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By Eugene S. Meieran

The effects of methods of crystal growing, wafer sawing, polishing, routine handling, diffusion, and epitaxial growth on the defects in GaAs are reviewed and studied using reflection and transmission X-ray topographic techniques. In general, it was found that boat-grown crystals exhibited fewer defects than Czochralski crystals, although all crystals showed large numbers of precipitates visible when examined in the electron microscope. Mechanical surface treatments such as sawing and mechanical polishing introduce damage to a depth of about 5 µ, most of which can be removed by suitable chemical or chem-mechanical polishing. In addition, defects can be introduced through routine handling of wafers, for example with metallic tweezers. These defects can be quite severe, and have been observed 20 µ below the wafer surface. Defects can also be introduced through diffusion and epitaxial growth. These defects, which include precipitates, growth pyramids, stacking faults, dislocations, and so forth, can be detrimental to device fabrication. It is shown that wafers or films which appear defect-free optically can contain defects visible in the X-ray topographs. WHILE the use of GaAs in the semiconductor industry has increased very rapidly in the last few years, due mainly to the recent development of many important GaAs devices,1,2 the major limit to the production of commercial quantities of many GaAs devices remains a severe lack of suitable materials technology. This lack is apparent in two critical areas. First, production quantities of high-quality GaAs crystals, reproducibly doped and precipitate-free, simply are not available commercially, although some reasonable quality material is available on a limited first-come, first-serve basis. Second, in comparison to silicon technology, little is known about the effects of processing variables on the defects either present in as-grown GaAs or introduced through processing and handling of wafers. These areas are now receiving some attention from semiconductor device manufacturers, who are studying defects in GaAs in order to better understand how either to prevent their occurrence or to cope with their existence. Most investigations of the defects in GaAs have been made by optical microscopy3-5 or transmission electron microscopy techniques.'-' Recently, however, the imaging techniques of X-ray topography, electron mi-croprobe analysis, and scanning electron microscopy are being applied to the study of GaAs.9-14 In the case of X-ray topography, a one-to-one image is obtained that must be photographically enlarged. In compensa- tion, the defects within entire wafers may be imaged by simple scanning (Lang technique15) if the wafer is reasonably perfect, or by using the scan oscillation technique developed by Schwuttke16 if the wafer is warped or distorted. The purpose of this paper is to both review and extend the general application of X-ray topographic techniques to GaAs. Emphasis will be placed on the effects of growth and process variables on the quality and perfection of both bulk and epitaxial GaAs. Reference to optical or electron microscopy results will be made when useful. Since the effects on defects of a wide variety of processing variables such as crystal growing, sawing, polishing, diffusion, and epitaxial growth will be somewhat superficially reviewed, a fairly extensive bibliography of the most important recent results in these areas is included. However, for completeness, important defects will be illustrated here, although such defects have been previously shown by others. While this paper is concerned with defects rather than with the physics of X-ray scattering, the mechanisms of contrast formation in the topographs will of necessity be briefly mentioned. EXPERIMENTAL GaAs crystals, both boat-grown18 and Czochralski-grown,'8 containing a variety of dopants of various concentrations, were purchased from outside vendors. Wafers were sliced from the crystals using a Hamco ID saw and were mechanically polished using 1 µ diamond paste. Chem-mechanical polishing was done in bromine-methanol as described by Sullivan and Kolb.18 Chemical polishing was done using a modified sulfuric-peroxide solution, 11 parts H2SO4, 1 part 30 pct H2O2, 1 part DI water.5 Zinc diffusion was carried out in a closed tube, using a 10 pct Zn-In source at 825°C for 1 hr. Oxide masking techniques were used to select the area to be diffused. Epitaxial wafers were either purchased or prepared here. All epitaxial runs prepared here were carried out using a Ga-GaAs-AsC13 source in a closed tube at a substrate temperature of 750°C. Wafers were chem-mechanically polished and gas-etched prior to deposition. The X-ray topographs were taken on a Krystallos Lang camera, operating in the transmission scanning geometry (Lang technique15) or in the reflection scanning geometry (modified Berg-Barrett technique20,21). MoKa, radiation was used for all transmission topographs using a Jarrell-Ash 100-µ spot focus. CuKal radiation was used for all reflection topographs using a General Electric CA-7 1-mm spot focus X- ray tube. Topographs were printed from an intermediate contrast inversion film, so the contrast shown in all figures here is the same as that of the original 50-µ-thick emulsion L4 Iiford nuclear plate used to record the topograph.

Jan 1, 1969

By Arcy A., J. G. Davis, D&apos Shock

Results of a pilot operation in the Carlsbad Basin are discussed. After hydrafracing between wells, a block of potash was removed by solution techniques. The distance between frac wells was about 200 ft, the thickness of potash mineralization, 5 ft. By proper manipulation, a feed of concentrate brine was obtained. The ex-periment showed that the thin-bedded potash could be removed by the solution techniques. The details of well construction, method of operation, and removal rates are discussed. Continental Oil Co.'s laboratory research on the fundamentals of potash solution mining has been expanded by means of a series of field tests, and subjects such as well completion and hydraulic fracturing were added to the investigation. Both single-well and multi-well systems were studied in the field work. Discussion Background: The current paper discusses one field test in which potash was solution mined by a two-well system from a thin sylvinite zone. The potential economic value of solution mining evolves from (1) the use of drilled holes and solution techniques instead of excavated shafts and caverns and (2) the ability to mine both land and marine deposits through any type of overburden geology and below conventional mining depths. Recent interest has been focused on potash' and other soluble minerals, such as trona. Solution extraction minerals, such as copper and uranium, are also worthy of important consideration. In addition, many of the techniques are directly applicable to the construction of horizontal underground storage carverns in salt. There are two general approaches to potash solution mining. The first is to mine on a single-well basis, in which the same well bore is used for both injection and production. This method is slow, and the areal extent may be quite limited in other than very thick ore zones. The second, and the preferred approach, is to mine on a multi-well basis in which the solvent is circulated between wells. This technique, if applied in a manner which allows the ore zone to be mined from the bottom upward, results in nearly all the solution taking place from the cavern roof. Salt removal rates, therefore, are very much higher than from a single-well system.l Wells can be interconnected into a multi-well pattern by several means. One is to join single-well caverns in the lower part of an ore zone. Another is to use the hydraulic fracturing techniques developed in the oil fields.' We preferred the fracture approach because of its potential for creating the greatest area of salt exposure. Test Site Description: The field tests were conducted in New Mexico's Carlsbad Basin, where the potash deposits are flat and uniform over reasonable distances. Here, 12 potash zones are present in the massive Salado Salt section. The specific target was the Third Ore Zone which is about 4 ft thick at our location and about 1150 ft deep. The test pattern was designed in the shape of an equilateral triangle with a fourth well located in the center, 200 ft from each of the vertex wells. This configuration allowed the ore zone to be hydraulically fractured from the center well with good assurance that the fracture would intersect the bore of at least one outside well. Several multi-well test patterns would be available if the fracture connected all wells. Well Completion: Surface casing was set in the top of the Salado Salt at 600 ft to shut off water flows from the surface sands, and the salt section was drilled and diamond-cored to a point below the Third Ore Zone. A drilling fluid made of diesel oil with a small amount of emulsified water was used to drill and core the salt. This fluid was highly successful in preventing enlargement of the drilled hole and in promoting good core recovery. The three outside wells were completed by setting 51/2-in. casing at the base of a streak of anhydrite about 20 ft above the ore zone. Pipe was set high so that the intersection point of the fracture could be detected even if the fracture migrated above the ore zone as it progressed outward from the center well. The center well itself was completed by cementing 51/2-in. casing through the Third Ore Zone. Cement bond logs run on the center well have shown excellent bonding. Fracturing Practice: A mechanical tool was used to cut a notch through the casing and into the salt at a point about 1 ft below the ore zone in the center well. The purpose of this notch was to fix the point of fracture entry into the salt. The fracturing was done with water at injection rtaes as high as 30 bbl per min. The salt parted at 1450 psi; and it required only 5 min for the fracture to reach the well which was 200 ft to the south. It took about 5 min more to reach the other two wells. Caliper surveys were run to locate the point of fracture entry in the three outside wells. The fracture appears to have drifted downward slightly, entering the outside wells at the top of a streak of carnallite 8 or 9 ft below the ore zone. A cross section of the wells selected for the multi-well test is shown in Fig. 1. The figure includes KC1 values based on core analysis and the trace of the fracture plane between the wells.

