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By Harlowe Hardinge, R. C. Ferguson

Laboratory and plant data covering 12 different operations show that lower than "standard" ball mill speeds increase grinding efficiency. In the case of high pulp-level mills, the gain is so great that the increase in capital cost of the larger lower speed mill will pay for itself in less than a year's time.

Jan 1, 1950

By AIME AIME

BLANDFORD. C. BURGESS, the new Chairman of the Industrial Minerals Division, took the advice of Horace Greeley in reverse-he turned his hack on San Francisco and the Golden Gate, and after a few side excursions toward Alaska and Arizona, hit the trail eastward, not for the lonesome pine, but for Spruce Pine, N. C. Born Aug. 10, 1893, in San Francisco. Burgess found his first job, shortly after finishing high school at 19, as axeman for a surveying party of engineers working for the Southern Pacific Co. in Oregon. Later he moved on up with them into Alaska. He liked the engineering profession, and decided to equip himself further so he entered the University of California in the fall of 1913. and for the next two years devoted himself to acquiring an education in civil engineering.

Jan 1, 1945

By F. W. Davis

SOME idea may be gained of the tremendous consumption of refractories by the open-hearth steel manufacturers from a statement made by A. T. Green at a meeting reported by T11.e Industrial Chemist of London, as follows: "At a very progressive steel plant in the Midlands, with a battery of five open-hearth furnaces working. twelve months and making 3000 tons of steel per week, the cost of refractories per ton of steel produced averages about $0.50 for the actual open- hearth casting and $0.12 for those operations incidental to the rolling of the metal." .These figures, when translated into the annual tonnage of steel, represent a very considerable expenditure.

Jan 1, 1930

By H. S. Martin

The Phosphate Recovery Corporation operates three flotation plants, Nos. 1 and 2 concentrators about three miles northeast of Mulberry, Florida, and No. 3 plant at Wales, Tennessee. These plants represent the first commercial phosphate flotation operation and are also believed to be the largest nonmetallic flotation operation in the world at the present time. The details of this paper will be confined to plant No. 2, this being the newest and largest concentrator in Florida, and the flow sheet being practically the same as at plant No. 1. The No. 3 plant has been operated but a short time and has been shut down since December, 1932, on account of the decrease in phosphate rock production. The phosphate washers usually are located centrally on a known deposit so that about two hundred acres of ground can be mined economically to each washer location. The washers are moved to new areas when the distance becomes too great for economical pumping. The flotation plants are built either adjacent to a washer, so that current debris may be utilized, or on the site of a former washer where there is sufficient accumulated debris available for mining, and the flotation plants must also be moved from time to time. Most of the water used in the Florida flotation plants is recovered after passing through a circulating system where most of the fine suspended matter is settled out, but some make-up water is obtained from deep wells near the plant. Power is obtained from the Tampa Electric Co. through the distribution facilities of the International Agricultural Corporation. Flotation concentrate is hauled from the plant by trolley over the International Agricultural Corporation's trolley system, to the drying plant at Prairie, one mile northwest of Mulberry. Ore Treated In the pebble phosphate district of Florida, the phosphate mineral, or collophane, is usually found in horizontal beds of varying thickness

Jan 1, 1935

By Frank A. Hill

After a long struggle with an underground mine-fire and its accompanying evils, having experienced the discouragement of many retreats, the uncertain hope of varying advances, and the gratification of final success, I am tempted to give the members of the Institute some of the details of the fight. I do not write with the thought of treating a novel subject, but with the hope that some one as unfortunate as ourselves may be led by our experience to avoid our mistakes and to profit by our successes. The fire occurred on June 16, 1890. It was a calamity awful in its results, ringing the death-knell of thirty-one stalwart miners, bringing sorrow and desolation to many homes, and destroying in a few hours the work of years. While there have been a number of disasters in the history of American mining in which there was a greater loss of life and property, I know of none in which so simple a cause led to results so serious. A description of the mine, with the details of the accident, is necessary for a full understanding of the conditions existing at the time. The Hill-Farm-Parrish mine is in Dunbar township, Fayette county, Pa., about one mile from Dunbar station, on the Pennsylvania and Baltimore & Ohio railroads, about four miles south of Connellsville, nine miles northeast of Uniontown, and in the heart of what is celebrated as the Connellsville coke region. The mine is owned and operated by the Dunbar Furnace Company ; and all the coal produced is made into coke and used in the company's furnaces, one mile to the east. The mine is opened by two slopes, the HillFarm and Parrish, the latter known also as the Ferguson. The Hill-Farm slope is 2600 feet northeast of the Parrish. There are 150 ovens at the former and 70 at the latter slope. The Hill-Farm slope is 4100 feet in length, and the length of the Parrish at the time of the accident was 3700 feet. The average dip of the coal is about 8 degrees S of W. The workings of the two slopes are con-

