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By R. M. Hudson, P. E. Perry

Weight-gain data obtained by nitriding low-carbon sheet steel in an amrnonia CNH,) atmosphere indicated that the process obeyed a parabolic rate law. The calculated actization energy for nitriding in the range 964" to 1268°F agreed reasonably well with published data. At 1358"F, rate data indicated that the activation energy decreased. Weight-gain data obtained by uszng mixtures of NH3 -Nz at 1268°F containzng jrom 10 to 100 zol pct NH3 also obeyed a parabolic rate law. The rate of 'nitriding increased with an increase in the NH3 content of the gas Mixture. It is well-known that steel heated in gas mixtures containing ammonia (NH3) takes up much larger quantities of nitrogen than steel heated in nitrogen, both gases having a total pressure of 1 atm;' this phenomenon can presumably be attributed to the catalytic decomposition of NH3 on the steel surface to furnish nascent (monatomic) nitrogen. This process was studied bv Brunauer. Jefferson, Emmett, and Hend-ricks at furnace temperatures of 752" and 831°F2 using mixtures of NH3 in Hz. Englehardt and wagner3 reported that, at a furnace temperature of 914°F and under their experimental conditions, both nitriding and denitriding were controlled by the rate of gas-metal reactions at a steel surface rather than by the rate of diffusion of nitrogen in iron. The present study was undertaken to obtain information on the kinetics of nitriding low-carbon steel strip at higher temperatures so that practical rates for short-time strip-annealing treatments could be estimated. Variables studied included time: temperature, and NH, content in the annealing atmosphere. Mechanical and chemical characteristics of steel nitrided in this manner will not be considered in the present article. MATERIALS AND EXPERIMENTAL WORK The samples used were from a commercial low-carbon steel, 0.0244 cm thick, in the cold-reduced condition. The chemical composition of this steel is given in Table I. Panels were cut to 5.1 by 17.8 cm, degreased in toluene, and weighed just before treatment. Four specimens were nitrided under each of the experimental conditions. A study was made of the nitriding rate of steel in a 100 vol pct ammonia atmosphere, 740 mm pressure, at five specific temperatures within the range 964" to 1358°F. The nitriding rates of steel in ammonia-nitrogen gas mixtures containing 10, 18, 26, 50, and 100 vol pct ammonia, 740 mm total pressure, at 1268°F were also determined. All atmospheres used were dried by successively passing them through drying towers packed with soda lime and with Linde Molecular sieve Type 4A. Quoted gas compositions refer to those entering the furnace. Specimens were held in the constant-temperature zone of a vertical annealing tube furnace for times of 14, 3, 5, 10, or 15 min. Gas flow rates were maintained at 3.8 cu ft per hr, which was nineteen volume changes per hour for the system used. The rate of flow was selected to provide a high level of free NH3 for cracking on the steel surface where the ammonia gas is most effectively used as a nitriding agent. The vertical annealing tube furnace consisted of a Hevi-Duty tube furnace with a 2 1/2-in.-ID mullite ceramic high-temperature tube. The constant-temperature zone (controlled within 10°F) was about 10 in. long. After each specimen was degreased, a hole was punched in one end, for attaching the specimen by hook to a chain so that it could be lowered into or raised from the high-temperature portion of the tube by means of a power-driven winch. A stainless-steel access port with O-ring seals was connected by suitable glass-to-metal seals to the cool upper portion of the furnace tube. After the weighed specimen was placed in the access port, the furnace tube was evacuated to approximately 10"3 torr, and then the system was flushed thoroughly with the atmosphere under study. When the gas flow rate and constant-temperature zone of the furnace were established, the specimen was lowered into the constant-temperature zone. The atmosphere flowed from the top to the bottom of the vertical furnace tube and was then vented. For all these runs, during the first 3 min of the time the specimen was in the constant-temperature zone of the furnace the specimen was heating up to the tempera-

