Search Documents

By Sharpin PC

The countercurrent gas-solid-heat transfer during the drying of brown coal briquettes in the pilot carbonization plant at Morwell has been analysed and theoretical gas and solid temp-erature distributions through the drier have been calculated. Although the calculations rest on several simplifying assump-tions, to be corrected as the experimental work develops, the theoretical temperature distributions compare well with those observed in practical operation. Valuable conclusions are reached as to the effects of changes in drier operating con-ditions on the rate of drying of the briquettes which-controls the 2 strength of the char produced. The analysis shows why a limitation was reached in the improvement of char-strength in the pilot plant in 1961 and a prediction is made of ' a way ' in ' which the limitation could be overcome.

Jan 1, 1963

Minute of the Board of Directors, Jan. 26, 1917 In the name of all the members of the American Institute of Mining Engineers, this Board extends to. Mr. Herbert C. Hoover, an honored Vice-President of the Institute, on the occasion of his present temporary return to his native land, the cordial welcome of his colleagues, and their congratulations upon the noble work splendidly done by the Commission for Relief in Belgium of which he is the head. It is understood that a leading purpose of Mr. Hoover's visit to America at this time is the collection of additional funds, to be administered by his Commission in the care of the destitute children of Belgium. To this enterprise endorsed by both the belligerent parties, as well as inspired by the purest and tenderest sentiments of humanity, contributions are solicited from engineers, especially through an organization known as the "Belgian Kiddies Limited," which this Board, heartily approving its object and method, recommends to the consideration of the members of the Institute. On motion duly seconded it was unanimously VOTED.-That this minute be spread upon the record of the Board, and published in the Bulletin, and that a copy thereof be transmitted to Mr. Hoover, and to the San Francisco Section of the Institute.

Jan 3, 1917

By R. W. Smith

It is well known that certain silicates such as the feldspars and beryl can be readily floated from quartz at a low pH value using a long chain cationic collector in the presence of a fluoride.1-3 However, the mechanism whereby the fluoride activates feldspars and beryl is not known. Indeed, only a few authors have even speculated about possible mechanisms.1,3,4 As a first approach to the problem, it is perhaps best to look closely at the interesting character of hydrofluoric acid and how it dissolves silica and silicic acid. Hydrofluoric acid, unlike hydrochloric acid, is a weak acid with a dissociation constant of about 3.53 x 10-4 at 25°C.5 The reason for the weak acidic character of HF lies in the very small size of the fluoride ion.6 The pKa value is 3.45 which means that at pH 3.45 half the HF is present in molecular form and half in ionic form. The anion present is probably HF2.-6 At pH values below the pKa value, molecular concentration increases rapidly at the expense of the HF2- anion. It is known that HF readily attacks glass, silicates, quartz and silicic acid. The equation usually cited pertaining to the first step in HF attack of silica is6-'

