Search Documents

By Nural Kuyucak, Bohumil Volesky

"Extensive screening revealed a seaweed (alga) biomass type which in its non-living state possesses a very high cobalt sequestering capacity comparable to that of activated carbon and the ion-exchange resin currently used in the cobalt production process. Performance of the new bio-sorbent material was studied by examining its equilibrium metal uptake isotherms generated under different solution conditions such as initial cobalt concentration pH, temperature, and the presence of selected cations and anions. The rate of cobalt uptake was determined, which is a crucial parameter for recovery process design. Almost all cobalt sorbed can also be desorbed with a solution of CaCI2. The bio-sorbent material can be used repeatedly in the sorption-desorption cobalt concentration process. IntroductionIt has been well documented that certain types of microbial biomass, living or non-living, possess a high potential to sequester and accumulate inorganic ions present in aqueous solutions. Metal concentration by microbial biomass from a solution is termed bio-sorption. This phenomenon is quite complex and includes adsorption of metals onto the surface of a microorganism and/or into the cellular structure in combination with ion-exchange, complexation, and/or micro-precipitation. Bio-sorption is generally considered to be a rapid physical/chemical process. The cell wall structure is porous and allows metal ions, as well as large organic nutrient molecules, to pass freely through. Polysaccharides of the cell wall could provide binding amino, carboxyl, phosphate and sulphate groups. In addition to these functional binding groups, polysaccharides often have ion-exchange properties. Sometimes, bivalent cations, such as Ca2+ or Mg2+, help the formation of ionic bond bridges between the negatively charged cell surfaces and positively charged cations in the solution, Proteins in the cell wall could offer functional groups and also offer peptide bonds to bind ions. Interactions between metal and the cell wall components are responsible for the sequestering of metals by way of bio-sorption. Many metals feature a complex solution chemistry and it is not always possible to determine what ionic species are actually present in the solution. The equilibria involved are dependent on pH, concentration, the anions present and other factors. The transport system for the ions are sometimes dependent on both temperature and energy. Biosorbent material could also be regenerated for multiple reuse."

Jan 1, 1988

By L. Hutton, S. W. Colley

"The release of soluble salts of base metals from acid mine pits and in the waste water from metal refiners is an avoidable source local pollution and contamination. Tightening of the regulations controlling natural resource extraction and industrial wastewater discharge is mandating the removal and recovery of metals from waste streams, and the remediation of contaminated sites. There is an economic incentive in recovering the valuable copper and nickel, as the value of the recovered metal can offset remediation costs and for high flow waste streams can be a source of income. Extraction of metals from waste streams by conventional Ion Exchange and chelation resins is widely practised, but has limitations on applicability in complex and dilute feeds due to the structure and properties of polymeric resin beads. Composite Advanced Ion Exchange (AIX) materials have been developed for the recovery and purification of base metals from base metal mining and metal processing industries. A silica-composite based resin has been developed for the selective extraction of copper from high iron containing feeds. This resin can be eluted with sulfuric acid yielding a copper stream suitable for return to solvent extraction or to electrowinning. We describe the development and application of the resin and process to two acid mine drain feeds of varying copper and iron concentrations, and show that the copper concentration can be considerably upgraded even at small scale with a final metal content of >95% copper.INTRODUCTIONWaste water with high sulphate concentrations, low pH and containing complex and variable mixtures of metals is an inevitable product in the mining, extraction and metal refining industries. One problematical water source is Acid Mine Drainage (AMD) which in addition to the metals of interest also contains a wide range of contaminating elements. Purge streams from metal refining are less complex in composition but contain significant quantities of the value metals. The typical treatment of such waste streams is treatment with lime to increase the pH of the water, precipitating the dissolved metals and sulphate as a sludge of mixed metal oxides/hydroxides and sulphates. The process is effective in producing a water stream that can be safely discharged but if there are significant concentrations of value metals such as copper, nickel, zinc then there can be a considerable loss of metal value."

Jan 1, 2016

By Herbert Clark Hoover, Lou Henry Hoover

QUESTIONS as to the methods of smelting ores and of obtaining metals I discussed in Book IX. Following this, I should explain in what manner the precious metals are parted from the base metals, or on the other hand the base metals from the precious'. Frequently two metals, occasionally more than two, are melted out of one ore, because in nature generally there is some amount of gold in silver and in copper, and some silver in gold, copper, lead, and iron ; likewise some copper in gold, silver, lead, id iron, and some lead in silver ; and lastly, some iron in copper2. But I will begin with gold. Gold is parted from silver, or likewise the latter from the former, whether it be mixed by nature or by art, by means of aqua valens3, and by powders which consist of almost the same things as this aqua. In order to preserve the sequence, I will first speak of the ingredients of which this aqua is made, then of the method of making it, then of the manner in which gold is parted from silver or silver from gold. Almost all these ingredients contain vitriol or alum, which, by themselves, but much more when joined with saltpetre, are powerful to part silver from gold. As to the other things that are added to them, they cannot individually by their own strength and nature separate those metals, but joined they are very powerful. Since there are many combinations, I will set out a few. In the first, the use of which is common and general, there is one libra of vitriol and as much salt, added to a third of a libra of spring water. The second contains two librae of vitriol, one of salt-petre, and as much spring or river water by weight as will pass away whilst the vitriol is being reduced to powder by the fire. The third consists of four librae of vitriol, two and a half librae of saltpetre, half a libra of alum, and one and a half librae of spring water. The fourth consists of two librae of vitriol, as many librae of saltpetre, one quarter of a libra of alum, and three-quarters of a Mbra of spring water. The fifth is composed of one libra of saltpetre,

