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By Tom Shumka

All mineral processing facilities that use girth gear driven mills need to inspect the gear teeth on a routine basis, whether it is every six months or every three years. The inspection frequency depends upon gear tooth condition, and the objective is to ensure operational integrity of the gear teeth. Conventional methods such as magnetic particle testing, visual inspection, or dye penetrant examinations rely heavily on interpretation. At best, these techniques can determine whether a defect exists, but are unable to provide information on defect severity. This paper describes the use of combined Eddy Current Array (ECA) and Alternating Current Field Measurement (ACFM) to provide a complete survey of all surface breaking indications on the whole gear tooth depth. This method accurately determines the size, length and depth of any cracks found on the surface.

Jan 1, 2012

By Arne Landsberg

Experiments were made with a batch reactor to determine the effect of gas pressures, temperature, and gamma radiation intensity on the reaction CO + Ch ? COC12. The equation, [dp = 0.0110 (1 - 0.01t) (PCOI)1/2 PC12] where [dP] is the change of pressure of phosgene with time (atm/hr), t is the temperature (°C), PCO and PC12 are the reactant pressures (atm), and I is the radiation intensity (r/hr), was found to best fit the data. Oxygen and a large ratio of reactor surface to volume retarded the reaction, but inert gases had no effect. A low-temperature reactor system is proposed to take advantage of the conditions which give a high reaction rate with gamma radiation and a simple scheme of product purification.

Jan 1, 1970

By S. P. Mehrotra

In this review article, various approaches and mathematical models that have been used to simulate, design, and synthesize flotation circuits are examined. First, a brief review of flotation kinetics is presented which is followed by a discussion on simulation of flotation circuits. The existing literature on optimal design of flotation circuits has been divided into two broad categories. In the first category, a generalized integral approach is used wherein the optimal circuit design involves determination of both optimal interconnection of various flotation cells/ banks of cells in terms of structural parameters and optimal values of various operating parameters. In the second category, a conventional circuit configuration is assumed to be the best configuration; the optimal design here only means the optimization of operating parameters. The merits and demerits of these two approaches are discussed.

Jan 1, 1987

By Davies B, Rogers A, Grainger A, Todd J, Brenman R, Jones L, Horton B, Eager L

Research into the control of diesel particulates (DP) has been. conducted by BHP Coal for more than 7 years. Personal monitoring of employee exposures (n = 480 full shift samples) conducted at nine underground coal mines has indicated that the exposure of the workforce ranges from less than 0.1 to 2.2 mg/m3 of DP dependent on job type and mining operation. Approximately 50% of the mass of DP captured is elemental carbon (EC) which is the species currently being considered by some international regulatory authorities as the exposure standard. Five technologies for controlling DP were investigated in a combination of studies conducted in an above ground simulated tunnel, in a special controlled section of underground mine roadway and validated by application in standard coal mining operations at Tower Colliery. Tests conducted under controlled conditions indicate that dependent on the type of fuel in use, the introduction of low sulphur fuels can reduce DP levels in return airways by up to 50% and in actual mining situations a reduction of 20% can be achieved in exposure of the workforce. In addition, subjective responses from the workforce indicate that exhaust emissions from low sulphur fuels provide lower irritation and a more pleasant aroma. The use of water filled scrubber tanks reduces the level of DP emissions by 25%. Chemical decoking of engines resulted in a reduction of 20% in DP in return airways. A commercially available non-flammable disposable dry exhaust filter constructed from synthetic organic fibres with an operational lifetime in excess of 20 hours was found to reduce DP exhaust emissions by 80%. Investigations have indicated that the use of increased ventilation to control DP levels particularly in multiple vehicle situations does not follow a simple dilution factor and in some instances compliance with current regulatory requirements may not produce the required reduced exposure levels. The results from single component control strategies provide considerable reduction in exposure to DP, however the most efficient and cost effective control methodology is the use of a combination of individual systems modelled to operations conducted at each mine.

