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By E. C. W. Perryman

On electropolishing, high-purity Cu-Sn and Cu-Sn-P alloys with more than 5 to 9 pct Sn were found to contain many grain boundaries with a ridge-and-furrow profile. The effect was not eliminated by solution treatment and was present at the new boundaries in recrystallized material. It could be produced by diffusing tin into the 3 pct Sn alloy and it is concluded that the effect is due to enrichment of certain boundaries in tin, or possibly in an impurity present in the tin, in solid solution. IN the hot working of tin bronzes, especially those with moderately high tin contents, considerable difficulty is frequently encountered from intercrystal-line weakness, which results in cracking at the edges in sheet on strip rolling and in the unsupported regions of the rod in rod rolling.' These difficulties are not at all pronounced with up to 3 pct Sn, but at 5 pct Sn impose serious limitations and at higher tin contents, especially if the phosphorus content is also high, they may become very severe. In some work carried out at the laboratories of The British Non-Ferrous Metals Research Association it was found that a notable lack of ductility in tension at elevated temperatures, associated with intercrystal-line failure, was characteristic of tin bronzes even of relatively high purity. That the intercrystalline fracture is not due to a brittle or molten impurity phase at the grain boundaries was shown by the fact that the temperature at which intercrystalline fracture first occurred decreased with decrease of rate of straining. Tensile tests on some commercial tin bronzes, reported by Goetzel,² show a similar fall in ductility with increasing temperature. As no visual evidence had been obtained showing that the grain boundaries of the tin bronzes were different from those in copper, a more detailed microscopical examination was carried out, and the results of this are given in the present report. Several workers"' have observed that electrolytic polishing is a powerful tool for detecting small amounts of a second phase and in particular for detecting high solute concentrations, "equilibrium segregation," at grain boundaries. Since it had been found that the suggested solutions for electropolishing bronze and the standard solutions for brass and copper did not give satisfactory results it was first necessary to find a suitable electropolishing solution.' Experimental Procedure Materials Used: The cast and wrought materials used for this work were the same as those used for the mechanical tests referred to above. They comprised 3, 6, and 9 pct Sn alloys without phosphorus and the same three basic alloys with 0.03 and 0.4 pct P. A 5 pct Sn alloy without phosphorus, of similar purity, was also examined. The basis materials were Chempur tin, high purity 15 pct phosphor-copper and cathode copper, and spectrographic analyses are given in Table I. Treatment: The cathode copper was first melted under charcoal, degassed by plunging marble chips beneath the surface, and cast through a coal gas flame into sand molds to produce a number of small ingots which after machining were of a suitable size for subsequent vacuum melting. Chill cast bars of the alloys, approximately 1¼ in. in diameter, were then made by melting and casting in vacuo, the tern-

Jan 1, 1954

By F. W. Glaser, Benjamin Post

A LTHOUGH most transition metals form a wide variety of boride compounds, the existence of only one zirconium boride, ZrB2, had been established prior to this investigation.' The crystal structure and some properties of a hitherto unreported zirconium boride, ZrB12, are described in this paper. Only one other dodecaboride of a transition metal, UB12, has been reported up to the present.' Chemical analysis of the new compound showed 44 pct Zr and 56 pct B, compared with 41 pct Zr and 59 pct B computed for ZrB12. The difference is within the range of error of the analytical method employed. ZrB12 shows marked metallic properties. It is obtained as a fine black powder. Measurements of electrical resistivity were made at —79°C, + 22°C and +64°C. At 22°C the electrical resistivity is approximately 60 microhm-cm. Over this range the temperature coefficient of resistivity is +0.00162. The thermal conductivity at room temperature is 0.122 watts per cm per "C. The product of the electrical resistivity and thermal conductivity is therefore 8.05, which is not far from the normal Wiedemann-Franz ratio (approximately 7.5 at room temperature). These measurements were made on hot pressed samples which were not always high density specimens. The hardness of ZrB12 on the Rockwell A scale varies between 92 and 92.5. Crystal Structure Determination Single crystals of ZrB12 of a size suitable for X-ray diffraction analysis could not be obtained and powder samples had to be used. Filtered Cu radiation was used throughout. Powder diagrams were indexed on the basis of a face-centered cubic unit cell. After correction for film shrinkage, a Bradley and Jay extrapolation³ to ? = 90" indicated that a, = 7.408 ±0.002A. The volume of the unit cell is 406.5A.V he assumption that there are four "molecules" of ZrB12 per unit cell leads to an X-ray density of 3.63 g per cc. The measured density is 3.7 g per cc (as measured by the immersion method). Relative intensities of reflections were determined by integrating the intensities of diffraction peaks using the count register of a North American Philips wide range spectrometer. Intensities measured in this way showed good agreement with photographic intensities estimated visually using multiple film techniques. The usual Lorentz, polarization, and multiplicity corrections were applied to the observed intensity measurements. There are striking similarities between ZrB12, and UB12. The unit cell of the latter is also face-centered cubic and contains four molecules. a, = 7.473, compared with 7.408 for ZrB12. The radius ratio rB/rU is 0.57; rB/rZr is 0.54. In both ZrB12, and UB12 the four metal atoms in each unit cell are in special positions; only the boron positions need be determined. The latter may be inferred from the extent to which diffraction of X-rays by the 48 boron atoms reinforces or weakens the diffraction by the metal atoms. This effect is relatively much greater in the case of the zirconium compound. In their determination of the crystal structure of UB12, Berthaut and Blum' assumed holohedral symmetry (space group Oh5 , Fm3m) and reported that the U atoms are in positions 4(a): 000; 01/2 1/2; ½ 0 ½ ; ½ ½; the boron atoms were reported to be in positions 48(i) with x = 1/6: ½xx; ½xx; x½x; x½x; xx½; xx½; ½xx; ½xx; x½x; x½x; xx½; xx½

