Search Documents

By Kamal Adham

Hydrochloric acid is used as lixiviant in such hydrometallurgy processes as synthetic rutile production and nickel extraction. The intermediary metal chloride is normally roasted to release gaseous HCl and a solid metal oxide. A large amount of fuel is required for this thermal regeneration, mainly to vaporize the water content of the feed solution. To conserve fuel, some energy recovery from the off-gas is currently achieved, but the fuel costs can further be reduced by process optimization and energy recovery from the gaseous, aqueous and solid products of the regenerator. Here, first the existing limitations to fuel efficiency in the industrial scale HCl regeneration roasters are described. Then, for the case of a dilute feed solution, options for pre-evaporation and fuel minimization are modeled and compared. Finally, energy recovery technologies including heat pumps, acid heat exchangers and solid waste heat boilers are described, and their potentials as the heat source for pre-evaporation of the feed are evaluated.

Jan 1, 2003

By R Fury, I Skepper, D White, G Miller

Although the Pressure Acid Leaching (PAL) of nickel laterites has been conducted at Moa Bay, Cuba, since the early 1960s, the commissioning delays generally encountered by the æsecond generationÆ of PAL lateritic nickel producers in the late 1990s have demonstrated the potential complexity of the PAL process and the importance of technical risk management in maximising the realised project value. This paper describes some of the strategies used by the Ravensthorpe Nickel Project (RNP) to manage the technical aspects of the Ravensthorpe project risk. Central to these strategies is the use of Front End Loading (FEL) to deal with issues early in the development phase, when changes to the project structure can be made most effectively and cheaply. Such an approach requires a management philosophy that recognises risk as a potential cost, which accepts responsibility for dealing with risk, and which is prepared to provide adequate resources for risk management.

Jan 1, 2004

By Eustáquio Vieira Júniorr, Dalton Martins Neto, Filipe da Costa Oiveira

O Alto-Forno 2 da Ternium Brasil, no Rio de Janeiro, iniciou sua primeira campanha em 16 de dezembro de 2010. No decorrer de sua campanha, verificaram-se problemas de deslocamento de staves de ferro fundido e deformação dos staves de cobre chamado “efeito banana”, causando a perda da capacidade de refrigeração destes componentes do sistema de arrefecimento. Após a análise dos eventos foram executadas diversas ações para recuperação e preservação do Alto-Forno 2, sendo estendidas também ao Alto-Forno 1. Dentre as ações de preservação para o Alto-Forno 2 foi estabelecido que deveriam ser substituídos os staves danificados e alguns setores da carcaça que apresentavam trincas e deformações, e consequentemente a perda de suas propriedades mecânicas, visando eliminar as interrupções na operação do Alto-Forno 2 para reparos localizados e redução das instabilidades operacionais causadas pela não uniformidade das superfícies dos staves. O trabalho apresenta o detalhamento da técnica utilizada para substituição dos staves, a seleção dos materiais assim como os preparativos operacionais que garantiram o bom desempenho do Alto-Forno 2 nos momentos que antecederam a parada e após seu retorno à operação, mostrando a viabilidade técnica e econômica da atividade.

Oct 1, 2019

By Greg Bold, Mahmood Khwaja, Yuannian (Jerry) Wan, Michael S. Schultz, William Simcoe

Beaver Creek Clean River Project will satisfy the consent decree requirements by capturing and treating combined sewage overflows. The project consists of, approximately, 2,700 feet of 30-inch trenchless pipe installation, a new screening/disinfecting facility, an expansion of an existing diversion structure, and a 72-inch internal diameter, 530-foot long mined tunnel. The tunnel portions are being progressed as early release packages. This paper presents the geotechnical exploration program and the subsurface conditions encountered; interpretation of the geotechnical conditions; and, approach to developing stand-alone packages for the tunnels to mitigate construction and schedule risks and continue to advance the project.

