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By Franklin G. Pardee

WARTIME depletion of the reserves of iron ore in the Lake Superior region of the grade and character now being shipped down the Lakes was serious. The time has come to take stock of the resources that remain in order to plan our future program of supply for our blast furnaces and protect, as far as possible. the tremendous investment made in the Lake Superior iron mining industry. Hugh M. Roberts and William H. Crago have estimated the reserves of the Lake Superior region in the United States at two billion long tons. These reserve figures are of direct-shipping ore and those concentrates produced by methods now in commercial use or those methods that may be expected in the near future. In their estimate they have assigned 392 million long tons to the Michigan ranges (all reserves in long tons) : 112 million tons for the Gogebic. 140 million tons for the Menominee, and 140 million tons for the Marquette.

Jan 1, 1948

By AIME AIME

IN furtherance of the policy of acquainting those members of the Institute who live at a distance from New York with all the details of administration, the thirty delegates sent by the local sections and the technical divisions were invited to attend the meeting of the Directors on Tuesday evening as well as the Directors' dinner immediately preceding. Including the Directors and officers, new and old, the members of the Papers and Publications Committee and the section delegates, more than 70 sat down at the dinner table in the Engineers Club. The attendance at the business meeting that followed was not quite so large, doubtless for the reason that the ladies' fashion show, held in connection with the informal dance, offered attraction that eclipsed that of watching the wheels of Institute business go around.

Jan 1, 1930

By Vincent P. Gi. ccnella

GOLD was discovered in Gold Canyon on May 15, 1849. Following this discovery placer miners worked the gravels in the canyon for-ten years, finally discovering the outcrop of the Comstock lode at Gold Hill in May, 1859, and in Ophir ravine on June 12 of the same year. Before long large quantities of gold and silver, were taken from the lode and one of the West's most spectacular mining booms drew thousands of fortune seekers to Nevada. After a long period of production activity waned and in late years little mining was done. The recent reopening of the old mines and the discovery of ore in other parts of the vein, and in other veins of the district, has led to a revival of interest in the Comstock. Virginia City, Gold Hill, and Silver City, situated along the great vein system, are enjoying a period of prosperity and a large influx of people.

Jan 1, 1934

By AIME AIME

THE petroleum economics session," held on Wednesday morning, Feb. 20, 1929, presided over by Campbell Osborn, chairman, proved to be of un- usual interest and resulted in serious and constructive discussion of the papers presented. The first paper on the program, "Gasoline Economics and Refinery Operation," was by H. J. Struth, petroleum economist of the Gulf Publishing Co., Houston, Tex. While this paper was intended to cover the re- finery situation, it also presented the author's reasons for believing that the oil producer should give cognizance to gasoline demand as a most reliable barometer by which to parallel the production of crude petroleum. The discussion which followed brought out some interesting points in connection with the immediate outlook for the industry as a whole during the present year. Some advanced the opinion that, regardless of the out- come of proration efforts, the refiner is in a position to conduct his operations on a reasonably profitable basis, provided that he exercises control over them. This would mean running less crude and resorting to wider utilization of cracking to produce the gasoline demand. Thus, if the refiner uses diligent care in scheduling his still runs, the producer will be obliged to carry over a large stock of crude this year, unless he is able to keep production below the limits prescribed by the demand for gasoline.

Jan 1, 1929

By R. E. Grant

THE Cerro de Pasco Railway Co., owned and operated by the Corporation, is a common carrier whose chief functions are transportation of ore and concentrates from the mines at Cerro de Pasco to the smelter in Oroya, and haulage of coal from the coal mines at Goyllarisquisga to the coal washery at Fundicion. Connecting with the Peruvian Central Railway at Oroya, the C. de P. Railway maintains joint, daily freight and passenger service from Lima and the port of Callao to Cerro de Pasco, terminal of the C. de P. main line and gateway to the Huanuco Valley. Extending from Oroya to Cerro de Pasco the main line is a standard-gauge roadbed of 70-lb. rail, 132 km. long with a maximum compensated grade of 2.25 per cent and a curvature of 16°, climbing from an elevation of 12,272 ft. above sea level at Oroya, lowest station on the line, to 14,208 ft. at Cerro de Pasco. The highest point reached by the C. de P. is on the coal branch at Alcacocha where the rails are 14,385 ft. above the sea.

