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By C. G. Dunn

This note describes a method for revealing micro-structures in tantalum through an {hkl} effect which was found during a study involving amorphous and crystalline tantalum oxides. Three steps are involved. First, an amorphous film of Ta2O5 is formed anodically1 on the surfaces of the tantalum. The amount needed depents on the thickness of the substrate tantalum; 1600Å of oxide, however, is generally satisfactory in the 1/2 -mil (12 µ) to 3-mil thickness range. The film at this point is uniform in color. Second, the anodized specimen is heated to 800°C in. vacuo during a period of a few minutes and held at temperature for 5 min. During such a treatment some oxygen leaves the oxide through dissolution into the substrate tantalum (e.g., at 10-8 Torr oxide films thinner than about 800 completely disappear on 5-mil strip). Considerable crystallization of the amorphous oxide also occurs adjacent to the metal/oxide interface but not throughout the oxide thickness. The thickness of oxide needed as a residue is not too critical; values between 500 and 1000Å (optical estimate') may be most useful. (The presence of a residual oxide layer after the heat treatment usually is not apparent; in fact, in most instances the surfaces have a metallic appearance. This can be the case also for thicker residual films needed in the detection of a crystalline oxide phase by surface X-ray diffraction—e.g., if the initial oxide film is 3000Å thick, enough crystalline oxide is formed for X-ray detection.) The third step eliminates the metallic appearance at the surface and reveals (or produces) a varied colored film of tantalum oxide. Two methods can be used and both will be illustrated. If the specimen is dipped in 48 pct HF for a few seconds, the tantalum is found to be covered with a multicolored oxide. Moreover the colors correlate with the grain structure of the substrate tantalum through an orientation dependence of the type illustrated in Fig. 1, where results of an orientation analysis by the Laue X-ray method have been plotted. Other film conditions would have provided a different set of colors for the same orientations. Any such correlation, however, provides a basis for a qualitative assessment of the distribution of orientations in a large sample. The cold-rolled structure of tantalum foil produced by a recrystallization anneal and a cold-rolling reduction of 95 pct is not easily obtained by usual metal-lographic methods.' The structure, however, is easily revealed by the present technique, Fig. 2. The alternative third step is to reanodize the specimen. The optical nature of the final anodic film depends on the presence of the crystalline oxide phase; color variations indicate optical thickness variations in the film. As the reanodization voltage is increased from zero, straw and light brown colors appear (as usual), followed now by variations in color from grain to grain depending on {hkl} orientation. Suitable end points, which are determined by voltage and time, are easily established. Fig. 3, for example, shows the grain structure developed in 5-mil tantalum strip during a 30-min re-crystallization and grap-growth anneal at 1800°C. An anodic film of 1600Å thickness was added prior to the special 800°C anneal. Reanodization was done at constant current density (near 0.2 ma per sq cm) in an aqueous solution of H3PO4 (0.01 pct) and was terminated after the initial brown colors were replaced by a deep blue at approximately 30 v. Although good grain contrast can be obtained with bright field illumination, even greater contrast for black and white micrographs may be obtained with polarized light, as in Fig. 3.

Jan 1, 1967

By F. R. Cattoir, R. W. Kimball, C. T. Anderson

ONE of the principal impurities in all steels is sulphur. Sulphur-bearing, manganese-free steels exhibit hot shortness. Manganese is added to steel to improve the hot-working properties. If no sulphur were present in steel, it is probable that hot shortness would be nonexistent. This paper is the first of a series to be issued by this Laboratory reporting the measurements of hot forgeability tests and the physical properties of Fe-C alloys to which additions of various alloying elements have been made. The present paper describes the results- obtained by the addition of varying amounts of sulphur to Fe-C alloys. To obtain control over residual elements in the various charges melted in the arc furnace, it was considered advantageous to use sponge iron from one source as the melting stock rather than scrap metal having an unknown history. Small amounts of unwanted alloying elements might be introduced into the charge when scrap was used, thereby influencing the results of the various heats. A sponge iron having a high silica-lime ratio was used. Ore from Sunrise, Wyo., had been reduced to sponge iron and briquetted at the Bureau of Mines sponge-iron plant at Laramie, Wyo. The briquettes were 5 in. in diam and 2 to 3 in. in thickness, and weighed about 10 lb each. The chemical analysis of the sponge iron is as follows: C, 0.67 pct; Mn, 0.10; SiO2, 4.75; CaO, 1.4; P, 0.044; S, 0.72; MgO, 0.4; A12O3, 1.1; total Fe, 87.5; Fe metallic, 79.2; and reduction, 90.5 pct. Where a reducing agent was required, crushed graphite electrodes usually were used. The charcoal available contained 0.20 pct S. An analysis of the available coke showed it to contain 0.70 pct S. Where high sulphur heats were required, elemental sulphur additions were made to the ladle. Limestone of good quality was obtained locally and had the following analysis: CaO, 53.7 pct; MgO, 0.8; ignition loss, 42.4; R2O3, 0.2; SiO2, 3.0; and P2O5, 0.014. Melting Procedure Sponge iron was melted to produce metal stock for the experimental alloys in a silica-lined, three-phase, direct-arc, size ST, Moore Rapid Lectromelt furnace with a 500 kva rating. Fig. 1 shows this furnace installation. About 25 tons of sponge iron was melted in 75 heats, averaging 927 lb of sponge iron to the heat. An addition of carbon was required to complete the reduction of a portion of the iron oxide remaining in the sponge to prevent high losses of iron oxide in the slag and a low carbon content in the resulting metal. As reducing agents in preparing the melting stock, charcoal, coke, and a carbon product resulting from the thermal decomposition of natural gas were used. The quantity varied from 20 to 60 Ib per furnace charge, with an average of 38 lb. An average analysis of the metal obtained gave 0.52 pct C, about 0.01 pct Mn, 0.070 pct P, and 0.092 pct S. The average yield of metal was 647 lb with 241 1b of slag, the sponge-iron recovery being 70 pct. The metal obtained in melting the sponge iron was cast into pigs weighing about 20 lb each to facilitate recharging into the furnace for further refining. The pouring of the pigs is shown in Fig. 2. The average power consumption for the production of the 24 tons of metal obtained was 1704 kw-hr per ton.