Jun 13, 2021

By Myron W. Mellor

Much has been published concerning the subject of coal preparation as related to electric power generation however it is always a most vital topic for both utilities and coal producers, It also constitutes a field of study that is never finished since new concepts and changing demands continually require altered perspectives. One graphic illustration that has been used to emphasize the rapidity with which times are changing is the fact that during World War I, a station that consumed 1000 tons per day was looked upon as a large central station, while today some single generators require 1500 tons during the same period, For further emphasis, at that time a 20,000 horsepower turbo-generator was a mighty large machine; today, a unit of this size is planned for driving the boiler water feed pump required for a single large main unit. During the past ten years alone, electric utilities have more than doubled their percentage of coal consumed as compared to the total market. They now account for approximately 40% of the United States consumption and one-third of all production including export, Conversely, approximately 70% of all U. S. steam electric generation is by coal and this percentage is expected to increase. It is further predicted that utility consumption will increase from the current 160,000,000 tons per year to between 400 and 500 million tons in 1975 which is approximately equal to todays total production

Jan 1, 1959

By G. M. Willis, F. L. Hennessy

The oxygen pressure in equilibrium with silver and Ag2O-B2O3 melts has been measured between 800' and 900°C, to obtain the thermodynamic properties of the liquid. The compound Ag20. 4B20:1 appears to exist in the liquid, which shows marked heat content and entropy effects. A KNOWLEDGE of the thermodynamic properties of binary liquid silicates, borates, and phosphates would be of considerable assistance in the interpretation of the behavior of multi-component metallurgical slags. However, the literature contains comparatively few studies of the thermodynamics of binary slags. The system Ag20-B,O, attracted our attention as it was known to give a single liquid phase,',' in which high contents of silver could be obtained (up to 61 pct Ag according to Foex2). Further, it would be expected that the partial pressure of oxygen over melts in equilibrium with metallic silver could be used to determine the activity of Ag2O in the Ag,O-B,O, system. In many respects, it may be expected that the reaction of a basic oxide with boric oxide would be analogous to its reaction with silica. Liquid immiscibility frequently occurs in both borate and silicate systems. With B2O3 and SiO reaction with a basic oxide presumably involves a breakdown of the three-dimensional network of the acid oxide by reaction with oxygen atoms common to more than one silicon or boron atom. Ag2O-B2O3 was therefore investigated as a model of a slag system in the hope that its thermodynamic properties would assist in understanding those of other systems. Several methods for determining the activity of a component in a slag have been described in the literature. Chang and Derge" used high temperature electromotive force measurements to obtain the activity of SiO2 in CaO-SiO2 and Ca0-Al203-Si02 slags, but the cell reaction in their work is not clear. low has used rate of volatilization and vapor pressure measurements combined with phase diagrams to obtain activities in the systems KO-SiO,, Na,O-SiO, and Li,O-SiO," and PbO-SiO26 Taylor and Chipman7 extrapolated their results for the distribution of FeO between liquid iron and CaO (+Mg0)-FeO-SiOl slags to obtain the activity of FeO in the binary FeO-SiO2 system. In principle, one of the most direct methods for obtaining the activity of a metallic oxide in a phase is by comparison of the equilibrium oxygen pressure for the system metal-pure oxide with that of metal oxide-containing phase. Schenck and othersa have studied the stabilization of Ag2O on combination with other oxides (MO,) in the solid state by measurements of the oxygen pressure in systems of the type Ag-Ag,O-xM0,-MOy-0, (gas). Schuhmann and Ensio" have determined the activity of FeO in iron silicate slags in equilibrium with solid iron, using CO/CO2 mixtures to establish known partial pressure of oxygen. Although the method gives the activity of FeO without ambiguity, the slag is not a binary system, and interpretation of the results in terms of the hypothetical binary system FeO-SiO, is not possible. If a metal is solid at temperatures at which the properties of the slag containing its oxide are to be studied, this method has the considerable experimental advantage that the metal can be used as the container for the slag, and contamination by contact with refractories is avoided. In this work, crucibles for Ag2-B,O, melts were made from silver, and the liquid brought to equilibrium with definite pressures of oxygen gas. The oxygen pressure PO, thus fixes the activity of Ag20 in the liquid silver borate. For the reaction at a given temperature. is substantially constant, is directly proportional to the square root of the equilibrium oxygen pressure. Varying the oxygen pressure changed the silver oxide content of the liquid and it was possible to obtain the activity of Ag2O over a range of composition. Experimental Procedure In principle, the method consisted of bringing melts in silver crucibles or boats to equilibrium at a fixed temperature under a definite pressure of oxygen and analyzing the glass after solidification. Materials: B2O3 glass was prepared from A.R. quality boric acid by fusion in platinum. The silver

