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By B. H. Sage, W. N. Lacey, W. M. Morris

The volumetric behavior of isobutane at temperatures below its critical temperature has been studied by several investigators. Seibert and Burrelll measured the vapor pressure of isobutane from the ice point to the critical temperature. Dana and co-workers2 determined among other thermodynamic quantities the density of the saturated liquid and the saturated gas and the vapor pressure from approximately 0 to 130 F. Sage and Lacey3 studied a number of the thermodynamic properties of this hydrocarbon from 70" to 250" F. The specific volume in the gas and liquid region was determined at pressures up to 3000 Ib. per sq. in.? throughout this temperature interval. In addition, the vapor pressures were measured at 30" intervals. These data taken together serve to establish the thermodynamic behavior of isobutane at temperatures between 0" and 250" F. with reasonable accuracy. However, apparently there are no data available at the higher temperatures. For this reason an investigation of the volumetric behavior of isobutane at temperatures between 100" and 460" F. was carried out with apparatus that has been described in another paper (p. 136, this volume). Materials The isobutane used in this investigation was obtained from the Philgas Division of the Phillips Petroleum Co. That company's special analysis upon this sample indicated it to contain less than 0.03 mol per cent of impurities. In order to avoid traces of noncondensable gases, this hydrocarbon material was subjected to two successive fractionations at a high reflux ratio in a column approximately 4 ft. long and % in. in diameter, which was packed with small glass rings. The middle portion of distillate from the first fractionation was used in the second fraction-ation and a portion of the overhead from this second distillation process was repeatedly condensed at liquid-air temperatures at a pressure only slightly above the sublimation pressure of isobutane at this temperature.

Jan 1, 1940

By W. N. Lacey, B. H. Sage, W. M. Morris

The volumetric behavior of isobutane at temperatures below its critical temperature has been studied by several investigators. Seibert and Burrelll measured the vapor pressure of isobutane from the ice point to the critical temperature. Dana and co-workers2 determined among other thermodynamic quantities the density of the saturated liquid and the saturated gas and the vapor pressure from approximately 0 to 130 F. Sage and Lacey3 studied a number of the thermodynamic properties of this hydrocarbon from 70" to 250" F. The specific volume in the gas and liquid region was determined at pressures up to 3000 Ib. per sq. in.? throughout this temperature interval. In addition, the vapor pressures were measured at 30" intervals. These data taken together serve to establish the thermodynamic behavior of isobutane at temperatures between 0" and 250" F. with reasonable accuracy. However, apparently there are no data available at the higher temperatures. For this reason an investigation of the volumetric behavior of isobutane at temperatures between 100" and 460" F. was carried out with apparatus that has been described in another paper (p. 136, this volume). Materials The isobutane used in this investigation was obtained from the Philgas Division of the Phillips Petroleum Co. That company's special analysis upon this sample indicated it to contain less than 0.03 mol per cent of impurities. In order to avoid traces of noncondensable gases, this hydrocarbon material was subjected to two successive fractionations at a high reflux ratio in a column approximately 4 ft. long and % in. in diameter, which was packed with small glass rings. The middle portion of distillate from the first fractionation was used in the second fraction-ation and a portion of the overhead from this second distillation process was repeatedly condensed at liquid-air temperatures at a pressure only slightly above the sublimation pressure of isobutane at this temperature.

