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By Sunil S. Basarkar, Vinothkumar S

Ground Improvement Techniques serves to improve various engineering properties for supporting various foundations. These may be undertaken either by conventional or advanced methods. The Controlled Modulus Column (CMC), also known as Rigid Inclusion is a soil improvement technique to reduce the total and differential settlement by using semi-rigid soil reinforcement columns. The CMC technique can be executed by displacement or non-displacement methods. It does not aim to bypass the compressive layer or to install a pile that will directly support the entire load from the structure. Principle of the technique is to introduce a load transfer platform between the head of the column and structure and transform a uniform load into soil. Initially, the structural load transmitted into the soil generate the settlement greater than CMC piles. When the settlement between the soil and column became equal at neutral point, maximum structural load shall be balanced by the positive friction and tip resistance to stabilize the foundation without exceeding the allowable settlement limit. This paper describes the behaviour of soil reinforcement with CMC column and their installation process with reference to a project at the Dry Bulk Terminal Port, San Pedro- Abidjan (Western Africa). Methodology of CMC, requirements of Ground Improvement, arrangements and outcome of this method are presented in this paper.

Sep 1, 2022

By K. Law

"The Hatch Product Transport (HPT) system is a highly flexible and configurable route selection and sequencing system for controlling large bulk material handling facilities. The system has a generic control algorithm that can be configured to suit any material handling facility. It can also be easily reconfigured to cater to plant expansion or modifications without incurring significant disruption to the existing production, costs in testing, and re-commissioning, thus achieving cost savings throughout a facility’s lifecycle.This new material handling control system has been installed at BHP Billiton’s Port Hedland iron ore terminal to facilitate its expansion to beyond 100 Mt output capacity."

Jan 1, 2006

By Kyle A. Perry, Ethan A. Steward

The mining of underground coal presents several hazards for miners, including the risk of an explosion fueled by methane gas and coal dust. Methane gas, produced during coal formation, can continuously leak into old workings and build up through its lower explosive limit. Underground coal mines are required to maintain safe conditions, either by ventilating old workings or sealing them off using approved methods. Seals must be designed to withstand instantaneous pressures for a minimum of four seconds. A design strength of at least 50 pounds per square inch (psi) is required for atmospheres monitored and maintained inert, 120 psi for non-inert or not monitored, and greater than 120 psi for special cases. Due to the high cost and testing environment availability, most mine seals are designed through calculations and computer modeling and not subjected to full-scale testing in a representative environment. High pressure is not the only threat that mine seals may be exposed to. During an underground explosion, pressure waves and gas expansion may propel common mine items and objects to a high velocity, generating enough energy to damage mine seals and reduce their strength. Damaged mine seals may fail to contain their rated pressure, allow high pressure gas and fumes to vent through the seal during an explosion, or allow gasses to leak through the seal later after an explosion has occurred. This paper examines the effects of high velocity impacts of common mine materials and items on a reinforced mine seal rated to 120 psi.

Jun 2, 2023

By G Sartor, A Rich, D Grimsey, R Forzatti, M White

An in-depth process model was developed for the pyrometallurgical, off-gas systems and water balance of the Kalgoorlie Nickel Smelter. This model was used to assess plant capacity with changing concentrate grades, increased throughput and tighter environmental emissions under a range of potential future operating conditions. Comparison of modelled results allowed for flow sheet optimisation across a range of metrics including sustainability, processing capacity and costs. Process modelling software, METSIM® (ver 2020.06 by METSIM International), was used to simulate the flash furnace, integrated electric slag cleaning furnace, Pierce-Smith converters, matte granulation, waste heat boiler, hot gas handling equipment, wet gas cleaning plant and acid plant. The METSIM® model was divided into three separate, yet interconnected models: metals, off-gas and water balancing. This allowed for improved modelling efficiency and traceability while minimising manual error. The METSIM® model was supported by inputs from other specialised software. Chemical thermodynamics software, FactSage™ (ver 8.2 by GTT Technologies), was used to establish relationships for the flash furnace fluxing strategy and determine the operating temperature. Arena® (ver 16.0 by Rockwell Automation), a discrete event modelling software, was used to simulate material movements within the aisle as well as Pierce-Smith converter operation, allowing for integration with upstream and downstream systems. A dynamic data exchange (DDE) was used to connect the results of each software package, interfacing through Excel® (version 4203 by Microsoft). The integration between models provided a streamlined approach to test capacity, bottlenecks, water consumption and emissions under a range of operating conditions, enabling a more robust process. Further downstream modelling techniques were used to assess mechanical equipment. METSIM® outputs provided key parameters for combustion assessments using computational fluid dynamics and finite element analysis for the furnace mechanical design.