Jan 1, 1998

W. C. MATTESON (communication to the Secretary*).-The criticism and question raised by Arthur Knapp regarding the standardization of nomenclature is most important. Faulty rock classification-is generally the result of carelessness or ignorance on the part of the driller. Two remedies might be suggested. In a field where several large companies are operating on an extensive scale, a geologist from each concern might be assigned to superintend the gathering of well-log data and the classification of samples. The geologists from the several operating companies might then combine their data, which would doubtless give valuable information to all interested parties. At present, coordination is not a big factor, unfortunately, but the time will come when conservation will demand such systematic coordination on the part of competing companies. The second remedy lies in instructing and educating the driller to a thorough understanding of the importance of an accurate log and correct classification of the various formations. The writer does not agree with the statement that "90 per cent. of the logs as taken today are absolutely worthless to any one but the one who has taken the log." While mistakes in nomenclature often occur, the driller is generally able to classify the important water-, oil-, and gas-bearing formations with a fair degree of accuracy. Such information is often sufficient to permit accurate correlation and also constitutes valuable data for projection purposes. It must be borne in mind that to attempt to use well-log data in a strict scientific sense of accuracy is impracticable and impossible. A broad interpretation and a comprehensive knowledge of the practical limits of such' information are essential in applying it successfully. Even experienced geologists do not always agree on rock classification. The question as to what constitutes correct nomenclature should receive the earnest and immediate attention of geologists, operators, and producers. Although standard textbooks on geology give correct definitions and descriptions of the general rock species, such textbooks fail to develop the subject in sufficient detail for the work under consideration. A committee composed of appointed members from the American Institute of Mining Engineers, the Geological Society of America, and the

Jan 6, 1917

By J Centofanti, D Conti, R Riske, C Morley, A Cook

Why is it so difficult? Why are there differences throughout the resources industry in how reconciliation factors are reported and calculated? Why is there no standard formula to use? These are common questions asked when mining companies try to compare reconciliation results across operations or attempt to undertake internal or corporate governance reporting processes. For many mining companies the calculation of reconciliation factors is often a very time and resource intensive part of mandatory reconciliation reporting. Some major mining companies, that move millions of tonnes of material per annum, dedicate full time resources to the calculation of reconciliation factors. The willingness of these companies to set aside resources demonstrates the value that operations place on good reconciliation reporting. Reconciliation is about measuring the variance between two like measures at different points along the mining sequence. It can be undertaken between predictive models, forecast plans and actual measured performance. Calculations are used to derive a variance between two sections within the mining sequence, with the result being commonly known in the resources industry as a æfactorÆ. Mining companies use the calculation of reconciliation factors as key performance indices (KPIs) to provide a æhealth checkÆ of their operation, with variances often pointing to issues either with the accuracy of the original estimate or the quality of the measurement being used in the comparison. There are many reconciliation factors that can be calculated and reported. This paper will set out, clarify and provide a recommended standard means of calculating each specific factor that, where adopted by a company, will ensure compliance with the international reporting codes, such as JORC. Using case studies from Rio Tinto Group (Rio Tinto) and BHP Billiton Mitsubishi Alliance (æBMAÆ), and the authors experience across a wide range of mine sites, the outline of a generic solution for tracking a parcel of material from the pit through to the port along with appropriate reconciliation factors is provided. The intention of proposing standardised reconciliation factor terminology and methodology is to provide the foundations of a system to enable communication and comparison across different commodities, companies and mines sites.

