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By J. G. Morlet, A. R. Troiano, H. H. Johnson

Delayed failure in steel occurs by controlled initiation and growth of a crack. The incubation period for crack initiation was measured. Crack initiation and Propagation are controlled by interaction between hydrogen concentration and triaxial stress state. The incubation period results from stress-induced diffusion of hydrogen to the point of crack initiation. THIS paper describes the phenomenon of delayed failureland the kinetics of crack initiation and propagation in uniformly hydrogenated steel. The investigation was prompted by service failures of high-strength-steel components at applied stresses far below the conventional yield strength, after the part had successfully sustained equal or higher stresses for an extended time interval. This delayed failure phenomenon, often termed static fatigue, is associated1 with the presence of hydrogen. This is not surprising, since the voluminous literature on flaking and hydrogen embrit-tlement demonstrates that hydrogen may exert a potent embrittling influence. Flakes, or internal hairline cracks in alloy-steel forgings, are related to the presence of hydrogen retained from the steel-making process.2 On the other hand, embrit-tlement arises from hydrogen introduced during surface treatments such as acid pickling or electroplating. Laboratory delayed failures have been induced in notch specimens of 4340 steel by electrolytic charging of the specimen surface with hydrogen and subsequent static stressing.l,4,5 Static fatigue was observed over a wide range of applied stresses; however, failure did not occur below a critical applied stress, designated as the static fatigue limit. In this instance the extended time for failure resulted primarily from the macroscopic redistribution of hydrogen. A crack formed to the depth of the hydrogen enriched "case* upon loading; further crack growth naturally awaited diffusion of hydrogen into the material ahead of the crack. The crack-propagation rate was therefore controlled primarily by the macroscopic diffusion of hydrogen into the specimen interior during the test. Thus, in this instance static fatigue was associated with the movement of a gross concentration gradient. However, delayed failure in steel of uniform hydrogen concentration is of greater fundamental interest, as well as commercial significance. With a homogeneous hydrogen distribution a different mode of delayed failure might be expected. As the heterogeneous hydrogen distribution became more uniform,4,5 the initial crack-propagation rate decreased markedly and, in fact, what appeared to be an incubation period for crack initiation was observed. However, the macroscopic concentration gradient precluded an accurate evaluation of these observations. Although the existence of an incubation period, up to this time, has not been established definitely, it is not amiss to point out some implications of the concept. It is of interest in all hydrogen-induced embrittlement phenomena, such as flaking, delayed failure, and hydrogen embrittlement. Much discussion has centered around the possibility of an

Jan 1, 1959

By J. E. Wilson, F. P. Lebar

TYPICAL of southwestern Wyoming are coal structures that dip from 4° to 17°. Those at the Reliance and Winton mines of the Union Pacific Coal Co. average 91/2 and 15°, respectively, and dip almost directly to the west. By using a hoist for main haulage, a method of mining has been developed whereby four places are driven on the pitch of the seam. Slightly upgrade from the strike at intervals of 300 ft. a two-entry system is driven to the north and to the south. In both fields, which are nongassy, an exhaust system of ventilation is used. Slope, manway, and lower or haulage entries are placed on the intake. Two air-courses and upper or breaking entries are placed on the return. A retreat system of mining is used exclusively. From the opening of its first coal mine, in the year 1868, until 1923, when the Joy loader was introduced into The Union Pacific Coal Company's operations, slopes, aircourses, and manways were driven by hand. Development work was conducted on the night shift or off shift, and the main hoist was used for haulage. The slope was driven down the pitch with crosscuts turned at intervals of 75 ft. and entries at 230 ft. Connections to the workings above were made by driving up the pitch 75 ft. Mule haulage was used to furnish cars to the hand loaders driving planes up the pitch. A sheave was placed at the upper end of the plane with a I¼-in. hemp rope dou- bling around it and having me end attached to the car and the other to the mule. The mulc, pulling downhill, raised to the working face a small wooden car of one-ton capacity. With the introduction of mechanical loading, mule haulage and small wooden cars disappeared and auxiliary hoists, electric locomotives, and steel cars with a capacity of 4 tons were substituted. Development work was done during two or three shifts of the 24-hr. period. Driving of haulage slopes down the pitch by hand continued. Crosscut intervals were changed to Ioo ft. and the crosscuts were driven with shaking conveyors. With the use of a 90° swivel, aircourses and manways were driven up the pitch. Entry intervals were changed from 230 ft. to 300 feet. Mobile loaders of the Joy type were first employed by this company in the year 1923 at Hanna, Wyo. In 1928, two 4-BU Joy loaders were transferred from Hanna to Winton No. I mine, where they were used in driving slopes and entries. At the time of transfer, the machines were about worn out and were not suited to the steep pitch, therefore frequent breakdowns occurred. However, experience justified the belief that the mobile loader was fitted for driving slopes in this field. During 1937 a unit was installed in Reliance No. 7 mine, and during 1939 one in Winton No. 7½ mine. With the introduction of this type of mobile loader, a new era of development began. Speed undreamed of in hand-loading days became a reality. The cost of development down the pitch has been reduced until it