Jan 1, 1965

By J. C. Martin

A theoretical analysis of steam stimulation is presented for single sands. The analysis includes the effect of steam production and most of the effects of heat conduction. The results show the effects of a number of important variables on the performance of an idealized well under steam stimulation. Calculated responses are presented which indicate the effects of steam production, amount of steam injected, water production, formation thickness and formation damage. Results indicate that steam production can cause large reductions in the heat contained in the formation. This effect can be eliminated by drawdown control. Water production reduces the amount of oil produced during stimulation. The optimum amount of steam to inject depends on economic factors as well as the well response. In many cases, the increased temperature resulting from stimulation reduces oil viscosity near the well sufficiently to overcome the effects of formation damage even if the damage is not removed during steam injection. Calculated responses for thin sands are more favorable than anticipated. INTRODUCTION Little has been published on the theory of steam stimulation'-' despite the interest it has created and the wide variation in well responses. The results of the present analysis provide an insight into steam stimulation, and the methods employed provide a foundation for future work. Analyses presented in Refs. 1 and 2 are very limited and apply to gravity drainage conditions. Ref. 3 contains an analysis similar to the one presented here. The idealized models used and the assumptions made in Ref. 3 are different from those used in this paper. The analysis assumes that after steam injection has heated a small portion of the volume within the radius of drainage of a single uniform sand, a shut-in soaking period is allowed before returning the well to production. The effects of gravity, capillarity, transient pressure and water-sensitive sands are neglected. The injection and soaking times are assumed short compared to the stimulated production time. The initial temperature is assumed uniform; thus, the results apply primarily to first-cycle stimulation. The effects of gas production other than steam are neglected, and the water-oil ratio during production is assumed constant. Steam stimulation involves the simultaneous variation of the temperature, pressure and saturations. General mathematical equations for these variations are complicated and can be very difficult to solve. Simplified equations based on idealized models are used to reduce the mathematics sufficiently to allow approximate solutions to be obtained. DISCUSSION INJECTION An idealized model for which heat conduction is neglected is used to represent the behavior of a well during steam injection. The mathematics for this model is presented in Appendix A which also contains an approximate solution for the behavior of the no-conduction model. SOAKING During soaking, the well is shut in. Only the temperature, pressure and saturation distributions at the end of soaking are needed in the analysis. During soaking the heat is considered to be conducted in a uniform medium from an initially uniformly-heated circular cylinder confined to the producing interval. At the end of soaking the saturations and pressures are assumed to correspond to the cold zone. Analysis of the heat flow during soaking is included in the next section. The radius of the heated cylinder is calculated from the following heat balance (for constant quality steam injection). At the end of the soaking period it is assumed that little or no free gas is present near the well, and that the soaking period has been sufficiently long that the steam zone has had time to expand and the steam has condensed. The condition where there is no soaking is considered in the next section. PRODUCTION In this section, an approximate method is presented for solving the equations of heat and fluid flow associated with the production of oil and water during steam stimulation. Where initial pressure drawdowns are sufficient to cause steam to flow into the wellbore, steam production is assumed to occur within a short initial adjustment period (Appendix B). The production practices followed soon after the well is returned to production can have a large influence on the amount of oil produced during the stimulation cycle. Under most conditions, there is a period of time in which some or all of the water in the heated zone is converted into steam and produced. This flashing of hot water is caused by the pressure in the heated zone dropping below

By José Gutiérrez, Cosme Soto, Octavio Vargas

El presente trabajo detalla las etapas más relevantes del proceso de cambio de la Guía Industrial 7 (IG-7) a la regulación S-K1300 cuya finalidad es reportar Recursos Minerales en la Bolsa de Nueva York. Los autores desean brindar una guía sobre las situaciones y retos más importantes sucedidos durante el proceso de adaptación y auditoria para reportar recursos minerales bajo regulación S-K 1300 en la Cia. de Minas Buenaventura. También, plantear una metodología para ponderar tanto las variables que le dan soporte a la estimación de las leyes, como los ítems que brindan calidad a la información de Geología.

May 10, 2023

By B. G. Bunting, J. H. Johnson, H. J. Schock

This paper describes an experimental method for monitoring diesel-generated exhaust gas pollutants in a deadended drift to assess the effect of control approaches. Experiments were conducted to determine the relative merits of these ventilation configurations: no auxiliary ventilation, induction ventilation at the entrance to the drift, and ventilation of the dead-ended drift with positive displacement tubing. The drift used in this experimental work was approximately 32 m long and slightly downsloping, with an everage height and width of 2.4 and 8.6 m, respectively. For this drift, it was found that ventilation with positive displacement tubing provided the best removal of diesel-generate pollutants. Induction ventilation appeared to be the least effective of the three methods examined.

Jan 1, 1982

By J. H. Anderson, G. A. Parks, B. K. Jindal, H. Leslie Bullock

H. Leslie Bullock (Engineering Consultant, Oak Park, 111.) — In reading over the paper, I find that I have no quarrel with the thoroughness of investigation of the points studied, but I am forced to question the selection of oxides from oxides as the subject of the investigation, the inclusion of silica gel as an example, and to question the validity of some of the conclusions. Separation of oxides from oxide, in minerals where the liberation of values is possible by grinding, are comparatively rare. Most oxides are only slightly soluble and the action of carbon dioxide or other acid forming ingredient in the air must be added to humidity to produce surface action. Silica gel is a very special synthetic substance in which the adsorption is determined by total surface, pore dimensions and temperature. Quartz is our most prevalent oxide and its action in electrostatic separation is far more sensitive to its three thermal transition points than to humidity.