Jan 1, 1953

By J. R. Long, T. R. Graham

THIS report is concerned with part of a series of investigations carried on by the Federal Bureau of Mines on alloys, particularly nonferrous alloys, made with electrolytic manganese. A broad general program instituted after commercial quantities of electrolytic manganese became available was necessary in order to compare the effects of electrolytic manganese with those of the ordinary commercial grades. Representative analyses of these two materials show the commercial manganese metal to contain up to 2 per cent iron, a maximum of I per cent silicon and 0.06 per cent carbon, while the electrolytic manganese rarely exceeds 0.01 iron, 0.02 sulphur, with no silicon or aluminum. In the literature, the emphasis has been largely on high-strength casting alloys containing up to 5 per cent manganese, and few data are available on wrought manganese alloys. These factors, coupled with the strategic position of copper and zinc, have given impetus to the Bureau's War Research Program for the development of alloys containing nonstrategic manganese for the purpose of supplementing or providing alternates for the more strategic metals. The alloy reported here was studied, along with several other ferrous and nonferrous alloys, as possible cartridge-case material, and was chosen after a review of the properties of the ternary alloys of copper-manganese-zinc. PRELIMINARY WORK In a cursory survey of this system, alloys ranging from 60 to 95 per cent copper, 0 to 50 per cent manganese, and 5 to 40 per cent zinc were investigated. The alloys containing 60 per cent copper were found to fall into the two-phase alpha plus beta region of the system, and since those containing 70 per cent would not permit a saving, only alloys containing 65 per cent copper were considered. The tensile properties of these 65 per cent alloys are plotted in Fig. I as a function of manganese content for annealed material and for four conditions of cold-work In the annealed condition the increases in strength and decreases in elongation are minor up to 15 per cent manganese; beyond this, the changes become more significant. In the cold-worked condition, the first 5 to 10 per cent of manganese appears to have the greatest strengthening, effect, the rate of increase dropping off as the manganese increases beyond this amount. These effects are more pronounced with moderate than with severe cold reduction. It is also interesting to note that while the elongation of annealed material drops regularly with increasing manganese, the elongation in the cold-worked state is relatively little affected by increasing manganese content, particu-

Jan 1, 1944

By R.J. Anderson

Roughly, a crack in a casting may be considered, for the moment, to be due to fracture of the alloy resulting from the stress set up by the contraction in volume on passing from the liquid to the solid state. Cracks may be external or surface, internal or deep-seated, or incipient or so-called strain cracks. Draws may appear as depressions, unevenness, and "pinching in" of the surface of a casting. Roughly, draws are due to contraction in volume and are governed largely by the same factors as cracks. A casting may be cracked, however, without being drawn. Shrinkage is a foundry term and refers to the contractio~l in volume of a metal or alloy on passing from the liquid to the solid state. Patternmaker's shrinkage is the total contraction in volume (including liquid, solidification, and solid shrinkage) that occurs when an alloy is poured into a mold. The contraction in volume of aluminum is one of the principal factors affecting the occurrence of cracks, as will be shown later, and the question of shrinkage and its control requires careful study in any treatment of cracking in castings. In the case of sand and die castings, cracks have been attributed to a number of causes, but in the case of most light aluminum alloys, they are due to the large contraction in volume on freezing and the lack of its regulation or control. The most important factors are: (1) Contraction in volume; (2) composition of alloy; (3) quality of melting charge; (4) design of casting; (5) method of molding; (6) hardness of ramming; (7) method of gating; (8) hardness and characteristics of cores; (9) chills; (10) risers; (11) melting temperatures; (12) furnace used for melting; (13) pouring temperatures; (14) inclusions in alloys; (15) hot shortness of alloys; and (16) physical properties of alloys at high temperatures. Of these, the first, second, third, and eleventh to sixteenth involve ascertainable metallurgical facts; the remainder are largely matters of opinion, judgment, and technical knowledge of men experienced in the production of castings.