Jan 1, 1954

By Harold B. Janzen, M. A. Nobles

Campbell and Martin1 described a new exploratory logging tool which was developed as the result of a new concept of the phenomenon that takes place when a porous formation containing mobile hydrocarbons and irreducible interstitial water is invaded by mud filtrate. They postulate that invasion will create a bank of interstitial water between the flushed zone and the undisturbed formation. This postulate was confirmed by Wyllie.' Thus, if R,, is greater than R, and mobile hydrocarbons are present, the resistivity profile with increasing radii from the borehole is high:low:high, as shown in Fig. 1. If mobile hydrocarbons are absent, the bank of interstitial water is indistinguishable from the undisturbed formation and the resistivity profile, when R is greater than R,, is high:low, as shown in Fig. 2. The zone containing the bank of interstitial water and residual oil was named the "low zone". Campbell and Martin conducted extensive electrolytic wedge and resistivity analog model studies to select a logging system that would reflect the presence or absence of the low zone. The system they selected was that of a family of lateral curves. The model studies indicated that the presence of a low zone could be detected in approximately 60 to 70 per cent of the producing sand reservoirs with a family of lateral curves provided that the sonde effectively occupies 90 per cent of the diameter of the hole. These studies were conducted with D, = 5d. The presence or absence of the low zone is best determined by a plot of the apparent resistivity vs spacing as shown in Figs. 3 and 4. A dip or inflection in the profile that repeats at successive depth intervals is considered diagnostic. To reduce the shunting effect of the hole and mud, a sonde of insulating material that is surrounded by a series of flexible rubber bumpers was designed. The bumper efficiency is considered to be the ratio of the bumper diameter to the hole diameter. Field tests conducted by Campbell and Martin on 10 wells with a tool that provided for station readings indicated that dips or inflections could be detected in 19 out of 25 known producing zones. INSTRUMENT DEVELOPMENT Halliburton developed a logging system to simultaneously and continuously record eight lateral curves. The instrumentation is described in the literature.' The original logs made

By M. L. Schmulian

"The Windarra nickel deposits display many of the characteristics that typify Archaean volcanic peridotite-associated nickel sulphide ores of Western Australia. The Fe-Ni-Cu sulphide mineralization, which comprises dominantly disseminated sulphides, occurs at the base of a differentiated ultramafic volcanic pile grading upwards from massive meta-peridotitic flows to thin, locally spinifex-textured meta-picritic units. The entire mafic-ultramafic belt has been subjected to mid-amphibolite- facies metamorphism. The ore-bearing ultramafic is immediately underlain by dominantly sulphide-facies banded iron formation (BIF), which commonly contains nickel sulphides adjacent to its contact with mineralized ultramafic. BIF-hosted ores are formed both by physical remobilization of ultramafic-hosted sulphides and by migration of Ni and Cu into pre-existing iron sulphides.At Mt. Windarra the mineralization comprises eight steeply dipping, steeply plunging elongate oreshoots, which display a marked parallelism with major and minor fold structures in the underlying BIF. Seven of the shoots occur at or close to the base of the ultramafic pile, and are hosted by at least three overlapping flows. The zone of overlap occurs at the northern end of each flow, where picritic ultramafic, representing a dominantly liquid portion of the flow, occupies the basal contact. A gross south- north ultramafic flow direction is inferred. The eighth shoot occurs in a stratigraphically higher position within the ultramafic sequence.At South Windarra at least two overlapping mineralized flows occupy the basal contact, the ore zone having a strike extent three to four times its downdip extent. There is no obvious structural control to the mineralization."

