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By William S. Hannan, H. Rush Spedden

FLOTATION may be defined as a process whereby mineral particles are concentrated by selective adhesion to air-liquid interfaces. The process involves attachment of desired mineral particles to air bubbles, and removal of the mineralized air bubbles from the surface of the pulp as a mineral concentrate. PROBLEM Although great strides have been made in understanding the principles of flotation, one part of the process which has not been adequately explained is the mechanism by which selected mineral particles become attached to air bubbles. A glance at the froth of an operating flotation cell demonstrates adequately that use of proper reagents and conditions will result in such attachments; but how such attachment takes place is not definitely known. A better knowledge of this factor might lead to improved flotation practice either through altered machine design or the application of scientific innovations. Direct observation of the behavior of mineral particles and bubbles in an operating cell does not appear promising because of the complexity of the system. For this reason, conclusions concerning the problem must be deduced from theoretical considerations or from observation of simplified systems designed to reproduce conditions thought to exist in an operating cell. PRESENT THEORIES Two mechanisms have been recognized as fundamental in particle-bubble attachment: gas precipitation and direct encounter. It is a simple matter to demonstrate in the laboratory that attachment can be brought about by either mechanism. As to the relative importance of the two in a particular flotation system, however, there is a divergence of views. Taggart1 states, Under exceptional circumstances sufficient force and time to effect attachment may conjoin in an ore pulp undergoing agitation, and a preformed bubble adhere to a collector-coated mineral particle, but the occurrence is rare. . . . Pulp-body froth flotation effects selection in the body of a conditioned pulp by causing gas bubbles to precipitate from solution in the liquid phase preferentially at the surfaces of collector-coated particles, and to cling to these particles. Gaudin2 states that, within the pulp body of an agitation machine, attachment of mineral particles to air bubbles occurs as a consequence of contact between the two. This theory has been supported by theoretical reasoning and much circumstantial evidence. Perhaps the most interesting bit of evidence in favor of this theory is the difficulty in the flotation of fines. If attach-

Jan 1, 1947

By Luther W. Lennox

During the last few years, one of the great problems in the milling of all ores has been that of grinding. This subject involves not merely the cost of the operation, but also the selection of the proper degree and character of grinding to yield the best metallurgical results on the given ore. Considering the diversity of machinery, one is led to wonder at the variety of grinding methods employed, even when realizing that metallurgy demands varying products. In an attempt to investigate the relative grinding resistances of a number of ores now being milled in this country and Alaska, the manage-mxitofthe Portland mills requested Samples of average mill-run of ore from various companies. The request met with a ready response, indicating the desire of all operators to gain information on the subject. The difficulties involved in this investigation were numerous, lack of time for outside problems during this strenuous period being a serious one. Also, we were unable, in the time, to obtain a correct 150-mesh screen; in the screen analyses tabulated and plotted herewith, the 150-mesh screen was used merely to protect the 200-mesh screen, not to ascertain points on the curves. The experimental grinder was a small iron tube-mill, 8 by 121/2 in., in which was placed a definite number (74) and weight (3450 gm.) of 3/4-in. steel balls, 1 Ib. water and 1 Ib. ore. To obtain uniform conditions, each ore was first crushed and screened, and from the sized products a "standard feed" was artificially prepared, the same standard being adopted for all tests in that particular series. The prepared feed was

