Search Documents

By G. V. Smith, C. O. Tarr, R. F. Miller

Metallurgists have long recognized that the Fe3C type of carbide is not a stable phase in steel and that, given sufficient time, it will decompose with formation of graphite, at least at temperatures below about 205o°F.l This slow graphitization has never been of much concern to users of hypoeutectoid steels, for in such steels it occurs only during prolonged exposure at elevated temperature. In I935, Kinzel and Moore2 reported complete graphitization of the carbide of a 0. I5 per cent carbon steel that had been in service for about 26,000 hr. at a temperature of about IIOO° to 12oo°F. In discussing this paper, both Mathews and Sauveur reported graphitization of slightly hypereutectoid steels. In an extensive investigation of graphitization of high-purity iron-carbon alloys, Wells1 produced graphite at 7oo°C. (I29o°F.) in an alloy containing as little as 0.13 per cent carbon, and showed that graphite may precipitate either directly from austenite or from decomposition of Fe3C, also that the rate of graphitization tends to increase with increase of temperature, at least up to a certain point, and with the presence of graphite nuclei. Jenkins, Mellor and Jenkinson,3 studying the structural changes in carbon steels ranging from 0.17 to 1.14 per cent carbon during stress-rupture tests at elevated temperature, observed graphite in an aluminum-killed 0.40 per cent carbon steel after fracture in 4340 hr. under a stress of 17,900 lb. per sq. in. at 840°F. and in many of the steels after stress-rupture test at 12oo°F. Unstressed samples of 0.60, 0.86 and I.I4 per cent carbon steels graphitized almost completely in 360 hr. at I200°F., while samples of 0.90 and 1.10 per cent carbon steels were somewhat graphitized, and steels containing 0.24, 0.40 and 0.57 per cent carbon showed no sign of graphite. Their results indicate that graphite precipitates the more readily the higher the carbon content, though this tendency is influenced to some extent by deoxidation practice, and that graphitization is accelerated by plastic deformation. In a recent study of the graphitization of 0.4 and 0.6 per cent carbon steel strip, made by M. A. Hughes,4 it was found that at I2oo°F. graphite appeared after 72 hr. in aluminum-killed but not in silicon-killed steel, and that the rate of graphitization was increased by slow cooling from I6oo°F. and by cold-working prior to annealing. In creep tests of normalized 0.15 per cent carbon steel killed with 2.5 Ib. of aluminum per ton, at the U. S. Steel Corporation laboratory at Kearny, spheroidization and some graphitization were found after 3000 hr. at Iooo°F. under a stress as low as 1500 lb. per sq. inch. .

Jan 1, 1944

By C. O. Tarr, G. V. Smith, R. F. Miller

Metallurgists have long recognized that the Fe3C type of carbide is not a stable phase in steel and that, given sufficient time, it will decompose with formation of graphite, at least at temperatures below about 205o°F.l This slow graphitization has never been of much concern to users of hypoeutectoid steels, for in such steels it occurs only during prolonged exposure at elevated temperature. In I935, Kinzel and Moore2 reported complete graphitization of the carbide of a 0. I5 per cent carbon steel that had been in service for about 26,000 hr. at a temperature of about IIOO° to 12oo°F. In discussing this paper, both Mathews and Sauveur reported graphitization of slightly hypereutectoid steels. In an extensive investigation of graphitization of high-purity iron-carbon alloys, Wells1 produced graphite at 7oo°C. (I29o°F.) in an alloy containing as little as 0.13 per cent carbon, and showed that graphite may precipitate either directly from austenite or from decomposition of Fe3C, also that the rate of graphitization tends to increase with increase of temperature, at least up to a certain point, and with the presence of graphite nuclei. Jenkins, Mellor and Jenkinson,3 studying the structural changes in carbon steels ranging from 0.17 to 1.14 per cent carbon during stress-rupture tests at elevated temperature, observed graphite in an aluminum-killed 0.40 per cent carbon steel after fracture in 4340 hr. under a stress of 17,900 lb. per sq. in. at 840°F. and in many of the steels after stress-rupture test at 12oo°F. Unstressed samples of 0.60, 0.86 and I.I4 per cent carbon steels graphitized almost completely in 360 hr. at I200°F., while samples of 0.90 and 1.10 per cent carbon steels were somewhat graphitized, and steels containing 0.24, 0.40 and 0.57 per cent carbon showed no sign of graphite. Their results indicate that graphite precipitates the more readily the higher the carbon content, though this tendency is influenced to some extent by deoxidation practice, and that graphitization is accelerated by plastic deformation. In a recent study of the graphitization of 0.4 and 0.6 per cent carbon steel strip, made by M. A. Hughes,4 it was found that at I2oo°F. graphite appeared after 72 hr. in aluminum-killed but not in silicon-killed steel, and that the rate of graphitization was increased by slow cooling from I6oo°F. and by cold-working prior to annealing. In creep tests of normalized 0.15 per cent carbon steel killed with 2.5 Ib. of aluminum per ton, at the U. S. Steel Corporation laboratory at Kearny, spheroidization and some graphitization were found after 3000 hr. at Iooo°F. under a stress as low as 1500 lb. per sq. inch. .

