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By D. D. Lambert, E. C. Simmons

Rare earth element (REE) analyses of cumulus plagioclase from the PGE ore zone of the Stillwater Complex indicate that pressure fluctuations in the magma chamber acting on a single magma cannot be responsible for features such as the reappearance of Mg-rich olivine on the liquidus. The data are more consistent with a model involving multiple injection and mixing of geochemically distinct magmas. The PGE-bearing sulfides of the J-M Reef are associated with such a reappearance of olivine, indicating that the unusual location of the ore zone may be related to the addition of new magma, compositionally distinct from magmas that produced cumulates in the Ultra- mafic zone of the complex.

Jan 1, 1984

By James M. Winston

When I began my career (the first assignment was mucking the "drainage" ditch) an experienced miner told me, "Remember son, happiness is a journey, not a destination. . . ." If you missed the 100th Anniversary of AIME in New York this year, you are missing the journey. There are not enough superlatives to describe the event. Especially since New York is "known to have it all." An Indefinable Plus There was a little something different at this meeting. I cannot explain what, but there seemed to be more of everything. There were more wives there this year-what a pleasure to see all the lovely women mingling through the conference- which was reflected through our own attire and mannerisms. In fact, everyone looked so great, we checked to see if it really was a convention of miners. You wives keep coming to all of the events, because so much is added by your presence.

Jan 1, 1971

By AIME AIME

ONE unique distinction can be claimed by the new Chairman of the Coal Division, C. E. Lawall: he is the only A.I.M.E. member also a university president, though several engineering colleges are headed by Institute members. Only last year he was promoted from director of the school of mines to president of West Virginia University, following a term as acting head of that institution of over 3000 students. He was born in Catasauqua, in eastern Pennsylvania, on Nov. 21, 1891, and went to Lehigh, receiving an E.M. in 1914, and an M.S. seven years later. His engineering career began in the Pittsburgh Testing Laboratories. After three years there he came to Palmerton for

Jan 1, 1940

The Institute of Metals Division and the American Foundrymen's Association will meet in Philadelphia Sept. 29 to Oct. 4. Many things of interest to the members of the Institute have been constructed and developed in the Philadelphia district since the last meeting in that city (1907), including the great plant at Hog Island, the new foundries at the League Island Navy Yard and the great foundries of the Westing-house Company at Essington. Invitations are being extended to foundrymen and industrial engineers generally in. England, France, Belgium, Italy, and other European countries, South American countries and Australia, to attend this convention, since the time. seems unusually opportune for holding a meeting of international scope.

Jan 5, 1919

By Ken Sublette

The mining industry has been a leader in the application of ultrasonic level monitoring systems, utilizing the "sonar-in-air" concept for the accurate inventorying of material not only as an end within itself, but going on to activate alarms, turn off feeders, operate tripper systems, and totalize the inventory in numerous bins as well as other more sophisticated applications. The virtues of ultrasonic level monitoring are no doubt appreciated by most users. However, to be of maximum service to the expanding mining industry, the manufacturer must be fair in pointing out ultrasonic's limitations as well as its virtues. The limitations can be surmounted with new technology and through a proper understanding of the principles of operation and application.