Jan 1, 1920

By F. S. White, E. L. Kinsella

THE solids fluidization process brought out by the Standard Oil Development Co. in the early forties for catalytic cracking of petroleum enabled rapid transfer of large quantities of heat from gases to solids under closely controlled temperature conditions. As the technique developed, it was natural that applications for the process outside the petroleum industry would be sought. The calcination of limestone to ' quicklime requires the transfer of a large quantity of heat at high and closely controlled temperatures. For these reasons, this possible application was one of the first to be investigated. Laboratory work conducted by the Dorr Co. indicated that lime produced by solids fluidization would be of exceptional quality. Calculation of theoretical heat balances showed that savings in fuel could be expected. Accordingly, a pilot plant of 10 tons per day capacity was erected by the New England Lime Co. at Adams, Mass., to substantiate the process. Operation of the pilot plant, previously described,1 showed that excellent lime could be produced with a saving in fuel. The work also indicated the necessity of preparing feed to remove the finer fractions if dust losses were to be held to a tolerable level. A single-stage fluidized solids drier-stripper was developed to accomplish this sizing.2 Subsequently a commercial lime reactor was erected at Adams, beginning operation in June 1949, followed by air sizer facilities completed in November 1951. This paper will describe these two applications of solids fluidization. The raw material for preparation of lime by the fluidizing process is a high calcium crystalline lime stone having the approximate chemical composition shown in Table I. The stone is first prepared by crushing and grinding in conventional equipment to pass a 6-mesh sieve. After crushing, the material is sent to the FluoDry unit for drying and dedusting. Fluidized Drying and Sizing As shown in Fig. 1, the FluoDry unit consists of a 1/4-in. cylindrical steel shell, 9-ft ID by 22-ft 6-in. overall height. Attached horizontally at the bottom is a 6-ft diam combustion chamber, approximately 7 ft 6 in. long. A refractory constriction dome, consisting of first-quality fire brick shapes, partitions the inside into two sections. The lower section is called the windbox and the upper the bed compartment. The vertical wall of the shell is lined with 6-in. first-quality rotary kiln blocks. In the bottom of the windbox a hoppered section is formed with castable refractory to permit the windbox to be readily cleaned via a 6-in. screw conveyor. The combustion chamber is similarly lined with refractory shapes. On the 6-in. diam section, 4 1/2 in. of insulating brick, HW-26, are used. The inner combustion chamber is lined with 4 1/2-in. Korundal brick to withstand the high flame temperatures encountered. An 8-in. steel feed pipe, entering vertically through the top and fitted with an air-operated cone valve,

Jan 1, 1952

By D. Murgue

The circulation of air in underground workings is subject to a gradual and continuous reduction of its pressure, from intake to outlet, caused by the friction between it and the more or less rough and uneven surfaces of the passages. For comparison with the flow

Jan 1, 1894

By R. S. Dean

REQUIREMENTS for war materials have led to large scale experimentation upon metallurgical innovations. It is of interest to inquire what this may contribute of permanent value to our existing technology, as innovations adopted during war are apt to be discarded promptly at its end. This is because utilization of substandard ores usually requires a new technology for ore treatment, and a new use-pattern for employment of the products. Thus two very different problems are involved: first, devising a process; then, adopting its products by industry, with readjustments of the use-pattern if necessary. A new process may be as good or better than an old one, but the readjustments required for use of its products may prevent its general adoption if this implies scrapping existing plants and investing much additional capital. Metallurgical innovations are of three kinds: I. The use of substandard material in processes already established; 2. The grading-up of substandard material to render it more suitable for established processes; 3. The adjustment of technology and use-pattern to the raw materials that we have.

Jan 1, 1945

By Elmer Weber, W. M. Baldwin

Solid lead obeys a single parabolic weight increase vs. time law. In contrast, liquid lead undergoes three successive parabolic weight increases vs. time laws, the first of which has a low constant relative to the latter two. The conversion times for the change from one parabola to the next decrease with increasing temperature. IN recent reports on the subject,1,2 it was noted that zirconium and titanium scale in air by a complex mechanism. The scale first forming on the metal is protective to the extent that it gives a low constant, K, for Tammann's, and Pilling and Bedworth's parabolic equation: w² = Kt [1] relating weight increase, w, due to chemical reaction of the metal with the air, and time, t. After hundreds of hours of apparent stability in some cases the first scale yields to another that offers little protection to the metal. This transition from one scale to another, from a slow parabolic oxidation reaction to a fast one, was not due to impurities in the atmosphere or incidental effects (changing environment, etc.) but was a specific behavior of the metal itself, the transition occurring at definite times (dependent on temperature) and showing other reproducible traits. In view of this behavior how can long-time service behavior be predicted from short-time laboratory tests, not only in the case of these metals, but in any case? Certainly a systematic study of the type of scaling behavior described above—wherever it is found—would help to answer this question. The present paper is a report on the behavior as it is found in lead—the only metal to the authors' knowledge for which the behavior has been described at all, if inadequately, for our present purpose.* At least four oxides of lead are known, of which one occurs in two allotropic forms. They are ß (red) tetragonal PbO stable up to 486°C;8 a (yellow) orthorhombic PbO stable from 486°C up to its dissociation temperature in air at about 2300°C;9 minium or Pb3O4 which from the dissociation pressure data given in Fig. 1 decomposes to PbO at 540°C in air; lead sesquioxide or Pb2O3,; and lead dioxide or PbO2 which, according to Fig. 1, decomposes in air at 400°C to minium. In view of the high dissociation temperature of PbO, lead will scale up to at least its boiling point. Further, it is known that oxygen is almost insoluble in liquid lead.'V his implies a fair probability that an oxide scale would not dissolve in the molten metal and would afford the same protection to lead in the liquid state as in the solid. All of the oxides of lead for which specific gravity data are available are more voluminous than an equivalent weight of metal or a lower oxide from which they might form, hence the scales will be in compression. Lead oxides are known to be ductile, so it would be anticipated that they would form coherent nonporous scales. It is not surprising to learn, then, that both solid and liquid lead scale according to the Tammann, and Pilling and Bed-worth law.14,15 (Gruhl states that at 600°C and above lead oxidizes linearly with time because of "spitting" of the scale.) The parabolic constants K reported by various investigators3,14-16 are badly scattered, however, as shown in Fig. 2. The oxides formed on solid lead were described as being reddish-brown but were not chemically identified by Pilling and Bedworth.15 Gruhl's descripdin³ of the appearance of the scales On his liquid samples indicates that a (yellow orthorhombic) PbO is formed initially on the specimens but gives Way eventually—at least at temperatures below 486 °C— to .ß (red tetraunal) PbO, and that below 540°C minium—Pb3O4 :is firmed at an even later time as an overlay on either the red or yellow PbO. Fig. 3 is a graphical interpretation of Gruhl's description. Gruhl does not indicate any change in the parabolic scaling rate as yellow PbO converts to red. He does indicate that minium reduces the scaling rate, al-