Jan 1, 1923

By R. J. Anderson

Roughly, a crack in a casting may be considered, for the moment, to be due to fracture of the alloy resulting from the stress set up by the contraction in volume on passing from the liquid to the solid state. Cracks may be external or surface, internal or deep-seated, or incipient or so-called strain cracks. Draws may appear as depressions, unevenness, and "pinching in" of the surface of a casting. Roughly, draws are due to contraction in volume and are governed largely by the same factors as cracks. A casting may be cracked, however, without being drawn. Shrinkage is a foundry term and refers to the contractio~l in volume of a metal or alloy on passing from the liquid to the solid state. Patternmaker's shrinkage is the total contraction in volume (including liquid, solidification, and solid shrinkage) that occurs when an alloy is poured into a mold. The contraction in volume of aluminum is one of the principal factors affecting the occurrence of cracks, as will be shown later, and the question of shrinkage and its control requires careful study in any treatment of cracking in castings. In the case of sand and die castings, cracks have been attributed to a number of causes, but in the case of most light aluminum alloys, they are due to the large contraction in volume on freezing and the lack of its regulation or control. The most important factors are: (1) Contraction in volume; (2) composition of alloy; (3) quality of melting charge; (4) design of casting; (5) method of molding; (6) hardness of ramming; (7) method of gating; (8) hardness and characteristics of cores; (9) chills; (10) risers; (11) melting temperatures; (12) furnace used for melting; (13) pouring temperatures; (14) inclusions in alloys; (15) hot shortness of alloys; and (16) physical properties of alloys at high temperatures. Of these, the first, second, third, and eleventh to sixteenth involve ascertainable metallurgical facts; the remainder are largely matters of opinion, judgment, and technical knowledge of men experienced in the production of castings.

Jan 1, 1923

By Hewitt Wilson

IN 1903, T. M. and E. H. Alvord, of Marblemount, Wash., built a soapstone-grinding mill in the Skagit River Valley and are reported to have produced "ground talc" during 1904 and 1905, shipping to the paper mills in Wisconsin. Between 1916 and 1920, the Western Talc Co. built and operated a talc-grinding mill north of Mondovi, on the banks of the Spokane River, in eastern Washington, and sold powdered talc to the Inland Empire Paper Co. of Spokane. ? The most active develop-ment in recent years has been by two companies in the Skagit Valley-the Skagit Talc Company, Inc., which has been sawing soapstone block for the soda-recovery furnaces of the pulp and paper companies, and the Asbestos-Talc Products of Washington, Inc., at Burlington, which has been mining and dry-grinding a soft serpentine for the structural filler and insulation trade. Many prospects have been opened in the northern part of the state on both sides of the Cascade Mountains, and these activities undoubtedly are the forerunner of an industry that promises to attain considerable magnitude in the North Pacific States. At the present time, talc is imported from California for use as paper filler, and soapstone block from Virginia for use in the soda-recovery furnaces. A small market has been created locally for tailor and foundry:, pencils, stove grills, and block soapstone for art objects. The results of the present study, as yet incomplete, indicate that the use as a refractory and as a ceramic filler and flux can be expanded.

Jan 1, 1936

Discussion of the paper of R. H. RICHARDS and BOYD DUDLEY, JR., presented at the New York meeting, February, 1915, and printed in Bulletin No. 97, January, 191.5, pp. 67 to 72. R. H. RICHARDS, Boston, Mass.-I believe that the manner of working for efficiency in almost all lines is to study the conditions of highest efficiency, and then to measure what is being clone. We can then see how near we have approached the highest efficiency. Spigots in practice often use many times the water theoretically needed. There are places where that is necessary for safety reasons. There are, however, places where it is unnecessary, and in these places it seems to me that this work of Mr. Dudley's will be a great help to the mill man to arrive at the greatest economy of water and highest efficiency. ALBERT R. LEDOUX, New York, N. Y.-A good many years ago I received a telegram from that distinguished engineer, Hamilton Smith, which simply said in substance: "I have discovered that liquids will flow faster from a square orifice than from a round orifice of the same area, under the same head." I wondered why he sent me the telegram, but some time afterward he told me that he had been making experiments along that line in Montana; that he thought the discovery was interesting

Jan 5, 1915

By Charles R. Austin, Carl H. Samans

In an earlier serics of studies on 18-8 stainless steel at 600º, 700º, and 800ºC.l one pretreatment was used throughout; viz., 15 min. in hydrogen at 950°C., followed by an air quench. Several manufacturers of this alloy since have expressed doubt as to the suitability of the temperature employed, recommending instead the more customary Strauss treatment as promising superior results. In this subsequent investigation on the effects of the temperature of pretreatment several interesting points have arisen, which are described in this paper. Previous work on our equipment had shown a marked difference between alloys of "similar chemical composition" that had been manufactured by different companies. Accordingly, one mill-bar length was selected from which to prepare all specimens. It could then be assumed that any marked differences in creep characteristics would be due to effects resulting from variations in the pretreatment of the alloy. The material was furnished by the Allegheny-Ludlum Steel Co. in the form of 5/16-in. dia. rod, finished by air cooling from a mill anneal at 1950°F. (1066°C.). It was analyzed only for the elements shown: carbon, 0.07 per cent; chromium, 18.73; nickel, 9.46; manganese, 0.40. Three pretreating temperatures were chosen, the specimens being held for 15 min. in hydrogen at either: (1) 1150°C., to conform to the recommended Strauss treatment; (2) 950°C., to compare with the results of previous tests; or (3) 75Q°C., to initiate precipitation of carbides in the material before testing. As the test cross sections were only 1/8-in. dia., air cooling followed the annealing treatment. These treatments permitted two direct comparisons: (1) between the 1150" and 950°C. treatments to indicate the effect of grain size when all carbides were probably in solution at the start of the test; and (2) between the 950" and 750°C. treatments to indicate the effect of carbide "nucleation" for similar grain sizes.