Jan 6, 1974

By D. G. Westlake

Resistance was measured as a function of temperature, 77° to 350°K,for niobium with hydrogen concentrations up to 3.76 at. pct. Cooling curves exhibited a discontinuity in slope that was attributed to the initiation of hydride formation. A thermal hysteresis was explained in terms of diffusion and the effects of mechanical constraint on nucleation and growth. The heat of solution of hydrogen in saturated Nb-H solid solution was 2. 737 * 0.045 kcal per g-atom, including an unknown stress contribution. The critical ternperatures for hydride formation during cooling and for embrittlement are correlated but not coincident. This, too, has been explained in terms of mechanical constraint and stress-itlduced tratzsfomtation. Nb-H alloys undergo a ductile-brittle transition with decreasing temperature.'-3 Similar behavior has been noted for v-H.1,5 For the latter system, there is evi-dence6 suggesting coincidence of the temperature of minimum ductility and the critical temperature T, for initiation of metal hydride precipitation during cooling. A decrease in ductility due to the presence of brittle hydride particles is readily explainable. The fact that ductility begins to decrease at some temperature higher than T,4,5 has led us6 to suggest that precipitation may be strain-induced locally during tensile testing. Wood and Daniels' have reported that a plot of temperatures for 10 pct reduction in ductility vs hydrogen concentration in niobium is not coincident with, but parallels, the solvus.7,8 They believe this indicates a correlation of precipitation and embrittlement. Unfortunately, the two reported solvuses 7,8 to which Wood and Daniels refer are not in agreement with each other. Furthermore, neither solvus was determined experimentally: each was a plot of calculated solubilities. Thus. neither is highly dependable for determining whether embrittlement coincides with initiation of hydride precipitation. Longson 9 studied phase relations in the Nb-H system between 77° and 473°K by dilatometry. Comparison with metallographic observations convinced him that discontinuities in the slopes of his dilatometric plots were coincident with the initiation of hydride precipitation. Plotting the logarithm of the hydrogen concentration vs the reciprocal of the temperature at which precipitation was initiated during cooling, he obtained a straight line shown in Fig. 1. Walter and chandler,'' using X-ray techniques to detect the for mation of a second phase? have obtained three experimental points in the temperature range 295° to 338°K which fall within Longson's experimental error for this plot. A similar plotg of temperatures at which dissolution was completed during heating was a parallel line shifted toward higher temperatures. A straight-line plot was obtained, also, for the temperatures of the ductile-brittle transitions,9 but it was shifted toward still higher temperatures. Longson calculated an activation energy of 2.980 * 0.300 kcal per mole for the hydrogen embrittlement mechanism, compared with 3.180 * 0.400 kcal per mole for hydride formation. Despite this agreement, he concluded, "It seems unlikely that embrittlement results from hydride formation..." because hydrogen embrittlement was observed at temperatures above the solvus. It is our contention that embrittlement is correlated with precipitation of the hydride.6 Because only Longson has investigated Nb-H phase relations at sub-ambient temperatures, we deemed it advisable to re-determine the temperature dependence of the solubility using the resistometric technique already proven successful for the V-H system.6 Coincidence of our solvus with temperatures for embrittlement would

Jan 1, 1970

By E. M. Tory, P. T. Shannon

An analysis of batch and continuous thickening in terms of the movement of planes of constant concentration (i.e. continuity waves) is presented. Use of solids flux as a primary variable greatly facilitates the analysis and clarifies the relationship between batch and continuous thickening. An "ideal" slurry is defined as one whose settling rate is a function only of the local solids concentration. An analysis of continuous thickening of this ideal slurry in an ideal thickener explains many aspects of the steady — and unsteady — state behavior of real slurries, such as the main features of a thickener's "solids profile" (including the break attributed to rake action), the sudden appearance at abnormally high feed rates of a zone of constant concentration and the velocity with which it rises, and the effect of detention time at constant weight of sludge per unit area. Where deviations exist, they are explained in terms of the batch settling behavior of real slurries. The purpose of this paper is to interpret continuous thickening phenomena in terms of batch settling behavior. Both types of thickening may be considered as the process of propagating concentration changes, due to the downward movement of the solids, from the bottom of the settling vessel upward through the slurry.' These concentration changes may be either finite or infinitesimal as in the case of the propagation of a continuous concentration gradient. The slurry itself may be moving downward as in the case of continuous thickening. The downward velocity of the slurry may be such that the concentration changes being propagated up from below remain stationary relative to the thickener walls. This is the case for steady-state thickening. It seems appropriate to analyze continuous thickening in terms of the movement of planes of constant concentration. This has already been done for batch settling."3 Although our main interest is in real slurries, there are certain aspects of both types of settling which can be deduced from a theoretical analysis of highly idealized systems. To this end, an "ideal slurry" is defined as one for which the dimensionless settling rate at any point is a function only of the local solids concentration.1,2 An "ideal thickener" is one in which there is no radial variation in either the solids concentration or in the downward component of slurry velocity. The underflow outlet is a point sink. It is to be expected that the behavior of non-ideal systems will deviate in some measure from theoretical results. However, the same characteristics which cause deviations in continuous thickening should be evident in batch settling, permitting a rational explanation of the former in terms of the latter. PREDICTED RESULTS FOR AN IDEAL SLURRY IN AN IDEAL CONTINUOUS THICKENER General Theory: In continuous thickening, the downward solids flux (mass/area-time) relative to the thickener, G, results from two different

