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By F. F. Frick, Frederick Laist

In a leaching process, having obtained the copper in solution, the choice of the precipitation method is influenced by the following factors: 1. Availability of precipitant. 2. Adaptability to the leaching process. 3. Final product desired. 4. Regeneration of leaching solutions. 5. Fouling of solutions. There are three general classes of precipitation methods: 1. The use of iron, scrap or sponge. 2. Electrolytic deposition. 3. The use of some gas or reagent by which the copper is obtained, usually in the form of an intermediate precipitate which requires further treatment. For example, the precipitation of, the copper as Cu2Cl2 from chloride solutions; with SO2 gas. The use of iron is adapted to almost any process. It has the great advantage of extreme simplicity, and the recovery of the copper and any values present in a highly concentrated, easily treatable form. The disadvantages are the cost in isolated places, the uncertainty of the scrap-iron market, and the fouling of the leaching solutions. The latter is a serious factor, when a reagent such as salt is used in them, which makes necessary their re-use. Where applicable, electrolytic deposition is very attractive. The copper is obtained in a form directly marketable, there is a regeneration of acid and no fouling of solutions. Unfortunately, chloride solutions do not lend themselves to electrolysis. An entirely satisfactory anode material has not yet been discovered, although magnetite, apart from being rather brittle, seems to answer the requirements fairly well. The use of a method of the. third class is involved in many special

Jan 1, 1915

By P. H. Cardwell

The effect of various plastics upon the permeability of a sand and the mechanism of their ensuring permeability within the consolidated sand body is discussed. Data are presented on various properties of the plastic materials used in sand consolidation and the effect of temperature and usable temperature ranges are considered. The recovery of petroleum from uncon-solidated sands presents serious production problems, owing to sloughing of the formation. The solution of some of these problems usually has been by mechanical methods.' The ideal way of controlling the sloughing tendencies of these un consolidated formations, however, is to prevent the movement of the individual sand grains by the use of a bonding medium. A step in the desired direction was taken by Irons and Stcesser2 when they taught the use of liquid plastics to produce a consolidating deposit that prevents sloughing. More recently, Wrightsman and Buckley3 proposed a modification of this process. In this use of the liquid plastic, the sand grains become coated and the ensuing hardening of the plastic by polymerization or condensation cements together the sand Particles. Liquid plastics that have been suggested for this Purpose are of the following types: phenolformaldehyde, alkyd resins, vinyl type resins, polystyrene and the acrylic esters. When the flow of fluids through a sand must not be materially reduced, it is essential only to cement together the sand grains with liquid plastic and leave a portion of the interstitial space for fluid flow. TO be assured of obtaining fluid flow through the sand interstices after injection of plastic, it has been necessary in the past to remove the excess plastic from the interstices between the particles before it sets. Wrightsman and Buckley suggest two methods for the removal of the excess plastic from the interstices of the sand: (I) to flush the excess plastic back into the formation, away from the well bore, by use of oil or water; (2) to produce the well before the plastic has set, thereby moving the excess plastic into the well bore. Under certain well conditions it is very difficult to remove the excess plastic from all parts of the formation by either of these methods and leave the formation consolidated with no sections completely sealed. The method* described herein of retaining permeability within a sand body is to use a liquid plastic that upon setting ensures permeability within the consolidated sand body. This cements the sand grains but obviates the need for removing plastic from the interstices of the sand. One of the ways of accomplishing this is to use a liquid plastic that occupies a considerably greater volume than the solidified resin it yields on further polymerization or condensation in situ. In order to be satisfactory, the volume of the plastic while liquid should be at least one and one half times the volume of the solid formed. Preferably,

