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By Jean A. Andre

In 1969 "Société des Mines et Fonderies de Zinc de la Vieille-Montagne" produced 221,000 tons zinc ingots and 22,000 tons zinc dust, thus rating highest on the world's zinc producer list. The Company's plant at Balen, Belgium, with an output of 135,000 tons electrolytic zinc is the most important one of this group; it is an integrated metallurgical zinc and lead unit with recovery of most by-products. The present paper describes the zinc production facilities. The roasting section includes four fluid bed roasters (total concentrates charged: 740 tpd) and two sulfuric acid having a corresponding capacity. Calcine is leached in a fully automated plant by a two-step continuous process. Leaching residues, mixed with lead furnace slag, are treated in a shaft furnace. The recovered zinc fume is leached separately. In the near future, the leaching residues are to be treated by a wet process, developed in the Company's own laboratories. Purification of solutions is accomplished in two steps: antimony and zinc dust are added in the first one, only zinc dust in the second one for removal of cadmium. Electrolysis cells are partly of a conventional type. A new type of cell configuration was put onstream in October, 1969, planned output 60,000 tpy. Main features of the new cell rooms are the fully automatic pulling, stripping and replacing of the jumbo-size cathodes (immersed area 2.6 m2). Zinc cathodes are remelted in induction furnaces followed by in-line automatic casting and stacking machines.

Jan 1, 1970

By W. L. Remick

The hydrotator coal-cleaning process was developed as an economic necessity to meet the ever-increasing demand for an inexpensive method of cleaning coal down to the sizes ordinarily referred to as "dust." As the most urgent demand seemed to be in the anthracite field, all experimental work has been conducted in that territory during the past two years, with the exception of a few months during the strike of 1925-26, when some experiments were performed in the Alabama bituminous fields. The first commercial plant was constructed at the Middle Creek Colliery of the Philadelphia & Reading Coal & Iron Co.,. Pottsville, Pa. This plant is now operating. Application The field of application of the process is: 1. Cleaning anthracite fines, ordinarily described as "slush" or "silt." Slush contains all sizes from 3/32 in. down to and including I(dust." (Anthracite passing a 3/32-in. mesh is also referred to as No. 2 Barley and No. 4 Buckwheat.) 2. Cleaning sizes too fine for recovery by other methods. 3. Removal of coal from sand circulated in the Chance sand-flotation process. 4. Cleaning of bituminous sizes from % in. down to "dust." 5. As equipment for the performance of the froth flotation process. 6. Other separating, extraction and washing processes which may be considered outside the realm of coal cleaning. Principle of Operation Fig. 1 shows the method of classification practiced under the Hydrotator patent.' In coal cleaning the machines are operated as "hindered settling" classifiers, the flow of solids and liquids being so controlled that the units may be combined in series.

Jan 1, 1927

F. E. Thompson, Pottstown, Pa.: If Mr. Webster's endeavor to open up the subject of cast-iron should prove as prolific of results as did the discussion on " The Physics of Steel," he must certainly feel richly repaid. His remarks concerning the secretiveness and conservatism of the average foundry-man recall to my mind an instance of a blast-furnace which, for the last year, has been producing much foundry-iron. The manager, believing that much more of his product could be used in the foundry than the foundry-men were will-

Jan 1, 1896

L50 Adirondack L1 Alaska L2 Arizona L58 Arkansas L66 Billings Petroleum L3 Black Hills L4 Boston L5 Carlsbad Potash L6 Central Appalachian L60 Central New Mexico L7 Chicago L8 Cleveland L9 Colorado L57 Colorado Plateau L10 Columbia LII Connecticut L55 Dallas L12 Delta L65 Denver Petroleum L13 Detroit L14 East Texas L15 El Paso Metals L71 Evangeline L45 Florida L54 Fort Worth L16 Gulf Coast L61 Hobbs L62 Hugoton L68 Illinois Pet Basin L17 Kansas L18 Lehigh Valley L52 Lou-Ark L47 Mexico L19 Mid-Continent L20 Minnesota L56 Mississippi L21 Montana L22 Nevada L64 Niagara Frontier L23 New York L67 New York Petroleum L25 North Pacific L24 North Texas L26 Ohio Valley L27 Oklahoma City L28 Oregon L63 Panhandle L29 Penn -Anthracite L30 Permian Basin L51 Peru L31 Philadelphia L32 Pittsburgh L33 St Louis L34 San Francisco L59 San Joaquin L35 Southeast L36 Southern Calif L69 Southern Calif Pet L53 South Plains L37 Southwest Texas L48 Southwest Alaska L38 Southwest N Mex L44 Spindletop L39 Tri-State L40 Upper Peninsula L41 Utah L70 Venezuela L42 Washington, D C L43 Wyoming L49 West Central Texas L46 Philippine