Jan 1, 1968

K. W. Turner, Sail Francisco, Cal. (communication to the Secretary*): The recent papers in the Transactions by Vogt,' Lindgren2 and Weed: on ore-deposits that have formed as a direct result of igneous intrusions, show that deposits of this class are widely distributed over the world, and are occasionally of commercial value. This is especially true if we consider under this head all deposits in the zone of contactrnletamorphism, the origin of which may be ascribed to the gases and vapors generated by the heat of the intrusive rock. Mr. Smith's description of the Chillagoe garnet-formations containing copper, leads one to regard these depoaits as of contactrmetamorphic origin, although he gives certain reaeons for supposing them to be of igneous origin.

Jan 1, 1904

By A. B. Cron, R. MacPhail, L. Melis, K. Armstong

"Mt. Milligan is a porphyry gold/copper deposit in north-central British Columbia. Diluted and mineable drill-indicated reserves total 449 million tons at an average grade of 0.013 oz gold/ton and 0.19% copper. Large-scale commercial development of the deposit will make Mt. Milligan Canada's third largest gold mine.Metallurgical investigations for the Mt. Milligan project were done in three phases: scoping tests in the first half of 1989; bench-scale work from October 1989 to April 1990; and a pilot plant program in May and June 1990. Various process alternatives for the recovery of gold and copper are described and results are presented. Net smelter return evaluations led to the selection of optimum process conditions for maximizing revenue from gold/copper flotation concentrates.The selected flotation circuit and basic design criteria are described. Forecast average recoveries over the presently-defined 20-year project life are 75.2% for gold and 90.5% for copper in a copper concentrate averaging 17.6% copper and 1.0 oz gold/ton. 1.0 PROJECT LOCATIONThe Mt. Milligan porphyry gold/copper deposit is located in northcentral British Columbia, 150 km north of Prince George, British Columbia. The site is at an elevation of 1,100 m in an area of logged, gently-rolling topography. Nearby communities include MacKenzie and Fort St. James. Climate in the area is moderate and there is direct road access to the property. A location map is presented in Figure 1-1."

Jan 1, 1991

By Greg Partington, Darryl Thorburn, Charlene Wildman, Elisa Puccioni, Connie Payne, Campbell McKenzie

"Mineral prospectivity modelling of polymetallic nodule deposits has been completed over the Cook Islands Exclusive Economic Zone (CIEEZ) using the GIS based Weights of Evidence modelling technique. Polymetallic nodules, also known as manganese nodules, have been explored as a possible resource for a number of metals including cobalt since the early 1970s. Recent data on the nodule composition and abundance in the CIEEZ has led to a renewed interest in the prospectivity for manganese nodules in the region. The predictive modelling has used the most recently accepted mineral model for polymetallic deep-sea nodule deposition to identify factors that are most likely to map the presence of this type of mineralisation in the CIEEZ.Manganese nodules form on the deep seafloor as concretions formed by concentric layering of iron and manganese hydroxides around a core and they grow at a very slow rate, on the order of millimeters per million years. The available data for the CIEEZ indicates a greater abundance in the area of nodules formed by hydrogenetic processes, which are the result of slow precipitation of metallic components from seawater. The environment in which the nodules are most abundant is at depths between 4,000 m and 6,000 m in areas of low sedimentation rate. Hydrogenous nodules commonly grow on siliceous and pelagic clay sediment, they are less common on other types of sediment."

Sep 1, 2014

Asian countries are now facing very crucial aspects of urban living under the recession of the economy. The current situation is such that those hard aspects may make the living standards worse and worse in the next century, unless proper measures are taken on the infrastructure for urban lives. More than half of the population in Asian countries are now living in cities. Nowadays, the socio-economic development of the Asian countries has been closely linked to the development of world economy because of the border-less economy system. The population inflow to big cities is inevitable as the Asian countries step into an industrialised economy. Such a tendency will be further accelerated when Asia becomes a centre of financial business in the 21st century. The government of any country has realised the situation very well. The United Nations has established a specific agency to solve the problems caused by the rapid urbanisation. This global agency for urbanisation is named United Nations Center for Human Settlement and it is so called Habitat. There are three Habitat offices in the world, Nairobi in Kenya, Santiago in Chile and Fukuoka in Japan. The activities of Habitat offices cover a wide field of issues such as housing, urban development, infrastructure and environment, etc. Habitat Fukuoka Office is serving Asia and Pacific in co-operation with the government offices concerned.