Jan 1, 1940

By Carl H. Samans, Charles R. Austin

In an earlier serics of studies on 18-8 stainless steel at 600º, 700º, and 800ºC.l one pretreatment was used throughout; viz., 15 min. in hydrogen at 950°C., followed by an air quench. Several manufacturers of this alloy since have expressed doubt as to the suitability of the temperature employed, recommending instead the more customary Strauss treatment as promising superior results. In this subsequent investigation on the effects of the temperature of pretreatment several interesting points have arisen, which are described in this paper. Previous work on our equipment had shown a marked difference between alloys of "similar chemical composition" that had been manufactured by different companies. Accordingly, one mill-bar length was selected from which to prepare all specimens. It could then be assumed that any marked differences in creep characteristics would be due to effects resulting from variations in the pretreatment of the alloy. The material was furnished by the Allegheny-Ludlum Steel Co. in the form of 5/16-in. dia. rod, finished by air cooling from a mill anneal at 1950°F. (1066°C.). It was analyzed only for the elements shown: carbon, 0.07 per cent; chromium, 18.73; nickel, 9.46; manganese, 0.40. Three pretreating temperatures were chosen, the specimens being held for 15 min. in hydrogen at either: (1) 1150°C., to conform to the recommended Strauss treatment; (2) 950°C., to compare with the results of previous tests; or (3) 75Q°C., to initiate precipitation of carbides in the material before testing. As the test cross sections were only 1/8-in. dia., air cooling followed the annealing treatment. These treatments permitted two direct comparisons: (1) between the 1150" and 950°C. treatments to indicate the effect of grain size when all carbides were probably in solution at the start of the test; and (2) between the 950" and 750°C. treatments to indicate the effect of carbide "nucleation" for similar grain sizes.

Jan 1, 1940

By R. L. Stephenson

The effect of fabrication variables on the creep-rupture properties of TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C), Cb-TZM [columbium-modified TZM (7140-1.5 pct Nb-0.5 pct Ti-0.8 pct Zr-0.05 pct C)], and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C) has been studied at 982º. 1093º, 1204º, and 1315°C for rupture times up to 1000 hr. The creep tests were performed in vacuum creep furnaces, employing cold-trapped oil-diffusion pumps, operating at pressures 2 X 10-7 tory. After-test chemical analyses showed no significant changes in interstitial content. The creep-rupture properties of TZM, fabricated according to current mill practice, were determined in the stress-relieved and in the re crystallized conditions to provide control data. Specimens of TZM, Cb-TZM, and TZC fabricated according to each of two experimental fabrication schedules were then tested. The schedules differed in terms of in-process annealing temperatures and warm -working temperatures. The data make several conclusions evident. Fabrication variables do indeed have a profound effect on the long-time creep-rupture properties of molybdenum alloys. Strengths of these alloys compare very favorably with those of other refractory metal alloys in the temperature range studied. FOR several years we have been engaged in the evaluation of the creep-rupture properties of promising refractory metal alloys. We consider the determination of these properties to 1000 hr at several temperatures necessary for a valid comparison. Such an evaluation indicated that the creep strengths of Mo-0.5 pct Ti and TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C) compare favorably with those of other refractory metal alloys. Tensile and recrystallization data of other investigators1,2 show an effect of fabrication variables. More specifically, those fabrication schedules which produce high strength through work hardening exhibit the least thermal stability. A similar conclusion was reported by perkins3 for Cb-TZM. This would lead one to expect that, in terms of creep, those materials showing higher strength at short times and low temperatures would exhibit lower strength at long times and high temperatures. If these expectations were fact, a substantial improvement could be made in these alloys by optimizing their fabrication schedule in terms of their anticipated service temperature. We therefore undertook a study of the effect of fabrication variables on the long-time creep properties of TZM, Cb-TZM (Mo-1.5 pct Cb-0.5 pct Ti-0.08 pct Zr-0.05pct C) and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C). MATERIALS All materials used were supplied by the Climax Molybdenum Co. of Mich. Our original intention was to test the same heat of each alloy in different conditions. Fabrication difficulties prevented this; however, heats with nearly identical analysis were selected. The compositions of the materials used are listed in Table I. All materials were supplied in the