Jan 1, 1953

By R. R. Sayers

TWO serious hazards from coal dust confront the bituminous-coal miner- -a physical or safety hazard and a physiological or health hazard. The first threatens the miner with loss of life from coal-dint explosions, and the second with loss of health and earning capacity from inhaling large quantities of the dust. Studies by the Bureau of Mines have shown that coal dust, except some grades of anthracite dust, is capable of initiating an explosion when no explosive gas is present and that its property of extending or propagating an explosion has been responsible for nearly all the widespread explosions that have occurred in bituminous mines in the United States in the present century. For years many mining people believed that low-volatile coal dust was not explosive but not only is it explosive but if the source of ignition is intense, it is as explosive as the dust of many high-volatile coals because the war is creating increased pressure for greater coal production and because of the trend toward greater mechanization in mines, explosion and health hazards from coal dust are likely !n increase considerably.

Jan 1, 1943

THE discussion at the annual meeting of the paper on "Devices for Detecting Dangerous Gases in Mine Air" (published in. MINING AND METAL-LURGY, February 1, 1927, p. 69) was prefaced by the following description of a new portable methane indi-cator, presented by D. C. Ashmead: Two comparatively recent disasters in Utah are directly responsible for the perfection of the new methane detector. The first of these occurred on May 1, 1900, when 200 work-men lost their lives. The second disaster did not occur for more than two decades, when, on March 8, 1924, at the Castle Gate Mine No. 2, 172 workmen were killed. A dis-sembled safety lamp was later found at the seat of the ex-plosion. This indicated, as a possible cause, that the safety lamp had gone out and the fire boss had tried to relight it. These two disasters brought, the mine operators of the State of Utah to the concentrated attempt to end the loss of life through mine explosions. The Governor of the State appointed a committee, known as the Utah Mine Op-erators Committee, to study the phases of the problem, and this Committee in turn enlisted scientists all over the country in cooperative research. One group, under the direction of E. K. Judd, of the Union Carbide and Carbon Research Laboratories, of Long Island City, New York, concentrated its efforts on develop-ing a methane detector which would be completely ade-quate. This is now successful, since in laboratory as well as actual coal-mine tests the apparatus has instantaneously and accurately detected the presence of extremely small amounts of methane.