Jan 1, 1999

By E. P. Youngman

Great Britain has never had a basic raining law such as is in force in most foreign countries. This lack may be due to the fact that, with the exception of gold and silver, all metals or minerals belong to the owner of the surface land. Even with respect to the precious metals, gold and silver, which are not abundant in Great Britain, the right of the Crown, though still technically acknowledged, is not always insisted unon. All other metals and minerals are vested in the ground landlord, who may sell, lease, or other¬ wise convey them. The State has little to do with the mining industry except in. regulatory and judicial matters. The Government must settle controversies and provide for easements, rights of way for railroads, roads, and canals, or, in general, effect the same control that it exercises over other industries. As mining was carried on in very early times in England, of necessity a certain legal procedure came into existence, which in effect was little more than a private contract between the owner of the mineral (whether an individual or the State) and the miner. The nature of such contracts, of course, has changed radically with the changed relations between classes, as England lias developed from the feudal into the modern State. From the medley of ancient procedure and custom, a concession system of mining in^its simplest form lias evolved. Of the earlier conditions. Van Wagenen says

Oct 1, 1931

By G. L. C. Young

The first full-scale Reichert cone concentrating plant to be erected at a large South African gold mine was at President Steyn Gold Mining Company, Welkom. ThiR plant was installed as a part of the runof-mine mill extension of 150000 t per month that was commissioned in 1976-1977.

Jan 1, 1982

By J Rubio

This work presents design features of an innovative in-line mixing helical (coiled) reactor for flocculation and flotation as a solid-liquid separation process for suspended particles (including liquid droplets). The device has been named flocs generator reactor (FGR), a compact system whereby the flocculation of particles is assisted by the kinetic energy transfer from the hydraulic flow through the reactor and/or by the injection of microbubbles (30 - 70 ¦m). The flow mixing presented a plug flow regime with a low dispersion degree, promoting the required hydrodynamic conditions to disperse the polymer flocculant (cationic polyacrylamide) and to generate æstrongÆ flocs of Fe(OH)3 or clays (as colloidal model systems) with aggregation using an anionic polymer, Al2(SO4)3 and poly aluminium chloride (PAC), and oil emulsions destabilisation with a high molecular weight cationic polymer. The solid-liquid separation of the flocs was then achieved either by settling or by flotation with microbubbles. This paper discusses advances in this new in-line flocculation-rapid flotation device to remove æaerated aggregatesÆ, aggregates with entrained and entrapped bubbles. Studies were carried out with different models of FGRs (varying the length:volume ratio) and process efficiency (mainly kinetics) evaluated as a function of polymer concentration and some operating parameters, namely, feed flow-rate, air:solids ratio and residence time. Results showed that the aerated flocs are readily floated with rising rates in the order of 120 mh-1, values higher than those obtained for the settling of the non-aerated flocs (18 - 24 mh-1). The FGR requires short residence times and generates dense, well structured flocs (with a mass fractal dimension, dF of about three) which withstand high shear forces. Mechanisms involved appear to include small bubble formation and their rapid occlusion (entrapment) within flocs, nucleation of bubbles at floc/water interfaces, polymer coiling as a result of æsalting outÆ effects at the aqueous/air interface and plug flow type of mixing (flocculation). Successful examples of emulsified oil and solids removal from water are shown and because in all cases high efficiencies were obtained (>90 per cent removal). Due to the high process efficiency and high loading capacity shown, the FGR appears to have good potential as an in-line flotation-separator device in applications requiring high rate solid-liquid or liquid-liquid separations.