Jan 1, 1954

By P. Schwarzkopf, J. H. Brophy, J. Wulff

A constitutional diagram has been proposed for the tantalum-rhenium alloy system. Rhenium dissolved in tantalum up to 48 wt pct, and the maximum solubility of tantalum in rhenium is 5 wt pct. Intermediate x and s phases were found. X-ray diffraction, metallography and melting points were employed. SEVERAL investigators have described the phases present in the tantalum-rhenium alloy system, but no detailed account of the phase diagram prior to the present investigation appears to be available. Greenfield and Beck' reported the solubility of 48 to 54 at. pct Re in tantalum, a s phase at 41 at. pct Ta, and x phase isomorphous with a Mn from 37 at. pct Ta to less than 25 at. pct. They employed as-arc melted specimens and heat treatments at 1200 °C lasting 72 hr.2 Duwez3 reported the existence of a a phase at the composition Re3Ta2. Niemiec and Trzebiatowski4 observed a lattice parameter a = 9.69A, for the x phase at a composition Ta7Re22, but no s phase. Savitiski and Tylkina5 have shown a hardness maximum at the composition 40 at, pct Ta and a somewhat lower plateau from 35 to 10 at. pct. Knapton6 indicated results similar to those of Greenfield and Beck.' The present investigation describes the phase relationships in the tantalum-rhenium alloy system determined by melting point measurements, X-ray diffraction and fluorescence, and metallography. EXPERIMENTAL PROCEDURE Commercial 99.7 pct Ta powder from Fansteel Metallurgical Corp. and 99.9 pct Re powder from Chase Brass and Copper Co. were used for alloy preparation. The powders were weighed to desired nominal compositions and then pressed without binder into compacts weighing 5 or 10 g. The compacts were arc-melted six times on alternate sides on a water-cooled copper hearth using a nonconsumable tungsten electrode in an atmosphere of titanium gettered helium, at a pressure of 500 mm Hg. In most cases this procedure yielded alloy buttons of satisfactory homogeneity. A series of alloy specimens were analyzed wet chemically for use as standards for X-ray fluorescence. All specimens were analyzed by fluorescence and the results showed that the compositions differed by less than 3 pct Re from the original as-weighed nominal composition.* On the basis of self-

Jan 1, 1961

By John Henry Harden

WITH imperfect instruments it is impossible to make accurate surveys; the results are inaccurate maps, with their attendant consequences. The design of the writer is to describe an improved form of tripod head, and certain defects in an English transit and a miners' dial, with the method taken to remedy the defects of the transit. When the present transit superseded the surveyor's compass, there was one special objection brought against it, and with some show of reason ; namely, that the tripod of the compass with its ball and socket motion, allowed a quicker levelling-up (and, consequently, more work) than was possible with the transit. To this objection it was replied, that the ball and socket would not allow the instrument to be levelled with the same degree of precision that could be attained with the levelling screws, and that if time was sacrificed greater accuracy was attained. Nevertheless, it is a well-known fact that in this country, and especially in England, the compass or miners' dial holds its ground solely from its rapid adjustment. Ever since the introduction of the transit, efforts have been made to give to this instrument the same facility of levelling possessed by the compass or dial, and the same means have been tried, i. e., a . ball and socket motion, since a modification of this in some form was the only method that would answer. The upper part of a transit is, however, much heavier than the corresponding parts of a compass, and, therefore, requires more binding power, which cannot be ob¬tained with an ordinary ball and socket joint. It has been a study with instrument-makers to combine the facility of these two tripods -the quickness of the ball and socket with the steadiness and accuracy of the screws; but in all attempts in this direction the ball and socket of the compass has been literally followed, the entire stability of the instrument depending upon the friction of the ball in its socket. There is great need for a tripod that can be more easily manipulated than the present form, for it rarely happens that an engineer has a level surface on which to set his instrument, and very often