Jan 1, 2009

By George Burgess

NOTE BY THE EDITOR.-This resume of a Technologic Paper which is published in full by the U. S. Bureau of Standards, is brought before the membership of the Institute with the object of affording an opportunity for the open discussion of results of an investigation by the authors named above, of some phases of the manufacture of steel rails which are of great importance to manufacturer and consumer alike. This resume will be presented at the Pittsburg Meeting of the Institute. Discussion is invited, by either members or non-members of the Institute. The discussion may be sent in writing to the Editor, in advance of the meeting, or should preferably be presented in person at the meeting. To those who desire to discuss, copy of the full Technologic Paper (No. 38), as published by the Bureau of Stanaards, will be sent upon request addressed either to the Bureau of Standards, Washington, D. C., or to the Editor, American Institute of Mining Engineers, 29 West 39th Street, New York, N. Y. Summary of Researches and Conclusions The main objects of this investigation were to determine, from measurements taken at representative rail mills, the present American practice regarding the temperatures at which rails are rolled; to demonstrate the ease and accuracy with which such temperatures may be measured, without interfering in any way with the manufacture of the product; to find out what the "shrinkage clause" in rail specifications really means; and, finally, to determine some of the physical properties of rail steels, particularly those of interest in manufacture, some of which seem to be insufficiently known as yet. 1. Ingot Temperatures.-Measurements made in four mills show that ingots for rails are rolled at temperatures ranging from 1,075° to 1,150° C. (1,965° to 2,100° F.), and that, in a series of 20 to 40 ingots, the variation in temperature from one ingot to another is only 10° to 20° C. 2. Finishing Temperatures.-Rails are finished at temperatures ranging broadly from 880° to-1,050° C. (1,615 to 1,922° F.), but usually ranging within 50° C. of 935° C., and occasionally above 1,100° C.

Jan 9, 1914

It is not often that mines have as much warning of the approach of bad ground conditions as was the case at the Western Mining Corporation, Kambalda Nickel Operations Lafranchi/Schmitz Decline. Most aspects of this operation are in fact quite unique and like the best solutions, the answer to the problem of weak and foliated ground conditions was relatively simple; requiring the use of readily available explosives although the idea of using it in this manner may not be the most obvious.The use of high shock energy POWERGEL 2131 cartridges proved to be the correct answer, in conjunction with small changes in drill pattern design. The resulting lack of overbreak bears testimony to the success of the concept and the commitment of the miners to achieving a safe working environment.

Jan 1, 1992

By Mark R. Stephenson

Everyone knows that mining is a noisy job, but did you know that you are nine times more likely to lose your hearing than someone who works in a quieter job? If unprotected from noise on the job, by age 50, you will probably need hearing aids. Obviously, the best solution is to engineer out the noise, but that isn?t always im­mediately possible. Until mines are quieter, one way you can help save your vital sense of hearing is to use hearing protectors whenever the noise around you is hazardous. Even if you already have some hearing loss, you can use hearing protectors to prevent your hearing from getting worse. When loud noise is present, proper use of hearing protectors will help miners pre-vent most or all noise-induced hearing loss.

Jan 1, 1998

By George W. Riter

(Canal zone meeting, November, 1910.) A DISTINGUISHED engineer, the active head of a large mining company, has said that surveying attains the dignity of a profession only in the hands of a few men-the few who know how to keep notes that will be understood by even a novice without further word of explanation. Of all mine-records, survey notes are perhaps the most important. The maps made from them serve as a working-guide, and as framework for other data ; and when, from any cause, access to underground workings is shut off, the surveyor's record often becomes invaluable. So seldom does a surveyor have a chance to check underground surveys by making a closure, that he is compelled to rely on the precision of each step of his work for the accuracy of the final result. When data are fully recorded on the spot, the notes, even in the hands of second parties, become evidence of the care and precision with which the surveying was done. It is worth a great deal to be able to pick up the work of a former surveyor where it was left o$; and to be able to carry it forward without retracing from the beginning. The purpose of this paper is to describe the survey-note system of a mine now under my direction, in which underground surveys had to be relied upon entirely for the proper division of rich ore-bodies between neighbors, thereby placing a premium on accurate surveying and permanent records. In survey-work, it soon turns out that paper is the least item of expense, and that little is gained by trying to economize note-book space. For many purposes it is best to record notes on cards or loose-leaves, which may be left in the office at the end of the day's work, and need not be carried into the mine again, there to become smeared with grime and grease. With the loose-leaf or card system, all notes relating to the same local-