Jan 1, 1947

By P. H. Cardwell

The effect of various plastics upon the permeability of a sand and the mechanism of their ensuring permeability within the consolidated sand body is discussed. Data are presented on various properties of the plastic materials used in sand consolidation and the effect of temperature and usable temperature ranges are considered. The recovery of petroleum from uncon-solidated sands presents serious production problems, owing to sloughing of the formation. The solution of some of these problems usually has been by mechanical methods.' The ideal way of controlling the sloughing tendencies of these un consolidated formations, however, is to prevent the movement of the individual sand grains by the use of a bonding medium. A step in the desired direction was taken by Irons and Stcesser2 when they taught the use of liquid plastics to produce a consolidating deposit that prevents sloughing. More recently, Wrightsman and Buckley3 proposed a modification of this process. In this use of the liquid plastic, the sand grains become coated and the ensuing hardening of the plastic by polymerization or condensation cements together the sand Particles. Liquid plastics that have been suggested for this Purpose are of the following types: phenolformaldehyde, alkyd resins, vinyl type resins, polystyrene and the acrylic esters. When the flow of fluids through a sand must not be materially reduced, it is essential only to cement together the sand grains with liquid plastic and leave a portion of the interstitial space for fluid flow. TO be assured of obtaining fluid flow through the sand interstices after injection of plastic, it has been necessary in the past to remove the excess plastic from the interstices between the particles before it sets. Wrightsman and Buckley suggest two methods for the removal of the excess plastic from the interstices of the sand: (I) to flush the excess plastic back into the formation, away from the well bore, by use of oil or water; (2) to produce the well before the plastic has set, thereby moving the excess plastic into the well bore. Under certain well conditions it is very difficult to remove the excess plastic from all parts of the formation by either of these methods and leave the formation consolidated with no sections completely sealed. The method* described herein of retaining permeability within a sand body is to use a liquid plastic that upon setting ensures permeability within the consolidated sand body. This cements the sand grains but obviates the need for removing plastic from the interstices of the sand. One of the ways of accomplishing this is to use a liquid plastic that occupies a considerably greater volume than the solidified resin it yields on further polymerization or condensation in situ. In order to be satisfactory, the volume of the plastic while liquid should be at least one and one half times the volume of the solid formed. Preferably,

Jan 1, 1947

By Reuben B. Ellestad, Fremont F. Clarke

Lithium chemical plant extraction methods are discussed with reference to 1) base exchange with alkali sulphates; 2) processing based on roasting with lime; 3) miscellaneous methods; and 4) application of the Lithium Corp. process to extraction of lithium from run-of-mine, low grade spodumene ore, or concentrates. IN the early days of the lithium industry most of the production was from lepidolite, zinnwaldite, and amblygonite. Nearly all the early extraction processes described in the literature involve heating the finely ground mineral with sulphuric or hydrochloric acid. On subsequent water leaching most of the bases present in the mineral (especially aluminum) are dissolved as sulphates. As a result, the leach solution required extensive chemical purification before the lithium could be precipitated as carbonate. Following the remarkable growth of the lithium industry to its present size, zinnwaldite and amblygonite ores must be considered of minor importance only. Attention is now focused on spodumene, abundant enough in North America to be a major source of supply, and there are important supplies of lepidolite and petalite in Africa. The extraction processes described below all apply to spodumene, although several will also operate on other lithium minerals, such as petalite. Base Exchange with Alkali Sulphates: A distinct advance was made with the disclosures of Wadman and von Girsewalt. In these methods the finely ground silicate ore (spodumene or lepidolite) is intimately mixed with an excess of alkali sulphate (usually K2SO4) in at least a 1 to 1 proportion, and the mixture was heated to a relatively high temperature. Base exchange results, with the formation of lithium sulphate. A water leach dissolves the lithium sulphate, together with the excess potassium sulphate. Successful operation of this type of process requires very thorough grinding and mixing, as well as careful temperature control. The use of K2SO4 is objectionable from cost considerations since purification of lithium carbonate requires the use of potassium carbonate, if the K2SO4 is to be recovered and recycled. The lower solubility of K2SO4 as compared with Na2S04 is also objectionable, since it limits the concentration of the Li2SO4 solution to be precipitated by K2SO4. Early laboratory-scale investigation of this process by Lithium Corp. was not encouraging. Other related base exchange processes are those of Lindblad, Wallden, and Sivander3 and Sivander, Gard, Villestad, and Wallen4. The former covers the reaction of lithium silicate minerals with a sodium sulphate solution, at 100" to 300°C (under pressure), while the latter involves the extraction of silicate minerals with molten sodium sulphate. Both these processes would seem to be difficult and expensive to operate.