Jan 1, 1970

By James Howe

EVERY engineer and user of wire rope is desirous of information that will enable him to determine whether the performance of any particular piece of rope is satisfactory, and what conditions can be changed so as to increase the life of a rope. In most cases, it is far from easy to analyze the conditions of service and tell which is the greatest factor in determining the life of wire rope. If we start on a layout for an entirely new rope system, the task of making conditions satisfactory is simplified so far as the engineering details are concerned; but if the plant requiring wire rope is in operation, any change is likely to involve the expenditure of consider-, able money to replace and change over machinery that must be kept in constant operation, because a large monetary loss will result from a shutdown for even a few days. Often wire rope is kept operating under bad conditions, as the user thinks that it is cheaper and quicker to replace the rope than to make alterations in the hoisting machinery. A typical case is a metal mine operating in what is now almost the center of a large mining city, where it owns a few acres of mineral rights. It was expected that the shaft would go to a depth of 1000 ft. (305 m.), so a moderate sized rope, about 1 ¼ in. (31.7 mm.), was used on a 6-ft. drum with a 7-ft. head-frame sheave and rather short lead from drum to head sheave. This mine has gone deeper each year until, it is now 2500 ft. deep and the rope speed has been increased from 1500 ft. per min. to over 3000 ft. The original rope just filled the drum in one layer, now it overwinds three layers. The original ropes were probably 6 X 19 crucible steel and lasted from 12 to 18 mo.; now, the highest grade plow steel is used, yet the average service is only about 6 mo. The cause is not hard to find. If the engineers had known at the outset what would be done with this hoist, the design would have been very different. Conditions at this mine, from a wire rope standpoint, have gradually become worse and it is difficult to see how rope service on this hoist can be com-pared with the service of previous years with any fairness to the wire-

Jan 2, 1922

By Y. Astafyev

In applying computers at the enterprises it is necessary to develop an open-pit model which completely corresponds in its structure, properties and characteristics to real open-pit mining. This model is used for controlling open-pit operations which ultimately define the system controlling ore reserves. The preparation and reserving of the latter are highly expensive and labour-consuming, therefore the investigations are aimed at developing the ore reserve control system which is capable to provide open- pits with the necessary ore reserves on the basis of equipment relibility characteristics, and thus helps to solve the ore reserves problem which is to define their optimum dimensions under conditions of stochasticity of production processes. In accordance with the tasks of the investigation it may be conventionally divided into three parts. The aim of the first part is to develop a structural open-pit system model consisting of a set of elements which are represented here by drill-rigs, shovels, trucks, unit trains, plant receiving bins and dumps (Fig. 1). The combination of similar elements makes up technological components the sequence of which forms simple systems. The latter, in their turn, grouping according to the type of mined rocks and inter- acting in parallel, form the "Stripping" and “Mining” subsystems. In addition to this, there is the "Ore Reserves" subsystem which serves as a "store" and includes opened-up, prepared and ready for extraction ore reserves.

Jan 1, 1977

By Henry G. Granger

A RESIDENCE of 14 years in the Republic of Colombia, spent in almost continuous traveling and prospecting-trips, has given me an intimate knowledge of the resources of that wonderful country. The man who best knows Colombia is unquestionably General Rafael Reyes, President of the Republic for the past three years, and with seven years more to serve in his present term. Such is the strength of his personality and the wisdom of his policies that his term of office will no doubt endure as long as he is willing to serve. The vastly improved economic situation and the brilliant outlook for Colombia are so directly due to the influence of President Reyes that a few lines concerning him. will not be amiss, if they serve towards a better understanding of his personality. Born of a distinguished ancestry in the mountains of Boyaca, he is now 57 years old, just the age of his friend Porfirio Diaz when be began the work which has placed Mexico in the rank of great modern nations. It was Reyes who came to Washington to protest against the action of the government of the United States of America in reference to the establishment of the Republic of Panama, and, without entering into a discussion of this affair, it can be fairly said that there was not an American in Colombia whose feelings of justice were. not outraged at the government action and subsequent refusal to submit the matter to the impartial judgment of the' Hague. President Reyes is an accomplished linguist, speaking English, French, German, Portuguese, Spanish, and Italian. He has a remarkably. powerful voice, which can readily be heard by a large assemblage. His height is about 6 ft., and his weight exceeds 200 lb. He has clear gray eyes. Reyes was the leader of those who favored the approval of

Sep 1, 1908

By Michael J. Messel

OF the various minerals that occur in fibrous form known as asbestos, chrysotile is the variety most in demand for commercial uses, and, last year, over 683,000 tons of the various grades were produced in Canada and United States, exclusive of African and Russian production, which figures are uncertain. Production has not been able to keep up with the increased demand, and an acute shortage exists. Canada, Russia, and Africa are still the most important producers. However, Russia consumes most of its production at home and exports very little. The United States consumes over 60 pct of the total production and produces only about 4 pct of the total from deposits in Vermont and small quantities from Arizona. This paper will review mainly, some of the more recent developments concerned with the extraction and processing of this fibrous mineral for various industrial uses, such as textiles, insulation, building materials and brake linings.

