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By W. J. Babyak

The habit planes for hydride precipitation in large grains of alpha zirconium and Zircaloy-4 were determined in specimens containing 161 and 136 ppm hydrogen, respectively. In zirconium, the hydride platelets precipitated on various pyramidal planes inclined to the basal plane at angles ranging from 10 to 50 deg and 75 to 90 deg. Hydrides were most frequent at inclinations of about 20 deg and 90 deg. In Zircaloy-4, hydride plates were inclined to the basal plane at angles vanging from 5 to 25 deg with the predominant inclinatioiz equal to 12 deg; no platelets were found near the prism plane position. In both zircoinium and Zir-caloy-4, hydrides were principally, but not exclusively, parallel to (1011) type planes. When the Zircaloy-4 gmins were subjected to tension stresses of 12,100 psi and 19,400 psi during hydride precipitation, the hydride habit was unchanged except that precipitation favored those habit planes which were inore nearly perpendicular to the stress direction. The stress-orientatioiz effect increased with the magnitude of the stress. THE hydride habit plane in a zirconium has been determined by several investigators. Langeron and Lehr1 in 1956 found platelets parallel to (1010) slip planes. In 1962, Westlake and Fisher2 confirmed these findings and showed that hydride precipitation on twin planes, as reported by Kunz and Bibb,3 was probably due to incomplete removal of worked metal from specimen surfaces. Secondary habit planes, ( 1011) and (1015), were also found by Westlake and Fisher under particular charging conditions where a hydride layer may have existed at the hydrogenation temperature. Most recently, walters4 and westlake5 again observed the (1010) habit exclusively in zirconium. Louthan and hgermans have reported that hydrides precipitate on various ( 101l ) and (112l) planes positioned 31.5 to 90 deg to the basal plane in Zircaloy-2. The present investigation was concerned with the hydride habit in Zircaloy-4 in relation to that in zirconium and the possible change in habit when precipitation occurs under stress. The latter consideration was prompted by the stress-orientation phenomenon originally reported by Marshall and Louthan.7, 8 I) EXPERIMENTAL Materials and Specimens. Chemical analyses of all materials are given in Table I. The zirconium specimen was a 1 by 4 in. section cut from wrought crystal bar that was hot-rolled at 790°C to 0.300 in. and cold-rolled to a final thickness of 0.095 in. All surfaces were mechanically polished and then chemically polished with a solution of H2O, HNO3, and HF (10:10:l by volume) prior to annealing. Grains as long as 0.25 in. were grown by thermally cycling the specimen three times (in 10-5 mm Hg vacuum) between 825" and 1000°C at approximately 125°C per hr. The specimen was isothermally annealed at 825°C for 24, 40, and 120 hr after each cy-

Jan 1, 1968

By A. K. Mukherjee, J. E. Dorn

A modified Peierls model is Presented for the rationalization of the asymmetric plastic behavior of single crystals of bcc metals. The model assumes that the asymmetry of slip arises from a tendency toward asymnetric splitting of the a/2[111] screw dislocation. The approach differs from former theories however insofar as it assumes that the splitting is so minor ttut only the core energy is modified and that no real partial dislocations exist. As a consequence, the concepts of a line energy of a partial dislocation, interaction between partial dislocations, constriction energies, and stacking fault energies are not invoked. Instead the present analysis is based on a specialization of the Peierls mechanism which assumes an asymmetric dislocation core which is modified by the effective stress and permits cross slip. The theoretical predictions on the stress-temperature -strain rate and orientation relationship agree qualitatively with the limited experimental data that are currently available. Additional experimental work over wider ranges of conditions is suggested to provide more complete evaluation of the possible validity of this theory. RECENT experimental investigations on the low-temperature thermally activated deformation of bcc metals have confirmed the existence of several unique orientation effects. These will be described with the aid of the standard stereographic projection shown in Fig. 1. If slip were determined exclusively by crystal symmetry, the deformation characteristics would be symmetrical about X; = 0 and independent of whether the specimen were subjected to a tension or a compression stress, regardless of what combinations of slip planes might be operative. Experiments, however, reveal that neither of these symmetry based predictions are valid. A schematic representation of the commonly observed asymmetry of both the yield stress and the plane of slip is shown in Fig. 2. A reversal of the direction of stressing results in an inversion of the asvmmetric behavior. 1) Asymmetry bf Yielding. A detailed investigation on the asymmetric yielding in an Fe-2.7 pct Si alloy was repoEted by Tabka, Tikeuchi, and Furubayashi,1 Similar trends have been observed by Keh and Nakada on iron,' Stein on molybdenum,3 Bowen, Christian, and Taylor4 on columbium, Sherwood, Guiu, Kim, and pratt5 on Ta, Cb, and Mo. The degree of asymmetry not only depends on the atomic number and alloying but, in all cases that have been examined, it also increases with a decrease in the test temperature. 2) Asymmetry of the Slip Plane. Asymmetric $I-~: curves of the type shown in Fig. 2 have been found for several Fe-Si alloys6-8,1 and columbium.4 There is general agre_ement that near X: = 30 deg slip occurs by the [111](211) mode so that ?1 = 30 deg. As X; decreases it appears that [111](211) to [111](101) cross slip takes place leading to slip band traces on intermediate planes. And as xi approaches 0 deg, sharp