Jan 1, 1940

By E. R. Borcherdt

IT is notable that the first large-scale mine operation equipped entirely with detachable bits was the Badger State mine of the Anaconda Copper Mining Co. in Butte, Montana, just 30 years ago. This mine in 1922 was producing approximately 1200 tons of ore per day. Much of the data presented in C. L. Berrien's article' describing the development and installation of the Hawkesworth detachable drill bit were obtained from these operations. As in any pioneering effort, no precedent existed and many difficult problems required solution, so that the changeover to detachable bits at all Butte hill mines was not completed for 6 years. There was widespread disbelief as to the probable efficiency of the new installation. Some attempts were made in 1931 by the owners of the Hawkesworth patents to interest Ontario gold mine operators in the bit. These efforts were not successful, but they undoubtedly stimulated thinking which resulted in the invention and patenting of several well-known Canadian detachable bits, one of which is now a widely used throwaway bit. The success of the Butte installation also led to the development of the threaded type of bit connections by several well-known manufacturers, and in 1935 these bits were introduced to the mining industry on a national scale. The original Hawkesworth bit was not provided with a water hole but, depended upon water passing through the clearance opening between the tongue in the bit and the groove in the rod to flush cuttings from the drill hole, see Fig. 1. In December 1935 it was found that this method of introducing drilling water to the bit face resulted in high dust counts. To correct this a water hole was drilled on the central axis of the bit, passing through the tongue. Unfortunately, quenching water would rise through the small water hole, spot-hardening the tongue to cause breakage, never completely eliminated. In the fall of 1936 large-scale tests indicated that savings would be effected by use of a threaded type of bit, which was therefore adopted as standard for all Butte mines. This type of bit was used until 1947, when it was superseded by a one-use slip-on type. Since the first use of the Hawkesworth bit every detachable bit of importance has been investigated, and where advantages which might reduce costs or increase efficiency were indicated, substantial tests of the bit were carried on in the Butte mines. When tests demonstrated the advisability of changing from one kind of detachable bit to another the change was made at one level or in one area each day until the new rod and bit equipment was used throughout the mine. This involved a minimum of cost and disruption of drilling. Intelligent selection of a detachable bit to obtain optimum results requires careful consideration to achieve a balance between the three principal types of equipment used in the drilling process: 1—drill bits, 2—drill steel, and 3—drilling machines. Optimum results imply maximum output and minimum cost per unit of output. Since every rock type differs in drillability and it is generally impractical to provide equipment for more than one or two types of rock which may occur in one operation, selection of equipment must encompass average drilling conditions. However, on exceptional occasions several widely differing conditions may make it mandatory to provide equipment best suited to each condition. The choice of rock-drilling equipment is a most controversial subject and one that is further complicated by unreliable and frequently misleading performance claims. Small operators without the means for making accurate evaluations of equipment frequently suffer from these over-enthusiastic claims. It is apparent from experience in rock drilling throughout the world that rock drillability is not alike in any two places, and that selection of proper equipment can only be made after conducting thorough trials of various types of equipment. Some recent drilling tests in tactite and hornstone at the Darwin, California mine of the Anaconda Co. present some interesting clues on rock drillability. Microscopic examination of thin sections of these rocks reveals that mineral composition and rock texture are equally important in governing drillability. The Darwin hornstone is at times so abrasive that the carbide bit cutting edges become flattened to 3/32 in. in 2 to 4 ft of drilling, and some carbide bits were dulled to this point after 9 to 10 in. of drilling. This wear was determined to be the proper point for resharpening to eliminate carbide insert breakage or breakage of the steel rod when drilling with 1½ to 1?-in. bits, with a drifter of 2 3/4-in. diam and 90 to 100 psi air pressure, see Supplement A. Before considering the merits of various bit designs it may be well to review the mechanics of drilling rock with percussion drills. A sharp bit cuts by penetration and chipping. The amount of penetration governs the amount of chipping and depends upon the contact area of the cutting edge, the foot-

Jan 1, 1954

By Thomas R. Cunningham, A. B. Kinzel

Silicon, unfortunately, is not in the same category as some other metals with respect to the absolute value of the highest purity material prepared. Tucker, in England, and Becket, in this country have developed procedures for the purification of silicon, and Becket's process has made industrially available silicon of a purity of 99.8 per cent or better. However, even the term "silicon metal" may be a paradox to some people, although not more so than the term "amorphous" as applied to silicon. These terms come from commerce, and "metal" is used to distinguish industrially high-purity silicon from ferrosilicon, silicon-aluminum, and other high-silicon alloys. Alloys of iron and silicon with 95 per cent Si or less are known as ferrosilicon, with a designation of silicon content where necessary, arid the term "silicon metal" is invariably applied to the grades containing 96 per cent Si and higher. The Becket method of purification was referred to in a monograph on the Alloys of Iron and Silicon, and the Tucker procedure was described in some detail in that publication.' In order to get silicon of still higher purity, a sample, prepared by the Becket method, analyzing 99.84 per cent Si, 0.020 Fe, 0.016 Al, 0.005 Ca, 0.025 C, 0.033 per cent 02, 0.006 H2, 0.006 N2, and 0.001 per cent Mn, was crushed to pass a 100-mesh sieve and further purified by a modification of Tucker's procedure. This modification differs from Tucker's method in that after treatment the 100-mesh alloy was centrifuged to remove the last traces of acid. Our directly determined analysis of this purified sample shows: Si, 99.952 per cent; Fe, 0.009; Al, 0.012; Ca, 0.003; C, 0.006; or 99.982 per cent. Silicon by difference equals 99.97 per cent. The variation between silicon by difference and silicon as directly determined is important. Although Tucker mentions the amount of insoluble matter in commercial silicon both before and after his treatment, he does not mention the existence of carbon in the alloy; nevertheless, he reports silicon by difference. Any final figure as to purity obviously results from agreement between direct determination and