Apr 1, 1911

By N. J. Grant, B. C. Giessen, R. Koch

The system Nh-Ir was investigated over the complete concentration range by metallography and X-my techniques, using forty one alloys. The solubility limits of terminal and intermediate phases and the solidus temperatures were determined. Five intermediate phases were found: a Nb3Ir, cubic, Cr3O type; tetragonal, ofecr thorhomhic, isostruc-turn1 with (ta-Rh); and a Nhlr3. cubic, AuCu, type. a Nb3lr and a Nbfr3 melt congruently; three eutectic and three pentectic reactions occur. The phase diagram of the Nb-Ir system had not been fully treated in the literature; only surveys of intermediate phases were found.1"5 In this study, the details of the phase boundaries were investigated as well as the crystallography of the intermediate phases. EXPERIMENTAL METHODS The experimental procedures such as arc melting of powder compacts, heat treatments, solidus measurements, X-ray, and metallographic observation were identical with those used in the work on the Nb-Rh phase diagram.&apos; They will therefore not be repeated here except where the conditions differed. The purity of the niobium powder was as stated in Ref. 6; the iridium powder of 99.9+ pct purity from J. Bishop and Co., Malvern, Penn., did not contain impurities exceeding 100 ppm, except rhodium (200 ppm). The melting points and vapor pressures of both elements are very similar. This fact contributed to a very small weight loss on melting and facilitated preparation of homogeneous alloys. As shown in Ref. 6 for Nb-Rh, no oxygen pick-up exceeding 200 ppm had to be considered; this was regarded as valid also for Nb-Ir. A total of forty one alloys were used in the determination of the phase diagram; their concentrations are shown in Fig. l, which presents the phase diagram. The concentration limits as determined by the weight-loss method averaged <0.2 at. pct, and never exceeded 0.5 at. pct. Heat treatments were carried out as described in Ref. 6. Depending on the concentration, only tantalum, tungsten, or iridium containers were employed, avoiding oxide crucibles altogether. Alloys from 0 to 25 and from 65 to 100 at. pct Ir were homogenized at 2095°C for 15 hr, intermediate compositions from 25 to 65 at. pct Ir for 65 hr at 1780°C. A typical annealing-time schedule is presented in Table I. Solidus points were measured as described in Ref. 6 with the modification that samples rich in niobium were held between pieces of tantalum foil and samples of high iridium concentrations were held between rhenium platelets or in iridium wire. After each run it was ascertained metallographically that no reaction with the holder had occurred. Rhenium was selected as holder material after it had been shown in separate tests that the melting points of Re-Ir alloys rise continuously from 2440°C. Metallographic examination was carried out as described in Ref. 6, and the same procedure and etchants were used successfully. While metallographic discrimination between a Nb3lr and o was easily possible, X-ray diffraction was necessary to separate al and ct2. X-ray powder patterns were taken and evaluated as for Nb-Rh6 yielding the error limits indicated in Table 111, to be introduced later. For the determination of the invariant reactions and phase boundaries, the same techniques as for Nb-Rh6 applied. The general accuracy of invariant concentrations is regarded as somewhat higher than for Nb-Rh due to the small slope of most solvus lines.