Jan 1, 2005

By L. C. IlsLey

Briefly, a permissible schedule of the Bureau of Mines establishes certain minimum standards for safety; it gives details of test methods adopted to determine whether these standards have been met, and a list of charges for such tests. Any manufacturer has the privilege of submitting his product for test in accordance with the conditions outlined in the schedules. His action is wholly voluntary, for the Federal Government has no jurisdiction as to what equipment shall be used in mines, this authority being left to the various States. When the product of a manufacturer has met the schedule requirements, he is permit¬ted to advertise this fact and to attach an approval plate with the bureau's seal to each machine he makes that is identical in every way with the equipment tested, inspected, and approved by the bureau. This work of approval has grown by the addition of new schedules until at present a great many mines are using one or more classes of permissible equipment, and there is still a demand for other approved apparatus in the ever-widening field of electrically operated machinery. The safety of electrical equipment of this type depends on four fundamentals, namely, (1) correct principles of design; (2) proper assembly of parts at the factory; (3) proper assembly and installation of equipment at the mine; (4) and proper operation and maintenance after installation. The first two factors are within the province of the manufacturer. The bureau either inspects and tests several models of one product, such as electric cap lamps, or one model, such as an electric motor. If this series of tests proves satisfactory, the manufacturer is given the privilege of making other appliances, and assembling them in the same way; the approval plate he attaches is his guaranty that the equipment is identical with the one tested and inspected by the bureau. The third and fourth factors concern those who use such permissible equipment, and it is to them that this paper is mainly addressed, in an effort

Jan 1, 1922

ZAY JEFFRIES (communication to the Secretary*).-Having seen Mr. Ruder's micrographs of electrolytic iron, I am of the opinion that the tentative explanation offered verbally is correct. Mr. Ruder has informed me that both of the samples were cooled in the furnace. The structures as shown in Figs. Band C resulted from the last cooling through the temperature range near 900° C. Assuming that the rate of cooling through this range was the same in both cases, the differences in struc-ture of the gamma iron in the two samples must have ]:)]-ought about, in some way, the variations in grain size and grain shape shown in Mr. Ruder's micrographs. Even though there is practically no temperature gradient in muffle-furnace treatment during the "soaking" period, during both heating and cooling, there is a temperature gradient. Fig. B should normally have been fine-grained prior to the last cooling, due to the comparatively low maximum temperature to which it was heated (1,000° C.). On cooling through the allotropic change point at 900°, these small gamma grains, iii conjunction with the temperature gradient, should form an ideal condition for germination. Germinant grains should form near the surface of the sample (the-colder portions) and the small gamma grains would be progressively absorbed as they changed into non-gamma iron. The elongated grains in Fig. B, converging toward the axis of the piece of iron, indicate that germinant grains first formed near tine surface and advanced their boundaries toward the interior of the sample. The gamma grains in Fig. C, however, should have been large, prior to the last cooling, due to time high temperature treatment (1,250 to 1,300° C.). In other words, to use one of Prof. Howe's expressions, the crystalline organization should be very complete and the change from gamma to non-gamma iron on cooling would take place reluctantly. This resistance to change from gamma to non-gamma iron would probably be greater in the interior of the large grains than at their boundaries. Non-gamma iron centers or nuclei would probably form at a great many places, at the grain boundaries, thus masking the influence, to a large

Jan 6, 1917

By M. Bryson, J. Taguta

The Prieska deposit, mined between 1971 and 1991, is one of the world’s top thirty volcanogenic massive sulphide (VMS) base metal deposits. The Prieska Copper Mine in the Northern Cape Province was closed by Anglovaal when underground mining had extended to depths which did not allow for safe and economic extraction of the deposit at the time. The mine has a recorded historical production of over 1 Mt of zinc and 430 k tonnes of copper from 46.8 Mt of milled sulphide ore, achieving life-ofmine metal recoveries of 85% for copper and 84% for zinc into high quality concentrates (refer ORN ASX release 15 Nov 2019). Orion Minerals Ltd is currently investigating the feasibility of developing a new mine in the footprint of the historical Prieska Copper Mine, using the extensive remaining infrastructure, with the intent of extracting the unmined zinc-copper mineralisation from the Prieska deposit. This paper reports results on the flowsheet development philosophy on the hypogene ore, and challenges encountered in the process. This study initially failed to replicate historic copper and zinc recoveries employing the historic production flowsheet and reagent conditions unmodified on bench scale, as the copper and zinc were co-floating. Flowsheet modifications were therefore made to improve differential flotation and recovery, resulting in achieving comparable saleable products and recoveries from processing the hypogene ore on bench scale. Flotation variability test work on the hypogene ore focused on the use of the original flotation procedure and reagent suite using a sodium cyanide-zinc sulphate depressant system on the copper circuit, and it generated a saleable copper product of 20-26% Cu grade at 80-86% recovery. The zinc circuit generated a saleable zinc product grading at 48-55% Zn at 80-94% recoveries. Some zinc losses were due to the deportment of some zinc in sauconite. It is recommended that further test work may further improve the copper grades and recoveries. Keywords: Prieska, flotation, hypogene ore, flowsheet development, sulphide flotation, reagents