Jan 1, 1942

By J. E. Wilson, F. P. Lebar

TYPICAL of southwestern Wyoming are coal structures that dip from 4° to 17°. Those at the Reliance and Winton mines of the Union Pacific Coal Co. average 91/2 and 15°, respectively, and dip almost directly to the west. By using a hoist for main haulage, a method of mining has been developed whereby four places are driven on the pitch of the seam. Slightly upgrade from the strike at intervals of 300 ft. a two-entry system is driven to the north and to the south. In both fields, which are nongassy, an exhaust system of ventilation is used. Slope, manway, and lower or haulage entries are placed on the intake. Two air-courses and upper or breaking entries are placed on the return. A retreat system of mining is used exclusively. From the opening of its first coal mine, in the year 1868, until 1923, when the Joy loader was introduced into The Union Pacific Coal Company's operations, slopes, aircourses, and manways were driven by hand. Development work was conducted on the night shift or off shift, and the main hoist was used for haulage. The slope was driven down the pitch with crosscuts turned at intervals of 75 ft. and entries at 230 ft. Connections to the workings above were made by driving up the pitch 75 ft. Mule haulage was used to furnish cars to the hand loaders driving planes up the pitch. A sheave was placed at the upper end of the plane with a I¼-in. hemp rope dou- bling around it and having me end attached to the car and the other to the mule. The mulc, pulling downhill, raised to the working face a small wooden car of one-ton capacity. With the introduction of mechanical loading, mule haulage and small wooden cars disappeared and auxiliary hoists, electric locomotives, and steel cars with a capacity of 4 tons were substituted. Development work was done during two or three shifts of the 24-hr. period. Driving of haulage slopes down the pitch by hand continued. Crosscut intervals were changed to Ioo ft. and the crosscuts were driven with shaking conveyors. With the use of a 90° swivel, aircourses and manways were driven up the pitch. Entry intervals were changed from 230 ft. to 300 feet. Mobile loaders of the Joy type were first employed by this company in the year 1923 at Hanna, Wyo. In 1928, two 4-BU Joy loaders were transferred from Hanna to Winton No. I mine, where they were used in driving slopes and entries. At the time of transfer, the machines were about worn out and were not suited to the steep pitch, therefore frequent breakdowns occurred. However, experience justified the belief that the mobile loader was fitted for driving slopes in this field. During 1937 a unit was installed in Reliance No. 7 mine, and during 1939 one in Winton No. 7½ mine. With the introduction of this type of mobile loader, a new era of development began. Speed undreamed of in hand-loading days became a reality. The cost of development down the pitch has been reduced until it