Jan 1, 1964

By L. S. Birks

The bainite transformation in a 3.5 pct Ni-1.25 pct Cr steel was studied under various conditions of cooling and stress. Several characteristics may be specified: 1) transformation in the bainite region (925° to 575°F) is very little affected by the manner of cooling from the austenitizing temperature at 1600°F to 575°F)tothe upper limit of bainite transformation at 925°F; 2) starting time for the bainite transformation is the same order of magnitude for either isothermal transformation or continuous cooling, but the rate of transformation is somewhat greater for isothermal transformation; 3) tensile stress accelerates both isothermal and continuous cooling transformation, and 32,000 psi stress changes the form of the isothermal transformation diagram to correspond in appearance to the continuous cooling diagram; 4) transformation for nonlinear, continuous cooling may not be determined directly from the linear, continuous cooling transformation diagram, but may be predicted by assuming first that the fractional amount of austenite transformed in a given small temperature interval depends on the approximate linear cooling rate during that temperature interval and then by summing stepwise over the whole temperature range. IN a previous publication&apos; an X-ray spectrometer was described with which the X-ray diffraction from a specimen could be observed continuously under controlled temperature and tensile stress. This instrument has now been applied to a study of the austenite-bainite transformation in a Ni-Cr steel for both isothermal and continuous cooling conditions, with and without stress. Certain characteristics of the transformation lead to a method of predicting the amount of transformation to be expected at a given temperature for any type of cooling curve. Material and Specimen Preparation The steel chosen for the investigation was a Ni-Cr steel having the composition in the following percentages: 0.30 C, 0.27 Mn, 0.019 P and S, 3.50 Ni, and 1.25 Cr. In order to fabricate specimens suitable for the X-ray spectrometer, a 1/4 in. plate was ground down to 0.060 in. and then cold rolled to about 0.035 in. Next it was heat treated by quenching in oil from 1650°F and tempering at 1200°F for 1 hr. Then it was etched in dilute nitric acid to reduce its thickness to 0.014 in. and cut into blanks in the shape of flat tensile specimens 3 1/4 Vi in. long, 7/16 in. wide, with a notch % in. long and 7/32 in. wide; see Fig. 1. X-Ray Technique Since the X-ray spectrometer has been described in detail elsewhere,&apos; only a brief outline of the principles will be repeated here. A focusing, pow- der-diffraction arrangement&apos; was used, as shown schematically in Fig. 1, and the specimen was mounted vertically in a vacuum furnace (not shown in the figure). The X-rays, moving in a horizontal plane, enter and leave the furnace through beryllium windows. As shown in the figure, X-rays diverging from the line source A are diffracted by the specimen B and converge at the detector slit C. The detector D and the slit C may be set at the proper angle in the horizontal plane to receive X-rays diffracted by either the face-centered phase (austenite) or the body-centered form (ferrite, bainite, martensite). The specimen is heated by electrical conduction between connectors E, and E,, and a Pt—Pt-10 pct Rh thermocouple spot-welded to the center of the notched region on the side away from the X-ray beam indicates the temperature continuously on a Brown recorder. Temperature control is exercised manually with a variable transformer on the input to E,-E,. Any desired time-temperature relationship is easily obtained by first drawing the desired curve on the temperature recorder chart and then adjusting the variable transformer during the run so that the thermocouple

Jan 1, 1957

H. D. HIBBARD, Plainfield, N. J. (written discussion *).-While this valuable and timely paper may not go to the root of the matter, it deals with many of the elements and factors involved. It might be taken as the engineer&apos;s solution of the case, starting with the assumption that steel is steel, while the tendency for a rail to have transverse fissures may, and probably does, depend, in part at least, on conditions met before it reaches the track. Admitting with the author that "brittleness of fracture in all grades of steel is characteristic of fatigue tests" we may yet look farther back to find out, if possible, why some rails and some steels are more prone to have transverse fissures than others, for it has been found that rails from certain heats of steel developed these fissures under a service which

Jan 3, 1918

By A. J. W. Headlee

RECENT interest in germanium centers around its use as a semi-conductor of electricity in electronic devices. It is generally believed that germanium transistors, diodes, triodes, photocells, and rectifiers will largely replace the present-day vacuum tubes. The germanium electronic devices are much smaller, lighter, and more resistant to shock, and they require only a small fraction of current required for conventional devices. Hence only a small amount of heat is given off by the equipment. This development will require many times the quantity of germanium now being produced, which in 1948 was approximately 1000 lb1 and was obtained almost entirely from zinc ores in Missouri, Kansas, and Oklahoma. No one knows with certainty what the demand will be for germanium by 1956. It may be 40,000 lb.1 Known concentrations in zinc ores are not sufficient to