Jan 3, 1927

By Charles M. Rolker

The Mariposa estate, a grant made by the Mexican Government to Juan 13. Alvarado, during the time when California was still under the dominion of Mexico, was purchased in 1847 by J. C. Fremont, and the United States patent issued to him in 1856. By sale, or its equivalent, money advanced, the property came into the hands of the Mariposa Company, June 25th, 1863, and through a varied existence of work and temporary inactivity, has as yet been kept as an undivided property, and rests at present with the Mariposa Land and Mining Company of California. I pass over this period of 15 years without giving the history of the ups and downs of the estate, partly because it is familiar to many, and also because I think in such a case this paper would assume too much the character of a narrative. The estate is situated in Mariposa County, California, about 170 miles southeast of San Francisco. It begins in lat. 37' 26' 38'' north, and long. 119' 55' west, and runs 6 miles north; thence 69 miles west; thence 5 miles northwesterly towards the Merced River; thence 84 miles southerly; thence 3 miles easterly; thence 1 mile southerly; thence 2 miles easterly; thence 2 miles southerly; thence 2 miles easterly; thence 1 mile southerly; thence 2 miles easterly; thence 1 mile northerly, and thence 2 miles easterly to the place of the beginning; embracing 44,387 acres (70 sq. miles) more or less. To describe this vast estate in detail as to its full geology, its numerous quartz veins, its many facilities to exploit them and work them by cheap methods, would lead me further than I intend to go at present, and I will content myself to describe the latest workings of the company and its immediate field of operations. As long ago as 1860 the late Dr. Adelberg advised the running of an adit from the northwestern edge of the estate at Benton Mills 011 the Mereed River. His object was to undercut the deepest workings of the then paying mines on the estate—the Pine Tree and Josephine. Following this advice, the tunnel known as "River Tunnel " was commenced. Its entrance is in S. 5, T. 4, s. R. 17 E. It is run in

Jan 1, 1879

By Prof John E. Church

It is a well-known fact that under similar conditions a ton of pig iron can be made from any ore with less fuel when charcoal is used than when coke or anthracite is employed for heating. The cause of this superiority is entirely undiscovered, and no explanation has yet been offered which has won even temporary acceptance. Such as they are the hypotheses heretofore presented are of two general kinds, and they come from those two divisions of the working force which are so often antagonistic in all professions, the scientific and the practical men. The theory of the scientific men is drawn from the chemical reactions which are known to go on in the furnace, and it is well expressed in a recent paper by Prof. Akerman, of the Stockholm (Sweden) School of Mines. It makes the superiority of charcoal as a fuel in the blast furnace to depend upon its quick and thorough reduction of carbonic acid. This property belongs to charcoal in virtue of its porous structure. Its cells have a diameter of only one twenty-four hundredth of an inch, and one grain of charcoal has been computed to have a surface of two and four-tenths square feet. According to the theory in question, carbonic acid is formed by the first impact of the air upon the fuel; but in charcoal furnaces the acid is immediately reduced to oxide by taking the necessary amount of carbon into combination, and the gas reaches its highest reducing power even in the near vicinity of the tuyeres. Coke, being harder, does not produce so strong a reducing gas in that part of the furnace. Carbonic acid is formed as in the case of charcoal, and remains longer before its reduction to oxide is completed. Anthracite is the

Jan 1, 1879

By Paul C. Merritt

Chrysotile asbestos producers in Quebec may soon experience a unique situation-i.e., strong competition from American ore sources for the short fiber market west of the Mississippi River. This com- petition will be forthcoming from Copperopolis and Coalinga, two deposits now being developed on opposite flanks of the San Joaquin Valley in central California. The combined output now planned from both deposits is 100,000 tons annually, equivalent to about 50% of the annual market demand in the western, central and Gulf States, and more than twice the tonnage sold in 1960 by all other American asbestos producers combined. The principal companies involved in these new undertakings are Jefferson Lake Asbestos Corp. (subsidiary of Jefferson Lake Sulphur Co.), Hidden Splendor Mining Co., Coalinga Asbestos Co. (Johns- Manville Corp. in conjunction with Kern County Land Co.), Union Carbide Corp., and Asbestos Corp. Ltd. Jefferson Lake's principal interest is at Copperopolis where the company's new 70,000-ton per yr mill recently went on stream. The company also holds some claims at Coalinga, but this latter area is better known as the site where Hidden Splendor, Coalinga Asbestos Co. and Todd Industries (a local company) have established operating mines and mills capable of turning out 30,000 tons of fiber each year. Coalinga is also the site of exploration by Union Carbide Nuclear and Asbestos Corp. Ltd.