Jan 1, 1956

By D. O. LIVINGTON

(Presented by invitation at a meeting of the Spokane Local Section of the institute, Feb. 17, 1912.) THE Pilares de Nacozari mine is located in Sonora, 75 miles south of Douglas, Ariz. The town of Douglas is on the International Boundary and is the place at which the ores from the Bisbee mines are smelted. The Moctezuma Copper Co. owns the mines at Nacozari, and the copper-concentrates shipped to the Copper Queen smelter, at Douglas, make a good smelting-mixture with the Bisbee ores. The Moctezuma Copper Co. and the Copper Queen smelter at Douglas, as well as the railroad from Douglas to Nacozari, are owned by the Phelps Dodge Co. The ore-deposit occurs in the form of a large ellipse with a major axis of approximately 2,000 ft. and a minor axis of about 600 ft., the major axis bearing about 90 W. of N. The whole of this ellipse is more or less mineralized; the surface being principally an iron gossan with some occasional copper-stains. Below the oxidized zone, which is not more than 50 ft. deep, the minerals are pyrite and chalcopyrite, with occasional seams of chalcocite, the latter being rare. There appears to be no well-marked zone of secondary enrichment, the oxidized gossan over the greater part of the deposit changing suddenly to what is apparently the original unaltered ore. The copper-values are concentrated around the perimeter of the ellipse, and it is principally around this perimeter that the mining is done. The ore mined averages a little more than 3 per cent. of copper, with a small amount of silver, less than an ounce per ton. Some ore of considerably higher grade than this has been shipped, however, but the above average is of the mill-run. The ore is wider near the two ends of the ellipse than along the sides, and is mined in some cases to a width exceeding 200 ft. The country-rock for the first vertical 500 ft is a volcanic acid breccia, probably rhyolitic; below

Sep 1, 1912

Jan 1, 1944

By A. Singh, W. M. Fleming, J. J. Santana, A. E. Torma

The present study investigated the extraction of uranium from a low-grade ore by sulfuric acid and the removal of radium from the leach residues by brine solutions. The optimum leaching conditions were found to be 1.5 mole [£]-1 H2SO4, 6.Og[9]-1NaClO3, 75°C,50% pulp density and 750 rpm with respect to the rate of uranium extraction. The maximum theoretical attainable rate of uranium extraction was determined to be V = 1.09 x 10 -2 mole [¢]-1h-1 with respect to pulp density. The order of reaction was found to be zero regarding the effect of sodium chlorate concentrations. The apparent activation energy of uranium extraction was calculated from the Arrhenius plot to be [A]E a - 2.36 kcal mole-1 (9.87 kJ mole-1). Based on a statistical design, an empirical equation has been developed describing the rate of uranium extraction with the leaching parameters. This equation can be used to generate data which may be useful for scaling up the process to pilot plant level. The most efficient brine solution for the extraction of radium - 226 from the leach residue was found to contain one mole[f] -1 CaCl2 and 0.01 mole [2] -1 HC1. The two step leaching with this solution resulted 87% removal of radium from the leach residue. On the basis of this study, a flow-sheet has been proposed for the extraction of uranium and radionuclides from the ore and leach residue to yield almost innocuous tailings.

