Search Documents

By E. P. Klier, Jane Jellison

The course of the transformations on cooling in a series of Cu-A1 alloys has been followed by means of thermal analysis, X-ray diffraction, and optical metallogrAphy. Specimen size was found to have a pronounced effect on the time of completion of the pearlite transformation due to modification in the unmber of nuclei. The ordeving transformation zvas observed for all cooling rates for all alloys studied, and is considered insuppvessible. At intermediate cooling' rates, a transitional struchire for 011 alloy compositions and based ox the bainite reaction was observed. The alloys of aluminum and copper possess a eu-tectoidal region at from about 9.4 to 16 pct Al. Above the critical temperature, the disordered bcc phase, 0, is stable. At subcritical temperatures, the 0 phase decomposes under equilibrium conditions into the stable phases, a and y,. At the eutectoid composition, these phases develop a lamellar pearlite structure, in appearance much like that found in steels. During rapid quenching from supercritical temperatures, the diffusion processes required for the formation of the equilibrium phases are suppressed, and the 0 transforms to an acicular martensitic phase, designated B or y' depending on the aluminum content, or to a mixture of the two. Early investigators of this system concentrated on determining the equilibrium phase diagram, ''' the structure of the equilibrium phases,3 and later the isothermal decomposition of the 0 phase at subcritical temperatures, or the decomposition of the martensite on tempering. Other work which treated the nonequilibrium transformations concentrated largely on the martensite transformations and the structure of the b and y' phases.15"17 Since the pearlite and martensite transformations in this system resemble those in steels, the one being formed by nucleation and growth of adjacent lamellae of the equilibrium phases, and the other by a diffusionless, shear-type transformation, the present study has been undertaken to investigate the structures formed on continuous cooling, with the objective of constructing cooling transformation diagrams analogous to those derived for alloy steel systems. In particular it was desired to determine whether parallels between the A1-Cu and iron-iron carbide systems on continuous cooling extended to encompass the intermediate phase, namely the bainite structures, which form by a combined martensitic-diffusion mechanism,'' but which are supersaturated with respect to the equilibrium phase upon which their crystal structure is based. To this end the transformations in representative alloys of the Cu-A1 B eutectoid system have been followed, using the methods of thermal analysis, X-ray diffraction, and optical microscopy. EXPERIMENTAL PROCEDURE Materials. The materials tested were those used by Klier and Grmko 5 in their study of the isothermal decomposition of these alloys. The alloys were melted in graphite crucibles and chill-cast into 5 by 2 by 1/4 in. ingots. The ingots were then hot-rolled to sheets 1/8, 1/16, and 1/32 in. thick. The compositions are given in Table I. Specimen Preparation. Specimens for thermal analysis were in the form of small squares approximately 1/4 in. on a side. For the 11.9 and 13.5 Al-Cu alloys, the sheet thickness was 1/16 in. and for the 10.5 A1-Cu alloy the 1/32-in. sheet was used. One lead of a chromel-alumel thermocouple was spot-welded to either face of the square with the specimen itself thus forming the hot junction of the thermocouple. Specimens for X-ray analysis were prepared as filings from martensitic sheet stock and were sealed in glass ampoules under 1/2 atm of argon. Metallographic examination of the powder specimens was carried out on a portion of the heat-treated filings mounted in lucite. All specimens were examined metallographic ally after etching