Jan 9, 1962

By Willard P. Ward

Having been engaged during the past year in the manufacture of ferro-manganese in a blast furnace, I have imagined that some further information on this subject might be of interest to that large number of members of the Institute who are engaged in the iron and steel industries. The great question of the economical production of good steel, ingot metal, or homogeneous iron (we scarcely know now what to call it) from good materials, and at reasonable prices, has, thanks to the intelligence and energy of a few American engineers, been successfully solved in this country. Nearly all first-class railroads, and many that would not rank so high, have adopted the Bessemer rail. Martin boiler-plates are rapidly gaining ground, in competition with

DR. PeRsifor Frazer, Philadelphia, Pa. (communication to the Secretary):* Mr. Campbell's very interesting contribution, after complimentary mention, finally decides against the acceptance of the classification proposed by me in a paper bearing the same title and read at the Wilkes-Barre meeting, May, 1877.2 That paper was written primarily for the Second Geological

Jan 1, 1906

By L. M. Yokum

Tremendous strides have been made in front end loaders in the last 15 years. Fifteen years ago a 21/4-cu-yd front end loader was the largest standard machine you could purchase. Today there are two commercially available 15-yd front end loaders and many 10-yd loaders. The estimated total worldwide market for all front end loaders over 1 cu yd has increased to over 30,000 units yearly. The trend for front end loaders, in general, and for the mining market, in particular, is to larger and larger loaders. Today there are 18 and 24-cu-yd front end loaders in prototype form. It is not inconceivable that within another 15 years there will be front end loaders in the 50-cu-yd class with design features quite different from today's. These larger loaders are being designed at the demand of the mining industry, and the design criteria are being directed at this market area. The costs of these larger loaders may be greater per unit of capacity, but it is the intent of the various manufacturers that they will be more reliable, be easier to service, give greater availability, live longer, and cost less to maintain, than previous loaders. It is also the intent of the manufacturers to compete directly with the large mining shovel as the front end loaders become appropriately larger and more reliable. There has been some trend in this direction in the past with smaller shovels and loaders. In Table 1 are data for U.S. production of front end loaders (5 to 6-cu-yd class and 10-cu-yd class) and U.S. production of cable-operated, crawler-mounted power shovels, draglines, and cranes (11/z to 5-cu-yd class) for the years 1965 and 1970 (Source: Bureau of Census, U.S. Department of Commerce). Many believe that the decline in shovel production, in particular, is due at least in part to the acceptance of the front end loader as a primary production tool. However, the foregoing comparison is for a smaller shovel class than for front end loaders. It has generally been a rule of thumb that a front end loader is competitive on a cost and production basis with a shovel when it is approximately twice as large as the shovel. This same relationship may not hold true with the larger 10 to 15-cu-yd electric shovels, but at some point, direct competition will probably occur. Current Trends There are many trends today that are significant. One major usage trend in large front end loaders involves load and carry operations. This application is defined as "performing the functions of loading, hauling and dumping with one machine over distances within its economical limits." Many people are using front end loaders to transport material as well as load it. It is estimated that nearly half of all 10-cu-yd front end loaders sold in 1970 went into primary load and carry work. Many times, significant savings result from using the load and carry system, instead of small truck and shovel operations, for distances in excess of 1000 ft. Strip mining in coal utilizes great numbers of front end loaders in this manner. In-pit crushing of limestone is developing on an ever-increasing level, especially in Europe, and this stimulates interest in load and carry operations. In Table 2 is a cost example for 10-cu-yd front end loader in a limestone quarry. More than likely, load and carry use will continue to increase over the next few years. While some types of mining do not lend themselves to load and carry in the pit, such areas as surge piles are applicable and should be studied. In the area of machine operating cost reduction, there

Jan 1, 1974

By George C. Stone

The stack gases from regenerative furnaces lare very seldom utilized for the production of steam. If the temperature of the gases is not higher than 300" C. (572" F.) there is no economy in their use for this purpose, as the amount of available heat is very small and the temperature is so little above that of the steam that the interchange is too slow. With higher temperatures of the waste gases, however, good results can be obtained. At the plant of the New Jersey Zinc Co. (of Pa.) at Palmerton there are a number of return tubular boilers, each 6 ft. in diameter and 20 ft. long, with 96 3.5-in. tubes, which are heated by the waste gases from the spelter furnaces. These furnaces have continuous regenerators heating the air only and the stack gases reach the boilers at a temperature of about 450". The gas producers for one of these furnaces require 14 tons of anthracite (a mixture of Nos. 2 and 3 buckwheat), and the waste heat from the furnace gives a little more than 42 h.p. in steam. The boilers are not well adapted for the purpose, as they are much too large for the amount of heat going to them and the area of the tubes is not sufficient to take the gas from two furnaces without causing an objectionable amount of back pressure. The plant was built without any idea of using waste-heat boilers, and it was impossible to place the latter as close to the furnaces as they should be. Furnace and boiler are connected by an underground brick flue in which the temperature of the gas drops about 100°, losing 40 per cent. of its available heat. If the boilers were close to the furnaces the horse power of each would be 70 instead of 42. Even under these unfavorable conditions the boilers have been very advantageous, as one boiler easily supplies the steam necessary for two batteries of producers. With such low gas temperatures the heating surface of the boilers is, of course, not as efficient and the flue areas need to be considerably larger than for coal firing.