Jan 1, 1982

By Harlan W. Nelson, James B. Purdy

A study of data obtained during laboratory tests to determine the suitability of bituminous coals for use in residential underfeed stokers of the clinkering type has led to the following general conclusions: 1. Performance data obtained during the test furnish useful and practical information upon which to judge the performance of stoker coals. 2. Conclusions derived from the results of evaluation tests are in general agreement with use experience of the coals in the field. The method is of practical use in this regard. 3. Few direct relationships were found between data furnished by the evaluation test and determinations by standard laboratory tests. This is particularly true with regard to coke formation and clinker formation, two of the most important factors in determining the degree of satisfaction to be obtained in applications of the small underfeed stoker. It has not been the intention in this paper to prescribe this evaluation test as the best method for the evaluation of coals for use in residential stokers. That there are other test methods having similar objectives serves to point out the necessity for full-scale laboratory tests. At the present time, a standard test procedure for the evaluation of coals for use in residential stokers is not available. For the past several years a joint committee, appointed from the membership of the Residential Stoker Committee of Bitulninous Coal Research, Inc., and from the Engineer- ing and Research Committee of The Stoker Manufacturers Association, has been working to develop a standard procedure for testing and evaluating bituminous stoker coals. This procedure has been completed to the extent that it has been drawn up in tentative form. It is now planned to install the equipment in several laboratories and to run check tests, using portions of identical lots of coal, to determine the degree of reproducibility offered by the method. Completion of this standard test procedure should greatly facilitate the evaluation of coals for use in residential stokers. Acknowledgments The cooperation of coal operators sponsoring the coal evaluation tests, in granting permission to use data and results from their tests, is gratefully acknowledged. Acknowledgment is also made to Carroll F. Hardy, Chief Engineer, Appalachian Coals, Inc., for his interest and timely suggestions on the preparation of this paper. Special thanks are due to Ralph Sherman, Assistant Director, Battelle Memorial Institute, who was largely responsible for development of the evaluation procedure, for helpful suggestions and advice. References I. H. A. Sherman: The Evaluation of Coal for Use in Domestic Stokers. Univ. of Ill., Eng. Experiment Station, Circular No. 39 (1939). 2. . Q. Shotts: The Relation of Free- swelling Indexes to Other Characteristics of Some Alabama Domestic Stoker Coals. TP 2314, Coal Tech., (Feb. 1948); Trans. AIME (1948) 177, 502. 3. . J. Helfinstine and C. C. Boley: Correlation of Domestic Stoker Combustion with Laboratory Tests and Types of Fuels 11. Combustion Tests and Preparation Studies of Representative Illinois Coals. Ill. State Geol. Survey, Re1. of Zntlestigations No. 120 (19467 ) p. 35. DISCUSSION E. R. Kaiser*—AS a former fuel engineer assigned to residential stokers at Battelle, the writer has read with considerable interest the paper by Messrs. I'urdy and Nelson. It is gratifying to note that earlier test techniques have been developed and that criteria found important in the years 1935 to 1938 are still important in judging the performance of stoker coals for residential heating. The authors have plotted a number of the primary coal data singly against performance data of the stoker in an effort to establish relationships. Unfortunately, wide scattering of points usually resulted, which did not illustrate what experience generally indicates to be the case. For example, Fig 3 indicates almost no trend in the percentage of released ash converted to clinker with change in ash-softening temperature. Other factors, such as fuel bed temperatures and zones of heat release must have influenced the results. In the present state of our knowledge, we cannot explain all of the reasons why suitable stoker coals perform satisfactorily, nor why one satisfactory coal may be better than another. It would therefore