Jan 1, 1893

By AIME AIME

BESIDES commanding increasing importance as an alloying element in combination with ferrous and other nonferrous metals, the variety of uses for pure nickel continues to widen. For coinage it is growing in popularity. These coins have been minted for 27 countries in 72 issues representing 69 denominations. Approximately 3,000,000,000 pieces have been struck, the aggregate weight, of which amounts to nearly 14,000 tons. . Danzig, Iraq and Japan are the most recent governments to adopt, pure nickel coinage. France is adding the denomination of five francs to its other nickel currency; they replace silver pieces. Germany is now minting a new issue of one Reichsmark coins of pure nickel. The Japanese program for 1933 called for the issue of 35,000,000 10-sen pieces and 30,000,000 5-sen pieces. In radio tube manufacture the consumption of pure nickel was approximately twice that of 1932. During 1.933 the nickel plating process by which bright deposits may be plated

Jan 1, 1934

By John B. Hastings

The origin of the watery vapors of vulcanism has always been an object of interest and speculation to the seismologist, and as theories of the genetic origin of ore-deposits have of late years been pretty well narrowed down to the expiring forces of plutonic action, the same question has attracted mining engineers and geologists, as is well shown by the discussions of the subject in our Transactions. The important part taken by volcanic emanations in the origin of pegmatites and quartz-veins, described in my paper, Origin of Pegmatite,' and their latent power to concentrate into useful deposits such scattered gold as occurs in the Hartsel granite, make a discussion of their derivation but a natural third and final step. It is coilceded that enormous amounts of vapor accompany vulcanism, though perhaps we are apt to forget that steam has 1,700 times the volume of water, besides which the column seen over Vesuvius and other volcanoes is greatly mixed with air; the immensity of such volumes compared with solids and liquids is shown by the experiment of Gautier, who, by heating dessicated granite to 100' C., evolved from it gases 20 times, and steam 90 times, its own volume. Dana appraised the average amount of water left in ordinary rocks as 2.5 per cent. T. M. Read estimated that the Mississippi river carries to the sea annually 150,000,000 tons of rock material. If these Mississippi sediments, as deposited, contained 20 per cent. of water, it would be 600,000,000 cu. ft., or 4,500,000,000 American gallons, annually. Allowing the vapor suspended over a volcanic cone to be mixed with 80 per cent. of air, this amount of water converted into steam would replenish anew, every 9 min., a column 15,000 ft. high, 2,000 ft. in diameter at the base, and • 10,000 ft. at the top. Read's estimate is only half of the amount given in a more recent and probably correct one.2

