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By H. R. Banks

The Sullivan concentrator has completed 20 years of operation. During this period a considerable amount of data has been accumulated concerning the characteristics of several types of flotation machines in their application to the problem of the differential separation of the lead sulphide, zinc sulphide and, in more recent times, iron sulphide, in the ore from the Sullivan mine. It is the author's intention to sketch briefly experiences encountered when the several types of flotation machines were introduced into the flow. Original Flotation Equipment and Ore The original flotation equipment consisted of four 18-cell lead-roughing machines, whose concentrate was cleaned in an 8-cell and recleaned in a similar 8-cell machine. Zinc concentration was carried out in four 18-cell machines. One 8-cell zinc re-treatment machine received the reground zinc middling. The 168 cells handled some 3000 tons of original daily feed. These cells were of the standard Minerals Separation type, equipped with 24-in. impellers. Spindles were driven through geared line shaft at a speed of 255 r.P.m. The impellers were the 45' type, except for the last three cells of the zinc-rougher machines, which were of sub-aeration type, with full bottom shroud and half shroud for the top side of the impellers. Four-pound air was introduced. This recognition of the benefit of intensified flotation operation for "gleaning" was an important phase in the early operation and will be discussed further on in this paper. Sullivan ore during this period is described as a finely disseminated mixture of four sulphides, totaling go per cent made up of 13.6 per cent galena, 14.4 per cent mar-matite, I per cent pyrite and 61 per cent pyrrhotite. The specific gravity of the ore was approximately 4.4. There has been a gradual change in the ore content. The 10 per cent of nonsulphide constituents has increased to between IS and 20 per cent and all three sulphides have dropped somewhat. Added equipment and changing technique have made possible the treatment of 8000 tons per day of mill feed instead of the 3000 originally handled. Special Features of Flotation at Sullivan Sullivan flotation differs greatly from customary practice. The very heavy return of lead rougher middling and lead cleaner tailing, totaling at times 125 per cent of the new feed tonnage, has been the subject of much investigation. The practice is still employed. This operating condition is mentioned because it is the author's belief that the in-

Jan 1, 1947

By James A. Barr

The writer's first experience with flotation was during World War I, in the bene-ficiation of Alabama graphite schist ores. One plant used a cone with a peripheral overflow; dried ore was distributed by a rotating disk onto the surface of the water. No reagents were added' The flake-graphite film floated along with some fine silica. Dewatering screens separated the flake. Naturally unit capacities were low but results were satisfactory. Minerals separation mechanical flotation machines were used in another graphite mill. pine oil was added directly to the head cells, with very good results. All the graphite concentrates from both types of flotation were carefully refined after drying by passing through burr mills, followed by very close sizing on sifters. In March 1927, the writer ran a very successful flotation test on minus 28-mesh, deslimed, Tennessee brown phosphate "sand,"† using a mechanical laboratory machine built in the shops of the Anaconda Copper Mining Co., through the courtesy of Ernest Klepetko. The machine was soon converted to a subaeration type, with improved results. This phosphate research program was greatly enlarged and led to the formation of the phosphate Recovery corporation. The development of nonmetallic flotation followed rapidly. The first flotation machine for bene- ficiation of phosphate was installed in January 1928, in a pilot mill, by International Minerals and Chemical Corporation, at Mulberry, Florida. These machines were Minerals Separation, 24-in., sub-,,,tion types, with weir control of pulp between cells. The sand bleeders were very small—about 1¼-in. diameter. As the feed flake. Is to 25 per cent plus 28-mesh material, the cells choked up frequently. This was corrected by cutting a 2 by 6-in. bleeder opening above the impellers, at grid level, which short-circuited the coarse fractions directly into the feed of the next cell. The matter of size classification and grinding was a considerable problem, which does not come within the scope of this article. Because of the troubles noted above, cascade-type roughers were installed in the second flotation plant, built about 1930. Experimental cells had been tried in 1928. General plant layout is shown in Fig. 1 and details of the cascade construction in Fig. 2. The cascade installation in plant NO. 2 gave good results and eliminated troubles due to choke-ups and coarse feed. The capacities and metallurgical results equaled those of the modified 24-in. Minerals Separation flotation machines in plant No. I The objections to the cascade installation are the floor space and mill height required. In 1939 an improved Minerals Separation machine was tested in parallel with the cascades. Extensive tests indicated