Jan 1, 1950

By H. Bernstein

Grain coarsening tests were carried out on AI-4.5 pct Cu and AI-4.5 pct Si alloys. The effects of three variables, melt composition, pour temperature, and mold temperature, were determined. It was found that the macrostructure generally coarsened with increased pour and mold temperatures. Coarsening was extreme in the unrefined alloys but was retarded by the active grain refiners like titanium and columbium. The effect of boron was spectacular in suppressing coarsening tendencies. The results of the investigation support the carbide theory of nucleation as opposed to the peritectic theory. A REVIEW of prior work on the subject of grain refinement in the light metals indicated that, for the most part, it had been concerned with the positive effects of addition agents upon structure. This work produced various theories of refinement. Prominent among them were the peritectic theory and the transition element carbide theory. Certain inadequacies in the former theory appeared to be explained satisfactorily by the transition element carbide theory. In order to appraise these theories further, a study was undertaken of the permanence of grain refinement effects when subjected to thermal or chemical variations. It was considered that a study of this kind would be of practical value, since the light metals are exposed to thermal and chemical variations in the normal course of foundry operations. Accordingly, two alloys of commercial importance were selected for this investigation, the A1-Cu and A1-Si alloys. Experimental Procedure and Results Raw Materials: The base alloys, A1-Cu and A1-Si, were prepared from virgin aluminum and hardeners, induction melted, and pigged for remelting. The grain refiners, including titanium, columbium, zirconium, and boron, were added as master alloys. Analyses of the raw materials and base alloys are listed in Table I. Melting and Casting Practice: The metals were melted in clay-graphite crucibles in a Hevi-Duty pit-type resistance furnace, equipped with a Leeds and Northrup Micromax Recorder and Controller. After melt down of the base alloys, the additions were made. For each casting, approximately 80 grams of metal were poured into a preheated graphite mold held in a transite flask. The mold (Fig. 1) weighed 320 grams. To determine the effect of superheat upon structure, a set of melts was heated successively to four temperature levels, 705°, 775°, 845°, and 915°C, and test specimens were cast at each level. Prior to each pour, the furnace temperature was held constant for 20 min. Next, a set of melts was put through a superheat cycle and test specimens were cast at melt temperatures of 705" and 915°C successively. The crucibles then were cooled in air to 705°C as deter-mined by immersion thermocouple and additional test specimens were poured. The cooling interval was approximately 1 min. Another set of melts was furnace cooled with the cover slightly ajar and test specimens cast as before. The interval in this case was 15 to 20 min, varying with the superheat temperature. The mold temperature for all these tests was 400°C. To determine the effect of cooling rate without superheat upon structure, a set of melts was heated to 705°C, and castings were poured at mold temperatures of 205", 400°, and 540°C. An interval of 15 min elapsed between each pour. Mold temperatures were measured by a direct reading millivolt-meter, using a chromel-alumel thermocouple located at midwall thickness of the mold. To demonstrate the phenomenon of chemical coarsening, agents such as chromium and beryllium, which had acted as coarseners in a previous investigation,' were added to the A1-Cu alloy. Test speci-

Jan 1, 1955

By E. C. Pechin

THE Lucy furnace, owned by Messrs. Carnegie, Kloman & Co., and located on the Alleghany River, on the outskirts of Pittsburgh, is a splendid modern furnace, 75 feet high, and 20 feet bosh. She had been working well on low grade ores of about 50 per cent., producing daily 68 to 75 tons. There was on stock 500 tons of Republic ore, one of the purest and best of the Lake Superior ores, averaging over 68 per cent. of iron, which had been procured for the purpose of making a trial for Bessemer iron. This was charged by itself, and Mr. Skelding, the founder, reports that he did not succeed in getting a single cast when it came down, before the furnace chilled from the hearth to the top of the boshes, some 25 feet. Every effort was made to save her, without avail, and the disagree-