Jan 1, 1949

By Y. Nakahiro

The removal of heavy metal compounds from a synthesized waste cyanide solution is achievable by a precipitation-flotation method. However, the differential separation of constituting metals by this method was thought to be very difficult. The present author found that addition of ferrous salt to the synthesized waste cyanide solution of cadmium and copper can modify the separation characteristics of these metals. In this paper, the separation of cadmium from copper in the synthesized waste cyanide water by the precipitation-flotation method is discussed. This differential flotation uses ferrous salt as a precipitant and sodium oleate as a collector. Based on a series of fundamental flotation tests, actual differential flotation tests were made. The separation of cadmium from copper in the synthesized waste cyanide water was found to be satisfactory. This method can be effective for the removal of difficult-to- separate colloidal precipitates from liquids by the sedimentation method, provided the applicability of this method to the separation of the other metals is promising. This consists of the intensive studies which have been conducted at author's laboratory.

Jan 1, 1980

By Nagel, Theodore

USE of oxygen in metallurgical operations was investigated by a committee of unusually able engineers more than ten years ago. A record of their work appeared under the title "The Use of Oxygen or Oxygenated Air in Metallurgical and Allied Processes," Serial 2502, Report of Investigations, U. S. Bureau of Mines. Shortly thereafter the A.I.M.E. published "Use of Oxygenated Air in Metallurgical Operations," based on a symposium at the New York meeting, February 1, 924. Quoting from the Bureau of Mines report In view of the many recent developments in oxygen manufacture, and considering the increasing cost and decreasing quality of our raw materials, the Bureau of Mines has taken the matter of the application of oxygen or oxygenated air to the metallurgical centers for consideration and has appointed an advisory committee to study the problem.

Jan 1, 1935

By E. A. Nesbitt

THE important permanent-magnet alloys 15 years ago contained carbon and depended upon it for their permanent- magnet properties. In recent years great, advances have been made in a number of new alloys substantially free of carbon. These include Remalloy,l an alloy of iron, cobalt, and molybdenum, the various iron- nickel-aluminum alloys of the Mishima2 type, and the more recent Alnico V3 in which the best properties are developed by heat-treating in a magnetic field. The Mishima and the Alnico types of alloys are very brittle and after casting must be ground to size. This article describes a permanent-magnet material4 that can be machined as cast, and when handled with some care can be .rolled to thin sheet and drawn to fine wire. Optimum magnetic properties are developed by a simple heat- treatment, and at this time the ductility A of the alloy disappears. If the cast alloy is heat-treated without cold-working the magnetic energy product is about 1.0 X 106. This material is called Vicalloy I (pronounced vicalloy, V for vanadium, I for iron, and C for cobalt). When the alloy is first hot-worked and then considerably reduced in area by cold-swaging, drawing or grooved rolling, it is found that after heat-treatment the magnetic energy product measured in the direction of previous extension can be increased to 2.0 to 3.5 X l06. These higher values have been obtained only after reductions in area of 75 to 95 per cent, and since the material hardens considerably during working, the reduction ordinarily can be accomplished only in fine wires, although larger sizes can be reduced by the use of powerful machinery. When the material has been cold- worked in such a manner as to improve its energy product substantially, it is called Vicalloy II. Commercial use of Vicalloy has been made in the recording of speech. Tape 0.002 by 0.050 in. has been found superior in quality to all others tried, and is now used in the Western Electric Mirrorphone In a variety of forms Vicalloy I or II is useful in many laboratory instruments, and in experiments in which the sizes and shapes required cannot be obtained with the other more brittle permanent-magnet materials. In 1936, during a study of other age- hardening magnetic systems, it occurred to the author that some of the iron-cobalt-vanadium alloys might be suitable for permanent magnets. The proportions of iron, cobalt, and vanadium were varied and a range of alloys of particular interest was found, as shown by the indicated area in Fig. I. The limits of this range of com- position are 30 to 52 per cent iron, 36 to 62 per cent cobalt, and 4 to 16 per cent vanadium. The compositions indicated by points outside this area were also tested. PREPARATION AND PROPERTIES OF VICALLY I The alloys were usually cast in graphite molds into bars ¾ in. in diameter and