Jan 1, 1947

By A. W. Fahrenwald

Cell depth has been for many years a controversial question in a flotation-machine performance. In the impeller type of machine, we are really talking about impeller submergence—i.e., the depth in the pulp at which the impeller is required to produce aeration. The Flotation Machine a Compressor A flotation machine can be considered as an air compressor or blower in which the aeration mechanism takes in air under atmospheric pressure† (14.7 Ib. per sq. in.) and blows it into the pulp (the pulp being the receiver) against a head of 14.7 plus cell depth in feet times 0.4333 lb. per sq. inch. In commercial machines the impeller is submerged in the pulp to depths ranging from about 2 ft. in the smaller machines to as much as 5 ft. in some of the larger ones. In the 2-ft. cell, the hydrostatic head on the impeller is (2 X 1.25 =) 2.50 ft. (assuming a pulp density of 1.25), equal to (2.50 X 0.4333 =) 1.078 Ib. per sq. in. For the 5-ft. cell, the hydrostatic head against which the impeller must make air is (5 X 1.25 X 0.4333 =) 2.708 Ib. per sq. inch. In the small 2-ft. machine, the volume reduction is (1.078 ÷ 0.147 + 0.01078 =) 6.85 per cent and in the large, 5-ft. machine, the volume reduction is (2.708 0.147 + 0.02708 =) 15.5 per cent. It is obvious that for unit volume of free air intake the larger machine receives a lesser (8.65 per cent less) volume of aeration* than the smaller machine. The bubbles in escaping from the pulp expand and are greater in volume at the surface than at the moment of their formation in the pulp; 7.33 and 18.4 per cent larger, respectively, in the small and large machines. Just how this situation affects flotation is not known. It is interesting to note, however, that the bubbles are smaller in the zone of the coarsest particles and largest in the upper zones of the her, more easily suspended mineral particles. It would seem that the relationship might be reversed advantageously. The deep cell is at a greater disadvantage in this respect than the shallow cell. Nothing, however, presumably can be done about this situation. The shallow cell is a partial corrective. Not only does the compression ratio of aeration increase with impeller submergence but the hydrostatic head against which the impeller must operate also increases. The Flotation Machine as a Pump Since, in impeller machines that rely upon their own operation to produce aeration, pulp Passes through the im-

Jan 1, 1947

By H. F. A. Hergt, K. L. Sutherland, J. Rogers

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By Herbert H. Kellogg, Hugo Vasquez- Rosas

Recently the long-chain primary amines have been used extensively for the flotation of silicate minerals. The use of amines to float sulphide minerals has been investigated by several authorsl-5-l8 but most of this work has been done with the short-chain (less than six carbon atoms) primary amine compounds or the more expensive secondary, tertiary and quaternary amines. Perhaps the fact that the long-chain amines are good collectors for the common gangue minerals has led investigators to omit them from consideration as collectors for the selective flotation of metallic sulphides. The work reported in this paper was designed to investigate the use of a typical long-chain amine salt, laurylamine hydro-chloride, as a collector for the flotation of galena-sphalerite ores. The results show that laurylamine hydrochloride (LAmHCl), when used in small amounts, is a good collector for the selective flotation of sphalerite and galena from the common gangue minerals. The differential flotation of sphalerite from galena was not accomplished but the amine flotation of sphalerite after the standard xanthate flotation of galena is possible. The experimental work reported herein is not complete enough to be able to say whether amine flotation of lead-zinc ores would prove superior to xanthate flotation, or whether the method is even applicable to a more complex ore than the one used for this work. However, the apparent reagent costs for the flotation operations described in this paper seem to be less than for xanthate flotation. This fact alone should be sufficient to encourage the millman to investigate the use of these amine reagents, especially as these reagents are available on a commercial scale at a reasonable price. This paper has as its secondary purposes to illustrate how contact-angle measurements have aided in this investigation, and to bring forward some evidence concerning the mechanism of the collecting action of primary amines. Contact-angle Tests The contact-angle measurements were made by the method described by del Giudice6 and used in recent work by Taggart and his collaborators.7-9 The mineral specimens for the contact-angle tests were carefully chosen, to avoid cracks and inclusions of other minerals. All specimens were mounted in "transoptic" plastic mounts and the surfaces were cleaned by polishing with levigated alumina on a cloth-coverkd glass polishing wheel. Distilled water was used on the lap during the polishing and at all subsequent steps in the contact-angle tests. The mounted mineral specimens were handled with glass forceps and special care was exercised to prevent exposure of the clean surface to air or any other source of contamination.