Jan 1, 1944

By W. B. Plank, A. C. Callen

WAR and normalcy do not walk hand in hand, whether it be in industry, the educational field, or in the daily lives of individuals. Schools and departments offering curricula in mineral engineering have been seriously disrupted, beginning with 1942 and reaching a low during 1944. Selective Service regulations and voluntary enlistments have effectually stopped the flow of college-trained men into the mineral industry, and the flow into the colleges is little more than a dribble. The year just closed has been a most serious one for our institutions. Until March many of our faculties had been kept reasonably intact because of the large training programs of the Army and Navy. Although the number of

Jan 1, 1945

By PHILIP N. MOORE

THE development of the power of the Tennessee River at Muscle Shoals has become a matter of political interest as well as engineering possibility. The controversy over it has been so active that the facts have been obscured, the possibilities exaggerated. Although the members of the American Institute of Mining & Metallurgical Engineers are not generally specialists in hydroelectric development, those who visited Muscle Shoals in October, following the Birmingham meeting of the Institute, were interested, and many of them surprised to learn the actual conditions. These have long been familiar to those who have studied the matter through the reports of the U. S. Engineers on the subject. The approved plan contemplates three dams-No. 1, a low dam close to the City of Florence, planned in the interests of navigation, since the construction of the other dams has rendered impossible the use of the river without it. No. 2-named the Wilson Dam is now under construction. Concerning it political argumentation has waged. No. 3 Dam-much smaller, is planned to be erected several miles above No. 2.

Jan 1, 1925

By J. B. Morrow

BITUMINOUS COAL production for 1937 up to Nov. 27, was 400,000,000 ions, an increase of 3.43 per cent over the comparative period in 1936. The in- crease in consumption, however, was not so great as the increase in production. Stocks of coal, mostly in the hands of consumers, on Nov. 1 were 57,000,000 tons, compared to 44,400,000 tons at the same periods in 1936. The prospects were that both production and consumption for December, 1937, would be lower than for the corresponding month of 1936. , Anthracite production for the period ending Nov. 20 was 43,900,000 tons, com- pared to 48,500,000 tons for the corresponding period in 1936, or a decrease of 9.5 per cent. Production of mechanically loaded coal in. 1936 was approximately 57,000,000 tons, an increase of 17.5 per cent over

Jan 1, 1938

By FREDERICK MCAKCCOY

THE production of tin from Mexico has never reached the point of being considered a national industry, but the distribution of tin ores is so widespread that there are possibilities that one day it may become of importance. Of the twenty-seven states of the Republic, tin claims have been taken up in sixteen. In all there had been taken up to the end of 1926, two hundred and twenty-five claims, of a total area of about 7400 acres. The first historical mention of tin in the Americas is found in a letter of Cortez to the Emperor, Charles the Fifth, of Spain, which is as follows: Speaking of his manufacture of some small cannon, he says: "For these reasons I took considerable pains to get copper from some provinces of this country, and bought it at a high price in order to get it quicker.