Jan 1, 1909

By L. D. Jaffe, R. K. Pitler

IT would clearly be advantageous to produce molten titanium, suitable for alloying and casting, directly from the relatively inexpensive tetra-chloride, without using a metallic reducing agent. Accordingly, a preliminary investigation has been made of the production of titanium by hydrogen reduction of the tetrachloride in an electric arc furnace. For the reaction: TiCl4(g) + 2H2(g) ? Ti(s) + 4HCl(g), Lockhart and his colleagues' have calculated equilibrium constants at 800" to 1500°K, based on tables of Brewer.' Extrapolating these data on the assumption that the heat of reaction varies linearly with temperature, and using Brewer's value for the heat of fusion, there is obtained for the reaction: TiCl4(g) + 2H2(g) ? Ti(l) + 4HCl(g) an equilibrium constant at 2100°K (100" above the melting point) Kp = (PHCl)4/pTlcl4 (Ph2)2 = 0.167 atm. If this is correct, starting with hydrogen saturated with TiC14 at 25°C, where the vapor pressure of the latter3 is 12.6 mm, and maintaining the overall pressure at 1 atm, 99 1/4 pct of the TiC14 would be reduced to Ti at equilibrium. An arc furnace designed for the melting of titanium and lined with water-cooled copper was used for the preliminary experimental check. Its inside diameter was 2 7/16 in. and height 6 in. The water-cooled electrode was tipped with 3/4 in. diam tung-sten. In the one run carried out, the furnace was charged with a starting batch of 293.35 g of scrap titanium,' analyzing 99.24 pct Ti. After the system was twice pumped out and flushed with argon to remove air, the arc was struck in argon and kept at 400 amp dc, electrode negative, for 1 min to melt the starting batch. Commercial tank hydrogen, dried by passing over silica gel and bubbled through technical grade TiC14 at room temperature, was then admitted to the furnace. The inlet tube directed this gas downward toward the arc and melt; the gas outlet was at the top of the furnace. The quantity of gas passed through was not measured accurately but is estimated to be about 50 liters per min at a few mm of mercury above atmospheric pressure. The arc was held in the H2-TiC14 mixture at 400 amp with little difficulty. After 10 min the arc burned through the copper lining above the melt, admitting water and ending the run. (This had happened frequently in straight melting runs under argon, and is not thought due to the atmosphere used.) In the furnace were found an ingot, several small pieces, and a little metallic powder, evidently formed when water entered the hot furnace. Some titanium also clung to the electrode. The portions were weighed and separately analyzed for titanium. Their total weight was 321.76 g of 94.82 pct overall purity. Much of the impurity consisted of tungsten broken off when the titanium was removed from the electrode. No detailed impurity analysis was made because the starting materials were impure and flooding the furnace introduced further contamination. Thus, the metal recovered contained 305.08 g Ti, as compared to 291.12 g in the starting batch. Titanium could not have been carried over from previous melting runs in the furnace, as the interior was sandblasted and the electrode ground clean before the run. Evidently at least 13.96 g of Ti were produced from TiCl4. Since this would require complete reduction of 430 liters of TiCl, gas at 12.6 mm of Hg, the efficiency of the process must have been rather high. Experimental work is continuing. No reason is seen why the process could not be scaled up to the size of a 30-ton steel-melting arc furnace. In a large unit there would be a large molten pool from which liquid metal could be withdrawn for alloying and casting. The problems of electrodes and power supply are similar to those arising in arc furnaces for melting titanium. Unreacted TiC14 and the HC1 in the exhaust gases could be recovered; unreacted H2 could be dried and re-used. The melt would be saturated with hydrogen, whose solubility in liquid titanium is unknown. Small amounts of hydrogen seem to have little effect on the properties of titanium.5 If the amount introduced was so large as to impair properties or cause casting difficulties, it could be reduced by holding the melt under an inert gas or by pumping on it, prior to casting. Acknowledgment The authors would like to thank I. Preble and M. Goldman for their valuable aid in the experimental work and the thermodynamic calculations, respectively. References 1R. J. Lockhart, J. J. Ward, M. J. Hussey, and J. W. Clegg: In unpublished report, "U. S. Air Force Project Rand. Titanium and Titanium Base Alloys." Battelle Memorial Institute (1949) 37-44. 2 L. Brewer et al: Chemistry and Metallurgy of Miscellaneous Materials—Thermodynamics. Ed. by L. L. Quill. pp 13-39, 60-192. (1950). McGraw-Hill Book Co. 3 K. Arii: Scientific Reports. Tohoku Imp. Univ. (1933) 22, 182. 4 R. S. Dean, J. R. Long, F. S. Wartman, and E. L. Anderson: Transactions AIME (1946) 166, 369-381; Metals Technology (Feb. 1946) TP 1961E. * R. I. Jaffee and I. E. Campbell: Transactions AIME (1949) 185, 646-654; Journal of Metals (Sept. 1949) TP 26813.