Jan 1, 1950

By J. Kent Smith

THE object of this investigation was to ascertain the effect of varying percentages of beryllium upon pure copper and the properties of the resultant alloys in their softest condition, the effect of heat hardening on them, and the extents to which these properties could be augmented by different combinations of heat hardening and cold rolling. The data compiled in this paper represent partial results of continuing work done by the writer during the years 1930 and 1931, which was a continuation of the unpublished ground work incepted in the laboratory of the Beryllium Corporation of America by H. B. Pulsifer in the year 1926. A short bibliography on beryllium alloys is appended to this paper. It has, of course, long been known that copper subjected to cold work is hardened and strengthened to a considerable extent, furthermore it had been qualitatively noted in previous experiments that copper-beryllium alloys seemed to take on hardness and strength as the result of cold work at a greater rate even than does plain copper. It was decided therefore to endeavor quantitatively to determine such rate of increase, as also the relative increases by combinations of cold working and heat hardening. The results are summarized in Tables 3, 4 and 5. A preliminary series of experiments had indicated that by an exposure to the heat of 575° F. for 2 1/2 hr. age-hardening of a 2.50 per cent beryllium-copper alloy took place. Slab ingots of nine different beryllium-copper alloys were prepared under identical conditions by means of the addition of a previously prepared 12.5 per cent beryllium-copper alloy to well melted and deoxidized pure copper. The ingots were then reduced by hot rolling to 12 gage (about 0.080 in.). These strips were heated to 1450° F. and quenched in cold water, and thus brought to their softest condition. (See Table 1.) Strips were next "precipitation-hardened" by reheating to a definite temperature. Similar strips to those itemized in Table 1 (which had been quenched from 1450° F.) were reheated for varying periods of time at 575° F. The hardness figures show that a metastable condition, of which the range of stability is dependent entirely upon time at the given temperature, begins to be noted in copper samples containing as little as 0.85 per cent beryllium. It is extremely noticeable in samples containing

Jan 1, 1932

By T. R. Yu, D. B. Counter

"In an effort to increase productivity, the use of fly ash as a binder for consolidated backfill was studied. From laboratory and underground tests f or its cementitious properties and environmental effects, it was found that a portion of Portland cement could be replaced by the same amount of type ""C"" fly ash to produce an acceptable consolidated rockfill product for use at Kidd Creek.The environmental concerns in terms of dust control and emanation of radon gas were unfounded from measurements. The dust count was comparable to the use of Portland cement only, or with ground blast furnace slag, and the radiation readings were low, averaging one-seventh the regulation level.Since May 1984, a total of over 100 000tonnes of fly ash has been consumed as a binder blended with Portland cement, producing over four million tonnes of consolidated rockfill. To date, the fill in the stopes has performed very satisfactorily, while yielding considerable cost savings.IntroductionThe Kidd Creek minesite, located 27 km north of the city centre of Timmins, Ontario, produces 4.5 million tonnes of base metal sulphide ore annually. The mining method for both No. I and No .2 mines is mainly sub-level blasthole stoping with delayed backfilling.No. 1 mine was developed with a shaft to a depth of 930 m in 1973 to recover the ore between the floor of the open pit at the 216 m horizon, and the 792 m horizon. Stopes are normally 18 m wide, 22 m to 65 m long, with heights varying from 90 m to 135 m. Vertical rib pillars between stopes are typically 24 m wide and sill pillars are 30 m thick.Pillar recovery is implemented after the consolidated rockfill placed in the mined stopes has cured for a period of at least three months. This allows a maximum recovery of the ore with a minimum of dilution, while also maintaining safe working conditions.No. 2 mine was developed from a second shaft, sunk to a depth of 1530 m in 1978, for the recovery of ore beneath the No. I mine. Sub-level stoping in No .2 mine is similar to No.1 mine in methodology, yet differs in sequencing, as no rib pillars are left."

Jan 1, 1988

By Rixon K. L

Hargraves (1983) has reviewed the phenomenon of instantaneous outbursts of coal and gas with special attention to Australian occurrences. The purpose of this discussion is to highlight some problems and omissions in his review that reflect particularly on the authors' structural geological investigations of outburst-prone coal seams.It is surprising to find that much of the authors' reported work has either been glossed over or the results distorted by Hargraves (1983) and it is, therefore, important to clarify the contribution that structural analysis of coal seams can make.For many years it has been known that faults provided preferred loci for gas outbursts (for example, Briggs 1920-21) but the roie that faults played in outburstprone seams was unclear. The present authors reviewed the association of faults and outbursts drawing upon local investigations and the world-wide literature (Shepherd et aI., 1981), and discussed some wideranging aspects that result from the high coincidence of faults and outburst sites. Without repeating large segments of this article the authors will discuss four aspects of coal seam faulting and fracturing.

Jan 1, 1983

By R. B. G. Yeo

Pronounced isothermal martensite formation at room temperature was measured dilatometrically in a steel containing 0.01 pct C, 24.9 pct Ni, 0.26 pctAl, 2.58 pct Ti and 0.25 pct Cb. It is shown that martensite will form isothermally if stabilization of the austenite-martensite transformation is eliminated by removal of carbon. The decarburization of two iron-nickel alloys allows isothermal transformation to martensite to occur at temperatures above their athermal Ms temperatures. In an Fe-22.4 pct Ni alloy, at the 0.008 pct C level, the Ms temperature during air cooling is 85°F higher than that during- water quenching-. At the 0.15 pct C level this difference is reduced to only 5°F. The introduction of carbon causes stabilization during air cooling which lowers the Ms temperature virtually to the same level as determined during mate?. quenching. Thus in the 0.15 pct C alloy, the Ms temperature is almost independent of cooling rate. It is suggested that rival theories of martensite formation should be reexamined in alloys of sufficiently low carbon and nitrogen content to eliminate the complication of stabilization. The Ms temperature of a steel containing 0.01 pct C, 24.9 pct Ni, 0.26 pct Al, 1.58 pct Ti and 0.15 pct Cb, solution treated at 1500°F and air cooled as 1/8-in. diam specimens, was found to be 57 °F. 1 However, when held for several hours at room temperature the steel hardened slightly and became appreciably ferromagnetic. Isothermal transformation to martensite was first revealed by Kurdjumov and Maksimova2 in an iron-base alloy containing 0.6 pct C, 6.0 pct Mn and 2 pct Cu. Most of the other studies of isothermal martensite have also been confined to highly alloyed steels which transform at subzero temperatures; for instance, DasGupta and Lement, 3 Cech and Hollomon, 4 Machlin and Cohen,5 Shih, Averbach, and Cohen.6 Averbach and cohen7 noted a rapidly decaying volume increase at room temperature in a steel containing 1 pct C, 1.5 pct Cr and 0.2 pct V. cina8 and Marshall, Perry, and Harpster9 have described the isothermal transformation to martensite at room and subzero temperature in stainless steels. Kurdjumov10 has recently reviewed the subject, noting that the isothermal formation of martensite can be observed only in the temperature range somewhat below Ms or below -50°C. The isothermal formation of martensite may be characterized as follows: 1) It occurs in steels of widely different compositions, the main prerequisite being a low transformation temperature. 2) The transformation occurs by the formation of new plates and not by the growth of old ones. 3) The isothermal transformation is suppresed by stabilization during slow cooling or holding at temperatures near room temperature. However, the factors governing this mode of transformation are still not fully understood. The formation of martensite isothermally suggests an activated process. The early theories of martensite formation did, in fact, utilize classical nucleation concepts. Kurdjumov 11 first proposed the presence of thermally activated nuclei of different sizes and compositions which would grow if they reached critical size during cooling. This treatment was enlarged and developed quantitatively by Fisher, Holloman, and Turnbull12,13 and was later reviewed by the latter two authors.14 Fisher15 associates Ms with a nucleation rate of one per cc per sec. At slightly higher temperatures the nucleation rate is so low that isothermal formation of martensite is not observed in reasonable times. At slightly lower temperatures the nucleation rate is so high that it could not be suppressed by rapid cooling. By judicious use of parameters Fisher 16 was able to obtain good agreement between classical nucleation theory and the incubation times of martensite formation.4 However the application of these principles to martensite formation in iron-nickel alloys15 predicts that an alloy containing about 30 pct (31 at. pet) Ni would not transform. The presence of an Ms temperature at -223° C in an alloy containing 34.1 pct (33 at. pct) Ni led Kaufman and cohen17 to reject the hypothesis of homogeneous nucleation in favor of the reaction path theory originally proposed by Cohen, Machlin and Paranjpe.18 This theory conveniently explains the formation of martensite athermally but becomes labored when dealing with isothermal formation. Kaufman and cohen19 did explain the isothermal activation of embryos by assuming it to be a result of the expansion of their boundary dislocation loops but this treatment predicts an upper temperature limit of isothermal martensite formation.