Jan 1, 1946

By R. W. Diamond

THREE mills are now operated by the Consolidated Mining & Smelting Co. of Canada, Ltd:: (1) The Sullivan concentrator, Chapman, B. C. (near Kimberley, B. C.), (2) the St. Eugene concentrator, Moyie, B. C., and (3) the Tadanac (customs) concen-trator, Trail, B. C. Differential flotation is the only concentration method employed in all three plants. Tables are used for pilot work only. Flotation equip-ment and control are similar in the three mills, and the flow sheets at the St. Eugene and Tadanac mills, while much simpler, are modeled after that of the Sul-livan concentrator. Successful differential flotation of Sullivan ore com-menced in the spring of 1920, in the pilot concentrator at Trail. During 1920, 193,804 tons were treated by this process. This operation continued without interrup-tion and with steady growth. For the first 7 months of . 1923, which concluded the pilot plant operation, ap-proximately 1100 tons were treated daily. I believe the Sunnyside plant of the United States Smelting &. Refining Co. was the only successful and large scale operation practising differential flotation prior to 1920. in North America. The Sullivan ore, because of its high iron content, was quite a different problem from that at Sunnyside. The entire tonnage of Sullivan ore had to be separated into three sulfide concentrate products-lead concentrate, zinc concentrate and iron concentrate. The choice and arrangement of equipment, and the original flow sheet for the Sullivan concentrator were controlled by the results of the exhaustive pilot mill test. These covered a continuous period of 3 1/2 years and involved the treatment of 1,076,368 tons of Sullivan ore. Satisfactory recoveries are made from feed; 11.0 per cent lead and 7.5 per cent zinc in the form of lead concentrate containing 69 per cent lead, 4.5 per cent zinc, and zinc concentrate containing 3.0 per cent lead and 49 per cent zinc. (The pure zinc mineral in Sulli-van ore is marmatite, 'containing approximately 54.5 per cent zinc and 10 per cent iron. It is apparent, there-fore, that 49 percent concentrate is high grade for this particular ore.)

Jan 8, 1927

By James P. Kimball

Jan 1, 1885

By AIME AIME

On Nov. 11, 1909, M. Alexandre Pourcel, of Paris, France, upon the proposal of a large number of distinguished members, and the unanimous recommendation of the Council, was elected by the Board of Directors an Honorary Member of the Institute. M. Pourcel has devoted forty-three years to the metallurgy of iron and steel ; and the work which he did between thirty and forty years ago constitutes an important part of the founda¬tion of the practice of to-day. Among his striking contribu¬tions are : (1) his perfection, in 1869, of the manufacture of high-grade ferro-manganese in a carbon-lined open-hearth furnace, instead of the costly crucibles previously used; (2) his discovery, in 1874, of the method of making solid steel cast¬ings; (3) his manufacture, in 1875, of ferro-manganese and silico-spiegel in the blast-furnace; and (4) his anticipation, in 1875, of modern American blast-furnace practice, by the pro¬duction, in a very small furnace, of Bessemer pig containing 2.5 per cent. of silicon, from a burden yielding only 46 per cent. of iron, and with a consumption, per ton of pig, of only 1,8401b. of coke, containing 15 per cent. of ash. These brilliant pioneer achievements, together with his contributions to cur¬rent technical literature, won for him the Bessemer gold medal of the Iron and Steel Institute ; the great" medal of honor," which is the highest award of the French Society of Mineral Industry, and other gold medals, as well as the distinction of honorary membership of the Comité des Forges de France, which was conferred upon him in 1891. In recent years, M. Pourcel has been instrumental, as consulting engineer of the Société de Commentry-Fourchambault, at Decazeville, France, in an extraordinary development of the manufacture of special steels. The Invar plant, of this company, is said to make a greater variety of such steels (includ-