Jan 1, 1970

By J. D. Edwards

When Charles Martin Hall invented the electrolytic process for the production of aluminum, one basic requirement was a supply of pure alumina. Now, more than 50 years later, the same requirement still holds, and there are no technical straws in the wind to indicate that this situation is likely to change. Long ago, Aluminum Company of America took a number of steps to see that this country should not face shortages of alumina and aluminum in time of emergency. As one step to this end, the Company developed and used a supply of bauxite in South America in order to conserve dwindling Arkansas reserves. Another, and more a program than a step, was to investigate every type of process that might bear the possibility of utilizing the low-grade ores of aluminum that are more plentiful than bauxite. It is a long story, but the investigation included electric-furnace processes, acid extraction processes and alkaline extraction processes, with or without preliminary furnace and sinter treatments. Some of the processes developed were operated in commercial production. This work has been continuous since the first World War. The turn of the wheel came sooner than was expected when, in 1942, bauxite shipmerits through the caribbean became uncertain and hazardous through the operation of submarines. The tremendous requirements of aluminum for the war effort were consuming high-grade bauxite at an alarming rate and a national search for substitutes began. High-grade bauxites, for technical and economic reasons, have been defined as those containing about 7 per cent or less of silica. While bauxite of this grade was limited in amount in the United States, there was in sight a substantially greater volume of low-grade, high-silica bauxite not amenable to economic treatment by the Bayer process, but richer in alumina than the clays or other available low-grade ores. It was at this point, and after several years of intensive research on this particular phase of the problem, that Aluminum Research Laboratories brought to completion the invention of one of its research staff, which made practical the utilization of large reserves of low-grade bauxite in America. Bayer Process The Bayer process has been almost universally used for the production of alumina from bauxite. This process, in outline, comprises the digestion of hely ground bauxite in a solution of caustic soda (NaOH) under pressure and at an elevated temperature. Alumina in the bauxite goes into solution as sodium alumi-"ate and the impurities—oxides of iron, titanium and silicon—remain undissolved. The undissolved residue, known as "red mud,'' from its color, is separated and run to waste. AluKlinum hydrate (A12O3.3H2O) is precipitated from the solution of sodium aluminate, and the liquor containing the caustic soda and some alumina is returned to the Process for digesting more bauxite. The aluminum hydrate, after washing, is calcined at a high temperature to produce

Jan 1, 1949

By James W. Halley

' FINE-GRAINED " steels have been standard products for many years. This paper describes an investigation of the effects of some of the more common grain-growth; inhibitors used to produce these steels. The properties, response to heat-treatment, and the deoxidation practice necessary to produce "fine-grained" steels have been the subjects of numerous papers. It has been shown that a substantial quantity of' aluminum is necessary to produce this type of steel, and it has been indicated that titanium and zirconium produce a similar result. For some time there was a lively argument between those who felt that aluminum refined the grain and those who felt that aluminum oxide was the effective agent. This argument subsided with an apparent victory for those promoting aluminum oxide. Most of the work on grain size has divided steels into two broad classifications based upon McQuaid and Ehn's original carburizing test at 1700°F. or some similar test at this temperature. If the steel coarsened at this temperature, it was coarse grained, while if it did not it was fine grained. Quantitative data concerning how much a certain amount of aluminum raised the coarsening temperature and affected the properties, all other factors being constant, are very meager. Similar information regarding titanium and zirconium is practically nonexistent. The published information on aluminum yields some quantitative information. Epstein, Nead and Washburn' gave the first quantitative information on the amount of aluminum necessary to prevent grain growth at 1700°F. They showed that the addition of a pound to a pound and a half of aluminum per ton (0.05 to 0.075 per cent) would assure steel that would not .coarsen during a McQuaid-Ehn test at 1700°F. Herty, McBride and Hough2 reported that a steel containing 0.020 per cent acid-soluble aluminum coarsened between 1742° and 1832°F., while steels containing 0.016 per cent and 0.017 per cent acid-soluble aluminum coarsened between 1652~ and 1742°F. compared with similar aluminum-free steels that started to coarsen at 1580°F. Herty3 also showed a marked improvement in low-temperature notched impact resistance with increasing acid-soluble aluminum up to 0.030 per cent. McQuaid4 compared the coarsening of steels containing 0.011 to 0.204 per cent total aluminum and found a maximum coarsening temperature at 0.098 per cent aluminum. He had no samples between 0.015 and 0.098 per cent aluminum. Houdrement5 found a marked decrease in coarsening temperature with aluminum contents above 0.50 per cent. Kinzel, Crafts and Egan6 found that aluminum and zirconium improved thy low-temperature impact resistance of a low-alloy steel, while titanium was detrimental. Sims7 shows that sulphur increases the coarsening temperature and that the maximum coarsening temperature is between 0.04and 0.06 Per cent added aluminum. The

Jan 1, 1946

By J. H Lightfoot, Stuart E. Buckley

Deep drilling has led to the development of numerous pools which yield products consisting predominantly of natural gas accompanied by high-gravity water-white or slightly straw-colored liquid. Yields of this "condensate" or "distillate," as it is commonly called, vary from traces to over a hundred barrels per million cubic feet of gas. The fact that this liquid exists in the reservoir as an integral part of the gas phase and is formed by condensation attending simultaneous reduction of pressure and temperature after its entry into the well was apparently first recognized about 1932.l The nature of the physical phenomena involved in this condensation was clarified for the petroleum industry in 1933 by a report by Sage, Schaafsma, and Lacey2 of the results of an experimental investigation of the behavior of mixtures of methane and propane. Search of the literature has revealed that the condensation of liquid from gaseous mixtures by isothermal pressure reduction is not a new discovery. Kuenen was led by theoretical considerations to expect such a phenomenon, and in 1892 reported3 the results of experimental verification of his deductions. This was followed by a considerable amount of work on the phase relations of mixtures by Kuenen 4,5,6 and by 0thers,7,8 mostly in European universities. Since 1930 investigators in this country have reported experimental data on the properties and behavior of a number of hydrocarbon systems."' It is now generally known that in the presence of natural gas the solubility in the gas phase of the heavier and normally liquid hydrocarbons increases rapidly with increasing pressure above 500 to 1000 Ib. per sq. in. Thus, at pressures of 2500 Ib. per sq. in. or higher a gas may contain appreciable quantities of hydrocarbons with normal boiling points as high as 6o0°F., which in turn may be condensed from the gas phase by the reduction of their solubility therein attending pressure reduc-tion. The combined effects of pressure and temperature on condensation and vaporiza-tioi of mixtures are most readily visualized by the study of phase diagrams. Since the construction, application, and interpreta-tion of such diagrams have been described fully in readily available literature, 18-20 this paper will not review the theoretical aspects of this subject. While the behavior of gas-distillate sys tems is now clearly understood, at least in a qualitative way, most of the published work deals with the results of laboratory studies of binary systems or of synthetic mixtures of hydrocarbons, and although several systematic investigations of the effects of separator pressure and temperature on the yields of liquid product from gas-distillate wells have been made21,12z it appears that in all cases the limitations have precluded the construction of even approximately complete phase diagrams for naturally occurring systems. There has 2