Jan 1, 1967

By A. A. Watts, R. I. Jaffee, F. C. Holden, H. R. Ogden

Hypoeutectoid Ti-Cu alloys are responsive to heat treatment, and considerable variation of mechanical properties may be produced by transformation of the ß phase. Control of cooling rate, isothermal transformation, or quench tempering determine the transformation structure and properties. The transformation products are similar to those of carbon steel. THE equilibrium diagram for the Ti-Cu system has been studied by various investigators, and the most recent diagram is that determined by Jou-kainen, Grant, and Floe.' The titanium-rich portion of this diagram is reproduced in Fig. 1. The alloy compositions and annealing temperatures used in this work are shown. The Ti-Cu alloys containing up to 17 wt pct Cu are representative of an active eutectoid alloy system. Joukainen et a1.l have stated that ß phase cannot be retained on quenching and this has been confirmed in the present work. The similarity between the Ti-Cu system and the Fe-C system is evident and, as will be shown later, many of the transformation products appear to have similar microstructures. Heat treatments in this program were designed to produce the structures of primary interest for study and determination of mechanical properties. Experimental Procedures Preparation of Alloys: Five ½ lb ingots, ranging in composition from 0.8 to 6.83 pct Cu, were prepared by double arc melting in an atmosphere of high purity argon. Titanium melting stock was obtained from high purity iodide titanium, and copper additions were made from copper wire clippings. Segregation was reduced by inversion melting, in which the once-melted ingots were inverted in the crucible and remelted. The double-melted ingots were forged at 1600°F to ¾ in. diam rods, with both heating and forging operations being carried out in air. Surface scale was removed by grit blasting and grinding, after which the forgings were vacuum annealed at 900°C. The alloys then were swaged to ¾ in. diam rod at 750°C and test specimens were cut from this material. The vacuum annealing operation was to remove dissolved hydrogen, which is commonly present in the iodide titanium as-received. Although vacuum fusion analyses were not obtained for all these alloys, past experience indicates that the 6 hr treatment with a limiting pressure of 10- to 10-5 mm of Hg is sufficient to reduce the hydrogen level to 10 to 30 ppm. Vacuum fusion analysis of the 0.8 pct Cu alloy showed 19 ppm of hydrogen. In addition to the five hypoeutectoid alloys, three 15 g ingots were prepared with nominal copper additions of 9, 10, and 11 pct. Fabrication procedures were similar, except that these alloys were rolled to 0.040 in. sheet. Microstructure specimens only were obtained. Table I shows analyzed compositions and fabrication temperatures for these alloys. Heat Treatments: All heat treatments were made in potentiometer-controlled, resistance-wound tube