Dec 1, 1909

By L. O. Howard

THERE are three active mines in the Chewelah-Colville district, the United Silver Copper near Chewelah, and the Old Dominion and the Chloride Queen near Colville. The Admiral near Valley is also doing development work. The Chewelah district is in the south central part of Stevens County in the Colville Valley. Chewelah, a thriving town of 1600 people, and the scene of operations of the Northwest Magnesite Co., is about the center of the district. It is situated in a farming community on the Spokane-Nelson branch of the Great Northern railway, about 65 miles north of Spokane. Only two or three of the mines in the district have been extensively developed, although many have been prospected. The general elevation of the valley, is about 1600 or 1700 ft., that of the mountain ranges on each side about 3000 to 4000 ft., with gentle slopes and rounded glaciated tops. Prospecting is often difficult because of much glacial debris.

Jan 1, 1925

By W. C. Hayes

The site selected for the United States prototype pumped storage project of Union Electric CO. was Proffit Mountain, five miles from Taum Sauk, the highest point in Missouri. Factors influencing final location were: high local relief; satisfactory rock type and structure; and an economic location in respect to existing transmission systems. The upper reservoir was constructed by excavating rhyolite porphyry from the crest of Proffit Mountain and constructing a rock fill dike encircling the area to form a 4350-acre foot reservoir. A 6564-ft tunnel connects the upper reservoir with the generating and pumping facilities. A concrete gravity dam on the East Fork of the Black River forms the 6350-acre foot lower reservoir. Precambrian rhyolite porphyry forms the crest of Proffit Mountain and the floor of the upper reservoir. The tunnel was excavated in rhyolite prophpy, granite porphyry, dolomite, shales and conglomerate. Abutments and the foundation of the gravity dam are in rhyolite porphyry, and much of the valley floor of the lower reservoir is underlain by dolomite and shale. Core drilling provided data on soundness of rock type, structure, depth of weathered zone and potential water loss in the fractured igneous rocks. After a six-year study of pumped storage and cost comparison with alternate stream generating units, the Taum Sauk pumped storage project was authorized by Union Electric Co. on Dec. 11, 1959.' The site selected is located in the St. Francois Mountains of southeast Missouri approximately 90 miles south of St. Louis (Fig. 1). The lower reservoir was provided by damming the East Fork of the Black River, a small tributary of the Black River with a minimum flow of about 1 sec ft. Construction of the upper reservoir was effected by quarrying the crest of Proffit Mountain - five miles from Taum Sauk Mountain, the highest point in Missouri — to provide material for a rock fill dike surrounding the quarried area. This provided a 55-acre mountain top lake with a water depth of 92 ft (Fig. 2). A vertical shaft and tunnel connect the upper and lower reservoirs through the two reversible pump-turbine motor-generator units operating under 800 ft of hydraulic head (Fig. 3). The output rating of the plant is 350,000 kw with daytime generation of about 2.2 million kw-hr under normal use. Night pumping will replenish water to the upper reservoir in about 91/2 hours3. The automatic operation is remotely controlled from the Osage plant and from the dispatchers office in St. Louis. GENERAL GEOLOGY Mountains of the St. Francois area consist of Precambrian granites, granite porphyries, extrusive fel-sites and basic dikes. Basal conglomerates overlain by Upper Cambrian Bonneterre dolomites and shales onlap the exhumed Precambrian knobs and hills and are exposed in the narrow valleys. Cambrian and Ordovician residuum as much as 200 ft thick is present on the slopes of many hills. Proffit Mountain consists of rhyolite porphyry and granite porphyry. All excavation for the upper reservoir was in rhyolite porphyry, and the same rock is present under the Bonneterre at the plant site and under alluvium at the lower reservoir dam site. The region has been dissected to the stage of early maturity with only small upland flats remaining. Considerable local relief (a requisite for the project) approaches 1000 ft. Streams flowing across the Precambrian ridges have formed restricted narrows, termed shut-ins. A shut-in approximately two miles downstream from the plant site provides an excellent site for the lower reservoir dam. TEST BORINGS Preliminary to final approval of the project, 12 test borings were made to determine subsurface geologic conditions (Fig. 2). Drill hole No. 12 at the lower reservoir dam site showed 20 ft of alluvium over solid rhyolite porphyry. Drill holes No. 1, 2 and 3 were drilled in the tail race area to depths of 66 ft, 75 ft and 95 ft respectively, and all bottomed in Bonneterre. Drill hole No. 4 at the plant site provided NX core to a total depth of 98 ft in Bonneterre. Drill