Jan 1, 1970

By Walter L. Maxson, Fred C. Bond

THIS paper is a continuation of two earlier papers, l, 2 and presents new data on the grindability of various ores and other materials-the results of several years of intermittent research work on the nature of grinding and interpretation of test results. It is divided into five parts: 1. The tabulated results of several hundred grindability tests on a wide variety of ores. 2. A method of correcting screen analyses and calculating from them the surface and other properties. 3. A description of a new method of measuring the "surface energy" of an ore by pendulum impact tests. 4. Test results. 5. A general discussion of the test results and their application to grinding problems. 1. GRINDABILITY OF VARIOUS ORES This part is a continuation of the paper listed as reference No. 1. The method of testing is described in detail in that paper. The sample to be tested is crushed to all through 6 mesh in rolls set at x6-in. opening in closed circuit with a screen. Of this sample 700 C.C. is ground dry in a laboratory ball mill under constant conditions of mill speed and ball charge in closed circuit with a screen of the desired size at 250 per cent circulating load. The mill is cylindrical, 12 by 12 in., and rotates at 70 r.p.m. It contains a charge of 285 iron balls weighing 20,125 grams and ranging from 1 ½ to ¾ in. in diameter. Each test is continued for a sufficient number of periods to establish equilibrium at 250 per cent circulating load, or until the composition of the circulating load is constant for successive periods. Tests are conducted at the mesh size to which the ore is to be ground in practice, and the results are expressed as the net production in grams of screen undersize per revolution of the mill. This is designated as the

Jan 1, 1938

By R. G. Treuting, R. M. Brick

Despite the basic importance of slip in the plastic deformation of metals, and the considerable experimental investigation, thought, and speculation that have been devoted to the fundamental nature of these processes, surprisingly few data have been reported regarding the microscopic appear- ance and distribution of slip lines,‡ the external manifestation of the slip process. Photographs hitherto reproduced in the literature are in general at low or unspecified magnifications with no correlation to the prior shear. A single-crystal cylindrical tensile specimen of alpha brass about 1/2 in. in diameter, one of many previously prepared by H. L. Burghoff,1 was available for study. A plane about 3/16 in. wide, parallel to the specimen axis and normal to the plane containing the slip direction and the specimen axis, was ground and metallographically polished along the entire 5-in. gauge length. Heavy etching produced a surface free of both scratches and flow. The specimen was strained in tension until slip markings first became visible on the polished surface (Figs. 1 and 2). Re-stressing the crystal caused additional markings to appear at an initially lower stress than previously was required. Stretching the specimen to produce a dense concentration of slip lines caused such variations in level in the polished surface (normal to the slip direction) that microscopic study at higher magnifications became impossible. After annealing 15 hr. at 850°C, the specimen recrystallized to form two grains with a boundary approximately normal to the specimen axis and about midway along its length. Each was X-rayed, and two planes were again polished along the length of the specimen, in this case each parallel to the slip direction in one of the two crystals. A light longitudinal scratch parallel to the specimen axis was drawn down the center of each plane. A Huggen-berger extensometer was attached to the crystal A, whose slip plane would have the higher resolved shear stress of the two, and the specimen was again strained in tension.

Jan 1, 1942

By R. M. Brick, R. G. Treuting

Despite the basic importance of slip in the plastic deformation of metals, and the considerable experimental investigation, thought, and speculation that have been devoted to the fundamental nature of these processes, surprisingly few data have been reported regarding the microscopic appear- ance and distribution of slip lines,‡ the external manifestation of the slip process. Photographs hitherto reproduced in the literature are in general at low or unspecified magnifications with no correlation to the prior shear. A single-crystal cylindrical tensile specimen of alpha brass about 1/2 in. in diameter, one of many previously prepared by H. L. Burghoff,1 was available for study. A plane about 3/16 in. wide, parallel to the specimen axis and normal to the plane containing the slip direction and the specimen axis, was ground and metallographically polished along the entire 5-in. gauge length. Heavy etching produced a surface free of both scratches and flow. The specimen was strained in tension until slip markings first became visible on the polished surface (Figs. 1 and 2). Re-stressing the crystal caused additional markings to appear at an initially lower stress than previously was required. Stretching the specimen to produce a dense concentration of slip lines caused such variations in level in the polished surface (normal to the slip direction) that microscopic study at higher magnifications became impossible. After annealing 15 hr. at 850°C, the specimen recrystallized to form two grains with a boundary approximately normal to the specimen axis and about midway along its length. Each was X-rayed, and two planes were again polished along the length of the specimen, in this case each parallel to the slip direction in one of the two crystals. A light longitudinal scratch parallel to the specimen axis was drawn down the center of each plane. A Huggen-berger extensometer was attached to the crystal A, whose slip plane would have the higher resolved shear stress of the two, and the specimen was again strained in tension.