Jan 1, 1947

By Robert E. Cuthbertson

It is the purpose of this paper to describe in detail the laboratory development and mill application of an unusual combination of flotation reagents employed in the concentrator of the Climax Molybdenum Co., on the Continental Divide, near Leadville, Lake County, Colorado. This development originated in an ore-dressing research laboratory maintained by Climax at the experimental plant of the Colorado School of Mines, which is staffed by men directly employed by the Climax Molybdenum Co. Mill-scale testing of laboratory developments was supervised by a representative from the testing laboratory, working in close cooperation with the operating staff at the mill. General milling practice at Climax is ably described in a paper by E. J. Duggan,1 mill superintendent. Other aspects of the Climax project have been described in papers by W. J. Coulter,2 by Butler, Vanderwilt and Henderson,= by Allen Kissock,4 and by Leo H. Glanville.5 Consequently, this paper will be corfined to the metallurgical aspects of recent reagent developments, avoiding, as much as possible, repetition of material covered in these earlier publications. Brief History of Reagent Practice at Climax Prior to the year 1937, the only reagents employed at Climax for froth production and collecting action in the flotation of molybdenite were steam-distilled or destructively distilled pine oils. The only exceptions to this practice were brief periods of mill testing, when reagents of various types were tried on an experimental basis. None of these experimental runs was sufficiently encouraging to justify its continuation as regular practice. Sodium cyanide has been employed since the very early days of milling at Climax as an inhibiting agent for control of pyrite and chalcopyrite. Alkaline reagents such as lime or soda ash have been used in recent years to minimize the detrimental effect of iron salts on flotation of molybdenite. The presence of these harmful salts is attributed to the decomposition of fine metallics abraded from liners and balls in the first stage of regrinding rougher concentrate. Flint pebbles are used in subsequent regrinding, since alkaline reagents are not entirely adequate to offset the inhibiting effect of iron salts as the grind becomes progressively finer and the grade of concentrate progressively higher. Climax metallurgists were familiar at an early date with the use of petroleum products such as kerosene and gas oil as promoters of flotation of molybdenite. Charles C. Oliver6 discussed the use of pine oil and kerosene as early as 19-20, in connection with the milling practice at Dominion Molybdenite Co., Quebec. Nevertheless, the early attempts to apply this knowledge in the Climax concentrator were complete failures. In the light of recent experience, it may seem strange that the early mill tests with petroleum

Jan 1, 1947

By S. A. Falconer

One of the outstanding achievements in connection with this country's war efforts has been the ability of our mining industry to supply from domestic sources many of the minerals of strategic importance that formerly were obtained principally from abroad. In order to meet the war-born demands for these scarce minerals, it has frequently been necessary to develop special methods for treating ores and waste products hitherto considered too lowgrade to be workable; and to improve the efficiency of older beneficiation processes. Important in this respect have been the recent technological advances in the field of froth flotation of nonsulphide minerals. Because of the refractory nature of many of these domestic ores, and, in many cases, the limited available technical data regarding their treatment, much research work has been necessary. The following examples describe the procedures and reagents used, and the results obtained, in certain laboratory flotation investigations conducted by American Cyanamid Company's engineers at the Cyanamid Ore Dressing Laboratory on ores containing such minerals as scheelite, manganese oxides and carbonate, ilmen-ite, brookite, kyanite, garnet, spodumene, mica, feldspar, celestite, fluorite, chromite, corundum, and cassiterite. In presenting these data, we wish to point out that many of the minerals listed have previously been tested, and their amenability to flotation reported, by other investigators—notably those of the United States Bureau of Mines. In some instances the procedures and reagents used in the treatment of some of the following described ores follow rather well-established lines, and with one or two exceptions, the reagents used were well known. However, many of the ores tested did not respond well to simple conventional procedures and it was necessary to adopt special methods of conditioning and desliming, reversal of the usual order of floatability of some of the minerals, multiple cleaning, etc., in order to secure separations. Except where otherwise noted, all numbered and trade-marked reagents mentioned in this paper are marketed by the American Cyanamid Co. or the American Cyanamid and Chemical Corporation. Tungsten ORes Tungsten minerals, vitally important in the war industries of the United States, rank high in the list of those we formerly had to import in order to supply our needs. Most of our domestic ores of tungsten contain scheelite as the valuable mineral. Today there are in the neighborhood of twelve tungsten operations in this country where flotation is used as the main or accessory form of benefication. It has, of Course, been known for some time that scheelite and other tungsten minerals respond to treatment by flotation.

Jan 1, 1947

By J. C. Williams

The operations described in this paper are those of the flotation plant of the Valley Forge Cement Co. at Conshohocken, Pa., and concern the use of a particular cationic reagent—namely, DP-243. The role of this reagent in this plant may be better understood by first considering the purpose of beneficiating cement rock in general and the specific problems at the Valley Forge plant. The ultimate purpose of beneficiating cement rock is to obtain a kiln feed of the desired chemical composition in a form suitable for the most efficient kiln operation. The chemical composition is governed by the type of cement to be made. Before government restrictions (the purpose of which is to simplify operations during wartime) limited the types of portland cement a manufacturer is permitted to produce, five principal types of cement were generally recognized by the industry. They are based upon chemical and physical specifications proposed by the American Society for Testing Materials, federal and other governmental agencies, state highway departments, water boards and other users of large quantities of cement. The physical as well as chemical specifications for any particular type of cement necessitate proper proportioning of the major components—that is, the silica, alumina, iron and lime—and it is necessary to establish and maintain definite limits for each in the raw mix. The manufacturer must then prepare a kiln feed of a composition that will yield a final product that will fulfill the desired specification. This step is further complicated for kilns using coal as fuel, by the amount and analysis of the ash introduced. The amount and nature of the dust lost during burning will also affect the composition of the kiln feed. The problem of preparing a kiln feed of the desired chemical composition is not a simple one, and it is the final product that governs the methods used to obtain such a feed. For example, in starting with a material deficient in lime for the mix sought, it may not be sufficient to raise it to the required lime content. The other constituents must also be present in the proper proportions. In some cases, it may be necessary to raise the lime content to a point greatly exceeding that of the final mix, then, by addition of one or more other materials lower in lime, obtain the mix. The rock used at the Valley Forge plant is a metamorphosed argillaceous limestone of the Jacksonburg formation, the same formation as that of the Lehigh Valley cement rock (which occurs approximately 50 miles north), and its oxide composition is similar to that of the latter. The only practical differences between the two are that, as a result of metamorphosis, crystallization of the Valley Forge rock is considerably coarser and it contains less carbon than the Lehigh Valley rock as well as slightly more magnesia in the form of magnesian mica. The calcium carbonate content of the various strata in the Valley Forge quarry ranges from about 65 per cent to over 85 per cent, the average for the entire quarry being somewhat under the requirement for manufacture of cement, which usually is from 75 to 76 per