Jan 1, 1945

By R. G. Green, R. L. Dowdell

LEAD POISONING as a result of eating lead pellets deposited in marsh areas is a cause of high mortality among ducks, geese, and other waterfowl ingested lead shot become trapped in the gizzard with gravel and are slowly ground away by the grit. Absorption of lead as it passes through the intestine in a finely divided state produces severe lead poisoning which is usually fatal. Ducks and geese with lead poisoning develop first a typical green diarrhea. Later, paralysis of the wing muscles prevents flight. As the poisoning continues with further grinding of the shot trapped in the gizzard, increasing paralysis reduces the bird to helpless-

Jan 1, 1937

By R. S. McClellan

Western Talc Company, Inc., with headquarters in Los Angeles, Calif., has just completed an extensive modernization and expansion program at its talc mine near Tecopa, Calif., and at its talc and clay mills at Dunn Siding, Calif., the nearest rail shipping point to the mine. The basic objective of the program was to provide facilities necessary to produce 300 tpd of a wide range of ground talc and clay grades for the ceramic, paint, paper, rubber and other industries. In the planning of the program every effort was made to provide a system which would permit a high degree of quality control and uniformity of the finished products, along with efficient operation. Several years ago, R. T. Vanderbilt Co., Inc. purchased Western Talc Co. after a comprehensive investigation of its properties, including an extensive diamond drilling campaign. Western Talc's properties embraced a number of claims in the Resting Springs mining district in the northern part of San Bernardino Co. and the southern part of Inyo Co., Calif., some seven miles southeast of the town of Tecopa. Operations by the original company were started on a small scale in 1913 and production from that date to the time of purchase of the company by Vanderbilt is estimated at 250,000 tons. The major part of this output was sold to the ceramic wall tile industry.

Jan 3, 1968

By Gene D. Clayton, Robert R. Dimock

A time-consuming and expensive preshearing program to minimize the adverse effects of blasting on slope stability at Kennecott Copper Corp.'s Ruth Pit in east-central Nevada has been eliminated in favor of down-the-hole, nonelectric delayed blasting which can produce a smooth wall effect and improve blast fragmentation. The new blasting approach resulted from a Kennecott engineering investigation aimed at improving the stability of the extremely variable rock conditions found throughout the pit by reducing the vibrational energy imparted to the walls with conventional bench blasts.

Jan 4, 1977

By A. W. Furbank

IN reviewing the aerial cameras produced in different countries, it becomes apparent that in nearly all of them an attempt has been made to secure the greatest possible angle of view. This angle, of course, is determined by the objective. The objectives most commonly in use in aerial cameras have a maximum angle of 65°. The objective developed for this new Zeiss camera combines freedom from distortion and brilliant definition, with an angle of 95°. Aerial mapping, it is claimed, has been placed on a different economic basis, and new possibilities presented, par-ticularly in connection with automatic stereoscopic plotting instruments, to which some short references are made. One way of enlarging the angle of view is to couple several instruments with their axes convergent, thereby producing a multilens camera. Typi-cal of cameras of this sort in the United States is the Bagley four-lens camera, which later was developed into the five-lens camera (T3-A) of the U. S. Air Corps. More recently, in order to get away from the unfavorable Maltese cross image field of the five-lens camera, and to obtain a more practical form, two five-lens cameras were combined. By using them in tandem and rotating them by 45° relatively to each other, a ten-lens camera was produced, covering an octagonal ground area, with a total angle of view of 140°. Similar designs have been evolved in other countries. In all of them, however, a number of difficulties have arisen, quite apart from their large weight and high cost. Because of their complex mechanism, numerous shutters and magazines, and the high precision with which these parts must be interadjusted and synchronized, these cameras are far from dependable. Moreover, a multilens camera by itself does not yet constitute a complete outfit for producing pictures suitable for photogrammetric survey. Because all the component pictures, except the central one, are obliques, it is always necessary to employ rectifying apparatus which transforms the marginal views to the perspective of the central one. In multilens cameras with many individual magazines, it is not convenient to