Aug 21, 2024

By Gerald Verbeek, Erick Baziw

Downhole Seismic Testing (DST) is an extensively utilized geotechnical tool for site characterization. DST provides low strain (<10-5) in-situ interval shear and compression wave velocity estimates. These velocities are determined by obtaining relative arrival times of source waves as they travel through the stratigraphy and are recorded by one or more vertically offset seismic sensors. The DST arrival times have associated measurements errors and resolution limitations, which become more pronounced as the depth interval of analysis is reduced. Baziw Consulting Engineers (BCE) has developed a new DST analysis technique, the so-called DSTPolyKF algorithm, whereby the arrival times of DST data set are used to define a high order polynomial. The main advantages of this new technique are four-fold: 1) the ability to utilize all arrival time estimates irrespective of measurement errors. 2) the ability to analyze the data with user specified and even small (≤ 0.5m) depth intervals. 3) the ability to apply sophisticated data fusion for significantly more accurate DST interval velocity estimation. 4) the use of polynomial regression accuracy parameters to quantify how well the “best fit” polynomial fits the acquired arrival time data sets. This paper outlines the mathematical details of the best fit polynomial where a Kalman filter formulation is implemented. The performance of the DSTPolyKF algorithm is demonstrated by processing real DST data sets.

Oct 1, 2022

By David N/A Doucet, Colter N/A Angell, William N/A Joa, Kyle N/A Wagner, Catherine N/A Johnson, Marty N/A Langenderfer

The Kingery-Bulmash (K-B) equations are a widely accepted means of predicting air-blast parameters from surface explosive detonations. The parameters predicted from these calculations include incident and reflected pressure, time of arrival, shock front velocity, incident impulse, reflected impulse, and positive phase duration. K-B calculations are based on curve fitting of experimental data and can be used to predict air-blast parameters for explosive weights from less than 1 kg (2.2 pounds) up to 400,000 kg (440.9 US Tons), and ranges of 0.05 to 40 meters (1.9 inches to 131.2 feet). The K-B equations can also determine the parameters for multiple explosive types using scaled distances and relative equivalency to TNT. An experiment was designed to demonstrate if the measured results for incident pressure, time of arrival, shock front velocity, incident impulse, and positive phase duration equal the expected results reported for the detonation of a small quantity of explosive determined by the K-B Calculator. Three surface-detonated 300-gram (0.66 pound) hemispherical charges of Composition C-4 were observed via high-speed imaging and hydrostatic pressure monitoring. The hydrostatic pressure generated from each charge was measured via piezoelectric pressure transducers at a scaled distance of 10 from the charge epicenter, and at elevations of 0.30, 0.61, and 1.22 meters (1, 2, and 4 feet) above ground level. Variances in experimental values from the K-B predicted values were recorded for each measured blast parameter. Time of arrival, which was redundantly confirmed through high-speed imaging analysis and hydrostatic pressure monitoring, showed the highest deviation from the predicted values at more than double the K-B predicted value. This report compares the observed blast parameters from the test series with the expected blast parameters from the Kingery-Bulmash Blast Parameter Calculator. Differences between the experimental and predicted values are reconciled through analysis and discussion of testing conditions, instrumentation setup, and scaling methods.

Jan 1, 2019

By George P. Tateosian

Merchants perform a number of functions in the copper market. As a major distribution arm of the copper industry, they secure scrap and other copper bearing materials for processing into usable refined shapes. These are ultimately sold to fabricators. Merchants &apos; hedging and arbitrage activities help keep values in proper relationship from product to product or region to region. Through these switching and trading operations, they optimize the flow of copper from mine to consumer. And finally, merchants act as a repository for copper units during times of surplus and a stockpile from which to draw during tines of shortage.