Jan 1, 1941

By J. H. Lightfoot, Stuart E. Buckley

Deep drilling has led to the development of numerous pools which yield products consisting predominantly of natural gas accompanied by high-gravity water-white or slightly straw-colored liquid. Yields of this "condensate" or "distillate," as it is commonly called, vary from traces to over a hundred barrels per million cubic feet of gas. The fact that this liquid exists in the reservoir as an integral part of the gas phase and is formed by condensation attending simultaneous reduction of pressure and temperature after its entry into the well was apparently first recognized about 1932.l The nature of the physical phenomena involved in this condensation was clarified for the petroleum industry in 1933 by a report by Sage, Schaafsma, and Lacey2 of the results of an experimental investigation of the behavior of mixtures of methane and propane. Search of the literature has revealed that the condensation of liquid from gaseous mixtures by isothermal pressure reduction is not a new discovery. Kuenen was led by theoretical considerations to expect such a phenomenon, and in 1892 reported3 the results of experimental verification of his deductions. This was followed by a considerable amount of work on the phase relations of mixtures by Kuenen 4,5,6 and by 0thers,7,8 mostly in European universities. Since 1930 investigators in this country have reported experimental data on the properties and behavior of a number of hydrocarbon systems."' It is now generally known that in the presence of natural gas the solubility in the gas phase of the heavier and normally liquid hydrocarbons increases rapidly with increasing pressure above 500 to 1000 Ib. per sq. in. Thus, at pressures of 2500 Ib. per sq. in. or higher a gas may contain appreciable quantities of hydrocarbons with normal boiling points as high as 6o0°F., which in turn may be condensed from the gas phase by the reduction of their solubility therein attending pressure reduc-tion. The combined effects of pressure and temperature on condensation and vaporiza-tioi of mixtures are most readily visualized by the study of phase diagrams. Since the construction, application, and interpreta-tion of such diagrams have been described fully in readily available literature, 18-20 this paper will not review the theoretical aspects of this subject. While the behavior of gas-distillate sys tems is now clearly understood, at least in a qualitative way, most of the published work deals with the results of laboratory studies of binary systems or of synthetic mixtures of hydrocarbons, and although several systematic investigations of the effects of separator pressure and temperature on the yields of liquid product from gas-distillate wells have been made21,12z it appears that in all cases the limitations have precluded the construction of even approximately complete phase diagrams for naturally occurring systems. There has 2

Jan 1, 1941

By Hugh H. Waesche

High quality quartz crystals weighing more than 50 grams are required in several important industrial applications.30,31 Primarily, they are the basic raw material for precision, electronic, frequency control components; this includes oscillators and filters in both radio and telephone services. Quartz crystals are also necessary for optical lenses and prisms in special applications requiring high ultraviolet light-transmission as in spectrographs. Quartz wedges are regular components for petrographic microscopes. The application of crystalline quartz as a transducer* in ultrasonic devices has increased in recent years despite strong competition from barium titanate and magnetostrictive [f] devices. Some quartz is fabricated into delay lines for radar. Man has valued quartz for fabrication of art objects since the dawn of history. The art forms were and are painstakingly carved and polished to form intricate figurines, bowls, statuettes, and the well-known crystal balls. The largest known ball, made of perfect quartz from Burma, is now in the National Museum in Washington. It is 12 7/8 in. in diameter and weighs 106 lb 12 oz. Clear, pure quartz chips and small crystals not meeting the electronic-grade dimensional requirements are known by the Brazilian term lasca. They are used to produce fused quartz having wide application in laboratory equipment, as special glasses, for torsion suspension in scientific instruments, and as a source material for growing large artificial quartz crystals 18,35 Electronic applications far exceed all other uses in importance so any discussion of high-quality quartz crystals must be concerned almost exclusively with those functions. Historical Background Because of their ubiquitous character and natural beauty, quartz crystals have long been of interest and known to man. They have been found among early Egyptian and Chinese art forms and the Sumerians are believed to have fashioned seals, beads, and other jewelry from quartz crystals, perhaps 5,000 years ago. Also, American Indians made arrow heads and fashioned some simple objects of different kinds. The origin of the name quartz, although of Greek derivation, is uncertain. The Greeks appropriately applied their word for frozen water or ice, krustallos, to quartz. The present-day, large-scale practical applications of quartz crystals began in 1880-1881 when Pierre and Jacques Curie reported discovery of the "piezoelectric" effect. They found this effect first in Rochelle salt, a common product of grape-wine refineries, while studying crystal symmetry. Piezoelectricity is that property found in certain crystals, including quartz, whereby electrical charges of equal and opposite sign appear on opposite parts of the crystals when they are stressed. If equal and opposite forces are applied to two opposing prism edges of a single untwinned quartz crystal a positive electrical charge will appear on one edge and a negative charge on the other. The amount of the charges will be directly proportional to the force applied. This property seems to be intimately related to pyroelectricity