Jan 1, 1951

By Shiou-Chuan Sun

DISCUSSION shiou-chuan sun (author's correction) - Too late for revision, the author realized that the data on stability of froth presented in this paper were not based on the same height of froth column. It is recommended herein that the stability of froth is better calculated by dividing the time elapsed until the froth disappeared by the volume (in cu cm per sq cm) or height of the froth column, and is expressed in sec per cm. The stability data in Tables I, II, and III of this paper were recalculated, in accordance with this recommendation, and the results are shown respectively in the accompanying Tables VII, VIII, and IX. Compared with Tables I, II, and III of the paper, the stability data of Tables VII, VIII, and IX are more reliable in disclosing the persistence of froth of various frothers having different frothabilities. For example, the conclusion given in the paper that the stability of froth is generally proportional to the volume of froth becomes invalid when the stability of froth is expressed in sec per cm, as shown in Tables VII, VIII, and IX. Table VII shows that both the stability and volume of froth increase with the addition of small amounts of n-hexyl alcohol, and that further additions of n-hexyl alcohol decrease the stability but increase the volume of froth. Table VIII indicates that the stability of different types of frothers is governed by their chemical composition and is difficult to predict from their frothability. Table IX shows that the stability of different frothers with similar nonpolar groups tends to increase with a decrease of the hydro- philic property of their polar groups, and consequently with the decrease of their solubilities. This is further substantiated by the fact that the stability of frothers, as listed in Table IX, is generally lowered by the solvent effect of absolute ethyl alcohol. Table IX shows also that the stability of froth tends to increase with the decrease of the volume of froth* provided the frothers used have similar nonpolar groups and dissimilar polar groups.

Jan 1, 1953

By Shiou-Chuan Sun

DISCUSSION shiou-chuan sun (author's correction) - Too late for revision, the author realized that the data on stability of froth presented in this paper were not based on the same height of froth column. It is recommended herein that the stability of froth is better calculated by dividing the time elapsed until the froth disappeared by the volume (in cu cm per sq cm) or height of the froth column, and is expressed in sec per cm. The stability data in Tables I, II, and III of this paper were recalculated, in accordance with this recommendation, and the results are shown respectively in the accompanying Tables VII, VIII, and IX. Compared with Tables I, II, and III of the paper, the stability data of Tables VII, VIII, and IX are more reliable in disclosing the persistence of froth of various frothers having different frothabilities. For example, the conclusion given in the paper that the stability of froth is generally proportional to the volume of froth becomes invalid when the stability of froth is expressed in sec per cm, as shown in Tables VII, VIII, and IX. Table VII shows that both the stability and volume of froth increase with the addition of small amounts of n-hexyl alcohol, and that further additions of n-hexyl alcohol decrease the stability but increase the volume of froth. Table VIII indicates that the stability of different types of frothers is governed by their chemical composition and is difficult to predict from their frothability. Table IX shows that the stability of different frothers with similar nonpolar groups tends to increase with a decrease of the hydro- philic property of their polar groups, and consequently with the decrease of their solubilities. This is further substantiated by the fact that the stability of frothers, as listed in Table IX, is generally lowered by the solvent effect of absolute ethyl alcohol. Table IX shows also that the stability of froth tends to increase with the decrease of the volume of froth* provided the frothers used have similar nonpolar groups and dissimilar polar groups.

Jan 1, 1953

[A Aalseth, Earl P. (M 51) Geol, Amerada Petr. Corp., Box 1498, Billings, Mont. Abadie, Henry G. (M 43) Asst to Supvr of Oper, Long Beach Oil Dev. Co., 255 S. Santa Clara, Long Beach 7, Calif. Abbe, T. Waldo (A 56) Ass't Dist Oper Supt, Sun Oil Co., Beaumont, Tex. Abbott, J. L. (M 56) Partner, Pritchard & Abbott, 501, Century Bldg, Fort Worth, Tex. Abbott, Richard H. (J 51) Owner, Abbott & Howard, 422 W. Hermosa, San Antonio, Tex. Abbott, Seth J., Jr. (M 51) Tekoil Corp., .2;A6 Mercantile Nat'l. Bank. Dallas, Tex. Abbott,. William G. (M 50) Div Mgr, Rice Eng. & Op. Inc., Box 1142, Hobbs, N. M. Abderhalden, R. R. (J,59) Box 100, Carmi, Ill. Abel, Malcolm D., Gen Mgr, Bakke Oil Co., Midland, Tex. Abel, Raymond L. (M 28) Prof of Chem Engr, Univ. of Pittsburgh, Pittsburgh 13, Pa. Abel, Wayne K. (M 57) 1513 Patton Drive, Odessa, Tex.]