Jan 1, 1940

By A. B. Kinzel, Thomas R. Cunningham

Silicon, unfortunately, is not in the same category as some other metals with respect to the absolute value of the highest purity material prepared. Tucker, in England, and Becket, in this country have developed procedures for the purification of silicon, and Becket's process has made industrially available silicon of a purity of 99.8 per cent or better. However, even the term "silicon metal" may be a paradox to some people, although not more so than the term "amorphous" as applied to silicon. These terms come from commerce, and "metal" is used to distinguish industrially high-purity silicon from ferrosilicon, silicon-aluminum, and other high-silicon alloys. Alloys of iron and silicon with 95 per cent Si or less are known as ferrosilicon, with a designation of silicon content where necessary, arid the term "silicon metal" is invariably applied to the grades containing 96 per cent Si and higher. The Becket method of purification was referred to in a monograph on the Alloys of Iron and Silicon, and the Tucker procedure was described in some detail in that publication.' In order to get silicon of still higher purity, a sample, prepared by the Becket method, analyzing 99.84 per cent Si, 0.020 Fe, 0.016 Al, 0.005 Ca, 0.025 C, 0.033 per cent 02, 0.006 H2, 0.006 N2, and 0.001 per cent Mn, was crushed to pass a 100-mesh sieve and further purified by a modification of Tucker's procedure. This modification differs from Tucker's method in that after treatment the 100-mesh alloy was centrifuged to remove the last traces of acid. Our directly determined analysis of this purified sample shows: Si, 99.952 per cent; Fe, 0.009; Al, 0.012; Ca, 0.003; C, 0.006; or 99.982 per cent. Silicon by difference equals 99.97 per cent. The variation between silicon by difference and silicon as directly determined is important. Although Tucker mentions the amount of insoluble matter in commercial silicon both before and after his treatment, he does not mention the existence of carbon in the alloy; nevertheless, he reports silicon by difference. Any final figure as to purity obviously results from agreement between direct determination and

Jan 1, 1940

By W. A. Schaeffer, Sidney A. Justin, Jr. H. D. Easton

Restriction and proration of petroleum production have increased materially the difficulties attendant upon the estimation of reserves, particularly in large, "flush" fields. Such practices preclude the use of decline or other curves, from which, under capacity production conditions formerly prevalent, much could be learned as to the ultimate recovery to be expected from a given field or lcase therein. In restricted fields that would produce at many times the low rate allowed by the regulations in force if allowed to flow without restraint, one is forced to use other information than production performance to predict the volume of oil recoverable. Examples are: at Kettleman Hills, California; the Conroc, Van and East Texas fields, Texas; the Iowa field, Louisiana. It is beyond the scope of this paper to apply a definite method to the determination of the reserves in any actual field, therefore the discussion will be limited to a consideration of available methods and an enumeration of important factors governing the accuracy of such estimates. The problem is to determine not only oil in place but recoverable oil in place, for a given field or tract, which is complex and depends not only on the characteristics of the reservoir but also on the plan of development, the production allocation scheme, the rate of production and many other factors. Many data must necessarily be considered, weighed as to inportance, and assigned quantitative values. Estimates of recovery in prorated fields have been discussed by Brace', Shaw2, Snider3 and others. The wide difference in estimates of ultimate recovery from a number of important recently developed fields demonstrates the inadequacy of

Jan 1, 1935

By B. E. Fernow

MINING interests in the Western mountains are very seriously affected by the danger to property and life from destructive snowslides and avalanches. This is a danger which the miner has largely brought upon himself by an improvident stripping of the timber from the mountain slopes, and, therefore, he might be expected to take an interest in the reforestation of the areas thus devastated. A canvass was lately undertaken by the writer to ascertain approximately the extent of the damage suffered from this source, but the difficulty of obtaining reliable data has proved too great to permit, as yet, even an approximation. So much, however, is certain : that the loss of life is considerable, and that much property is destroyed almost every winter. True, neither the number of avalanches, nor their destructiveness, nor the amount of loss compares with what Switzerland experiences. This is due not only to the greater precipitousness of the Alps and to different climatic conditions, but also to the fact that in Switzerland a larger number of settlements is exposed to these dangers. A very complete and interesting official report on the very numerous and destructive avalanches occurring in Switzerland during the season of 1887-1888 has just been published as a contribution to the inquiry, whether and how these dangers can be averted. Peculiar weather-conditions, in addition to heavy falls of snow, were the reasons for the frequency of the phenomenon during that winter. This report records 1094 avalauches, by which 850 houses were destroyed or severely damaged; 84 persons and 752 cattle were buried; traffic on railroads and on highways was greatly interrupted, and the damage to personal property alone was valued at over $100,000. One of these snow-masses covered about half an acre, with a cone 250 feet in height. During the same year in Tyrol the number of avalanches was 3647. Of these 1355 run over permanent beds; that is, they recur annually, so that they are

Jan 1, 1890

By Courtenay de Kalb

So far as the writer is aware, no detailed investigation into the behavior of ores or rocks when subjected to crushing under digerent conditions has yet been made. He cannot himself claim to have carried such investigations very far; but the results of some studies which he has been pursuing for a couple of years, as opportunity permitted, seem sufficiently interesting and suggestive to warrant a brief statement of them, preliminary to nildertaking a more exhaustive course of experiments. Criticisms and suggestions are earnestly invited, with a view to making these studies as instructive as possible. As a part of the examination of ores, preparatory to concentration, my students have been required to take lots of 100 pounds each, and crush them. These are then screened through a series of hand-sieves, 15 inches in diameter. The products remaining on each screen are weighed, and from the results is plotted a curve, called the sizing-curve. It was assumed at first that different ores would yield, under like conditions of crushing, curves showing unlike characteristics as to the quantities remaining on the various sieves. After a number of such curves had been obtained it became evident, as often happens, that this a priori reasoning was faulty. The curves presented practically identical characteristics, and only by varying the crushing-conditions were variations in the curves obtainable. Another peculiarity, which was as little anticipated, appeared by inspection of these results, namely, that successive crushing to smaller sizes did not greatly augment the quantities of the filler products, so long as the machines employed applied the crushing-force to the ore-particles in the same manner. In these experiments the fines were not eliminated between successive crushings. I believe it will be readily admitted that rock can be crushed