Jan 1, 1938

By R. B. Woodworth

In the sinking of bore holes, there are but two fundamental operations —drilling and hoisting—which determine in the main the character of drilling mechanism and structures. There are endless ramifications, however, in the execution of these fundamental operations, according to the purposes for which the bore holes are drilled, their maintenance after completion, the protection and convenience of workmen, etc. The three main lines of use for bore holes are in mineral exploration, the sinking of water and salt wells, and the exploitation of pqtroleum and natural gas. This paper has to do more especially with the last. Here again there are many divergences. Wells may be drilled by either the percussive, the hydraulic, or the abrasive method. Finally, each of these methods, as applied by drillers of diverse nationalities, has followed somewhat different lines of development. The American system of cable-tool drilling has perhaps had the widest application; the hydraulic rotary is also in extensive use; but the Canadian system, the Galician system, and the Russian free-fall system all have their points of recognized merit and are preferred by operators accustomed to their use. These differences in drilling procedure, which rest ultimately on essential variations in geological conditions, are reflected in the drilling structures as well as in the drilling mechanism. The purpose of the present paper is to record those stages in the development of the application of steel to the construction of drilling mechanism and structures with which the writer has been intimately associated, and to contribute to the history of the art of drilling other data acquired in the course of his personal investigations. It is necessarily limited by reason of space to American practice, with especial reference, therefore, to the cable-tool system and the hydraulic rotary method of drilling wells for oil and gas.

Jan 1, 1916

By V. E. Elliott, C. L. Meyette

THE conditioning of semifinished steel products such as billets, blooms, and slabs to remove surface defects before further processing to finished products is a necessary accompaniment to steel mill rolling operations. A knowledge of the kinds of defects which occur and of the conditions in melting, teeming, and rolling that may lead to their occurrence is favorable to the production of quality products. Surface defects may be classed as either of mechanical origin such as those that occur in the heating and rolling operations and include breaks, tears, guide marks, mechanical laps and the like, or they may have been in the ingot before heating and rolling. Examples of the latter are ingot cracks, blow-holes, scabs, and inclusions which lead to the numerous known types of seams -and surface flaws. Most of the common types of surface defects and methods for their identification by visual examination or by the aid of macro-etch tests are well known. The conditions which caused their formation are also appreciably understood and this knowledge has been instrumental in the establishment of methods for metallurgical control. There are, however, defects of doubtful origin. In any endeavor to trace the causes for their occurrence, the question of first concern is: I. Whether they were formed in the rolling procedure. 2. Whether they existed in the ingot prior to rolling. In the case of semifinished products which are rerolled to finished products there is also the question of whether they were formed in the primary or in the secondary rolling. In metallurgical laboratories where numerous or routine examinations of the quality of rolled products are made over the course of time, there will doubtless be many puzzling cases of defect origin. Microscopic examination of the defects may, however, reveal a characterizing condition that can be used to classify them broadly with respect to their origin. Such a condition has been observed and, after detailed investigation, is described here with the thought that it may offer a useable and relatively simple solution to a bothersome problem. BASIS FOR CLASSIFYING In this discussion the term "mechanical type defects" will be used to designate those that have occurred as a result of the rolling operations such as in rolling from the ingot to billets, blooms, or slabs or in rerolling to finished products. The term "steel type defects" will he used to designate those that were present in the ingot prior to primary rolling or that were in the semifinished product prior to secondary rolling to finished product. The basis for distinguishing between the two types of defects lies in the relative degree of subscale formation surrounding them. Subscale is defined' as a zone of

Jan 1, 1948

[A Aamodt, H. C., A55 C Sales, Great Lakes Carbon Corp., 18 E. 48th St., New York, N.Y. Aamot, Olav Crone, M29 2126 M4, Galveston, Texas Aaronson, Hubert I., M47 E Prin Res Engr, Ford Motor Co., Met. Dept., Sci. Lab., Engrg. Staff, P. O. Box 2053, Dearborn, Mich. Aase, Glenn D., M54 D Prin Engr, Air Pollution Control Dist., 1480 Mission St., San Francisco 3, Calif. Abbett, W. A., Jr., M56 8629 Beverly St., Duluth 8, Minn. Abbey, Robert G., M56 138 Dartmouth Rd., Bala Cynwyd, Pa. Abbott, A. G., Jr., J52 E Test, Dev Engr, Chrysler Corp. Missile Div., P. O. Box 2628, Detroit 31, Mich. Abbott, Mark L., A58 Rep, General Refractories Co., 208 S. LaSalle St., Chicago, Ill. Abbott, W. K., J58 E Dev Met, Int'l Nickel Co., Inc., 67 Wall St., New York 5, N.Y.]

