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By Enid C. Plante, K. L. Sutherland

Practical metallurgists are unanimous in stating that oxidation of mined sulphide ore adversely affects separation of the constituent minerals under standard conditions in a mill. Frequently, the need for different operating conditions in different plants is attributed either to the extent of oxidation of the mineral surfaces or to soluble oxidation products. The investigations reported in this paper study the effect of oxidation on the primary condition necessary for flotation, namely that of adhesion of an air bubble to the mineral. Oxidation Products from Sulphide Minerals Weinig and Carpenter1 state that the relative rates of oxidation of some sulphides are: FeAsS > FeS2 > CuFeS2 > ZnS > pbS > Cu2S tetrahedrite. They also show that oxidation is rapid at first, that sulphides of older geological formations are more stable than those of recent date and that mixtures oxidize more rapidly than any one mineral alone. The more rapid oxidation of mixtures is borne out by results of Gottschalk and Buehler2 who found that PbS, zns and cus oxidized 8 to 20 times faster when pyrite was present. Only the end products of oxidation, sulphate and the metal ion, were identified in these tests. Gaudin3 states that pyrite is difficult to oxidize in the laboratory. Winchell,4 using pyrite containing 99.98 pct FeS2, allowed water to percolate through a bed of this ground material. At the end of three months only a trace of Fe+++and So4- were found. Even after 10 months the quantity of Fe+++ was only 7.8 mg and SO4- 25.5 mg per liter of percolating solution. Car-michael5 confirmed Winchell's results on the slow oxidation of pyrite. Usually the oxidation of sulphide surfaces has been conducted in neutral or acid solutions, the acidity being caused by the oxidation products. Eliseev and Nagir-nyaka found that treatment of pure pyrite with lime gave only thiosulphate, but considered it possible that thiosulphate was obtained not by oxidation of the pyrite itself, but by oxidation of calcium disul-hide. Mitrofanov7 suggested that thiO~ulphate was formed by the following process: oxidation of sulphide to give free sulphur (this frequently happens with marcasite), followed by oxidation of the sulphur to sulphur dioxide and reaction of the sulphur dioxide with sulphur to give thiosulphate. Ferric and ferrous hydroxides, or similar compounds, were shown to be present. The Research Staff of the United Verde Copper Co.8 treated ore from the United verde mine with lime. Thiosulphate, sulphide and polysulphides were stated to be

Jan 1, 1949

By David B. Reger

The expansion of the previously discovered gas pools and an intensified search for additional pools in the Oriskany and deeper sands were the principal petroleum activities in West Virginia during 1941. One small oil pool was discovered and another was considerably extended. One small gas pool was discovered, several isolated well discoveries were expanded into definite pools, and various recognized pools were substantially increased. The proved oil territory of the state was increased about 600 acres and the proved gas territory about 45,000 acres. The new discoveries of oil did not equal withdrawals but gas reserves added were greater than gas withdrawals. Oil activity, as in the past several years, was slight because of unfavorable crude prices. Most operators prefer to leave oil in the ground rather than to drill for it without a better return. Gas activity increased greatly because of better demand, even though the price of gas did not improve. The account of operations, as gathered from trade journals and other reporting services, shows that 838 new wells were drilled, resulting in 114 new oil wells with 2606 bbl. of daily new production; 558 new gas wells with 949,226,000 cu. ft. of daily open flow; and 166 dry holes. Also, 86 old wells were drilled to deeper sands with 9 bbl. and 56,030,000 cu. ft. of added production. On the new wells the oil average was 22.86 bbl. per well per day; and the gas average was 1,701,000 cu. ft. per well per day. On new wells the ratio of dry holes to completions was 13.61 per cent. On deeper drilling to other sands the ratio of failures was 15.12 per cent. From an exploratory standpoint one strictly new oil pool (Higginbotham Run) was opened in Kanawha County and one strictly new gas pool (Lost Run) in Taylor County. One entirely isolated wildcat gave commercial Oriskany-sand gas production and may open a pool. Various other wildcats greatly extended the boundaries of known Oriskany-sand gas pools and various others may have opened new pools in the shallow sands. On the other hand, various Oriskany tests in Harrison, Monongalia, Roane and Wood Counties were dry and all five tests to the White Clinton sand (Sil.) in Boone, Harrison, Kanawha and Wood Counties failed to find commercial production. The principal oil wells completed, by counties, were: Calhoun, 24; Clay, 7; Gilmer, 6; Hancock, 9; Kanawha, 9; Pleasants, 10; and Ritchie, 14. Production for the year was estimated by the Oil Weekly as 3,421,000 bbl., compared with U. S. Bureau of Mines final figures of 3,444,000 bbl. in 1940. The leading counties in gas-well completions were: Boone, 32; Braxton, 19; Cabell, 16; Calhoun, 46; Clay, 20; Gilmer, 37; Jackson, 94; Kanawha, 82; Lincoln, 17; Putnam, 46; Ritchie, 33; Upshur, 20; and Wayne, 33. Production for the year is estimated by the author as 210,000,000,000 cu. ft., as compared to the U. S. Bureau of Mines' final figures of 188,751,000,000 cu. ft.* in 1940.

Jan 1, 1942

By David B. Reger

The expansion of the previously discovered gas pools and an intensified search for additional pools in the Oriskany and deeper sands were the principal petroleum activities in West Virginia during 1941. One small oil pool was discovered and another was considerably extended. One small gas pool was discovered, several isolated well discoveries were expanded into definite pools, and various recognized pools were substantially increased. The proved oil territory of the state was increased about 600 acres and the proved gas territory about 45,000 acres. The new discoveries of oil did not equal withdrawals but gas reserves added were greater than gas withdrawals. Oil activity, as in the past several years, was slight because of unfavorable crude prices. Most operators prefer to leave oil in the ground rather than to drill for it without a better return. Gas activity increased greatly because of better demand, even though the price of gas did not improve. The account of operations, as gathered from trade journals and other reporting services, shows that 838 new wells were drilled, resulting in 114 new oil wells with 2606 bbl. of daily new production; 558 new gas wells with 949,226,000 cu. ft. of daily open flow; and 166 dry holes. Also, 86 old wells were drilled to deeper sands with 9 bbl. and 56,030,000 cu. ft. of added production. On the new wells the oil average was 22.86 bbl. per well per day; and the gas average was 1,701,000 cu. ft. per well per day. On new wells the ratio of dry holes to completions was 13.61 per cent. On deeper drilling to other sands the ratio of failures was 15.12 per cent. From an exploratory standpoint one strictly new oil pool (Higginbotham Run) was opened in Kanawha County and one strictly new gas pool (Lost Run) in Taylor County. One entirely isolated wildcat gave commercial Oriskany-sand gas production and may open a pool. Various other wildcats greatly extended the boundaries of known Oriskany-sand gas pools and various others may have opened new pools in the shallow sands. On the other hand, various Oriskany tests in Harrison, Monongalia, Roane and Wood Counties were dry and all five tests to the White Clinton sand (Sil.) in Boone, Harrison, Kanawha and Wood Counties failed to find commercial production. The principal oil wells completed, by counties, were: Calhoun, 24; Clay, 7; Gilmer, 6; Hancock, 9; Kanawha, 9; Pleasants, 10; and Ritchie, 14. Production for the year was estimated by the Oil Weekly as 3,421,000 bbl., compared with U. S. Bureau of Mines final figures of 3,444,000 bbl. in 1940. The leading counties in gas-well completions were: Boone, 32; Braxton, 19; Cabell, 16; Calhoun, 46; Clay, 20; Gilmer, 37; Jackson, 94; Kanawha, 82; Lincoln, 17; Putnam, 46; Ritchie, 33; Upshur, 20; and Wayne, 33. Production for the year is estimated by the author as 210,000,000,000 cu. ft., as compared to the U. S. Bureau of Mines' final figures of 188,751,000,000 cu. ft.* in 1940.