Jan 1, 1960

By Hugh D. Pallister, Richard W. Smith

The Alabama flake-graphite industry has flourished only in times of war when importations of foreign graphite for crucible use have been greatly curtailed or cut off. World War I was a boom period and in 1918 some 30 plants produced 7,795,475 Ib. of flake graphite. The industry languished following the war and no graphite was produced from 1929 to 1939. The Federal Bureau of Mines began investigating the Alabama graphite deposits in 1940 and worked out modern recovery methods that were applied to production during part of World War 11. A prospecting program disclosed reserves of over 25 million tons of graphtic schists. In 1942 the War Production Board authorized the enlargement of the only plant then producing flake graphite and the construction of two new plants. Production of flake graphite from these three plants in 1943 is estimated at 8,100,000 lb. Increased imports from Madagascar late in 1943 shut down one of the new plants and curtailed production at the other. Alabama flake graphite has not yet been able to compete with Madagascar graphite for use in the manufacture of any but small graphite crucibles. The future of the industry must depend on meeting the higher carbon content demanded for other uses. Introduction The flake-graphite deposits of Alabama are confined to a narrow belt extending for about 60 miles southwest from the northeast corner of Clay County across Coosa County to the edge of the Coastal Plain in Chilton County (Fig. I). The continuity of the beds is broken by a 10-mile gap between Millerville in Clay County and Goodwater in Coosa County. The Clay County beds extend about 27 miles northwest of this gap, with a width of 3 to 4 miles near Millerville and of less than a mile at the northeast end. The Coosa-Chilton are? is about 33 miles long with a fairly consistent width of 2 to 3 miles. Geologically the graphite belt lies near the northeast boundary of the outcrop of metamorphic rocks of the Ashland series, a complex group of intensely folded and faulted beds of pre-Cambrian age composed mostly of quartz-mica schist, in which the mica is predominantly muscovite; garnet-mica schist, in which biotite is more common; and hornblende schist. Flake graphite is found in commercial quantities only in the quartz-mica schist. The best graphite, both in quantity and quality, is found in schist cut by numerous small pegmatite stringers along the planes of the schistosity. The pegmatites themselves contain little graphite, but the adjacent country rock is normally rich. . The schist was derived through the recrystallization of shale during the intrusion of the pegmatites, the graphite being derived from amorphous carbon in the shale. The intrusion of the pegmatites, and therefore the size and quantity .of the graphite flakes, seems to have a structural control.

Jan 1, 1948

By Hugh D. Pallister, Richard W. Smith

The Alabama flake-graphite industry has flourished only in times of war when importations of foreign graphite for crucible use have been greatly curtailed or cut off. World War I was a boom period and in 1918 some 30 plants produced 7,795,475 Ib. of flake graphite. The industry languished following the war and no graphite was produced from 1929 to 1939. The Federal Bureau of Mines began investigating the Alabama graphite deposits in 1940 and worked out modern recovery methods that were applied to production during part of World War 11. A prospecting program disclosed reserves of over 25 million tons of graphtic schists. In 1942 the War Production Board authorized the enlargement of the only plant then producing flake graphite and the construction of two new plants. Production of flake graphite from these three plants in 1943 is estimated at 8,100,000 lb. Increased imports from Madagascar late in 1943 shut down one of the new plants and curtailed production at the other. Alabama flake graphite has not yet been able to compete with Madagascar graphite for use in the manufacture of any but small graphite crucibles. The future of the industry must depend on meeting the higher carbon content demanded for other uses. Introduction The flake-graphite deposits of Alabama are confined to a narrow belt extending for about 60 miles southwest from the northeast corner of Clay County across Coosa County to the edge of the Coastal Plain in Chilton County (Fig. I). The continuity of the beds is broken by a 10-mile gap between Millerville in Clay County and Goodwater in Coosa County. The Clay County beds extend about 27 miles northwest of this gap, with a width of 3 to 4 miles near Millerville and of less than a mile at the northeast end. The Coosa-Chilton are? is about 33 miles long with a fairly consistent width of 2 to 3 miles. Geologically the graphite belt lies near the northeast boundary of the outcrop of metamorphic rocks of the Ashland series, a complex group of intensely folded and faulted beds of pre-Cambrian age composed mostly of quartz-mica schist, in which the mica is predominantly muscovite; garnet-mica schist, in which biotite is more common; and hornblende schist. Flake graphite is found in commercial quantities only in the quartz-mica schist. The best graphite, both in quantity and quality, is found in schist cut by numerous small pegmatite stringers along the planes of the schistosity. The pegmatites themselves contain little graphite, but the adjacent country rock is normally rich. . The schist was derived through the recrystallization of shale during the intrusion of the pegmatites, the graphite being derived from amorphous carbon in the shale. The intrusion of the pegmatites, and therefore the size and quantity .of the graphite flakes, seems to have a structural control.

Jan 1, 1948

By W. D. Potter, E. T. Peters

Single-crystal films of boron have been prepared by thermal reduction of purified BCl3 with subsequent deposition of boron onto oriented silicon substrates. The structural properties of films prepared under various experimental conditions have been determined by light microscopy and "grazing-" angle electron-diffraction analysis. An orientation relationship is proposed for silicon and a-rhombo-heclral boron which can be described as: (111)Si (112)B; [110]Si [110]B ElEMENTAL boron is known to have a high energy gap* and consequently has potential value as a high- *Energy gaps of 1.35 to 1.55 ev1-3 and 2.0 ev4 are reported for ß-rhombohedra1 and a-rhombohedra1 boron, respectively. temperature semiconductor.5 Exploitation of this property, however, has been hampered by the unavailability of pure, single-crystal boron. Two recent symposia6,7 have treated the subjects of purification, crystallization, crystal structure, and properties of boron and provide a foundation for further investigation in these areas. The structure, lattice constants, and observed ranges of stability for four reported polymorphs of boron8°12 are listed in Table I. The rhombohedral structures are generally accepted as true polymorphs whereas the tetragonal structures are believed to be transient. Most currently available single crystals of boron are grown by Czochralski and floating-zone methods. Unfortunately, these crystals generally contain numerous defects and are highly strained as a result of the polymorphic transformations and thermal contractions which accompany cooling. Recently, Armington, Potter, and Tanner13 have reported the formation of single-crystal films of boron on silicon single-crystal substrates through thermal reduction of BC13 by hydrogen. Boron E. T. PETERS, Junior Member AIME, is Senior Scientist, ManLabs, Inc., Cambridge, Mass., and W. D. POTTER is Research Chemist, Air Force Cambridge Research Loboratories, L. G. Hanscom Field, Bedford, Mass. formed at temperatures near 1000°C was identified as the a-rhombohedra1 form, consistent with expectation. The present paper describes a continuation of this work with specific reference to characterization of the structural features of the deposited boron films. The ultimate goal of this program is to produce large-area single-crystal films of a-rhombohedra1 boron to be used for electrical and optical studies by other workers. PREPARATION OF BORON FILMS The experimental procedure of preparing thin films is similar to that described by Theuerer14 for the epitaxial growth of silicon by thermal reduction of SiC14 and has already been described as applied to the preparation of boron thin films.13 Briefly, a mixture of BCl3 vapor and dry hydrogen is passed over a heated silicon substrate. Thermal reduction of the BC13 allows deposition of boron on the substrate. The substrates were {111}-oriented, single-crystal silicon. Square specimens 0.63 cm on an edge by 0.1 to 3.0 mm thickness were prepared by