Jan 1, 1879

By T. Toda, R. Maddin

A study has been made of the microstructure and mechanical properties of splat-cooled aluminum-base gold alloys with gold concentration from 0.25 to 5.0 wt pct. These alloys have been quenched from the liquid state by a torsion-catapult technique, which has made it possible to pepare specimens suitable for mechanical property measwements. From the electron micrographs it has been shown that the solid solubility of gold in aluminum can be extended to 2.5 wt pct (0.35 at. pct) by splat-cooling, while the maximum equilibrium solubility is known to be less than 0.3 wt pct (0.04 at. pct). The very fine grain size (several tenths of a micron), the extended solid solubility, and the fine dispersion of a second phase (AuAl2) contribute concurrently to a substantial strengthening effect. In Al-5 wt pct Au splat-cooled specimens of less than 50 thickness, the yield strength is 17 kg per sq mm or 6 times as large as the strength of bulk specimens. For the Al-1.0 to 2.5 wt pct Au solid solution obtained by splat-cooling, the yield strength reaches 7.5 kg per sq mm after an aging treatment (for 10 hr at 200°C), while it is 3.7 kg per sq mm for the corresponding bulk specimens. A great deal of research has been done in recent years on the structure and the properties of metals and alloys rapidly quenched from the liquid state.' The term "splat-cool" has been used with the meaning of a rapid quenching from the liquid state., The splat-cooling techniques have produced large numbers of new structures, which are expressed in terms of metastable phases,3 concentrated solid solutions,4 amorphous phases,5'6 new phases,7 and so forth. Nearly all previous studies have concentrated on the physical properties; i.e., crystallography, structure, electrical resistivity, magnetism, and so forth, of the splat-cooled metals and alloys. The mechanical strength of splat-cooled metals and alloys has hardly been investigated except for some recent work by MOSS' on A1-V alloys. The principle common to all experimental techniques developed to obtain very rapid quenching rates is based on the heat transfer by conduction. Liquid must be in good thermal contact with a substrate of high heat conductivity. Both of the published devices known as the "gun" and the "piston and anvil" techniques suffer from certain shortcomings. For example, the specimen obtained by the gun technique is very small and flaky, and hence inadequate for mechanical properties measurements. On the other hand if the material is forced to yield a continuous speci- men by the piston and anvil technique, it is probable that some plastic deformation occurs during the quench. A novel method for rapid quenching of a liquid metal or alloy, the "torsion-catapult", has been devised by Roberge and Herman9 at the University of Pennsylvania. In the apparatus the melt is thrown out of a curved furnace by a catapult and impinges on a copper substrate. The apparatus has the advantage of producing a continuous foil which is relatively large in size and of a quality suitable for the measurements of mechanical properties. The quenching rate is estimated to be of the order of l05 to l06 ºC per sec, (comparable to rates achieved by the piston and anvil technique). In selecting an alloy to be studied we were made aware of the fact that gold was believed to be "insoluble" in in and consequently age hardening in the A1-Au system appeared to be interesting. Quite recently Heirnendahl13-15 revealed that the solid solubility, as determined by transmission electron microscopy, was 0.3 wt pct Au at 640°C and 0.25 wt pct Au at 600°C, decreasing with decreasing temperature. In an A1-0.2 pct Au alloy after quenching from a solution treating temperature of 600°C the yield stress was 2 kg per sq mm, and it increased up to 6 kg per sq mm after aging for 1 to 10 hr at 200°C. The precipitation occurred in the form of platelike particles mainly on (100) matrix planes. The intermediate phase n', the equilibrium phase n (AuAl2), and lattice relationships between both precipitates and the matrix were also investigated by electron microscopy. One of the purposes of the present research is to determine whether or not the solid solubility in this system, in which gold has a very small solubility in

Jan 1, 1970

By Goodman, Richard E.

A complete rational analysis for design of excavation slopes and loaded rock masses is a desirable but perhaps unattainable goal. Irregular external and internal boundary conditions, poor understanding of failure criteria for large masses of rock, capricious material properties, and the importance of indeterminate forces and inaccessible and virtually un- sampleable rock defects emphasize the importance of experience in this aspect of rock engineering. The experience must be correlated with geological factors. In certain regions the accumulation of such experience through the observation of existing rock slopes in various formations constitutes an important aspect of studies for design of rock excavations.

Jan 1, 1969

Henry Carlisle: This is June, 1961, and my friend Arthur Bunker is on the other side of the tape recorder. I, Henry Carlisle, am pursuing the hobby of chronicling the interesting parts of the mining careers and the lives of well-known mining engineers. Now, Arthur, supposing we skip, for the time being, where you were born and brought up, and start right in with where you went to school. Arthur Bunker: I graduated from Taft School and then went to Yale, Sheffield Scientific School, and took a course in electrical engineering. I was quite fascinated by higher mathematics and physics, and this offered more in mathematics and physics than any other one of the engineering courses at that time. The school was only a three-year course, and so I graduated from there in 1916.