Jan 1, 1971

By S. Kobayashi, A. E. Armenákas, C. Mylonas

Earlier work1-4 has shown that commercial mild steels under static loading at the lowest natural operating temperatures fracture in a brittle manner only when damaged by a suitable history of straining. Notched and then compressed plates have fractured in subsequent tension at loads as low as 10 pct of the limit load and precompressed smooth bars at a subsequent extensional strain as low as 0.01. The comparison of the average net fracture stress with the flow limit stress was shown to be an excellent criterion of brittle or ductile behavior of mild steel structures when only loads and general stress levels are known. The present investigation shows that the deformation at fracture is a far more sensitive measure of brittleness than the fracture stress. Both criteria, deformation and stress, are used to determine the amount of uniform precompression of two mild steels, ABS-B and Project E-steel, resulting in brittle fracture under the strong constraint of a subsequently machined severe circumferential groove. The fracture stress equaled or exceeded the theoretical flow limit Ól = 2.680., ('based on the elevated yield stress at each prestrain) up to prestrains of about 0.20 and then fell off to about 1 at prestrains of 0.60. Yet a prestrain of only 0.05 reduced the elongation at the shoulders by a factor of about 4. The total plastic elongation of a region surrounding a sharp notch in prestrained steel deternines whether or not fracture will be initiated in large structures, hence is a direct and realistic measure of the remaining ductility and provides an excellent test of the material's resistance to embrittlement. ALMOST all engineering structures of mild steel which failed in service in a so-called "brittle" manner exhibited appreciable local plastic deformation (more than 1 pct) and a mixture of "cleavage" and "shear" fracture surfaces. Furthermore, the peak local stress in an advancing crack is always high. Such simple criteria as pure cleavage, absence of plasticity, or fracture stress, so useful in other fields, are insufficient to characterize brittleness in engineering structures at ordnary temperatures. The "brittle)' behavior of engineering structures is caused by the limited ductility at cracks or notch regions, as shown by recent work at Brown University summarized and extended in Refs. 1 to 4. It was also shown that the local ductility of mild steel may be catastrophically reduced by a suitable strain and temperature history similar to those which may occur in real structures. Localized yielding begins at the notch roots at low loads but is contained by surrounding elastic regions. The plastic strains are hence small. They increase slowly with the load up to the flow limit or limit load for an ideally plastic material. Unrestricted plastic flow then occurs. At such strains the real material locally st rain-hardens and fractures. With work-hardening materials no flow limit exists, and the transition from low to high plastic strains is gradual but increases more rapidly at loads close to the flow limit of an equivalent perfectly plastic material. When the available ductility is sufficient for reaching the limit load, the behavior is normal or "ductile". With insufficient ductility, fracture will occur at a low load and will be defined as "brittle". Accordingly the sufficiency or not of the ductility at a notch is reflected in the magnitude of the fracture load or average net stress as compared with the limit load or flow limit. The application of this criterion gave surprising results. Service failures under semistatic loading occurred mostly below the limit load, hence were "brittle". On the contrary all static tests with undamaged commercial mild steels reached the limit load in spite of the deepest notches and temperatures below Charpy impact transition (say about -30°F or higher). Notched bars showed no brittleness even under fully dynamic axial loading up to 1.5 x107 psi per sec at -23°F and about 2.5 x l06 psi per sec at -ll0°F, but broke in a brittle manner at -200°F and l03 psi per sec.' To propagate a fracture at low load, experimenters had to trigger it by superimposing a strong dynamic impact at a notch cooled by liquid nitrogen as in the Robertson5 or Esso tests.' Once started the cracks would run through warmer regions of smaller stress. Obviously the ductility of the apparently undamaged commercial steels was "sufficient" in the laboratory tests but not in the service fracture, where it must have been reduced by some embrittling procedure of fabrication or service. These conclusions were confirmed by the achievement of low static stress (brittle) fracture initiation in unwelded steel after a local reduction of ductility by simple prestraining. Symmetrically notched plates of undamaged mild steel cooled below the Charpy V-notch transition range were tested in central static tension: Undamaged plates withstood loads of limit intensity, but when subjected to prior in-plane com-pressive prestraining perpendicular to the notch axis and to accelerated aging, the plates fractured completely or partially at very low static loads, as low as one-tenth of the flow limit.2-4 However, damage could not be easily related to the strongly variable prestrain around a sharp notch. To obtain easier strain measurements, it was decided to use axially precom-pressed bars and bent bars. Final testing was done by