Jan 1, 1874

By M. J. Pool, P. J. Spencer

Using liquid tin as the solvent metal, the heats of solution of silver and gold in dilute Ag-Au-Sn alloys have been determined at 723°K by solution calorimetry. From the values obtained, the various enthalpy interaction coefficients in the liquid solutions have been calculated. The self-interaction coefficients Au and Ag values of 2413 and -6322 cal per g-atom in binary Au-Sn and Ag-Sn alloys, respectively. For an alloy containing 0.04 mole fraction Ag, Au is equal to 2443 cal per g-atom, and in an alloy containing 0.04 mole fraction Au, Ag has a value of —8883 cal per g-atom. Ag Au has been determined as —2650 cal per g-atom. ADDITION of a second solute to a dilute binary alloy may cause striking changes in the thermodynamic characteristics of the alloy. As yet, such influences cannot be reliably predicted and it is only by accumulation and critical assessment of data that definite patterns can be established. Solute interactions in dilute solutions were first treated mathematically by Wagner,1 who derived expressions for the Gibbs energy interaction coefficients. For an alloy consisting of. two dilute solutes, i and j, in a solvent s, these coefficients are given by: where yi is the activity coefficient of component i and x represents the mole fraction of solute or solvent. Other interaction coefficients have since been established in terms of the various partial molar thermodynamic properties of an alloy; the definitions of these are summarized in a recent paper by Lupis and Elliott.2 Mathematical and experimental studies of such coefficients have received much attention recently, providing a very useful theoretical background to an understanding of the nature of solute interactions taking place in dilute solutions. One of the definitions to arise from such work has been the extension of Wagner's treatment by Lupis and Elliott4 to include an enthalpy interaction coefficient, defined as. where ?Hi is the relative partial molar enthalpy of component i. ?Hi is related to the relative partial molar enthalpy at infinite dilution, ?Hio, and to the enthalpy interaction coefficients by the expression: Values of ?Hi can often be obtained with a high degree of accuracy by calorimetry, and, if the composition of the alloy is carefully controlled by making calculated solute additions throughout a series of measurements, application of Eq. [2] will enable reliable enthalpy interaction coefficients to be determined. Partial heats of solution must be investigated as a function of solute concentrations down to xi = 0, and, since ? values are obtained from the slope of mi plotted against x, great care must be taken to obtain precise data. The data for binary systems which are presently available often require extrapolation of ?Hi values from compositions as great as xi = 0.05 or even 0.1 to obtain limiting heats of solution. Reliable enthalpy interaction coefficients are thus impossible to obtain from published data for most of the alloy systems already investigated. The aim of the present work was to determine values of Au, Ag, Ag, and Au in the limit xsn -1 for the relatively simple Ag-Au-Sn system and from these results to gain some insight into the possible influence

Jan 1, 1969

By Edmund C. Pechin

The Lucy furnace, owned by Messrs. Carnegie, Kloman & Co., and located on the Alleghany River, on the outskirts of Pittsburgh, is a splendid modern furnace, 75 feet high, and 20 feet bosh. She had been working well on low grade ores of about 50 per cent., producing daily 68 to 75 tons. There was on stock 500 tons of Republic ore, one of the purest and best of the Lake Superior ores, averaging over 68 per cent. of iron, which had been procured for the purpose of making a trial for Bessemer iron. This was charged by itself, and Mr. Skelding, the founder, reports that he did not succeed in getting a single cast when it came down, before the furnace chilled from the hearth to the top of the boshes, some 25 feet. Every effort was made to save her, without avail, and the disagree-

By R. L. Doan

WHEN the Plutonium Project was started in the spring of 1942 there was no technology to produce uranium metal of the required purity. Not only was there no such metal available; no one knew how to make it or fabricate it after it was made. Since this time vast technical effort has been ex-pended in the atomic energy field. A short 15 years later the metallurgy of uranium is probably better known than that of any other metal, with the possible exception of steel. At the beginning of the 1942 drive to obtain pure uranium metal the most available raw material was black uranium oxide (U3O8) of about 92 pct purity from the Great Bear Lake region of Canada. It took only three months for the project chemists to develop a process for bringing the purity of this oxide up to 99+ pct and another three months for Mallinckrodt Chemical Co. of St. Louis to build the purification plant and get it into operation. In early summer of 1942 the purified brown oxide (UO2) started moving to the Metal Hydrides Co. in Beverly, Mass., and to the Westinghouse Research Laboratory in Bloomfield, N. J., both of which had been granted Government contracts to try to make pure uranium metal.

Jan 9, 1957

By John Hall

(New York Meeting, October, 1913.) THE Fremont test for measuring the energy consumed in breaking a notched bar of steel is not so well known in this country as it deserves to be. The test specimen used in this test is about 3/8 by 1/4 by about 11/4 in., notched with a hack saw on the lower side to cause the piece to break at a fixed point. A weight of 10 kg. falling 4 m., and provided with a knife or. chisel which strikes the specimen, breaks the test piece by impact. The residual force in the falling weight after it has broken the specimen is recorded by a suitable device, and the difference between the total energy and the residual energy of the weight (in kilogrammeters) is the force consumed in breaking the specimen. An experience of several years with the Fremont testing machine has shown its great value in readily detecting brittleness not revealed by tensile testing or slow bending testing. In this paper it is proposed to discuss (1) the supersensitiveness of the test as applied to cast steel and (2) its value in revealing the effect of heat treatment under certain conditions.