Jan 1, 1956

By William Loblowitz

A simplified system of flotation testing has been developed recently at the Bureau of Mineral Research of Rutgers University. The technique involves the known principle of skin flotation and can be used with minute quantities of sample and reagents in a beaker. A vessel containing the conditioned sample with added water and flotation reagents is held inclined and rotated slowly. Water-repellent particles come in contact with air and float on the surface of the liquid, while wettable particles are submerged. The float is poured off and filtered whereas the nonfloat remains in the beaker. The filtrate may be returned to repeat the process. This procedure can be made quantitative. Separations are obtained and are remarkably complete and repeatable. The effect of different reagents, optimum quantities, pH and other variables can be determined in a fraction of the time required for conventional testing. However, the method gives no information on the effect of frothers and the quality of froth to be expected in a cell, and it is not practical for particles finer than 200-mesh. Unlike other preliminary tests, separate float and nonfloat products are obtained, and their contents can be determined quantitatively by chemical analysis or grain counts. After the optimum reagent combination has been determined, the effect of fines and frothing may be verified in the conventional flotation cell. On the other hand, agglomeration-tabling can be directly duplicated from beaker tests. Procedure: Five to ten grams of sample are weighed into a 100-ml beaker. Flotation reagents and a small initial quantity of water are stirred together; additional water is then added to produce the proper water-solids ratio. The beaker is then tilted to 45" and rotated slowly. After three to five rotations, liquid and float are poured off and filtered; the filtrate may be recycled until the separation is completed. One test generally requires less than 10 min. Reagent concentration and pH remain quite constant because of the recycling of the filtrate. Two to four tests may be made simultaneously, and the effect of varied conditions may be observed by comparison. Considerable time is saved in preparation and handling since small quantities of sample suffice for a series of systematic tests. Repeatability One test was repeated four times under constant conditions. The sample used was a quartz sand containing approximately 24 pct feldspar and some clay aggregates. The +28-mesh grains had been screened out, and most of those finer than 100-mesh had been removed by hydraulic classification. The results are presented in Table I. For comparison, 500 g of the sample were separated by agglomeration-tabling using the same reagent combination and quantities as given in Table I. The weight percent float was 18.3 pct, composed almost entirely of feldspar and with only traces of quartz. Most of the remaining feldspar was recovered in a middling product with 2.2 pct by weight.

Jan 1, 1952

By John Chipman, Helen Towers

DEVELOPMENT of a simple radioactive tracer technique for measurement of the diffusion coefficient of calcium ion in liquid slag has already been reported. The investigation was of a preliminary nature designed to explore the possibilities of using radioactive isotopes and to establish a method, and no great accuracy was claimed for the results. It was shown, however, that Ca15 could be used successfully, and the values obtained for the diffusion coefficient appeared to be of the right order of magnitude. However, it was considered that a better technique could be devised for carrying out the diffusion. The experiments were, therefore, continued to find a more accurate method, to check the calcium results, and to extend the investigation to include measurements of the diffusion coefficient of silicon in the same slag. There were two flaws in the original technique. Convection was the cause of too many failures, and the interface between the two slags in the diffusion cell was curved rather than plane, probably due to a surface tension effect caused by the addition of the tracer Ca45 in the form of chloride. Two methods of overcoming these defects were tried. Since it was planned to study diffusion of the short-lived isotope Si"' also, the development of methods was restricted to those which gave promise of being reasonably rapid. Method 1—The principle was identical to that previously used with respect to the diffusion conditions, but there were three differences in technique. Temperature control was more rigid, the tracer was added to the slag as Ca45O rather than the chloride and, finally, an effort was made to translate to high temperatures the elegant method developed by Cohen and BruinV or bringing together the two liquid layers and beginning the diffusion. A master slag was melted in graphite, ground to a fine powder, and analyzed (38.5 pct Ca0-20.9 pct Al2O3-40.5 pct SiO2). The tracer was received as Ca45C12 in an aqueous solution of CaC12 + HC1. From this, calcium oxalate was precipitated, ignited to calcium oxide, and added as such to the slag to give an activity of approximately 5 µc per g. The mixture was then melted into the form of a cylinder 3/16 in. diam and about 1 in. long. A solution identical to the tracer solution without Ca45 was given exactly the same treatment. The resulting Ca40O was mixed with that slag which was to form the tracer-free half of the diffusion cell, and this was likewise melted into a cylinder of the same size. Slag cylinders, two with and two without Ca15, were set in graphite blocks as shown in Fig. 1, and the crucible was lowered into position in the fur-

Jan 1, 1958

By Robert Glass Cleland

[PHELPS DODGE COPPER PRODUCTS CORPORATION OFFICE, 40 WALL STREET, NEW YORK 5, N. Y. OFFICERS Whipple Jacobs President Howard T. Brinton Vice-President Edgar P. Dunlaevy Vice-President Weightman Edwards Vice-President S. Allan Jacobs Vice-President]

Jan 1, 1952

[E. E. SCHUMACHER, Chairman ARTHUR PHILLIPS, Past-Chairman L W. KEMPF, Senior Vice-Chairman E. A. ANDERSON, Vice-Chairman H. A. MALONEY, Treasurer FRANK T..SISCO. Secretary 29 West 39th Street, New York 18, N. Y.]