Jan 1, 1942

By Walter E. Duncan, Oscar F. Tangel, A. M. Gaudin, Franklin Dewey, R. A. Johnson

Xanthates have been used as collectors of sulfide minerals in the concentration of ores by flotation for over a decade, yet much remains to be done to elucidate the underlying reasons for the remarkable effectiveness of these compounds in this connection. Briefly stated, the known facts concerning the effect of these reagents on the floatability of minerals are as follows: 1. Xanthates are without effect on silicates, silica, and generally on minerals currently regarded as "gangues." 2. Xanthates in very small amount increase enormously the floatability of sulfides of copper, lead, silver, iron and mercury. 3. If zinc sulfides are first '(activated," as by treatment with a copper salt, they are readily floated by xanthates; otherwise not. 4. Elemental copper, silver and gold have their floatabilities increased by xanthates. 5. Sulfides of elements that are not typically metallic—e.g., stibnite, realgar, molybdenit—are not made to float markedly better by treatment with xanthates. 6. Oxidized minerals of lead and copper are floated if treated with large amounts of xanthates, but not so if treated with amounts of the same order of magnitude as required for sulfide flotation. Oxidized zinc minerals are not floated unless xanthates having unusually long hydrocarbon chains (e.g., eight carbon atoms or more) are used. Iron oxides and carbonate are not floated by xanthates. From a flotation standpoint the most striking feature about xanthates is the very small amount required to accomplish startling changes in the behavior of some minerals. The amounts used in practice to effect excellent concentration are frequently of the order of 0.05 lb, of agent per ton of ore; that is, of the order of one part of agent per forty thousand parts of ore. Changes in amount of agent of the order of 0.01 lb. per ton of ore (or 0.002 lb. per ton of pulp, on a 4:l basis) have marked effects on the metallurgical results obtained. Yet these changes represent a variation of but one part per million parts of pulp.

Jan 1, 1935

By F. G. Smith

A FEW years ago, the writer encountered a, problem that, at first, seemed to be due to peculiar conditions affecting grain growth. Large cups made from heavy metal failed in the first drawing operation in the process of making seamless tubes. The metal, as cast, appeared to be sound and strong; it rolled successfully and withstood the first cupping operation, but on the first draw it failed, with a crystalline fracture. The failure appeared in the slightly worked part of the bottom of the cup, and microscopic examination revealed exceptionally large grains. Knowing the general conditions governing recrystallization of brass, which were later published by Matthewson and Phillips, an investigation was outlined with the idea of including various conditions under which new grains might form, and which would include the effect that a previous anneal might have upon the anneal following. These conditions were produced by annealing specimens of brass at five different temperatures, indenting them with a 10-inn. ball under four different pressures, and then reannealing at each of the five temperatures five specimens each of which had been annealed at one of the five temperatures.

Jan 8, 1919

By R. L. Templin

THE increasing use of aluminum and its alloys in commercial fields has demanded a better understanding of their machining properties. This fact is exemplified by problems that have arisen in the automotive and airplane industries, but many in other fields might be cited. As pure aluminum and its alloys in their various commercial conditions show appreciable differences in their machining properties, it is not surprising that quite divergent solutions have been offered for the machining problems encountered. However, if the fundamental requirements of the most suitable cutting tools for these metals are understood, these machining problems lend themselves more readily to satisfactory solutions. Since the machining of free cutting brass and mild steel is understood by most persons accustomed to working these metals, it may serve our purpose better to first make a general comparison of the tools more commonly used in machining these metals with the tools most suitable for machining aluminum, then proceed to a more specific discussion of the individual tools. COMPARISON OF CUTTING TOOLS Cutting tools commonly used for machining free cutting brass usually have little, if any, top and side rake; they are ground on a medium to coarse abrasive wheel and used without any cutting compound or with a cutting compound that has a paraffin base. Those ordinarily used for steel have some top and side rake, are usually ground on a medium to fine abrasive wheel, and are often used with soluble-oil cutting compounds. The proper tools for aluminum and its alloys should have appreciably more side and top rake than the tools for cutting steel; should have very keen edges obtained by grinding with fine or very fine abrasive wheels supplemented in many cases by hand stoning with an oil-stone; and should be used with suitable cutting compounds whenever possible. In many cases, tools suitable for machining aluminum and its alloys are not appreciably different from tools commonly used for cutting hardwoods. The front clearance of a tool most suitable for machining aluminum and its alloys should be about 6°, the top rake from 30° to 50°, making the total angle of the cutting edge of the tool from 35° to 55°. A side

Jan 1, 1928

By R. E. Miner, J. K. Jackson, T. L. Wilson

THE nature of the decomposition reactions producing hardening in aluminum-rich A1-Ag alloys is now fairly well understood. The silver is not uniformly dispersed even at temperatures above the solvus line: rather, it is clustered into zones and associated with dislocations.' During quenching, nearly all of the silver segregates into zones' and some is attracted to dislocations, producing stacking faults. Growth of these faults produces the semicoherent y precipitate.1 During aging, the larger zones and the y precipitates grow at the expense of the smaller zones. The large zones persist up to about 350°C; where they redissolve in favor of the y' and y precipitates.' The equilibrium hcp y precipitate occurs both by a cellular reaction at the grain boundaries1 and by growth of the Y' plates to a critical size where incoherency results. Damask and Nowick 4 observed an internal friction peak in an A1-6 at. pct Ag alloy at about 140°C (0.25 cps). The peak was found to exhibit a systematic instability. After aging at successively higher temperatures between 155' and 23Z°C, the peak first migrated to higher temperatures while increasing in height, then returned to lower temperatures and decreased in height. After aging at temperatures above about 200°C, the peak position remained constant while the height decreased very slowly. In quenched specimens, elastic after-effect measurements inhcated a rapid initial transient in peak position from low temperatures up to 155°C. The authors concluded that a stress induced growth and resolution of the clusters and the 7' was the most reasonable mechanism to account for the behavior. It would seem, however, very unlikely that both the clusters and the y' precipitate would provide damping contributions whose relaxation time and activation energies were identical, which is required for them to produce the same internal friction peak. The present investigation was motivated by this apparent anomaly and the development of a very low thermal inertia torsion pendulum5 capable of monitoring transient behavior. Low frequency internal friction measurements were made on four binary A1-Ag alloys nominally containing 5, 10: 15, and 20 at. pct Ag. The results of measurements made on a 10 at. pct Ag alloy in the quenched condition are shown in Fig. 1. There are two peaks apparent in the spectrum, one centered at about 160°C, the second at about 210°C. The two peak spectrum was observed in each alloy, but it was best resolved in the 10 pct Ag specimens. Because of the instability in the internal friction, 4 it seemed possible that the second peak was not a peak at all, but simply a manifestation of a single, sharply transient, peak. This effect has been observed in Au-Ni alloys.6 The existence of the higher tempera-