Jan 1, 1962

By D. W. Lillie

It has been demonstrated that considerable bend ductility exists in bulk specimens of polycrystalline high-purity silicon. The possibility of hot-forming at 1200°C is suggested. EXCELLENT corrosion resistance in many media and low cross section for absorption of thermal neutrons (0.13 barn) would make silicon of interest to nuclear engineers were it not for extreme brittle-ness and the difficulty of fabrication by any reasonable means. The use of silicon for structural purposes also has been considered in view of its light weight and oxidation resistance. Johnson and Han-sen' have investigated the properties of silicon-base alloys and concluded that there was no way of making pure silicon or silicon-rich alloys ductile at room temperature. In view of reports of appreciable ductility in germanium single crystals above 550°C'." and some plastic deformation in single-crystal silicon above 900oC,' the present investigation was undertaken to define more precisely the limits of high-temperature ductility in pure silicon. After this investigation was begun torsion ductility in both germanium and silicon was reported by Greiner." Through the courtesy of F. H. Horn, a small bar of cast extra high-purity silicon was obtained and small bend specimens were made from it by careful machining and grinding. All of the reported tests results were obtained from samples from this bar (bar No. 1) and one other of similar source (bar No. 2). No complete analysis was obtained but, based on analysis of similar semi-conductor grade material, metallic impurities were under 0.01 pct total. Vacuum-fusion analysis for oxygen showed a value of 0.0018 2 0.0003 pct for the first bar tested and metallographic analysis showed no evidence of a second phase. Bend tests were carried out on an Instron tensile machine using a bend fixture with a 1 -in. span loaded at the center. Supporting and loading bars were 0.250 in. round and the load was applied by downward motion of the pulling crosshead of the machine. Specimen thickness and width were approximately 0.10 in. and % in. respectively. Loading rate was controlled by holding crosshead motion constant at 0.02 ipm. In some cases a smaller specimen was used on a 5/8-in. span with a 0.129-in.-diam loading bar. The entire bend fixture was surrounded by a hinged furnace and all heating was done in air atmosphere. Temperature measurement was made with thermocouples fastened directly to the bend fixture within less than 1 in. from the specimen. Autographic stress-strain curves were recorded during each test, and breaking load, total deflection, and plastic strain could be obtained from these curves. Stress was calculated from the beam formula S = 3PL/2bh2, where P is the load in pounds, L the span in inches, b the specimen width in inches, and h the specimen thickness in inches. This formula is strictly correct only in the elastic range but has been used to calculate a nominal stress for convenience in the plastic range. The stress given is the maximum stress in the specimen. Results The results of the complete series of tests are shown in Table I. The first group of tests (specimens Nos. 1-6) showed the beginning of plastic flow at a test temperature of 900°C, so two additional tests (Nos. 8 and 9) were made at 950°C on small-size specimens from bar No. 2. Specimen No. 8 was tested in the as-machined condition, and No. 9 was heat-treated in hydrogen at 1300°C for 2 hr, cooled to 1200°C and held 1 hr, cooled to 1000°C and held 1 hr, cooled to 900°C and held 1 hr, and finally cooled to a low temperature before removal from the hydrogen. It is apparent that the heat-treatment had a significant effect on yield strength and ductility. In addition, the magnitude of the yield point was conslderably reduced in the heat-treated specimen as is shown m Fig. 1 by tracings of the stress-strain curves. After obtaining a furnace capable of reaching higher temperatures specimens Nos. 10 to 13 were tested at 1100 and 1200°C. Strain rate was increased by up to a factor of 10 to see whether the ductility observed was excessively strain sensitive. Specimen NO. 10, strained at 0.02 ipm and 1100oC, was still bending at a deflection of 0.322 in. when the load rate was increased to 0.2 ipm, resulting in immediate