Jan 1, 1946

By David H. Browne

One of the most difficult problems in the chemistry of iron-ore, and one, the solution of which, so far as I am aware, has never been attempted, is the distribution, throughout a given vein, of Bessemer ore, and its relation to the formation of the deposit. In those hematite-mines in which both Bessemer and non-Bessemer ore occur, the sorting of the ore as it lies in the deposit becomes a problem of much economic as well as scientific interest. It would seem, from a superficial examination. or, indeed, from any examination not conducted for this especial purpose, as if high- and low-phosphorus ores were mixed in inexplicable confusion ; and a mining-chemist is very apt to fall into a system of adventitious analyses, taking first-class ore wherever he can find it, and overlooking its relation to the formation and position of the vein. I hope that a few notes which I present on this subject may be found worthy of consideration, as throwing a new light upon this obscure topic. During the last three years, while acting as chemist of the Lumberman's Mining Co., I have made some 3000 analyses of iron-ore from the Ludington mine at Iron Mountain, Michigan. These analyses were necessary in order to separate Bessemer and non-Bessemer ore which occurred intermixed in the deposit. During the last year, I attempted in several ways to find some reason or method in the distribution of phosphorus, and have finally become cognizant of the arrangement herein outlined. I have been obliged to confine my attention to our new mine, and, in that, to that portion wherein

Jan 1, 1889

By V. H. Gottschalk

SEVERAL years ago a group in the metallurgical division of the U. S. Bureau of Mines began a study of the application of new developments in physics to metallurgical problems'. Among these developments were the extensions of what may be termed by analogy the "sound spectrum." Electromagnetic waves, from X-rays to radio waves, have been quite thoroughly explored for metallurgical use, but the sound spectrum, extending from low-frequency vibrations involved in certain types of metal failure by fatigue through the range of audible sound to inaudible vibrations having frequencies of many kilocycles, has had only meager consideration from metallurgists. Because of the general interest in the process recently demonstrated by St. Clair3 for flocculating smoke by means of sound waves, this article is written to point out possible applications of sound and supersonic (ultrasonic) waves in the metallurgical industry.

Jan 1, 1937

By Frank R. Corwin, Selden S. Rodgers

PAGE I. Introduction,........... 383 11. Brief History of Present MacDoUgall Plant,.... 384 III. First Experimental Work on Increasing Capacity of Furnaces, 385 IV. Effect On MacDouRall Plant of IncreaBed Draft from New Smelter Stack,,.......... V. Increasing the Capacity of the MacDouGall FurnaceS,.. 391 (A). Test of Arthur Crowfoot on Increasing Capacity,.... (a). Description of Test,........ (6). Discussion of Results Obtained from Test,... 393 (B). Investigation Carried Out by John A. Church, Jr.,... 395 (a). Advantages of High Speed,......398 (C). Effect on Regular Operation of Department by Applying Results Obtained from Experimental Work ..... 399 (D). Fundamental Principles Involved in Increasing the Tonnage, . 400 VI. Treatment of an INcreased Amount of Ore Screenings,.. 401 VII. Maximum Percentage oF Ore Screenings in a MacDoUGall Feed, 403 VIII. Tests to Further Increase Capacity of Furnaces,... 406 IX. Tests to Decrease PercentaGe of Flue Dust made by MacDouGall Furnaces,............. (A). Repath-Marcy Furnace......... 408 (B). Modified Hepath-Marcy Furnace,....... (C). Crouse Furnace Designed for Dust Prevention,.... 413 (a). Tests on Crouse Furnace,....... X. Concrete Hearths,.......... 419 XI. Conclusion,............ I. Introduction. Since the first installation of MacDougall roasters at the Great Falls smelter of the Anaconda Copper Mining Co., the capacity of the furnaces.has been more than doubled. During the first nine or ten years of the operation of the MacDougall department the tonnage treated by the furnaces remained practically unchanged. Experimental work carried out in 1906, however, showed that increasing the draft of the furnaces would bring about an increase in capacity. In 1909 the MacDougall department was connected to the new smelter stack and