Jan 1, 1929

F. E. Thompson, Pottstown, Pa.: If Mr. Webster's endeavor to open up the subject of cast-iron should prove as prolific of results as did the discussion on " The Physics of Steel," he must certainly feel richly repaid. His remarks concerning the secretiveness and conservatism of the average foundry-man recall to my mind an instance of a blast-furnace which, for the last year, has been producing much foundry-iron. The manager, believing that much more of his product could be used in the foundry than the foundry-men were will-

Jan 1, 1896

By Stanford O. Grodd

The Sanford Lake district encompasses an area covering 24 square miles in the central Adirondack Mountains of northern New York State. Discovery of the titaniferous magnetite deposits dates back to 1826. Several attempts to exploit the ores for iron prior to 1942 proved uneconomical because of difficulties with the associated titanium, lack of transportation facilities, and the isolated location. Since 1942, the National Lead Company has produced ilmenite concentrates for the titanium pigment industry, and a magnetite by-product used in the steel and refractory industries. Rocks of the area are Precambrian in age and of igneous origin. The area has a history of erosion, deformation, and metamorphism, subsidence, and finally uplift and glaciation. The resulting topography is extremely rough with drainage patterns controlled by a combination of fault patterns and glacial modifications. The district is within the large anorthosite massif making up the central high peak area of the Adirondacks. All of the various lowsilica rock types associated with the massif are found within the boundaries of the district. These consist of both the Marcy and Whiteface types of anorthosite and of gabbroic anorthosite, gabbro, and different grades of titaniferous magnetite ores. All of the rocks contain the same minerals and differ only in their percentages of these consitituents. Gabbro, and ore associated with it, demonstrate flow structure as both have foliation and lineation. Anorthosite and its associated ores are massive and show very little primary structure. Minor pegmatites and diabase dikes provide evidence of remobilization in selected areas and of late intrusion as well. Faulting is prevalent and follows a regional pattern of major faults trending northeastsouthwest and of minor faults at nearly right angles to them. There are four mineralized areas where an economic grade of ore has been found. Three of these have both gabbroic-type ore and anorthositic-type ore. The fourth has only gabbroic ore. Ores are graded according to their TiO, content, and these range from 9.5 per cent to over 30.0 per cent TiO,. Ore bodies of both types are related to gabbro and conform to the configuration of the gabbro bodies within the anorthosite. At least three distinct theories of ore genesis have been expounded by different investigators. Others propose some variations of one or more of these. Although complete agreement probably never will be reached, it is certain that no one process of ore emplacement can explain the complicated picture as seen today. Further understanding of the ores and their origin will require detailed mapping, sampling, and mineralogical studies of the entire district, and then it may never be understood without qualification.

Jan 1, 1968

By B. A. Rogers

IN addition to the usual methods of manufacturing steel, a number of special processes have been the subject of considerable experimentation-and use in manufacturing practice. A number of these methods have been of a type in which a rapid refining action has been secured through the intimate mixture of fluid slag with fluid metal. The persistence with which more rapid methods are sought is indicated by the current interest in the Aston' method for producing wrought iron and in the Perrin2 process for dephosphorizing and deoxidizing steel. In the Perrin process, in particular, the mixing action is extremely vigorous and the reactions proceed with surprising speed.

Jan 1, 1936

By AIME AIME

COMMITTEES. CANAL ZONE.-Col. George W. Goethals, U. S. A., Chairman; Lt.-Col. H. F. Hodges, U. S. A. ; Lt.: Col. D. D. Gaillard, U. S. A. ; Lt.-Col. William L. Sibert, IT. S. A. ; H. H. Rousseau, U. S. N.; Col. W. C. Gorgas, U. S. A.; Maurice H. Thatcher ; Joseph Bucklin Bishop ; Lt.-Col. Charles F. Mason, U. S. A.; S. B. Williamson ; Major Eugene T. Wilson, U. S. A. ; Edward Schildhauer ; Henry Goldmark ; Edward C. Sherman ; W. G. Comber ; W. B. Corse ; J. A. Walker; Joseph A. Le Prince; J. A. Smith ; Lt. Frederick Mears, U. S. A. HAVANA.-V. T. Polledo, Chairman; Diego Lombillo Clark, Jose Primelles, J. R. Villalon, Jose Artola, J. Ducassi, Luis Morales, Enrique Montonlieu. ENTERTAINMENT ON SHIPBOARD.-William L. Saunders, Chairman; Mr. and Mrs. S. D. Warriner, Mr. and Mrs. Thomas Robins, Mr. and Mrs. George.D. Barron, Mr. and Mrs. R. B. Watson, W. E. Greene. GENERAL MANAGEMENT. .Joseph Struthers, Chairman; Albert E. Vaughan. There were ten sessions of the Institute held for the presentation and discussion of, technical or professional papers. Eight of these sessions were held on the steamer while en route, and two in the ball-room of the Hotel Tivoli, at Ancon, C. Z. Mr. David W- Brunton, President of the Council, presided at all the sessions, except the sixth, at which Mr. Charles Kirchhoff, past President, occupied the chair. The following list includes the papers presented in oral abstract by the authors: First Session., October 24. The Summit Hill Mine-Fire, by W. A. Lathrop, Philadelphia, Pa. Mine-Fire at the Calumet and Hecla Mine, No. 8 Shaft., by S. D. Warriner, Wilkes-Barre, Pa. Fire in the Big Lick Stope, Lykens Valley and Williamstown Colliery, by R. V. Norris, Wilkes-Barre, Pa. Mine-Fire in the Hecksherville Valley, Schuylkill Field, Pa., by W. J. Richards, Pottsville, Pa.. Fire in the Monarch Mine, near Rock Springs, Wyo., by S. A. Taylor, Pittsburg, Pa.