Jan 1, 1899

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 Richard H. Willey

Efficient handling of large tonnages in open-pit mining demands, primarily, an abundance of well fragmented rock. To accomplish this, a drilling and blasting department composed of a well-knit, versatile group of workers and supervisors must be established. Some costs will remain relatively on the same level over a period of years, while others can be greatly lowered as will be shown. 'The Utah Copper Division, Kennecott Copper Corp., Bingham Canyon, Utah, has been ever alert for improvements in operating methods and equipment to gain increased efficiency and lower costs. Bingham Canyon MIne The greatest dimension of the mine is 8000 ft northeast-southwest with a width of 5000 ft southeast-northwest. From the lowest level, at an elevation of 6040 ft above sea-level, the mountain rises in 27 benches on the west side to W level (elevation 7800 ft) and 21 benches on the east side to Q level (elevation 7460 ft). At the inception of open-pit mining in 1906, the overcapping of leached porphyry had to be removed to reach a commercial grade of sulphide ore. The overcapping or waste now remaining is quartzite with intercalated limestone beds. The limestones are usually soft in nature except in the south-middle portion of the mine where they have been meta-morphized along the contact zone. This area usually gives drilling and blasting operations a great deal of trouble. Here occurs the greatest amount of secondary blasting, as the well-established fracture planes cause the altered beds to break into large boulders. Several massive quartzite "ribs" occur in the overburden, and as a result, the uniform breakage is difficult to obtain. The major quartzite areas have been subjected to complex folding, fracturing and faulting because of the intrusion of the underlying stock. The monzonite porphyry, which carries the commercial values, presents no serious drilling problem because of its softness and extensive minute fracturing throughout the mass. A series of major slips or faults pass through the ore body which, although of considerable advantage to the drilling and blasting department, sometimes works to the disadvantage of the track department. Drilling an11 blasting of the porphyry apparently becomes easier as depth is attained. but highly siliceous streaks throughout the pit still present difficulties. At no place is the rock of such character as to allow excavation without preparations. On certain higher elevations or levels, old fill material can be dug by the shovels, but only at some risk to equipment because of bank slippage. Past Methods At the outset of shovel operations in 1906, drilling was done with the Ingersoll-Rand F-24 piston drill mounted on an un-

Jan 1, 1949

By J. Eric Belford

The Kidd Creek orebody is a massive base metal sulphide deposit with surface dimensions of 168 m by 670 m. The steeply dipping ore- body has been evaluated to a depth of 1 524 m. To date, the mining of the orebody has been divided into three stages. The first stage of mining was an open pit operation which supplied ore from 1966 until 1977 when a depth of 219 m was reached at the widest or north end of the orebody. The second stage of mining, called No.1 Mine, was the development of an underground mine to replace the pit and recover the ore from the floor of the pit to a depth of 792 m. Development of the underground mine started in 1969. Full production of 273 000 tonnes per month was attained in 1977. The third stage of mining called No.2 Mine, was initiated to accommodate a production expansion and included the development of a second underground mining operation to recover the ore from the bottom of No.1 Mine, i.e. the 2600 level; to a depth as yet undetermined but most likely the 4600 foot level. Development of the No.2 Mine began in 1974. Full production of 91 000 tonnes per month will be achieved in 1982. The choice of the 2800 level as the partition between the two underground mines was based on the following factors: The 2600 level is the lowest level which can conveniently be mined through the No.1 Mine crusher on the 2800 level. Development and trial stoping methods for mining at depth could be evaluated in the 2600 to 2800 block utilizing the existing hoisting facilities of No.1 Mine. Early development of the ore in the 2600 to 2800 block would provide additional mill feed sooner than could be achieved by developing from No.2 Shaft. The underground mining plan then is to mine from the pit floor down to the 2600 foot level and at the same time mine from the 2800 level down to at least the 4600 foot level. PLANNING The Kidd Creek operations are designed to follow a logical mining sequence. The grade of ore supplied to the concentrator is the result of following the mining plan. The philosophy of mining has been to mine downward in horizontal slices. In the case of No.1 Mine the slices are 122 m thick while in No.2 Mine the slices will be 183 m thick. The point of this approach is to mine the pillars immediately after creating them rather than allowing them to stand, deteriorate and generate uncontrollable situations. Two types of ore are handled separately to optimize recoverable values in concentrates. The 'A' type ore is a copper zinc ore with some silver and little lead. The 'C' type ore is a zinc silver ore with some lead and copper