Jan 1, 1914

By R. Lee-Aston

HALLOWAY mine of Tennessee Copper Co. at Copperhill, Tenn., has been under development for several years. It has two shafts, the A shaft, 1336 ft deep from the surface to the 16 level, and the B shaft, lying 500 ft to the southeast and extending 1385 ft deep from the 10 level down to the 24 level. A section through the two shafts, Fig. 1, shows the development work entailed by the proposal and the area involved. The Problem: For operational reasons it was necessary to extend the B shaft from the 10 level to surface, and the pilot hole and raising method was chosen. This method had been used to extend the Company's Boyd manshaft from the 10 to the 14 level in 1954, but no satisfactory hole surveying method had been employed. In that instance, when the hole was located it was found to be about 8 ft from its calculated position. The success of this shaft extension method lies in the ability to keep the pilot hole within the proposed shaft diameter for nearly the entire length. The approximate 670 ft of extension distance in one hole was thought to be excessive because of deflection encountered locally in other core drilling. Since a connection between the two shafts, intermediate between the surface and the 10 level, would be required at some future date, the pilot hole drilling was done in two sections. This intermediate level was fixed at the 6 level and distances became 470 ft from surface to the 6 level and 230 ft from the 6 to the 10 level. A rock pentice of 25 ft was left temporarily in place just above the 10 level.

Jan 3, 1958

By R. S. Archer

In the microscopic examination of aircraft-engine parts made of heat-treated alloy steels, the writer has been forcibly impressed by the failure of the usual etching processes to disclose any but gross defects in heat treatment. It seemed particularly desirable to bring out the grain size of the steel, which is indicated in the ordinary etching processes chiefly by the change in orientation of structure from grain to grain. After various attempts, a fairly successful method has been found, which is here presented in the hope that it may be of use to those who have occasion to examine these steels in the hcat-treated condition. The specimens worked with have been mostly chrome-nickel steels heat treated (that is, hardened and tempered) to a Brinell hardness of around 300. A few experiments with other specimens will be referred to later. Briefly, the method employed consists in etching the steel about 10 min. in a fresh solution of picric acid in ethyl alcohol, and then rubbing off the smudge of carbonaceous matter on moist broadcloth. Different samples of almost identical analysis, heat treatment, and physical properties (including resistance to impact) respond quite differently to this treatment. In some, the grain boundaries are developed quite readily, while in others, especially in those whose grain is unusually fine or in which the final hardening heat has not quite obliterated the previous crystallization, the results are more obscure. The exact time of etching to secure the best results also differs for various samples, and the greatest success is usually attained by a process of "tinkering." Such a process is illustrated in a series of micrographs, the first six of which were taken at a magnification of 300 diameters. The properties of the steel are as follows: Carbon, per cent............... 0.42 Brinell hardness.............. 293 Nickel, per cent................ 1.35 Yield point, pounds per square Chromium, per cent............. 0.90 inch........................ 131,000 Copper, per cent................ 0.025 Maximum strength, pounds per Manganese, per cent............ 0.74 square inch................. 144,500 Phosphorus, per cent............ 0.024 Elongation in 1 in., per cent... 28 Sulfur, per cent................ 0.036 Lod impact, foot-pounds...... 51 Reduction of area, per cent...... 57.3