Jan 1, 1956

Jan 1, 1947

Jan 1, 1947

By AIME AIME

ON Sept. 24, 1875, a remarkable deposit of silver ore was discovered by James Ryan and Samuel Hawkes at the east base of Grampian Hill in central Beaver County, Utah.. A shaft was begun and had been sunk about 30 ft. in ore when the claim was sold on Feb. 17, 1876, to A. G. Campbell, Matthew Cullen, Dennis Ryan, and A. Byram for $25,000. To them is due the credit of having developed the mine and started the district on the road to its present state of prosperity. Their development resulted in proving the vein to a depth of over 280 ft. and about 2500 tons of ore was extracted and turned into bullion. In February, 1879, the mine came into the possession of the Horn Silver Mining Co., and since then over $65,000,000 worth of ore has been taken from the mine. Two smelters were built in 1878, near the mine; 400 men were employed underground, and 1000 on the surface, burning charcoal, hauling wood from the surrounding hills, and freighting and hauling hay for the hundreds of horses used in the work. Ore was hauled thirty miles to the

Jan 1, 1936

By Edward Griffith

The anthracite industry, which produces about 50 million net tons of coal annually, has been talked of as being able to last for another century; but if the water record of the past century continues into the expected century, this expectation of many years production still to come out of the remaining reserves will not be attained. The industry will be a submerged one in fact as well as in name. A recorded forecast of what has since occurred appears on page 34 of the Mine Inspectors' reports of 1897: It should also be noticed that bodies of water had accumulated in parts of abandoned mines before duplicate surveys of the same were required by law; and as a result we have today to contend with bodies of water, the exact location and position of which are not correctly known. Since that date, 47 years ago, the implications of the foregoing comment have grown enormously. This is shown in Fig. I and in the following table showing flooded and partially flooded areas that have come into existence since the early 1930's in the northern anthracite field: Number of Year Flooded Areas 1932...................... 2 1933...................... 3 1934..................... 3 1935...................... 5 1936...................... 7 1937...................... 9 1938.................... 11 1939...................... 11 1940...................... 11 1941...................... 14 1942...................... 14 1944...................... 26 Similar conditions exist in other fields in the anthracite region. In the period between 1923 and 1940, abandonment of collieries in the southern field resulted in the flooding of approximately 60 sq. miles (30 per cent) of the field. The ahandonment of collieries in this field has imposed additional expense for pumping on the collieries still operating. This condition will be aggravated by the extension of developments and cause suspension of operations if economic conditions do not justify the assumption of additional pumping costs. During the years, the region's rainfall has not altered, but the quantity going inside the mines through breakages in the surface, brought about by extraction of the coal, has increased materially, as indicated by the ratio of tons of water pumped to tons of coal produced underground for one of the large companies in the northern anthracite field: Year Ratio 1920................. 8.4:1 1925.................. 10.6:I I930.................. II.4:I 1935................. 26.2:1 1940.................. 32.7: I 1942.................. 30.3:I The data in Table I shows the total amount of water pumped and its ratio to underground production for one of the large companies in the southern anthracite field, and shows a rapidly growing serious situation. Rainfall quickly affects the workings in all the fields. In mine inspection district 7 of the southern field the rainfall in 1935 was 92,083,000,000 gal. The total water pumped was 36,274,000,000 gal. (39.4 per cent of the rainfall). The operating mines