Jan 8, 1963

By Bunting S. Crocker

EBBLE grinding at Lake Shore is not a temporary BlE wartime substitute. The tube milling plant, with a 1000 ton per day capacity, grinds a hard siliceous ore to 90 pct — 325 mesh. The plant, prior to using pebbles, was consuming 4.3 lb of 11/4-in. grinding balls per ton of ore, which amounted to 785 tons of balls per year. At September 1951 prices, $132.60 per ton, this steel cost amounted to $104,400 per year, or $0.285 per ton milled. By the Lake Shore method of substituting screened rock for this steel, all of this cost is saved. This is one of the major economies in Lake Shore mill practice. Regardless of the ultimate price of grinding balls, a change back to steel balls is not considered. The present pebble plant is more flexible than a steel ball plant and equally efficient. For example, if it is desired to change the size of grinding media, the pebble charge in any mill can be changed completely in 4 to 5 days, as against 76 days to change completely a 1-in. steel ball charge. To change pebble size it is necessary only to change two sets of screens and clean out the rock feed storage bin. This will take 8 to 10 days as against 3 to 4 months to clean out the customary supply of grinding balls kept on hand. Also it has not always been possible to purchase all desired sizes of balls at any price. In an analysis of savings effected by the use of the pebble mills, the flexibility of the Lake Shore grinding plant should be discussed, as it has a direct bearing on these savings. The plant has always used several units to handle tonnage rather than sending all the tonnage through a single unit. This principle may result in using small diameter mills, but no objection to that is seen. At no time has any advantage been found in cost per ton ground in large diameter mills. Both the capacity and the power of any mill varies as the diameter raised to the 2.6th power. Consequently large or small mills are equally efficient, and a plant, should be designed to use as many units or combination of units as is consistent with reasonable operating practice. Mills under 5 ft diam are harder to reline, etc. To define the case at Lake Shore, 2600 tons per day formerly were milled in seven 7x6-ft ball mills and twelve 5x16-ft (and two 6x16-ft) tube mills.* This gave an excellent test plant and an extremely efficient one. In this plant the ratio of ball mills to tube mills was 1:2. When the much cheaper pebble mills were substituted for the tube mills, this ratio was changed to one ball mill to four pebble mills to take the greatest possible advantage of the cheaper operating mill, i.e., the pebble mill. This flexibility without loss in efficiency has been an important item in the cost savings. It is interesting to note that the use of pebbles for fine grinding was proved first in the laboratory in a 12-in. ball mill. In fact, since 1934 all testing on — 8 mesh material has been done in this 12-in. mill. Scope of the Tests A paper on fine grinding at Lake Shore Mines was published in July 1940.' This paper covered 7 years of intensive research on fine grinding as well as sizing methods and equipment, plant scale grinding tests on 5x16-ft tube mills with and without grate discharges both with 1-in. and -in. balls, the use of laboratory mills to evaluate plant changes, and several reports on classifiers and classification. In the following July the addendum report2 was added in which the idea of series-circuit grinding was introduced, and the results of running five stages of tube mills and bowl classifiers were shown. Since 1940, the ball milling end of the plant has been altered extensively as a result of tests on the use of 3-in. rods in 7x6-ft mills and the use of the Tyler repulping screen with from 7 to 14 mesh screens. These tests are lengthy and may be covered in a separate report later. The scope of this report is confined to ore ground by rod milling and ball milling until it passed through an 8 mesh Tyler Ty-rod screen. The —8 mesh screen undersize then was pumped to a primary bowl classifier in open circuit and the sands from the bowl sent to the primary pebble mills, see Fig. 1. In the pebble mill circuit the ore is ground to 90 pct —325 mesh (24 pct + 28 microns). In studying the flowsheet, attention should be paid to the efficiency of the classification equipment used. The Tyler repulping screen is an efficient machine on the 8 to 10 mesh separation, and the bowl classifier is equally efficient at the 325 mesh separation. Efficient classification is a necessity for series-circuit stage grinding. The ore is hard siliceous porphyry, 60 pct SiO,, 80 pct insoluble. Its grindability at different meshes has been shown near the top of the list in F. C. Bond's grindability tests.' Lake Shore is not shown, but an adjacent mine with identical ore, Wright-Hargreaves, is. Reasons for the Changeover Since 1936 grinding balls have been rising steadily in price with no sign of stopping. For a mill that used 4.5 to 5.2 lb of grinding balls for every ton of ore ground this rise represented an alarming increase in grinding costs. In many cases the quality of the grinding balls fell off as the scrap steel became more difficult to obtain. The ratio of tube mills to ball mills increased with the use of the Tyler repulping screen in the ball mill circuit. Originally only 3.0 lb of balls per ton were used in the tube mills, and this