Jan 1, 1942

By R. C. Buehl, M. B. Royer

A three ton per day blast furnace using blast temperatures up to 2200°F was operated to recover manganese from open-hearth slag and manganiferous iron ore. The spiegel product containing 12 to 24 pct Mn was blown in a basic converter to high manganese oxide slag as described in the paper which follows this one. HE steel industry, which uses over 900,000 short tons of contained manganese yearly, depends on the maintenance of supplies of manganese from foreign sources such as India, Gold Coast, and Union of South Africa. Domestic ores furnish less than 10 pct of the yearly requirements of metallurgical ores and, unfortunately, the United States has no large, or even moderate, grade deposits that could supply a major portion of the requirements for many years. It may be necessary to obtain manganese from low grade materials, even though the cost is appreciably higher than when imported ores are used. An American Iron and Steel Institute questionnaire prepared in 1949 revealed the startling fact that open-hearth slags contained about as much manganese as is imported annually. The quantity of slag produced each year by integrated steel plants (not including cold-melt shops) and the manganese contained in the slag follows: Flush slag, 4,500,000 net tons a year containing 408,000 net tons Mn; tap slag, 7,230,000 net tons a year containing 364,000 net tons Mn; for a total of 772,000 net tons Mn. Some of this slag is returned to blast furnaces but about 75 pct would be available for the recovery of manganese. In several decades, when many of the present sources of high manganese ores have been depleted, open-hearth slag and manganiferous iron ore may become the major source of the manganese required for steel production. In 1948, manganese-ore imports from the U.S.S.R. were 427,000 net tons or 34 pct of the foreign ore. Imports from this source were only 81,000 tons in 1949. It became evident that adequate stockpiles of manganese could not be accumulated for many years. The Bureau of Mines initiated an extensive research program on methods for increasing domestic production of manganese and entered into a cooperative agreement with the American Iron and Steel Institute for recovering manganese from open-hearth slags whereby the Institute provided additional research funds and trained operating personnel. Description of Process and Equipment Numerous pyrometallurgical and hydrometallur-gical processes and combinations of the two can be applied to the recovery of manganese from open-hearth slag and manganiferous iron ore. The process being developed at the Pittsburgh Station of the Bureau of Mines consists of: 1—Reduction of open-hearth slag in a blast furnace to recover the iron and manganese as spiegel-eisen with 12 to 24 pct Mn. 2—Selective oxidation of the manganese from the blast-furnace metal in a basic-lined converter to produce a high manganese slag with up to 60 pct Mn content, which is a synthetic ore for the production of ferromanganese. This process has the advantage over other processes in that the equipment which would be used, such as blast furnaces and converters, has been highly

Jan 1, 1953

By Iam Pou Ng

Combustion aerosols consist mainly of elemental and organic carbon (EC and OC). Since EC strongly absorbs light and thus affects atmospheric visibility and radiation balance, there is great interest in its measurement. To this end, the National Institute for Occupational Safety and Health (NIOSH) published a standard method to determine the mass of EC and OC on filter samples. Another common method of measuring carbon in aerosols is the aethalometer, which uses light extinction to measure "black carbon" or BC, which is considered to approximate EC. A third method sometimes used for estimating carbon in submicron combustion aerosols, is to measure particle size distributions using a scanning mobility particle sizer (SMPS) and calculate mass using the assumptions that the particles are spherical, carbonaceous and of known density. With an eye toward evaluating the use of these methods for measuring carbon in freshly emitted diesel aerosols, the objective of this paper is to compare the results among these methods and to investigate the role of OC when measuring the mass concentration of elemental carbon (or black carbon) in aerosols emitted by a medium-duty Diesel engine. Results indicate that the aethalometer response correlates well with the data from filter samples (R2 = 0.99), with a very slight positive interference at high levels of OC.

Jan 1, 2008

By L. Karka

The gold processing plant location in the Chalkidiki coastal area has been studied as a land use conflict case study in the context of a EU research program. The sustainability assessment of the plant establishment is made on the basis of a group of sustainability principles and criteria adopted in the framework of the SPECTRA project. Since the gold processing project has not been implemented yet its sustainability assessment is made on the documents submitted by TVX Gold during the procedure for the siting consent and the granting of environmental conditions. The assessment, appearing on a table, reveals an important effort to achieve a high degree of protection during the operation and after completion of the activity. The specific nature of the development and the knowledge of the local opposition in favour of tourism development have obviously influenced the priorities set.

Jan 1, 2003

By A. D. Davis, C. J. Webb, F. W. Beaver

The proposed National Underground Science Laboratory will be housed in the former Homestake Gold Mine at Lead, South Dakota. Uses will include underground neutrino experiments that must be shielded by several thousand feet of rock, as well as ground-water research in fracture-flow environments, and investigation of the microbiology of extreme environments. The Homestake Mine has about 300 miles of underground workings. Seepage of ground water into the mine openings is approximately 500 gallons per minute. Average annual precipitation in the northern Black Hills is approximately 28 inches per year. The majority of this becomes surface-water runoff or evapotranspiration, with little ground-water recharge because of the low permeability of the Precambrian rocks in the area. Dewatering of the workings over the 125 years of operation of the mine has influenced the subsurface hydrology of the 8,000-footdeep mine.