Jan 1, 1970

By J. E. Dutrizac, R. J. C. MacDonald, T. R. lngraham

When sintered disks of synthetic chalcopyrite (CuFeS2) were leached in acidified aqueous solutions of ferric sulfate, the following reaction stoichiometry was obtained: CuFeS2 + 2Fe2(SO4)3 = CuSO4 + 5FeSO4 + 2S Over the temperature range from 50º to 94ºC, the reaction displayed parabolic kinetics. The parabolic rate constant for the dissolution of copper is given by the equation: log.k(mg2/cm4-hr)= 11.850 - 3780/T The activation energy for the dissolution process is 17 ± 3 kcal per mole. The parabolic kinetics have been attributed to the progressive thickening of a sulfur film on the surface of the chalcopyrite. When the leaching solutions contain less than 0.01 molar Fe+3 , the Fe concentration influences the rate of leaching, probably through a mechanism involving the diffusion of ferric sulfate through the sulfur layer. At higher Fe+3 concentrations, the rate control in the leaching. reaction has been attributed to the diffusion of ferrous sulfate through the sulfur. The rate of reaction is insensitive to changes in acid concentration and in disk rotation speed. ThE reaction of acidic ferric sulfate solutions with various sulfide minerals is of practical interest for both bacterial and heap leaching. This leaching medium is generally used with low-grade ores that cannot be treated profitably by conventional means. In both bacterial leaching1-3 and heap leaching, the active agent for sulfide dissolution is ferric sulfate. Although the reactions of ferric sulfate with chalcocite, covellite, and bornite have been investigated,4*7 the kinetics of leaching chalcopyrite with ferric sulfate have not been thoroughly studied. This paper reports a study of that reaction. EXPERIMENTAL Reagent-grade sulfur was purified by the method of Bacon and FanelliB and then it was vacuum-distilled to remove any soluble magnesium salts that had been introduced during the purification procedure.9 From stoichiometric quantities of the purified sulfur and hydrogen-reduced electrolytic copper sheet (99.90 pct Cu), CuS was synthesized at 450°C in a vacuum-sealed, pyrex vessel. About 24 hr was required for the completion of the reaction. A similar procedure involving hydrogen-reduced iron wire (99.90 pct Fe) was used to synthesize FeS1.002. A 2-furnace arrangement was required. The iron was heated to 800°C while the sulfur was maintained at about 400°C. Although the reaction to consume the sulfur was rapid, the material required additional heating (1 week) in a sealed silica ampoule at 800°C before it was homogenized. X-ray powder diffraction analysis confirmed that the copper sulfide was covellite and that the iron sulfide was troilite. The composition of the iron mineral was confirmed by wet chemical analysis. The two sulfides were ground to minus 100 mesh, weighed in equimolar amounts, mixed thoroughly, and pressed into pellets at 80,000 psi. The pellets were vacuum-sealed in pyrex ampoules and then sintered for 3 days at 550°C after an initial heating at 450°C for a few hours. The pellets were then cooled, polished with 3/0 emery paper, rinsed in acetone, and stored. The material had the characteristic brassy color of chalcopyrite and was shown by X-ray diffraction to be CuFeS2. Microscopic examination of the polished surfaces revealed small inclusions of pyrite (approximately 0.5 vol pct) as the only impurity. The presence of small amounts of a second iron compound will not alter the amount of dissolved copper but might increase the amount of ferrous ion slightly. It was calculated that dissolution of all of the pyrite and 100 mg of Cu (a typical value) would change the expected ferrous concentration by only 4 pct. Microscopic examination of a pellet after leaching revealed that the pyrite was not preferentially solubilized; only those pyrite grains at the surface were attacked. Hence, the pyrite is unlikely to alter the rate of copper dissolution. The chalcopyrite disks were about 1.7 mm thick and 27 mm in diam. They were about 80 pct of theoretical density, and for this reason their true reaction area was somewhat larger than the 5.8 sq cm area presented by the polished face. The disks were cemented to lucite cylinders in such a way that only the polished face was exposed. The disks were then leached by methods previously described.6,7 RESULTS AND DISCUSSION Stoichiometry and Kinetics. The initial experiments were directed to the problem of resolving the stoichiometry of the leaching reaction. Disks of CuFeS2 were leached at 80°C for various periods of time in acidified ferric sulfate solutions that were protected from oxidation by a cover of flowing nitrogen. When the disks had been partly leached, they were removed, their soluble salts were washed out, and then they were treated with CS2 in a Soxhlet extraction apparatus. The ratio of elemental sulfur to dissolved copper thus obtained was approximately 2 to 1. After the extraction of elemental sulfur from the pellet, the residue consisted of unreacted chalcopyrite only. For runs in which an appreciable amount of copper was dissolved, the ratio of ferrous ion to cupric ion in the solution was

Jan 1, 1970

By S. Shapiro, G. Krauss

The strutural and cr~stallo~aphic features of the plates of austenite produced by the martensite to aus-tenite or reverse martensitic tramformation have been determined in an Fe-33 wt pct Ni alloy. Micro-focus X-ray techniques and single-surface trace analysis 072 bulk samples yielded two distinct habit planes, (0.174, 0.309, 0.~35)~ and (0.375, 0.545, 0.749jM. The former plane uas the one predorninantly observed and its existence was verified by transn~ission electron microscopy. The orientation relation-ship between the reversed austenite and the parent martensite was approximately the same as the Nishiyamna and other relationships reported for the direct tramformation. Replica and thin-joil obser-vations show that both high densities of tangled dis-locations and occasional twins constitute the fine structure of the reversed austenite. Application of the phenomenological theory to a variant of the predominant habit plane defines an irrational plane and direction for the second shear in accordance with the comnplexity of the fine structure. The shear accompanying the reverse martensitic transformation is at least 0.51, the maximnum value of- the tangent oJ the tilt angle measured on surface replicas. A mechanism relating the fine transformation twins in martensite to the nucleation of reversed austenite of the predominant habit is proposed. The reversal of Fe-Ni martensite takes place both at the edges of martensite plates and in a piecewise fashion within them.' The shear-type nature of the reverse transformation is verified by the surface relief which accompanies both edge-type reversal2 and the fragmentation of plates of martensite' as a result of rapid heating above the A, (austenite start temperature). The orientation relationship between the edge-type reversal product and the parent martensite, as determined by transmission electron microscopy, is reported to be within 4 deg of either the Kurdyumov-Sachs or Nishiyama relationships,' but there is no work at present in the literature relating to the crystallography of the platelike reversed austenite. The fine structure of reversed austenite after heating to 50°C above the Af is reported4 to be composed primarily of tangled and jogged dislocations in concentrations up to 10" per sq cm. A replica investigation of partially reversed Fe-Ni martensites5 corroborates the increase in dislocation density following reversal and presents indications of other possible modes of fine structure. This paper reports on an investigation performed to examine in detail the morphology and crystallography of the plates of reversed austenite and the shear which accompanies their formation in a matrix of Fe-Ni martensite. EXPERIMENTAL PROCEDURE Discs of a high-purity Fe-32.9 wt pct Ni single crystal served as the starting material. The single crystal had been produced in the course of an earlier investigation6 and the carbon content was determined at the time to be 0.006 wt pct. The M,, and the A,, were respectively -120" and 300°C. Partial transformation to martensite was performed at -125°C and reversal of some of the martensite was accomplished by heating in the temperature range 340" to 355°C. Most samples were heated to the reversal temperature by immersion' in a salt bath for 2 min. For surface-relief studies some polished and etched Samples were heated in a tube furnace for ten min in a hydrogen atmosphere maintained over the samples throughout the heating and cooling cycles. Samples were prepared for metallographic examination by electropolishing and etching with an HC1-HNOs-H20 et~hant.~ On one of the surface-relief samples two sets of fiducial scratches were placed on the etched sample by drawing it over a slurry of 0.06 p alumina on a "microclothJ'. The orientations of individual plates of martensite were determined by X-ray analysis. A Rigaku-Denki microbeam X-ray generator in conjunction with a Micro-Laue camera with facility for precision location of the sample in front of the beam was employed for this purpose. The collimator size was 30 p and the specimen to film distance was 5 mm. The Laue photograms were enlarged to an equivalent 3-cm specimen to film distance for analysis. The orientation of each of the plates of martensite was compared to that of the parent austenite and the relationship be -tween the two phases was, in all cases, within a few degrees of those predicted for the direct transformation. The orientation relationship between one of the larger plates of reversed austenite and its parent martensite was determined in a similar manner. The habit plane of the islands of reversed austenite in the X-rayed plates of martensite was determined by a single-surface trace analysis. Each reversal island had with the parent phase one comparatively straight boundary which was presumed to represent the habit plane trace. The pole locus technique7 was applied to traces from six different plates of martensite to determine the indices of the habit plane. A 40-cm stereographic net was employed for this analysis The morphology and fine structure of the reversed austenite were studied by electron microscopy of pre-shadowed direct carbon replicas,5 and the macroscopic shear was evaluated by a two-stage replica technique similar to that employed in electron fractog-