Jan 1, 2020

By J. W. Freeman, E. E. Reynolds, A. E. White

Fram a study of 63 systematic alloy modifications it was found that molybdenum, tungsten, and columbium, added individually or simultaneously, and increases in chromium cause major improvements in 1200°F rupture strengths of Cr-Ni-Co-Fe base alloys. Rupture strengths were a function of the effect of composition modifications on both the inherent creep resistance and the amount of deformation the alloy would tolerate before fracture. THIS paper describes the results of an investigation of a series of alloys with systematic variations of the chemical composition of the following basic alloy: C, 0.15: Mn, 1.7; Si, 0.5; Cr, 20.0; NI, 20.0: Co, 20.0: Mo, 3.0; W, 2.0; Cb, 1.0; N, 0.12; Fe, 32.0 pct. The 62 modifications of this alloy were produced under conditions which minimized all factors influencing properties at high temperatures except composition. Melting, fabrication, and heat treatment were carefully maintained constant. Stress-rupture properties at 1200°F were used as the primary criteria of evaluation of the alloy. The objective of the study was to obtain data for determining the fundamental role of the influence of alloying elements on properties of heat-resistant alloys at high temperatures. In addition the results should be useful in determining optimum chemical compositions, the sensitivity of properties to variations in composition, and the degree to which alloy content could be reduced while retaining worthwhile properties. It is difficult or impossible to develop correlations between properties at high temperatures and systematic variations in chemical composition from published data for wrought heat-resistant alloys developed for gas turbines.' ' The main reason for this is the extreme dependence of the properties on conditions of treatment of the alloys." In most cases variation in final treatments between alloys so influences the properties that the influence of chemical composition is obscured. In addition it is recognized Table I. Basic Alloy and Some Modifications Used Basic AllOy, Variations in Element Pct Composition, Pct C 0.15 0.08. 0.40. 0.60 Mn 1.1 0.03,0.25.0.50,1.0,2.5 S1 0.50 1.2, 1.6 Cr 20.0 10, 30 Ni 20.0 0, 10,30 Co 20.0 0. 10, 30 MO 3.0 0. 1.2.3, 5, 7 W 2.0 0, 1, 5, 1 Cb 1.0 0.2,4,6 N 0.12 0.004, 0.08, 0.18 Fe 32.0 that variations exist between heats of the same alloy which are related to melting practice and that there is a strong possibility that conditions of hot working influence response to final treatments. The development of heat-resistant alloys has been based on the gradual accumulation of data roughly related to composition from extensive testing programs. There is every reason to believe that in most cases the optimum compositions have been achieved by this procedure in the alloys commercially available. There are, however, very little data showing the influence of systematic variations of composition free from the influence of other factors, particularly for alloys of the type investigated. Several investigators of cast alloys have demonstrated compositional effects, notably Grant,1-6 Epremian,t Guy,8 and Harder and Gow.9 Sykes10 eviewed the work on the wrought alloy Rex 78 and the systematic variations of carbon, copper, molybdenum, and cobalt leading to the development of the stronger Rex 337A alloy. From the papers by Wilson11 and Henry12 it is possible to deduce the beneficial effect of substituting cobalt for iron in 0.45 pct C-20 pct Cr-20 pct Ni-4 pct Mo-4 pct W- 4 pct Cb alloys. Wilson mentioned but did not present the extensive compositional studies involved in developing these alloys. Binder" showed optimum properties for 3, 2, and I pct, respectively, for molybdenum, tungsten, and columbium in 20 pct Cr-20 pct Ni-20 pct Co-30 pct Fe alloys for limited systematic variations of these

Jan 1, 1953

By R. S. Kinasevich

As part of other work related to the studies of kinetic factors that influence the flotation of specific sulphide minerals, specially designed kinetic flotation experiments at Cominco included work done on -65 + 100 mesh and -100 + 150 mesh, high purity galena. The flotation collector used was sodium isopropyl xanthate containing radioactive sulphur-35. Radiation monitoring of the galena fractions from stage flotation tests indicated that the adsorbed radioactive xanthate was uniformly distributed among the floated fractions and the non-floated, or residual portion of the galena. This anomalous behaviour could not be correlated to changes in Seebeck coefficients, to lattice distortions, or to the nature of the mineral surface as revealed by infrared spectroscopy and by microscopic measurements.