Jan 1, 2003

By William H. Pomroy, Annie M. Carigiet

This U.S. Bureau of Mines report is an analysis of underground coal mine fire incidents occurring in the United States during the 15 years from 1978 through 1992. The fire data used in this analysis were obtained from Federal Mine Safety and Health Administration (MSHA) mine fire investigation reports. Fires were analyzed by year, state, coal bed thickness, mining method, evacuation measures taken, ignition source, burning substance, location, equipment involved, detection method, time of day, number of injuries and fatalities, and method of extinguishment. In all, 164 fires are reported, or an average of 10.8fires per year. The most common ignition source was electricity, the most common burning substance was coal, the most frequent fire location was the belt entry, belt conveyors were the most common equipment involved in fires, and water was the most common extinguishing agent.

Jan 1, 1995

By T. E. Sterner

A laboratory investigation was conducted to determine the applicability of the thermal oil-recovery method as a means of increasing ultimate oil recovery in the Appalachian region. The primary objective was to establish self-sustained combustion in consolidated and unconsolidated sand test assemblies saturated with various amounts of Pennsylvania Grade crude oil and synthetic brine. Tests using blocks of sandstone were unsuccessful because of sealing problems and fracturing of the rock due to thermal stresses. A combustion wave of about 700° F was propagated through the sand-oil-water packs in the linear tube tests. The high air flux used resulted in high oil consumption and rapid movement of the combustion wave through the tubes. Analytical tests on the sand pack showed that sufficient fuel was deposited during the linear tube experiments for a self-sustained combustion wave.

Jan 1, 1967

By Ann C. Kim

This Bureau of Mines report summarizes the methods and results of many of the laboratory studies on spontaneous heating of coal published in the last 50 years. It includes a brief description of experimental methods, indices of combustibility, and important contributing factors. Adiabatic calorimetry, isothermal calorimetry, [0], sorption systems, or temperature differential are the most frequently used experimental methods. Indices of combustibility include various heating rates, crossing point temperature, ignition temperature, and CO index. Factors that affect the spontaneous heating of coal include air flow rate, changes in moisture content, particle size, rank, temperature, pyrite content, geological factors, and mining practice. Experimental conditions and results from 20 papers are summarized in an appendix, and the bibliography contains 45 references.

Jan 1, 1977

By Volker Ruth

DURING an experimental investigation of the Kirken dall effect in the Ag-Au system, cracks along grain boundaries in connection with a shift of adjoining crys tallites are observed on the gold-rich side of the couple. Also on the gold-rich side the formation of a zone of small protrusions is found.' The growth law of the width of this zone indicates that the protrusion formation is a secondary effect of diffusion. The protrusions are not found within a distance of approximately 60 from a grain boundary. Unaffected regions along grain boundaries were also observed by Doherty and Davis during precipitation of vacancies in aluminum2 and by Wyon and Lacombe during precipitation of iron in aluminum.3 Thus we may suppose that we have an effect analogous to precipitation in which the crystal tends to maintain its equilibrium vacancy concentration by transporting excess atoms to the surface. At an early stage (i.e., before sintering has influenced the shape of the protrusions) the protrusions have similar shapes (three sided pyramids and roof shapes) and similar orientations within a single grain but vary from one grain to another. Further experiments were carried out on cylindrical Au-Ag single crystal couples. During the weld-

Jan 1, 1963

By P. R. Taylor

Titanium carbide and titanium diboride powders have been successfully synthesized by direct treatment of ilmenite concentrates in a non-transferred arc thermal plasma reactor. Methane gas was used as the reducing agent and boron oxide was used as the boron source in these processes. Free energy minimization plots were used to predict the behavior of each system under different molar ratios and operating conditions. Products were characterized by XRD, SEM and chemical analytical techniques. The average size of the ceramic product is in the submicron range. Metallic iron apparently is finely deposited on the surface of the titanium carbide or titanium diboride particles. Minor impurities such as silica, manganese and zircon were converted to the carbide form.