Jan 1, 1961

By L. D. Lamont, W. C. Muehlhof

Throughout the anthracite industry's history, the problem of handling and disposing of refuse material has been one of major importance. In the early days of the industry's activities, only the large sizes of anthracite were satisfactory for market requirements and the smaller sizes were deposited as refuse. As time went by, more efficient coal-burning equipment was developed and a market demand was created for the finer sizes of coal. This demand made it possible to recover marketable coal from banks deposited as refuse in the earlier days of mining. The same condition holds good today and we can see a definite trend toward the objective of utilizing the No. 4 and No. 5 buckwheat sizes. Under present conditions, we know that a limited market exists for No. 4 and 5 buckwheat; we know that the finer sizes of anthracite can be burned as pulverized fuel; we know that these fine sizes can be processed and sold as briquettes, and we also know that the heat content of these fine sizes of coal is comparable with that of the sizes now merchandized. Therefore, it should be the objective of the industry to conserve these fine sizes of coal in such manner that if and when processing facilities are developed, and market demands exist, the material can be salvaged and made available to meet these demands. From the standpoint of economical future reclamation, the ideal method of disposing of refuse containing the finer sizes of coal is to deposit it in banks separate and apart from other breaker refuse. By this procedure, the minimum amount of material will be processed in future salvage operations to recover the No. 4 and No. 5 buckwheat sizes. Many collieries in the anthracite region are operated under leases that have a specific term. These lease agreements provide that, upon expiration of the lease by term, exhaustion or otherwise, the ownership of the refuse material reverts to the lessor. Therefore, a question was raised in the minds of these operators: Why should I assume the expense of such procedure when I have no assurance that I will benefit by the future processing and sale of these fine sizes? Under present conditions, the answer to this question is not one of choice but of necessity, as restrictions imposed by legislation make it mandatory on operators of preparation plants to take necessary steps to properly treat silt-laden waters before permitting them to enter the streams. By reason of these restrictions, the disposal of fine sizes becomes a secondary rather than a primary operating consideration, and the procedure for disposing of this refuse becomes a matter of choice governed principally by topographical and geographical conditions. Methods of Handling Refuse There are three principal methods of handling and disposing of fine-size refuse; namely:

Jan 1, 1947

By W. C. Muehlhof, L. D. Lamont

Throughout the anthracite industry's history, the problem of handling and disposing of refuse material has been one of major importance. In the early days of the industry's activities, only the large sizes of anthracite were satisfactory for market requirements and the smaller sizes were deposited as refuse. As time went by, more efficient coal-burning equipment was developed and a market demand was created for the finer sizes of coal. This demand made it possible to recover marketable coal from banks deposited as refuse in the earlier days of mining. The same condition holds good today and we can see a definite trend toward the objective of utilizing the No. 4 and No. 5 buckwheat sizes. Under present conditions, we know that a limited market exists for No. 4 and 5 buckwheat; we know that the finer sizes of anthracite can be burned as pulverized fuel; we know that these fine sizes can be processed and sold as briquettes, and we also know that the heat content of these fine sizes of coal is comparable with that of the sizes now merchandized. Therefore, it should be the objective of the industry to conserve these fine sizes of coal in such manner that if and when processing facilities are developed, and market demands exist, the material can be salvaged and made available to meet these demands. From the standpoint of economical future reclamation, the ideal method of disposing of refuse containing the finer sizes of coal is to deposit it in banks separate and apart from other breaker refuse. By this procedure, the minimum amount of material will be processed in future salvage operations to recover the No. 4 and No. 5 buckwheat sizes. Many collieries in the anthracite region are operated under leases that have a specific term. These lease agreements provide that, upon expiration of the lease by term, exhaustion or otherwise, the ownership of the refuse material reverts to the lessor. Therefore, a question was raised in the minds of these operators: Why should I assume the expense of such procedure when I have no assurance that I will benefit by the future processing and sale of these fine sizes? Under present conditions, the answer to this question is not one of choice but of necessity, as restrictions imposed by legislation make it mandatory on operators of preparation plants to take necessary steps to properly treat silt-laden waters before permitting them to enter the streams. By reason of these restrictions, the disposal of fine sizes becomes a secondary rather than a primary operating consideration, and the procedure for disposing of this refuse becomes a matter of choice governed principally by topographical and geographical conditions. Methods of Handling Refuse There are three principal methods of handling and disposing of fine-size refuse; namely:

Jan 1, 1947

By Marcus A. Grossman

THE institute has established this lectureship to honor the memory of a great American metallurgist, one whose fame has continued long after his passing. As one scientist recently stated it," All metallurgical texts gradually become outdated and outmoded, except those of the great Henry Marion Howe." It seems fitting, then, that, once every year, we should review, in his honor, some aspects of the science in which he was such a distinguished leader, and also discuss any new data that may help to clarify our concepts. It is my privilege, for which indeed I express the deepest appreciation to this Institute, to offer for consideration a few thoughts on the toughness and fracture of hardened steels. Before proceeding to the data, I wish to express my great indebtedness to many associates whose stimulating discussions, generous contributions of data and cooperation in experiments are gratefully acknowledged. (But I wish to absolve them of any blame that may arise from the way in which their discussions and data have been used!) First, Dr. Edgar C. Bain, Vice President, Carnegie-Illinois Steel Corporation, whose amiable but merciless criticisms and always constructive and thoughtful suggestions help unfailingly to guard against pitfalls. Then to associates at Gary Steel Works, especially Mr. H. B. Wishart, Mr. W. K. Smith and Mr. V. Elliott, for great assistance in securing data. Also to Col. C. H. Greenall, Director of Laboratories, Frankford Arsenal, and his metallurgical staff, including Messrs. J. K. Desmond, H. Markus, D. F. Armiento, H. Rosenthal and Henry George, for numerous data and illustrations. Further to Dr. J. R. Low and Dr. M. Asimow, for helpful discussions of effects of states of stress during deformation and rupture, to Mr. J. M. Hodge for discussions and data, to the staff of the U. S. Steel Corporation Research Laboratory for advice and data, and to the Metallurgical Staff at Duquesne Steel Works. The individual acknowledgments will also be found under illustrations. Acknowledgment is also due to Mr. S. C. Snyder for incredibly meticulous scrutiny of manuscript. To all of these, grateful thanks.

Jan 1, 1946

By K. L. Fetters, F. M. Walters

ALL previous records were broken by the Iron and Steel Division, in the number of sessions, the number of papers, and the attendance. In addition to ten papers (all preprinted) on properties, structure, aid hardenability of, carbon and alloy steels, eight formal papers were presented on one or more phases of steelmaklng, and a symposium on the determination of hydrogen and nitrogen in steel. This last started at 2 p.m. and was going strong with more than a third of the audience still present at 6 p.m.

Jan 1, 1944

By WILLIAM J. LINNEY

MAGNETITE ore from Lyon Mountain, so- called "Low Phos Chateaugay," has long been known to the iron and steel industry for its almost complete absence of impurities. These magnetites occur along the northern foothills of the Adirondacks in several parallel and folded stringers which are continuous for several miles, striking generally northeast-southwest and dipping usually over 45° to the northwest, or roughly toward the St. Lawrence River. Ore of minable thickness is found in shoots of various sizes as to length and breadth, but of undetermined and possible great depth.