Jan 1, 1970

By R. W. Stormont, F. Wald

The phase diagram of the Pseudobinary section PbTe-Fe was determined. It was found to contain a monotectic and a eutectic reaction, the latter one taking place at 14 at. pct Fe and 875° * 5°C. The solid solubility of iron in PbTe was found to be 0.3 at. pct by electronmicroProbe analysis. No solubility of PbTe was detected in iron. Slight deviations from true pseudobinary behavior were found to occur in the range of - 5 to 10 at. pct Fe. In the course of a general investigation of reactions of various metals with lead and tin telluride,' the lead telluride-iron system was reinvestigated. It had been established much earlier than iron does not chemically react with lead telluride but forms a eutectic with a melting point of 879" The eutectic composition or other related information has never been reported, but for a number of years iron has been in general use for contacting of lead telluride and lead telluride alloys for thermoelectric applications. It seems therefore desirable to clarify the exact constitution of the system to furnish a base for the long-term evaluation of bonds made between lead telluride and iron either by pressure contacting or by brazing methods. I) EXPERIMENTAL METHODS Lead telluride-iron alloys were prepared in 10-g charges, using premelted lead telluride. This material was prepared from high-purity, semiconductor-grade lead and tellurium obtained from the American Smelting and Refining Co. and described as 99.999 pct pure. The iron used was "Armco" iron; the major impurities found here were 0.02 pct C, 0.018 pct Si, and 0.015 pct Cr. All remaining impurities were less than 0.01, the total of all impurities not exceeding 0.15 pct. Charges were prepared in closed quartz arnpoules which were evacuated and in some cases backfilled with high-purity argon to retard excessive lead telluride evaporation and deposition in slightly cooler parts of the ampoule. For high iron concentrations, this can lead to total separation of the constituents, since the vapor pressure and the sublimation rate of PbTe are quite high.4 Nevertheless, since the ampoules are closed, no change in overall composition was expected and the nominal composition of all alloys was assumed to be retained. X-ray diffraction analysis, thermal analysis, and microsections were used in the evaluation of the alloys. The nature of the system was such that X-ray diffraction was not particularly helpful. It merely served to establish that at all concentrations PbTe and a! iron were in equilibrium at room temperature. Thermal analysis was carried out by taking direct temperature vs time curves on a Sargent recorder where a width of 10 in. was kept as 1 or 0.5 mv by use of an automatic bucking voltage network. Quartz ampoules with minimized dead space, coated with boron nitride and fitted with a thermocouple reentrant, were used as containers for the charge. At high temperatures and over long periods of time, boron nitride reacts with iron. For the thermal analysis runs, however, this was not significant. More significant was the fact that the vapor pressure of PbTe at some of the meas -uring temperatures apparently exceeded I atrn quite considerably. This, in some cases, caused the slightly softened quartz tubes to blow out if great care was not taken to contain them and minimize time and temperatures used. As containers pure nickel tubes were used which also served to avoid temperature gradients in the quartz ampoule. Nevertheless, the experimental difficulties at high temperatures were severe and the monotectic temperature could therefore not be determined accurately. In general, the accuracy reached by the thermal analysis setup in this case is *4"C as determined with gold, silver, and tin, under the conditions of analysis here. Inherently, the apparatus is capable of reaching accuracies better than i 1°C. Also, difficulties were encountered in microsection-ing. They were related to polishing, since it is rather difficult to avoid pulling the iron out of the weak and brittle lead telluride matrix. It proved best to follow a procedure where, after grinding to 600 grit on carborundum paper, a polish with 6 p diamond was used on nylon cloth. Finally, #3 "Buehler" alumina and an automatic polisher were used for -5 min only, to avoid relief. The best etching results were achieved with

Jan 1, 1969