Jan 1, 1953

By Bunting S. Crocker

EBBLE grinding at Lake Shore is not a temporary BlE wartime substitute. The tube milling plant, with a 1000 ton per day capacity, grinds a hard siliceous ore to 90 pct — 325 mesh. The plant, prior to using pebbles, was consuming 4.3 lb of 11/4-in. grinding balls per ton of ore, which amounted to 785 tons of balls per year. At September 1951 prices, $132.60 per ton, this steel cost amounted to $104,400 per year, or $0.285 per ton milled. By the Lake Shore method of substituting screened rock for this steel, all of this cost is saved. This is one of the major economies in Lake Shore mill practice. Regardless of the ultimate price of grinding balls, a change back to steel balls is not considered. The present pebble plant is more flexible than a steel ball plant and equally efficient. For example, if it is desired to change the size of grinding media, the pebble charge in any mill can be changed completely in 4 to 5 days, as against 76 days to change completely a 1-in. steel ball charge. To change pebble size it is necessary only to change two sets of screens and clean out the rock feed storage bin. This will take 8 to 10 days as against 3 to 4 months to clean out the customary supply of grinding balls kept on hand. Also it has not always been possible to purchase all desired sizes of balls at any price. In an analysis of savings effected by the use of the pebble mills, the flexibility of the Lake Shore grinding plant should be discussed, as it has a direct bearing on these savings. The plant has always used several units to handle tonnage rather than sending all the tonnage through a single unit. This principle may result in using small diameter mills, but no objection to that is seen. At no time has any advantage been found in cost per ton ground in large diameter mills. Both the capacity and the power of any mill varies as the diameter raised to the 2.6th power. Consequently large or small mills are equally efficient, and a plant, should be designed to use as many units or combination of units as is consistent with reasonable operating practice. Mills under 5 ft diam are harder to reline, etc. To define the case at Lake Shore, 2600 tons per day formerly were milled in seven 7x6-ft ball mills and twelve 5x16-ft (and two 6x16-ft) tube mills.* This gave an excellent test plant and an extremely efficient one. In this plant the ratio of ball mills to tube mills was 1:2. When the much cheaper pebble mills were substituted for the tube mills, this ratio was changed to one ball mill to four pebble mills to take the greatest possible advantage of the cheaper operating mill, i.e., the pebble mill. This flexibility without loss in efficiency has been an important item in the cost savings. It is interesting to note that the use of pebbles for fine grinding was proved first in the laboratory in a 12-in. ball mill. In fact, since 1934 all testing on — 8 mesh material has been done in this 12-in. mill. Scope of the Tests A paper on fine grinding at Lake Shore Mines was published in July 1940.' This paper covered 7 years of intensive research on fine grinding as well as sizing methods and equipment, plant scale grinding tests on 5x16-ft tube mills with and without grate discharges both with 1-in. and -in. balls, the use of laboratory mills to evaluate plant changes, and several reports on classifiers and classification. In the following July the addendum report2 was added in which the idea of series-circuit grinding was introduced, and the results of running five stages of tube mills and bowl classifiers were shown. Since 1940, the ball milling end of the plant has been altered extensively as a result of tests on the use of 3-in. rods in 7x6-ft mills and the use of the Tyler repulping screen with from 7 to 14 mesh screens. These tests are lengthy and may be covered in a separate report later. The scope of this report is confined to ore ground by rod milling and ball milling until it passed through an 8 mesh Tyler Ty-rod screen. The —8 mesh screen undersize then was pumped to a primary bowl classifier in open circuit and the sands from the bowl sent to the primary pebble mills, see Fig. 1. In the pebble mill circuit the ore is ground to 90 pct —325 mesh (24 pct + 28 microns). In studying the flowsheet, attention should be paid to the efficiency of the classification equipment used. The Tyler repulping screen is an efficient machine on the 8 to 10 mesh separation, and the bowl classifier is equally efficient at the 325 mesh separation. Efficient classification is a necessity for series-circuit stage grinding. The ore is hard siliceous porphyry, 60 pct SiO,, 80 pct insoluble. Its grindability at different meshes has been shown near the top of the list in F. C. Bond's grindability tests.' Lake Shore is not shown, but an adjacent mine with identical ore, Wright-Hargreaves, is. Reasons for the Changeover Since 1936 grinding balls have been rising steadily in price with no sign of stopping. For a mill that used 4.5 to 5.2 lb of grinding balls for every ton of ore ground this rise represented an alarming increase in grinding costs. In many cases the quality of the grinding balls fell off as the scrap steel became more difficult to obtain. The ratio of tube mills to ball mills increased with the use of the Tyler repulping screen in the ball mill circuit. Originally only 3.0 lb of balls per ton were used in the tube mills, and this

Jan 1, 1953

By Bunting S. Crocker

PEBBLE grinding at Lake Shore is not a temporary wartime substitute. The tube milling plant, with a 1000 ton per day capacity, grinds a hard siliceous ore to 90 pct - 325 mesh. The plant, prior to using pebbles, was consuming 4.3 lb of 1 1/4-in. grinding balls per ton of ore, which amounted to 785 tons of balls per year. At September 1951 prices, $132.60 per ton, this steel cost amounted to, $104,400 per year, or $0.285 per ton milled. By the Lake Shore method of substituting screened rock for this steel, all of this cost is saved. This is one of the major economies in Lake Shore mill practice. Regardless of the ultimate price of grinding balls, a change, back to steel balls is not considered. The present pebble plant is more flexible than a steel ball plant and equally efficient. For example, if it is desired to change the size of grinding media, the pebble charge in any mill can be changed completely in 4 to 5 days, as against 76 days to change completely a 1 1/4-in. steel ball charge. To change pebble size it is necessary only to change two sets-of screens and clean out the rock feed storage bin. This will take 8 to 10 days as against 3 to 4 months to clean. out the customary supply of grinding balls kept on hand. Also it has not always been ' possible to purchase all desired sizes of balls at any price. In an analysis of savings effected by the use of the pebble mills, the flexibility of the Lake Shore grinding plant should be discussed, as it has a direct bearing on these savings. The plant has always used several units to handle tonnage rather than sending all the tonnage through a single unit. This principle may result in using small diameter mills, but no objection to that is seen. At no time has any advantage been found in cost per ton ground in large diameter mills. Both the capacity and the power of any mill varies as the diameter raised to the 2.6th power. Consequently large or small mills are equally efficient, and a plant should be designed to use as many units-or combination of units as is consistent with reasonable operating practice. Mills under 5 ft diam are harder to reline, etc. To define the case at Lake Shore, .2600 tons per day formerly were milled in seven 7x6-ft ball mills and twelve 5x16-ft (and two 6x16-ft) tube mills.* This gave an excellent test plant. and an extremely efficient-one. In this plant the ratio of ball mills to tube mills was 1: 2. When the much cheaper pebble mills were substituted for the tube mills, this. ratio -was changed to one ball mill to four pebble mills to take the greatest possible advantage of the cheaper operating mill, i.e., the pebble mill. This flexibility without loss in efficiency has been an important item in the cost savings. It is interesting to note that the use of pebbles for fine grinding was. proved first in the laboratory in a 12-in. ball mill. In fact, since 1934 all testing on -.8 mesh material has been done in this 12-in. mill. Scope of the Tests A paper on fine grinding at Lake Shore Mines was published in July 1940.1 This paper covered 7 years of intensive research on fine grinding as well as sizing methods and equipment, plant scale grinding tests on 5x16-ft tube mills with and without .grate discharges-both with 1 1/4-in. and 3/4-in. balls, the use of laboratory mills to evaluate plant changes, and several reports on classifiers and classification. In the following July the addendum report' was added in which the idea of series-circuit grinding was introduced, and the results of running five stages of tube mills and bowl classifiers were shown. Since 1940, the ball milling end of the plant has been altered extensively as a result of tests on the use of 3 1/2-in. rods in 7x6-ft mills and the use of the Tyler repulping screen with from 7 to 14 mesh screens. These tests are, lengthy and may be covered in a separate 'report later. The scope of this report is confined to ore ground by rod milling and ball milling until it passed through an 8 mesh Tyler Ty-rod screen. The -8 mesh screen undersize then was pumped to a primary bowl classifier in open circuit and the sands .from the bowl sent to the primary pebble mills, see Fig: 1. In the pebble mill circuit the ore is ground to 90 pct -325 mesh (24 pct + 28 microns) In studying the flowsheet, attention should be paid to the efficiency of the classification equipment used. The Tyler repulping screen is an efficient machine on the 8 to 10 mesh separation, and the bowl classifier is equally efficient at the 325 mesh separation. Efficient classification is a necessity for series-circuit stage grinding. The ore is hard siliceous porphyry, 60 pct SiO2, 80 pct insoluble. Its grindability at different. meshes has been shown near the top of 'the list in F. C. Bond's grindability tests' Lake Shore is not shown, but an adjacent-mine with identical ore, Wright-Hargreaves, is. Reasons for the-Changeover Since 1936 grinding balls have been rising steadily in price with no sign of stopping. For a mill that used 4.5 to 5.2 lb of grinding balls for every ton of ore ground this rise represented an alarming increase in grinding costs. In many cases the quality of the grinding balls fell off as the scrap steel became more difficult to obtain. The ratio of tube mills to ball mills increased with the use of the Tyler repulping screen in the ball mill circuit. Originally only 3.0 lb of balls per ton were used in the tube mills, and this