Jan 1, 1981

By D. M. Boulin, E. S. Greiner

Single crystals of vanadium were bent at 293" and 77°K to a maximum fiber strain of about 1 pct. Analysis of slip line and etch markings of- crystals deformed at either temperature show the slip planes are {112}. The slip directions at 298° and 77°K, deterwined from the asterism axes of rotation of crystals compressed in a {110} direclion, were (111). Etch pits, associated with dislocations, were observed in the plastically deformed vanadium. There was no evidence of mechanical twinning. THIS paper presents results on single crystals of vanadium plastically deformed by bending and compressing at 298° and 77°K. Bcc metals have been observed to slip on {110}, (1121, and (123) planes while the slip direction has invariably been found to be ( 111) 1 Lindley and smallman2 have studied the deformation intension of polycrystalline vanadium between 298° and 20°K and reported that at and above 77°K the deformation is predominantly by slip, but at 20°K the deformation is associated with twinning. Later, Edington and smallman3 found that single crystals of vanadium compressed in a (111) direction at 77°K deformed by twinning on { 112}( 111) systems. Clough and pavlovic4 have reported that mechanical twins were observed in vanadium loaded by impact at 77°, 173°, and 195°K, respectively. PREPARATION OF SINGLE CRYSTALS The vanadium single crystals were made from commercial vanadium reported to contain 0.03 pct C, 0.03 pct 0, 0.02 pct N, 0.0X* pct Ca, 0.0X pct Si, proximately 0.8 cm diam, 4 cm long and were grown in (100) and (110) directions. A crystal for studies of etch pits was gound to have a face parallel to a {l00} plane by the Bond crystal-orienting technique.7 In order to avoid straining, the crystals were placed on the steel mount with a low-melting organic compound (glycol phthalate) before grinding. Crystals for the bending experiments were ground to have the four side faces parallel to ( 100) planes. The crystals were electropolished8 in 10 pct H2So4 using a current density of about 3 amp per sq cm to remove the strained surface material. The crystals were bent slowly by three-point loading in a stainless-steel jig designed by Sylwestrowicz.9 The end rollers of the jig were 3.8 cm apart. DEFORMATION AT 298°K The bent vanadium crystal, after removal from the jig, had a radius of curvature of 20.4 cm over the 2-cm length close to the center loading roller, where the maximum bending moment occurred. This radius of curvature corresponded to a maximum fiber strain of 0.9 pet. The side faces contained slip bands as shown in Fig. 1. These bands are straight where the strain is high, top and bottom of micrograph, but are curved on either side of the neutral axis in the center. This curvature of the slip bands in the low-stress area may be due to cross slip. The plastically deformed crystal was subsequently electropolished and then electroetched in 10 pct H2SO4 solution, using a current density of 0.25 amp per sq cm. The structure is shown in Fig. 2. The directions of the traces on two adjoining faces were plotted stereo graphically, Fig. 3.* Since there were two sets of

Jan 1, 1968

By J. H. Jackson, P. D. Frost, C. H. Lorig, A. C. Loonam

THIS paper describes (1) the effect of sodium on the tensile ductility of magnesium-lithium base alloys, and (2) the precautions necessary to avoid sodium contamination. Effect of Sodium on Properties The harmful effect of sodium in magnesium-lithium base alloys has been recognized by other investigators.1,2 However, quantitative data on its effect have not hitherto been published. The effect of sodium on the ductility of an 87 pct Mg-9 pct Li-4 pct Zn alloy is shown in fig. 1. The sodium was introduced by adding sodium chloride to the flux, which consisted of 50 pct LiC1-50 pct KC1. Moderately high ductility was obtained at an indicated sodium content of about 0.05 pct. Actually, the value probably was less than 0.05 pct, be-cause analyses of the lithium, which were more accurate than those of the alloy, indicated that the highest ductility was obtained when its sodium content was 0.02 pct or less. In fact, in alloys having somewhat greater strength than this particular composition, the sodium content of the lithium must be under 0.01 pct to avoid embrittlement. The effect of sodium on the ductility of several alloys having fairly low strength levels is shown in fig. 2. These alloys were melted with a flux containing 75 pct LiC1-25 pct LiF, to which various quantities of sodium chloride had been added. Sodium had no significant effect in pure magnesium but markedly decreased the ductility of the magnesium-lithium-zinc alloy, even though the alloy contained only 3 pct Li. As the lithium content of the binary alloys was increased, the ductility of the sodium-free alloys also increased. However, the effect of sodium on ductility became progressively more pronounced. Sodium raised the minimum hot-rolling temperatures, particularly those of the high-strength alloys, but its effect, in this respect, was less critical than its effect on tensile ductility. For optimum cold roll-ability, a low-sodium content was required. No deleterious effect of sodium on the stability of properties at slightly elevated temperatures was found. Control of Sodium in the Alloys Optimum ductility is obtained in the magnesium-lithium base alloys when sodium-free materials are used. Commercial lithium was formerly the chief source of contamination. Now purified lithium is usually available. When lithium of ordinary purity is used, the effects of sodium can be minimized by using a flux consisting of 75 pct LiC1-25 pct LiF. Bubbling nitrogen through the melt also helps remove sodium. The damaging influence of sodium on the ductility of the magnesium-lithium base alloys was observed very early in the alloy development program. The discovery came about as a result of chemical analyses made on the lithium used in the alloys. Ductile alloys had been made from lithium containing about 0.2 pct Na, whereas the lithium used in the brittle alloys contained about 0.9 pct Na. The first magnesium-lithium alloys were melted under commercial fluxes ordinarily used in melting magnesium alloys. These fluxes were unsuited for scavenging the contaminating sodium, and the resulting alloys were not ductile. Next, a flux containing 50 pct KC1-50 pct LiCl was tried. This was somewhat more effective but still was not satisfactory. After a number of different experimental fluxes had been investigated, one containing 75 pct LiC1-25 pct LiF was adopted. This flux made it possible to obtain good ductility in the alloys. The