Jan 1, 1965

By Francis Lucas

EACH year we gather in this auditorium to honor the memory of a . distinguished American metallurgist and educator. I cannot bring to you reminiscences of Prof. Henry Marion Howe as other lecturers have done. It was not my good fortune to enjoy the privilege of studying and ,working under his direction. As I have reflected on the published works of Professor Howe, it has seemed to me that his mind was trained on the nature of metals and on the mechanism which produced known but unexplained effects. He was interested in controlling and regulating the causes so as to produce specific effects, useful in serving mankind. I recall an afternoon in May, 1925, when, at the invitation of Mrs. Howe, I visited his former home, Green Peace at Bedford Hills, N. Y. The purpose of my visit was to receive at the hands of the widow -an engraving of Professor Howe, a reproduction of a painting from life. Mrs. Howe showed me his study. The walls of this large attractive room, brilliantly illuminated by the spring sunshine, were literally covered with the scrolls of honors and of decorations which had been conferred on Professor Howe by governments, academies, universities, societies and. institutions the world over. As we walked about the room, she pointed out the significance of each honor and recited a few details of each occasion. I sensed the pride with which Mrs. Howe, then in the late autumn of her life, told me of her husbands' achievements, of his struggles, of his disappointments and of his successes. There was a surprisingly familiar note in the recital to which I was listening. I have found the same theme running as a disconnected thread through the written accounts of the lives of most men of science. We then went to the drawing room to chat for a few minutes before I said my farewells. As we seated ourselves, Mrs. Howe turned to me and asked: "Mr. Lucas, what of this great microscope of yours? Cannot it be applied to the study of disease? What a great blessing it would be if it could be directed to relieve the suffering of mankind."

Jan 1, 1931

By C. E. McWhorter

IN underground mining recent trends toward mining large tonnages of low-grade ore have created, among other things, a need for cheaper and more flexible ore transport. A relatively new development has been the adaptation of shaker conveyors to meet this need. Although widely used in coal mining, only in the last few years have shaker conveyors been used in underground metal mining. The equipment consists of a driving engine, either electric or air powered, upon which is mounted a drive trough supported in ball-bearing frames. The trough line, or conveying medium, is made up of a number of sections, each section connected to another, usually with bolts. The length of each trough section is controlled by the length that can best be handled underground, but is usually from 9 to 13 ft over-all. The length of a complete conveyor line is determined by the character and weight of material to be handled as well as by the size of the ore body. Trough lines vary in lengths from 100 to 300 ft and the trough has a cross-section area of 127 sq in., and is 22 in. wide by 6 ½ in. deep.

Jan 1, 1948

By O. P. Dolph

SPANIARDS were probably the first to mine the rich surface ore in the veins cutting the rhyolite capping that outcrops on the hills of La Mazata, oil the Allyones side of the Magdalena valley in Jalisco, Mexico, although the name comes from a word of Indian origin meaning "deer". The camp is about 12 km. west of Magdalena, a town on the Southern Pacific Railroad, and about 17 km. north of Etzatlán, on the Mexican National Railroad, at an elevation of 4500 ft. The climate is subtropical with no extremes of heat or cold, the rainy season beginning in June and ending in October.