Jan 1, 1947

By Edward Griffith

The anthracite industry, which produces about 50 million net tons of coal annually, has been talked of as being able to last for another century; but if the water record of the past century continues into the expected century, this expectation of many years production still to come out of the remaining reserves will not be attained. The industry will be a submerged one in fact as well as in name. A recorded forecast of what has since occurred appears on page 34 of the Mine Inspectors' reports of 1897: It should also be noticed that bodies of water had accumulated in parts of abandoned mines before duplicate surveys of the same were required by law; and as a result we have today to contend with bodies of water, the exact location and position of which are not correctly known. Since that date, 47 years ago, the implications of the foregoing comment have grown enormously. This is shown in Fig. I and in the following table showing flooded and partially flooded areas that have come into existence since the early 1930's in the northern anthracite field: Number of Year Flooded Areas 1932...................... 2 1933...................... 3 1934..................... 3 1935...................... 5 1936...................... 7 1937...................... 9 1938.................... 11 1939...................... 11 1940...................... 11 1941...................... 14 1942...................... 14 1944...................... 26 Similar conditions exist in other fields in the anthracite region. In the period between 1923 and 1940, abandonment of collieries in the southern field resulted in the flooding of approximately 60 sq. miles (30 per cent) of the field. The ahandonment of collieries in this field has imposed additional expense for pumping on the collieries still operating. This condition will be aggravated by the extension of developments and cause suspension of operations if economic conditions do not justify the assumption of additional pumping costs. During the years, the region's rainfall has not altered, but the quantity going inside the mines through breakages in the surface, brought about by extraction of the coal, has increased materially, as indicated by the ratio of tons of water pumped to tons of coal produced underground for one of the large companies in the northern anthracite field: Year Ratio 1920................. 8.4:1 1925.................. 10.6:I I930.................. II.4:I 1935................. 26.2:1 1940.................. 32.7: I 1942.................. 30.3:I The data in Table I shows the total amount of water pumped and its ratio to underground production for one of the large companies in the southern anthracite field, and shows a rapidly growing serious situation. Rainfall quickly affects the workings in all the fields. In mine inspection district 7 of the southern field the rainfall in 1935 was 92,083,000,000 gal. The total water pumped was 36,274,000,000 gal. (39.4 per cent of the rainfall). The operating mines

Jan 1, 1947

By T. S. Lundy, J. I. Federer

Chemically purified Zr95and Cb95 have been used in determining self-diffusion coefficients in the bcc phase of iodide zirconium over the temperature range of 900o to 1750°C. The temperature dependence of the diffusion coefficients could not be described by the usual Arrhenius-type equation over the entire temperature range. Values of the apparent frequency factors (D0)a and activation energies (Q)A for ZR95 varied from 4.8 x 10-6 to 2.5 x 10-2 sq cm per sec and 20,700 to 46,900 cal per mole, respectively, between 900°and 1750°C. Similarly, for Cb95, values of (Do) a and (Q)A varied from about 2.4 x 10'5 to 0.25 sq cm per sec and 26,500 to 56,800 cal per mole, respectively. The data may be described in terms of the a to ß transition temperature of 1136 °K and the absolute temperature of the diffusion anneals by the following eauations: SEVERAL studies on the diffusion of Zr95 in zirconium have been reported.1"5 The values of the constants contained in the usual Arrhenius-type equation for describing the temperature dependence of the diffusion coefficient, D = Do exp [- Q/(RT)], are summarized in Table I. The reported values of Do, the frequency factor, and Q, the activation energy, are seen to vary by factors of about 60 and 1.6, respectively. Examination of the data from any one study indicated reasonable consistency of measurements. The large discrepancies of over-all results, therefore, cannot be explained on the basis of experimental scatter. One possible explanation for the differences in results could be a varying impurity content of the zirconium. Another possibility is that the radioactive daughter, Cb95, influenced the values of some of the determined diffusion coefficients. Therefore, the first of the three purposes of this study was to reconcile the large differences in diffusion results that have been obtained. Several empirical relations have been proposed to relate the diffusion coefficients in solids with physical properties, such as the absolute melting point, the heat of fusion, and the heat of sublimation.

Jan 1, 1963

By B. E. Field

Cobalt is a silvery white metal with a slight bluish cast. It strongly resembles nickel in its appearance and properties, notably its resistance to corrosion, although its alloys with other metals differ decidedly in their properties from those of nickel. The name "cobalt" was derived from the German Kobold, meaning goblin, and this came to be applied to the cobalt minerals which, although they resembled ores, did not readily yield metal when smelted by the primitive processes available in the Middle Ages. Cobalt minerals were used as pigments by potters and glass workers before the Christian era. Cobalt blue glass was found in the tombs of the Egyptians and in the ruins of Troy, and many colors used by the ancient Greeks and Romans contained cobalt. The ancients were entirely unaware that the colors they used were caused by cobalt and the metal itself was not isolated until about the middle of the eighteenth century, by Brandt, although the preparation of cobalt compounds had been carried on in a small way ever since the opening of the silver-cobalt deposits at Schneeberg, Germany, in 1470.