Jan 1, 1995

By Richard W. Hutchinson, Christopher Osterman

The Selebi-Phikwe deposits are hosted by amphibolite to granulite facies gneisses of the Limpopo belt. The sulfide orebodies are generally stratiform and conformable to the foliation of the wallrock gneiss. Sulfide remobilization has occurred during metamorphism and has produced discordant sulfide veins, called piercement structures, which project into the hanging wall and footwall gneisses. These piercement structures are compositionally similar to the stratiform sulfides, consisting mainly of pyrrhotite, pentlandite and chalcopyrite. However, texturally the piercement sulfides are coarse grained and inclusion-free, whereas the stratiform sulfides are fIne grained and packed with tectonically produced wallrock inclusions. The piercement structure sulfides and adjacent stratabound sulfides were sampled and analyzed for major base metals and PGE's for comparative purposes. Most of the piercement structures were enriched in Cu, Ag and Au, whereas they were generally depleted in Ni, Co, Fe and PGE's. Changing elemental associations were observed from the stratabound sulfides and along the length of the piercement structures. This and the degree of depletion or enrichment of various major and minor elements in the sulfide piercement structures may reflect the relative mobilities of metals under metamorphic conditions. The similarities between sulfIde piercement structures and the footwall Cu-PGE veins in some Sudbury deposits are reviewed.

Jan 1, 1994

By D. A. Farmen

INTRODUCTION In early 1978, engineering personnel at The Carter Mining Company began using photogrammetry coupled with a computer modeling technique to aid in mine planning efforts. The decision to develop this approach was based on the following needs: 1. A method to accurately capture excavated quantities for reporting purposes, 2. A method to produce accurate up-to-date maps for planning purposes, and 3. A computer-based mine-planning technique that would be compatible with techniques used in the past. The system developed utilizes a photogrammetric contractor to provide thousands of aerially-surveyed data points for input into the computer system. Each month the Rawhide and Caballo mines are flown by the photogrammetric contractor. The terrain of the active pit area is digitized and punched out on computer cards. This information is read into The Carter Mining Company's computer facilities, and an updated two-dimensional topographic grid model of the pit is generated. This surface is used to generate quantities moved during the month, to update isopachs, and to update quantities contained in fixed block progression polygons used for forecasting purposes. The system has greatly reduced the amount of manhours spent in field surveying and provides a useful tool for expeditiously evaluating many different forecast cases. It also provides the

Jan 1, 1983

In 1972 the Marra Mamba Iron Formation in the Lower Proterozoic Hamersley Iron Province of Western Australia was recognised as a stratigraphic horizon with significant potential for high grade iron ore reserves. Within the Newman area the Marra Mamba Iron Formation has been subdivided into four strati- graphic units: Lower BIF member, Middle BIF and shale member, Upper BIF member and Upper shale member - and a standard natural gamma log reference section compiled for the entire formation. The recognition of the Upper shale member as an additional unit contrasts to the previously proposed stratigraphy. Enrichment of the Marra Mamba Iron Formation to ore grade (0)8 percent calcined Fe) in the Newman area is restricted to the Upper BIF member and to a lesser extent to the Middle BIF and shale member. Typical ore from Orebody 29 is friable interbedded martite-ochreous goethite, signifi aptly different both physically and chemically from the Brockman Iron Formation ores of the Tom Price-Whaleback type. Large scale customer acceptance trials (in excess of 4 million tonnes) have shown that Marra Mamba ore crushed to fines and blended with Mt. Whaleback fines in a ratio of up to 15:85 forms an acceptable sinter feed.

Jan 1, 1981

By BO HYUN KIM, MARK K. LARSON

The floor-heave and no-floor-heave phenomena at a western U.S. coal mine could not be properly simulated in numerical models using conventional shear-dominant failure criteria. Although the previous numerical study using FLAC3D very reasonably demonstrated these phenomena, 3DEC modeling in conjunction with the discrete fracture network (DFN) technique was performed to better understand the true behavior of floor heave associated with underground mining in an anisotropic stress field. As a result, the latter models predicted floor heave that agreed with relative amounts of observed heave from each gateroad system, but the cause of heave was mainly related to the degree of anisotropy instead of the size of the pillar.