Jan 1, 1968

By N. J. Grant, Per Knudsen, J. T. Blucher

The fatigue behavior of three SAP alloys was studied in ternzs of strain rate and temperature, at high strains. The k values in the modified Manson-Coffin equation, Nk4 = C, were less than 0.5 under all test conditions, and change with strain amplitude for the lower-oxide alloys at about 2 pct strain. Lowest k values were near 0.25. Strain rate had no effect on life at 80 F, but had an increasingly greater effect with increasing temperature above 500". Life decreased with decreasing strain rate, above 500"F, and with increasing temperature. Ductility at fracture in a tension test was indicated to be an important factor in determining 1ife in these big+-strain tests with the SAP alloys. INEVITABLY, in the course of mechanical tests at elevated temperatures, particularly if significant time at temperature is involved, there are large changes in structure; these changes make it difficult to relate behavior patterns over ranges of temperature or strain rates at high temperatures. Such changes are to be expetted in low cycle fatigue at low strain rates and high temperatures. Accordingly, it was of great interest to examine the low cycle fatigue behavior of SAP / an aluminum oxide dispersion-strengthened aluminum, a type of alloy which had shown unusual structure stability to temperatures as high as 1000" to 1150°F and resisted recrys-tallization essentially to the melting temperature.'j3 Since the matrix is pure aluminum, there are no complications of averaging, agglomeration, or phase solution. It was also desirable to check the Manson-Coffin equation4?' for the SAP alloys, namely N~E~ = , where ep is the total plastic strain amplitude, k and C are constants, and N is the number of cycles to failure. Here, too, was an opportunity to check the roles of temperature and strain rate with a very stable material. Tavernelli and coffin6 had concluded that k had a value of about 0.5 for many alloys and C was equal to ~/2, where E is the fracture ductility determined from a static tension test. The results were obtained from low-temperature tests where creep and diffusion processes are unimportant. Manson7 found k = 0.6 fitted his data reasonably well; however, in later analyses of a large amount of low cycle fatigue data generated at room temperat~re@"~ he found k to vary from 0.6 for short lives to 0.21 for long-life fatigue tests. In the latter studies,89g Manson separated the total strain range into elastic and plastic components when he found that k was influenced by the nature of the strain. The use of EL (total strain) instead of EP (total plastic strain)4'5 makes a difference in the resultant k value. The ratio of changes with temperature, strain rate, and strain; further, there are the problems in the determination of the elastic strain. Based on these considerations, and the improved fit of points in a plot of by Wells and Sullivan,' is also utilized in these studies. Anderson and wahl,14 using commercial 1100 aluminum, and Blucher and Grant,15 using 99.99 pct pure aluminum, found an increase in life with increasing test temperature. Anderson and Wahl were the first to report low cycle fatigue results from SAP materials. With increasing temperature, the role of strain rate becomes more important. In this regard, care must be exercised to differentiate between frequency (wherein strain rate may vary from zero to a maximum in each cycle, sinusoidally, for example), and constant strain rate, as used in the present study, in a saw-tooth type cycle; in the latter case, the frequency is not specified but can easily be calculated from the strain and strain rate data. It has generally been found that life in low cycle fatigue tests decreases with decreasing frequency16 or with decreasing strain rate at elevated temperatures.15 Coffin,17 reviewing Eckel's work,16 also reported that k increased with decreasing frequency for acid lead, yielding values from 4.0 at a frequency fo 6.6 cycles Per day to 1-46 at a frequency of 7440 cycles per day; the value of k decreased to 0.58 at a frequency of 2.38 x lo6 cycles per day. EXPERIMENTAL PROCEDURE Three SAP alloys, of two nominal compositions, were tested. Alcoa supplied XAP 005 as 2-in.-diam extruded bar, of nominal composition A1-7 wt pct A1203. The Danish Atomic Energy Commission supplied SAP 930 (A1-7 wt ~ct Ala3) and SAP 865 (A1-13 wt pct Al&) manufactured by Swiss Aluminium Ltd., in the form Of $-in.-diam extruded rod. Metallographic comparison of the structures of XAP 005 and SAP 930 showed the former to have a more uniform oxide distribution. Button-head specimens were machined in the longitudinal direction of the bar with 0.4 in. gage length by 0.2 in. diameter, with a fillet radius of j-B in. After machining, the specimens were electropolished in a 1 to 4 mixture of perchloric acid to methanol to remove all machining marks. All test bars were in the as-extruded condition. The fatigue tests were performed on a hydraulically activated, axial strain machine, with complete reversal of strain.15 Test conditions were:

Jan 1, 1969

By Malcolm McColl, C. A. Mead

Thin films (of mica have unique attributes that are exceptionally good for studies of high-field conduction mechamisms in thin-film insulators and the quantum mechanical tunneling of electrons from metal to metal. The principal advantages of using mica films are that the films are crystalline and the cleavage planes occur every 10Å. This property results in films whose thicknesses are integral multiples of 10Å and whose surfaces are uniformly parallel over sizable areas. Hence, very well-defined metal -mica-metal structures are possible. Furthermore, the fact that the insulator is split fro??! a bulk sample allows the index of refraction, dielectric constant, forbidden energy gap, and trapping levels and their density- to be obtained directly from measurements performed on thick samples Of mica rather than requiring that these properties be interred from the conduction characterrsties alone. In the work to he described, all the cleaving was done in a high vacuum just prior to the evaporation of metal elertrodes so as to avoid air contamination at the interfaces. Results of these studies indicate that the current through the 30 and 40Å films exhibited quantitative agreement with the theoretical voltage and temperature dependence derived by Strallon for the tunneling of electrons directly from metal to metal. Thicker films at room temperature exhibited volt-ampere curves suggesting Schottky emission of electrons from the cathode into the conduction band of mica. However, the thermal activation energy was smaller than that found from other measurements, and the experimsntal Schottky dielectric constant was larger than the square of the index of refraction. These facts would indicate that the electrons were being injected into polaron stales ill the iusulator. At low temperatures and high fields, the current through the thicker films did not exhibit the Fowler -Nordheim dependence as would be predicted by a simple extention of the theory of field emission into a vacuum. THE mechanism of electrons tunneling through insulating films has received considerable attention in the last few years due to the devices possible utilizing tunneling'-4 and the success of tunneling in the study of superconductivity.5,6 Until the recent paper by Hartman and chivian7 on the study of aluminum oxide, there had been no reported successful quantitative experimental fit to the theory. Their method of fabrication necessarily results in a polycrystalline insulator, the stoichiometry of which is nonuniform from one side to the other. This structure also introduces complications to the shape of the barrier which is set up by the insulator since the insulator possesses a spatially nonuniform band structure and dielectric constant. Due to these facts an analysis of the data in terms of a pviori barrier shape is of questionable validity. The use of muscovite mica not only overcomes these disadvantages but, as an insulating thin film, provides physical properties (dielectric constant. trapping levels and their densities, forbidden energy gap, and so forth) that are identical to the easily measured values of the bulk sample. Furthermore, it is a single-crystal insulator whose cleavage planes (10Å apart8,9) provide uniformly parallel surfaces of well-known separation. This material is therefore ideally suited to the study of electron-transport phenomena. Von Hippel10 using a 6.5-µ-thick sample was the first to observe the high-field conductivity (=5 x l06 v per cm) of mica. No attempt was made to develop an empirical formula, but Von Hippel concluded from intuitive arguments that the current was being space-charge limited by trapped electrons. Mal'tsev11 in a more recent investigation at high fields observed a dependence of the conductivity a on the field F of the form exp(ßF1/2). This dependence was attributed to the Frenkel effect,12,13 a Schottky type of emission from filled traps. No mention in the English abstract was made of the thicknesses of his samples or, and more important, of how well the value of ß fit Frenkel's theory. In 1962 Foote and Kazan14 developed a technique for splitting mica to a thickness of less than 100Å and observed a dependence of the current density j on the field of the form j = jo exp(ßF1/2) on a thin sample thought to be 40Å thick. Assuming that this was a Schottky emission process and that the appropriate dielectric constant for such a mechanism would be closer to a low-frequency value of 7.6, Foote and Kazan calculated from ß an independent thickness of the mica of 36Å. No further investigation was made of the phenomenon. However, the work reported in this paper indicates that the film measured by Foote and Kazan was probably 60Å thick, the error arising from the measurement of the very small metal-insulator-metal diode areas that were used, along with the diode capacitance and dielectric constant, to calculate the thickness. In the research reported in this paper, Foote and Kazan's technique was modified to cleave muscovite in a vacuum of 10-6 Torr, immediately after which metal electrodes were evaporated creating Au-mica-A1 diodes. Aluminum was chosen because of its strong adhesion to mica, as necessitated by the

Jan 1, 1965

By Donald E. Meyer

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

Jan 1, 1970

COUNCIL The following served on Council during the year under review: Office bearers: Messrs V. C. Robinson (President), Prof D. D. Howat and Dr J. P. Hugo (Vice-Presidents), J. K. E. Douglas (Immediate Past President) and D. G. Maxwell (Honorary Treasurer). Ordinary Members of Council: Dr M. G. Atmore, Dr J. M. Bereza, H. P. Carlisle, W. W. Malan, C. E. Mavrocordatos, Prof R. P. Plewman, Dr R. E. Robinson, Dr M. D. G. Salamon, P. W. J. van Rensburg, L. W. P. van den Bosch, P. A. von Wielligh. Branch Chairmen: J. Meintjes, J. M. Meyer (Acting), J. N. Saunders (Retired). Past Presidents serving on Council: R. J. Adamson, M. Barcza, H. Britten, R. C. J. Goode, P. Lambooy, Prof J. de V. Lambrechts, Dr J. T. Mclntyre, J. F. Reid, H. Simon. Ten Council meetings were held during the year with an average attendance of eighteen and the standing committees held forty-six meetings. FINANCE The annual accounts, which are attached to this report, show an excess of income over expenditure of R5 051 compared with an excess of expenditure over income last year of R4 608. This major reversal of fortunes is due in the first instance, of course, to the increased subscriptions. There were, however, other important contributors, particularly sales of the Proceedings of the Symposium on Open Pit Mining and profits on the operation of symposia and colloquia. It would appear from a study of the accounts that there has been a substantial drop in expenditure on secretarial fees. In actual fact, however, our total expenditure on secretarial fees was higher. A portion of this expenditure was charged against the administration of the Symposium on Open Pit Mining and, in addition, the charge against the Journal accounts for secretarial fees was increased. It will be recalled that in last year's annual report it was mentioned that subsequent to the new arrangement for publication of the Journal, the expected improvement in the finances of the Journal had been slow in materialising. After a total period of 18 months there was still no sign of improvement and it was accordingly decided to end the arrangement. As a result, the drain on the finances of the Institute was considerably lessened in the second half of the year. During the course of the year Council became concerned about the rapid depletion of our accumulated funds and gave careful and detailed attention to all aspects of the Institute's financial affairs. Particular attention was given to: 1. The fact that the Institute does not have a solid financial backing and must appeal for funds every time any special event such as a symposium is held. 2. The responsibilities of the Institute to the profession and the community, with particular reference to the desirability of establishing Institute bursaries and participating in other educational activities. 3. The rapidly rising cost of living. 4. The immediate financial position of the Institute. 5. The rapidly increasing cost of publishing the Journal due to the increasing number of papers available. In the meantime the immediate financial position of the Institute has improved but as this is due largely to non-recurring or irregular items of revenue, it should not be given undue weight. After careful consideration it was decided that an appeal should be made to industry for financial assistance, which would be used to cover the cost of symposia and other unusual expenditure and also, if possible, to build up the capital resources of the Institute so that there is a solid foundation for the future. Before appealing to industry, Council wished to be quite certain that there could be no criticism of the Institute for not having done our best in a personal capacity. Furthermore, Council examined many comparative statistics, including those circulated to members, which showed that, while expenditure per member has risen at an average annual rate of 7,5% over the last fifteen years, subscription revenue per member has risen at only 3,4% per annum. It was with this background that your Council decided to raise the subscriptions. Initial approaches have been made to the big mining groups and there has been a very generous response, although the details of how financial assistance will be provided have not yet been worked out. It seems likely that some form of affiliated company membership will be the most suitable method of achieving this. When these details have been fixed, it is the intention to extend the appeal to all corners of the mining industry as well as manufacturing and metallurgical industries. It is believed that these measures will ensure that the finances of the Institute are placed on a firm foundation on which the expanding activities can be planned. The MacArthur Forrest Memorial Fund shows an excess of income over expenditure of R73 and the total fund was, therefore, increased by this amount to R4 411. The balance sheet shows that the market value of quoted shares and debentures increased during the year fron R6 540 to R9 160. The market value is now almost exactly the same as the book value. Accumulated funds now amount to R23 010 compared with R17 959 a year ago.