Jan 1, 1935

By Edward Judd

CONSTRUCTION of the long projected Moffat tunnel, on the Denver & Salt Lake R. R., between Tolland and Irving, Colorado, is now actually and actively progressing. This 6.1-mile bore through the Rocky Mountains, at an elevation of about 9200 ft., will eliminate 33 1/3 miles of probably the most tortuous standard-gage track in the world, and at the same time will avoid the necessity for crawling over the snow-bound continental divide at an elevation of 11,660 ft Completion of the tunnel within the stipu-lated four years, is expected to nave an immediate effect on the develop-ment of the known coal fields in north-western Colorado, already penetrated at Craig, the present terminus of the road, while it will also enable the railroad to carry out the original designs of its founder, David H. Moffat, for through traffic from farther west. The intention now is to accomplish the latter object by an extension from McCoy following the canon of the Grand River down to a connection with the Denver & Rio Grande at Dotsero. Legal impediments to the financ-ing of the tunnel having been removed by action of the Colorado legislature in April, 1922, the Moffat Tunnel Improvement District issued bonds to the amount of $6,720,000 which have been widely and quickly distrib-uted through a New York banking house. Responsi-bility for the execution of the project has been vested in the Moffat Tunnel Commission, to which a board of consulting engineers has been appointed for carrying out the details of administration. This board includes D. W. Brunton and L. D. Blauvelt, of Colorado, and J. Vipond Davies and J. Waldo Smith, of New York; R. H. Keays, who has managed large tunnel projects in New York, is chief engineer for the Commission.

Jan 11, 1923

Jan 1, 1967

Jan 1, 1967

By F. Habashi

Conclusive evidence is given showing that the dissolution of gold in cyanide solution follows mainly the over-all equation A similar equation can also be written for the dissolution of silver. Theoretical derivation of the velocity equation for this reaction has been obtained, which describes quantitatively the experimental facts. The equation is as follows: where [CN-] and [O2] = the concentrations (in moles/ml) of cyanide and dissolved oxygen, respectively. DcN- and Do2 = the diffusion coefficients of cyanide and dissolved oxygen; 1.83 x 10-5 and 2.76 x 10-5 cm2 sec-1, respectively. A = the surface area of the metal in contact with the aqueous phase, in cm S = the thickness of the boundary layer; varies between 2 and 9 x 10-3 cm, depending on the speed and method of agitation. Rate being expressed in g. equiv. sec-1. INTRODUCTION During recent years a number of papers have been published on the kinetics of dissolution of gold and silver in cyanide solution.1,6 The authors agree that the rate of dissolution is diffusion-controlled, but disagree regarding the mechanism of the reaction. Some authors'-3 support the Bodlander equations: The apparently conflicting results, when critically reviewed, are concordant and lead to the conclusion that the proper equation for the dissolution reaction should be only Eq. 1. This conclusion is based on the following facts: 1) For every 2.2 equivalents of metal dissolved one mole O2 was consumed. 2) For every 1 equivalent of metal dissolved, 2 moles of cyanide were consumed.' 3) Hydrogen peroxide is formed during the dissolution of gold or silver, and for every 2.2 equivalents of metal dissolved, one mole H2O2 was produced.1,2 The fact that Kudryk and Kellogg4 did not detect H2O2 during the dissolution of gold should not throw doubt on the many affirmative reports of other investigators. Lund2 has shown that depending on the crystalline nature of the silver surface, (e.g. method of etching the sample) H2O2 may undergo catalytic decomposition heterogeneously according to: Further Kudryk and Kellogg4 carried out their experiments in the presence of 0.5% KC1 to achieve a greater electrolytic conductivity, and Matsudaira7 has shown that H2O2 is catalytically decomposed (homogeneously) in the presence of C1- ion in alkaline solution. 4) Experiments carried out by Boonstra8 and Lund2 showed that the dissolution of gold and silver respectively in KCN + H2O2 in the absence of oxygen was a slow process. Thus the reaction takes place to a minor extent only. Further kinetic studies showed that: 1) The rate of dissolution depends on the surface area of the metal in contact with the liquid phase, thus indicating that the process of dissolution is a heterogeneous process. 2) The rate of dissolution depends on the speed of stirring,5,6 thus indicating that the process is controlled by a physical phenomenon.