Jan 1, 1943

By G. L. Fisher, R. Maddin

The rate of self-diffusion in silver single crystals during torsional strain was measured over a wide range of tenperatures and strain rates. The torsional strain was applied in a cyclic manner by reversing the divection of twist aftev a certain fraction of the total strain was reached. Surface roughening was substantially reduced in cyclically strained specimens compared with those strained entirely in one direction. Diffusion coefficients were determined using a special sectioning technique whereby slices could be removed parallel to the surface of a strained torsion specimen. The accuracy of the technique was first determined using roughened specinzens statically diffused to various penetration depths. Simultaneous strain-diffusion experiments were then performed over the temperature range 550' to 800 using strain rates of lo-' to 2.2 x 10' sec-'. The increase in silver self-diffusivity during torsional plastic strain was small. In only one case was the enhancement greater than twice the static value of the diffusion coefficzent. The enhancements increased slightly with decreasing tenzperature and increased with increasing strain rate. A dislocation pipe mechanism of enhancement was found to explain the present results satisfactorily. The magnitude of the enhancements and the tenzperatures at which they were observed suggests that a steady-state dislocation density of 10' to 109 dislocations cm-2 existed during the high-tempevature deformation. The diffusion coefficient in an fcc metal can be increased by 1) an excess concentration of point defects and 2) the rapid movement of diffusing atoms along grain boundaries and dislocations. Plastic deformation may be responsible for enhancements by both of these mechanisms. The results of simultaneous strain-diffusion experiments have caused a controversy over the magnitude of the effect of strain upon diffusion. Experiments reporting large enhancements have been criticized for the manner in which the diffusion coefficient was measured. Several of these experiments have been contradicted by other results obtained in a similar manner. No enhancement was reported by two investigators''' who performed their experiments at high temperatures where strain is expected to have little effect upon diffusion. A recent theoretical analysis3 indicates that strain enhancement by a vacancy mechanism will be small and exist only at low temperatures and rapid strain rates. It is doubtful whether any experiment has yet proven that strain enhancements can occur by an excess vacancy mechanism. In the present research, experiments were performed at extremes of temperature and strain rate in an attempt to measure enhancement of diffusion by strain. Self-diffusion of silver during torsional deformation was chosen since two separate investigations4j5 indicate that at least a small enhancement exists under these conditions. An accurate method of determining the diffusion coefficient, mechanical sectioning, was employed after a technique was devised to apply it to the roughened surface of a strained torsion specimen. First, the accuracy of the technique was determined for different penetrations (2fi). Then diffusion experiments were performed at temperatures between 550" and 800°C at strain rates of 10"" to 10"" per sec. I) EXPERIMENTAL PROCEDURE Preparation of Specimens. The experimental procedure detailing the growth of crystals, their treatment, and the annealing techniques during straining are contained in earlier publications.496 The dimensions and orientations of the torsion specimens are shown in Figs. 1 and 2. licatiin of Torsional Strain. The torsion procedure was changed from that used previously. The specimens were strained in cycles to reduce the gross distortion and surface roughening inherent in twisting to high strains in one direction. For all strains above 0.30, the total surface strain was obtained as follows: the specimen was twisted to 0.10 strain in a clockwise direction; the direction was reversed; the backlash in the torsion apparatus was taken up; and the specimen was twisted in a counterclockwise direction through the initial starting point to 0.20 surface shear strain in the opposite direction. The strain reversal took no more than 1 min to accomplish. The total accumulated surface shear strain was arbitrarily taken as the sum of the 0.10 strain in the clockwise direction plus 0.20 in the counterclockwise direction. Although cyclic torsional strain was beneficial, surface roughening and specimen distortion were not entirely eliminated. The variation in the diameter at various points on the specimen was often much greater than the depth of the diffusion zone. Since serious errors might result if specimens were sectioned in the usual manner, a technique of lathe sectioning was devised to allow sections to be taken parallel to planes of equal concentration.