Jan 1, 1951

By Fritz Wald, Martin Weinstein, Herbert E. Bates

ONE of the methods for preparing a fiber-reinforced composite is that of directional solidification of a eutectic melt. Its major drawback lies in the fact that the matrix in this case is a pure constituent (or a terminal solid solution of fixed concentration) and the ratio of fiber to matrix volume is fixed. Only very few, if any, pure metal matrices possess technically useful properties, and the necessity for alloying is the inevitable consequence of this fact. Nevertheless, structures similar to binary eutectic ones can be obtained in higher-order systems by pseudoeutectic reactions of a type where crystallites and a solid-solution matrix are simultaneously precipitated from a liquid.1"3 Trials to solidify such alloys directionally—the matrix consisting of a solid solution of chromium, nickel, and silicon and the reinforcing phase being Cr3C2— will be reported elsewhere.4 This note describes constitutional studies carried out primarily to determine -the position of the pseudoeutectic and further to insure that no undesirable reactions between the reinforcing phase and components of the matrix occur in the solid state at elevated temperatures. In the investigation it was specifically desired to reinforce a matrix which is as close as possible to the 80/20 Nichrome composition with Cr3C2 to insure good oxidation resistance and improve the strength at high temperatures. No konstitutional information on the quaternary C-Cr-Ni-Si svstem in the range of interest was found in the literature. Nevertheless, the two most important ternaries c-cr-Ni5 and have been completely investigated. On C-Cr-Si some investigations have been conducted,7"9 and C-Ni-Si was studied with a few alloys in the course of the present investination 9 Eight alloys were prepared to investigate the changes in the constitution of the ternary C-Cr3Ce-yNi eutectic5 with silicon contents up to 10 wt pct. Five alloys were made with varying chromium and carbon contents around compositions containing -60 to 70 wt pct Ni and 5 to 6 wt pct Si. The latter alloys were designed to locate the y(Ni-Cr-Si-C)-Cr3C2 pseudoeutectic reaction and to determine the maximum chromium content in solid solution compatible with a two-phase equilibrium between y and Cr3C2 only. The alloys were prepared from electrolyte nickel, semiconductor-grade silicon, high-purity chromium (99.999 pct pellets), and semiconductor-grade graphite. They were melted inductively in high-purity alumina crucibles under flowing argon. Twenty-gram charges were prepared and investigated by optical microscopy (including hot-stage investigations), X-ray powder methods, and electronmicroprobe analysis. The alloys were studied in the as-cast condition and also after a homogenization annealing treatment of 48 days at 900°C in evacuated quartz ampoules. The structures of all alloys based on the ternary eutectic plus silicon in the as-cast state consisted generally of an inhomogeneous solid solution and at least two other phases. Annealing of the alloys showed that the solid solution was homogenized but that an incomplete solid-state reaction had taken place in all alloys with silicon contents over 5 wt pct. This reaction is clearly visible in Fig. 1 around the large Cr3C2 crystals (gray areas). Below this concentration, the alloys consisted of a homogeneous matrix and precipitates of Cr3C2 plus graphite, Fig. 2. The Cr3C2 was entirely unreacted here. From these observations and subsequent X-ray and microprobe investigations, it was deduced that the