Jan 1, 1961

By Leonid V. Azároff, H. N. Murty

In the course of investigating the soft X-ray absorption spectra of Ni-A1 alloys, Das and ~zfiroff' observed an anomalous brittleness in solid solutions containing 3 to 5 at. pct Al. The brittle alloys also had anomalously larger lattice constants' and the fine structure at the nickel K edge of an alloy containing 3.96 at. pct A1 unexpectedly resembled that of NiA1 more closely than that of a solid solution containing 5.51 at. pct Al. This led them to suggest the possibility that short-range ordering was produced during the homogenization anneal to which each specimen was subjected, similar to that observed in dilute solutions of vanadium and of chromium in nickel: as the principal cause of embrittlement. It was decided to repeat the above measurements on several alloys in this composition range in order to test the above hypothesis and to establish the effect of heat treatment on the alloys' properties. Three solid solutions in this range were prepared containing, respectively, 3.16, 4.00, and 4.54 at. pct Al, in addition to alloys containing 6 and 9 pct. All samples were annealed in vacuum at 1800°F for 100 hr and then furnace-cooled to room temperature, as in the original study. The lattice constants of these alloys are shown by open circles in Fig. 1 and can be seen to fit quite closely the curve established by the previously measured values, indicated by solid circles. (The experimental errors are of the order of the size of the circles, +o.oo~R.) The three alloys containing 3 to 5 at. pct A1 were found to be quite brittle, as previously reported. In order to test the possibility of ordering, these three solid solutions were again heated to 1800°F and, following a few hours at that temperature, were quenched directly to room temperature. All three alloys lost their brittleness. In order to verify the proposed ordering hypothesis, it was decided to subject each sample to several cycles of quenching and annealing (disordering and ordering). After some experimentation, it was established that reproducible results could be obtained by anneal-

Jan 1, 1968

By E. H. Crabtree

This paper traces the experimental and pilot plant work completed by the authors since 1939 including the various methods which have been developed in applying coarse activated carbon to cyanidation. The methods and results developed by the authors in desorbing gold and silver from carbons are given and the possibilities for the re-use of the desorbed carbons are discussed

Jan 1, 1950

By A. J. Weinig

The method described is a modification of Schutzenberger's whereby the solution in titrations and the standards are protected from the atmosphere by a layer of kerosene. Indigo-disulfonate is the indicator and sodium hydrosulfite the standard. The method is rapid and delicate. It has been tried on a variety of mill solutions and mill men have found the method of value. THE important part that dissolved oxygen plays in the cyanide treat-ment of gold and silver ores is commonly recognized by most metallurgists and mill men.. But heretofore there has been no simple method on which the mill man could rely for determining the amount of oxygen in the various mill solutions. A few methods are adaptable to the, laboratory, such as the gasometric1 determination by actually measuring the oxygen. Winkler's2 iodometric method, and Schutzenberger's3 method, which depends on the reducing action of sodium hyposulfite on a blue solution of indigo carmine; but these are not readily adaptable to the needs of the mill man and cannot be applied to cyanide solutions without modification. The gasometric method is the most accurate but it takes too long to complete a determination. White's' method (a colorimetric method that depends on the degree of coloration imparted to a solution of pyrogallic acid in the presence of caustic soda) although much more rapid than any of the methods named, often gives misleading results on account of grading of colors of different solutions, which nearly always contain various kinds of salts. The method herein described was devised for the use of the mill man, the aim being to develop a simple, practical, accurate method. It is a modification of the Schutzenberger method and depends on the reducing

Jan 8, 1924

S. F. Emmons, Washington, D. C.: Mr. Malcolmson's paper on the intensely interesting deposits of the Sierra Mojada creates a strong desire to visit the region so well described. Although it is difficult to intelligently discuss a locality that one has never seen, I cannot refrain from offering some remarks in the nature of a tentative suggestion: 1. Age of Beds.—Mr. Malcolmson speaks of the enormous thickness of limestone forming the Sierra Mojada as belonging to the Carboniferous series. If this is not a typographical error, it seems that he should present some evidence for such age, for Chism,* in his previous article on the district, says the only fossils found there were said to be Cretaceous; and it is well known by the investigations of R. T. Hill and others that the great thickness of limestone in this part of Mexico is of Cretaceous age. 2. Structure of Mountains.—Mr. Malcolmson presents good reasons for thinking that the structure of the two related mountain masses (Sierra Mojada and Sierra Planchada) is not the simple anticlinal fold given by Mr. Chism's section, it being evident that there has been faulting as well as flexure. I venture to add that the facts presented by Mr. Malcolmson seem to suggest the possibility that, instead of being simply an eroded anticline, the valley between the two ranges may have been formed, in part at least, by the irregular faulting down of the intermediate block, on the surface of which the volcanic breccia had originally accumulated at a higher level. The sections of the Exploradora and the San Josh mines, in the smooth surface of the contact, with clay selvages and the occasional slickensides, certainly suggest a structural fault between the limestone and breccia. The arrangement of some of the