Jan 1, 1938

By George C. Bravner

WITH the great expansion currently being made in the aluminum output of the United States, not only by the company that has heretofore been the sole producer but by a now organization in the field it is only natural to wonder to what degree the; ore reserves of the United States can contribute to the growing consumption. For the three-year period 1937-'39 the U.S. Bureau of Mine's figures indicate that the annual domestic production of bauxite averaged about 370,000 long tons, compared with average, annual import of about 194,000 long tons. About 85 per cent of the imports came from Surinam, nearly all of which went into aluminum manufacture. Not all of the or -kipped from mines in the United States is used to make alumimun however as Bureau figures indicate that in these three years an average of only 48 per cent of the domestic ore shipment were so used the abrasive chemical and other industries taking respectively 27, 21, and 4 per cent of the output. The recent increase in the demand for bauxite has been of course in it use for aluminum manufacture. This as is well known is largely attributable to the world race for supremacy in

Jan 1, 1941

By W. E. D. Stokes

The faster that aircraft fly the sooner some new and stronger material must be found to take the place of the present aluminum alloy used in all-metal planes. Experts of the National Advisory Committee for Aeronautics. in studying hi-speed aircraft, are convinced that the present all-metal plane, of semi-monocoque, aluminum alloy construction, is not the ultimate in aircraft design. Magnesium alloys and steel are under consideration.

Jan 1, 1942

By Voyle R. McFarland, Robert A. Burmeister, David A. Stevenson

The distribution of lead between phases in the Ag-Sb-Te system was studied using microautoradio -graphy. Two compositions were investigated, both containing an intermediate phase Known as silver antimony telluride as the major phase, and one containing AgzTe and the other SbzTes as the minor phase. For both compositions, two thermal treatments were used: nonequilibrium solidification from the melt and long equilibration anneals of the as-solidified structure. For each composition, lead was segregated in the minor phase of the as-solidified structure, but was distributed in the matrix after anneal. The electrical resistivity and carrier type were insensitive to the distribution of lead in the two-phase structure. ThERE has been considerable interest in the Ag-Sb-Te system because of its thermoelectric properties. The major interest has been in compositions on the vertical section between AgzTe and SbzTes, particularly the 50 mole pct SbzTes composition AgSbTez (compositions are conveniently expressed as mole percent SbzTes along the AgzTe-SbzTes section). One of the major problems in the proper evaluation and utilization of this material is the inability to control the electrical properties through impurity additions: all alloys prepared to date have been p-type, even with the addition of large amounts of impurities. It has been shown Wit all the compositions previously studied contain an intermediate phase of the NaCl st'ructure as a major phase (denoted by b) and a second phase, either AgzTe or SbzTe3, as a minor phase.'-3 One explanation for the unusual electrical behavior of this material is that the impurity additions have a higher solubility in the second phase than in the matrix; the impurity would segregate to the second phase, leaving the bulk matrix essentially free of impurity.4 In order to investigate this mechanism with a specific impurity element, the distribution of lead between the two phases was determined using autoradiography. Lead 210 was chosen because of the suitability of its 0.029 mev 0 particle for autoradiography and also because of the interest in lead as an impurity in this system.5'6 EXPERIMENTAL PROCEDURE Two compositions were taken from the vertical section between AgzTe and SbzTes, 50 mole pet SbzTes (Viz. AgSbTez) and 75 mole pct SbzTes, in which AgzTe and SbzTes appear, respectively, as the minor phase. Lead containing radioactive lead (pb210) was added to the above compositions to provide a concentration of 0.1 wt pct Pb. The material was placed in a graphite crucible in a quartz tube which was then evacuated and sealed. The samples were melted and solidified by cooling at a rate of 8°C per min and then removed and prepared for microa~toradiography. After autoradiographic examination of these samples, they were again encapsulated and annealed in an isothermal bath at 300°C for a number of days and prepared for examination. An alternate method of preparation employed a zone-melting furnace; the molten zone traversed the sample at a rate of 1.2 cm per hr and the solid was maintained at a temperature of 500°C both before and after solidification. This treatment had the same effect as solidification at a slow rate followed by an anneal for several hours at 500°C. In order to obtain the best resolution, thin sections of the alloy were prepared by hand lapping to a thickness of approximately 20 p. Other samples were prepared for examination by lapping a flat surface on the bulk sample. The resolution, although somewhat better in the former procedure, was adequate in both instances and the majority of the samples were treated in the latter fashion. A piece of autoradiographic film (Kodak Experimental SP 764 Autoradiographic Permeable Base Safety Stripping Film) was stripped from its backing, care being taken to avoid fogging due to static-electrical discharge. A small amount of water was placed on the sample, the film applied emulsion side down on the surface of the sample, and the sample and the film dipped into water in order to assure smooth contact. After drying, the film was exposed for 2 to 5 days, the period of time selected to give the best resolution. The film was developed on the specimen and fixed and washed in place. Two major factors must be considered in establishing the reliability of an autoradiograph: the in-