Jan 1, 1965

By W. S. Pellini, F. N. Rhines

IN many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummer1 have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium 0f experimentation. New values obtained in this way are believed to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by R. S. Dean2 and by E. E. Schumacher and F. C. Nix.3 Their points are represented in Fig. I. In their work the solidus was not located at antimony concentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228°C.; J. E. Stead,7 247°C.; Campbell,8 228°C.; W. Gontermann,9 245° to 252°C.; R. Loebe,10 245°C.; E. Heyn and 0. Bauer,11 245°C.; H. Endo,12 250°C.; R. S. Dean,2 249° to 258°C.; E. Abel, 0. Redlich, and J. Adler,13 245°C.; W. Broniewski and L. Sliwowski,14 250° to 252°C.; H. Seltz and B. De Witt,4 250°C. A temperature of 249°C- appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 249°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1942

By James W. Halley

"Fine-grained" steels have been standard products for many years. This paper describes an investigation of the effects of some of the more common grain-growth inhibitors used to produce these steels. The properties, response to heat-treatment, and the deoxidation practice necessary to produce "fine-grained" steels have been the subjects of numerous papers. It has been shown that a substantial quantity of aluminum is necessary to produce this type of steel, and it has been indicated that titanium and zirconium produce a similar result. For some time there was a lively argument between those who felt that aluminum refined the grain and those who felt that aluminum oxide was the effective agent. This argument subsided with an apparent victory for those promoting aluminum oxide. Most of the work on grain size has divided steels into two broad classifications based upon McQuaid and Ehn's original carburizing test at 1700°F or some similar test at this temperature. If the steel coarsened at this temperature, it was coarse grained, while if it did not it was he grained. Quantitative data concerning how much a certain amount of aluminum raised the coarsening temperature and affected the properties, all other factors being constant, are very meager. Similar information regarding titanium and zirconium is practically nonexistent. The published information on aluminum yields some quantitative information. Epstein, Nead and Washburn' gave the first quantitative information on the amount of aluminum necessary to prevent grain growth at 1700°F. They showed that the addition of a pound to a pound and a half of aluminum per ton (0.05 to 0.075 per cent) would assure steel that would not coarsen during a McQuaid-Ehn test at 1700°F. Herty, McBride and Houghg reported that a steel containing 0.020 per cent acid-soluble aluminum coarsened between 1742° and 1832°F., while steels containing 0.016 per cent and 0.017 per cent acid-soluble aluminum coarsened between 1652° and 1742°F. compared with similar aluminum-free steels that started to coarsen at 1580°F. Herty3 also showed a marked improvebent in low-temperature notched impact resistance with increasing acid-soluble aluminum up to 0.030 per cent. McQuaid4 compared the coarsening of steels containing 0.011 to 0.204 per cent total aluminum and found a maximum coarsening temperature at 0.098 per cent aluminum. He had no samples between 0.015 and 0.098 per cent aluminum. Houdrement6 found a marked decrease in coarsening temperature with aluminum contents above 0.50 per cent. Kinzel, Crafts and Egan6 found that aluminum and zirconium improved the low-temperature impact resistance of a low-alloy steel, while titanium was detrimental. Sims7 shows that sulphur increases the coarsening temperature and that the maximum coarsening temperature is between 0.04 and 0.06 per cent added aluminum. The fact that the coarsening temperature passes through a maximum with increasing aluminum content appears to be well established. The aluminum content that

Jan 1, 1947

By James W. Halley

"Fine-grained" steels have been standard products for many years. This paper describes an investigation of the effects of some of the more common grain-growth inhibitors used to produce these steels. The properties, response to heat-treatment, and the deoxidation practice necessary to produce "fine-grained" steels have been the subjects of numerous papers. It has been shown that a substantial quantity of aluminum is necessary to produce this type of steel, and it has been indicated that titanium and zirconium produce a similar result. For some time there was a lively argument between those who felt that aluminum refined the grain and those who felt that aluminum oxide was the effective agent. This argument subsided with an apparent victory for those promoting aluminum oxide. Most of the work on grain size has divided steels into two broad classifications based upon McQuaid and Ehn's original carburizing test at 1700°F or some similar test at this temperature. If the steel coarsened at this temperature, it was coarse grained, while if it did not it was he grained. Quantitative data concerning how much a certain amount of aluminum raised the coarsening temperature and affected the properties, all other factors being constant, are very meager. Similar information regarding titanium and zirconium is practically nonexistent. The published information on aluminum yields some quantitative information. Epstein, Nead and Washburn' gave the first quantitative information on the amount of aluminum necessary to prevent grain growth at 1700°F. They showed that the addition of a pound to a pound and a half of aluminum per ton (0.05 to 0.075 per cent) would assure steel that would not coarsen during a McQuaid-Ehn test at 1700°F. Herty, McBride and Houghg reported that a steel containing 0.020 per cent acid-soluble aluminum coarsened between 1742° and 1832°F., while steels containing 0.016 per cent and 0.017 per cent acid-soluble aluminum coarsened between 1652° and 1742°F. compared with similar aluminum-free steels that started to coarsen at 1580°F. Herty3 also showed a marked improvebent in low-temperature notched impact resistance with increasing acid-soluble aluminum up to 0.030 per cent. McQuaid4 compared the coarsening of steels containing 0.011 to 0.204 per cent total aluminum and found a maximum coarsening temperature at 0.098 per cent aluminum. He had no samples between 0.015 and 0.098 per cent aluminum. Houdrement6 found a marked decrease in coarsening temperature with aluminum contents above 0.50 per cent. Kinzel, Crafts and Egan6 found that aluminum and zirconium improved the low-temperature impact resistance of a low-alloy steel, while titanium was detrimental. Sims7 shows that sulphur increases the coarsening temperature and that the maximum coarsening temperature is between 0.04 and 0.06 per cent added aluminum. The fact that the coarsening temperature passes through a maximum with increasing aluminum content appears to be well established. The aluminum content that