Jan 1, 1902

By Thomas T., Read

THE decades immediately before and after the end of the nineteenth century (1890-1910) were a period of increased activity in mineral industry education. One reason for ,this, undoubtedly, was the rapid increase in mineral production in the decade 1880-1890; pig iron and copper production tripled; coal, lead, and zinc output more than doubled. Most of the other mineral substances followed the same general trend. Aluminum production began in 1886; petroleum output, which in 1888 was less than it was in 1882, almost doubled in the next three years. Gold alone showed no appreciable change until its discovery at Cripple Creek in 1891, followed by the Klondike in 1896, brought to boiling a public interest in minerals that had been simmering for some years previously. The first cyanide plant in the United States was erected at Bodie in 1893, and the first chlorination plant at Cripple Creek* the next year. Silver- lead smelting had already greatly developed, and the metallurgy of copper was almost transformed. The hearth area and smelting capacity of copper reverberatory furnaces more than quadrupled between 1878 and 1894; matte converters were first erected at Butte in 1884. Copper production of the United States in 1899 was 30 times that of 1872. While it was the increased technology used in mineral production that really made the field attractive for educated young men, undoubtedly they did not realize that, and were impressed mainly by the quantitative increase in output. Another factor was the increased general interest in engineering education; three times as many men took engineering degrees in the United States in 1890 as in 1880; 1893 showed almost a 56 per cent increase over 1890. Industry had come to recognize that technical training was worth while. The mineral industry lagged somewhat at first; the total number of mining degrees

Jan 1, 1941

By M. J. GAVEN

COMING over from the plant on the Denver and Rio Grande yesterday afternoon I was an interested listener to a smoking-room conversation that had to do with the experimental plant near Rifle. The people who were talking didn't know me and I didn't know them, but I learned quite a little. I understood that the plant would never operate; that it was not intended to operate; that the "oil trust" would keep it from operating; that our tramway had eaten up all our money and still was not working and would not work; that the plant was run by a bunch of kids, and that the superintendent was probably the biggest kid of the bunch. I plead guilty to the latter. But the people who were talking were misinformed. The plant is producing oil. The first sample of oil that came from our unit at the Bureau of Mines experimental plant at Rifle, Colo., was produced on Sept. 18, the first that came out of the condenser, and it is still coming. This sample of oil may mean to the United States what the first oil produced from the first well meant.

Jan 1, 1926

By F. W. Bradley

MY first Nevada City mining reminiscence is one of seeing Capt. Thomas Mein, over 52 years ago, in the old Wyoming mill on Deer Creek about a mile below the town of Nevada City. Captain Mein was then superintendent of the Wyoming mine, where the old fashioned Cornish pump was used, as well as hurdy-gurdy water wheels for power. This mill was one of the typical, up-to-date mills of that time and consisted of stamps, fed by Chinese hand feeders, who also cobbed the ore down to a small enough size to be fed into the mortars. Stamps at that time were of light weight and crushed about one ton to one and a half tons to the stamp, the pulp going over plates, then into sluices with self-raising gates. When a sluice became full the pulp was shut off and directed into the parallel sluice, also with a self-raising gate. The concentrate thus collected in the sluice was shoveled out and carried to Cornish buddles and there cleaned up, preparatory to being sent to a local custom chlorination works.

Jan 1, 1929

By Charles Hardy

?POWDER METALLURGY? is the production of semiformed or fully formed metal products by compressing metal powders. It had its beginnings in the fabrication of tungsten and molybdenum bars and wire by compression, sintering, and swaging. Powder metallurgy, although still in its infancy with other metals, has shown remarkable progress in recent years. Production of Metal Powders-The first step in any powder-metallurgy process is the production of metal particles of suitable shape and size. Mechanical processes for producing metal powders, as by crushing, stamping, or grinding, are usually not suitable, as the resulting particles may cause laminations and decreased strength in the finished articles. The principal metal powders now in use on a large scale are produced by electrolysis or by reduction of metal oxides by gases.