Jan 1, 1965

Jan 1, 1902

By J. B. Fisken

(Butte Meeting, August, 1913.) BEFORE touching upon the immediate subject of this paper a few facts of a historical nature as to the general application of electricity to mining might be of interest. As to what was actually the first application of electricity to mining, opinions will no doubt always differ. My experience does not go back far enough, nor are the records to which I have had access of any value as covering this point. Sydney F. Walker, a man whose pioneer experience in the application of electricity to mining purposes dates back as far as 1876, ,gave an interesting resume of the subject in an address before the South Wales branch of the Association of Mining Electrical Engineers at its 1.913 session, and, unless his statements are shown to be wrong, they should be accepted as facts. According to Mr. Walker, the ignition of charges of blasting powder was the first operation in mining to be accomplished with the aid of electricity. Very frequently this energy was furnished by a static machine and occasionally by a magneto generator. Later, this was followed by the application of electricity to bell signals, and we are told that this application was looked upon skeptically and regarded as an expensive experiment by the mining managers of those early days. At the Paris Exposition of 1878, there was exhibited an electric lamp, which suggested future possibilities to the mining engineers of those days. The first successful application of electric lighting to underground excavations that I have been able to find any record of is that of M. Blavier. In the year 1879' he installed two Serrin lamps and successfully illuminated one of the large underground chambers in the Angers slate quarries. Another early application of electricity to the lighting of mines is that in the large chambers in the salt mines of Maros-Ujvár, in Hungary; these have been regularly and successfully lighted elec-

Jan 6, 1913

By F. M. Smith, R. H. Moore, J. R. Morrey

Electrodiffusion in y cerium reported by Henrie has been confirmed and a Preliminary estimate made of the relative rates of electrodiffusion of iron, cobalt, and nickel. These diffuse to the anode at rates decreasing in that order. In addition, copper and manganese exhibit slow, but detectable, diffusion to the anode and molybdenum exhibits detectable diffusion to the cathode. The electrodiffusion of carbon, .zirconium, antimony, magnesium , and silicon in y cerium could not be detected. Iron and cobalt diffuse in y cerium at rates proportional to the current density and with no apparent dependence on temperature. Decreasing polarization of iron and cobalt with increasing temperature, which cancels the expected rate increase, would account for this behavior. The electrodiffusion rate of iron in y uranium and in E plutonium has been measured. Diffusion of iron is anode-directed. Tin was found to diffuse to the cathode, in y uranium, at an appreciable rate. In all of these solvent metals, negative ions diffuse to the anode and positive ions to the cathode. The potential field effect appears to account satisfactorily for these results. FROM early experimental work summarized by Jost1 and Seith,2 the driving force for electrodiffusion was attributed to the potential field acting on ions in a metal. More recently, Heuman,3 Wever,4 and Huntington5 have shown that momentum interchange between conduction electrons and mobile entities in the metal contributes to electrodiffusion. Electron momentum interchange is anodically directed and the direction of diffusion resulting from the field force is dependent upon the charge on the diffusing entity. These two effects may either reinforce or oppose each other. Glinchuk6 has pointed out that momentum transfer in defect conductors should be cathode-directed and this appears to be the case as demonstrated by wever's4 work on iron. Barnett's7 work, on the other hand, indicates that, even in defect conductors, electrons show a negative E/m ratio when accelerated with respect to the lattice and should lead to anode-directed momentum transfer. In discussing this problem, Wever and seith8 suggest that defect electrons interact preferentially with activated ions so as to allow a net movement toward the cathode while still maintaining an electron momentum transfer in the anode direction. Williams and Huffine9 and Henriel0 have demonstrated that electrodiffusion may be useful for purification of yttrium and cerium. In yttrium, Williams and Huffine note that movement of several metallic impurities toward the anode is in keeping with observations in most other metallic systems and indicates that yttrium remains a normal electronic conductor at least to 1230°C. Close inspection of their data shows, however, that oxygen, nitrogen, and the transition elements diffused toward the anode, while nontransition elements diffused toward the cathode. This suggests that potential field effects may have been appreciable. The present work was concerned with the applicability of electrodiffusion as a technique for purification of plutonium, but, because of the obvious hazard inherent in work with this metal, experiments to develop the technique were carried out using cerium and uranium. The results of electrodiffusion measurements on these metals and on plutonium are reported here. EXPERIMENTAL The metal specimens prepared for this work were 6 in. long, 1/4 to 1/2 in. wide, and 1/16 to 3/32 in. thick. The uranium specimens were machined from a bar which analyzed 310 ppm Fe and the electrodiffusion of iron was followed by spectrographic and by chemical analysis. Cerium and plutonium specimens were cut from sheet rolled from ingots obtained from molten salt-metal equilibrations during which radioactive tracers were introduced. The electrodiffusion of the tracers was subsequently determined by counting methods. The specimens were electrolyzed between nickel electrodes containing resistance heaters used to equalize the specimen and electrode temperatures, thereby reducing thermal gradients. The temperature of the electrodes adjacent to the ends of the specimen was measured with chromel-alumel thermocouples which were connected to the heater controls. The surface temperature of the specimen at a point midway between the electrodes was measured with a sapphire rod pyrometer, the output of which controlled the dc power supply. This assembly was enclosed within an evacuable chamber containing a quartz viewing window. The temperature of the specimen over its entire length could be scanned with a portable pyrometer through