Jan 1, 1942

By C. L. Mantell

ALTHOUGH SO common and well known a metal, tin is really a less abundant element than many of those less familiar and usually ranked with the scarce or rare elements, such as cerium, yttrium, lithium, beryllium., titanium, zirconium and vanadium. The color of tin is white, with a slightly bluish tinge. When it is compared with nickel, the latter metal is brown. When placed alongside of tin, chromium is definitely blue. Tin is whiter than silver or zinc. Exceedingly thin films of tin show various shades of brown by transmitted light. The metal has a brilliant luster, and when mirror-polished, has high light reflectivity. The luster depends to a large extent upon the pouring temperature at which the metal is cast. If the temperature be, too high, iridescent colors may show on the surface. These are the result of oxide film formation. If the pouring temperature be too low, the surface is dull. Small amounts of foreign metals, such as lead, arsenic, antimony and iron, decrease the luster of tin and impart a yellowish tinge to the metal. The structure is decidedly crystalline. The cast metal is a mass of crystals. When a bar of tin is bent, it emits a characteristic creaking sound. This is called the "cry" of tin, resulting from the grinding of the crystals one against the other during the bending of the metal. Tin metal may lose its crystalline structure by cold working, but grain growth occurs rapidly under the influence of heat. Metal which has been cast at a low temperature may become amorphous as the result of mechanical work. If such material be heated to temperatures well. below the melting point, say at 110° C. for a half hour or for a few minutes at 150° C. recrystallization occurs. If the surface of tinned plate, tin foil, or tin metal in cast form be etched with hydrochloric acid containing a little free chlorine, attack occurs at the intercrystalline faces. The surface shows patterns resembling the frost flowers on window panes in winter. The etched appearance is called moiré metallique. Fine dendritic surface crystals of tin may be obtained by casting the metal on a surface of polished steel. In commercial tin plate, the intercrystalline boundaries are shown by fine grooves or channels, which result from the method

Jan 1, 1929

By Albert G. Anderson

I'm sure many of you have wondered what the term "Cross Flow Filtration" means. I shall explain it so that you more clearly understand it, and I hope you will be able to make it a useful tool for you in the future. In the simplest form of cross flow filtration contaminated fluid. or feed stream, is fed at a high velocity down the center of a porous tube, clear fluid weeps through the porous wall of the tube while the suspended solids concentrate in and are swept away by the feed stream. (See figure A). The high velocity flow of the feed stream tends to keep the inside of the tube free from a build up of contamination. By utilizing this cross flow approach to filtration, we have been able to concentrate such things as paint pigments, titanium dioxide, iron oxide, precipitated metals such as uranium yellowcake or silver, cadmium, some metal hydroxides, as well as gelatinous particles such as yeast cells. You will recognize that cross flow filtration lends itself to a recirculation loop system due to the necessity of maintaining a high velocity on the inside of the tube. This means that we generally have a storage tank from which we are recirculating, and the solids will concentrate in the storage tank. (See figure B). The storage tank design becomes an integral part of the total system and is very important to the total function of the system. The cross flow filter system requires only low pressure, and will work with centrifugal pumps, diaphram pumps or in some cases no pump at all. As an example, if we wanted to filter a 10 GPM (37.8 liters/min.) stream that contained 1% of submicronic particulate, we would flow the 10 GPM (37.8 liters/min.) into the storage tank and recirculate through the filter at a flow of anywhere from 30 GPM to 100 GPM (113.6 to 378.5 liters/min.) depending upon the filterability of the particles from the liquid. As the contaminated fluid recirculates, the solids will build up in the storage tank and loop until they reach a level, which is dependent upon the design of the tank. Then the settling rate in the tank becomes equal to the amount of the solids being fed to the tank, and as a result you reach an equilibrium in the amount of solids being presented to the inside of the porous tubing. We have in effect created a dynamic settling tank or thickener. A flow of 10 GPM (37.8 liters/min.) of clear filtrate comes off for either recycle or disposal with periodic removal of thick mud from the bottom of the tank. The thick mud can be either processed through a centrifuge, a rotary drum filter. a flat bed pressure type filter, or other means. Often the small volume of filtrate from the mud de-watering stream can be recycled back into the recirculation tank so that any fines in the feedback are again concentrated, thus closing the loop on the continuous process 100% removal system. Cross flow filtration will not do efficient molecular separation. We work primarily with discrete solids but we do separate them totally from the liquid carrier fluid. I know some of you will raise your eyebrows when I say that we remove 100% of the particulate, but in measurement tests, we have measured the filtrate cleanliness with instruments that record as low as .05 ppm and the instruments read zero, so that it is less than .05 ppm.

Jan 1, 1980

By David Baker

A Discussion of the Paper of David Baker, read at the Lake Superior Meeting, September, 1904. (Washington Meeting, May, 1905.) MR. JOHN J. PORTER, Chicago Ill. (communication to the Secretary*) :-Mr. Baker's account of his experiences with stock-distribution has been particularly interesting to me, as it confirms the opinions which I had formed concerning the rapid failure of linings in several furnaces that have recently come to my notice. These furnaces, four -in number, are of modern construction, having been built or remodeled within the past two years, and are equipped with a well-known type of skip-hoist and double-bell charging-apparatus. In every case, a hot spot has developed within a few months after blowing-in, which has already compelled relining in two cases, and the probabilities are strongly against a long campaign in the other two. Since the hot spot in each case appeared in a position approximately opposite to the skip-hoist, and since the sizing, mentioned by Mr. Baker, is very apparent, it would seem as though there could be no doubt concerning the cause of the trouble. Nevertheless, there are some who cannot see it in that light; for the managers of two of these plants, at least, do not admit the existence of bad distribution, and have satisfied themselves by putting in cooling-plates, thickening the lining of the in-wall, and changing the brand of the fire-brick used for the construction of the walls. From observations of the clumping-action of the skip-hoist, and from subsequent inspection of the stock-distribution in the furnace itself, I arrived at the conclusion, some time ago, that no system of filling could be perfectly satisfactory where the stock is dumped into the hopper from one side, also that some