Jan 1, 1979

By Jesus Garcia Iglesias, Jorge Loredo

"Abstract -The Asturian fluorspar district consists of vein and stratiform deposits where mineralization is controlled by a combination of lithological and tectonic factors.It is postulated that these fluorspar deposits have been formed under disequilibrium conditions created during circulation of ascending hydrothermal solutions along faults and other high permeability conduits. Mixing of solutions is inferred from fluid inclusion studies. Cavity filling and replacement processes are very important in localizing the ore deposits and in determining their morphology.Permian volcanic rocks in the area yield a regional positive geochemical anomaly in fluorine implying that Permian vulcanism may be a possible primary source of fluorine.On a regional scale a relationship can be established between some of the ore deposits and important tectonic lineaments. The stratiform deposits preferentially occur within a calcareous-detrital facies located at the margins of basins. These basin margins are related to important synsedimentary faults.Fluorite is the only economic mineral in these deposits. Quartz, carbonates, barite and pyrite are common minerals accompanying fluorite. Other minerals that may occasionally be present as minor components are: marcasite, chalcopyrite, fahlore, sphalerite, galena and related supergene minerals."

Jan 1, 1994

By R. B. Lantz

Low Froude Number (Fr) theory* predicts that stably-stratified fl& around a terrain obstacle will divide into a lower layer passing essentially horizontally around the obstacle and an upper layer passing essentially over the obstacle. The prediction was formulated by Sheppard (1956) and Drazin (1961) and confirmed experimentally in the towing tank model d experiments of Hunt et a1 (1978) and the atmospheric full scale experiments of the US EPA Complex Terrain Model Development Program (1982- 1985). The US EPA Complex Terrain Dispersion Model, currently under development, employs the layering principle with the flow in each layer calculated independently by potential flow (PF) theory after the layer thicknesses are established according to a simple function of Fr, i.e., Hc /H = 1 - Fr where Hc is the dividing streamline freight and E is the obstacle height. Use of PF theory in the CTDM is attractive because numerical solutions can be obtained simply and economically, as compared to lengthy Navier-Stokes (N-S) solutions, but realism is sacrificed in creating a surface of discontinuity between the tm layers and eliminating the effects of shear and gravity in each layer.

Jan 1, 1986

By Arthur Phillips

The progress made in recent years in the art of dispersion-hardening has naturally led to an intensive study of alloy systems capable of yielding supersaturated solid solutions at ordinary temperatures. In general, the investigations have been confined to rather precise determinations of solubility limits and to experimental approaches designed to furnish more complete information regarding the rate and nature of precipitation under appropriate thermal conditions. Efforts are being made to focus more sharply on the atomic changes that are a direct consequence of the instability of the supersaturated solution. Here precision X-ray methods have come to be of considerable importance because lattice parameter measurements indicate very precisely the concentration of solute atoms in the solvent lattice. In spite of the general acceptance of parameter values as a criterion for the placing of solubility limits, it may be suggested that no thorough appraisal has been made of the several factors that conceivably may affect such measurements. More specifically, little attention has been devoted to the significance of surface energy conditions, specimen size and method of preparation, with particular regard to the genesis of the grains and the surface concentration changes as a consequence of heat treatment and etching. Stenzel and Weertsl recently published the results of a detailed study of precipitation reactions in aluminum-rich copper alloys. They found that, although copper lowers the lattice constant of aluminum, a 5 per cent copper alloy quenched from 150" and 225&apos; C. had parameter values unquestionably higher than that of pure aluminum. Their results seem to substantiate, at least qualitatively, the earlier work of von Göler and Sachs,2 who indicated a parameter value, for the same alloy annealed for 24 hr. at 200° C., some 0.0008Å. larger than that of pure aluminum. Stenzel and Weerts attributed the abnormal lattice dimension to the effect of strain induced by the precipitation of CuA12. Weerts3 later

