrous sulfate, ferrous oxalate, or the chlorides of iron. However, complete conversion to ferrous sulfide was not achieved at temperatures of 400° to 500° C. for kinetic reasons. Extensive sulfiding of iron, magnetite, ferric oxide, and ferrous oxalate occurred below 400° C., and some conversion of ferrous sulfate to ferrous sulfide occurred at 400° C. In the hydrogenation of coal, ferrous sulfide is the form of iron likely to be available for heterogeneous catalysis when starting with the metal, oxide, sulfate, or oxalate.

Jan 1, 1960

By L. A. Neumeier

The Bureau of Mines evaluated the properties of a Zn-0.75 pct Cu-0.12 pct Ti alloy extruded at temperatures between 400° and 720° F. The extrusions were made with a reduction ratio of 28-to-l and at relatively slow speed. Rod was also extruded at 560° and 640° F with a reduction of 255-to-l. With increased extrusion, temperature, extrusion pressures decreased substantially and creep resistance of the rod improved significantly. Coefficients of thermal expansion were low in the long rod dimension. Microstructures, hardness, and tensile properties were also evaluated, and a limited evaluation was made of bend ductility at 32° F for the rod extruded with the 255-to-1 reduction.

Jan 1, 1969

By Alfred W. G. Wilson

THE state of development of its iron and steel industries serves as a 1eading index to the general condition of a nation&apos;s business affairs. In this paper, the authors present an economic study of the progress of this group of industries in Canada for the decade 1927-1936. The statistical data and most of the tables which accompany this article have been com-piled by John Casey, Statistician, Bureau of Mines; the text and some of the computations have been prepared by the seni0r author. The principal source of statistical information has been the publications of the Dominion Bureau of Statistics; where other sources have been consulted, they are noted in the text. All weights are given in short tons. Records for the years 1913 and 1918 are also presented in the group of tables dealing with iron ore and pig iron; they will serve as a basis for comparison with nearly normal years in the two decades prior to 1927-36, which included the abnorma1 years of the Great War. GENERAL REVIEW At the beginning of the decade under review, this group of industries had returned to almost normal production, as determined by pre-war conditions. Iron ore consumption showed a steady increase between 1927 and 1930; a marked decline began in 1930 and reached its culmination in 1932, when the recorded consumption of ore was 293,353 to11s, about 16 per cent of the average consumption during the first four years of the decade; the last four years of the decade show a gradual increase in consumption; the amount of ore used in 1936 was still slightly below the amount used ten years before, in 1927 (see Table 1, top).

Jan 1, 1938

By Barrie C. Butt

The opportunity for an exploration geologist to follow a successful exploration project through the feasibility, financing, construction, development and exploitation phase is rare. In addition, it is not often that the exploration geologist can be present during the mining of a deposit to explain why certain actions were taken or interpretations made and to find out how these interpretations turned out in actuality. At the Woodsreef chrysotile asbestos mine in New South Wales, Australia, mining has been in progress for six years and the writer has been intimately associated with the project during the five years of exploration and the six years of exploitation. The industry is possibly aware of the fact that the Woodsreef Mine has had major production problems, the majority of which have stemmed from the unique characteristics of the ore body and of the fibre. Because of these unique features, a large volume of research has been undertaken by Woodsreef and by other scientific organisations in Australia, England and Canada on the Woodsreef fibre. The answers to some of the problems have negated some semi-sacred concepts of asbestos ore milling and led to the development of new techniques, such as the adoption of microscopic fibre counts as a routine procedure; the modification of accepted evaluation procedures; the development of new machines for dedusting fibres, and to the recognition of a fibre with a unique milling behaviour pattern and, possibly, properties. The problems experienced can be divided broadly into those associated with the geology and those associated with the physical properties of the fibre. It is possible that the same features may manifest themselves in other deposits around the world, and if they can be recognised during the exploration stages a feasibility evaluation may be just that little closer to the actual.

Jan 1, 1978

By H. W. St. Clair

In about 1930, Degussa applied for a patent on a process for the of oxides, carbides, sulfides, and other nonmetallic impurities by filtration in the molter state. The filtering media listed were wire screen, coke, and ceramic materials, and quartz. It was also suggested that filtration might be combined with chemical reaction between the metal and the filter medium or that might be added to the system. No patent was granted on the general scheme, but several years later a patent was granted on a continuous process purification of crude light metals, especially or alkali earth and their alloys. The melt was stirred at 1 temperature at which the impurities (such as oxides and salts) remained solid and the metal was drawn through a filter tube. The impurities collected under the filter and were removed by a screw conveyor. Crude sodium was purified by this process in Degussa&apos;s Knapsack plant. During the last war, when the refining of scrap became a very urgent Problem in Germany, experimental investigations were extended to separation of other metals and metallic compounds by filtration. Preliminary experiments seemed to confirm the opinion of Dr. L. Weiss that the principles of wet chemical filtration might be applied to a great extent in the purification of metal and alloys.