Jan 1, 1959

By J. E. Powell, F. H. Spedding

WHILE rare earths are reported to be widely distributed in nature and are not really rare," in practice, there are only a few minerals which are sufficiently rich in rare earths to serve as practical sources. Perhaps the best known of these is monazite which is a phosphate mineral containing rare earths and thorium. This mineral occurs as a dense brown sand in gravel beds and is particularly rich in the light rare earths of the cerium subgroup. This mineral is processed commercially for its thorium, cerium, and lanthanum content, and, consequently, furnishes rich concentrates from which neodymium, praseodymium, samarium, europium, and gadolinium may be obtained. Unfortunately, monazite is rather lean in rare earths heavier than gadolinium. A second mineral which is rich in the light rare earths is bastnasite, a fluoro-carbonate. Extensive deposits of this ore have been discovered in the western United States and have received considerable newspaper publicity in recent years. While bastnasite is very rich with respect to cerium, lanthanum, and neodymium, it contains even less heavy rare earths than does monazite. One of the better sources of heavy rare earths of the yttrium subgroup is gadolinite, a black silicate rock from which the rare-earth content can be extracted readily by acid leaching. It is obtained chiefly from Norway at the present time, although there are known deposits in the United States. Other sources of heavy rare earths include fergu-sonite, euxenite, and samarskite which are refractory tantalo-columbate ores. These minerals require caustic fusion or reduction to carbides with carbon before the rare-earth content can be extracted. All of the minerals which are rich in the heavy rare earths contain yttrium as a major constituent. After the rare earths have been extracted as a group from an ore by chemical means, it is generally convenient to precipitate them from acid media with oxalic acid in order to eliminate certain non-rare-earth impurities such as iron, beryllium, etc., which are usually present. The oxalate can then be readily ignited to R2O3. The oxide can be dissolved in acid and is the starting point for subsequent separation into the pure components. Perhaps the principal reason why the rare earths have not been studied as extensively as other elements of the periodic table, whose natural abundances are comparable, is that they are extremely difficult to separate from each other by the usual chemical means. Prior to 1945, the separation of one trivalent rare earth from another was a laborious process. All separations were based on repeated fractionation processes, i.e., fractional precipitation, fractional decomposition, fractional crystallization, etc. These processes were repeated from a few hundred to many thousands of times in order to obtain individual rare-earth salts of reasonable purity. Of course, mention should be made that, in the few cases where a rare earth could be oxidized or reduced to a valence state other than three, more conventional chemical means could be utilized to separate the oxidized or reduced ion from the other normally trivalent rare earths. The ionic states which deserve special mention are CeIV, SmII, Eu11, and Yb11. When it is possible to remove an element of the series efficiently, due to an optional valence state, its immediate neighbors also become easier to isolate. For example, binary mixtures of lanthanum and cerium, and praseodymium and cerium can be obtained by a relatively small number of fractional operations. The tetravalent state of cerium then allows the complete resolution of the binary mixtures by ordinary chemical means. Although the tetravalent state of cerium has been known for a long time, the divalent states of samarium, europium, and ytterbium were not used extensively in separations prior to 1930 because they are relatively unstable in aqueous media.'-" No attempt will be made to give a comprehensive review of the extensive literature dealing with the separation of rare earths. Rather, this paper will be confined to a review of those methods which have been developed at Iowa State College during recent years, and which have proved extraordinarily successful for the isolation of highly pure rare earths in quantity. It was obvious that, if pure rare earths were to become generally available, methods would have to be developed wherein the thousands of fractional operations made necessary by the similarity of rare-earth properties could be performed automatically. The development of chromatographic techniques and ion-exchange resins appeared to offer a mechanism by which this objective could be accomplished. A number of early attempts were made to separate rare earths by these means; for example, Russell and Pearce12 passed a mixture of rare earths through a cation-exchange column and reported

Jan 1, 1955

By F. B. Foley

IT is with an unusual degree of personal satisfaction that I find myself in a position to pay tribute to the memory of Henry Marion Howe. One could not have spent any length of time in the presence of Dr. Howe without profiting intellectually. I do not hesitate to say that my years of association with him were the most stimulating of all my years of metallurgical study. He always impressed one with his own eager search for knowledge. Never dependent on the written word alone he sought information from anyone whose opinion he valued. His ability to piece together bits of apparently conflicting data from various sources so as to build up a logical hypothesis was unique. A small slight man with the intellect of genius he would have gone to the top in any endeavor he undertook and it was fortunate for metallurgy that its study attracted him as it did. Howe was a modest man. I like to recall an incident which left a lasting impression with me. The lab- oratory in his home, "Green Peace," was in the basement and access was by way of stairs leading down from his secretary's room. In using these stairs my attention was attracted many times to an ordinary cardboard shoe box which reposed on the shelf above the landing. It was crudely labeled on its side in black ink "Vanity Box." My curiosity was aroused to the point that I finally asked his secretary what it was. With some amusement she took the box from its shelf on the stairway, opened it and showed me its contents—numerous letters, from the foremost men of science of every civilized country throughout the world, commending his "Metallography of Steel and Cast Iron." I recall that in reply to one who thought there was not enough of Howe's own researches in his book he wrote, "Primarily I am a writer, secondarily an investigator." Howe wrote to make his readers think. No one ever strove harder than he to be right but above all, whether his viewpoint proved ultimately to be right or wrong, he was always content if by his stand, he provoked a reader to take the next step along the path to greater knowledge. I doubt that he was ever afraid to be wrong for he was always secure in the thought that his effort was guided by a sincere search for the truth. One continually searching for truth is entitled to occasional excursions up the wrong alley. A glance backward to the metallurgical confusion of some thirty to forty years ago, or need one go back so far, provides convincing proof of what a host of companions one may have in a common acceptance of ideas which the future will prove to be wholly untenable. Well over a hundred years have passed since investigators have interested themselves in the effect of increasing the temperature of iron and steel on their mechanical properties. We are told by Charles Walrandl in "Industrial Annals" for June 11, 1822, that bend tests, conducted in a Russian steel works of Prince Demidoff, on steel bars "highly heated" and bent during cooling became brittle when bent at an iris blue color. He concluded, "That when steel is heated to a temperature between 473°F and 662°F the mettle was more brittle between these limits than at a much lower or at a much higher temperature." It was a curious bit of information recognized as true to this day and still not explained satisfactorily. In 1878 Charles Houston in Annales de Mines associated this brittleness with an increase in tensile strength at 572°F. When this relatively low temperature is exceeded it is recognized that steel becomes weaker as temperature is increased up to the melting point, where no strength of practical importance remains. It is easy to believe, in fact it goes without saying, that this weakening as the temperature of a metal is increased is the result of the motion of the atoms making up the metal, a motion which itself is evidence of the temperature increase. However, if we are considering iron or steel we find that this decrease in strength is not a steady one, for, besides the increase in strength just referred to, one comes to a temperature, the critical temperature, where results of tests indicate the metal to be extremely weak and then as temperature increases to become sensibly stronger again. This apparent anomaly was made the subject of the first Howe Memorial Lecture, delivered by Albert Sauveur in 1924. It may be of interest to review these findings of Sauveur. He used two methods of investigation. One involved the twisting of bars. The bars were heated in an