Jan 1, 1934

BASIC open-hearth slags have no obviously unique features when compared with slags from other metallurgical operations. Open-hearth slags form and exist at temperatures ranging from 2500 to 3100 F (1370 to 1700 C). In the course of an open-hearth heat, the liquid slag changes slowly and continuously in chemical analysis-the changes reflecting changes in temperature, changes in metal analysis, solution of charged materials, solution of feed additions, and solution of refractories. Through- out the process, the slag performs specific primary functions that are responsible for a large measure of the technical and economic importance of basic open-hearth steelmaking. It is intended in this chapter to present the chemical reactions by which the primary functions of basic open-hearth slags are carried out, to describe the physical and chemical principles governing the extent to which these reactions proceed and can be regulated, and finally to indicate the limitations imposed on other features of the process by the fulfillment of the primary functions. Basic open-hearth slags perform three primary functions. First and foremost, the slag provides a means of removing phosphorus from the liquid metal. The ability to remove phosphorus is largely responsible for the widespread use of the basic open- hearth process. Second, the slag serves as a controlling factor in transferring the oxygen required for the other oxidizing reactions. Third, the slag provides a means of eliminating some sulfur from the open-hearth bath. While the extent of sulfur removal is not comparable to that of phosphorus, the ability to remove some sulfur contributes much to the value of the process. The effectiveness with which the slag fulfills its functions varies with temperature and composition. Since operating temperatures are fixed largely by the specified nature of the product and the equipment, the speed and extent to which the functions of the slag are carried out depend largely on its composition. The necessity for regulating slag composition to accomplish the re-

Jan 1, 1951

BASIC open-hearth slags have no obviously unique features when compared with slags from other metallurgical operations. Open-hearth slags form and exist at temperatures ranging from 2500 to 3100 F (1370 to 1700 C). In the course of an open-hearth heat, the liquid slag changes slowly and continuously in chemical analysis-the changes reflecting changes in temperature, changes in metal analysis, solution of charged materials, solution of feed additions, and solution of refractories. Throughout the process, the slag performs specific primary functions that are responsible for a large measure of the technical and economic importance of basic open-hearth steelmaking. It is intended in this chapter to present the chemical reactions by which the primary functions of basic open-hearth slags are carried out, to describe the physical and chemical principles governing the extent to which these reactions proceed and can be regulated, and finally to indicate the limitations imposed on other features of the process by the fulfillment of the primary functions. Basic open-hearth slags perform three primary functions. First and foremost, the slag provides a means of removing phosphorus from the liquid metal. The ability to remove phosphorus is largely responsible for the widespread use of the basic open-hearth process. Second, the slag serves as a controlling factor in transferring the oxygen required for the other oxidizing reactions. Third, the slag provides a means of eliminating some sulfur from the open-hearth bath. While the extent of sulfur removal is not comparable to that of phosphorus, the ability to remove some sulfur contributes much to the value of the process. The effectiveness with which the slag fulfills its functions varies with temperature and composition. Since operating temperatures are fixed largely by the specified nature of the product and the equipment, .the speed and extent to which the functions of the slag are carried out depend largely on its composition. The necessity for regulating slag composition to accomplish the re-