Jan 1, 1936

By T. K. Redden

Protective coatings based on the formation of a surface coating of nickel aluminide (NiAl) were applied to the nickel-base superalloys IN 100, SEL 15, and U-700. Coated specimens were exposed to an oxidizing environment at temperatures between 1600 and 2200 F for times up to 1000 hr. The oxidation resistance and stability of the coating were evaluated by weight gain measurements, metallographic examination, and X-ray diffraction study of surface oxides and coating. The composition of the coating and diffusion zone was determined by electron microprobe traverse of samples before and after high-temperature exposure. Intermediate phases formed in the coating and diffusion zone were identified by X-ray diffraction in situ and after electrolytic extraction. The outer coating was found to consist of the inter-metallic compound, NiAl, while the diffusion zone contained MC, M23C6 or M6C carbides, and a phase in a matrix of NiAl + Nidl. Oxidation resulted in formation of an A1203 n'ch scale containing some Tz02. Depletion of aluminum during oxidation resulted in degradation of the outer coating to Ni3Al and the nickel alloy matrix. Diffusion of aluminum into the base metal was found to be slight and did not influence coating life significantly. The o formed in the diffusion zone during coating decomposed during elevated-temperature exposure to form stable carbide phases characteristic of the base metal. Diffusion zone phase changes were found to have no effect on the life of the aluminide coating in the oxidizing envzron?nent. THE oxidation resistance of many high-strength nickel-base superalloys is inadequate for extended exposure at temperatures above about 1600°F. In addition, some applications for these materials require that they be exposed to environments containing sulfur compounds and sodium salts which can cause surface attalk known as sulfidation or hot corrosion. In order to provide the necessary corrosion resistance to the high-strength alloys, protective coatings based on an aluminizing process have been developed. These processes, usually based on a pack cementation technique, result in the formation of a NiAl-rich outer coating layer either during the coating process or by a subsequent diffusion treatment. The performance of the aluminide coatings is affected by interactions between the coating layer and the base metal both during the coating process and during subsequent exposure at elevated temperatures. Knowledge of these interactions is required to guide the development of coatings capable of longer life and improved reliability. Goward et al.' recently reported the metallurgical factors which influence coating per- formance on MAR-M200. The present work is concerned with correlating the interactions and performance of coating compositions on several representative materials. EXPERIMENTAL PROCEDURES Materials. Three cast nickel-base superalloys which are used for turbine buckets in air-breathing engines were studied: IN 100, U-700, and SEL 15. Their chemical compositions are given in Table I. The alloys were vacuum-induction-melted and cast to slabs approximately 0.3 in. thick from which rectangular specimens 0.25 by 0.5 by 1 in. were machined. Coating Procedures. The machined specimens were coated by CODEP processes which were developed at the author's laboratory. These are based on pack cementation in various media to deposit either aluminum or aluminum in combination with titanium. The coating process which deposits only aluminum is designated CODEP-C, while the CODEP-D process deposits titanium in combination with aluminum. The CODEP-D process was applied only to IN 100. Both CODEP processes are applied at 1950" or 2000°F for 4 hr without need for a subsequent diffusion treatment. An outer coating about 1 mil in thickness is produced by these processes. Test Procedures. Coated specimens were exposed to static oxidation for periods ranging from 24 to 1000 hr at temperatures of 1600" to 2200°F. Terminal weight gain measurements and visual examination were used to evaluate oxidation resistance. including oxide spalling and coating failure. Both as-coated and exposed specimens of each alloy were studied by metallographic examination, electron microprobe analysis (EMA), and X-ray diffraction analysis either of the exposed surfaces or of phases extracted from the coating and diffusion zone. RESULTS As-Coated Condition. The microstructures of as-coated conditions were generally similar, irrespective of base materials or the particular coating process. They are typified by IN 100 coated by CODEP-D as shown in Fig. 1. The predominately single-phase outer layer, area A, Fig. 1, was identified by X-ray diffraction as the intermetallic compound NiA1. The NiAl zone extended inward to the original base metal interface. The diffusion zone, area B, Fig. 1, included carbide phases, a lamellar phase oriented perpendicular to the base metal surface, and a matrix phase consisting of a mixture of NiAl and Ni3Al. The phases in the diffusion zone were electrolytically extracted using a 10 pct HCl in methanol solution at approximately 1.3 amp per sq cm. The extracted phases were found to be M6C, MC, or M=C6 carbides and o as shown in Table I1 for each of the alloys. The d spacings from a typical diffraction pattern are

Jan 1, 1969