Jan 1, 1951

By R. K. Dann, L. W. Roberts, R. B. Benson

The mechanical properties of 300-series stainless steels were investigated in both high-pressure hydrogen and helium environments at ambient temperatures. An auslenitic steel which is unstable with respect to formation of strain-induced a (bee) and € (hcp) mar-tensile is embrittled when plastically strained in a hydrogen environment. A stable austenitic steel is not embriltled when tested under the same conditions. The presence of hydrogen causes embrittlement at the mar-lensitic structure and a definite change in the general fracture mode from a ductile to a quasicleavage type. The embrittled martensitic facets are surrounded by a more ductile type fracture which suggests that the presence of hydrogen initiates microcracks at the martensitic structure. If a steel is unstable with respecl to fortnation of strain induced martensile, plastic deformation in a hydrogen environment will produce rapid embrittlement of a notched specimen in comparison to an unnotched one. FERRITIC and martensitic steels can be embrittled by hydrogen that has been introduced into the alloys, either by thermal or cathodic charging prior to testing.1-5 However, conflicting reports exist as to whether austenitic steels that are stable or unstable with respect to formation of strain-induced martensite can be embrittled by hydrogen.8-12 A recent investigation has shown that cathodically-charged thin foils of a stable austenitic steel can be embrittled.13 An earlier investigation of a thermally charged 18-10 stainless steel revealed a significant decrease in the ductility only at the lowest test temperature of -78°C, although strain-induced bee martensite was shown to be present in one specimen tested at ambient temperatures.' When martensitic steels are tested in a hydrogen atmosphere, they are embrittled.'4-'7 It has been observed in this Laboratory that 304L steel, which is unstable with respect to formation of strain induced martensite, forms surface cracks when plastically strained in a high-pressure hydrogen environment. Work in progress elsewhere concurrent with this investigation has also established that 304L is embrittled when tested in a high-pressure hydrogen atmosphere." The objective of this investigation was to study the effect of a high-pressure hydrogen environment on the tensile properties of a stainless steel that contained strain-induced martensite (304L) and one that did not (310). EXPERIMENTAL TECHNIQUES Notched and unnotched cylindrical specimens were machined from 304L* and 310 rods that were heat- treated at 1000°C in argon for 1 hr followed by a water quench. The chemical analyses of these steels are given in Table I. The unnotched specimens had a reduced section diameter of 0.184 & 0.001 in., a gage length of 0.7 in., and were threaded with a 0.5-in.-diam. thread on each end. The notched specimens had a reduced section diameter of 0.260 * 0.001 in. and a 0.75-in. gage length, with a 30 pct 60 deg v-notch at the center. The notch had a maximum root radius of 0.002 in. The tensile bars were fractured in a hydrogen or helium atmosphere of 104 psi at ambient temperatures. The system used for mechanically testing the specimens is to be described in detail elsewhere.19 Several specimens of each type were tested in air using an Instron testing machine. The same yield strength and ultimate tensile strength were obtained in 104 psi helium with the above system as with the conventional testing machine. Magnetic analysis was employed to determine that there was a (bee) martensite in plastically deformed 304L and that it was not present in plastically deformed 310. The magnetic technique depended on allowing the material being studied to serve as the core between a primary and secondary coil. Thus, any change in the amount of magnetic material present between the annealed and plastically deformed steels will be indicated by corresponding changes in the induced voltage in the secondary circuit." The ratio of the output signal of a nonmagnetic stainless steel to a completely magnetic maraging steel was 2000 to I. Several unnotched 304L bars tested in hydrogen were analyzed for hydrogen by vacuum fusion analysis. There was an increase in the hydrogen content to approximately 2 ppm for the specimens tested in hydrogen, as compared to less than 1 ppm for the as-received material. Several thin sections cut from notched areas of 304L specimens tested in hydrogen and containing the fracture surface contained approximately 1.5 ppm H. The accuracy of these determinations was estimated to be ± 50 pct.

Jan 1, 1969

By F. I. Grace, L. E. Murr

The mechanical responses and residual defect structures in 70/30 brass and type 304 stainless steel following explosive shock loading and cold reduction by rolling have been studied. A distinct relationship was observed to exist between the residual mechanical properties and micro structures observed by transmission electron microscopy. Shock-loaded brass deformed primarily by the formation of coplanar arrays of dislocations and stacking faults at lower pressures, and twin-faults (deformation twins and €-martensite bundles) at higher pressures (> 200 kbar). The micro -structures of cold-rolled brass were characterized by dense dislocation fields elongated in the rolling direction. Stainless steel was observed to deform by the formation of dense arrays of stacking faults at lower shock pressures and twin-faults at high shock pressures (>200 kbar). Lightly cold-rolled stainless steel deformed similar to low Pressure shock-loaded stainless steel, but transformed to a' martensite in heavily cold-rolled stainless steel. Discontinuous yielding was observed for the heavily cold-rolled stainless steel, and stress reluxution in the weyield region for cold-rolled and shock -loaded stainless steel was interpreted as an indication of the ability of twin-faults and stacking faults to act as effective barriers to dislocation motion. A simple model for the formation of the planar defects and a' martetnsite is presented based on the propagating of Shochley partial and half-partial dislocations. A considerable effort has been expended over the past decade in an attempt to elucidate the response of metallic-crystalline solids to the passage of a high velocity shock wave (e.g., smith,' Dieter,2 and zukas3). While it has been possible to obtain relevant information pertaining to the residual defect structures and mechanical properties, there have been few rigorous attempts to draw a direct comparison between these structures and properties. In addition, numerous investigators have recently observed the occurrence of deformation twinning in shock deformed fcc metals (e.g., Nolder and Thomas,4 and Johari and Thomas5), but little attempt has been made to elucidate the mechanisms of formation of these defects. Comparative data for metals deformed by shock-loading and the same metals deformed by more conventional modes of deformation such as cold-reduction by rolling is also generally lacking. The present investigation therefore has the following objectives: 1) to examine the mechanical properties of some explosively shock loaded and cold-rolled fcc metals of low stacking-fault energy as a function of their residual substructures; 2) to present a simple model for the formation twin-faults and related defect structures in the low stack-ing-fault energy materials of interest (70/30 brass, ySFg= 14 ergs per sq cm; and 304 stainless steel, ySF = 21 ergs per sq cm); 3) to make some deductions with regard to the residual characteristics of dislocation and planar defect substructures in cold rolled and shock loaded 70/30 brass and type 304 stainless steel. In particular, it was desirable to characterize the residual hardening effects of particular deformation substructures. I) EXPERIMENTAL PROCEDURE Sheet samples of 70/30 brass (0.005 and 0.15 in. thick; annealed at 659°C for 2 hr) and type 304 stainless steel (0.007 in. thick; annealed 0.25 hr at 1060°C) of nominal compositions shown in Table I were cold-rolled in one direction only to produce reductions in thickness of 15, 30, 45, 60, and 75 pct in the brass; and 5, 15, 25, 35, and 45 pct in the stainless steel. Identical sheet samples in the annealed (unrolled) state were subjected to plane compressive shock waves to various peak pressures ranging from 0 to 400 kbar in the brass and 0 to 425 kbar in the stainless steel; and with a constant peak pressure duration of approximately 2 microseconds. A detailed description of the shock loading technique has been given previously.6 Tensile specimens 1.0 in. in length and 0.125 in. in width were cut from the cold-rolled sheets (tensile axis parallel to the rolling direction), and the shock-loaded sheet specimens. Stress (load)-strain (elongation) measurements on the tensile specimens were made on a Tinius-Olsen load-compensating tensile tester using a strain rate of 2.7 x 10-3 sec-1. Tensile tests were repeated at least twice, giving essentially the same results. Stress relaxation measurements in the preyield region were also made using an initial strain rate of 5.4 x 10-4 sec-1. In addition to tensile and stress relaxation measurements, Vickers microhardness measurements were made on all samples. A total of 100 microhard-ness readings were obtained for each specimen following a light electropolish to ensure uniform surface conditions for all tests. The hardness averages ob-