Jan 1, 1964

By D Corley, J Moore, M Grant, A, W R

Resource estimates are the corner stone of technical and investment decision-making. Prior to mining, resource estimation uncertainty has the greatest potential to lead to poor investment decisions, despite a significant component of resource estimation uncertainty being unknowable at this critical stage in the mining cycle. This presents a conundrum to the resource geologist in terms of risk evaluation and resource classification. Ahead of mining, there is normally considerable focus on drill hole spacing analysis to determine the ‘optimal’ drill hole spacing, taking grade and geological continuity into account; cost-benefit analyses balance improved resource definition against cost; the law of diminishing returns and the exponential cost increases acting together as spacing is reduced. Typically, a lower limit to the drill hole spacing is identified. After completing the resource drilling to an agreed spacing, resource estimation is then undertaken. At this point it is common to attempt to bracket the resource estimation uncertainty. In many cases conditional simulation is used, based on a modelled, but largely assumed, variogram model. It is also assumed that the histogram of the available drill hole sample data is representative of the in-ground mineralisation. The purpose of this paper is not to diminish the importance of drill hole spacing and simulation studies, but rather to illuminate an important aspect of estimation uncertainty that, although previously recognised, is typically overlooked – the question of how representative the available data set is in characterising the true (but unknown) distribution of mineralisation. To do this, we lift the lid on one of OceanaGold’s former operations, the mined-out Globe Progress Mine, by resurrecting a high quality, close-spaced, reverse circulation (RC) grade control data set. The Globe Progress Mine is within the West Coast Region of New Zealand, it was closed and transitioned to rehabilitation in 2016 and is now known as the Reefton Restoration Project. The exhaustive Globe Progress grade control data was used to repeatedly ‘redrill’ the deposit by extracting 35 m × 35 m spaced subsets from the original 5 m × 5 m spaced grade control data. Utilising closely spaced grade control data removed the need for assumptions regarding short range continuity, which are necessary with forward-looking analyses that are based upon broader spaced resource drilling. The extraction process used a nearest neighbourhood algorithm, repeatedly moving the origin in 5 mE, or 5 mN increments. Individual resource estimates were then completed for each of the extracted drill hole data sets (49 in total) as well as a grade control estimate based upon the exhaustive data set. Whilst the data unpinning each of the 49 estimates changed, the geological assumptions, variography, and modelling parameters remained constant. This approach was taken to isolate the impact of changing the input data. The 49 estimates were then compared against each other and the grade control estimate. The mean of all 49 sensitivity estimates was close to that of the grade control estimate in terms of contained gold, tonnes and grade. Whilst it is acknowledged that the grade control estimate itself is subject to some degree of estimation uncertainty, the close match between the average of the 49 estimates and the grade control estimate suggests that the resource estimation methodology is reasonable and appropriate. Whilst this comparison is important, the focus of this study is on the component of estimation uncertainty related to the underlying data, and this is reflected in the spread across the estimates. The spread across the 49 global estimates (highest to lowest) for this particular Mineral Resource Estimation Conference 2023 | Perth, Australia | 24–25 May 2023 142 case study was found to be significant (approximately 20 per cent in grade and metal) and that is attributable solely to the underlying data. This exercise quantifies a component of the estimation uncertainty that is inherent to all drill hole data and is distinct from the uncertainties associated with modelling methodology choices, sample and subsample quality and drill hole spacing-related interpolation uncertainty. Importantly, this uncertainty is unknowable prior to mining; we can only directly compare the resource drill hole data against grade control data after mining has taken place. For the case study, approximately 65 per cent of the estimates fell within 5 per cent of the grade control estimate for contained-gold, suggesting that for many projects the histogram of drill hole data is unlikely to differ noticeably from that of the in-ground resource. However, about 15 per cent of the estimates in this study differed by more than 7.5 per cent, suggesting that a not-insignificant proportion of estimates will be materially compromised. Whether or not the available drill hole data is representative comes down to the ‘luck of the draw’ and cannot be known at the time of resource estimation. Given the challenge of attempting to evaluate forward-looking estimation uncertainty, a component of which that can only be quantified retrospectively, what should we do as resource geologists? What are the implications for risk evaluation, resource classification and reconciliation? Furthermore, without rigorous post-mining data checks, resource geologists may conflate suboptimal modelling with the shortcomings of the underlying data. An example of this problem is discussed in the following section.

May 24, 2023

By C. Liley

Open cut blasting at the Ernest Henry mine has the potential to cause damage to nearby underground workings. This paper is a case study of the blast vibration management project which was conducted to ensure pit blasting did not adversely affect the stability of upper production levels or cause damage to the underground primary fan units.