Jan 10, 1953

By Eugene P. Pfleider

RECENT interest in germanium centers around its use as a semi-conductor of electricity in electronic devices. It is generally believed that germanium transistors, diodes, triodes, photocells, and rectifiers will largely replace the present-day vacuum tubes. The germanium electronic devices are much smaller, lighter, and more resistant to shock, and they require only a small fraction of current required for conventional devices. Hence only a small amount of heat is given off by the equipment. This development will require many times the quantity of germanium now being produced, which in 1948 was approximately 1000 lb&apos; and was obtained almost entirely from zinc ores in Missouri, Kansas, and Oklahoma. No one knows with certainty what the demand will be for ger-manium by 1956. It may be 40,000 lb.1 Known concentrations in zinc ores are not sufficient to

Jan 1, 1954

By D. M. Jones

In May 1999 the first campaign of the BHP San Manuel flash smelting furnace (FSF) will be concluded after having set world records for both campaign length and tonnage smelted for an Outokumpu copper flash smelting furnace. This paper reviews planned process and equipment modifications including: The installation of a new 36,000 mt concentrate storage facility; replacement of the existing dryer electrostatic precipitator with a baghouse; modification of the FSF dry charge bin and feed system to achieve mass flow and uniform feed to the concentrate burner; modifications to the FSF and its ancillary cooling systems; modifications to the waste heat boiler and offgas handling system to increase gas handling capacity and improve process efficiency;- and improvements to the FSF fugitive gas collection system. A brief review of the planning and execution of the scheduled 45 day shutdown is also given.

Jan 1, 1999

Copper refining electrolytes are maintained in the range 60-65¦C to ensure an efficient operation. The heat energy required to meet these temperatures has been traditionally derived from the electrical energy required for the electrolytic process and supplementary steam energy. In 1983, experiments were conducted at Copper Refineries Pty. Ltd. (CRL) to determine the effects of insulating the Tank House cells, and fully covering the cells. The results of these experiments showed conclusively that greatly reduced steam consumption would be required to maintain electrolyte temperatures. These positive results led to an Energy Conservation Programme for the Tank House, and this was implemented in 1984. A computerised cell cover monitoring system was developed, and is used to control cell coverage and fluid balance. The experimental work and the benefits obtained since implementation of the programme are discussed.

Jan 1, 1985

By Marlos Henrique Alves Gomes

Aços resistentes ao desgaste são amplamente aplicados em partes estruturais que exigem propriedades como resistência mecânica, tenacidade e resistência ao desgaste abrasivo. O presente trabalho foi realizado devido à necessidade de desenvolvimento de materiais necessários para minimizar os efeitos causados pelo desgaste abrasivo. Os objetivos são: obter microestrutura multiconstituída (ferrita, bainita, martensita e austenita retida) por meio de tratamentos térmicos; e compará-la a microestrutura martensítica revenida. O aço estudado possui a seguinte composição química 0,26%C-1,13%Mn-0,92%Si-0,72%Cr- 0,29%Mo-0,18%Ni-0,17%Cu. Conduziu-se os tratamentos térmicos na sequência apresentada: recozimento subcrítico a 700°C, têmpera em óleo (temperatura de austenitização 940°C) e tratamento isotérmico de transformação bainítica (temperatura de austenitização de 820, 860, 900 e 940°C) ou recozimento subcrítico a 700°C seguido de têmpera/revenimento (940°C e resfriamento em água/250°C por 2 horas). Microscopia Eletrônica de Varredura (MEV) foi empregada para se avaliar a microestrutura do aço. Dureza Rockwell C foi utilizada com intuito de comparar a dureza das diversas microestruturas obtidas. Constatou-se que com a diminuição da temperatura de austenitização houve decréscimo do valor de dureza; e as amostras temperadas e revenidas demonstraram dureza média maior que as amostras que passaram por tratamento isotérmico de bainitização. A microestrutura multiconstituída foi obtida.