Jan 1, 1967

By R. S. Kinasevich, D. D. Crabtree, D. W. Fuerstenau, T. P. Meloy, A. L. Mular

The effect of such variables as feed size, particle shape, cleavage, and hardness on the relative proportion of impact, abrasion, and chipping events in a tumbling mill is demonstrated. The concept of an average event, which is a combination of the three comminution mechanisms, is introduced. It is postulated that the average event in a particular mill determines not only the size distribution but also the energy-size reduction relationship for the comminution process. Fragmentation of particles in tumbling mills appears to result from a combination of impact, abrasion, and chipping grinding.' The relative rates of size reduction attributable to any of the basic grinding mechanisms must depend upon a number of variables, such as feed size, particle shape, hardness, and the number and kind of particles in the mill. The purpose of this paper is to show experimentally how these variables in the properties of materials affect the size distributions obtained by grinding the material's in a laboratory tumbling mill. The resulting size distributions will be intetpreted in terms of a combination of three comminution mechanisms. METHODS AND MATERIALS In this study, minerals of widely differing properties were ground either separately or as mixtures in laboratory mills using rods or balls for grinding media. The materials used include quartz, Tuolomne, limestone (99.8% CaCO3), barite, corundum, galena, pyrite, glass beads, and crushed glass. The mill used was 8 in. in diam. and 9-1/4 in. long. For the ball milling tests, 17.6 kg of steel balls (36: 7/8 in. balls, 178: 1 in. balls, and 44: 1-1/8 to 1-1/4 in. balls) were used. For the rod milling experiments, 17.6 kg of steel rods 9-1/16 in. long (25: 5/8 in., 10: 3/4 in., and 5: 7/8 in. in diam.) were used. In each test, 1 kg of solids were ground wet at 60% solids at 77 rpm. In all cases except where otherwise specified, the feed to the mill was 4 x 8 mesh material. Size distributions of the ground products were determined by a wet-dry sieving procedure with Tyler series sieves. Size distributions of mixed products containing limestone were determined by dissolving the limestone with acid and sizing the residue. EXPERIMENTAL RESULTS AND DISCUSSION If the size distribution of the product from a tumbling mill depends upon the relative proportion of impact and attrition (abrasion and chipping) events, altering the grinding conditions may change these proportions and consequently alter the size distribution of the product. Data to illustrate this point can be taken from Gaudin's classic 1926 paper.2 In one series of experiments, Gaudin ground quartz of different initial sizes for four hours in a laboratory ball mill with 7/8-in. balls. In Fig. 1, his data are reproduced as the cumulative fraction finer than the stated size for the following initial feed sizes: 13.3 x 9.4 mm, 6.7 x 4.7 mm, 2.6 x 1.6 mm, and 0.83 x 0.59 mm. As the feed size was decreased, a dramatic change in the shape of the size distribution curves took place, even though the amount of minus 100-mesh

Jan 1, 1964

By Harold Margolin, W. R. Hibbard, R. W. Fenn, H. P. Moore

Deformation lines, also called etch markings or strain markings, are non-effaceable lines developed in individual grains by etching a metal specimen which has been cold worked sufficiently to cause atomic non-conformity or slight orientation differences within the grains. Etching occurs more rapidly at these lines of high chemical reactivity to produce a result similar to that revealing grain boundaries. Wider etching effects forming bands have been found. They are believed to be bands of deformation lines which form areas of measurably different orientation from the crystal matrix. The crystallite rotations causing these bands have been shown by Barrett2 to contribute to deformation textures. Although deformation lines have been observed in many metals, the amount of deformation requireti for their appearance has been established only in general terms. Mathewson and Phillips3 observed the first appearance of deformation lines in cold-rolled alpha brass at about 20 pct reduction in thickness using the standard ammonium hydroxide hydrogen peroxide etchant. Price and Davidson4 noted defor- mation lines in common high brass after 26.5 pct reduction by cold rolling using the same etchant. Johnson6 observed dark thick forklike lines in 99.99 pct pure copper reduced 31.8 pct. Adcock6 observed deformation lines in 80-20 copper-nickel alloy rolled 50 pct. Samans7 found no deformation lines in alpha brass single crystals cold rolled 9.5 pct but they did appear after 25 pct reduction using ammonium hydroxide and hydrogen peroxide etchant. Barrett and Levenson8 observed deformation bands in drawn polycrystalline iron at very small reductions in area and noted that their initial appearance perhaps depends on grain size and other conditions. They reported deformation bands in a single crystal of iron reduced 6 pct by drawing. Brickg noted that deformation lines in 70-30 brass apparently associated with I I I I ) planes appeared after reductions of from 20-50 pct by cold rolling. Brick and Williamson10 noted that in single crystals of 70-30 alpha brass "as in polycrystalline brass, no deformation markings appeared until reductions exceeded 20 pct." Cook and Richards" reported that in Copper cold rolled less than about 50 Pet few strain markings were apparent but for higher reductions many strain markings appeared transverse to the rolled direction. In a review article Brick and Phillips12 noted that previous studies had not shown deformation lines in cold rolled alpha brass below 20 pet reduction and added that 4