Jan 1, 1970

By Paul A. Farrar, Harold Margolin

The system Ti-Cr has been re investigated From 40 to 100 pct Cr. The high-temperature modification of TiCr, was found to exist in the temperature range from 1365 where it terminates in the eutectoid reaction TiCr,(TI)* — HE chromium-rich region of the Ti-Cr system was investigated by Vogel and Wenderott,' Mc Quillan,' Van Thyne et dl.,' and Cuff Duwez and Taylor determined the crystal structure of the low-temeperature modification of TiCr, to be fcc a = 6.943A and Levinger' discovered the existence of a second (high-temperature) modification of TiCr, and determited its crystal structure to be hexagonal a = 4.932A, c/a = 1.617i. No information was obtained as to the temperature range over which each modification of TiCr? existed; therefore the present investigation was initiated. I) Experimental Techniques Alloys employed for the delination of this system were prepared from iodide titanium and high-purity chromium. The purity of these materials is as follows: Iodide titanium: purity 99.99 pct; major impurities—carbon 0.0001 pct; oxygen 0 to 0.002 pct; nitrogen 0 to 0.002 pct; silicon 0 to 0.005 pct; manganese 0.001 pct; copper 0.001 pct (Foote Mineral Co., Lot 609-29). Chromium #1: metallic purity 99.997 min.; interstitial content—oxygen 0.27 to 0.46 pct; hydrogen 0.028 to 0.038 pct; nitrogen 0.0002 pct (Ave-quipo Inc.). Chromium #2: purity 99.9 pct; major impurities—carbon 0.01 pct; oxygen 0.013 pct; nitrogen 0.02 pct; silicon 0.01 pct; sulfur 0.03 pct; iron 0.01 pct (Fulmer Research Institute Ltd.). A total of sixteen alloys of thirteen different compositions was prepared in the range from 40 to 95' *All percentages are given in weight percent. pct Cr. The compositions of the alloys prepared were as follows: Ti-40, 45, 50, 60, 62, 64, 66, 68, 70, 80, 85, 90, and 95 pct Cr. Two buttons were prepared of the 66, 90, and 95 pct Cr alloys. The 40 pct Cr and one of the 66 pct Cr alloys were prepared from the chromium # 2. All the other alloys were prepared from chromium #1. The alloys were arc-melted as 25-g buttons in a copper-hearth glass-walled furnace7 under an inert atmosphere of high-purity helium. The alloys were sintered at 250 amp and melted twice at 350 amp for 30 sec with the buttons being turned over between melts. Weight losses during melting were determined and in the range 45 to 68 pct Cr they were found, in all cases, to be less than 1.25 pct of the total alloy weight. A number of the high-chromium alloys shattered during cooling from either the first or second melt, which made the weight loss considerably larger than usual. The 70 and 80 pct alloys lost approximately 5.7 pct of their total weight, the 85 pct alloys 1.5 pct, the 90 pct alloy 2 pct, and the 95 pct alloy 3 pct. However, it is felt that the actual composition of the alloys in this region is probably within approximately 1 pct of the intended composition, as a large portion of the material lost was that due to shattering after melting. Nominal compositions were therefore used in plotting data and referring to the alloys. The alloys were cut into specimens, wrapped in molybdenum sheet, and encapsuled in argon-filled quartz or Vycor tubes for heat treatment. The heat-treatment times and temperatures are given in Table I. The specimens were quenched in iced brine (I.B.Q.) following heat treatment. The standard techniques of grinding, polishing., and etching were used in preparing the specimens for metallo-graphic examination. For alloys below 68 pct Cr