Jan 1, 1947

By Herbert H. Kellogg

Deposits of high-silica kaolinite clays occur at many places in central Pennsylvania. These white clays were formed apparently by weathering of argillaceous quartzite and limestone. Their geology, distribution and use have been reported by Leighton.1 The larger deposits have been mined from time to time, and the clay, after washing to remove coarse sand, has found use as rubber filler, foundry clay, and in white cements. In general, the clay from these deposits contains too much grit (quartz) to be useful as paper filler, and the silica content is too high to make it useful as china clay for ceramic ware. Gravity methods for the separation of quartz from these clays have failed because of the extremely fine size of the quartz grains, but by the methods of froth flotation described in this paper these sandy kaolins can be made to yield a purified kaolinite that has a chemical composition close to that of good-grade Georgia kaolins, and is free enough from grit to be used as a paper filler. As by-products of the separation, a fine (— 325-mesh) sand assaying 95.5 per cent SiO2, and a very he (—3-micron) clay are produced. The possible ceramic uses of these products are being investigated at The Pennsylvania State College. Experimental Procedure The Sample.—The clay sample used in these tests was obtained from a small mine near Tyrone, Pa. It had already been washed to remove coarse sand, and represented the finished product of this small mine and washery. Microscopic examination showed that the clay was composed almost entirely of the minerals quartz and kaolinite, and that the quartz was present mostly in particles larger than one micron, while the kaolinite particles generally were less than 20 microns in size. The kaolinite and quartz particles were physically separable by blunging the clay in water with a suitable dispersant. Preparation of Flotation Feed.—By the addition of NaOH in an amount equal to 3 lb. per ton of solids, the clay was completely dispersed in water. Flotation feed was prepared by allowing a dispersed suspension (10 per cent solids) of the clay to stand for the period of time required for a 2.5-micron particle of quartz to settle from the top of the container to the bottom. After this settling period the suspension was decanted from the settled solids. The settled solids were redispersed in water and the separation was repeated once. The two fine fractions were then combined. Thus the clay was divided into a fine and a coarse fraction by size separation at approximately 2.5 microns.* The fine fractioh was found to have a considerably lower sand content than the raw clay (Table I), and was not treated further. The coarse fraction formed the flotation feed for all the tests described in this paper. A size separation of this type can be

Jan 1, 1947

By William B. Senseman

For reasons well known to mining engineers, wet grinding is quite universal in plants having to do with the extraction of metallic values from crude ores. In the processing of the nonmetallic and industrial minerals, dry grinding is the more common method. The crude materials usually contain less moisture than is required for wet grinding and the products usually are marketed in dry form; most of them as powders. To grind wet, therefore, would entail the addition of water and an expense for drying the product, which is not justified. Furthermore, the material would be a dried cake that would still have to be pulverized or disintegrated before use. For producing fine products, air separators have largely replaced the earlier practice of sizing with screens and bolting reels. Mills in which the air-separating feature is an integral part of the design are now commonplace. Mill designs are many and air systems have developed along various lines, but for the purpose of this discussion, only the fundamental idea need be emphasized— the idea of using air for sizing and removing pulverized material from a grinding mill. About 20 years ago, when the use of mills equipped with air separation had become common practice, heated air or gas was introduced to such a system for the removal of moisture. The purpose of this discussion is to outline the developments and trends that have followed this experiment. It is an important development, for mills equipped with air separation are now universally used for pulverizing not only nonmetallic and industrial minerals, but a great variety of other materials. All such mills are essentially the same. Dried material is pulverized, removed by an air stream, trapped in a cyclone collector, and relatively clean air from the cyclone is returned through a fan to the mill. There is no theoretical need for a vent from the system. The practical need is to vent the air that leaks into the system, and, since the cyclone is not 100 per cent efficient as a dust collector, this vented air carries some dust with it. The initial attempt at drying was made on a system like that described, by the addition of a furnace. The minus pressure within the mill draws hot gas from the furnace. Infiltration air, along with the drying gases and evaporated moisture, is vented as before. The first application was made to a mill used for pulverizing coal. The coal contained very little moisture, so very little drying effect was needed for the success of this experiment. Actually, some calculated efficiencies of over 100 per cent were obtained before due allowance was made for the conversion of mill power into useful heat. When moisture is low, the heat obtained from the conversion of mill power is an appreciable part of that required. That drying can be effected in the short time interval available in a grinding mill of this type is better understood by visual-