Jan 1, 1967

Jan 1, 1968

By P. R. Sahm, T. V. Pruss

Mixtures of fine GaSb and Gds as well as preal-loyed GaSbl,As, powders were hot-pressed at 690°C and 25,000 psi. Dense alloys with compositional gradients of less than 5 pct were obtained from mixtures containing about 20 mol pct GaAs. For x < 0.2, there were increasing compositional gradients, and for x > 0.2 a GaAs-rich second phase appeared in the microstructure. Densification as well as alloying wlechanisms were enhanced by dissociation and, possibly, oxidation reactions of the powders. Densification of coarse prealloyed material, however, primarily depended on plastic flow phenomena and required temperatures just below solidus and pressures of 50,000 psi Thermal and electrical properties were measured. Although in no case was the figure of merit of melt growth materials approached closer than to within 25 pct, the better overall thermoelectric properties were found in coarse-grained, prealloyed materzals which had been compacted to near theoretical density and where grain regrowth had been induced. Similar results are believed to hold in other binary 111-V compound systems if processed under similar conditions. The densification of unalloyed GaSb powders during pressure sintering (= hot pressing) was shown to depend strongly on powder particle size.&apos; Fine powders displayed a "liquid skin effect" that enhanced compaction through the presence of liquid gallium, whereas coarse powders compacted predominantly by plastic flow. The liquid skin effect, in particular, appeared attractive for alloying GaSb with other, higher-melting, III-V compounds, and to densify these in a one-step operation. This is of special interest in the case of III-V compound alloys as the conventional techniques of melt growth or long-time annealing of powders2 is very time-consuming, especially in cases where a large separation of liquidus and solidus can be expected, such as in GaSbl alloys.2 It was felt that experimentation with this system, a particularly unfavorable example, would allow us to extrapolate to several other, more favorable, cases. Uses of Ill-V alloys are most evident in thermoelectric energy conversion devices.&apos; For this reason certain thermal and electrical properties were measured and compared to those of melt-grown material and to hot-pressed prealloyed powders. EXPERIMENTAL PROCEDURE The pressure-sintering apparatus has been previously described.&apos; Using this equipment, both powder mixtures of GaSb with GaAs and prealloyed GaSbl-,As, powders were hot-pressed. The mixtures were pre- pared from cast GaSb and melt-grown GaAs. The prealloyed material was obtained from stoichiometric melts, initially heated to 1200°C in an evacuated quartz ampoule, and then annealed in the solidus-liquidus interval. A typical annealing cycle consisted of a heating to 850°C (1 hr), extended successive annealing at 750°C (65 hr), and slow stepwise cooling (25 hr) to below solidus. The GaSb, GaAs, and GaSbl-,As, materials were ground in a vibrational mill to particle sizes below 500 . A jet mill reduced these further where necessary. Fine powders were analyzed by Coulter counting for their size distribution. Average sizes by volume were calculated from the data. Mixing of the powders, where necessary, was carried out through rapid vibrational motion. The hot-pressing operation consisted of a degassing period of 15 hr, in most cases at 690°C, followed by several hours of compression, normally 25,000 psi at 690°C for powder mixtures and 50,000 psi at 710°C for prealloyed powders. The chemical compositions were confirmed by X-ray fluorescence analysis. To estimate the degree of solid solution achieved, lattice parameters were determined and interpreted according to Vegard&apos;s rule. In addition, optical microscopy helped to correlate the relative amounts of the phases present as well as the degree of porosity to the measured density. To reveal grain boundaries, polished surfaces were etched4 with H 2 O:H 2 O:HCl = 2:l:l. In several cases microscopic concentration gradients were monitored by electron-probe analysis-. RESULTS AND DISCUSSION Alloying and Densification of GaSn-GaAs Powder Mixtures. After preliminary experiments showed that no appreciable alloying took place in mixtures of coarse GaSb (22.5 p) and fine GaAs (2.5 p) powders, hot pressing of mixtures was confined to fine powders only (3.1 and 2.4 p, respectively). Alloying and densification apparently occurred simultaneously with a grain regrowth mechanism which depended on the presence of a liquid phase.&apos; The liquid phase was provided by the dissociation of GasbS particles into liquid gallium and antimony above 555°C. This not only enhanced grain regrowth and densification, as in unalloyed GaSb,&apos; but took on additional importance here for the alloying process. Alloying was speeded up by the resulting liquid-solid interaction as compared to the very slow solid-state diffusion process normally expected at these temperatures.&apos; The results obtained with a series of powder mixtures have been compiled in Table I. It is seen that for mixtures with less than 20 mol pct GaAs, x < 0.2, the compositional ranges increased and for x > 0.2 a GaAs-rich phase and free antimony appeared in the microstructure in sizable amounts.

Jan 1, 1968