Jan 1, 2012

By Francesco Chiappalone, Daniele Nebbia, Lance Waddell, Greg Colzani

As part of the 3RPORT Project, a 5-mile tunnel is being excavated underneath the three rivers of Fort Wayne using a 19-foot diameter Slurry Tunnel Boring Machine. The groundwater pressure at the tunnel axis ranges from 4.5 to 5.3 bar. The rock mass hydraulic conductivity is very high with water inflows up to 10,000gpm imposing significant challenges to the project. After excavating 1,550-feet of the TBM tunnel, major leaks between the tailskin and the segmental lining were observed, indicating the potential deterioration of the tailskin brushes and the need for inspection and eventual replacement. The first part of the paper describes the planning of the intervention, including the design of the polyurethane grouting campaign, the procedures developed for the execution and the controls established during construction to timely assess the presence of potential hazards. The second part of the paper focuses on the experience gained during execution and lesson learned to prevent future occurrences of this nature.

Jun 13, 2021

By Denard Brandt, Isidro Martinez, Greg Baker, Laura Slattery, Teddy French

The Dos Pobres Mine is a copper oxide heap-leach mine located near Safford, Arizona. Mine production is 180,000 tons (163,293 tonnes) per day with a stripping ratio of 2:1. During the startup phase of the mine, the required fragmentation size was easy to achieve as the ore was highly weathered and fractured near the surface. As the mine depth increased, the proper fragmentation size became harder to achieve due to less weathering and different rock types. Because copper recovery increases as crusher product size decreases, achieving the appropriate product size at the crusher is the operating priority.

Jan 1, 2010

By Lala Zhao, Yuemin Zhao, Guangyuan Xie, Chusheng Liu, Chenlong Duan

"Screening is an important means of size classification used on granular or particulate materials. The vibrating modes of screen separator have a great effect on the screening process. Elliptical vibration mode is a complex motion mode which gets the common characteristics of both linear and circular vibration modes. However, the fundamental motion and screen penetration of the particles on the elliptically vibrating screen deck are still poorly understood. A numerical study of the motion of particulates flow along an elliptically vibrating screen deck is presented by means of a three dimensional Discrete Element Method (3D-DEM). The motion characteristic of the particle flow is analyzed at a particle scale. The effects of vibration amplitude, throwing index, vibration direction angle and screen deck inclination angle on the screening process are discussed. The results show that the particles average velocity increases linearly with the increase of vibration amplitude, throwing index and screen deck inclination angle, but decreases linearly with the increase of vibration direction angle. The screening efficiency is highest when the vibration amplitude, throwing index, vibration direction angle and screen deck inclination angle are 4.5 mm, 3.3, 40° and 6°, respectively. This work is helpful for developing a deep understanding of particle motion on the elliptically vibrating screen and for optimizing screen separator designs."

Jan 1, 2014

The topic of the relationships between energy and particle size has had two very active periods -the first in the early thirties, when the relative merits of Rittinger&apos;s and Kick&apos;s proposals were vigorously debated; the second in the early fifties, when Bond&apos;s Third Theory was published. This second stage has produced several contributions that have provided a clearer picture of energy /size correlations in comminution. Derivations of a general relationship have been made from single-fracture experiments and from the rate of comminution, and both methods arrive at an equation of the type E = AK-11? The constant A in the equation may be regarded as a grindability parameter. In some respects, an understanding of the phenomena associated with comminution is still lacking, and research in this field should therefore be expanded. T HE SEARCH for a relationship between the energy consumed in comminution and the size of the broken product has been long and varied, and many

Jan 1, 1964

By T. Newton, G. A. Bezuidenhout, P. J. Tauetsile, F. Trask

The technology to selectively leach gold, silver and base metals from ores, concentrates, and wastes, using an alkaline glycine solution, has initiated significant interest in using the new technology in various environments such as in-situ, in-place, dump, heap, and vat and agitated tank leaching. It has been shown that glycine acts synergistically with a number of other lixiviants to lower the net consumption of the other lixiviants while allowing low cost glycine solution recovery. Glycine is a non-toxic, stable, environmentally benign reagent that is available in bulk industrial quantities. It has the ability to dissolve most copper oxide and sulfide minerals, as well as native copper, whilst not interacting with acid consuming gangue nor dissolving iron and various or ubiquitous gangue elements. It acts synergistically with small amounts of cyanide to leach gold-copper ores at leach rates higher than either glycine or cyanide on their own, while significantly reducing cyanide consumption and eliminating detoxification requirements. The leaching behaviour of various glycine based systems will be reviewed, followed by the evaluation of the adsorption of gold onto activated carbon. Where the economics merit it, copper can be easily recovered using solvent extraction or sulfide precipitation.