Jan 1, 1949

By William H. Mount

INTRODUCTION Effective mine ventilation is required to maintain a healthy underground environment for humans. Without effective ventilation, the environment can become unhealthy or hazardous as a result of the depletion of oxygen, contamination with toxic gases, or the buildup of an excessive amount of particulate matter (dust). Each contaminant has an upper limit of concentration that should not be exceeded within an 8-hr period. This is known as the threshold limit value (TLV). The TLV represents an acceptable level of exposure that should produce no ill effects. Unfortunately, more than one contaminant may be present at any one time and the effects of the individual contaminants may be additive, i.e., the effects of each contaminant must be considered simultaneously to determine the potential danger to miners. Possibly the greatest threat to mine-air quality is the uncontrolled underground use of the diesel engine. The diesel engine was invented in 1892 by Rudolf Diesel. His intention was to develop a power source that could burn coal dust as a fuel, but he was unsuccessful in that attempt and had to resort to liquid petroleum fuels (Johnson, 1975). In 1898, the diesel engine was intro¬duced into the United States by Adolphus Busch, who anticipated using it as a prime mover in factories and generating plants. At that time, the diesel engine was a very large and very heavy engine, designed for fixed installations. By 1919, lighter engines were being developed, and by 1931, Caterpillar was marketing a diesel-powered, track-type tractor (Henderson, 1975). Since 1931, the diesel engine has evolved into an extremely popular prime mover in medium and heavy-duty applications. Efficiencies now are on the order of 40% and improvements such as turbocharging and aftercooling have produced engines capable of generating power at a ratio of 0.3 kW/kg (1.0 hp per 5.0 lb) of engine weight. Although the diesel engine is relatively efficient as a mobile power plant, it is far from efficient in terms of the energy produced from the energy potential of the fuel. About 60% of the heat value of the fuel leaves the engine as wasted heat, with about 50% of that heat being emitted through the exhaust pipe and the other 50% being emitted through the radiator or cooling fins. Perfect combustion in an engine would produce only water vapor (H_0), carbon dioxide (CO_), and nitro¬gen (N2) as the byproducts. Since the diesel is not a perfect engine, each pound of fuel burned generates 5.6 m° (200 cu ft) of exhaust gas, containing about 0.009 m3 (0.33 cu ft) of carbon monoxide (CO), 0.009 m&apos; (0.33 cu ft) of nitrogen oxides (NO, NO2, and NOD), and 0.57 m3 (20 cu ft) of carbon dioxide. The balance of the exhaust emission consists of free nitrogen and water vapor (Hurn, 1975). Contrary to popular belief, the diesel is not inherently dirty. Under normal operating conditions, a well-maintained engine neither smokes nor smells. However, the same well-maintained engine can and does produce toxic emissions. A diesel engine is not inherently safe and constitutes a distinct hazard to personnel. This chapter is devoted to a description of the various toxic substances that may be generated by a diesel engine. Although some of these substances may also be produced by blasting or natural causes, the focus of this chapter is on the relationship between the internal- combustion compression-ignition engine (the diesel) and the quality of the mine air. CARBON MONOXIDE Combustion Process During the combustion process (burning) of organic fuels, each atom of carbon combines with two atoms of oxygen, provided that a surplus of oxygen atoms is available. Thus, the carbon is oxidized to carbon dioxide. Most open flames, such as trash fires, camp fires, gas ranges, etc., produce carbon dioxide. However, with insufficient oxygen, incomplete combustion results as the carbon atoms each combine with one atom of oxygen to produce toxic carbon monoxide. Burning charcoal briquettes produce carbon monoxide because the combustion takes place inside the briquettes where sufficient oxygen is not available to the combustion process. Internal-combustion engines, whether burning gasoline or diesel fuel, also produce carbon monoxide. The only oxygen available to the combustion process is that trapped within the cylinder. If the amount of fuel delivered to the cylinder is excessive, there is insufficient oxygen for complete combustion and carbon monoxide production results. In a normally aspirated (nonturbocharged) diesel engine, the amount of air "sucked" into a cylinder is the same on every intake stroke, resulting in complete combustion only at low levels of engine loading, when small amounts of fuel are injected. Higher levels of engine loading cause larger amounts of fuel to be injected into the same volume of air in the cylinder. Unless the volume of air is increased, the combustion process becomes progressively less complete as the amount of fuel increases. Turbocharged engines are able to compensate some¬what for increased loading and increased fuel consumption. The turbocharger acts as a compressor for the intake air, forcing a larger volume of air into the cylinders as the engine speed increases. Hence the turbocharged engine burns cleaner than a naturally aspirated engine and produces slightly less carbon monoxide (Marshall and Fleming, 1971). Much of the underground equipment used today is powered by turbocharged indirect-injection diesel engines. Although these engines emit fewer toxic contaminants than naturally aspirated engines, they do not eliminate the problem. Since the turbocharger is driven by the exhaust gases, rapid accelerations can cause temporary overfueling of the engine until the turbocharger attains a speed sufficient to restore the correct air-to-fuel ratio. During this "turbocharger lag," the combustion cylinders contain insufficient oxygen, causing severe smoking and an increased output of carbon monoxide.