Jan 1, 1970

By Stanley C. Suboleski, C. B. Manula

INTRODUCTION In any mining operation all possible steps should be taken to increase efficiency. One area for improvement is mine planning and design, particularly in the area of equipment selection for room-and-pillar systems. Be- cause of the availability of a wide variety of face machines, a fair degree of selectivity can be exercised in the choice of equipment for a particular job. However, this choice must be made on the basis of quantitative facts and forecasts related to the mining application. The purpose of this section is to develop and analyze the details of the mining process. Some specific areas studied include the relationship of system design to productivity, suboptimization as a result of equipment changes, and measurement of system performance. The plan of work leading to a quantitative description of these study areas is based on the growing interest in total system design using simulation as an analytical method (Manula, 1963). CHARACTERISTICS OF PRODUCTION OPERATIONS FROM ROOM-AND-PILLAR SECTIONS For a given mining method, raw production in a given section of a mine is primarily dependent upon the coal seam thickness, roof and floor conditions, methane emission, the mining methods, and the man-machine element. Average section production varies from 300 to 800 st per shift for conventional and continuous mining in high seams and from less than 100 to 300 st per shift in low seams. Since the reject varies from 0 to 40%, these figures must be decreased by the appropriate percentage to reflect the amount of clean coal mined. Personnel requirements per production section per shift for the various methods are listed in Table 1. Table 1. Production Personnel Method No. Method No. Conventional 12-1 5 Longwall 9-14 Continuous 9-1 2 Shortwall 9-12 MINING VARIABLES To evaluate the constraints and interrelationships for various mining methods, it is necessary to categorize the variables which underlie system production potential. Seven critical independent variables which determine production can be identified and categorized (Suboleski, 1978) : Seam Height The five categories are as follows: less than 36 in.;. 36 to 55 in.; 55 to 100 in.; 100 to 180 in.; and greater than 180 in. Floor Quality Floor quality ranges from : Excellent: Smooth, hard, grades less than 1 to 1 % % , and dry. Good: Smooth, soft but dry, with grades less than 3 % . The floor will deteriorate, but cautious operation can prevent it. There may possibly be heaving at some later time. Fair. Soft and damp. There is occasional interference with equipment operation; requires the use of four-wheel drive shuttle cars; ruts with regular use, and may have adverse grades of 5 to 7%. This may be coupled with slippery bottom and/or occasional steep rolls. Poor: Soft and wet. Requires blocking of the bottom to support equipment. There are frequent steep rolls and grades in excess of 7%. Roof Quality Roof quality ranges from : Excellent: Men are able to work under the unsupported top during the initial production cycle if legally permitted. Good: The roof is bolted on a 4 x 4 or 5 x 5 pattern with short bolts (442 in.) or <seam height if the seam >42 in., or requires posting with no bolts on a 4 x 4 or 5 x 5 pattern. There are no falls. Average: The roof is normally bolted on a 4 x 4 or 5 x 5 pattern, but with long bolts (>seam height or >6 ft.). There are infrequent minor falls or there may be an excellent roof which is difficult to drill. Fair: This type often requires spot bolting in addition to the regular pattern or bolting with planks. The roof conditions require shorter than planned cuts, or narrow cuts. Poor: This type requires bolts plus crossbars and posts, or installation of yielding supports or truss-type support. It is almost certain to fall if this is not done. Methane Liberation This ranges from none detected to low (no buildup at the face, even with minimum ventilation requirements) to moderate (the curtains must be extremely tight and tubing close to the face or methane will build up to 1 % during the loading of the car) to high (methane will build up to 170 if the miner is operated at the normal rate, even with proper ventilation). Hardness of Coal Coal hardness falls into the following categories: Soft: Soft coal is easily cut by a continuous miner. A plow could be used by longwall. Average: Coal of average hardness could be easily cut by a miner, and a shearer would be used in the longwall. Moderate: Moderately hard coal causes difficult cut-