Jan 1, 1965

By AIME AIME

ABOUT 55 attended the general session of the Nonferrous Metallurgy Committee on Wednesday afternoon. In opening the proceedings the Chairman, Frank G. Breyer, served notice of his intention to make an early start this year in securing papers for his committee. He voiced the thought that more importance should be attached to the prompt publication of data on new advances in practice; the record of technical progress should be written before the sharpness of the current image becomes blurred by the veil of time. As an illustration, Mr. Breyer declared that great strides have been made in the zinc industry during the past nine years, whereby zinc ore is converted directly to the oxide in large mechanical furnaces, yet the literature is confined to patents.

Jan 1, 1933

By Clarence G. Merritt

Stainless iron, as mild stainless steel is usually called, an alloy ranging from 11.50 to 15.00 per cent chromium with carbon under 0.12 per cent, has been considered to be not appreciably affected in respect to corrosion resistance by heat treatment. This metal, while one of the most widely used of the "straight" chromium stainless alloys, has failed in many applications because of insufficient information regarding heat treatment. These failures have been attributed to many possible causes from an inherent lack of resistance to corrosion and misapplication to mlysterious electrolytic effects or comparatively minute non metallic inclusions. Many uses for a steel with such excellent physical properties as are latent in this alloy have been lost on account of corrosion failures which could have been avoided by applying proper heat treatment. The alloy has not received the recognition or attention it should because of the fact that the details of its metallurgical behavior were not thoroughly understood. Response to heat treatment of the steel is well known as regards tensile properties,1-2 but its application has been for improvement in tensile characteristics or on account of machining considerations rather than for corrosion prevention. The potential user of this steel has not been clearly advised in papers, either technical or commercial, that have been written about it in the last 10 years or more, of particular features that are of prime importance in developing the excellent properties of this metal. The data to be presented in this paper are concerned mainly with the effect of heat treatment on the corrosion resistance, but a study has also been made of the concurrent microstructural changes and an explanation developed for the phenomena revealed, as well as a correlation to the other physical properties—hardness, tensile characteristics and impact strength. Stainless steel, largely used for cutlery purposes, an alloy of approximately 13.00 per cent Cr with 0.30 per cent C;, must be hardened and the surface prepared by polishing or pickling for best resistance to staining and corrosion. Monypenny reports that a loss of hardness is

Jan 1, 1932

By Hugh O?Neill

IN PREVIOUS papers,1 the author has reported the results of experiments on the straining in tension of a single crystal test piece, about 0.6 in. long, of vacuum-melted electrolytic iron containing 1.8 per cent. of silicon. The crystal was originally in the "as cast" condition, and was stressed slowly along a tetragonal axis so that slipping along conjugate gliding planes finally transformed the original cylindrical portion into a pair of fracture wedges. One of these fracture wedges was sectioned along the stress axis in a plane at right angles to the edge of the wedge. A metallographic study of this plane of -section led to the conclusion that slip had taken place in the (111) direction along (112) planes making a V shape with the stress axis. The present paper describes the results of scratch-hardness tests conducted on the same section, in order to determine the distribution of strain hardness therein, followed by annealing, and considers the resulting variations in hardness. These observations supplement those made by Krivobok2 on similar material reduced 25 per cent. by hammering (i. e., by impact) in the cold. In order to investigate ageing effects, two small crystals of the same alloy were also tested.