Jan 1, 1947

By J. L. Lamont, W. Crafts

Studies of the effect of composition of steel on hardenability by Grossmann,' and as-quenched hardness by Field2 and by the authors, have made it possible to predict the results of quenching when the composition and cooling rate are known In order to extend the application of the hardenability calculation to the quenched and tempered condition in which steel is finally used, a survey has been made of the hardness changes caused by tempering. From this study a method has been developed for the prediction of hardness and tensile strength of steel in the tempered condition. The method of calculation was developed from Rockwell C hardness tests on quenched and tempered Jominy specimens and is expressed in Rockwell C hardness units. It is of an additive type in which the degree of softening from as-quenched hardness is estimated. Tem-pred properties may be calculated within about plus or minus 5 Rockwell C hardness or plus or minus 15,000 lb. per sq, in. tensile strength. This degree of accuracy is less than that necessary for the control of heat-treatment, but is adequate for the comparative evaluation and selection of alloy steels. The formula indicates that tempered hardness is primarily dependent on as-quenched hardness and, as in the hardening reaction, the progress of tempering is controlled mainly by the carbon content. Alloys tend to retard softening by a secondary hardening mechanism in which the alloy appears to migrate from ferrite to the carbide phase. The factors for the effects of alloys in tempering vary so much from the effects of alloys in hardening that different steels of equivalent hardenability may, after like heat-treatment, differ considerably in tensile strength. Procedure In developing the method for calculating tempered Rockwell C hardness, simple and complex steels were tested over a range from 0.08 to 0'65 per cent carbon and up to 2.68 per cent manganese, 2.18 silicon, 3.50 chromium, 4.94 nickel, and 1.06 molybdenum. The steels were made as small induction-furnace heats at the Union Carbide and Carbon Research Laboratories, Inc' The accuracy of the method was finally checked on a variety of carbon, low-alloy and high-alloy types of heat-treating steels produced under commercial conditions. The method was based on a study of tempered Jominy bars, and its validity was tested by correlation with the center hardness and tensile strength of oil-quenched and tempered bars from 1/2 to 4 in. in diameter. The method of calculation was derived from the differences in Rockwell C hardness between as-quenched and quenched and tempered Jominy specimens. Prenormalized Jominy hardenability speci-menS quenched from a normal temperature for austenitizatios were used to obtain a range of as-quenched Rockwell C

Jan 1, 1948

By I. R. Kramer, P. D. Gorsuch, D. L. Newhouse

Although many methods have been suggested for the calculation of tensile strength and yield point from chemical composition, their usefulness has been limited to a particular cooling rate or section size. Further limitations have been imposed by failure to take into account many of the alloying elements that exert a considerable influence on the tensile strength or yield point. These systems, nevertheless, have filled an important need in many instances. The value of a system for the calculation of the tensile properties from the chemical composition and cooling rate is that it permits the prediction of the effect of alloying elements and heat-treatment on the mechanical properties, so that more efficient use of alloying elements may be made. Furthermore, it aids in the choice of steel for a given application aid tends to decrease the number of steels that otherwise would have to be tested. It is the purpose of this work to present a method of calculating tensile strength and yield point from the chemical composition and to suggest a method of correlating the tensile-strength and yield-point factors and cooling rate. Steelmakers have been interested for many years in the calculation of the tensile strength of hot-rolled steels. Quest and Washburn' summarize several of the attempts that have been made to devise formulas. They show the inadequacy of each of these formulas and present one of their own. It is apparent from their work that a simple additive equation of the type TS = A + BX + Cy + DZ + . . . , where A, B, C, D, etc. are experimentally determined constants and x, y, z, etc., are the percentages of alloying elements present in the steel, is not adequate to analyze fully the situation encountered in the calculation of tensile strength. For example, it was found that the difference between the calculated and observed values became progressively greater as the carbon and manganese contents were increased. Therefore, the effect of manganese was given as a function of the carbon content. Grossmann, in his work on the harden-ability of quenched steels, and Walter, in his method of calculation of tensile strength of normalized steels, present two cases in which multiplying factors were successfully used to express the combined effect of alloying elements. The factors in both cases were obtained from the fractional increase in hardenability or tensile strength with increase of alloy content. Yield point often is more important in design than tensile strength. For quenched and tempered steels a linear correlation exists between yield 2nd tensile strength.4 This is not true, however, for normalized