Jan 1, 1947

By E. O. Kirkendall

The investigation reported herein was undertaken to obtain data to supplement those presented in an earlier paper,l particularly for longer times at a higher temperature. This information may further develop our knowledge of the mechanism of diffusion in substitutional solid solutions. Diffusion of solute atoms interstitially dissolved is not difficult to visualize: it can take place without much disturbance of the solvent atoms. The mechanism of diffusion of solute atoms substitutionally dissolved is not so easily understood. Many theories have been advanced. Rosen-hain,2,3 Frenkel,4 Smekal,5 Langmuir,3,6 Steigman, Shockley and Nix,' and Johnson8 all proposed theories to explain diffusion. Langmuir's proposed mechanism consisted of a simple cyclic interchange of atoms involving an interchange in lattice positions of four or more atoms. This mechanism, accepted by the author at the time of his previous publication,1 and apparently quite generally accepted, required a net exchange in positions of both solute and solvent atoms in equal numbers. In other words, the rate of diffusion of the solvent and solute atoms would be the same. That this cyclic interchange in lattice positions of solute and solvent atoms in equal numbers is the only true mechanism of diffusion is denied by the evidence presented in this paper. Experimental Procedure This modification of similar procedure1 will be outlined briefly. The method consisted of the following steps: I. A pure Muntz metal (60.6 per cent Cu, 0.1 per cent total impurities) that was almost all beta brass at 780°C. was chosen. 2. The brass was turned between centers in a lathe to a diameter of 0.5965 inches. 3. After the brass was cleaned, it was electroplated with pure copper to a diameter of about one inch. 4. The sample was heated slowly to 400°C. under reduced pressure and held at that temperature for 4 hr. to remove occluded gases. It was then cooled to room temperature. 5. The sample was heated to 780°C. ± 3°C. and held at that temperature for different lengths of time; then quenched. Samples were cut off each time after quenching. Metallographic samples 1/4 in. thick were removed at I hr., 6 hr., 24 hr., 96 hr. and 701 hr. After 96 and 701 hr. samples of about I in. were removed for X-ray analysis. 6. The metallographic samples were polished on the cross section and photomicrographs were taken. 7. The I-in. samples were polished and etched on both ends. With the aid of a microscope each was carefully mounted in a four-jaw chuck in a lathe, so that they could be accurately bored for an arbor. 8. Turnings were taken for each X-ray sample. After each set of turnings, the sample was heated in an oil bath for about 1/2 hr. at 300°C. It was then etched in 25

Jan 1, 1942

By E. O. Kirkendall

The investigation reported herein was undertaken to obtain data to supplement those presented in an earlier paper,l particularly for longer times at a higher temperature. This information may further develop our knowledge of the mechanism of diffusion in substitutional solid solutions. Diffusion of solute atoms interstitially dissolved is not difficult to visualize: it can take place without much disturbance of the solvent atoms. The mechanism of diffusion of solute atoms substitutionally dissolved is not so easily understood. Many theories have been advanced. Rosen-hain,2,3 Frenkel,4 Smekal,5 Langmuir,3,6 Steigman, Shockley and Nix,' and Johnson8 all proposed theories to explain diffusion. Langmuir's proposed mechanism consisted of a simple cyclic interchange of atoms involving an interchange in lattice positions of four or more atoms. This mechanism, accepted by the author at the time of his previous publication,1 and apparently quite generally accepted, required a net exchange in positions of both solute and solvent atoms in equal numbers. In other words, the rate of diffusion of the solvent and solute atoms would be the same. That this cyclic interchange in lattice positions of solute and solvent atoms in equal numbers is the only true mechanism of diffusion is denied by the evidence presented in this paper. Experimental Procedure This modification of similar procedure1 will be outlined briefly. The method consisted of the following steps: I. A pure Muntz metal (60.6 per cent Cu, 0.1 per cent total impurities) that was almost all beta brass at 780°C. was chosen. 2. The brass was turned between centers in a lathe to a diameter of 0.5965 inches. 3. After the brass was cleaned, it was electroplated with pure copper to a diameter of about one inch. 4. The sample was heated slowly to 400°C. under reduced pressure and held at that temperature for 4 hr. to remove occluded gases. It was then cooled to room temperature. 5. The sample was heated to 780°C. ± 3°C. and held at that temperature for different lengths of time; then quenched. Samples were cut off each time after quenching. Metallographic samples 1/4 in. thick were removed at I hr., 6 hr., 24 hr., 96 hr. and 701 hr. After 96 and 701 hr. samples of about I in. were removed for X-ray analysis. 6. The metallographic samples were polished on the cross section and photomicrographs were taken. 7. The I-in. samples were polished and etched on both ends. With the aid of a microscope each was carefully mounted in a four-jaw chuck in a lathe, so that they could be accurately bored for an arbor. 8. Turnings were taken for each X-ray sample. After each set of turnings, the sample was heated in an oil bath for about 1/2 hr. at 300°C. It was then etched in 25