Jan 1, 1928

By C. M. Loeb, T. E. Norman

The use of ball, rod and tube mills for grinding ore, cement and other materials has grown so rapidly during the past forty years that the world's annual consumption of ferrous grinding media for these mills is now estimated to be between one half million and one million tons per year. Ferrous grinding balls constitute the major portion of this tonnage. Obviously they represent sufficient value to justify thorough studies of the factors governing their performance. The selection of grinding balls is governed principally by: I. Quality (wear resistance, impact resistance, soundness, and the like). 2. Sources of supply and delivered cost. 3. Grinding characteristics or efficiency in the ball mill. This paper deals principally with the quality of ferrous grinding balls. In the study of these factors certain data relative to the fundamental nature of ball wear in ball mills have been obtained. These data are also presented and discussed briefly. The Development of a Suitable Wear Test A study of the fundamental factors governing the quality of grinding balls has been hampered seriously by the fact that a competent test has, in the past, involved the purchase of several hundred tons of balls of a specific type which were then run in one or more ball mills for a period ranging from several months' to several years' duration. Often, during the period of test, it became necessary to change operating conditions or the character of the ore fed to the test mill with the result that the rate of ball consumption changed and the test figures became of little value. Under such circumstances, progress in the development of better grinding balls, has been necessarily slow. Economic factors and variations in the quality of balls produced by different sources of supply generally make it necessary for each mill operator to determine for himself the most suitable type of balls for his mills. In our own ball mill grinding operations at Climax, Colo., we were faced with this problem. After we had run a few large scale wear tests at considerable expense we decided to investigate the possibilities of a small scale wear test which would be capable of testing numerous types of balls within a relatively short time. The most important requirement of any test is, of course, that it give results which can be used to predict accurately the wear in full scale operations. It was known that Ellis and his associates1,2 had developed a method of testing grinding balls by small scale tests run at the Ontario Research Foundation. Ellis' method of testing was used as a starting point in our investigations. In the course of our tests a number of modifications of the original method were found to be desirable so that, by an evolutionary procedure, a method of small scale

Jan 1, 1949

By R. C. Schmidt, B. E. Kennedy

The Mont Klahoyo magnetite deposit is located about 600 km (373 miles) northwest of Abidjan, Ivory Coast. During an exploration period ending in 1977 an international joint venture group investigated the deposit and proved reserves of 670 Mt (739 million short tons) grading 36% iron. The deposit occurs at the northeast end of the Baoubly-Kiriao chain of Precambrian iron formations with associated amphibolites, pyroxenites, and gneisses of the Liberian Shield. The ore body is represented by a highly metamorphosed banded quartz-magnetite iron formation with alternating beds of iron silicates and quartz-magnetite. Amphibolite-pyroxenites and sillimanite-cordierite-garnet gneisses form hanging and footwall rocks. The iron formation has been folded into an elongated, overturned 2-shaped major drag fold with axes trending and plunging approximately northeast. Beds are vertical or dip steeply to the southeast. The ore zone has an average thickness of 130 m (427 ft) and outcrops intermittently over a distance of approximately 5.5 km (3.4 miles). Based upon detailed studies of drill cores and the results of ore dressing test work, eight stratigraphic units, identified as K- 1 to K-8, are recognizable in the iron formation. Four interbedded units are low grade silicate zones (silicate facies) while the remaining quartz-magnetite units are oxide facies, representing the important Mont Klahoyo deposit ores. Ore-bearing "K" units are subdivided further into 11 ore types, based upon their specific lithologies, iron content, and concentration characteristics. Identification of these ore types proved particularly useful to mine planning and flowsheet design. A cap of oxidized material overlies the primary quartz- magnetite iron formation, but no enrichment has occurred. It is thought that the Mont Klahoyo iron formations were deposited chemically in a volcanic environment as a siliceous iron formation with volcanism the primary source of iron and silica. Metamorphism converted the siliceous iron formation to a coarse-grained, quartz-magnetite-silicate iron formation.