By Geo. A. Brown

This paper was written from conditions existing in the Cumberland Mines of The Union Pacific Coal Co., with my impressions and cause of same. These mines are located on a branch line of the 0. S. L. R. R., about sixteen miles south of Kemmerer, Wyoming. The mines are the property of The Union Pacific Coal Company with headquarters at Rock Springs, Wyo. There are two mines, No. 1 and No. 2, located about two miles apart in a seam of coal averaging about 16 feet thick which is split with a parting of rock from 4 feet to G feet from the bottom, averaging from 4 inches to 5 feet thick, mostly of soft fire clay, with an average pitch of 21 degrees to the west. The lower coal below the fire clay band being of a soft nature, much softer than the coal above it. The cover or roof next to the coal is of a massive sandstone formation from 4 feet to 60 feet thick while the floor of the seam is of a soft fire clay as far down as has been prospected. These mines are also of a dry and dusty nature, they generate lots of fire damp and are subject to fires from numerous causes. These mines were opened up in 1900 with five openings each, Main Slope, North and South Manways and North and South Aircourses driven parallel directly on the pitch of the seam which is fairly regular, entries being turned North and South at right angles off the slope about 300 feet apart. The entries were driven double 10 feet wide with chain pillars from 20 feet to 30 feet thick. The main entries are used for haulage and main intake, back entries for return aircourses. Rooms are turned on 50-foot centers and 20 feet wide, directly on the pitch Galvanized sheet iron chutes are used in the rooms. The slopes were driven down in No. 1 mine about 4,000 feet, in No. 2 mine about 5,000 feet where the cover would be about 1,400 feet in No. 1 mine and about 1,700 feet in No. 2 mine approximately. When a point about 2,000 feet on the slope had been reached with cover, 600 or 700 feet squeezing became noticeable on the entries and room pillars with slight bumps which extended clear to the upper entries of the mines and continued to get worse as the mines got deeper and with more cover as no pillars had been removed at this time. It should be stated here that faulty ground was found on the south side of No. 2 mine and on the north side of No. 1 mine, in some places looking like a fault of a down throw, some places like a want and other places like an erosion. The latter theory seems to be correct from prospecting and drilling. The mining of entries and rooms became more difficult with more squeeze and bumps of increased pressure which closed entries and aircourses and finally caused the lower workings of the mine to be abandoned. It was then decided to open up the entries from the 6th up, or approximately half way up the slope. The opening of these entries was started with the intention of extracting pillar coal but considerable danger was met with for the entries .were squeezed tight and when they were disturbed, bumps and squeeze conditions had to be contended with, also gas and fires due to the continued grind on the pillars due to overhead pressure bringing on friction which caused innumerable fires to start in the bottom coal. Bumps being so extensive at times as to close up aircourses for 500 or 600 feet, also discharge timber, coal and rock from the rib of slope and entries for hundreds of feet, dislodging tracks and throwing mine cars around just as if an explosion had taken place, filling places with gas and throwing dust into the atmosphere so that you could cut it with a knife. It became necessary to discontinue the use of black powder and naked lights entirely as a safety precaution. Permissible Powder Monobel No. 5 and Wico Electric Safety Lamps were installed. All coal was shot off the solid whenever it was necessary to shoot. ' In opening up these entries it was found that practically all of the weight was centered on room pillars up to the first crosscut chain pillars and barrier pillars between top of rooms of entry below and the one above which averaged 30 feet thick and in all practically 120 feet of ground. The rooms were mostly open from the first crosscut up to the face which showed that the points mentioned had taken the weight. It was found impossible in some of these entries to drive double entries again as the bumps and squeeze made it impossible to maintain them. This made ventilation quite a problem, small booster fans and flexoid tubing being used for ventilation until one entry could be connected with the one above which has solved most of our ventilation problems so far.

Jan 1, 1924

By D. P. Pope, T. Vreeland

Observations of dislocations in zinc using Berg-Barrett X-ray micrography confirm the validity of a dislocation etch for (1010) surfaces. A technique for measurement of the depth in which dislocations can be imaged in X-ray micrographs is given. This depth on (0001) surfaces of zinc was found to be 2.5 µ using a (1013) reflection and CoKa radiation. BUCHANAN and Reed-Hill (B & RH) have recently questioned the ability of a dislocation etch to reveal all of the basal dislocations which intersect (1010) surfaces in annealed zinc crystals.' This etch was developed by Brandt, Adams, and Vreeland who conducted a number of different experiments to check its ability to reveal dislocations.2,3 B & RH prepared (0001) foil specimens for transmission electron microscopy from annealed crystals and observed dislocation densities of about l08 cm per cu cm in the foils, while the etch indicated densities of the order of l04 cm per cu cm in their annealed crystals. As this etch has been used in a number of studies of dislocations in zinc, it is of considerable importance to reassess its validity in the light of the B & RH results. The X-ray work reported here was undertaken to check the ability of the etch to reveal dislocation intersections on (1070) surfaces of zinc. The X-ray technique was chosen for this check because it could be applied to the as-grown crystals with a relatively small amount of specimen preparation. We believe that the possibility of accidental deformation in preparation of the bulk specimens is considerably less than that for thin foil specimens suitable for transmission electron microscopy. Unfortunately, basal dislocations are not visible on Berg-Barrett topo-graphs of (1010) surfaces, which are the surfaces on which the etch is most effective. Therefore, a one-to-one correspondence between the etch and X-ray observations could not be made. Basal dislocations near (0001) surfaces have been observed by Schultz and Armstrong4 using the Berg-Barrett technique, but they did not report the as-grown dislocation density observed in their crystals. We have applied the X-ray technique in this study to surfaces oriented from 1 to 2 deg of the (0001) to determine the basal dislocation density, and have compared this density with that observed using the etch on a (1070) plane of the same crystal. The X-ray observations permit determination of the depth in which basal dislocations can be observed under the diffracting conditions used. SPECIMEN PREPARATION High purity zinc crystals are very soft, so a good deal of care must be exercised in the preparation of observation surfaces. As-grown crystals approximately 2.5 cm in diam and 20 cm long were acid cut into 1.25 cm cubes. A thin slab was cleaved from an (0001) surface to produce an accurately oriented reference surface on the specimen. Some of the cubes were examined in the as-machined condition while some were annealed in argon at 410°C for 2 hr. Heating and cooling rates were less than 2°C per min. Some of the specimens were scratched on a (0001) surface with a razor blade to produce fresh dislocations. Approximately 2 mm of material was acid lapped from one face of a cube to produce a surface oriented between 1 and 2 deg from the basal plane and parallel to the [1210] direction. A (1070) surface was also acid lapped. The lap used a 1 to 3 pct solution of HN03 in water to saturate a soft cloth which was backed by a stainless steel plate. The cloth was moved over the crystal surface at a rate of 20 cm per sec while a normal force of about 4 g was maintained between the cloth and the specimen. As-lapped surfaces were examined as were surfaces which were chemically and electrolytically polished after lapping. The small angle between a lapped surface and the (0001) plane was measured to 0.1 deg using a Unitron microgoniometer microscope (the cleaved surface was used as a reference in this measurement). The microscope was modified so that the intensity of reflected light could be continuously monitored on a meter. This modification produced nearly a ten-fold increase in the reproduceability of orientation readings. OBSERVATIONS The Unitron Microgoniometer observations indicated that the lapped surfaces had a terraced structure with the terraces quite rounded and spaced about 0.1 mm in the [1010] direction. The maximum change in slope between terraces was 0.25 deg, indicating a terrace height of about 0.1 µ. A Unitron measurement of the average angle between (0001) and a lapped surface was checked by micrometer measurement of the specimen and found to agree within 0.1 deg. The Berg-Barrett micrographs using (1013) reflections and CoKa radiation5 revealed subboundaries, short dislocation segments, spirals, and loops near the surfaces which were oriented from 1 to 2 deg of the (0001). Micrographs of surfaces prepared by lapping appeared very similar to those of the chemically and electrolytically polished surfaces. The loops and spirals were not extinct in (1013) or (0002) reflections, indicating that they have a nonbasal Burgers vector. Extinctions of the short, straight dislocations indicated that they belonged to an (0001)(1210) system. Fig. 1 is an example of a micrograph which shows a subboundary, and dislocation segments which are pre-