Sep 1, 2022

By E. Bakhtavar

Finding a ?practical spacing between the holes? for use of the expansive mortars is an important problem in dimension stone quarries. Objective has been to first introduce a relationship between this spacing and the dependent parameters in such a way that the required size and shape of the blocks is produced with the maximum efficiency and safety, minimum wastage, conservation of reserves and protection of environment. For this purpose, a dimensional analysis was used. On the basis of granite and marble rock types in Iran two separate relations are hence established to calculate the practical spacing between the holes.

Jan 1, 2011

By J. R. Welsh, D. J. Palmer, O. M. G. Newman

"The use of calcine for selective zinc precipitation requires specialist knowledge to achieve satisfactory flowsheet design. Calcine from the bed of a fluid roaster is preferred, and factors such as the size distribution of ground calcine, the stoichiometric ratio of the calcine precipitant to the initial dissolved zinc concentration and the moisture content of the resultant filter cake are parameters which require critical attention. Extensive testing in a fully-integrated electrolytic zinc plant pilot plant has demonstrated that properly designed selective zinc precipitation plants using calcine as the precipitant are reliable operating units.The advantages of using calcine instead of limestone for selective zinc precipitation include a decreased cost of reagents, as well as avoiding the formation of by-product gypsum.Process simulation modelling has demonstrated that the use of calcine in this context has widespread application in the design of zinc plants with superior impurity and water balance control characteristics. A particularly powerful approach involves closed circuit washing. In this mode, filtrate from the selective zinc precipitation step is used to wash a zinc plant residue such as jarosite, and the resulting filtrate is returned to the selective zinc precipitation section. IntroductionThe Selective Zinc Precipitation (SZP) Process, developed and patented by the Electrolytic Zinc Company of Australasia Limited (EZ) may be used to achieve simultaneously, water balance and impurity control in an electrolytic zinc plantO,2). Impurities which may be controlled by the SZP process include chlorine, magnesium, manganese, potassium and sodium.In the SZP process, basic zinc sulphate is precipitated from a zinc sulphate solution by either limestone, lime or a compound containing zinc oxide, usually calcined zinc sulphide concentrate (calcine) or alternatively zinc oxide fume .The solids containing basic zinc sulphate are separated, typically, by filtration and returned to the zinc plant circuit as a neutralizing agent. The zinc depleted solution can either be discarded, or used to wash residues, thereby achieving water balance and impurity control (Fig. I)."

Jan 1, 1988

By G du Toit, P L. Gillot, M Swanepoel

Randgold Resources’ Loulo-Gounkoto Complex is one of the largest gold mining operations in Mali, West Africa. The mine, which is situated on the western border with Senegal, treats more than 4 Mt/a of ore through a conventional three-stage crushing and ball milling circuit followed by a carbon-in-leach plant. Ore supply is achieved by a combination of open pit and underground mining, with the majority of the ore supply sourced from the Gara and Yalea underground mines situated approximately 2 km and 6 km respectively from the gold plant.In 2011, Randgold Resources commissioned Golder Associates to perform an evaluation study for providing structural backfill to both the Gara and Yalea underground mines using the current gold plant tailings. The test work performed as part of the evaluation study concluded the need for a tailings cycloning and dewatering facility capable of producing slurry at a solids concentration of 65 per cent with a particle size distribution that had minimum 25 per cent passing 20 µm and less than 5 per cent of -5 µm material. Tailings desliming was required to ensure a consistent feed quality to the paste preparation plants and to ensure that the system would be capable of handling variation in the feed composition from the gold plant.WorleyParsons, previously TWP Projects, was contracted by Randgold Resources to complete the engineering design for the slurry preparation plant, whilst Golder Associates was retained to complete the engineering design of the two paste preparation plants.This paper discusses the test work, design considerations and engineering design of the slurry preparation plant, termed the ‘intermediate plant’, as well as all ancillary facilities required for the delivery of the deslimed slurry to the paste preparation plants located at the two underground mines.CITATION:Swanepoel, M, du Toit, G and Gillot, P L, 2014. Case study – engineering design for a slurry preparation plant for a paste application in West Africa, in Proceedings 12th AusIMM Mill Operators’ Conference 2014 , pp 477–486 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Sep 1, 2014