Jan 1, 1983

By Richard W. Smith

KYANITE, long known to occur in Georgia, did not excite commercial interest until about 1930. Investigations revealed two main types of deposits: (1) separate kyanite crystals embedded in mica schist; and (2) crystal aggregates of kyanite associated with quartz in small and very irregular veins. The second kind at first sight appeared to be the best source of supply. Large boulders or dornicks of kyanite with more or less quartz were found on the surface at many places throughout the Piedmont and Highland sections of the state, but prospecting failed to disclose a sizable vein. These dornicks seem to be a surface accumula-tion from small veins or lens-shaped masses not more than one or two feet thick, and with a horizontal extent of not' more than a few feet. The larger surface accumulation of kyanite dornicks, where not too badly stained by iron oxide, may prove to be marketable, but it is extremely doubtful whether a vein large enough to mine will ever be found. In 1932 deposits of the kyanite-mica schist were known to occur in two places northwest of Clarkesville, in Habersham County. In 1934, at the request of and in cooperation with the Georgia Geological Survey, the United States Geological Survey made a thorough investigation2 of the deposits and found that the two known areas of kyanite-mica schist in Habersham County were but a part of an unsymmetrical, U-shaped belt (Fig. 1) with a western limb extending into Rabun County and somewhat longer than the eastern limb. The total length of the belt is about 30 miles. The width of outcrop ranges from 100 ft. to 1/4 mile or more. Deposits of kyanite-mica schist of very doubtful commercial importance were found in several other counties. Only the deposits of this kyanite-mica schist belt in Habersham and Rabun counties will be discussed in this paper.

Jan 1, 1936

By A. T. Tye

REGARDING the results of preferential flotation at Cananea, Weinig has stated that "The concentrating mill of the Cananea Consolidated Copper Company at Cananea, Mexico, furnishes an excellent example of modern flotation practice. The complete figures are given because they present so forcibly the advantages of modern selective flotation."' L. 0. Howard notes that "Perhaps the outstanding example so far published of improvements in results through the use of selective flotation is that at Cananea, Mexico."2 The following notes indicate the conditions under which the results were obtained at Cananea; also the effect of preferential flotation at the concentrator and at the smelter. In the majority of cases the full benefit of selective flotation is not fully realized, as the concentrates are shipped from the mill to smelters owned by other companies. The saving made at a certain concentrator by this method of flotation may be well understood but the saving resulting at the smelter from the results of preferential flotation at the mill is not so apparent, as the data are contained in the smelting records of some other company. Even at the smelter the great gains following preferential flotation may not be noted, as a variety of ores and concentrates from various sources are received and the difference from the changed concentrator operations of a certain mill may be obscured. As noted by Professor Weinig and Professor Howard, the results obtained at Cananea brought about a veritable metallurgical revolution at the smelter.

Jan 1, 1927

Jan 1, 1931

By Leonard Grimshaw

DIFFUSION Of carbon from gases into iron has been the object of much research, because of its long recognized importance in carburizing processes, but the direct diffusion of carbon from steel into iron has received relatively little attention. Because of the increasing use of clad metals in industry, direct diffusion from steel into iron is becoming of practical importance. Therefore, the object of this investigation was to study the diffusion of carbon from several different kinds of steel directly into relatively pure iron, realizing that elements in the steels other than carbon might influence the rate of carbon diffusion. The previous work on diffusion of carbon into iron has been consider-able, and includes many reports in foreign languages. This work has recently been well reviewed by Mehl1 and Krynitsky,2 and the reader is referred to their excellent bibliographies.