Jan 1, 1970

By M. Saghaeian, R. Hejazi, V. Sheikhzadeha, A. H. Baladastian, A. Dehghani Ahmadabadi

This paper describes research done to remove apatite (phosphorus) from hematite ultrafine (70% finer than 25 micron) concentrate, recovered by electromagnetic separators at the FST Tailing Recovery Plant located in Chadormalu Iron Ore Complex through reverse froth flotation. As a result, iron and phosphorus content in magnetic concentrate (flotation feed) were 53.52% and 0.58%, respectively. Therefore, to increase the Fe content and decrease the P content of the sample, reverse flotation tests were applied. Chemical reagents used in this research consisted of sodium silicate as a depressant, sodium hydroxide and sodium carbonate as pH regulators, Alke & Dirol as fatty acid collectors and MIBC as frother. Process parameters including dosages of collectors, depressant and frother, preparation times of depressant and collectors, steps and time of frothing and pH range were selected. After doing flotation tests, in optimum condition, dosages of collectors were 1200 g/t, depressant 1200 g/t, pH in the range of 9.5 to 10, preparation time of collectors in the first step was eight minutes and at the other steps, four minutes; the number of frothing steps 4 and frothing time in each stage was three minutes. In this case, it was observed that the amount of phosphorus in the final concentrate was reduced to 0.05%, the Fe content increased from 53.52% to 61.66% and the Fe recovery achieved was 82.21%. Keywords: Iron ore, hematite ultrafine concentrate, iron and phosphorus content

Jan 1, 2020

By M Spagnolo, M Ashley, D, L Reemeyer

PasmincoÆs Century Concentrator in North West Queensland commenced operations in November 1999. The nameplate production capacity of 500 000 tpa of zinc metal production in concentrate was achieved in August 2002. Completion of the production ramp up was successful due to the culmination of a number of initiatives throughout 2001 and 2002. Mine to mill interaction to understand and eliminate head grade related bottlenecks affecting Concentrator production and reduce feed variation. Grinding circuit process development û operating and process control strategies to improve stability and reduce grind size to support zinc recovery. Pumping upgrades to control spillage in ultrafine zinc flotation Low density zinc flotation strategy û to improve silica-sphalerite separation to improve zinc recovery while maintaining acceptable silica in final concentrate. Flotation circuit process development û froth crowders, froth cameras and reagent control strategies to improve primary zinc flotation performance. Review and implementation of longer campaigns between planned shutdowns to improve availability. Team reorganisation û to improve setting and implementation of metallurgical strategies. This paper describes these initiatives and their contribution in achieving the production target. It also notes the ball mill motor failures that delayed the successful achievement of the ramp up, and CenturyÆs response to minimise the production impact. The paper also outlines the capital improvement program that was implemented to improve zinc recovery to design 82.5 per cent recovery once the production rate had been achieved.

Jan 1, 2003

By C. E. Seaman, H. Jiang, S. Klima, T. W. Beck, Y. Zheng

Respirable coal dust has been long recognized as a leading cause of multiple lung diseases. Efforts aimed at reducing dust concentration in underground mines have been made, but increases in coal workers’ pneumoconiosis incidence rates over the last 20 years among U.S. miners are concerning. Dust deposition and water spray suppression are two types of dust removal mechanisms in underground mining activities. In this study, laboratory tests were conducted to investigate the respirable dust decay characteristics during deposition and suppression processes in a confined dust chamber. Dust concentration and size distribution were monitored continuously throughout each 60-minute test. A number-basis particle size distribution was used for analysis to capture the changes of smaller size fractions within the investigated dust sample. This study found that around 62.1% of respirable dust particles were deposited at the end of the deposition test. In addition, the final deposition rate for very fine particles can be less than 20%. The results from the suppression test indicate that larger particles were removed quickly; however, sub-micron particles remain suspended through the 60- minute water spray, and particles under 0.5 µm can be considered irremovable dust under single-spray operation conditions. This study also observed the resuspension of a significant amount of sub-micron particles by the water spray. The results of this study provide basic information for improving dust control strategies and can be utilized to improve the water spray performance for reducing airborne dust levels.

Mar 2, 2022

By Ayumu Tokumaru, Shuji Owada, Gangfeng Liu

"Several million spent catalytic converters are disposed annually worldwideandeach containing about 0.5-1g ofplatinum and 1-2g of all the platinum group metals (PGMs), then,it is fairly significant to recover PGMs from the spent automobile catalyst. The PGMs’ recovery is a proven technology, including pyro-and hydrometallurgicalmethods, and the highestrecovery can achieve approx. 98 wt.% by acid-leaching method, but theserecyclingtechnology seems to be too highlyenergy-consuming. SincePGMs aredistributed only in coat layer in spent catalyst, it is of great significance to enrich the coat layerwith some physical methods as a pretreatment.In this paper, according to the double-deck structureof the catalyst andthe different properties of the two main compositions, alumina-ceria phase of coat layer and cordieritephase of substrate, the concentration of the coat layer was investigated by combiningthree kinds of physical separation technologies, heating-quenching, crushing and surface grinding. In the first stage, thermal stresscouldgeneratebetween the two phasesby thermal expansion difference,to producefracturesin the thinnest part of coat layerand micro-cracksin coat layerand at the interface of coat layerand cordierite substrate. The second stage of crushing, by jaw and roll crushers, could break dominantly the coat layer and the third stage of surface grinding, carried out by attritor, promoted further separation and concentration of coat layer fromthe substrate.We also improved the attritor grinding by adding a new lift-arm to the cell for achieving better mobility of sample particles in the selective surface grinding."