Jan 1, 1952

By K. O. Stamm, B. A. Rogers

Because it is the basis of the economically important operation of hardening steel by quenching, the A3 transformation in iron has been the subject of numerous investigations. Although the contributions to this subject are interesting, no general review will be given here. Readers who care to follow the matter further are referred to the comprehensive summary by Cleaves and Thompson,l which covers the literature to about 1935. Their references to 53 papers on the subject suggest that further investigation is hardly justifiable. However, considerable interest has devel oped recently concerning the reversibility of the transformation. From thermo-dynamic considerations, the transition ought to occur at the same point on heating or cooling, if the change of temperature is sufficiently slow. Yet all of the earlier investigators found a difference of several degrees. Burgess and Crowe,2 who used thermal methods, obtained average temperatures of 912" for Ac3 and 900°C. for Ar3 on electrolytic iron. Their data indicate a considerable range of temperature over which the change occurs, both on heating and on cooling. Terry3 measured the susceptibility in the critical range and estimated from the steepest parts of his curves that Ac3 came at 9I8° and Ar3 at 903°C. Ishiwara4 was one of the first investigators to report a shorter interval between the temperature of the change in the two directions. He measured the change of susceptibility of kaolin-coated samples of steel, in a hydrogen atmosphere, at rater of heating and cooling so low that about 3 or 4 hr. were required for the transformation to complete itself. His results show some variability between samples, but indicate that the difference between Ac3 and Ar3 is in the vicinity of 6°C. Roberts and Davey5 measured the space lattice in pure iron in the vicinity of 900°C. and concluded that a change occurs reversibly between 907' 3" and 910" 3°C., probably between 907" and 910°C. Wells, Ackley, and Meh16 made dilatometric determinations of the Ac3 and Ar3 points in samples of hydrogen-treated carbonyl iron maintained under a vacuum. They used three rates of heating and cooling: 2°, ½°, and .?°C. per min. and found the spread between the two points decreased with low rates. At the slowest rate, the Ac3 transition occurred at 909° to 909. 5°C. and the Ar3 change at 907°C. in three of the samples believed to contain the lowest percentages of alien elements. They concluded that if the rate of temperature change and the content of alien eiements were low enough, the A3 transformation would be completely reversible at 909.50 + 1°C. The question of reversibility is an interesting one and when some iron with especially small percentages of alien elements became available the opportunity to conduct an investigation was welcomed. This iron was prepared by the Division of