By G. Baralis, P. Gondi, I. Tangerini, G. Scandola

The precipitation behavior of Zn-0.5 pct A1 alloy single crystals was studied by means of electrical resistivity measurements and by optical and electron microscopy. The single crystals for the resistivity measurements were prepared by an original method in - 100-p -thick sheets. The order of the precipitation kinetics ranged between 1 and 1.5. The dislocations play a relevant role in the first-order kinetics. Precipitation always occurs both on dispersed particles and on dislocations. Statistical examinations have shown that the first-order kinetics can have two different activation energies; i.e., the precipitation can have dz;fferent mechanisnrs which could not be identified, however, in the course of the research. During the tnetallographic exanzination of the precipitation structures a specific process of dislocation decoration was obsereed. The main purpose of this work was to study the contribution of dislocations to the precipitation. A number of authors have observed precipitation on dislocations and reference might be made to several monographs on the ubject.'' The possibility that dislocations also accelerate precipitation has been considered by Turn-bull3 and Fischer et al.4 The studies described in the present paper were carried out on zinc, chosen as a base metal owing to the ease with which dislocations can be introduced into it and because of the absence of excess vacancies after quenching in conditions where phenomena of accelerated precipitation still occur. Aluminum was preferred as alloying element because of the accelerated precipitation phenomena that resulted in a preliminary reearch. EXPERIMENTAL METHODS The observations refer to a Zn-0.5 pct A1 alloy. The zinc was 99.995 pct pure; a typical spectroscopical analysis is given in Table I. As a rule the alloy was subjected to homogenization, quenching, or slow cooling and annealing. Homogenization was carried out by heating at 390" to 410°C for 24 hr. From the homogenization temperature, some specimens were quenched and some slowly cooled at a rate of 2°C per sec. At this rate no precipitate was detectable under the optical microscope just after cooling. Quenching was carried out simply by dropping the specimens into water, aqueous ethylene glycol solution at -30" c, or liquid-nitrogen baths placed close to the homogenization oven. Vaseline oil baths were used with a thermal stabilization of 10-20 for both the aging treatments and the measurements; aging was generally carried out at 90" or 130°C. To avoid oxidation phenomena during heating, the vaseline oil baths had to be frequently renewed. The precipitation kinetics were studied by means of electrical resistivity measurements, using ans potentiometric method (reproducibility ± 5 x 10 5 v, that is 0.5 pct of the total voltage decreases on the specimens during precipitation). First, various types of specimens were tested, i.e., polycrystals, single crystals grown in capillary quartz tubes, and thin single-crystal sheets prepared by means of an original method requiring no container except for the natural oxide. Even if fully annealed, the polycrystals and the capillary grown single crystals showed resistivity in -creases, most probably due to dislocations introduced in the course of the measurements. Similar resistivity increases in pure zinc were noticed by another author. Only the single-crystal sheets showed no resistivity change; thus they were chosen for the subsequent tests. As already mentioned, these single crystals were obtained by using, as a container, the natural oxide on the zinc surface; the oxide strength is sufficient to maintain the original shape during melting with sheets up to 500 p thick. An initial zone melting and subsequent zone leveling, which led also to formation of the single crystals, were thus carried out on rolled sheets of the required thicknesses (- 100 p) and shape, lying on a flat silica surface. The resistivities were first evaluated by measurements at the liquid-nitrogen temperature. This method gave poor reproducibility, however, and this was attributed to the thermal cycles which had to be operated. To avoid cycles and handling, it was therefore decided to make measurements directly in the annealing oil baths; this required thermal stabilization at ilo-' "C. In this way only the resistance changes were measured. Specimens of pure zinc and of completely annealed alloy were always examined as controls together with those under consideration; only those measurement runs were taken into account where the reference samples showed no resistance increases. Again, the main inconvenience was due to oxidation and this was avoided by renewing the oil baths; even so data reproducibility was poor and the observations were therefore carried out on a large number (many hundreds) of specimens so as to provide indications of statistical value. For the transmission observations under the elec-

Jan 1, 1969