Jan 1, 1984

By J. Petersen, H. Naderi, M. H. Nikzad, M. Karimi

In this research, the thermodynamic study of sodium persulfate (Na2S2O8) solution in the presence and absence of H2SO4 and Fe3(SO4)3 was done. Eh-pH and equilibrium distribution diagrams were constructed using Outotec HSC Chemistry Software and the main stable ionic species were determined. Also, the mean activity coefficient and Pitzer model coefficients were evaluated. Effects of system composition, sodium persulfate concentration and temperature were investigated. According to the results, HS2O7 -, HS2O8 -, S5O3 2-, S4O3 2-, S3O3 2-, HS- and NaSO4 - are the main stable species in these three systems. Increasing of sodium persulfate concentration resulted in disappearing of SO4 2- and the appearance of NaSO4 -. The main effect of increasing the temperature from 25 to 75oC, is changing the stability regions of HS2O7 -, NaSO4 -, SO4 2- and S2-. From equilibrium studies, it was concluded that at 25 and 50oC, increasing the persulfate concentration results in a 55-60% decrease for HS2O7 - and an 20- 30% increase for HS2O8 -. At 75oC, HS2O8 - becomes the main species and its percentage decreases with increasing the persulfate concentration. Keywords: Thermodynamic, sodium persulfate, activity coefficient

Jan 1, 2020

By V. Prasad, A. Afacan, K. Popli, S. Dubljevic

Froth flotation is one of the most common and widely used separation processes in the mineral processing industry; however, its complexity means that complete understanding of the process has not yet been achieved. A dynamic fundamental model is needed to enhance the understanding of the process and to improve process control. It is challenging to capture all the phenomena involved; hence, we propose a multiscale modeling approach with a framework ranging from macroscopic (equipment scale) to microscopic (attachment, detachment) models along with distribution models for ore particle sizes. Real-time froth properties are obtained using a vision-based sensing system. These measurements can be used for developing a soft sensor for grade using statistical methods such as PCR (principal component regression) and PLS (partial least squares) regression. The fundamental model is updated in real-time using extended Kalman filtering. Attachment dynamics are studied for different particle size distributions. The modeling and soft sensing is tested on batch flotation cell for the pure mineral galena with different particle size distributions using Xanthate and MIBC as collector and frother, respectively. The model, online measurements and soft sensor are useful in developing monitoring methods for froth flotation.

Jan 1, 2015

By W. Murray Small

Nickel plays an important role in determining the properties of many stainless steels and superalloys. Cobalt also contributes significantly to the performance of certain grades of superalloys. A major technical aspect, in which both of these metallic elements are involved, concerns the solubility of nitrogen in these classes of alloys. Beyond certain content limits, dissolved nitrogen may contribute to the deleterious mechanical behavior by these alloys. It is therefore essential to control the level of this element during alloy processing. In this paper, results from several experimental studies have been assembled and are analyzed to describe phenomena related to the individual effects of nickel and cobalt on the solution of nitrogen in several groups of alloys. Both solid and liquid alloy systems are considered. This information may be used as a guide to limit or control the presence of this interstitial element in alloys.

Jan 1, 1993

By Hargraves A. J

At 4 MPa gas pres ure and 30°C the sorptive capacity of 10 selected Australian dried coal ranges from 17 to 23 m3/tonne of CH4 and 27 to 36 m3/tonne of CO2. Values for moist coals are about 25 per cent less. At 20°C, sorptive capacities are about 18 per cent greater. No clear relationship between coal rank and sorptive capacity was established.The permeability of coal to gas is dramatically reduced by progressive hydrostatic confinement. No single 'permeability' for a coal can be established because of relative affinities of coals and the gases (Ar, CH4 and CO2) used in experiments. Bedding plane permeability is significantly greater than permeability normal to bedding. Dependent on gas/coal combinations, permeabilities without confinement ranged from 150 to 0.05 millidarcies, and with 8 MPa hydrostatic confinement from 1.0 to 0.001 md. Generally, permeability is increased by reduction in temperature, and reduced by increase in moisture as one changes from Ar through CH4 to CO2. In retrospect, it is preferable to ubject permeability sample to 8 MPa hydrostatic stress only once, because changes occur in the samples and it is difficult to use other gases successively.The initial rate of desorption, DP, does not appear to be a reliable index of proneness to instantaneou outbursts for Australian coals.The methods used for determining quantitative gas-coal properties appear suitable and reliable for testing other coals.

Jan 1, 1985

The National Mining Hall of Fame and Museum (NMHFM) in Leadville, CO will induct the class of 2011 on Sept. 10, 2011. Representing the coal, metallurgical/processing, research and development, marble and lead industries, this year?s inductees cover a diverse crosssection of the mining industry. William Francis Diamond, Wayne Hazen, Redfield Proctor and Jeffrey Zelms will join 210 other mining industry pioneers when they are formally inducted into the National Mining Hall of Fame at the 24th Annual Induction Banquet and Ceremony. The members of this year?s class were selected for being visionaries, leaders and ambassadors both within their own sectors and across the industry at large. Diamond had an illustrious engineering and managerial career that spanned four decades with Island Creek Coal Co. During that time, he was responsible for the engineering and construction of the deepest coal mines producing in North America at the time.