Dec 1, 1910

By J. T. Ryan

SAFETY practice or the elimination of accidents in our coal mines is specifically a problem of management. It cannot be delegated to any governmental agency except that the various coal-producing states do and should have some minimum safety standard laws. However, the legislative method of attempting to control mine accidents is ineffective because of the delay between the necessity and the action. It will always be impossible to keep our various state mining laws up to date; and when the law says you must do a certain thin there is a tendency to do this and no more. Unless the scheme for setting up state regulations is so flexible that when a new hazard develops it can be immediately and adequately covered and the whole responsibility for accident elimination placed undivided on the

Jan 1, 1937

By V 9. 0 / 300 dpi

ATHOUGH turquoise mining was, so far as we know, the first large, well-organized mining operation,' gem mining, from the Roman con-quest of Egypt until the opening of the South African pipe diamond mines some 50 years ago, was largely carried on' by individuals 01' small companies in a relatively primitive way. Now" however" gem mining does not yield in efficiency or in scale of operations to the mining of other mineral products. In 1926 the diamond mines of the world milled some 9,000,000 cu. yd. and produced 0,43 cu. yd. diamonds, a remarkable example of concentration. The Premier Diamond Mining Co. up to Oct. 31, 1927, had milled 116,455,550 loads (each of 16 cu. ft.) from which 26,-217,144 carats of diamonds" worth £29,897,971 2s, 9d., were recovered. The Burma Ruby Mines, Ltd., operating sever-al alluvial mines in Burma in 1911-12, mined and milled 1,479,845 truckloads of gemmiferous earth for 15c. per load. We of the industry can there-fore, with good grace, disclose some of the myths and also describe some of the primitive mining methods of the, dark ages of our industry. The methods, so far as I know, were not patented, and if they were, the patents have expired, so that engineers in other branches of the art are free to use them if they see fit.

Jan 1, 1928

By Henry Louis

THE work performed by the Royal Commission on Mining Subsidence is likely to prove of permanent value, less perhaps for the conclusions it has reached and for the recommendations it has based upon these than for the admirable exposition which it affords of the law concerning mining subsidence and of the legal status of the person who has suffered damage by reason of such subsidence, as also of him whose working has caused the damage. The Commission was appointed by Royal Warrant in the middle of 1925 and delivered its final report in the middle of 1927. The terms of reference to the Commission were as follows: "To consider the operation of the law relating to the support of the surface of the land, and of buildings or works on or under the surface, by underlying or adjacent minerals; to enquire into the extent and gravity of the damage caused by subsidence owing to the extraction of minerals and the incidence of the resulting liability; and to report what steps should be taken, by legislation or otherwise, to remedy, equitably to all persons concerned, any defects or hardships that may be found to arise in existing conditions."

Jan 1, 1929

By Rclssell Gibson, F. S. Turneaure

The tin deposit of Monserrat; Bolivia, consists of one major vein 1600 m in length. The ore is unusual because of the notable quantity of teallite, even though cassiterite is the principal tin mineral. The deposit, formed at shallow depth under a wide range in temperature, may be classed as xenothermal. Polished sections reveal a complex history of replacement, with low-temperature minerals deposited before high-temperature minerals.