Jan 1, 1920

By Carmine D. &apos, Lemuel Tarshis, Joel Hirschhorn, Antonio

Vapor-deposited nickel films in the thickness range 700 to 4360A were tested in uniaxial tension utilizing a microtester designed specifically for this study. Contrary to the findings of some investigators, a definite thickness-strength relationship was observed below 3000 A with a four-to sevenfold increase in strength over that of bulk nickel. The films were characterized by high elastic strains and little plasticity. On the basis of these and other reported data, it is suggested that the high strength level in metal films is related to the manner in which they are produced. Vapor deposition, owing to its severe quenching effect. is believed to promote the formation of point defects which inhibit dislocation movement. IN recent years it has been reported that metals, when in the form of thin films, exhibit extraordinarily high strengths. The data published to date have been primarily concerned with silver and gold because of the ease with which these metals can be vapor-deposited and their high resistance to surface oxidation. Previous investigations into the mechanical strength of thin films has uncovered an apparent dichotomy of view on film behavior. Beams and his co-workers have reported a definite dependence of strength on film thickness. Other workers,"-'6 however, in separate studies on the strength of poly crystalline and single-crystal films have found no such thickness-strength relationship. The study of thin-film strength is extremely difficult because of the many variables associated with film preparation, handling, and testing. Moreover, the manner of test employed by different investigators has varied quite radically, ranging from simple uniaxial-tension to biaxial-bulge testing. The work reported herein was conducted in order to determine the mechanical behavior of a structural metal when in the form of a vacuum-deposited thin film and to gain some insight into the reasons for the high strengths exhibited by metals having such a con- figuration. In this study a method of test was chosen which would yield results which are easily interpreted and lend themselves to comparison with properties of the same material in bulk form. Moreover, specimen-preparation parameters and film-handling techniques are set forth so that other investigators can properly compare their findings with ours. EXPERIMENTAL PROCEDURES A) Film Preparation. Vacuum deposition was performed in an 18 by 30 in. bell jar using a standard New York Air Brake Co. vacuum station with a 6-in. oil-diffusion pump. Before evaporation the system was pumped to a pressure of less than 2 x 10"5 torr. A shield was employed to protect the substrates from the emission of contaminants during the critical melting and outgassing of the evaporant. The source consisted of from one to six filaments (0.020 in. diam). The length of each filament was about 5 in. and was placed 6 to 8 1/2 in. from the substrate in such a manner that the substrate face was at 90 deg incidence with respect to the evaporant beam. The temperature of the source was 2000"~ during evaporation. The films were deposited onto a substrate arrangement which was composed of four basic components, that is: 1) a 3 by 1 in. glass slide; 2) a 22-mm sq micro cover glass on 1); 3) a 22 by 50 mm micro cover glass coated with collodion on 1); and 4) a stainless-steel sheet mask containing twelve rectangular openings of 1-mm and 2-mm widths and lengths of 5 mm laid over 3). Thus, test specimens of 1-mm and 2-mm widths are deposited onto a collodion substrate which precludes epitaxial effects in the specirnens. 17-le The rectangular cover glass and square cover glass were positioned in such a manner that a strip of film would be evaporated along the length and across the width of the large glass slide. This boundary of evaporated film was used to determine the film thickness by multiple-beam interferometry. The square cover glass was used for X-ray and chemical analyses. Thickness of the deposits was varied by changing the number of filaments used (one to six). The duration of evaporation was 30 sec for each filamgnt which resulted in a deposition rate of 8 to 20A per sec. Evaporations were all performed at room temperature; however, radiant heat from the source raised the substrate temperature to 40" to 60°C. All substrates were cleaned by ultrasonic agitation in a solution of spectranalyzed isopropyl alcohol. Collodion was deposited on the micro cover glass by immersion in solution of collodion in amyl acetate. B) Thickness Control and Measurement. Film

Jan 1, 1963

By R. E. Boni, G. Derge

Application of surface tension measurements has been made to molten silicates in order to determine the effect of sulphur upon the surface tensions of synthetic blast furnace slags. In melts with the same molar ratios of AI2O3 + SiO2 to the basic oxides BaO, CaO, and MgO, the surface tensions increase in the order of oxides listed. Sulphur lowers the surface tensions of the basic BaO, basic CaO, acid BaO, acid CaO, and acid MgO slags in that order; and the concentration of excess sulphur at the slag surface increases in this same order of slags. The rate and amount of desulphurization of iron by these slags is favored by a low excess surface sulphur in the slag. IN a previous paper,1 the authors discussed the applications of surface tension measurements of molten silicates to problems of metallurgical interest. Of major importance is the aid that such studies lend to forming a working concept of slag structure. Since the ability of a slag to desulphurize metal depends strongly upon its composition,2"4 fundamental information about the structural differences between various slags which contain sulphur should aid the development of better desulphurizing media. For that reason, the present investigation concerns the effect of sulphur upon the surface tensions of synthetic blast furnace slags. Experimental Procedure , The maximum bubble-pressure method was used to measure the surface tensions of synthetic blast furnace slags in the temperature range 1300° to 1600°C. The method is based upon the equation which was developed by Schrödinger5 from a consideration of the forces of hydrostatic pressure and surface tension of a liquid which oppose bubble formation when a gas is forced through a tube immersed in the liquid. where y is the surface tension between argon and slag in dynes per centimeter; g is the gravitational constant, centimeters per second2; H is the manometer reading in centimeters; s2 is the density of manometer fluid in grams per cubic centimeter; S1 is the density of the medium in grams per cubic