Mar 1, 1905

By J. M. Dahl, R. J. Warrick, O. K. Riegger, H. Van Vlack

A liquid which is rich in oxygen (and silicon) develops at steel rolling temperatures in resulfurized and plain-carbon steels. This liquid fluxes solid manganese sulfide. The composition of the liquid and the resulting microstructures vary with the manganese/silicon/oxygen ratios in the steel. The observations and conclusions zuhich are presented are used 1) to suggest a mechanism for MnS deformation in resulfurized steels, and 2) to rationulize hot-shortness anomalies between plain-carbon and resulfurized steels. 1 HIS is a summary of the dependence of sulfide inclusion microstructures upon steel composition, and an interpretation of the behavior of sulfide inclusions at steel-rolling temperatures. Sulfide inclusions are known to have several metallurgical effects upon steel. Their effects upon hot-shortness are best appreciated. Although hot-shortness is well known, it is questionable whether its mechanism is fully understood because there are several anomalies in our interpretation. For example, why should not high sulfur contents produce extensive hot-shortness in free-machining steels ? A second metallurgical consequence of sulfide inclusions appears because sulfide inclusions improve machinability. Furthermore, globular inclu- sions are to be desired over elongated inclusions. To date, we know that lower silicon contents (< 0.010 pct) favor the globular sulfides, but we do not know why this interrelationship between silicon content and inclusion shape exists. Finally, the evidence is strong that the surface quality of a hot-rolled steel is particularly sensitive to the sulfur content. SUMMARY OF PREVIOUS WORK The role of sulfur in hot-shortness was first suggested during the past century. It is uncertain who was the first to conclude that sulfur was less deleterious in the presence of manganese, and that manganese altered the sulfide phase from a liquid FeS to a solid MnS at steel-rolling temperatures. However, Urban and chipman&apos; emphasized that liquid FeS may accumulate as an interdendritic film during solidification. More recently, Keh and Van lack&apos; showed that the intergranular liquid does not completely surround the metal grains at all rolling temperatures. Rather, a small finite dihedral angle exists when geometric equilibration is attained at

Jan 1, 1962

By Michel T. Halbouty

The area for which oil and gas development is reported for 1938 in this paper is larger than that covered by the report for 1937, in that besides Duval, Jim Hogg, McMullen, Starr, Webb and Zapata Counties, comprising the Laredo district, this paper also includes the South Corpus Christi district, which is composed of the following counties: San Patricio, Nueces, Jim Wells, Kleberg, Kenedy, Brooks, Willacy, Hidalgo and Cameron, all heretofore included in A.I.M.E. Gulf Coast reports. In the map, Fig. 1, the area known as South Texas is represented by the counties south of the heavy black line. Production in the South Corpus Christi district, which covers an area that extends inland for 50 miles and follows the coast line, is primarily in zones ranging from the Catahoula, through the Frio sands, into the Vicksburg horizon. General exploration is done mainly with geophysics because in this district production is directly dependent upon structural conditions. In the Laredo district most of the production is from sand lenses; therefore, because these shallow sand lenses represent old shore lines which are monoclinic in character, the most satisfactory method of exploration in the Laredo district is drilling. This type of production centers around Duval County and follows a northeast-southwest trend along the Mirando district. Although drilling operations showed a decline from the preceding year, 1938 was highly successful as far as new discoveries and developments were concerned, and results of the year&apos;s operations should have an important effect on the near future trend of exploration and drilling. Besides the discovery of several new fields and many new sands in established fields, 1938 saw the discovery of a new Vicksburg sand trend and the first marine drilling off the South Texas Gulf Coast. Many new fields were discovered during the year, but only a few were subjected to an extensive drilling program. Several already established fields, especially in the Laredo district, received a large amount of drilling as new sands and extensions enlarged the producing areas, a

Jan 1, 1939

By Michel T. Halbouty

The area for which oil and gas development is reported for 1938 in this paper is larger than that covered by the report for 1937, in that besides Duval, Jim Hogg, McMullen, Starr, Webb and Zapata Counties, comprising the Laredo district, this paper also includes the South Corpus Christi district, which is composed of the following counties: San Patricio, Nueces, Jim Wells, Kleberg, Kenedy, Brooks, Willacy, Hidalgo and Cameron, all heretofore included in A.I.M.E. Gulf Coast reports. In the map, Fig. 1, the area known as South Texas is represented by the counties south of the heavy black line. Production in the South Corpus Christi district, which covers an area that extends inland for 50 miles and follows the coast line, is primarily in zones ranging from the Catahoula, through the Frio sands, into the Vicksburg horizon. General exploration is done mainly with geophysics because in this district production is directly dependent upon structural conditions. In the Laredo district most of the production is from sand lenses; therefore, because these shallow sand lenses represent old shore lines which are monoclinic in character, the most satisfactory method of exploration in the Laredo district is drilling. This type of production centers around Duval County and follows a northeast-southwest trend along the Mirando district. Although drilling operations showed a decline from the preceding year, 1938 was highly successful as far as new discoveries and developments were concerned, and results of the year&apos;s operations should have an important effect on the near future trend of exploration and drilling. Besides the discovery of several new fields and many new sands in established fields, 1938 saw the discovery of a new Vicksburg sand trend and the first marine drilling off the South Texas Gulf Coast. Many new fields were discovered during the year, but only a few were subjected to an extensive drilling program. Several already established fields, especially in the Laredo district, received a large amount of drilling as new sands and extensions enlarged the producing areas, a

Jan 1, 1939

By J. D. Grozier, W. W. Mullins, H. W. Paxton

The morphology of the nucleation and growth of austenite into high-purity iron in NH3-H2, gas mixtzires has been studied. The growth rate of an austenitic rim (planar interface) from scratched surfaces of- polycrystalline iron specimens was determined as a function of temperature and percent NH3 and found to he in reasonahle agreement with growth-rate calculations based on a model which assumes the diffusion of nitrogen to he the rate-controlling step. Under certain conditions, austenite pew as platelets; growth rates of these along the surface of single crystals were found to he dependent on surface preparation, orientation, THE development of microstructures can conveniently be thought of in terms of nucleation and growth. The complex topic of nucleation in solid-solid transformations will not be discussed at length, although a few qualitative experiments were performed. Growth is determined by the mobility of the various possible interfaces under the available driving forces in a particular situation. In homophase transformations, it has been clearly demonstrated that the mobility is very sensitive to small amounts of impurities, to the kind of impurity, and to the orientation relations across the boundary.&apos; A degree of quantitative knowledge has temperature and percent NH3. On electropolished surfaces with a (110) pole, the maximum growth rate of platelets was determined and found to be in agreement within a factor of 2 to 3 with theoretical calculations of the edgewise growth rate of a platelet. The calculations are based on a model which assumes that the diffusion of nitrogen in the ferrite in front of the moving curved attstenitic interface at the tip of the platelet is the rate-controlling step. The growth direction on the surface of the single crystal and resztlting habit plane of the platelets were determined and found not to he unique but to vary systematically with the pole of the surface. been obtained. In the case of heterophase transformations, which are significantly more complicated to treat, a comparison of theoretical and experimental studies often shows rather poor agreement.&apos;-&apos; The main purpose of the experiments discussed below was to obtain additional quantitative data on crystallographic effects on boundary mobility in a system which was otherwise as simple as possible, viz. the growth of iron-nitrogen austenite into fer-rite. In the course of the experiments, it became necessary to re-examine the theory for the growth of Widmanstatten plates, especially the influence of anisotropic interfacial free energy. Some other minor experiments in the Fe-N system were performed, and are described briefly. EXPERIMENTAL METHODS A) Material Preparation. The floating zone purified iron used for this investigation was supplied by Battelle Memorial Institute. The nominal composi-