Jan 7, 1913

Jan 1, 1941

By General Meigs

I do not know that I can do any more than to express my entire concurrence in the views which have. been already expressed by Mr. Macdonald. It appears to me that he has we over the wholz subject. I might add in regard to appealing to the Govern-

Jan 1, 1882

By M. E. Grimes

Rio Algom Mines Ltd. owns eight uranium mines and mills in the Elliot Lake district of Ontario, seven of which were producing before 1960. At present only one mine is operating and meeting current contract requirements. Under present economic conditions, it is not feasible to mine ore of less than 2.0 lb per ton U3O8, although there are very large reserves below this grade, Rio Algom is interested in preconcentration for three possible applications: to extend ore reserves by permitting use of lower grade ore, to reduce costs on processing of present grade ore, and to reduce capital investment in expanding production to meet future production goals. Rio Algom has been investigating various applicable preconcentration processes since the early 1950s to date, on laboratory and pilot-plant scale. Methods investigated include gravity concentration by sink-float, high intensity wet magnetic separation, flotation of uranium, flotation of acid consumers, and a number of electronic sorting methods including radiometric, photometric, and conductimetric. No method tested has yet been satisfactory under Rio Algom's criteria of uranium recovery and cost, principally because uranium loss has been too high for a useful weight rejection. Metallurgical results of the preconcentration test work and the economic assessment therefrom are reviewed.

Jan 1, 1974

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.'" 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. E. Bash

WHENEVER electric and open-hearth steel men discuss the relative advantages of their respective methods, the question of temperature is always discussed, so that this paper is written in the hope that definite data may settle some of the questions and encourage further investigations along these lilies. The writer has had the opportunity of taking the tapping temperatures of steel from electric furnaces of different sizes in various plants and from a number of open hearths handling the same kind of steel. All temperature measurements were made with the same disappearing-filament type optical pyrometer and the corrections for emissivity applied were those worked out by Burgess,1 which are 0.40 for steel streams and 0.65 for slag. The correction is applied by calculating the curve giving the relation between the true and apparent temperature in the following formula: Log E = CZ log e( 1 _ 1 x \T2 T1) in which E = emissivity; C2 = 14,500; e = base of Napierien logarithms; ? = wave-length of light used = 0.65/4; T2 = true temperature, in degrees absolute; T,1 apparent temperature, in degrees absolute. The curve showing the relation between true and apparent temperature for steel and slag arc given in Fig. 1. For the purpose of comparison of open-hearth and electric furnaces, there are given in Table 1 the tapping temperatures of two 25-ton Heroult electric furnaces and one 6-ton with one 50-ton acid, one 40-ton basic, and one 65-ton acid open-hearth furnace, all making nickel ordnance steel for guns. The two 25-ton Heroult electric furnaces were finishing steel refined by the triplex process and the 6-ton Heroult finished steel that was partly refined in an open hearth.. In this table, the tapping temperature and the temperature of the steel stream into the first ingot

Jan 9, 1919

By C. Feng, P. Levesque

HE addition of rhenium to molybdenum is known to produce alloys with good workability.&apos; Lawley and Maddin found that the critical stress for twinning in this system was lowered by the addition of 35 pct Re, which suggests that twinning may re- place the usual slip operation as the major element of deformation. The twinning elements in bcc Mo-Re alloys have been reported as the (112) planes and the <111> directions.3 This note represents the continuation of this investigation, in which the authors found that the occurrence of twinning promotes the formation of a bcc tetragonal phase, previously identified as u by Greenfield and Beck.4 Specimens of Mo-35 pct Re alloy, prepared as described previusly, were solution annealed at 2400o, cooled to room temperature, and plastically deformed by compression to induce twinning. After subsequent aging for 8 hr at 1300°C, traces of a were observed along the grain boundaries and at the interfaces between the twins and the matrix, Fig. 1. With increased aging time the cr phase grew into larger clusters and finally occupied the entire twinned area, Fig. 2. Experiments also indicated that if twinning did not precede aging, there was no visible evidence of a in the microstructure.

Jan 1, 1962