Jan 1, 1948

By M. C. Udy, P. C. Rosenthal

The use of minute boron additions to steel has been given considerable attention in recent years. Comparisons made between boron-free and boron-containing heats of otherwise identical analysis have indicated, beyond a doubt, the potent effect of boron for increasing hardenability. The actual hardenability increase has been expressed as a multiplying factor, or in terms of the percentage of other alloying elements boron might replace. The present study presents the results of a systematic survey of the use of boron as an addition to two types of alloyed steels and as a replacement for various percentages of molybdenum in these steels. Both cast and wrought steels of the two basic compositions were prepared. Molybdenum, because of its scarcity at the time the investigation was started, was selected as the element to be replaced by boron. Attention was also given to the effects of boron on other properties of the steels, particularly their notched-bar toughness, to investigate other advantages or limitations of this element as an alloy addition. Experimental Work Steels Investigated The two basic compositions used in this survey of boron as a replacement for molybdenum are given in Table I. The cast steels were higher than the wrought steels in silicon content to improve the casting quality. Table i.—Nominal Composition of the Two Base Alloy Steels composition. Per Cent. steel Mn Si Ni Cr Xi-Cr-Mo Wrought 0.28-0.70-0.15-o.45—o.45-0.32 0.90 0.25 0.55 0.55 Cast 0.28-0.70-0.35-0.45-o.45- 0.32 0.90 0.45 0.55 0.55 hln-&lo Wrought 0.28-I .go-o.0.15-0.32 1.70 0.15 Cast o. 28- I.40- 0.35- 0.31 1.70 0.45 a Sulphur was 0.040 per cent maximum and phosphorus 0.030 per cent maximum. Each of these base steels, both cast and wrought, was made with molybdenum contents of o, 0.10, 0.20, 0.30, or 0.40 per cent, the total comprising 20 steels. In addition, each of these 20 compositions was prepared with boron additions in amounts of o.oo15, 0.003, and 0.006 per cent as ferroboron; and in amounts of 0.002 and 0.005 per cent as two commercial intensifier alloys, designated alloys A and B. The boron-treated steels totaled 100, and the entire series 120. Test Procedure Each steel was melted as an individual heat in a 50-lb., magnesia-lined induction furnace. Ingot iron scrap or mixtures of ingot iron and steel. scrap were used for melting stock. Deoxidation was carried out in the furnace with 0.10 per cent aluminum. The aluminum addition was

Jan 1, 1948

By J. L. Lamont, W. Crafts

Selection of an alloy steel for a heat-treated article has been facilitated by methods for the calculation of harden-ability,' as-quenched hardness and tempered tensile strength.2 Ductility and toughness may also be estimated if the steel is completely hardened on quenching, 5,6 and the present study was carried out in order to develop a basis for estimating the Izod impact strength of partially hardened steel. The investigation was directed toward the prediction of Izod impact strength in steels of normal commercial quality without consideration of special compositions or heat-treatments that might produce abnormal brittleness. It was found that Izod impact strength of alloy steel is controlled by hardness, degree of hardening on quenching, and grain size. In finegrained steels the impact strength for any given degree of hardening is inversely proportional to the tempered Rockwell C hardness, and the relation of impact strength to hardness is lowered by incomplete hardening. Calculation of the tensile strength and impact strength of heat-treating steels has shown that, except at very high strengths, tensile strength is raised by alloys without loss of impact strength whereas the tensile strength gained by higher carbon contents tends to be accom- panied by a disproportionate loss of toughness. Plain carbon steels give relatively low and unpredictable impact strength. The calculation is sufficiently accurate to be helpful in the selection of alloy steel, and common grades of alloy steel have been evaluated with respect to combinations of tensile strength and impact strength attainable after heat-treatment in sections from I to. 4 in. in diameter. Procedure The study of the relation of hardness to impact strength was based on test data derived from 24 heats from four producers. The steels included the following SAE and AISI compositions: 1020, 1030, 1040, 1340, 3310, 33167 4320, 43.30, 4340, 8620, 8630, 8640, 8720, 8730, 8740, 931°, 9317, 9440, 9917 and three high-alloy chromium-nickel-molybdenum steels. As far as is known, the steels tested were of normal commercial quality. They were supplied in 4-in. sections, which were forged to smaller sizes, prenormalized, and machined to final dimensions. Heat-treatment was carried out by heating to the usual austenitizing temperature for the grade of steel, holding for one hour per inch of thickness and quenching in still oil at room temperature. Previous work had indicated that this quenching treatment approximates a severity of H = 0.3; The bars were tempered as follows: 34 in., I in., and 1% in., 2 hr; 235 in., 3 hr; 4 in., ; hr. All bars were air-cooled from the tempering tem-