Jan 1, 1965

By J. O. Betterton, W. M. Spicer

The solubilities of antimony in the a and ß-forms of zirconium were determined between 750" and 1300°C. The a-phase forms by a peritectoid reaction, and the a/(a + ß) and ß/(a + ß) phase boundaries rise in temperature with in- &apos; creasing antimony. Impurities in the 99.95 pct zirconium were sufficient to influence the phase boundaries and the variation reported is approximate. The restricted solid solubility of the terminal zirconium phases, which is especially characteristic of this system, is thought to result from the low free energy of the Zr2Sb phase. ZIRCONIUM-antimony alloys are important in zirconium alloying studies since antimony is one of the highest valent elements which can be used to make zirconium alloys. The dilute alloys are of further interest as they have somewhat better corrosion resistance&apos; than pure zirconium. The first investigation of the phase diagram was made by Russi and wilhelm2 who found a eutectic reaction, liquid (- 17.5 at. pct Sb) = ß zirconium (- 11 at. pct Sb) + Zr2Sb, at 1430°C&apos;. The Zr2Sb phase was of complicated hexagonal structure, and by thermal analyses of the relatively impure alloys then available, Russi and Wilhelm found evidence for the peritectoid formation of the a-phase. EXPERIMENTAL In the present work, the phase diagram was re-investigated in the region 0 to 5 at. pct Sb and 750" to 1300°C using iodide-zirconium alloys. Details of the procedure have been described earlier. Essentially the alloys were prepared by arc casting and were then examined by the annealing and quenching method. The times of annealing varied from 1 hr at 1300°C to 30 days at 760°C. As in other zirconium phase-diagram studies1"5 the impurities in the zirconium were still sufficient to affect the results, and the experiments will therefore be described in 3 parts. The results from the first 2 parts of the work are shown in Fig. 1. Here the ß/(ß + Zr2Sb) and a/(a + ZrzSb) phase boundaries were determined with alloys made from 99.9 pct zirconium,* and cast under such conditions that the Vickers hardness of a alloys extrapolated to 95 to 110 VPN at 0 at. pct Sb. Such alloys were not suitable for investigations of the (a + ß) region, and the results shown in Fig. 1 near the (a+ ß) and (a +ß + Zr2Sb) regions were determined with purer alloys. These alloys had an extrapolated hardness range of 75 to 85 VPN and were made from 99.95 pct zirconium. A deviation from binary equilibrium occurs in Fig. 1 as indicated by the (a + ß) region of pure

Jan 1, 1959

By Jean Howard

ThE formation of the (100) [001) texture in 3-1/4 pct Si-Fe strip was first reported by Assmus ef a1.l in 1957. Since then much experimental work has been carried out with a view to establishing the mechanism involved. The papers cited above state that the (100) [001] texture was developed in strip rolled from material melted and cast in vacuum. (The impurity content of the ingot is reported as 0.005 pct.) The present note records that similar results can be obtained in material processed by powder metallurgy. A processing schedule is described.which enables the texture to be formed in strip up to 0.010 in. thick, but there seems no reason why this should not be achieved in thicker strip, provided that large grains are developed after sintering. The materials were prepared from Carbonyl Iron Powder Grade MCP (particle size 5 to 30 p) of the International Nickel Co. (Mond) Ltd. The powder contains about 0.15 pct 0, 0.01 pct C, 0.004 pct N, <0.002 pct S, $0.005 pct Mg and Si, and 0.4 pct Ni— that is, it is substantially free from metallic impurities other than nickel, which is thought to be unimportant in the present work. The silicon powder was 99.9 pct purity, or material of transistor quality (ground in pestle and mortar). The mixed powders (3-1/4 pct Si to 96-3/4 pct Fe) are heated in hydrogen at 350" and 650°C to deoxidize the iron before sintering loose at temperatures between 1350" and 1460°C (depending upon the ultimate thickness of strip required) for up to 24 hr. The object of the high-temperature sinter is to develop a large grain size at this stage. Alternatively, the loose sintering can be done at a lower temperature followed by rolling or pressing and then annealing at temperatures between 1350" and 1460°C. Both methods produce large grains, which remain large throughout the process. The compact is then hot-rolled to approximately 1/8 in. with high-temperature interstage anneals if necessary. This step is taken to avoid intercrystalline cracking which would occur if the material of such large grain size were cold-worked. The bar is then annealed at 1050°C and reduced to its final thickness by approximately 50-pct reductions and 1050°C interstage anneals. Throughout the process the dew point of the hydrogen furnace atmosphere is maintained at about -40°C. Samples were annealed in hydrogen at various temperatures and times. Secondary recrystalliza-tion to (100) [001] was developed on the thinner material (i.e., up to 0.002 in.) by annealing in hydrogen at 1050" to 1200°C with a dew point of - 40°C or in vacuum (10-5 Torr) at 1050°C. With the thicker materials (i.e., up to 0.010 in.) the best results were obtained by annealing in hydrogen at 1200°C with a dew point of - 55°C. Complete secondary recrystal-lization to (100) [001] textures was obtained. Above these temperatures secondary recrystallization to (110) [001] tended to develop. The final annealing of samples was normally carried out with the samples placed between recrystal-lized alumina plates, but some experiments were performed with the samples suspended so that their surfaces were not in contact with anything except hydrogen, and these were equally successful in developing secondary crystals. An approximate determination of the proportion of material (before secondary recrystallization took place) having crystals with the (100) or (110) planes in or near the rolling plane showed that 11 pct of the sample had (100) and 16 pct (110). The method used for the determination is described below. A sample was annealed at a temperature just below the secondary recrystallization temperature and etched to reveal the (100) planes. The approximate area covered by crystals having (100) or (110) in or very near the surface was measured on the screen of a Vickers projection microscope. This was repeated for twenty positions chosen at random and a mean of the results calculated. The main hindrance to developing the secondary crystals in the thicker materials was the difficulty of obtaining a large enough initial primary grain size before secondary recrystallization. This was overcome by increasing the particle size of the silicon powder used. During the course of the work, it had been observed that the larger the grain size after sintering the more likely it was that the material would be successful in developing secondary crystals at a later stage. An experiment was therefore carried out to determine whether the material with the larger grain was more successful in developing secondary crystals due to the large grain produced at the sintering state per se or whether it was due to the greater reduction of silica brought about when the sintering temperature was raised in order to increase the grain size. A comparison was made between two compacts, one of which was made with silicon powder of 60 to 100 mesh, the other with silicon powder which was finer than 200 mesh. F?r this experiment, use was made of a phenomenon previously observed that the larger the particle size of the silicon powder employed in making a compact, the larger is the grain size of the compact. The silicon powder was ground