Jan 1, 1937

Jan 1, 1924

Arizona ROBERT E TALLY, Chairman CARL F MILLS, Secretary-treasurer, P O Box 1462, Jerome, Ariz W. S. BOYD THOMAS H O. O'BRIEN F. W MACLENNAN Boston Meets first Monday each winter month GALEN H. CLEVENCER, Chairman HOLCOMB J BROWN, Vice-chairman F LEROY FOSTER, Secretary-treasurer, Room 8-219, Mass. Inst of Tech, Cambridge, Mass A. E WELLS H A WENTWORTH

Jan 1, 1923

By Richard Hunt

BINGHAM has produced 6 per cent. of this country's copper. In total production, it ranks fourth among the copper camps of North America, the order being Butte, Michigan, Bisbee, and Bingham. In its annual production, it held that same rank until 1919, when its production was exceeded by the combined production of the Globe-Miami district of Arizona. Bingham has also been a lead camp of the first order. Utah ranks third among the lead-producing states, and its production comes largely from three camps which, in the order of their productivity, are: Bingham, Tintic, Park City. Bingham's silver production is important, but it does not rank high as a silver producer. Utah owes its rank as first among the silver-producing states to Tintic, a camp 40 miles due south of Bingham. The United States Mineral Resources reports a total production from Bingham for the period 1865-1920 having a gross value of $528,043,432. Bingham is on the eastern flank of the Oquirrh range 30 miles south-west of Salt Lake City, from which it can be reached in an hour by auto, or by the Denver & Rio Grande or the Bingham & Garfield railroads.. The automobile route is a paved road across the floor of Great Salt Lake Valley, through farming country. The Bingham & Garfield railway leaves the level of Great Salt Lake at the northern end of the Oquirrh range, and in 20 miles it climbs 2100 ft., and deposits the traveler upon a shelf cut in the side of Bingham Canyon below most of the mines, which are farther up Bingham Canyon and its tributary Carr Fork. Below lies the town, a narrow ribbon running for a couple of miles along the bottom of a canyon 2000 ft. deep-an almost impossible site for a community numbering, in prosperous times, 5000 to 7000 inhabitants drawn from all quarters of the globe. Up the canyon and down, and beneath the steep slopes nearby, and beneath the town itself, are the mining operations of over half a century.

Jan 3, 1924

By J. C. Bradbury

The year of the Centennial is upon us. Not only is AIME marking its 100th birthday, but the cement industry is also celebrating 100 years of activity (see article by Roy Grancher, page 48). Fort Dodge, Iowa, and gypsum also tried to get into the act but missed by one year. Frank Apple-yard's gypsum article (page 53) informs us that the Fort Dodge area has been producing gypsum continuously for 99 years. That would seem to make AIME and the industrial minerals doddering oldsters. Not so-our Institute shows more energy than ever, and the word for industrial minerals is growth. These are the mineral resources of the future, the raw materials for the abundant life to come

Jan 1, 1971

By Heinrich Oscar Hofman

IN THE death of Professor Hofman who was born on Aug. 13, 1852 and died on April 28, 1924, the world has lost a great metallurgist and a great author of metallurgical literature. Measured in time his life was not quite seventy-two years, but measured in work accomplished it was much longer than this. It is not surprising that Dr. Hofman became a great scholar for his father, Karl Hofman, was on the faculty of Heidelberg University, and his early days were spent in these surroundings. He studied in the University under such men as Kirchoff and Bunsen and often spoke of the intimate relations he had with them. Following his course at Heidelberg, he studied at the Clausthal Mining Academy where he graduated with honors, receiving the degrees of Mining Engineer and Metallurgical Engineer in 1877.

Jan 1, 1924

By A. H. Geisler, F. Keller

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947

By F. Keller, A. H. Geisler

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947