Jan 1, 2011

By Kazutoshi Haga, Atsushi Shibayama, Altansukh Batnasan

The objectives of this study were to propose a viable alternative method for recovery of precious metals such as gold (Au), silver (Ag) and palladium (Pd) from waste printed circuit boards (WPCBs) and to regenerate the spent lixiviant solution for reuse. The proposed method generally consists of several steps as follows: 1). iodine-iodide leaching for metals extraction; 2). separation and recovery of precious metals and metal impurities from a pregnant leach solution; 3). regeneration of the spent iodine-iodide solution/lixiviant. In this method, more than 99% of Au leaching was achieved in the iodine-iodide solution from the solid residue of WPCBs that was obtained via sequential processes including incineration at 800 ?C and high pressure oxidative leaching with a diluted sulfuric acid at 120 ?C, while the leaching of Ag and Pd was less than 1%, respectively. Besides Ca, Cu, Ni, Co and Zn as main metal impurities, leaching efficiency of other metals did not exceed 1%. The precious metals and base metals as metal impurities present in the pregnant leach solution were separated and recovered by precipitation using L-AA and NaOH solutions. About 99.8% Au, 81.7% Ag and 72.8% Pd were recovered from the pregnant solution at pH of 2 with the addition of 0.1 M L-AA as precipitating agent. The remained small amounts of precious metals and metal impurities were precipitated at pH 13 using 1 M NaOH. The spent lixiviant after sequential precipitation was regenerated in the presence of hydrogen peroxide, hydrochloric acid and potassium iodide. It was revealed that over 90% of gold could be extracted from the residue of WPCBs with the regenerated lixiviant solution.

Jan 1, 2018

By Kevin Davey, Liza Forbes, Leanne Smith

Given the global scarcity and value of potable water, interest in the use of water of lower quality in mineral processing has grown significantly in recent years. Previous laboratory batch flotation tests conducted at CSIRO have shown that chalcopyrite floats strongly without collector in distilled water and that the collectorless flotability of chalcopyrite is unaffected by the use of brackish water, sea water or hypersaline water. In contrast, bornite is moderately flotable without collector in distilled water but all three lower-quality waters have a detrimental effect on the recovery of bornite. The depressant effect is so strong that the little recovery achieved in these waters was only slightly above what might have been expected from entrainment alone. This work has now been extended to another important copper sulfide mineral, chalcocite. In contrast to chalcopyrite and bornite, chalcocite does not exhibit collectorless flotability so the chalcocite tests in this study were performed in the presence of a standard collector (potassium ethyl xanthate). The results reveal that chalcocite is flotable with xanthate in distilled water but the lower-quality waters have a detrimental effect on the recovery of chalcocite. This effect is partly reversed by increase collector additions. Further tests were completed in order to investigate the effect of the different ions present in the saline waters on chalcocite flotation. Possible reasons for the observed differences are discussed in terms of the pulp chemistry of the system.

Jan 1, 2014

By Leslie F. Sawatsky

Each potential oil sands developer deals with the question of optional sources of raw water to supply large water demands that range from 50 to 80 million cubic metres per year for each of six existing and planned developments. The Athabasca River currently supplies nearly all of the water to the existing mines via conventional bank intakes, which has resulted in some concern over the effects of reduced river flows. This paper describes the various water supply options, and the likely scenario for future oil sands water supply projects. Various water supply options have been suggested including Athabasca River water via infiltration galleries, groundwater, combined Athabasca River water and alluvial groundwater using wells (i.e. bank filtration systems), diversion of tributary rivers, utilization of large lakes in the region and pumping from other large rivers in the region. Investigations show that the size of river catchment needed to support raw water usage by a typical oil sands mines exceeds 5,000 km2 eliminating all tributary rivers that are located in the oil sands region except those rivers with large drainage areas like Firebag and MacKay Rivers. Lakes cannot be used as a source of supply due to large water deficits for smaller lakes and the large cost of sourcing water from a lake as large as Lake Athabasca. A groundwater source alone would not likely meet the large water demands. River intakes on the Athabasca River will likely continue to be the most practical water supply option for oil sands mines north of Fort McMurray, although various types of Athabasca River intakes are possible. Existing intake systems include screened riverbank intakes, forebay intakes, and river bottom intakes. Infiltration galleries are not feasible for most sites, though some bank-filtration-type systems using high capacity wells may be an option if there is sufficient thickness of high-permeability alluvium at a suitable location in the Athabasca River valley.