Jan 1, 1949

By H. P. Moore, R. W. Fenn, Harold Margolin, W. R. Hibbard

Deformation lines, also called etch markings or strain markings, are non-effaceable lines developed in individual grains by etching a metal specimen which has been cold worked sufficiently to cause atomic non-conformity or slight orientation differences within the grains. Etching occurs more rapidly at these lines of high chemical reactivity to produce a result similar to that revealing grain boundaries. Wider etching effects forming bands have been found. They are believed to be bands of deformation lines which form areas of measurably different orientation from the crystal matrix. The crystallite rotations causing these bands have been shown by Barrett2 to contribute to deformation textures. Although deformation lines have been observed in many metals, the amount of deformation requireti for their appearance has been established only in general terms. Mathewson and Phillips3 observed the first appearance of deformation lines in cold-rolled alpha brass at about 20 pct reduction in thickness using the standard ammonium hydroxide hydrogen peroxide etchant. Price and Davidson4 noted defor- mation lines in common high brass after 26.5 pct reduction by cold rolling using the same etchant. Johnson6 observed dark thick forklike lines in 99.99 pct pure copper reduced 31.8 pct. Adcock6 observed deformation lines in 80-20 copper-nickel alloy rolled 50 pct. Samans7 found no deformation lines in alpha brass single crystals cold rolled 9.5 pct but they did appear after 25 pct reduction using ammonium hydroxide and hydrogen peroxide etchant. Barrett and Levenson8 observed deformation bands in drawn polycrystalline iron at very small reductions in area and noted that their initial appearance perhaps depends on grain size and other conditions. They reported deformation bands in a single crystal of iron reduced 6 pct by drawing. Brickg noted that deformation lines in 70-30 brass apparently associated with I I I I ) planes appeared after reductions of from 20-50 pct by cold rolling. Brick and Williamson10 noted that in single crystals of 70-30 alpha brass "as in polycrystalline brass, no deformation markings appeared until reductions exceeded 20 pct." Cook and Richards" reported that in Copper cold rolled less than about 50 Pet few strain markings were apparent but for higher reductions many strain markings appeared transverse to the rolled direction. In a review article Brick and Phillips12 noted that previous studies had not shown deformation lines in cold rolled alpha brass below 20 pet reduction and added that 4

Jan 1, 1949

By F. R. Morral

INDUSTRY has yet to find a universal solution to the problem of engineer personnel selection. Today, the choice of the right man for the right job is even more pressing than ever before. The age of the hard apprenticeship seems to have passed. In its place one finds the interviewer who must determine through personal contact and evaluation of college grades whether a graduate engineer will fit into his company's scheme. The problem, as it is constituted today, may be broken into four parts: Need for better use of human resources (there is a shortage of engineers, scientists, and skilled workers), productivity with higher efficiency, encouragement of personal pride in work performed, and employee's happiness on the job and away from it.