Jan 1, 1964

By K. Tanaka, J. D. Mote, J. E. Dorn

It) an attempt to ulLcoce.lP the operative strain-rate-contl-olliy: dislocation nieclzanistns, specially oviented sizgle clystals of the intel-nzediate 1zexagonal phase containing Ag plus 33 at. pct A1 were tested in tension over a wide range of temperatures. Slip was observed to take place by the {0001} <1120> {l100} mechani fracture took place across the(i100) plane and winning occurred by the (i01Z) ?lechanisn. Basal slip exhibited a strong yield point over the -alzge from 77 to 450°K, the upper ,esolved shear st]-ess having the exceptionally high value of 10,500 psi over this entire ?-a?zge of tenzpei,atuves. The critical 9-esolved shear stress for prismatic slip decreased f7-om 48,000 psi at 4.3"K to 23,000 psi at 170°K (Region 1) follozcirg zt:lzich it decl>eased sloz&ly to 21,500 psi at 475°K (Res&apos;on II); from 475" to 575°K (Regioz III), the c7-itical esolced shear stress dec&apos;-eased precipitously to 2000 psi; and from 575" to 750°K (Region IV) it decreased less afi&apos;dly to a low value of about 500 psi. Pvistintic slip in Region I was pobably controlled by the tliel-nally activated riecharzisui of nucleation and g,-ozcth of kinks in dislocations lying in Peierls potential troughs. In Region II for prismatic slip the critical 1-esolved shear stress was slzocn to be deteemined by sh0l.t-range 01-dering, Overall the forgiorz fo basal slip, 7.c.lre1-e a Strong yield-point phenorlienu ia7as observed, the critical vesolved slzea?-stress was shoztn to be determined by n conibirzation 0-f Szizuki locking and short-range-order Izavderzizg, The precipitous decrease in the critical resolved shear stress with increase in ter,/pe7-atrir-e over Region HI was tentatively ascribed to a decrease in the degree of slort-)ange 07-del;iqq (0)- clusteing) and also the effect of fluctuations the degree of o?der, It is at pgreser2t zrtzce)taitz as to 1t1hethe1- these or other possi1)le effects are also ,esponsible. fo- the data obsel-ved 172 Region IV. 1NTEREST in inter metallic compounds stems not only from their role in dispersion hardening of polyphase alloy ystems but equally from their potentialities for high strength, hardness, and stability not only at atmospheric temperatures but especially at elevated temperatures. As summarized in a re- cent symposium of the Electrochemical Society on "Mechanical Properties of Inter metallic Compound", most of the experimental evidence regarding the mechanical behavior of intermetallic compounds centers about the effect of temperature on the hardness and ductility of polycrystalline specimens. The available data reveal that the plastic behavior of intermetallic compounds might be rationalized in terms of the usual dislocation mechanisms appropriate to a solid solutions providing the additional complexities arising from crystal structure, long-range ordering, short-range ordering, and defect lattices are taken into consideration. It is apparent, however, in terms of the history on a solid solutions, that a complete detailed mechanistic rationalization of dislocation processes may not be possible until the deformation processes are studied in single crystals of intermetallic compounds. The present paper contains a preliminary report on the plastic behavior of single crystals of the hexagonal Ag-A1 intermetallic phase over a wide range of temperatures. The results confirm the thesis that single crystal data provide a most effective method of identifying operative dislocation mechanisms in intermetallic compounds. EXPERIMENTAL TECHNIQUES Several factors prompted the selection of the hexagonal Ag-A1 intermetallic phase for this preliminar investigation on the plastic properties of single crystals of intermetallic compounds: 1) This phase has a wide solubility range5 which would permit future investigations on the effect of composition and axial ratios on slip mechanisms. 2) Although it undoubtedly exhibits short-range ordering (or clustering) this intermetallic phase is free from complexities arising from long-range ordering.6 3) Since the atomic radii of aluminum and silver are practically identical, the possible complications due to Cottrell locking are minimized. 4)Whereas the dislocations on the basal planes are expected to dissociate into Shockley partials and are thus susceptible to Suzuki locking, those on the prismatic planes probably remain complete. 5) The axial ratio, being 1.61, is almost ideal, suggesting that short-range ordering may be almost spherically symmetrical. The present investigation was conducted exclusively with the hexagonal Ag-A1 alloy containing 33 at. pct Al. Preliminary investigations revealed that this alloy undergoes basal slip by the (0001)

Jan 1, 1962

By H. B. Probst

Mechanical twins were produced in zone-refined tungsten single crystals by explosive working at room temperature. These twins are parallel to (112) planes and have irregular boundaries rather than the classical plane twin boundaries. These boundaries aye grooved surfaces in which the grooves themselves are parallel to a <111> direction and the sides of the grooves appear to be par-allel to (110) planes. TWINS were produced in tungsten single crystals by explosive working at room temperature. These twins differ in character from any previously reported for tungsten; however, they are similar to those found in molybdenum after compression at -196°C.1 Deformation twins "resembling Neumann bands in ingot iron" have been observed in tungsten by Bech-told and Shewmon.2 This observation was made with sintered polycrystalline tungsten pulled in tension to fracture at 100°C and using a strain rate of 2.8 x 10-4 sec-1. More recently Schadler3 found deformation twins in zone-refined tungsten single crystals pulled in tension at -196"&apos; and -253°C. These tests were conducted using a strain rate of 3.3 x l0-4 sec-1, and the twin bands were found to be parallel to a (112) plane. Deformation twins in tungsten&apos;s sister metal, molybdenum, were observed by Cahn.4 These twins were produced by compressing small (0.7 mm) vapor-deproducedposited molybdenum single crystals at -183°C. The compression was performed &apos;by impact." By the use of precession X-ray techniques, Cahn was able to identify the twin plane as {112} and the shear direction as <1ll>. Mueller and Parker1 produced deformation twins in polycrystalline electron-beam-melted molybdenum by compression at -196°C. Their "loading rate" was 5000 psi per min which, judging from their stress-strain curve, corresponds to a strain rate of approximately 0.3 x 10-4 sec-1. These twin bands were found to be parallel to (1 12) planes; however, they differed in appearance from previously observed twins. In place of straight and parallel twin boundaries they were found to be irregular, jagged, and sawtoothed. The sides of the saw teeth were identified as (110) planes and irrational planes of a (111) zone. The twins observed in the present work in tungsten single crystals are similar in appearance to those of Mueller and Parker in polycrystalline molybdenum. The starting material used in this investigation was 3/16-in. diam commercial tungsten rod produced by powder-metallurgy techniques. This material was converted to a single crystal by the electron-bombardment floating-zone technique.= The process was carried out in a vacuum of 10-5 mm of Hg using a traversing speed of 4 mm per min. Segments (=2 in. long and 3/16 in. in diam) of two crystals (A and B) produced in this manner were studied. Crystal A received one zoning pass, while crystal B received two passes. The two crystals were explosively worked at Bat-telle Memorial Institute in the following manner. A 1/2-in.-thick layer of plastic was applied to the crystals to serve as a buffer in an attempt to prevent cracking. The composite, crystal and buffer, was then wrapped with 1/8-in.-thick DuPont sheet explosive EL506A2 and detonated in water at room temperature. Metallographic samples of the worked crystals were prepared, and back-reflection Laue X-ray patterns were obtained using unfiltered molybdenum radiation. RESULTS AND DISCUSSION Blasting the crystals as described above failed to prevent cracking. The crystals fractured into several fragments about 3/16 to 1/2 in. long; however, the fragments were of sufficient size to be useful for the subsequent study. The diamond pyramid hardness of the crystals after blasting was in the range 430 to 450 as compared with 340 for the as-melted material, which shows a definite hardening resulting from plastic deformation. These hardness values were obtained using a 1000-g load and taking readings only in sound portions of the crystals free of cracks. The crystals exhibited profuse twinning as shown in Fig. 1. No such structure is present in the as-melted condition. Most of these twins have jagged twin boundaries and are similar in appearance to those found in molybdenum by Mueller and Parker. The twins in both crystals were found to be parallel to {112} planes. This identification was made by using the conventional two-trace method. Subsequent efforts to describe these twins more fully were carried out on crystal A. If the longitudinal axis of crystal A is placed in the (001)-(011)-(Il l) basic triangle of the standard cubic stereographic projection, as in Fig. 2, then the two sets of twins shown in Fig. 1 are parallel to the (112) and (121) planes. Fig. 3 shows a schematic representation of a twin with jagged boundaries. This type of twin with a <111>