Jan 1, 2017

By Marius S. Darrow, William B. White, Rustum Roy

The PbS-PbTe systen has been studied by quench-ing and D.T.A. techniques f?om 400&apos; to 1150°C. Runs were made in evacuated silica tubes so that all equilibria are at the vapor pressure of the system. Lattice parameters of the quenched salnples , measured by X-ray diffraction, show a complete crystalline-solution series existing over a narrow temperature range between approximately 805" and 871°C. An exsolution dome extends from a maximum of about 805"C (approximately 30 mole pct PbTe) to 1 and 96.5 pet PbTe at 400°C. A narrow melting region, deternined by D.T.A., extends form 918c (mp PbTe), The shapes of the liquides and solidus curves imply the existence of a minimum at 871°C at approximately 65 pct PbTe. THe exact composition of the minimum could not be established due to the very narrow two-phase region. At compositions containing less than 50 pet PbTe, liquidus temperatures begin to increase, while the solidus remains almost flat to about 15 mole pet PbTe before beginning to vise toward the mp of PbS (1075 C). LEAD sulfide and lead telluride are isostructural (NaC1 type) semiconductors whose electrical and optical properties have been extensively studied and used in recent years. If appreciable crystalline solution exists between these compounds, the variation of physical properties with composition could be of interest. The purpose of this investigation was to determine the extent, if any. of crystalline solution, and to obtain the phase diagram for the system. To the knowledge of the authors, only three studies of the system PbS-PbTe have been reported, and, in chronological order, each investigation found an increasing amount of crystalline solution. In 1956, Yamamoto reported finding no evidence of crystalline solution between the compounds. Sindeyeva and Godov-ikov,&apos; in 1959, found very limited crystalline solution. but only under conditions of excess tellurium concentration. Finally Melevski s3 investigation in 1963 indicated that one solid phase exists in the region from PbS to 7 pct PbTe and from 82 pct PbTe to PbTe at 886&apos;C, with an eutectic at 55 pct PbTe at that temperature. Detailed data on the solvus boundary were not given. EXPERIMENTAL EQUIPMENT AND MATERIALS Commercially produced PbTe and PbS powders were used as starting materials. Batches of specific mole percent composition were accurately weighed and mixed in a plastic bottle, in a shaker mill. An analy- sis of impurity content is given in Table I for pure PbS and PbTe and for two randomly selected batches after the powders were mixed. Individual samples, ranging in weight from 0.2 to 0.5 g, were sealed in evacuated silica tubes which had been thoroughly washed and rinsed with acetone and distilled water. Thus all data taken were at the pressure of the system. Subsolidus relations were studied down to 400°C by heating the samples in a vertical tube furnace for 24 hr. The sealed tubes were quenched in water with quench time from the hot zone not exceeding 1 sec. Temperatures were measured by a chromel-alumel thermocouple and controlled to 53°C for most runs. The number and composition of phases present were determined from powder X-ray diffraction patterns taken at room temperature on a Norelco diffractome-ter, using silicon as an external standard. Above 850°C quenching techniques were, in general, found to be unsatisfactory, and differential thermal analysis (D.T.A.) was used to determine melting relations. The evacuated tubes were recessed about 1 cm at one end to accommodate the differential thermocouple. Al203 was used as the reference material in a similar tube containing the other side of the differential couple. For temperature measurements, a separate thermocouple was placed in the recess of the tube containing the sample to be measured, thus providing an opportunity to obtain thermal, as well as differential, analysis. All thermocouples for these measurements were Pt-Pt 10 pct Rh. Temperature and differential curves were recorded separately on synchronized strip-chart recorders. Thermocouples and recording equipment were calibrated using NaCl and gold standards, using the melting points 801" and 1063 C, respectively, which span most of the temperature range of interest. Heating and cooling rates generally were from 4 to 7°C per min. It was found, in fact. that rates ranging from 1.5 to 25°C per min did not significantly change the data obtained.

Jan 1, 1967