Jan 1, 1982

By Hollis L. Caswell

The present status of integrated circuits utilizing. superconductive switching. elements is reviewed with special attention given to fabrication techniques, methods for interconnecting completed circuits, and refrigeration requirements. Cryoelectronics has been largely an "inte- grated-circuit" technology since its conception because the switching speed of superconductive devices is attractive only when these devices are fabricated with thin-film techniques. It is true that cryotron circuits can be constructed from wires of appropriate materials (as indeed was done by Dudley Buck 1 in his early investigations) but these circuits will switch in times characteristic of milliseconds whereas similar circuits fabricated by thin-film methods have potential switching times of nanoseconds. Furthermore, cryo-electronic devices such as the cryotron lend themselves readily to fabrication by thin-film techniques since these components may be made from polycrys-talline thin films and are relatively insensitive to the presence of impurities (as measured by semiconductor standards). Therefore, during the past decade considerable effort has been devoted to developing techniques for batch fabricating circuit arrays containing superconductive switching elements. Technology had developed to the point several years ago that fabrication of cryoelectronic arrays containing up to one hundred devices was rather straightforward. However, larger arrays containing between lo4 and 106 components which are required for commercial development of cryoelectronics still pose very severe yield problems. Thus in a sense cryoelectronics found itself in 1962 at the point semiconductor technology finds itself today; namely, individual devices and small groups of integrated devices could be fabricated with acceptable yield and the outlook for building larger integrated-circuit arrays was bright. Unfortunately, problems associated largely with yield have made fabrication of these larger arrays difficult. Unlike semiconductor technology, cryoelectronics had to solve the problems of large-scale integration before it could become economically attractive. This has proven to be a sizable burden to bear. Since several reviews exist on superconductivity,2 superconductive devices,3 and cryoelectronic technology, no attempt will be made in this paper to summarize these areas. Instead a few specific topics will be dealt with in more detail. First, a brief description is given of selected superconducting switching and storage devices with special attention to several metallurgical techniques which improve the performance of these devices. Second, techniques used to fabricate cryoelectronic devices are described with emphasis on problems affecting yield. Third, techniques for interconnecting a number of cryoelectronic planes are described. And last, refrigeration of cryoelectronic components is discussed briefly since the low operating temperature of superconductive devices is an important consideration in this technology. SUPERCONDUCTING STORAGE AND SWITCHING DEVICES The basic superconductive switching device is the thin-film cryotron. The geometry of this device is attractively simple, since it involves only the intersection of two lines that are electrically insulated from each other. The switching element (gate) and control element (control) of a crossed-film cryotron are arranged as illustrated in Fig. 1. The material for the gate is selected to permit the gate to be switched from the superconducting to the normal (resistive) state by the application of a control current. Tin, which has a critical temperature (T,) of 3.7°K, is commonly used for the gate and the cryotron is operated at a temperature just below T, (for example, 3.5°K). The control material (normally lead, with T, = 7.2°K) is chosen so that the control is never driven normal during circuit operation. To improve cryotron operation, a ground plane, also of lead, is placed under all of the circuitry to act as a diamagnetic shield and improve the current-density uniformity across the width of various thin-film elements. Normally, line widths vary from 0.005 to ^ 0.020 in. and film thicknesses from 300 to 10,000A, although new fabrication techniques make narrower lines feasible. In fabricating cryotrons it is important that the edges of the gate elements be geometrically sharp to avoid undesirable switching characteristics associated with a thinner edge region, Fig. 2. One technique which has been used extensively to form patterns consists of placing a physical mask containing the film pattern between the evaporation source and the substrate and depositing through the mask. Film strips formed in this manner possess a penumbra at the film edges due to shadowing of the evapor-ant under the mask. Several techniques have been proposed for minimizing effects due to this penumbra. One of the more promising metallurgical techniques

Jan 1, 1967

By W. A. Backofen, D. Lee

Tlze condition of superplasticity or neck-resistanl flow that results front high strain-rate sensitivity has been observed in isothermal tension tests on several titanium alloys and one of zirconium hi general, il was associated with reasonably fine-grain micro-structures being stvained in the transformation range at rates below i - 10 -3 sec-&apos;. The metallographic mean-free path, L, was measured at room temperature after rapid cooling from the temperature of test-ing. The flow stress of Ti-GAL-4V at 950°C was proportional to La at different constanl <; the value of a decreased with increasing. E but at E< 1.5 x 10-4 sec-1 it varied only from 0.9 to 1.25. The findings were interpreted to mean that viscous boundary shear is the rate-controlling process of deformation at high levels of strain rate sensitivity in these materials. Elongation of over 1000 pet could be obtained, but a1 temperatures so high and rates so low that any practical application of the full effect would probably be difficult. As the transformation range was narrowed, by turning from Ti-6AL-4V to Ti-5Al-2.5sn to nomznally pure titanium, the allowable temperature varialion was correspondingly reduced. Superplasticily was not found in Armco iron, presumably because the transformation range was too narrow to allow the developtnenl of a reasonably stable microstructure for isolhermal lesting. THE work represented by this paper grew out of a recent study of texture hardening in a(hcp) titanium and zirconium-alloy sheet,&apos; of which part has now been published.2 It was found that, with heating, the tensile plastic-anisotropy index, R,* was decreased from well above 1 towards 1 as the temperature range for the a(hcp) -ß(bcc) phase change was entered. The clearest example of that trend is illustrated with previously unpublished data in Fig. 1. It might have been thought that such a development resulted simply from introduction of the cubic and therefore plastically less anisotropic phase. However, the accompanying change in the index of tensile strain-rate sensitivity, m = a log a/a log E, was rapidly upwards, to a high of 0.85 in some cases (also illustrated in Fig. 1). At the same time, the total tensile elongation rose to a maximum and the flow strength dropped away as R (and m) approached 1. Taken together, the observations cannot be understood as resulting from the presence of cubic phase, per se. It has been concluded instead that they reflect the largely noncrystallographic deformation which characterizes superplasticity. As demonstrated in other recent work? a necessary condition for super-plasticity is strain-rate sensitivity of flow stress sufficiently high that m is above a lower limit of -0.3. The origin of large m has been traced, in turn, to grain size so small that a substantial amount of viscous deformation is introduced by such processes as Nabarro-Herring diffusional flow4 and/or grain boundary shear.5,6 Because of problems in the processing of titanium and zirconium alloys—problems of high strength, limited ductility, and excessive springback, originating largely in slip resistance-it was natural to wonder if something useful might be done with superplasticity in those materials. Therefore experiments were made for more closely identifying and generally bounding the phenomenon with temperature and strain-rate limits, before attempting to decide about its exploitation. The results are being reported here. EXPERIMENTAL Materials. The two of primary interest were the titanium alloys of nominal composition (in wt pct) 5A1-2.5Sn and 6A1-4V. Others were a 4A1-1/4O2 titanium alloy, titanium of commercial purity (RC-70), Zircaloy-4. and Armco iron. All were received as annealed 3/16 in. thick sheet, except RC-70 which was & in. thick, and tested in that condition. Details of transformation temperature and grain size are given in Table I. The results of dilatometry for the measurement of transformation temperatures were unsatisfactory. Data were finally obtained by metallographic examination of each specimen after test, to determine from the amount of transformed 4 where the specimen had been heated in relation to the critical temperatures. Results were in reasonable agreement with information from the supplier. Strip tensile specimens were of full sheet thickness and taken along the rolling direction, except for those