Jan 1, 1914

By R. F. Slack, J. C. Draper, J. A. Younkins

In 1959, the Duquesne Light Co. was faced with the problem of moving more than 40 million tons of bituminous coal in Greene County, Pa. The coal had to travel a distance of about 4 ½ miles from a new mine portal in Rocky Run Valley to the company preparation plant and loading facilities on the Monongahela River. After careful study of this immense transport problem, Duquesne decided that the belt conveyor system described in the following pages offered the best solution. This system, now in operation, is probably one of the four or five longest permanent overland conveyor systems in existence. The general layout of the entire system is shown in Fig. I. A detailed description of the salient features of the system is presented below. THE MINE The valley of Rocky Run where the system begins is very, very narrow and very steep. It was chosen as the site of Duquesne's new mine portal because it was the only place on this particular property where the Sewickley coal seam cropped out. The valley also had two other advantages. First, it fronted on a state road and, second, it offered a site where some 4 million gallons of water could be stored for use in dust-allaying sprays needed in the mine. The company elected to construct a drift mine in the valley because this would require neither the hoisting time of a shaft mine nor the walking time of a slope mine. As part of the mine construction project, the valley was leveled by relocating its stream and filling its center with material cut from each side.

Jan 11, 1966

By Francis L. Sperry

Up to within a few years, the consumption of nickel has been more directly dependent upon the available supply than that of any of the other useful metals. The Gap mine, in Lancaster county, Pennsylvania,* has been, for the last quarter of a century, the only property in this country furnishing nickel in paying quantities. Its yearly output was about 300,000 pounds of metallic nickel, or nearly half the amount used annually in the United States. Foreign nickel from mines on the New Caledonia islands, in the South Pacific, found entrance into our markets as the production of the Gap mine fell off. The price of nickel was constantly maintained, and no special effort was made to extend its use. Over-production was cautiously guarded against, and all surplus metal was held by the banking-houses of the Rothschilds, who assumed the bonded indebtedness of the Sociètè le Nickel. The opening of the Ontario nickel-mines has, however, brought about a radical change; and nickel from the Sudbury district can be delivered in New York within four days, and in European markets within two weeks, as against two months consumed in transporting South Pacific ores. Former prices have been irretrievably smashed, and European trade-journals comment favorably on the influence which Canadian nickel has had in making lower prices, and breaking the backbone of the " nickel trust." Production and Costs. The quantity of nickel produced and the prices which it commanded may be briefly summarized as follows: The total production of the world from 1840 to 1860 was about 100 to 250 tons yearly of metallic nickel; from 1860 to

Jan 1, 1896

By F. M. Hamilton, H. F. Ameen

Results of a laboratory investigation of some sintering variables are presented. The effect on physical properties of mix component variation and rate of cooling of the sinter is illustrated by crush and tumbler test results and data of reducibility tests and microscopic examination of sinters are shown. The results of using solid additions in the mix to improve bed permeability are given. SOME of the variables encountered in the sintering of iron ores and their effect on sinter properties have been investigated at the Jones and Laughlin Ore Research Laboratory in Michigan. Ores requiring agglomeration before blast furnace utilization may be classed as coarse, intermediate or fine. Coarse iron ore is considered similar to a — 1/4-in. Mesabi wash ore containing some 95 pct of its particles between 94 in. and 100-mesh. Intermediate iron ore is considered similar to our New York State magnetic concentrates in which all the particles are — 20-mesh and about 60 pct are +100-mesh. Fine ores are considered as being at least 100 pct —100-mesh. This paper will deal only with the two coarser classifications. Most of the work has been done in a small experimental batch unit previously described in an AIME1 paper. Results being obtained form a basis for present and future trials in production sinter plants. It is expected that new production units that may be added in the future will benefit from laboratory studies. In general, the results reported here are obtained by laboratory study, but it is Experimental Sinter Machine: The laboratory sinter machine employed in the work consists of a chamber with 1 sq ft of grate area. It is mounted on