Aug 17, 2017

By R. C. Himes, K. Zanio, J. B. Wagner, J. W. Moody, J. F. Miller, W. Johnson

The recent research with which this paper deals has been concerned with the preparation of pure PbTe crystals suitable for control of radiative processes and othe.v electronic applications. The research has been directed toward the developrnent of methods for the preparation of puve, homogeneous, loul-ca,wier-density PbTe crystals suitable for use in the fabrication of optically pumped and electrically pumped diode lasers. Steps in the preparation of the crystals include 1) purification of the starting materials, 2) synthesis and purification of the PbTe, 3) growoth of PbTe crystals, and 4) adjustt~zertt of composition of the crystals This Paper describes the general preparation procedure employed and discusses some investigntiotzs of purification processes. THE as-received lead and tellurium are nominally 99.999 to 99.9999 pct pure. Assays furnished by the suppliers, obtained by emission spectrographic analysis, show only the presence of about 2 ppm Mg in the tellurium. Such analyses are not very informative, however, since they give no information on the concentrations of normally gaseous impurity elements such as oxygen. Both the lead and the tellurium in the as-received state usually contain appreciable concentrations of oxygen—primarily in the form of oxides on the surfaces of the material. To reduce the oxygen content, the lead is held in the molten state in hydrogen at -700°C for several hours. For this treatment, the lead is contained in a graphite boat which is rf-heated, and the hydrogen is passed through a liquid-nitrogen trap prior to use. Tellurium is subjected to multiple distillation in hydrogen to remove oxygen and other foreign impurities. If, in conducting the distillation, approximately the last 10 pct of the charge at each "stage" is left as the discard cut, purification of the tellurium proceeds as indicated in Fig. 1.l Tellurium used in this work has been distilled two or three times to reduce carrier concentration to about 10" per cu cm. The PbTe is prepared from the purified elements by reacting them in the molten state in sealed, evacuated, or hydrogen-filled silica ampoules. The charge is usually held above the melting point of PbTe (923°C) at 1000 C for 24 hr to ensure that it has been homogenized. Two methods have been employed for the growth of the required single crystals of PbTe: growth from the melt, which will be discussed first, and growth from the vapor phase. Large single crystals of p-type PbTe can be grown readily from the melt by the Bridgman method. For this method of crystal growth, the PbTe is synthesized in situ from proper proportions of the purified elements. Growth (dropping) rates in the range 1.3 to 6.5 mm per hr are employed. Material near the maximum melting composition (about 50.012 at. pct Te) is utilized to avoid composition change on freezing, and thus to obtain crystals of nearly uniform composition. Crystals prepared by use of procedures described up to this point were sufficiently pure and perfect that they could be used for the preparation of laser crystals in studies at Lincoln Laboratory.2-5 ADJUSTMENT OF COMPOSITION Good n-type crystals of PbTe cannot readily be grown from the melt. Further, growth from the melt of crystals of any compositions (n or p type) other than those near the maximum melting composition is difficult because of the large composition changes that must occur on freezing.&apos;" However, melt-grown crystals can rapidly be brought to other desired compositions by isothermal equilibration through the vapor phase with a two-phase Pb-Te stock material, essentially as described by Brebrick and Allgaier.1 The work to be discussed has been concerned with the preparation of n-type crystals; thus, the two-phase stock which was employed contained excess lead, and all ensuing discussion is of the preparation and properties of n-type crystals. The equilibration was designed to the shift composition to the lead-rich limit of stability at the selected temperature. Initial treatment of the crystals at high temperature was employed to minimize the total time required for the equilibration. Final adjustments of the composition and state of the crystals were made by use of low-temperature heat treatment at temperatures in the range 200" to