Jan 1, 1962

By O. C. Ralston, F. Fraas

VIRTUALLY all commercial use of electrostatic separation has employed separators depending on differences of conductance of the broken, solid mixtures treated by them. The two main types of conductance separators have been: (1) Those in which the separating field is as near a static field between two charged electrodes as it is possible to maintain in the face of the usual leakage that takes place between electrodes with some 5 to 50 kv tension between them and spacing of 1/2 to 3 in.; (2) those in which a convective discharge of corona or spray type, but not a spark discharge, takes place between the carrier electrode and a charged electrode facing it, which is of very restricted area, such as a row of needle points or a small diameter wire parallel to the face of the carrier electrode. The present paper deals with this latter type. The principle is usable in separators where the carrier electrode, usually grounded, has the shape of a roller, a conveyor belt, a vibrating table, a sloping chute, or a nearly vertical plate. The innovation studied by us has been the use of the convective field for charging material on the carrier electrode and succeeded by a field between the carrier electrode and an electrode made of a true dielectric which cannot take on a charge by conduction but is charged by being in the radius of the corona discharge. The acquired charge is of the same sign as that of the corona but is not dischargable by contact with a good conductor. However, high-tension charge tends to leak off because of the ionization of the ambient air. The field between this electrode and the carrier electrode is as near static as it is possible to obtain. There are some differences in behavior of this electrode and that of the gas tube electrode used by Sutton, as will be discussed below. Both electrodes cause increased adhesion of nonconductive particles to the carrier roll. The particles are pinned there because they are convectively charged on their outer surfaces facing the corona electrode. The electrodes also cause increased rate of release of conductive particles tending to be pinned by corona charging but conveying the charge to the grounded carrier roll almost as rapidly as it is received by the particles. The sign of the potential on the corona-emitting electrode makes little difference in the separation. An electrode usually emits negative corona somewhat more easily than it emits positive corona, as electrons are then the fundamental particles emitted. With a positive electrode the flow of electrons involved in positive corona discharge is onto the electrode from the ambient gas. Theory In the separator illustrated in fig. 1, the nonioniz-ing electrode is a rotating, nonconductive dielectric cylinder designated as B. The ions emitted by the corona electrode, or wire F, charge both the particles on the carrier electrode, or roll A, and the surface of the dielectric electrode B. Whereas the space between roll A and wire F contains ions, the space between electrode B and roll A is a pure static field free of ions. The dielectric electrode has been described by Bullock.1 However, the corona electrode, which Bullock uses for the purpose of charging only the dielectric electrode, is adapted here to also charge the particles on the carrier roll. In operation the ionic field from the corona electrode is balanced with the static field from the dielectric electrode. The ionic field charges the particle so that it adheres to the roll. The static field intensifies the discharge of the corona charge by interfacial conduction and permits the release of the particle. The ionic and static fields therefore have opposing effects.2 The values of both fields are adjusted so that the poor conductor will adhere and the good conductor will be released.

Jan 1, 1951

By O. C. Ralston, F. Fraas

VIRTUALLY all commercial use of electrostatic separation has employed separators depending on differences of conductance of the broken, solid mixtures treated by them. The two main types of conductance separators have been: (1) Those in which the separating field is as near a static field between two charged electrodes as it is possible to maintain in the face of the usual leakage that takes place between electrodes with some 5 to 50 kv tension between them and spacing of 1/2 to 3 in.; (2) those in which a convective discharge of corona or spray type, but not a spark discharge, takes place between the carrier electrode and a charged electrode facing it, which is of very restricted area, such as a row of needle points or a small diameter wire parallel to the face of the carrier electrode. The present paper deals with this latter type. The principle is usable in separators where the carrier electrode, usually grounded, has the shape of a roller, a conveyor belt, a vibrating table, a sloping chute, or a nearly vertical plate. The innovation studied by us has been the use of the convective field for charging material on the carrier electrode and succeeded by a field between the carrier electrode and an electrode made of a true dielectric which cannot take on a charge by conduction but is charged by being in the radius of the corona discharge. The acquired charge is of the same sign as that of the corona but is not dischargable by contact with a good conductor. However, high-tension charge tends to leak off because of the ionization of the ambient air. The field between this electrode and the carrier electrode is as near static as it is possible to obtain. There are some differences in behavior of this electrode and that of the gas tube electrode used by Sutton, as will be discussed below. Both electrodes cause increased adhesion of nonconductive particles to the carrier roll. The particles are pinned there because they are convectively charged on their outer surfaces facing the corona electrode. The electrodes also cause increased rate of release of conductive particles tending to be pinned by corona charging but conveying the charge to the grounded carrier roll almost as rapidly as it is received by the particles. The sign of the potential on the corona-emitting electrode makes little difference in the separation. An electrode usually emits negative corona somewhat more easily than it emits positive corona, as electrons are then the fundamental particles emitted. With a positive electrode the flow of electrons involved in positive corona discharge is onto the electrode from the ambient gas. Theory In the separator illustrated in fig. 1, the nonioniz-ing electrode is a rotating, nonconductive dielectric cylinder designated as B. The ions emitted by the corona electrode, or wire F, charge both the particles on the carrier electrode, or roll A, and the surface of the dielectric electrode B. Whereas the space between roll A and wire F contains ions, the space between electrode B and roll A is a pure static field free of ions. The dielectric electrode has been described by Bullock.1 However, the corona electrode, which Bullock uses for the purpose of charging only the dielectric electrode, is adapted here to also charge the particles on the carrier roll. In operation the ionic field from the corona electrode is balanced with the static field from the dielectric electrode. The ionic field charges the particle so that it adheres to the roll. The static field intensifies the discharge of the corona charge by interfacial conduction and permits the release of the particle. The ionic and static fields therefore have opposing effects.2 The values of both fields are adjusted so that the poor conductor will adhere and the good conductor will be released.