Jan 1, 1969

By Richard Borg

The partial molal free energy of Cd in each of the four intermediate phases, Cd3 Cu, Cd8 Cu5, Cd3Cu4, and CdCu2 is determined using the Knudsen vapor pressure technique. Measurements are made also within the two-phase regions, and thus the variation in FCd is now known across the entire phase diagram. The absolute values are all less the 2.0 kcal and increase regularly with increasing Cd concentration. The small absolute value of the free energy precludes the possibility of obtaining highly accurate values; nevertheless, the results are compatible with those previously reported for the liquid phase. Additional results are reported concerning the lattice parameters of the 6, E, and b phases. THE elements Cu and Cd combine to form four intermediate phases which are designated* and E and which include respectively the following inter metallic compounds: CdCu2, Cd3Cu4, Cd3 Cu5, and Cd3 Cu. The extent of each phase with respect to temperature and composition is shown in Fig. 1 which is the equilibrium diagram drawn according to Hansen.1 All four phases are brittle, and most probably are true intermetallic compounds. Only the crystal structure of the 6 phase has been thoroughly investigated.2,3 The structure is cubic and isotypic with y brass. The structure of Cd3 Cu has not been previously reported, It is hexagonal with a = 8.11 and c = 8.76 0.02Å and the structure is presently being determined.* The compounds Cd3 Cu4 and CdCu, have been each previously the subject of a single investigation. Cd3Cu, is presumed to be cubic4 with the space group Fd3m, whereas CdCu2 is hexagonal2 with the C14-type structure. Cu2 Cd is found by X-ray analysis to be hexagonat with lattice parameters a = 5.00A and c = 16.17Å. The material appears to be pure Cu2Cd as all reflections could be indexed on the basis of the single hexagonal structure. These values disagree with those of Kripyakevich and coworkers5 who report a = 4.96Å and c = 7.98Å. Their investi-

Jan 1, 1962

By David V. Ragone, James A. Craig, Richard E. Balzhiser

The Gibbs free energies of formation of UC2 and UC were measured by equilibrating two-phase mixtures of UC2 + C and UC, + UC with liquid bismuth. The measured equilibrium concentrations of uranium in the bismuth combined with available activity coefficient information yielded uranium activities in these two-phase regions. Measurements on UC2 were performed over the range 1015 to 1160 K and on UC over the range 1115° to 1165°K. The values obtained for UC2 are in excellent agveement with values determined using combustton calorimetry and low-temperature heat capacity measurements. The UC values are in fair agreement with the calorimetric values, differing by about 10 pct from the calorimetric determination. MUCH interest has been shown in the uranium carbides in recent years because of their potential as nuclear fuels. As nuclear reactor operating temperatures have been raised to increase thermal efficiency, new fuels have been required. The uranium carbides are of interest because of their high melting points, >2000°C, high thermal conductivity, and resistance to irradiation damage. The manufacture and use of uranium carbides are aided by a knowledge of their stability and reactivity under various conditions. In this regard the thermo-chemical properties of the carbides, i.e., heat capacity, heat of formation, free energy of formation, and so forth, are particularly important. A great amount of work has recently been done on the thermodynamics of the U-C system. Unfortunately, however, there has not been good agreement among the various investigations. This study of the free energies of formation of uranium monocarbide and uranium di-carbide in the temperature region 1100°-1200° K was undertaken to help clarify the situation. It should be noted that in the temperature range of this investigation, 1100°- 1200° K, the thermodynam-ically stable phase in equilibrium with graphite is U2C3, not UC2, Fig. 1. However, U2C3 is reported to be stable only under extremely low oxygen and nitrogen pressure. Although UC2 is metastable below 150O°C, it exists under most experimental conditions. It should also be noted that "UC," never exists as UC2 but with compositions near UC1.9. However, "UC2" will be used to designate the dicarbide phase except when the stoi-chiometry is necessary for clarity. METHOD The approach taken in this study of the free energies of formation of UC and UC2 was to determine the thermo- dynamic activities of uranium in the two-phase regions UC, + C and UC + UC, by equilibrating the two-phase mixtures with the liquid bismuth. When a mixture of solid UC2 + C is brought to equilibrium with liquid bismuth, the reaction that occurs is: Neither carbon nor UC, could be detected as dissolved material in the bismuth. The standard free energy for this reaction may be written: In the two-phase region UC, + C, Fig. 1, the thermo-dynamic activities of UC2 and carbon are unity. The activity of uranium in this region was determined by measuring the concentration of uranium in a liquid bismuth melt in equilibrium with the two-phase mixture. This concentration was then used in conjunction with the activity coefficient data of uranium in bismuth reported by Tien et al.' to determine the activity of uranium in the two-phase region, UC, + C. All of the quantities in Eq. [2] were then known, and the AG; (uc,) was evaluated. UC + UC2. For the studies involving UC + UC,, the reaction taking place when the two-phase mixture is brought to equilibrium with liquid bismuth is: The standard free-energy change for this reaction is given by:

Jan 1, 1969

By AIME AIME

PRESIDENT OF THE COUNCIL. D. W. BRUNTON DENVER, COLO. (Term expires February, 1911.) VICE-PRESIDENTS OF THE COUNCIL. W. C. RALSTON SAN FRANCISCO, CAL. W. L. SAUNDERS NEW YORK, N. Y. H. V. WINCHELL MINNEAPOLIS, MINN. (Term expires February, 1911.) BENJAMIN B. LAWRENCE NEW YORK, N. Y. JOSEPH W. RICHARDS SOUTH BETHLEHEM, PA. ALBERT SAUVEUR CAMBRIDGE, MASS. (Term expires February, 1912.)