Jan 1, 1942

By L. G. Schulz, P. Spiegler

The electrical resistivity and the temperature coefficient of resistivity were measured with a potentiometric method using pure mercury as a reference material. Measurements were made nea,v roorn temperature. A detailed study was made of Hg,TI, near its melting temperature. THE work to be described was originally undertaken to provide the necessary data for interpreting the results of some optical experiments,' but because of the growing importance of liquid metals,273 it appeared that the results of the resistivity measurements should be published separately. For convenience the alloys selected were those which are liquid at room temperature. Special consideration was given to the Hg-T1 alloy closely corresponding to Hg,Tl, because recent X-ray diffraction results of Smallman and Frost seemed to show that the solid structure may persist to some extent into the 1iquid. EXPERIMENTAL PROCEDURE A potentiometric method was employed in which the resistivity of mercury was used as a reference. The essential features of the samples are shown in Fig. 1. A capillary tube CT with a bore of approximately 1.5 mm was fitted into two end cups, T, which were made of Teflon. A pair of current electrodes CE were immersed into the excess liquid metal which partly filled the end cups. The potential electrodes PE were inserted into CT through short pieces N of a no. 18 hypodermic needle held in place with Saureisen cement SC. As shown, the lower ends of the PE7s were reduced in diameter to 0.25 mm to minimize the distortion of the liquid metal cross section. Several methods were used to insert an alloy into the sample, but the usual one with mercury alloys was to fill the sample container with a weighed quantity of pure mercury* and then add weighed the sample tube in a vacuum. Because of rapid corrosion, samples containing gallium were of necessity prepared in a vacuum. To obtain the specific resistivity of an alloy the resistance of the sample containing the alloy was measured and compared with the resistance when the container was filled with mercury. Resistances were measured in the temperature range of 20" to 60°C to obtain the temperature coefficient of resistance. The electrical measurements were made by connecting the sample in series with the standard one-ohm resistance, and the potential drop measured alternately over the sample and the standard resistance. To correct for stray thermoelectric effects provision was made for reversing the direction of the current, and the true potential drop was taken to be the average of that obtained for the two directions of current flow. Various materials were used for the electrodes, the most uniform results being obtained with nickel. EXPERIMENTAL RESULTS The numerical results are presented graphically in Figs. 2 and 3 and in tabular form in Tables I and 11. Following are remarks on results of individual alloys. 1) Hg-In—This was the first alloy studied, and

Jan 1, 1960

I. PRESIDING OFFICER, At all business meetings of the Institute the President, or, in his absence, the First Vice-President, or, in the absence of both of them, any other Vice-President or Director, chosen by the meeting, shall preside. At all other meetings of the Institute the President, or, in his absence, one of the Vice-presidents shall preside. If none of these be present the meeting shall elect a Chairman. The President shall do and perform such other duties as may from time to time be assigned to him by resolution of the Board of Directors of the Institute. II. ORDER OF BUSINESS. At each business meeting of the Institute the order of business shall be as follows: 1. Reading of minutes of preceding meeting. 2. Report of the President, 3. Report of the Treasurer. 4. Report of the Secretary. 5. Election of Directors. 6, Reports of Standing Committees. 7. Reports of Special Committees. 8. Special Orders. 9. Miscellaneous business. This order of business may be changed at any meeting, by a vote of a majority of the Members and Associates present. At all sessions of the Institute, other than business meetings, the order of proceedings and the time of adjournment shall rest in the discretion of the presiding officer. III. SECRETARY OF THE INSTITUTE. The Secretary shall keep a record of the proceedings of all the meetings of the Institute, He shall be custodian of the corporate seal, of the minute books and of all the legal documents belonging to the Institute. He shall have charge on behalf of the Institute of all correspondence. He shall notify all Officers and Directors and all members of committees of their election and appointment; shall issue notices of all meetings of the Board, and of the annual and other business meetings of the Institute; and shall, in calling special meetings of the Directors, specify the objects of such meetings. He shall act as clerk at all the meetings of the Board of Directors and at all meetings of the Institute, The Secretary shall be custodian of all technical or scientific papers submitted to the Institute for its consideration and shall have general charge and supervision of the editing and proof-reading of all material published by the Institute, and of the distribution thereof. The Secretary shall be the custodian of all back numbers of the Transactions and other publications of the Institute. There shall be kept under his direction an account in ledger form of all such back numbers, He shall on the first day of January of each year submit to the Library Committee a statement of the number of copies of Transactions, magazines and other publications printed during the preceding year, giving the number distributed and remaining undistributed; also a statement covering additions to and withdrawals from the total stock of Institute publications, with the number 'remaining on hand at date of statement,