Jan 1, 1964

By J. T. Norton, Joseph Gurland

IN spite of the extended use and high state of practical development of the cemented tungsten carbides, the structure of these alloys is still a matter of considerable controversy. The characteristic high rigidity and rupture strength of sintered compacts have been attributed to a continuous skeleton of tungsten carbide grains, formed during the sintering process. This view is based mainly on the work of Dawihl and Hinnuber,1 who reported that a sintered compact of 6 pct Co maintained its shape and some of its strength after the binder was leached out with boiling hydrochloric acid. After leaching, only 0.04 pct Co was reported to remain in the compact. They also showed that the assumed increasing discontinuity of such a skeleton, as the cobalt content is increased, could be made to account for the observed discontinuous increase of the coefficients of thermal expansion, the loss of rigidity, and the impaired cutting performance of alloys of more than 10 pct Co. Contradictory evidence was cited by Sanford and Trent,' who mentioned that a sintered compact was destroyed by reacting the binder with zinc and leaching out the resulting Zn-Co alloy. The skeleton theory also does not account for the observed change of strength of sintered compacts as a function of cobalt content. If the skeleton is responsible for the strength, the latter would be expected to decrease with increasing binder content. Actually, the strength increases and reaches a maximum around 20 pct Co. In addition, tungsten carbide is brittle and undoubtedly very notch sensitive. The highest value found in the literature for the transverse rupture strength of pure tungsten carbide prepared by sintering is 80,000 psi.3 herefore, such a skeleton does not easily account for a rupture-strength value of 300,000 psi and higher, commonly found in sint.ered tungsten carbide-cobalt compacts. In view of the conflicting data present in the literature, experiments were undertaken to determine whether the sintering of tungsten carbide-cobalt alloys leads to the formation of a carbide skeleton or whether the densification behavior and the properties of cemented compacts are consistent with a structure of isolated carbide grains in a matrix of binder metal. The specimens were prepared from powders of commercial grade. Tungsten carbide powder ranged in particle size from 0 to 5x10-4 cm. Mixtures of tungsten carbide and cobalt were ball milled in hexane for 48 hr in tungsten carbide lined mills. After milling, the specimens were pressed in a rectangular die (1x1/4x1/4 in.) at 16 tons per sq in. NO pressing lubricant was used. Sintering of the tungsten carbide-cobalt compacts was carried out in a vertical tube furnace equipped with a dilatometer (Fig. I), by means of which the change of length of the powder compacts could be followed from room temperature to 1500°C. An atmosphere of 20 pct H, 80 pct N was maintained inside the furnace. Decarburization of the samples was prevented by the presence of small rings of graphite inside the furnace tube. The temperature of the sample was measured by a platinum-platinum-rhodium thermocouple, which also was part of a temperature control system able to maintain a constant temperature within ±100C. Pure tungsten carbide compacts were prepared by sintering the carbide without binder or by evaporating the binder from sintered compacts in vacuum at 2000°C. Since complete densification of these samples was not desired, they were sintered only to 60 or 80 pct of the theoretical density of tungsten carbide. The specimens were prepared for metallographic examination by polishing with diamond powders and etching with a 10 pct solution of alkaline potassium ferricyanide. Cobalt etches light yellow and the carbide gray. The amount of porosity is exaggerated since it is difficult to avoid tearing out carbide particles, especially from incompletely sintered samples. Experimental Observations A number of specific experiments were carried out in order to study some particular aspect of the sintering problem. The details of these experiments, together with their results, are as follows: Electrolytic Leaching: The binder was removed by electrolytic leaching from sintered tungsten carbide-cobalt compacts for the purpose of determining the continuity of the carbide phase. The method used was based on the work of Cohen and coworkers4 on the electrolytic extraction of carbides from annealed steels. If the sample is made the anode, using a 10 pct hydrochloric acid solution as the electrolyte, the binder is dissolved, but the rate of solution of tungsten carbide is negligible. A current density of 0.2 amp per sq in. was applied. As shown in Fig.

Jan 1, 1953