Nov 1, 1910

By R. E. Carter, C. Wagner, F. D. Richardson

By means of inert markers of radio-platinum, it has been shown that cobalt metal oxidizes by out-ward diffusion of cobalt atoms through the oxide. Oxidation rates have been measured at various temperatures and oxygen pressures and have been found to agree with the rates calculated from the Wagner equation and the authors' values for the diffusion coefficient of cobalt in the oxide. The distribution of radio-cobalt in growing oxide loyers has been accurately measured and found to be different from that predicted from the Wagner oxidation theory. Attempts have been made to measure the change of lattice parameter of the oxide with composition. SEVERAL investigators have shown that cobalt metal oxidizes according to the parabolic law,1-3 but no detailed study has been made of the oxidation mechanism. Cobaltous oxide has a metal-deficient lattice, but the defect concentration which is dependent on the oxygen pressure is only approximately known.' From the similarities in the structures of "CoO" and "FeO" and the rate laws governing the oxidation of cobalt and iron, Gulbransen- as suggested that cobalt, like iron," oxidizes by diffusion of cobaltous ions through the oxide layer. To substantiate this hypothesis, he has attempted to measure the oxidation rate of cobalt as a function of the oxygen pressure but has been able to report only that the rate depends on a "small" power of the pressure. On the other hand, Preece," Valensi,' and Arkharov' all have suggested from indirect evidence that oxygen diffuses through the COO to the metal-oxide interface. The present authors, in a previous paper,' have shown that the rate of diffusion of cobalt in cobaltous oxide is dependent on the oxygen pressure. In that investigation, they also found that cobaltous oxide disks made by complete oxidation of cobalt metal were porous at their centers (Fig. 5L, ref. 4). Both these facts strongly suggest that oxidation of the metal proceeds via outward diffusion of cations. In order to establish the mechanism unequivocally, oxidation experiments were made with inert radioactive platinum markers, and the dependence of oxidation rate on oxygen pressure was measured. In addition, an attempt was made to determine the form of the cation vacancy gradient, which the marker experiment showed must exist across a growing oxide layer. This was done by depositing radioactive Co on the surface of a cobalt disk and then measuring the tracer distribution across the oxide layer produced by partial oxidation of the metal. Finally, an X-ray examination was made in an attempt to find the expected change of lattice parameter of COO with oxygen pressure. Experimental The apparatus and materials used were substantially the same as those previously described by the authors.4 Marker Studies: The use of inert markers to follow oxidation reactions was first attempted by Pfeil" in 1929, and radioactive markers have recently been used by Davies et al.' In the investigation reported here, the markers were applied as an (NH4)2PtCI6 slurry in several thin streaks across both faces of four disks of cobalt metal 1 mm thick and 14 mm in diameter. The disks were then oxidized almost to completion at 1200°C in pure oxygen. After oxidation, they were mounted and sectioned and auto-radiographs were taken to locate the markers. Oxidation Rate: The oxidation rate of cobalt was measured at 1148°C at oxygen pressures ranging from 0.0055 to 1.0 atm and at 1000°, 1148", and 1350°C under 1 atm of oxygen. The rate was deter-

Jan 1, 1956

Plans for the Petroleum Division during the ensuing year are in process of development, in contemplation of the usual fall meetings in the Mid-Continent and California areas, as well as the annual meeting to be held in New York in February, 1936. Houston, Texas has been suggested as the place for the Mid-Continent fall meeting, the exact date to be announced shortly. During the past year, the Division's technical programs, as in former years, have emphasized the wide fields of engineering endeavor in the petroleum industry yet remaining for more thorough investigation and discussion. An effort has been made to bring an international interest into the proceedings of the Division by inviting the participation of prominent foreign technologists. This viewpoint should promote a continuation in 1935 of past high standards, afford a more thorough understanding of problems throughout the membership, and maintain the Institute's position among the various technical organizations functioning particularly in the oil-producing and refining areas. In the list of subjects proposed for the fall meetings is the problem of estimating petroleum reserves. Various factors requiring study will include productive sand volume, porosity, average permeability, saturation, and types of recovery. Research papers are proposed dealing with energy consumption per unit of oil recovered, reservoir pressure or energy loss relationship to the usual volumetric method of estimation, and the study of oil and gas segregation within the reservoir. Other subjects tentatively suggested include new casing practice in relationship to wells producing from several productive zones, progress in lifting methods, repressuring, advanced methods in drilling economies, and the economics of conservation. Although the threat of overproduction yet remains, to a lesser degree than during the past few years, intensive activity is now being directed towards the discovery of new petroleum reserves. This situation undoubtedly will influence, in some considerable degree, the channels through which technical activities will be directed. A continuation of the commendable work on production statistics for the various oil-producing states and foreign countries has been effected. The usual papers dealing with the general economics of the industry will be reserved for the annual New York Meeting. The Stabilization Committee maintains its membership of nationwide authorities, and interest is manifest in new developments to meet the changing requirements of the industry.

Jan 1, 1935