Jan 1, 1982

By M. J. Blackburn

The phasal equilibria in TI&apos;:Al alloys has been studied Ry transmission electron microscopy, electron diffraction, and X-ray diffraction. It is shown that three-phase fields exist below the transformation, viz.: a disordered hexagonal solid solution a; an ordered hexagonal phase based on Ti3Al, aa; and a two-phase region. (a + (YZ) , occurring between the single-plzuse fields. The size. disiribution, and morphology of- the a, phase in the two-phase region is shown to be dependent upon the alloy composition and heat treatement. The ordering process in the a, phase leads to the formation of anliphase domain boundary networks; the contrast and stability of these networks is shown to be dependent on alloy composition. A new and relatively simple phase diagralil for the systemm is constructed. The phasal equilibrium at the titanium-rich end of the Ti:Al system has long been the subject of considerable controversy. crossleyl has recently reviewed the phase diagrams that have been advanced for the system and in his turn proposed yet another one. There would seem to be general agreement that a phase exists at a composition at or near Ti& with an ordered hexagonal DO,,-type structure. However, several other phases have been proposed; for instance, Ence and ~ar~olin&apos;s&apos; diagram includes two phases, Ti2A1 and Ti3A1, in the region up to 25 at. pct Al. The position of the proposed phase boundaries varies over a considerable compositional and temperature range, a point graphically illustrated in Fig. 1 of Crossley&apos;s paper.&apos; It is perhaps germane to briefly examine the techniques used by other workers in the establishment of the phase structure. These fall into three categories: 1) X-ray diffraction, the only limitation of which is the rather low intensity of superlattice reflections in this system.3 Thus, superlattice reflections become increasingly difficult to detect in the more dilute aluminum alloys. 2) A considerable amount of optical microscopy has been performed"2&apos;4 and it will be shown in a later section that many of the obscure mi-crostructures that have been observed can be attributed to hydrogen contamination. It is concluded, therefore, that such observations should be interpreted with considerable care. 3) The variation of some physical property with aluminum content has been measured.5"7 These methods are a useful indication of the existence of a transformation, but are usually insufficient in themselves to identify the transformation. The results using these techniques will be considered in more detail in the discussion. In this paper, the phase structure of alloys containing up to 25 at. pct A1 has been studied by transmission electron microscopy and X-ray techniques, and the results are used to generate a new and relatively simple diagram for the titanium-rich end of the Ti:Al system. EXPERIMENTAL A series of alloys containing 5.05, 10.16, 13.39, 13.99, 14.40, 20.83, and 25.05 at. pct A1 were obtained in the form of hot-rolled sheet 0.02 in. thick. These alloys contained 0.10 to 0.15 pct 0. Thirty-gram arc-melted buttons were prepared from iodide titanium and 99.99 A1 which contained 16.1, 16.9, 18.2, 19.0, 21.6, 22.2, 23.0, and 23.9 at. pct A1 and had an average oxygen content of 0.03 pct 0. The differences in oxygen content did not appear to influence the nature of the phase transformations which were found. Oxygen content may affect the temperature of these transformations, but insufficient samples of the high-purity alloys were examined to answer this question. The heat treatment of alloys was performed in dynamic atmosphere and vacuum furnaces or in helium -filled silica capsules. A special vacuum furnace was constructed to provide a high quenching rate in which rates of 4000°C per sec were obtained using water as the quenching medium. As pointed out by Crossley,&apos; it is important to avoid heat treatment in the a - [} phase field as the resultant segregation of the alloy into the two phases containing different amounts of aluminum can persist through subsequent treatments leading to ambiguous results. It will be demonstrated later that step cooling of specimens from the a phase region can also lead to anomalous effects. Thus, all solution treatments were carried out in either the a or 3 phase fields followed by water quenching and subsequent isothermal annealing at various temperatures. X-ray analyses were performed on a diffractometer on fine-grained bulk specimens. The value of long-range order parameter, S, wa_s calculated from the integrated intensity of the (1211) reflection. In general, the intensity of the (1011) superlattice reflection was compared with that of the (2021) fundamental reflection to correct for experimental differences between measurements. Thin foils for electron microscopical examination were produced by electropolishing using the technique described in an earlier paper.8 Dark-field techniques were employed to a large degree in this investigation using the gun-tilt method. Finally it should be noted that the lattice parameters of the D01,-type superlattice are approximately related to the disordered hexagonal phase parameters by Crf - c, and 2ad - a, where the subscripts s and d refer to the ordered and disordered unit cells, respectively.