Jan 1, 1942

By B. A. Rogers, K. O. Stamm

Because it is the basis of the economically important operation of hardening steel by quenching, the A3 transformation in iron has been the subject of numerous investigations. Although the contributions to this subject are interesting, no general review will be given here. Readers who care to follow the matter further are referred to the comprehensive summary by Cleaves and Thompson,l which covers the literature to about 1935. Their references to 53 papers on the subject suggest that further investigation is hardly justifiable. However, considerable interest has devel oped recently concerning the reversibility of the transformation. From thermo-dynamic considerations, the transition ought to occur at the same point on heating or cooling, if the change of temperature is sufficiently slow. Yet all of the earlier investigators found a difference of several degrees. Burgess and Crowe,2 who used thermal methods, obtained average temperatures of 912" for Ac3 and 900°C. for Ar3 on electrolytic iron. Their data indicate a considerable range of temperature over which the change occurs, both on heating and on cooling. Terry3 measured the susceptibility in the critical range and estimated from the steepest parts of his curves that Ac3 came at 9I8° and Ar3 at 903°C. Ishiwara4 was one of the first investigators to report a shorter interval between the temperature of the change in the two directions. He measured the change of susceptibility of kaolin-coated samples of steel, in a hydrogen atmosphere, at rater of heating and cooling so low that about 3 or 4 hr. were required for the transformation to complete itself. His results show some variability between samples, but indicate that the difference between Ac3 and Ar3 is in the vicinity of 6°C. Roberts and Davey5 measured the space lattice in pure iron in the vicinity of 900°C. and concluded that a change occurs reversibly between 907' 3" and 910" 3°C., probably between 907" and 910°C. Wells, Ackley, and Meh16 made dilatometric determinations of the Ac3 and Ar3 points in samples of hydrogen-treated carbonyl iron maintained under a vacuum. They used three rates of heating and cooling: 2°, ½°, and .?°C. per min. and found the spread between the two points decreased with low rates. At the slowest rate, the Ac3 transition occurred at 909° to 909. 5°C. and the Ar3 change at 907°C. in three of the samples believed to contain the lowest percentages of alien elements. They concluded that if the rate of temperature change and the content of alien eiements were low enough, the A3 transformation would be completely reversible at 909.50 + 1°C. The question of reversibility is an interesting one and when some iron with especially small percentages of alien elements became available the opportunity to conduct an investigation was welcomed. This iron was prepared by the Division of

Jan 1, 1942

By R. H. Lynn, T. C. Craig

During the year 1933, in the Texas Panhandle, 113 oil wells were completed, adding 33,337 bbl. to the daily potential of the field. The field potential on Jan. 1, 1933, as determined by the Texas Railroad Commission, was 149,260 bbl., with a daily allowable production of 41,000 bbl. The potential was raised gradually, until on July 16, 1933, it reached 155,344 bbl. with a daily allowable of 55,000 bbl. This potential and allowable was maintained over a period from July 16, 1933, to Sept. 8, 1933, when the potential was reduced to 136,893, with a daily allowable of 43,727 bbl. Since Sept. 8, 1933, there has been a gradual increase, until on Jan. 1, 1934, the field potential reached 159,740 bbl. with a daily allowable of 42,000 bbl. Of this amount 26,429 bbl. arc "marginal oil" and 2682 bbl. are exempt on account of water. Deepening of Wells During the year 64 wells were deepened, increasing their total oil production 9631 bbl. per day. Of this amount the Gray County granite wash contributed 9256 bbl. from 57 wells. It has been found in many places that the granite wash carries an additional oil pay from 50 to 75 ft. below sea level. The majority of the wells that were .drilled during the early development in Gray County encountered their oil above sea level. When the wells producing from the upper horizon have become unprofit-

Jan 1, 1934

By W. E. D. Stokes

WHEN history is written, the year of the blitzkrieg will go down as giving aviation its greatest impetus. No perceptible drop in military business, even with cessation of hostilities abroad, seems likely. The combined air force of the U. S. Army and Navy on July 1 was approximately 5000 planes, as against 50,000 planes currently discussed as necessary. Observers at the fronts are giving designers and metallurgists back home some realistic ideas to shoot at. As conventional runways reveal the location of airports to enemy raiders, operating bases are now masked. Difficult, often muddy and rough landing strips, requiring strong landing gears and exacting take-off and maintenance characteristics, are the specifications of war. This is "old stuff" to numerous mining operators in mountainous jungle areas where gradients up to 8 per cent are in more or less common use in such mountain landing fields. Although airplane building is not readily adaptable to assembly-line methods, a trend towards mass productions is now in evidence. Incidentally, a U.S. Army "Curtiss P-40" requires about 10,000 man hours of work to complete and is tied together with 75,000 rivets. During the past year a number of aircraft factories adopted the "shot-

Jan 1, 1941

By R. A. Haney, S. J. Gigliotti

Over the past ten years, analysis of the acceptability of face ventilation systems has been based on numerical criteria rather than solely a study of air flow and methane patterns in the face area. This type of analysis has become possible primarily because of the instrumentation and mathematical models developed by the Ventilation Division, Pittsburgh Health Technology Center, Mine Safety and Health Administration (MSHA). To properly use these mathematical models, large amounts of methane and airflow data must be collected in the face area during mining activities. To supplement underground testing of face ventilation systems, a full scale model of a face area was built. This model includes a full scale model continuous miner, a face ventilation system, a gas release system, and a remote methane detection system. The remote methane detection system consists of an array of twelve methane sensors located throughout the face area. Data from the sensors are transmitted to strip chart recorders. Methane, air quantity, and other data collected during a test are entered into a computer for analysis. This paper presents the data entry system, the models used for data analysis, the test results, and the application of these results to a face ventilation system.