Jan 1, 1951

By N. S. Bornstein, M. A. DeCrescente

ThE nickel and cobalt base superalloys employed in gas turbine engines under some conditions&apos; oxidize at an accelerated rate when exposed at elevated temperatures to atmospheres containing minor quantities of sea salt. It is generally agreed by investigators in the field that the major steps comprising this phenomena of accelerated oxidation, also called hot corrosion or more commonly, sulfidation, are a) a slag composed primarily of Na2S04 is formed on turbine components, b) the protective oxide scale is rendered ineffectual, c) the slag reacts with. the substrate to form metal sulfides, and d) the substrate is rapidly oxidized. Sodium sulfate, a minor constituent of sea salt, is formed within the gas turbine engine from the reactions between NaC1, the major constituent of sea salt, and the oxides of sulfur.&apos; Depending upon concentration, engine compression ratio, and temperature, the Na2S04 will be present in the gaseous or condensed state. It has been determined that in order for sulfi-dation to occur the Na2S04 must be present in the condensed state.&apos; Although a number of sulfidation mechanisms have been postulated, there is no consistent explanation of oxide scale breakdown and subsequent catastrophic oxidation. Some investigators believe that after oxide scale breakdown, the Na2SO4 reacts with the substrate to form lower-valent sulfur compounds. The accelerated rate of oxidation is due to oxidation of a nickel-sulfide phase." Other investigators believe that sulfur from the fused salt reacts with chromium in the alloy to form chromium-rich sulfides; thereby depleting the alloy of an element which imparts oxidation resistance.3,4 This publication will demonstrate that the accelerated rate of oxidation associated with sul-fidation is due to interactions between Na20, a con-stituent of NazSO.,, ancl the substrate. The aim of this study was to separate and determine the effect of compounds of sulfur and sodium on the oxidation kinetics of various nickel-base superalloys, in order to elucidate the sulfidation mechanism. The work reported herein is sponsored in part by the Naval Ship and Development Center-Investigation of EXPERIMENTAL PROCEDURE The nickel base alloys B-1900, U-700, and Waspaloy were chosen for this study. The nominal compositions are presented in Table I. The specimens, approximately 1 in. by 1 in. by 0.060 in. received in the "as cast" condition were polished with 600 grit emery, washed, and rinsed with acetone immediately prior to oxidation experiments. Sulfida-tion attack was duplicated in the laboratory by apply-ing a saturated aqueous solution of Na2S04 onto the al loy substrate and subsequently exposing the specimens in oxygen at elevated temperature. The method of Na2S04 application is described elsewhere in detail.6 In another set of experiments the affected substrate microstructure associated with sulfidation was reproduced free of the normal oxide scale, by reacting and diffusing elemental sulfur into the alloy. The experimental procedure is also described elsewhere in detail. All oxidation studies were performed using an Ainsworth thermobalance type RV-AU-1, which is readable to 0.01 mg and is reproducible to ±0.03 mg. The specimens, introduced into a heated furnace, were exposed in the temperature range 800" to 1000°C

Jan 1, 1970

By M. A. Goudie

The deposits occur in a large salt basin of Middle Devonian age. The potash, the final deposit in the salt basin, results from several interrupted cycles of evaporation and dessication. The deposits are extensive, and, at first glance, relatively undisturbed. With more and more wells being drilled, it has now become evident that salt solution has played a large part in changing the original deposits, resulting in some cases in partial to complete removal of the potash and the underlying halite. The most dominant factor in the removal of salt by solution appears to have been tectonic movement and consequent faulting, probably of relatively minor dimensions but of major importance. Evidence which indicates the tilting of the evaporite basin to the north and northwest is shown by the changing pattern of the basin during succeeding eras of potash deposition. The potash minerals of most importance economically are sylvite and carnallite. Reserve calculations indicate that 6.4 billion tons of recoverable high grade potash in K2O equivalent exist in the basin. The Devonian salt basin, which contains the Saskatchewan potash deposits, extends from just east of the foothills in Alberta, north as far as the Peace River area, across Saskatchewan and into Manitoba as far east as Range 10 west of the First Meridian and south into Montana and North Dakota (Fig. 1). The basin is closed everywhere except to the northwest. The known potash deposits are confined almost entirely to the Province of Saskatchewan, with the exception of a small area in western Manitoba bordering the Saskatchewan boundary. The following discussion will concern only the Saskatchewan part of the basin. The evaporite series in the basin is defined as the Prairie Evaporite Formation of the Elk Point Group, of Middle Devonian age. Recent work done by potassium-argon dating methods has indicated an Upper Middle Devonian (Givetian) age of from 285 to 347 million years for the potash. The Elk Point Group consists in ascending order of the Ashern, Winnipegosis, and Prairie Evaporite Formations. The Ashern formation, with an average thickness of 30 ft, sometimes called the Third Red Bed, consists of dolomitic shales and shaly dolomites. The Winnipegosis, is a reef-type dolomite, usually with good porosity, and in many cases oil-staining, although to date no production has been obtained. The thickness varies from 50 to 250 ft. The Prairie Evaporite formation, varying from 0 to 600 ft in thickness, consists of halite with interbedded anhydrite and shale, with considerable amounts of potassium salts in the upper part of the formation. The potassium salts are chiefly chlorides, although very minor occurrences of sulfates have been re- ported. The anhydrite beds do not appear to be continuous, although generally one or two bands of anhydrite underlie the lowest potash zone and are used as marker horizons. The shale occurs as seams interbedded with the salts, as large irregular inclusions in the salts and as very fine particles in intimate mixture with the salts. The Prairie Evaporite Formation is overlain by the Second Red Bed member, the Dawson Bay Formation and the First Red Bed Member of the Manitoba Group, listed in ascending order. The Red Beds are shales which vary in color from red to green, maroon, grey, grey-black, and reddish purples. They serve as marker horizons for coring the potash. The Second Red Bed averages 14 ft in thickness, the First Red Bed 35 ft. The Dawson Bay Formation, which everywhere overlies the First Red Bed and the Prairie Evaporite Formation in the area under discussion, is a reef type of carbonate, in some places limestone, in others limestone and dolomite, with vugular to pinpoint porosity averaging 130 ft in thickness. In some parts of the area, it has a salt section near the top of the formation, usually with interbedded shales and limestones. In other parts of the area, it is waterbearing and the salt is absent. Detailed mapping has indicated that the areas in which the Dawson Bay is water-bearing are areas which have been disturbed by faulting. Where the Dawson Bay is salt-bearing, the porosity has been plugged by salt. The total thickness of the salt varies from between 600 to 700 ft in the center of the basin to zero at the northern edge of the basin (Fig. 2).* The salt-free area in the center of the Province is believed to have resulted from removal of salt by solution. Evidence from several wells suggests that salt removal has been a continuing process from the time of deposition to the present day. One well drilled between the Quill Lakes for potash information encountered