Jan 1, 1948

By R. W. Mebs, G. W. Geil, D. J. McAdam

As shown in previous papers by the authorsg-17t the resistance of a metal to fracture, like its resistance to plastic deformation, is a function of all three principal stresses. A technical cohesion limit is the technically determined resistance to fracture under a specific stress system. The technical cohesive strength thus comprises an infinite number of technical cohesion limits corresponding to the infinite number Of possible com-binations of the principal stresses. The technical cohesive strength, therefore, may be represented by a surface in a diagram with the three principal stresses as coordinates. As shown in previous papers,'-'' the technical cohesive strength increases with plastic deformation, with decrease in temperature, and with increase in the strain rate. The technical cohesion limit, therefore, is affected by the same factors that affect the flow stress,$ namely, the stress system, plastic deformation, temperature, and the strain rate. More- over, the influence of each of these factors on the technical cohesion limit has been shown to be qualitatively similar to the three of the same factor on the flow stress.9-18 Advance of knowledge about the conditions determining fracture of metals has been retarded by the reluctance of some investigators to abandon preconceived ideas about how metals ''should,, behave. The incorrect idea is still prevalent that the conditions determining resistance to fracture are very different from those determining the flow stress. Attempts are still being made to express resistance to fracture in terms of a single parameter, such as a limiting value of the greatest principal stress, the maximum shearing stress, or the volume stress (one-third the algebraic sum of the three principal stresses). In these attempts, a sharp distinction is sometimes made between a ductile or ,plasticdeformation, fracture,, and a "brittle frat-ture.H In making this distinction, however, the meaning attached to the term "brittle fracture" sometimes is not made clear. The term could mean fracture after very little plastic deformation or it could be used to designate the type of fracture. An ordinary fracture of a ductile metal at room temperature starts as a cleavage, generally transverse to the direction of the greatest principal stress, but eventually changes to a shearing fracture' In some conditions, however, the metal fractures entirely by cleavage, with no evidence of plastic deformation during the fracture; the surface of such a fracture may have a

Jan 1, 1948

By Edward Saibel

The object of this study is to investigate the effect of prior tensile strain on the fracture stress of a metal. This is done in a theoretical manner starting from the point of view developed by the author in his thermodynamic theory of the fracture of metals. The results are compared with experimental findings and a rational interpretation is given to work that shows the variation of fracture stress with prior tensile strain. Theory op Fracture In the thermodynamic theory of the fracture of metals developed earlier,' it was shown that a critical strain energy per unit volume exists. This is characteristic of the material and may be calculated from basic thermodynamic data. When the area under the flow curve reaches this characteristic value, fracture occurs. The general criterion for fracture is expressed in the form « ± u. = JLJW/V [r] where L, is the latent heat of melting of the unit volume, AV/V is the ratio of the change in volume of the unit volume to the original unit volume on passing from the solid to the liquid state, uo is an initial energy density, and J is a conversion factor, which changes energy from heat to mechanical units. As a first approximation, it will he assumed that the stress-strain curve is the straight line that extends from the point of maximum load onward, extrapolated back to the axis of zero strain, for example, line AC of Fig. I. If the point of intersection of the straight line with the axis of zero strain is represented by v., and the slope of the straight line is p, the analytic form of the flow curve is a = (To + pd [2] and the strain energy per unit volume evaluated from Jud6 becomes (u,6 + pa2/2). When this latter term reaches the critical value JLbVIV (designated hereafter by M), it is assumed that fracture occurs. This leads to the following expression for the fracture stress: a; = V«r.2 + iMp [3] The strain at fracture may be calculated from Eqs 2 and 3. It is assumed in this paper that the initial energy density is either zero or that it may be neglected. Furthermore, the complicated states of stress and of strain existing in the necked region of the tensile specimen after "necking" has occurred will also be neglected for the present, so that average conditions will be assumed to prevail. Flow and Fracture Curves LudwigZ attributed to materials two fundamental properties: (I) a resistance to flow and (2) a resistance to fracture. He reasoned that at each instant the

Jan 1, 1948

By J. K. Stanley

Iron-cobalt alloys in the range of 35-50 pct cobalt are of interest in the electrical industry because they possess the highest magnetic saturation of any magnetic material known. l1,2The magnetic saturation induction of the 35 pct alloy is 24,200 gausses, compared to 21,600 for pure iron (Fig I). This difference is significant in electrical apparatus, whcre weight or space is at a premium. Saturation values higher than that for iron can be attained up to about 70 pct CO hut economics restrict the use to as low a cobalt content as possible without sacrifice of saturation. Fig 2 shows the iron-cobalt equilibrium diagram. Up to the present time, two factors have retarded the use of iron-cobalt alloys in the electrical industry for magnetic purposes.? One is the high cost of cobalt ($I.50 per pound) and the other ig the inherent brittleness of the binary iron-cobalt alloys. Straight iron-cobalt alloys up to 25 pct cobalt are ductile and easy to process to thin sheet or strip by conventional methods of hot and cold rolling, but the alloys containing higher percentages of cobalt, including those for which the saturation magnetization is a maximum (35 to 40 pct), are increasingly brittle with increasing cobalt, at least up to 50 pct, and are consequently difficult to process, either hot or cold. Work by White and Rah13 indicated that iron-cobalt alloys could be made ductile by alloying with vanadium, and after quenching the alloys (vanadium up to about 4 pct) were found to he colt1 rollable to very thin gauges. With this as a background, we resumed our work on these alloys with the objective of developing methods for economical commercial production of wide strip. For this purpose we have concentrated on the 35 pct alloy in order to obtain the highest possible saturation value. Experiments were carried out on many alloy additions to the iron-cobalt alloys and on the response of these compositions to heat treatments. This work finally culminated in a commercially producible iron-cobalt alloy which has been named Hiperco.* Materials StudIEd and Procedur' Binary alloys of iron and cobalt in the range of 35 pct cobalt are difficult to hot work (by forging or rolling) without such additions as C, Mn, Si, V, Cr, Mo, W Or perhaps others. Another beneficial effect of such additions is that they increase to a greater or less extent the strangely low electrical resistivity of these alloys about 10 microohms per cm3