May 1, 2004

By S. Klein, D. Crouthamel, D. W. Farmer, S. H. Phillips

Groundwater inflows during construction pose one of the greatest risks to the successful completion of tunnel projects. Inflows can result in safety concerns, difficulty in mining and ground support, impact sensitive environmental habitats, create surface settlement and increase costs. Adequately planned pre-excavation grouting programs benefit both the Owner and Contractor in reducing risks and controlling project costs and potential schedule delays. This paper outlines strategic guidelines for assessment of site conditions for pre-excavation grouting hard rock tunnels. It also describes the design of pre-excavation grouting programs with respect to project requirements.

Jan 1, 2005

By J. O. G. Sanderson

THE Brazeau river is a relatively short foothills stream in western Alberta and its drainage area is limited to approximately 2,400 square miles. It rises near the head of the North Saskatchewan river, about two-thirds of the way from Banff to Jasper, and is confluent with the North Saskatchewan at a point about 40 miles north of Rocky Mountain House. It is not the purpose of this paper to describe the geology of all of this area. Only the central portion, which lies east of the outer limestone ranges and takes in the outer folds of the foothills belt, will be dealt with. This area is shown on Figure 1. A small portion of the area described lies in the drainage basin of Pembina river, which flows into Athabaska river. The area to be discussed may conveniently be termed the 'Brazeau area', since Brazeau is the name of the river basin referred to above, of an out-lying limestone range, and of the only large settlement or community in the region, the mining town Brazeau. One of the first Factors of the fur trading post of Rocky Mountain House in the early years of the nineteenth century was Louis Brazeau. Coal mining during the past 25 years, and more recently exploratory drilling for oil, have brought the district into some prominence. The Brazeau area was visited by D. B. Dowling for the Geological Survey of Canada in 1906 and 1907 (1). His traverses and reports dealt mainly with the Kootenay coal deposits. It is doubtful if he traversed the outer foothills area with which the present paper deals. His reports on rich coal deposits in the Bighorn Basin area attracted commercial interests, and in 1908 large tracts were leased as coal lands. James McEvoy mapped and studied the coal seams in that year, and G. S. Malloch, of the Geological Survey of Canada, made a complete survey of the whole of the Bighorn basin. His report (2), published by the Survey in 1911, describes the stratigraphical geology and names the formations. Further references to the geology of the district, mainly in relation to coal, are made by D. B. Dowling (3) and by J. S. Stewart ( 4). In the period between 1913 and 1920, the area was traversed by private interests in search of likely oil structures. A well was started in 1914 along the Saskatchewan river about 19 miles west of Rocky Mountain House, and drilling was undertaken by Imperial Oil, Limited, in 1921 at Coalspur.

Jan 1, 1939

By H Utama, R Heryadi

The demand for environmentally friendly commercial explosives has increased globally due to concerns regarding environmentally friendly mining activities. Ammonium nitrate fuel oil (ANFO) and bulk emulsion explosives (BEE) are two kinds of civil explosives primarily used in coal and mineral mining in Indonesia. Indonesia is one of the leading countries in coal and mineral mining production and export, with abundant resources; therefore, the consumption of civil explosives such as ANFO and BEE is enormous. The selection and evaluation of commercial explosives are mostly done on the commercial and technical side, and no assessment is made based on environmental aspects. This preliminary study evaluates the economic value and environmental burden of greenhouse gas emissions produced by ANFO and BEE and determines which type of explosives is more environmentally friendly. The combination of environmental and economic indicators, eco-efficiency (E/E), was selected to investigate BEE’s economic and environmental performance compared to ANFO. The life cycle of greenhouse gas emissions of BEE and AN was determined using previously available studies and simple calculations. The cost of the product or explosives was used to represent the economic value. The E/E results showed that environmental and economic sustainability could be enhanced using BEE.