Jan 1, 1961

By E. Miller, J. M. Eldridge, K. L. Komarek

Aclivilies of magnesium in liquid Alg-Si alloys have been delermined between 5 and 60 at. pcl Si, close to the melling point of Mg2Si, by an improved isopieslic melhod. Silicon specinrens, held in alumina crucibles and graplrile conlainevs of special design, were healed in a letrlpevalure gvadient and equilibrated with mag-nesilcrrl rapor in a closed lilanium system. The ther-madynamic Junctions were calculated and compared with the thermodyuamic properties of the other three mg- Gvoup IVB systems. Lattice paramelers of three Mg2X compounds were measured. The bonding in the Mg2X compounds is largely covalent with small and uarying amounts of metallic and ionic conlvibutions. The Mg-Si phase diagram1 has one congruent melting compound, Mg2Si, of essentially stoichiometric composition, two eutectics, and very limited terminal solid solubilities. Little information is available on the thermodynamic properties of this system. The free energy of formation of Mg2Si has been determined by the Knudsen cell technique2 in the range 572" to 680oC, by the transportation method3 between 858" and 950oC, and by the electromotive-force method4 in the range 400o to 600°C. Kubaschewski and villa5 and caulfield6 have measured the heat of formation of Mg2Si. An electromotive-force study of magnesium-rich liquid alloys was recently published by Sryvalin el al.7 The present investigation was undertaken to complete a general survey of the thermodynamic properties of the homologous series of Mg-Group IVB systems, i.e., Mg-Pb,a9,Mg-Sn,10,11 mg-Ge,12and Mg-Si. An isopiestic technique, previously developed for similar measurements on liquid Mg-sn11 and Mg-Ge alloys,12 was modified for the Mg-Si system. Specimens of the nonvolatile component, silicon, were contained in dense alumina crucibles placed inside covered graphite crucibles which were heated in a temperature gradient in an evacuated and sealed titanium reaction tube and equilibrated with magnesium vapor of known vapor pressure. The alumina crucibles prevented contact between the highly corrosive liquid Mg-Si alloys and graphite. The graphite cruci- bles effectively preserved the high-temperature equilibrium composition of the liquid alloys containing highly volatile magnesium on termination of the experiments during the quench to room temperature. EXPERIMENTAL PROCEDURE Silicon of semiconductor-grade purity (E. I. du Pont de Nemours and Co., Brevard, N.C.) and 99.99+ pct Mg (Dominion Magnesium Ltd., Toronto, Canada) were used. Graphite crucibles with press-fitted lids were machined from high-density (1.92 g per cu cm) rods (Basic Carbon Corp., Sanborn, N.Y.) which had a maximum ash content of less than 0.04 pct. The alumina crucibles had a purity of 99.7+ pct (Triangle RR grade, Morganite, Inc., Long Island City, N.Y.). In preliminary runs the liquid alloys were contained in graphite crucibles following the exact procedure developed for the Mg-Ge system.&apos;2 These runs failed due to appreciable reaction between the molten Mg-Si alloys and graphite, and the results have been discarded. The procedure was then modified and the Mg-Si alloys were subsequently held in alumina crucibles. For most of the runs alumina crucibles of known weight and approximately 6.3 mm ID, 12.5 mm height, 1.0 mm wall thickness were loaded with weighed amounts of silicon and encapsuled in tightly covered weighed graphite crucibles 5/16 in. ID, 2 in. helght, 3/32 in. wall thickness). The graphite crucibles were machined from rods which were 85 pct of the theoretical density. These crucibles were therefore sufficiently porous so as to permit magnesium vapor to effuse through the silicon under the experimental conditions of approximately 970O to 1220°C and 1 day equilibration time. However, negligible magnesium was lost from the crucible during the quench due to the slow effusion rate through the pores of the graphite. The inner alumina crucible prevented the liquid alloys from contacting the graphite, and the very tightly fitting graphite crucible lids served to retain any magnesium vaporizing from the alloys inside the crucibles during the quenching step.12 The loaded silicon-alumina-graphite cells were positioned, one above another, on a 16-in.-long titanium thermocouple well and tied securely to the titanium tube with thin molybdenum wires held in grooves around the circumference of the graphite crucibles. A thin (0.005-in.) molybdenum strip prevented contact between the graphite crucibles and the titanium. This assembly was lowered into a titanium reaction tube (la in. ID, 16 in. long, $ in. wall thickness) closed on one end which contained a 11/2-in.-long cylinder of magnesium at the bottom. The inner titanium thermocouple well was positioned eccentrically in the large tube because of the eccentric mounting of the cells on the well. Appropriate modifications of the titanium cap"&apos;12 were made to join the inner and outer titanium

Jan 1, 1968

By Gilbert E. Doan, William C. Schulte

An extensive program of investigation is being carried out at Lehigh University in the study of arcs and arc welds of high-purity iron1, sponsored by the Engineering Foundation. The part of that program reported in the present paper deals with welds made of high-purity iron in an argon atmosphere and for comparison with them welds made of the same iron in ordinary air. Welds of commercial steel also were made in argon and in air. The primary purpose of the study is to discover the basic physical constants of iron welds when not contaminated either by impurities in the iron or by the action of oxygen and nitrogen of the air during welding. Upon these constants can be founded such future studies as will determine what effects the various impurities and alloy elements present in steel have upon its welding characteristics, and what influence is exerted by the action of oxygen and nitrogen. The welding of steel involves such a multitude of variables, both of composition and of procedure, that development in the fabrication of this most important metal has necessarily been slow, wasteful, and in many instances discouraging. In the present investigation, the simplest possible condition has been selected; namely, iron practically free from contamination and a nonparticipating atmosphere, the inert gas argon. This simplification reduces the number of variables to a point where more rigid control of the system is possible. Although this study is significant for the contributions it makes to the science of steel fabrication, yet it is hoped that it will not be without value also in increasing knowledge of the. nature and behavior of iron and steel in general. From the standpoint of open-hearth practice, and to some extent from the standpoint of electric-furnace practice also, the conditions of melting and casting iron in this investigation are extraordinary. The casting temperature is high, the mean temperature of the metal probably reaching 2000&apos; C. (3600&apos; F.)? The rate of chilling of

Jan 1, 1936