Jan 1, 1948

By A. S. Nowick, E. S. Machlin

One of the main criteria used to rate the heat-resisting properties of alloys is stress rupture.' During a stress-rupture test a tensile specimen is held under a constant load at a constant temperature until it fractures. The chief measurement made during this test is the time requird for rupture at the specific test stress and temperature. It was found empirically from a series of stress-rupture tests at a constant temperature that when the logarithm of the time for rupture is plotted against the logarithm of stress a straight line is obtained within experimental error This method of showing stress-rupture data has been adopted by many investigators and the NACA.' By interpolation and extrapolation from these plots, values of the stresses required to rupture the specimens (the rupture strengths) in 10, roo, and 1000 hr are obtained for specific temperatures. Alloys are then rated for a particular application on the basis of their rupture strengths at the rupture life that most nearly represents the application. Inasmuch as stress rupture is an important criterion in rating heat-resisting alloys, it would be advantageous to know the quantitative dependence of the time lor rupture on stress, temperature, composition, and structure. In order to obtain this information, an investigation was made at the NACA Cleveland laboratory during the spring of 1945. The theory of rate processes was used because it has been found to apply to certain processes such as chemical reactions, viscous flow, and creep that occur at a definite rate for given conditions. It was thought that stress rupture was such a process. An equation was derived that gives, for a given composition and structure, the dependence of the time for rupture on stress and temperature. The investigation is part of a general program to provide information that will lead ultimately to the development of better alloys in order that the efliciency and power output of gas turbines used in aircraft propulsion can be increased. Theory The theory of rate processes will first be discussed as a general theory. It will then be shown that if stress rupture of heat-resisting alloys can be treated as a rate process, certain equations must be satisfied. Later sections will then show that these equations are satisfied. General Theory of Rate Processes The theory of rate processes5 developed by Eyring and others has been applied to chemical reactions as well as to other processes such as viscosity of liquids and diffusion. In every case in which rate-process theory can be applied, there is a small subdivision, so that the macroscopic process is the net effect of all the small processes. This smallest subdivision is called the "unit process." For example, in a chemical reaction the unit process is

Jan 1, 1948

By M. Cohen, R. T. Howard

It has long been realized among metallurgists that a fast, reliable method for the quantitative determination of the percentage of microconstituents in an alloy would be of great benefit in studies of equilibrium and transformation in the solid state. For example, Polushkinl has shown that the compositions of two coexisting phases in a binary system at a given temperature may be calculated very simply with the aid of two alloys lying in the two-phase field if the relative amounts of the two phases in each alloy can be determined. Recently, Grange and Stewart2 have traced the course of the austenite-martensite reaction in a series of commercial steels by making visual estimates of the percentage of martensite formed as a function of cooling temperature. The correlation of mechanical properties with structure, a subject of wide-spread current interest, is likewise dependent upon quantitative microanaly-sis. Yet, there are very few investigations described in the metallurgical literature, wherein methods of quantitative microscopy are employed. Usually, the relative amounts of the microconstituents are estimated in a qualitative or semiquantita-tive way. The authors were faced with this problem some time ago in studying the kinetics of austenite decomposition. Several aspects of this research could not be treated satisfactorily by other quantitative tools, such as specific volume,' magnetic,6 dila-tometric, electrical resistance7 or x-ray measurements.a It became necessary to find an impersonal quantitative method that could be applied to microstructures. Fortunately, it was noted that geologists and petrographers had coped with quantitative microscopy to a considerable degree in their attempts to evaluate the mineral contents of rocks. A number of excellent articles were found on this subject, and since they appear to be unknown generally to many metallurgists, the first part of the present paper is concerned with a review of the literature in some detail. With this survey as a background, the authors have adapted the so-called methods of point-counting and lineal analysis to metallography, as described in the second part of the paper. Austenite-martensite structures were selected for illustration not only because they are important in many ways, but because such fine intermixtures are notoriously difficult to estimate visually. Literature Survey Perhaps the earliest work on quantitative microscopic analysis goes back to Delesse9 (1848) who proved mathemati-

Jan 1, 1948