Sep 1, 2024

By Nicholas J. Grant, Yoichi Ishida, Arthur W. Mullendore

An inert particle -marker technique was developed to provide a direct measurement of grain boundary sliding during creep in tile interior of aluminum specimens. Groin boundary sliding in the interior as measured by this technique was found to be nearly the same or slightly lower than that measured on the surface. These data disagree with those obtained by the grain-counting technique developed by W. A. Rachinger. In tests where both techniques were used, the grain-counting technique gave large and variable values of grain boundary sliding. It is shown that the grain-counting technique gines erroneozcs results because of a preferred direction of grain growth during creep. A question which has long plagued those who study grain boundary creep is whether or not surface measurements yield a true representation of the deformation in the interior of a specimen. The first attempt to measure grain boundary sliding in the interior of a creep specimen was made by Rachinger.1 His technique is based on the measurement of average grain diameters, both parallel and perpendicular to the tension axis, followed by a calculation of the grain elongation from these measurements. The difference between total elongation, Et, and the calculated grain elongation, Eg, is considered to be the result of grain boundary sliding, Egb. Surprisingly large values of Egb/ Et (90 pct) came out of creep tests of pure aluminum at temperatures above 250°C (480°F), utilizing the Rachinger technique. This value is very much larger than the values of 8 to 15 pct measured by numerous investigators on the surface of a specimen. Values obtained on the surface by Rachinger, however, were consistent with those measured by the displacement of reference scratches. Chaudhuri and Grant2 repeated the Rachinger method for A1-10 pct Zn, and found the same large values of Egb/Et inside the specimen. However, from purely geometrical considerations, grain boundaries cannot slide without grain deformation; therefore, they questioned the validity of Rachinger's grain-counting method. Several authors2,3 have suggested that grain boundary migration during high-temperature deforma- tion may tend to restore the equiaxed grain shape in order to minimize interfacial energy. Rachinger4 tested this hypothesis and found that it did not hold. Grains elongated by rapid extension retained their elongated shape during a subsequent slow creep test. It appears that some other factor was responsible for the abnormally high values of .Egb/El. McLean and Gifkins5 made a survey of the effect of grain size on the ratio Egb/ Et, and proposed that the high values were the consequence of a small grain size. They failed to explain the low value of Egb/Et which Rachinger observed on the surface of the small grain size specimens, and suggested that the surface effect on the value of Egb/Et does not always occur. Many of the disagreements arising from Rachinger' s work stem from the fact that there was only one method of estimating grain boundary sliding in the interior of a specimen, and that method was of an indirect nature. If a marker line of some sort could be introduced inside of the specimen, one could make measurements just as clearly as on the surface. In the present investigation, the technique utilizes a layer of finely dispersed oxide particles inside the specimen introduced by hot press-bonding of two pieces of aluminum. Rachinger attempted a similar technique but with the oxide distribution he obtained there was so much interference with grain boundary motion that quantitative measurements were not attempted. MATERIALS AND EXPERIMENTAL PROCEDURE A) Materials Preparation. Two pure aluminum rods (impurity content in percent: Si, 0.002; Cu, 0.004; Fe, 0.002; Mg, 0.000: Zn, 0.000; V. 0.001) 1 in. diameter by 2 in. high were jacketed end to end in a 4-in.-diam cylinder of commercial-purity aluminum, 4 in, high, which had a l-in.-diam hole. The l-in.-diam mating surfaces of the two pure aluminum rods had been electropolished initially. This interface provided the oxide-film internal -marker plane after the hot press-bonding process, see Fig. 2. The composite was annealed for 1 hr at 900 F and hot upset more than 50 pct reduction in height in one step. The resulting slab was then rolled to 1/2 in. thickness; the pure aluminum test material was cut out and annealed at 900°F for 1 hr and cold cross-rolled to 1/8 in. thickness. The sheet was machined into specimens with a 1/8-in.-square cross section and a 1/2-in. gage length. The following heat treatment was given the specimens: Specimen 5A series: annealed at 1000°F for 5 min for grain-size control and then cooled to 700°F and held for 15 hr for stabilization.

Jan 1, 1965