Jan 1, 1957

By W. S. Hyler, L. W. Berger, R. I. Jaffee

Hydrogen additions of 390 ppm to A-55 titanium and 368 ppm to Ti-8 pet Mn have no deleterious Hydrogenadditionseffect on the unnotched and notched rotating-beam fatigue properties of these materials. 'These amounts of hydrogen, however, are sufficient to cause severe notch-impact thesematerials.embrittlement in A-55 titanium and pronounced loss of tensile ductility in Ti-8 pet Mn. The lack of embrittling effect in fatigue in the latter alloy is consistent with the postulated strain-aging mechanism of hydrogen embrittlement in a-ß alloys. There is a significant strain-agingincrease in the unnotched endurance limit of A-55 titanium with the addition of hydrogen. This increase may be explained as the result of internal heating effects which would dissolve the hydride and cause solid-solution strengthening. TITANIUM and its alloys may be seriously embrittled by relatively small amounts of hydrogen. The form which this embrittlement takes has been shown to vary with alloy type. The a alloys, for example, suffer most strongly from loss of notch-bend impact toughness' when sufficient hydrogen is added, and this effect has generally been associated with the presence of hydride phase in the micro-structure. In a-ß alloys, on the other hand, hydrogen is most detrimental to tensile ductility in slow-speed tests,2-1 and the embrittlement may be detected in a most convincing manner by means of rupture tests at room temperature. This particular kind of embrittlement has not been associated with a change in microstructure, but has been classified rather generally as associated with a strain-aging type of mechanism.' In the present paper, the effect of an embrittling amount of hydrogen on the rotating-beam fatigue properties of both an a and an a-ß titanium alloy is covered. For this study, annealed commercially pure (A-55) titanium was chosen as an a alloy, and equilibrated and stabilized Ti-8 pet Mn as representative of a typical a-ß alloy. Nominal hydrogen levels of 20 and 400 ppm were evaluated, the latter amount having been shown previously to be severely detrimental to the impact toughness of commercially pure titanium and to cause pronounced strain-aging embrittlement in the Ti-8 pet Mn alloy. The only report of the effect of hydrogen on the fatigue properties of titanium is given by Anderson et al.,° in which a push-pull type of fatigue test was conducted on as-received commercial-purity titanium sheet. Much scatter was found in the results, but generally the presence of hydrides slightly decreased the fatigue strength of unnotched specimens in the longitudinal direction. The results of notched tests were masked too greatly by scatter to be significant. Experimental Procedure Preparation of Materials—Analyses of the A-55 titanium and the Ti-8 pet Mn alloy used in this investigation are given in Table I, which indicates the 8 pet Mn alloy to be more nearly a 6 pet Mn alloy. This alloy will be referred to as Ti-8 pet Mn, however, since this is the commercially designated composition. Both alloys were received in the form of5/8-in. diam rod and, after suitable surface preparation, 5-in. lengths were vacuum annealed at 820°C. Half of the rods for each material were then hydrogenated at 820°C to a nominal hydrogen content of 400 ppm. The hydrogenated and vacuum-annealed A-55 rods were hot swaged at 700°C from 5/8-in. diam to 1/4-in. diam, and then annealed 1 hr at 800°C and air cooled prior to preparation into test specimens. Fabrication of the Ti-8 pet Mn alloy was by hot swaging to 3/8-in. diam at 760" and then 1/4-in. diam at 704°C. This material was then annealed 1 hr at 704", followed by furnace cooling to 593"C, and finally air cooling to room temperature. Evaluation—In order to examine more completely the effects of hydrogen on the particular materials studied, slow-speed tensile and notch-bend impact properties were determined in addition to fatigue data. Tensile specimens were of the standard ASTM type with a reduced section of 1/8-in. diam and a gage length of 1/2 in. A subsize cylindrical Izod specimen was used for impact tests. These specimens had a 45" notch with a 0.005-in. radius and a 0.150-in. root diam, and the stress concentration factor of this notch in bending was Kr = 3. Both the ten-

Jan 1, 1959