Jan 1, 2014

By N. R. Mandre

In the present work an attempt has been made to study beneficiation of low-grade iron ore associated with manganese clay by selective flocculation. The representative samples obtained for this purpose were initially subjected to chemical and mineralogical studies. The chemical analyses indicated 42.56 % Fe, 6.25% Mn, 8.72 % SiO2 and 13.60 % Al2O3 in the representative sample. The mineralogical analyses carried out under optical microscope showed that the ore mineral predominantly comprised of iron oxides and hydroxides along with manganese and silicate as gangue minerals. Prior to the beneficiation studies, the samples were subjected to settling tests. These tests were carried out by using poly acrylic acid (paa), poly acryl amide (pam) and guar gum (gg) as the flocculants. From these studies it was observed that settling rate of particles increases with increase in pH and a maximum settling rate of 0.23 cm/secwas obtained at pH 9 in presence of poly acryl amide. Further, the samples were subjected to selective flocculation studies using above-mentioned reagents. From these studies better results were obtained in the experiments carried out with poly acryl amide as the flocculant. Thus, it was possible to upgrade the iron content from 42.5 to 53%, with a recovery of 92%. However, 51% Fe with recovery of 87% and 50% Fe with recovery of 94 % was obtained using poly acrylic acid and guar gum respectively.

Sep 1, 2012

By Luíza Freire Arold

Placas de Circuito Interno (PCI’s) são partes fundamentais de um computador, uma vez que são responsáveis pelo bom funcionamento deste. Porém, seu descartadas em áreas clandestinas, podem causar danos ao meio ambiente e a saúde pública, pois estas placas podem ter na sua composição elementos tóxicos que as tornam perigosas. O presente estudo visa qualificar e quantificar os metais presentes na fração não magnética das PCI’s, a fim de que subsequentes processos de recuperação de metais possam ser aplicados. Para que as análises pudessem ser feitas, as PCIs foram submetidas a etapas de moagem, quarteamento, separação magnética e digestão em água régia. As placas foram moídas em um moinho de martelos, utilizando grelhas de 2 mm. O resíduo cominuído seguiu para a etapa de separação magnética, obtendo-se duas frações, uma fração magnética e uma fração não magnética. Em seguida, a fração não magnética foi quarteada em amostras de 20 ± 5 g. Para realizar ensaio de digestão em água régia, foi escolhida aleatoriamente uma amostra. A digestão foi realizada durante 24 h a temperatura ambiente usando-se uma proporção sólido: líquido de 20:1. O licor obtido nos ensaio de digestão em água régia foi levado para análise química por espectrometria de emissão óptica por indução de plasma (ICP-OES). Os resultados mostraram que as placas de circuito impresso de computadores contêm na sua fração não magnética aproximadamente 60% dos metais da placa de vídeo.

Aug 7, 2018

By Williams RE, Ralston DR

Acid mine drainage is a serious environmental and economic concern, resulting in regulation of the mining industry and significant water treatment costs. An interdisciplinary approach is needed to analyze the many aspects of a complex acid drainage problem. This paper describes the integrated application of techniques from the following fields to the characterization of acid drainage at a large underground lead-zinc mine: 1) hydrogeology, 2) surface stream analysis, 3) structural analysis of fracture distribution, 4) hydrochemistry, 5) geostatistics, and 6) multivariate statistics. The Bunker Hill Mine in northern Idaho, is developed in highly fractured and faulted quartzites and discharges 95 L/sec of water with an average pH of 2.8 and an average zinc concentration of 120 mg/L. Research has been conducted on all aspects of the acid water production and drainage problem. Recharge to the mine has been investigated using geophysical techniques and tracer studies. Fracture mapping and geostatistical analysis of the fracture data have been used to determine characteristics of inflow to the mine workings. Hydrograph analysis techniques have been applied to water flow data within the underground workings. Chemical sampling and analysis have been used to identify acid producing workings, and better understand mechanisms controlling acid water production. Multivariate statistical techniques have been applied to analyze the quality and flow data. Research results from the many subprojects of the Bunker Hill study reveal the importance of an interdisciplinary approach to the analysis of acid mine drainage problems.

Jan 1, 1988

By Priscilla Danielle de Oliveira Lopes Costa

Na indústria aeronáutica, fadiga é um dos processos mais importantes quando se considera o dano e a falha das estruturas de uma aeronave. Adicionalmente, os materiais compósitos apresentam altas resistência e rigidez específicas. No entanto, os mecanismos de dano de um material compósito são complexos. Como consequência, o objetivo deste trabalho é identificar as propriedades à fadiga de materiais compósitos de fibras de carbono e resina epóxi, com configuração de lâminas 0°/90°/±45º e caracterizar os mecanismos de dano quando estes são submetidos à fadiga. Para tanto, nos corpos de prova foram realizados ensaios de fadiga em uma máquina universal de ensaios MTS, em controle por tensão com frequência de 10 Hz com carregamentos máximos de 6000, 5000, 4000 e 3000 N e R = 0,1 (tração-tração). O compósito em estudo demonstrou boa resistência à fadiga por controle de tensão, a vida infinita é de aproximadamente 48,5% da resistência à tração. O número de ciclos a fadiga depende da amplitude de tensão, assim como da tensão média, sendo que quanto menor a carga aplicada menor a amplitude de tensão (e a tensão média) e maior o número de ciclos a fratura. A fractografia após os ensaios caracterizou os mecanismos de dano durante o processo de fadiga, sendo que fratura na matriz, fratura das fibras e descolamento fibra/matriz são os mecanismos de falha dominantes durante a fadiga, através de análise por microscopia eletrônica de varredura.

Aug 7, 2018

By J. L. Gaigher

A simple mineralogical regression model is described, which was devised in order to help the flotation plant cope with rapidly changing headgrades and feed mineralogy. Minerals in the feed were determined by means of quantitative X-ray diffraction and compared with plant performance parameters and flotation reagent consumption rates, using regression analysis. A mineralogical regression model for predicting recovery served to motivate flotation plant personnel and also set standards whereby flotation performance could be measured. The reagent consumption model indicated in which direction any or all of five flotation consumption rates should be altered. All practically measurable parameters, even those showing poor or no correlation, were included in the model, provision being made for the continuous update of a batch of data of 30 lines. Compared with the method of multiple linear regressions, the r2 is poorer at 0,41 (versus 0,50), but the mean standard error of estimate for both methods is identical at ± 6,6 units. The regression model is simpler than the method of multiple linear regressions, and although the accuracy of prediction is not high (41%), the mineralogical regression model proved to be successful in practice. Flotation efficiency, as measured by the mean ratio of head to tails grade, for the 9 month period after the mineralogical regression model was implemented on an hourly basis, improved from 2,8 to 3,2, which is equivalent to an improvement in average flotation recovery of 5% relative.

Jan 1, 1987