Jan 1, 1983

By Kenneth A. Gutschick, Robert S. Boynton

Lime has become a general and loosely used term to denote almost any kind of calcareous material or finely divided form of limestone or dolomite, as well as burned forms of lime. However, according to Webster, lime is only calcined limestone (known as quicklime, unslaked lime, or calcium oxide). It also embraces the secondary product of quicklime, i.e., hydrated lime or slaked lime (calcium hydroxide). There are two basic types of limestone used for lime manufacture-high calcium and high magnesium (dolomitic). The dolomitic quicklimes and hydrated limes correspond to their "high calcium" counterparts. The only difference is that the dolomitic types are a combination of the elements calcium and magnesium, in varying percents, whereas high calicum limes contain less than 5% MgO down to 1/2%. In either case a pure form of limestone of at least 97% combined carbonate content is needed to make salable lime, barring a few exceptions. The calcination of both types is diagrammed chemically as follows: [ ] In the foregoing reversible reactions the limestone is burned (calcined) in lime kilns, with the carbon dioxide content of the stone expelled as a gas. The weight loss during calcination of pure high calcium limestone is 44%; with equimolecular dolomitic limestone, the weight loss is 48%. Since lime has a strong affinity for CO_, particularly if moisture is present, it will readily revert to its original carbonate form. This occurs when quicklime "air-slakes" and adsorbs CO.. from the air. Thus, quicklime is perishable and should be stored in dry, water-tight areas. Depending upon the type of kiln used and the physical structure of the stone, the size of the quicklime may range from sandlike granules to 8 in. lumps. However, pebble sizes ranging from 1/4 in. to 2 in. are the most common. Screened quicklime fines are also com¬pressed (pelletized) into 1 in. pellets. For some purposes ground or pulverized forms of quicklime are used, ranging from No. 10 mesh to dust. Generally a pebble of quicklime is about the same size as the pebble of limestone before calcination (perhaps shrinking slightly). A more stable form of lime is hydrated lime. This is obtained by adding water to quicklime, slaking it into a dry, fine, subsieve size white powder. Because its affinity for moisture has been satisfied, it is not vulnerable to further moisture like quicklime. However, it has the same strong affinity for CO_. The following reversible chemical reactions illustrate how hydrated lime when heated (or dehydrated) can revert to the original oxide form:

Jan 1, 1975

By Arnulf Muan, R. E. Johnson

Equilibrium CO2 /CO ratios of a gas phase coexisting with selected oxide phase assemblages of the system CaO-"Fe0"-SiOz and vnetallic iron have been determined at 1080°C. The data obtained are used to calculate activity-conzposition relations for metasili-cute, orthosilicate, and CaO- "FeO" solid solutions, and to determine a new value for the free energy of formation of C&S&0,. The metasilicate solution is practically ideal, whereas large deviations from ideality exist in the othe,r two solid solutions. BECAUSE of the geochemical and metallurgical importance of the oxides CaO, "FeO", and SiOz, the system CaO-"FeO"-SiO2 has been the subject of several experimental studies during the past 30 years. Following the delineation of phase relations at liquidus temperatures by a group of investigators at the Geophysical Laboratory of the Carnegie Institution of Washington in 1933,1 Chipman and associates in the early forties2,3 determined activities of FeO in liquids of this system. Since that time, many attempts have been made to interpret the data of Chipman et al. in terms of the constitution of the silicate liquids and the interaction parameters among the various constituents of the system (see for instance papers by Richardson4 and by Flood and coworkers5). One of the assumptions made in some of these interpretations4 is that the binary silicate systems CaSiO3-FeSiO3 and CazSi04-Fe2SiO4 mix ideally in the solid state. The objective of the present study is to provide experimental data on activity-com position relations in solid solutions of the system CaO-"FeO"-SiO2. Such data will contribute toward an understanding of the thermodynamics of silicate solid-solution phases in general, and will serve specifically to confirm or refute some of the assumptions made in interpreting liquid slag behavior. PREVIOUS WORK Phase relations in the system CaO-"FeO"-SiO2 in contact with metallic iron were determined by Bowen, Schairer, and Posnjak,1 and additional phase-equilibrium data for this system have been presented by Allen and snow.' A reproduction of the most up-to-date phase diagram for this system is shown in Fig. 1.7'8 Of particular interest in the present investigation are the relations among the various crystalline phases slightly below the lowest solidus temperature in the system, as shown in Fig. 2. The present work will be concerned primarily with some of the composition

Jan 1, 1968

In the seven years that have elapsed since the AIME World Symposium on Mining and Metallurgy of Lead and Zinc, there have been a number of significant milling innovations and trends implemented in lead-zinc flowsheets to either improve grade and recovery or to control escalating mill costs. First, mill controls and instrumentation, which only had a foot in the door in 1970, have become increasingly common. In Australia, research into automatic crushing control has been implemented by Mount Isa Mines, and in virtually any large lead-zinc mill worldwide, an assortment of on-stream x-ray analyzers, grinding circuit controls, level detection devices, and reagent metering methods can be found. The increased circuit control offered to mill operators by this new technology points to more efficient flowsheets, as well as to a greater dependence upon computer-controlled operation.

Jan 11, 1977

By F. G. Miller, E. B. Wilson

In 1972, coal mine productivity was in steady decline and labor and maintenance costs were spiralling upward. Yet, despite this sad state of affairs, nowhere in the US at that time was there a comprehensive and coordinated coal research and development plan in the offing. The Bureau of Mines had not yet been charged with such a responsibility, and industry was content to rely on machinery manufacturers for innovations. It was during this period that Bethlehem Steel Corp. determined that a new approach to coal mining research was needed for the industry as well as for the company itself. After studying Bethlehem's own mining practices, the state-of-the-art of mining research elsewhere, and development work by manufacturers, a comprehensive research package was presented to company management in late 1972. The ideas and experience of many operating and management personnel in the company contributed to the formulation of the final plan as approved.

Jan 10, 1976

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