Jan 1, 1963

By D. R. Parrish, K. W. Beaver, H. W. Wood, R. W. Rausch

A pilot test of forward combustion in the Shannon pool, Salt Creek field, Wyo., is described. The Shannon sand, 950-ft deep, contains a heavy (25" API), viscous (76 cp) oil. Natural reservoir energy is limited. Primary production, intermittent since 1889, recovered only about 2 per cent of the oil in place. The field is operated by Pan American Petroleum Corp. for the Midwest Oil Corp., the owner. The original pilot was a 1.32-acre five-spot. The expanded pilot has eight producing wells surrounding a roughly triangular area of about five acres with the injection well near the center. A control or comparison well was also recompleted in another part of the field. Operation of the pilot has been little different front an ordinary gas drive. Little special equipment was found to be absolutely necessary. Except for some use of a temperature-resistant cement, all wells were conventionally completed. In spite of poor oxygen consumption, the over-all performance of the pilot has been good. Total oil recovery to June 1, 1961, was 73,971 bbl. The wells of the original pilot alone had produced about 24,000 bbl, equivalent to 50 per cent of the oil in place, when fire breakthrough at the first well occurred. These wells have now produced oil equivalent to more than 74 per cent of the oil in place in the original pilot area and production is continuing. It appears that ultimate recovery will approach theoretical maximums before the wells must be abandoned. Performance of the pilot has been encouraging, and expansion to a fieldwide combustion operation is being investigated. INTRODUCTION The results of both laboratory investigations and field tests of underground combustion have been reported previously.' However, most of the field tests were primarily experimental. More information and experience are needed before forward-combustion operations can be engineered with confidence. The purpose of this paper is to present the results of a successful pilot test of forward combustion. These re- sults should increase confidence in forward combustion as a practical method for commercial oil recovery. HISTORY OF THE SHANNON POOL The Shannon pool is located on the north end of the Salt Creek field in Natrona County, Wyo. It is approximately 50-miles north of the city of Casper. The Shannon pool's3 discovery well was completed in 1889, making this one of the oldest oil fields in the Rocky Mountain region. Three more wells were drilled in 1890. First production was hauled in wooden barrels by horse and wagon to the railroad in Casper. In 1894 a small refinery, the first in Wyoming, was built in Casper to process the Shannon crude. In the following years the field changed hands several times. It appears that each new owner did some development drilling as several wells were completed in each of the years 1895, 1902, 1905 and 1912, with negligible development in the intervening years. Forty-eight wells were drilled in this period, but many were later abandoned. Discovery of the more prolific Salt Creek field proper ultimately forced suspension of operations at the Shannon pool. After 1915 there was only sporadic production, mostly to supply cheap boiler fuel to drilling rigs in the Salt Creek field. But even this was discontinued in 1931. Since then the pool had been dormant until the recent operations, which are the subject of this paper. The Shannon pool is now owned by the Midwest Oil Corp. Field operations are conducted for Midwest by Pan American Petroleum Corp. THE RESERVOIR Fig. 1 is a map showing subsurface contours of the Shannon pool. The reservoir is on a nose of the Salt Creek anticline dipping to the north at about 500 ft/mile. The trap is provided by a shallow fault on the updip side of the productive area. The downdip limits are bounded by water, but this water has not provided an effective source of reservoir energy. The Shannon sand outcrops at many places in the immediate vicinity, providing good surface indications of the Salt Creek anticline. At the Shannon pool the sand has been lowered by faulting and is overlain by about 900 ft of shale and other sands. The Shannon sand consists of two members. The upper, a water sand, is about 40-ft thick and is separated from the lower member by several feet of sandy shale. The oil pay occurs in the lower mem-

By J. A. Ede

The object of the writer is to call attention to a rather unique aggregation of economic products distributed over a line of succeeding formations about 3 mi. long, to be seen within a few miles of La Salle, Ill. Fig. 1 is an ideal section of the stratification exposed and exploited along a distance of 3 1/5 mi. in a southwesterly direction from the quarry of the Utica Hydraulic Cement Co. located near the historic site of Kaskaskia village to the Oglesby shaft at Oglesby. No attempt has been made to cover the whole field, special mention only being made (with the exception of two places) of the operations found along the course or parallel to the direction assumed in the ideal section. I have used Fig. 2, after J. R. Bent and De Witt Kelly, to locate the relation of the La Salle anticline to the coal mines of this district and to show the operation of No. 1 and 3 mincs of the Illinois Zinc Co. Anticline and the Rock Formations Owing to the structural deformation between La Salle and Utica, the older rocks of the state are exposed to the surface along the northern embankment and the bottoms of the Illinois River valley near the latter place. At; the Illinois Zinc Co. works, Sec. 16, Tp. 33, R 1, a well for water mas sunk 1828 ft. and samples taken every 10 ft. of the ground penetrated; duplicates were sent to Mr. Cady of the Illinois Geological Survey. A general compilation or synopsis study of this section is here presented. As the well is over 1 mi. west of the Western limb of the anticline, the section affords some reliable data. These samples were studied and interpreted by H. M. DuBois as Lower Magnesian, and by G. H. Cady as the Lower Magnesian. The results are given in Fig. 3. The most interesting geological feature of this district is the La Salle anticline. In 1865, Leo les Quereux, looking at Split Rock, asked how it happened that the upper coal measures overlie strata of the Lower Silurian and what has become of the formations which are generally found intermediate—the Upper Silurian, the Devonian and sub-carboniferous, and the lower member of the coal measures?

Jan 1, 1920