Jan 4, 1953

By Martin Rubenstein

CdS crystals have been grown from a number of metallic solvents such as bismuth, tin, lead, and cadmium. Etching studies have shown that plastic deformation occurs if the crystals are not removed from the solvent prior to the solidification of the solvent, on cooling. The deformed crystals show a umique exciton fluorescence as a function of edge dislocation density. If one grows the CdS in the eutectic alloy of the above four metals (commonly called Wood's metal) the crystals can be removed from the solvent with hot water and no plastic deformation occurs. In this paper, the liquidus solubility measurements of CdS, as a function of temperature, are presented. The data were obtained using a high -temperature filtration technique. CADMIUM-SULFIDE crystals have been grown from a number of metallic solvents1 such as cadmium, bismuth, tin, and lead. Liquidus solubilities of CdS in cadmium,2 bismuth,3 and tin4 have already been measured. Crystals of CdS, in all four metals, have been grown by solution growth: 1) by cooling a saturated solution and 2) by a solution transport method.1'"1 CdS crystals grown in these four solvents have a few characteristics in common: 1) 1.8°K photolumines-cent emission consisted mainly of the radiative recombination of the bound exciton commonly known as I,, 2) slip lines which could easily be seen by the naked eye, and 3) edge dislocation densities in the order of l05 per cu cm.1 It was decided that these slip lines and the high edge dislocation densities were caused by a plastic deformation of the CdS crystals. It was felt that this plastic deformation did not occur during the growth of the crystals nor during the cooling of the solution, but did occur when the solvent which was in contact with the crystals froze. If these assumptions were valid, the slip lines and the high number of dislocations could be reduced or eliminated by removing the crystals from the solvent before the solvent froze. Since crystals of CdS had already been grown separately in such solvents as bismuth, lead, tin, and cadmium, it was felt that crystals could be grown in a eutectic mixture of these four metals. In this work a eutectic (or near eutectic) mixture of bismuth, lead, tin and cadmium in the proportion 50, 26.5, 13.5, and 10 wt pct, respectively, was used to grow CdS crystals. Such a mixture has a melting point of about 70°C and is close in composition to the alloy commonly known as Wood's metals. If the crystals could be grown from this mixture of solvents, and if hot water (>75°C) could be used to separate the crystals of CdS from the metallic solvent, it was hoped that CdS crystals could be grown with little or no plastic deformation which had been ob- served when crystals were grown from these solvents uncombined. CdS crystals were grown from this low melting eutectic mixture of bismuth, lead, tin, and cadmium using the solvent transport method. CdS powder and the appropriate amount of metals were sealed in a quartz tube under a pressure of about 5 X 10-6 torr. This ampule was then placed in a vertical position in a furnace. The temperature was raised to about 900°C. The furnace was designed so that the top of the liquid column within the ampule was between 10° to 40°C higher than the bottom of the liquid column. These temperatures were measured on the outside of the quartz ampule. The ampule was maintained at temperature for 7 to 14 days (depending on the temperature at which transport was taking place) and then the furnace temperature was lowered until the temperature was about 125°C. The ampule was then removed from the furnace, placed in water maintained at about 90°C, and opened in this 90°C environment. The crystals could then be removed from this two-phase liquid (Wood's metal and water) by mechanically picking them out. Alternatively, the crystals could be quantitatively removed by adding an excess of mercury to the mixture of metals, crystals, and hot water. The hot solution of metals and the hot water could be evacuated using a small diameter tube connected to a vacuum. Small amounts of mercury and water could be removed by heating the crystals in vacuum. Crystals prepared using this technique showed no evidence of slip. However, some of these crystals did show edge dislocation densities as high as l04 per cu cm. Some few selected crystals showed no dislocations. Single crystals of CdS were grown as large as 5 by 5 by 0.5 mm. The ampules for the growth of these crystals were 13 mm O.D., 11 mm I.D., 150 mm! LIQUIDUS SOLUBILITY MEASUREMENTS The CdS starting materials was G.E. 118-8-2 powder which was fired in H2S at 1000°C, and then a vapor transport technique5 was applied to produce a "sound" mass of CdS. The Wood's metal was prepared by weighing out bismuth, lead, tin, and cadmium in the proportions of 50, 26.5, 13.5, and 10 wt pct, respectively. The bismuth, cadmium, and lead were from the American Smelting and Refining Co. (ASARCO) and all had purities of 99.999+ pct. The tin was 99.9999 pct spectroscopic grade from the Vulcan Materials Co. The appropriate mixture was placed in a quartz tube, evacuated to a pressure of 5 X 10-6 torr, melted to a liquid, cooled to room temperature under this same vacuum. This ingot was then placed in another quartz tube, evacuated to 5 x l0-6 torr, and sealed off under vacuum. The ampule was then horizontally placed in a furnace. The temperature was raised to 600°C, and over a period of several hours the ampule was vigorously shaken several times. The ampule was then removed from the furnace, and the metallic liquid was

Jan 1, 1970