Jan 1, 1951

By H. F. Ameen, F. M. Hamilton

Results of a laboratory investigation of some sintering variables are presented. The effect on physical properties of mix component variation and rate of cooling of the sinter is illustrated by crush and tumbler test results and data of reducibility tests and microscopic examination of sinters are shown. The results of using solid additions in the mix to improve bed permeability are given. SOME of the variables encountered in the sintering of iron ores and their effect on sinter properties have been investigated at the Jones and Laughlin Ore Research Laboratory in Michigan. Ores requiring agglomeration before blast furnace utilization may be classed as coarse, intermediate or fine. Coarse iron ore is considered similar to a — 1/4-in. Mesabi wash ore containing some 95 pct of its particles between 94 in. and 100-mesh. Intermediate iron ore is considered similar to our New York State magnetic concentrates in which all the particles are — 20-mesh and about 60 pct are +100-mesh. Fine ores are considered as being at least 100 pct —100-mesh. This paper will deal only with the two coarser classifications. Most of the work has been done in a small experimental batch unit previously described in an AIME1 paper. Results being obtained form a basis for present and future trials in production sinter plants. It is expected that new production units that may be added in the future will benefit from laboratory studies. In general, the results reported here are obtained by laboratory study, but it is Experimental Sinter Machine: The laboratory sinter machine employed in the work consists of a chamber with 1 sq ft of grate area. It is mounted on

Jan 1, 1951

By N. Albon, J. F. Miller, R. W. Coutant

The deposition of nickel from nickel carbonyl onto amorphous substrates has been studied, with attention being paid to the specific effects of the physical and chemical nature of the substrate and to the effect of oxygen on the crystal morphology. With substrates having microscratches or etch lines, nu-cleation was observed to occur preferentially at these surface features. Flame polishing of the substrate surfaces was found to remove any regularity in preferred nucleation sites. Nucleation was observed to occur less readily on substrates having relatively low surface energies, e.g., Teflon and carbon, than on materials having relatively high surface energies such as fused silica. At low oxygen concentrations [Ni(CO)4/O2 > 54 x 1031, apparently pure and well-formed nickel crystals were observed to nucleate and grow irrespective of the presence of oxygen. At higher concentrations of oxygen, a secondary growth process, dependent upon oxygen concentration and resulting in a gradual change in crystal morphology, was observed. It is concluded that the influence of oxygen on the nucleation and growth of nickel is determined by the relative kinetics of the various possible reactions, and that under the experimental conditions employed the 0-Ni interaction occurs at some nucleation or prenuclea-tion stage. THE purpose of the research on crystal nucleation in chemical vapor deposition as described in this paper has been twofold: 1) to examine some effects arising from the use of amorphous substrates, and 2) to study the specific effects of oxygen on the nucleation and growth of nickel in a nickel carbonyl-carbon monoxide system. The nickel-nickel carbonyl system was chosen for study for several reasons: 1) nickel films are of potential interest in electronic technology, and 2) the deposition can be carried out at moderate temperatures, thus making possible detailed study of the processes occurring and the use of a variety of substrate materials (including some which melt at relatively low temperatures). Fairly well-characterized chemical kinetics and a broad background of information are available on the py-rolysis reactions and on the mechanisms of Ni-O interactions. NUCLEATION AND GROWTH THEORY The theoretical background for the analysis of nucleation and growth by vapor deposition for a one-component system (physical vapor deposition) and the problems encountered therein have been reviewed by Hirth and pound.' More recently Mande12 has indicated the difficulties of applying such theory to chemical systems. One of the major problems involved is the possible multiplicity of chemical reactions and deposition routes. For example, those reactions which are probably of significance in a discussion of the pyrolytic deposition of nickel from nickel carbonyl under the conditions of the present experimental work are illustrated in Fig. 1. As is true with most cases of chemical deposition, many of the quantitative data necessary for a complete analysis of the system are either not available or not directly measurable. However, with the present system, sufficient data are available for a discussion of nucleation and growth on a qualitative basis. Classically, the rate of nucleation of a monatomic species being deposited from a vapor phase is given by

Jan 1, 1965