Jan 1, 1968

By Tano Balbin, Valery Astakhov, Juha Timperi, Lauri Koresaar

"Online elemental analysis is the basis of optimal flotation control in mineral concentrator plants. Traditionally XRF analyzers have been used as the online analysis method. However, online XRF analyzers struggle to measure elements below calcium in atomic number (Z=20). For many processes lighter element assays would be beneficial to improve control of grade and recovery. Processes where elements below Ca are required include P, Mg and Si in phosphate concentrators, Si, Mg and Al in iron concentrators, and S and C in gold concentrators. Laser-Induced Breakdown Spectroscopy (LIBS) based elemental analysis can readily be applied to these processes. LIBS is based on generating plasma in the slurry sample by a high energy laser and analysis of the plasma by optical emission spectroscopy. Capabilities of a new Courier® 8 analyzer based in LIBS technology are demonstrated for elemental analysis starting from lithium (Z=3). Results of a plant installation in a sulfide gold concentrator provide a good agreement with the analyzer and laboratory assays.IntroductionEffective process control can be regarded as one of the fastest paying investments for a mineral processing plant. Process optimization in flotation circuits requires constant feedback of the process state. If only manual laboratory samples are available, this optimization becomes difficult due to the long delay between taking the sample and acquiring the laboratory result. If the element grades are available in online basis, the operator or automatic process control system can make corrective actions in real time.Online X-Ray Fluorescence (XRF) analyzers have been in use at concentrators for decades. The XRF analyzers can provide a fast, accurate and precise analysis from slurry streams. However, the drawback of XRF analyzers is their lack of capability to measure elements below Ca (Z=20) in atomic number. The low energy X-rays of the low atomic number elements get absorbed by water in the sample, protective window of the analyzer, or air between the sample and spectrometer."

Jan 1, 2017

By Norman O. Lotter

Drill core is preferred as the sample material for metallurgical and mineralogical characterisation and flowsheeting of an orebody. The question arises as to how to do this at the economic optimum, since geologists have several other strategic uses for their drill core. The limiting factors are the cost of extra drilling for the metallurgical testwork and the need to preserve the drill core record. In this study, the representative sampling of drill core at an economic optimum for metallurgical testing is addressed. This phase of the drill core work is preceded by earlier drill core characterisation - for which other appropriate sampling protocols are used - that has provisionally categorised the orebody into geometallurgical units. In stratified sampling of drill core, use is made of a version of the stratified approach to compound distributions proposed by Cochran in 1946. Use is made of Gy’s 50-piece minimum sample mass model to estimate minimum requisite sample mass. In the case where sampling and testwork are required on a Lifeof- Mine blend of a given ore deposit, whereby defined ore types or geometallurgical units are present, the sample mass requirement is significantly reduced by working from drill-core at the geometallurgical unit level. A case study using Raglan drill core is discussed. Using nickel as an indicator paymetal, and sampling at a fundamental variance level of 8%, the minimum sample masses for disseminated sulphides, net-textured sulphides, and massive sulphides are 3.80, 7.37 and 4.39 kg respectively. When the same drill-core is sampled as a Life-of-Mine mixture without knowledge of the geometallurgical units, the minimum sample mass increases to 84.28 kg. It is thus possible to assemble a representative Life-of-Mine sample of drill-core more economically, at the same time validating its representativity. Equivalent calculations for copper, platinum and palladium are discussed, with outcomes consistent with this finding. When all four paymetals are considered, one selects the largest minimum mass out of all four cases. This results in minimum sample masses of 11.67, 74.90 and 175.16 kg for disseminated sulphides, net-textured sulphides and massive sulphides respectively. The simulated Life-of- Mine blend would require a minimum sample mass of 377.33 kg to cover all four paymetals.

Jan 1, 2010

By Walter E. Dean

Deep-sea manganese nodules are considered to be potential ores of manganese, nickel, cobalt, and copper. Considerable time, effort, and funds have been applied to the study of Se distribution of nodules on the sea floor and the location of economically important areas, but little effort has been spent in understanding the origin of nodules. Most theories that have been proposed to explain the origin of manganese nodules have been based on inorganic physicochemical processes. It is not by coincidence, however, that the area considered to be most economically feasible is in the zone of high biological productivity in the eastern equatorial Pacific Ocean and underlain by siliceous biogenic sediment. The genesis of manganese nodules and the concentration of many trace elements are intimately associated with biological processes.

Jan 1, 1982

By AIME AIME

In the uniform of his country for the second time, Harry Phillip Stolz. Chairman of the A.I.M.E. Petroleum Division, holds a commission as Lieutenant-Commander in the Naval Reserve and is attached to the office of Inspector of Naval Petroleum Reserves in California. During World War I he left his studies at Stanford University to join the Army and was granted a commission as Second Lieutenant of Infantry. He remained in the Army Reserve until 1938 when he resigned to accept a commission as a member of the Naval Petroleum Reserves Advisory Board. Born in San Francisco Jan. 29,1899, where his father had lived since 1880, he was in that city during the turbulent year of 1906 where the city was ravaged by fire and earthquake.

Jan 1, 1942

By A. C. Smith

Although only used in a few U.S. longwall mines, bleeder-less ventilation systems can be an effective spontaneous combustion control method in mines having a demonstrated history of spontaneous combustion. To provide insights for the optimization of bleederless ventilation systems for U.S. underground coal mines, a computational fluid dynamics (CFD) study was conducted to model the spontaneous heating in longwall gob areas using a bleederless ventilation system. A single longwall panel with a bleederless ventilation system was simulated, and typical longwall mine ventilation data were used in the simulations. The permeability and porosity profiles for the longwall gob were estimated using a geotechnical model and were used as inputs for the CFD modeling. The effects of gob permeability and resistance of the collapsed entries on the spontaneous heating were studied. The effectiveness of using nitrogen injection to prevent spontaneous heating in the gob was also examined.1

Jan 1, 2008