Jan 1, 1968

By Carl Altstetter, Emmanuel deLamotte

The influence of an external stress and plastic deformation on the allotropic transformation of single crystals of a Co-30.5 pct Ni alloy was investigated. Experimental results were obtained from dilatometry, X-ray diffraction, and optical and electron microscopy. The effects of stresses could be conveniently divided into three stress ranges. In range I, from 0 to about 400 g per sq mm, the specimens exhibited a multi-variant phase change on cooling and a considerable amount of retained cubic phase. In range II, from 400 g per sq mm to the elastic limit, hexagonal regions of a given orientation grew in size and the cubic phase disappeared with increasing stress level. In range III, just above the elastic limit, specimens transformed into hexagonal single crystals. It was found that plastic deformation, not applied stress, was the factor which determined whether a single-crystal product was formed. The observed macroscopic shear directions were mainly (112) on cooling, but the behavior was more complicated on heating under stress. To explain these properties of the phase change, a model based on the nucleation of partial dislocations is proposed. IT is well-known1 that, on heating, hcp cobalt transforms into an fcc arrangement by shearing on close-packed planes. The crystallographic orientation relationship of the phases is as follows: the habit plane is (OOO1)hcp ?{lll}fcc and a (1010)hcp direction is parallel to a (112)fcc direction. The temperature at which the transformation occurs in pure cobalt is around 420.C 1,2This temperature decreases with increasing nickel concentration: and at about 30 pct Ni it reaches room temperature. However, many of the transformation characteristics remain essentially the same, particularly the crystallographic features.495 A convenient way of studying the transformation is to alloy cobalt with nickel, thus avoiding the difficulties of doing experiments at the high temperatures needed to transform pure cobalt. Due to the hysteresis of the transformation it is possible to choose a Co-Ni alloy with an Ms temperature below room temperature and an A, temperature above room temperature. Either structure of such an alloy could then be studied at room temperature, depending on whether it had just been heated or cooled to room temperature. The choice of nickel is further favored by the small difference in lattice parameters between cubic cobalt and nickel and the similarity of their physical, chemical, and electronic properties. Co-Ni alloys are reported to have neither long- nor short-range order.6 The main purpose of this work was to investigate the influence of an external stress on the transformation characteristics of Co-Ni single crystals. It may be expected that slip, twinning, and transformation should have many features in common in cobalt, because the (111) planes of the cubic phase operate as slip planes when plastic deformation by slip occurs, they are the twinning planes, and they are the habit planes for the transformation. Many previous investigators7-&apos;6 have concluded that dislocations must play an important role in the nucleation and propagation of the transformation, just as they do for slip and twinning propagation. An external stress will affect their motion, and a study of its influence should yield further information about the atomic mechanism of transformation. The present work extends that of Gaunt and christian17 and Nelson and Altstette18 in both qualitative and quantitative effects of stress. The basic concept underlying all the present theories of the transformation of cobalt and Co-Ni alloys is the motion of a/6<112> partial dislocations over {1ll} planes of the cubic lattice. The ABCABC... stacking of the close-packed planes of the cubic phase can be changed into the hexagonal ABABAB... stacking by the sweeping of an a/6 <112> partial on every second plane. Twinning, on the other hand, requires a shear of a/6 <112> on each close-packed plane. The reverse transformation can be effected in a similar way by a/3 (1010) dislocations moving over every other basal plane of the hexagonal phase. Transformation theories2, 7- 12,14 differ in the details of the nucleation of the transformation and the propagation of the partial dislocations from plane to plane. EXPERIMENTAL PROCEDURE Nickel and cobalt rods supplied as 99.999 pct pure were induct ion-melted together under a vacuum of about 10-5 torr in a 97 pct alumina crucible. An alloy containing 30.5 pct Ni was found to have the desired transformation range, with an Ms near -10°C and an j4s in the vicinity of +10O°C. The ingots were swaged to &--in. rod and electron beam zone-leveled in a 10-6 torr vacuum. This procedure resulted in 12-in.-long single fcc crystal rods (designated I to VII) from each of which several tensile specimens of identical orientation were made. Chemical analysis of the bar ends indicated no contamination or gross segregation and no micro segregation was seen in electron micro-probe scans. Tensile specimens with a 9/32-in.-sq by 1-in.-long gage section were spark-machined from the rods and then electropolished or chemically polished to remove the machining damage and to provide a flat surface

Jan 1, 1970