Jan 1, 1968

By F. Weinberg

Measurements have been made of solute segregation during dendrilic growth by using radioactive solute elements and ,measuring the activity of den(12-ites cut from decanted specimens. This has been done for both lead awl tin based binary alloys contaitzing the following solute additions: Ag, T1204, was dependet on ko, the equilibrium distribution coefficient in the following way Fay k &apos;c 0.1, C/C 0.6; for k0 >0.1. 0.6 <c,/c,< I. Qualitative obse?-vations were madc of dendritic segregation, by using autoradiographic techniques, for the Sn + Ag110 and Sn + Tlo4 systems. The observation were found to he in general agreement with the measurements ofCA/Co. Autoradiographic were also obtained of scctiolccl delzr11-iie stalks. These indicated that the stalks had a substructure, dclileated by solute corzetlt?atio?zs nlolg the substructure walls. A new dendrite growth direction <JI2> is reported for tila. SOLUTE segregation in dilute binary alloys has been investigated by Pfann,&apos; Smith, Tiller, and Rut-ter,&apos; and others. They considered the case of a slowly advancing plane solid interface, and derived expressions for the distribution of solute in both solid and liquid during solidification. To determine these expressions, they assumed no diffusion in the solid and either complete mixing in the liquid:&apos; or diffusion controlled solute movements in the liquid without any convective mixing.&apos; The present investigation considers solute segregation during dendritic growth, in which case the solid-liquid interface is not plane, and the growth rates are rapid. Segregation under these growth conditions has not been treated mathematically, because of the relative complexity of the system. It has been suggested by Chalmer, on the basis of preliminary results, that an alternative to the diffusion and heat flow controlled conditions during growth is &apos;diffusionless" dendritic growth in which solid is formed with the same composition as the liquid. He suggests this type of growth may depend upon a solvent-solute relationship that permits some solid solubility without excessive increase in internal energy, as is the case for solutions of tin in lead. On the other hand, Montariol,4 and others, have shown experimentally that some segregation does occur during dendritic growth in metals using etching and radioactive tracer techniques to indicate the concentrations of the solute. The present investigation was undertaken to determine, both qualitatively and quantitatively, the extent of solute segregation associated with dendritic growth in a series of binary alloys, as a function of solute concentration. PROCEDURE The solvent materials used were Vulcan Electrolytic tin (99.997 pct purity) and Tadanac lead (99.998 pct purity). The solute materials were Zn, Sn, and Sb (better than 99.998 pct purity), Ag and Co (99.5 pct purity), and T1 (Fisher "purified" metal sticks). Activation of the solute metals was carried out in the reactor at Chalk River, Canada. Master alloys were prepared by induction heating from the radioactive solute metal and the pure solvent, under argon, in graphite crucibles. Pieces of these alloys were then added to the solvent to give the required solute concentration. Dendrites were grown in essentially the same manner as that described by Weinberg and Chalmer, , in which controlled orientation single crystals were grown dendritically in horizontal graphite boats, and the liquid decanted. The crystals were grown and decanted in an atmosphere of tank argon. Before decanting, a sample of the liquid was drawn up in a glass tube and allowed to solidify rapidly. The orientations of the single crystals were such that <loo> was parallel to the growth direction, and (100) in the horizontal plane for lead, and [1101 and (110) respectively for tin. With these orientations long dendrite stalks formed along the bottom of the boat in the dendrite direction (<100> for lead and [I101 for tin) from which secondary branches grew. Only these secondary branches, which grew freely in the liquid from the dendrite stalk to the liquid surface, were used in the measurements. Accordingly, effects due to substrates and oxides on the surface of the liquid need not be considered. In order to measure the solute concentration C, of the dendrites, individual dendrite stalks were cut from the decanted specimens, remelted, and formed

Jan 1, 1962