Jan 1, 1928

By James H. Courtright, Kenyon Richard

L. H. Hart (Chief Geologist, American Smelting & Refining Co.)— Because of a widely recognized association between breccia pipes of one form or another and many important copper deposits, conditions under which breccia pipes develop have been of great scientific interest for many years. Since these phenomena first attracted attention, many theories have been advanced to explain their origin. This is not unexpected, since it is likely that they have been formed by and under a wide range of conditions. Moreover, the entire subject is confused by the fact that the term brec-cia pipe is applied to a wide variety of occurrences. To discuss any part of the subject intelligently, therefore, it is necessary to start with definitions of the terms used. In their discussion of the Toquepala deposit, Richard and Courtright have carefully defined the terms they have used in their presentation of a very logical geological history of Toquepala breccias. This is a real contribution, as there is no reference in the literature known to the writer where the history of a series of breccia pipe epochs, confined essentially within one channelway, may be read with the degree of certainty that appears to be possible at Toquepala. Although the following comments are intended primarily to emphasize points brought out in the article by Richard and Courtright, certan subsequent detailed mapping by Hollister and Houston7 within the main central mineralized area of the Toquepala deposits not only supports most of Richard's and Courtright's con- clusions but also contributes additional facts that strengthen and broaden the whole concept of the origin of the Toquepala breccia pipes. In detailed mapping by Hollister and Houston,' the most significant feature disclosed is a well developed system of concentric fracturing in rocks peripheral to the main breccia pipe throughout an arc of 300°, interrupted only by the late dacite agglomerate in the north quadrant. Although Richard and Courtright noted that such fractures were developed in the southern and southeastern areas, continuity in the east and west quadrants is established by consistent orientation of the stronger set of fractures and joints. The existence of these structural weakness trends is emphasized by the emplacement of dike-like phenomena in and along members of this fracture system. Richard and Courtright described one of these dikes in the southeast quadrant. They referred to it as a ring-dike, composed of dacite porphyry. This suggests an apparent structural control of at least a part of the dacite porphyry intrusion by features related to the Toquepala breccia pipe center. This raises a perplexing question, since the dacite porphyry intrusion had been presumed to antedate breccia pipe activity. However, if this ring-dike is related to the breccia pipe center, it may indicate that some part of the dacite porphyry intrusion advanced in a manner resulting in an intensely localized stress center, which produced the concentrically arranged fracture system. The ring-dike would then appear to be evidence strongly sug-

Jan 1, 1959

By A. V. Deforest, C. W. Macgregor, A. R. Anderson

One of the important problems in the design of structures and machine parts subjected to rapidly applied loads is the determination of the strength and ductility of the material itself under such conditions. Realizing the need for such information, many investigations have been carried out in the past. Most of these experiments have been made using notched bars in bending either with the Charpy or Izod impact machine. While yielding valuable data on the effect of notches in the energy absorption of the material and on the condition of heat-treatment, this form of test does not lend itself readily to a determination of fundamental stress-strain relations. For this and other reasons, more attention has been paid recently to the tension impact test. An extensive literature already exists on the subject and only those investigations somewhat closely related to the present paper will be mentioned. For a more comprehensive list, the reader is referred to the Symposium on Impact Testing or the A.S.T.M., 1938. The work of Mann.' Clark and Dätwyler,2 Nádai and Manjoine,3 Winlock and Leiter,4 Deutler,5 and Brinkmann,6 however, deserves especial mention. In most of the previous investigations on the subject, when stress-strain relations were obtained under high rates of loading, it was the common procedure to determine stresses based on the original area and strains based on the original length. Stress-strain curves were then constructed by P ALo plotting So = 1/A0 as a function of eo = ALr,o where A0 and Lo refer to the original area and gauge length, respectively. At present there exists a paucity of true stress-strain data in the impact problem. The advantages of constructing so-called true stress-strain curves in order to reveal the fundamental physical properties of the material for the tension test were discussed recently by one of the authors.7'8 It was shown that the true physical behavior of the material in the tension test could best be represented P by plotting the average true stress, S = 2P as a function of 6 = q' = log —r = log ~9L where P, A, L, S, E, and q' refer to the load, the cross-sectioned area while the load P is applied, the actual gauge length, the average true stress, the true strain and true reduction in area, respectively. Besides giving a better physical representation, the method has certain additional advantages in that the stress-strain curve so plotted becomes a straight line from the maximin load point to fracture. The construction of such curves, however, while comparatively simple for the slow rates of loading customarily used in the tension test, presents certain dificulties for tensile impact in that both loads and diameters are required throughout the test. The continuous measurement of test-piece diameters to fracture under impact conditions offers considerable experimental difficulty. In order to make it feasible to

Jan 1, 1942

By A. V. Deforest, A. R. Anderson, C. W. MacGregor

One of the important problems in the design of structures and machine parts subjected to rapidly applied loads is the determination of the strength and ductility of the material itself under such conditions. Realizing the need for such information, many investigations have been carried out in the past. Most of these experiments have been made using notched bars in bending either with the Charpy or Izod impact machine. While yielding valuable data on the effect of notches in the energy absorption of the material and on the condition of heat-treatment, this form of test does not lend itself readily to a determination of fundamental stress-strain relations. For this and other reasons, more attention has been paid recently to the tension impact test. An extensive literature already exists on the subject and only those investigations somewhat closely related to the present paper will be mentioned. For a more comprehensive list, the reader is referred to the Symposium on Impact Testing or the A.S.T.M., 1938. The work of Mann.' Clark and Dätwyler,2 Nádai and Manjoine,3 Winlock and Leiter,4 Deutler,5 and Brinkmann,6 however, deserves especial mention. In most of the previous investigations on the subject, when stress-strain relations were obtained under high rates of loading, it was the common procedure to determine stresses based on the original area and strains based on the original length. Stress-strain curves were then constructed by P ALo plotting So = 1/A0 as a function of eo = ALr,o where A0 and Lo refer to the original area and gauge length, respectively. At present there exists a paucity of true stress-strain data in the impact problem. The advantages of constructing so-called true stress-strain curves in order to reveal the fundamental physical properties of the material for the tension test were discussed recently by one of the authors.7'8 It was shown that the true physical behavior of the material in the tension test could best be represented P by plotting the average true stress, S = 2P as a function of 6 = q' = log —r = log ~9L where P, A, L, S, E, and q' refer to the load, the cross-sectioned area while the load P is applied, the actual gauge length, the average true stress, the true strain and true reduction in area, respectively. Besides giving a better physical representation, the method has certain additional advantages in that the stress-strain curve so plotted becomes a straight line from the maximin load point to fracture. The construction of such curves, however, while comparatively simple for the slow rates of loading customarily used in the tension test, presents certain dificulties for tensile impact in that both loads and diameters are required throughout the test. The continuous measurement of test-piece diameters to fracture under impact conditions offers considerable experimental difficulty. In order to make it feasible to

Jan 1, 1942