Jan 1, 1950

By J. F. K. Brown, E. E. Roecker

For three years The Hudson Coal Co. has used egg anthracite instead of coke in its foundry cupola. It has long passed the stage of being told it cannot be done—the metal would be cold, of poor quality, or the speed of operation would be low. From observation, from use and from test. we know that our metal is about average; the cast iron invokes no adverse comment from the machine shop and the speed suits our foundry requirements. We have there-iore resolved into practice anthracite combustion processes in an industrial furnace formerly using coke, under conditions suitable to our needs. When it comes to translating what we know into use in another cupola, however, where operating conditions may be different, or to explaining why, with seemingly the same conditions in our own cupola, we have attained sometimes a temperature of 2800° in the metal and at another time 2600°, or a speed of 5 tons per hour against 2 35 tons per hour, we cannot do it. We cannot do this because there seems to be an unbridged gap between laboratory ideas on combustion and practical ideas on com-bustiqn, which we have been unable to cross in terms understandable to us as practical consumers. This gap or bridge centers around the problem of how combustion actually takes place; and we believe it is controlled by two factors: (I) the character of the surface of the fuel and (2) the space provided and needed within which the oxygen of the air is allowed to or can act on that surface. It has long been contended on behalf of coke that porosity is an important factor in combustion, although, admittedly, there are two schools of opposing thought on this question, as revealed in technical literature. It has been understood generally that a light, porous coke is the best metallurgical fuel because there are more square inches of carbon exposed to the blast of air, therefore more useful carbon-dioxide reactions can take place in the given space between the entrance of the air and the point where useful work is done. It is now our general idea that the heavier and the harder the coal, the better the metallurgical fuel, provided the surface of that fuel is suitable for fast reaction with the oxygen. Time and Space A cupola is loaded in layers of fuel and iron. The horizontal line where the first charge of iron rests on the coal is the top of the bed coal. With us that is 22 in., usually, above the tuyeres where the air enters. This means 600 lb. of coal. Every subsequent coal layer is 100 to 125 lb. of coal, and that 100 to 125 lb. of coal melts 1000 lb. of iron at around 2700° in the ladle. This quantity of coal represents a 3-in. layer spread across the cupola. The question arises: If this 3 in. of coal will melt 1000 lb. of metal, why was it necessary to use 600 lb., or 22 in., of coal beneath and between the first charge of iron and the air entrance?

Jan 1, 1944

By E. E. Roecker, J. F. K. Brown

For three years The Hudson Coal Co. has used egg anthracite instead of coke in its foundry cupola. It has long passed the stage of being told it cannot be done—the metal would be cold, of poor quality, or the speed of operation would be low. From observation, from use and from test. we know that our metal is about average; the cast iron invokes no adverse comment from the machine shop and the speed suits our foundry requirements. We have there-iore resolved into practice anthracite combustion processes in an industrial furnace formerly using coke, under conditions suitable to our needs. When it comes to translating what we know into use in another cupola, however, where operating conditions may be different, or to explaining why, with seemingly the same conditions in our own cupola, we have attained sometimes a temperature of 2800° in the metal and at another time 2600°, or a speed of 5 tons per hour against 2 35 tons per hour, we cannot do it. We cannot do this because there seems to be an unbridged gap between laboratory ideas on combustion and practical ideas on com-bustiqn, which we have been unable to cross in terms understandable to us as practical consumers. This gap or bridge centers around the problem of how combustion actually takes place; and we believe it is controlled by two factors: (I) the character of the surface of the fuel and (2) the space provided and needed within which the oxygen of the air is allowed to or can act on that surface. It has long been contended on behalf of coke that porosity is an important factor in combustion, although, admittedly, there are two schools of opposing thought on this question, as revealed in technical literature. It has been understood generally that a light, porous coke is the best metallurgical fuel because there are more square inches of carbon exposed to the blast of air, therefore more useful carbon-dioxide reactions can take place in the given space between the entrance of the air and the point where useful work is done. It is now our general idea that the heavier and the harder the coal, the better the metallurgical fuel, provided the surface of that fuel is suitable for fast reaction with the oxygen. Time and Space A cupola is loaded in layers of fuel and iron. The horizontal line where the first charge of iron rests on the coal is the top of the bed coal. With us that is 22 in., usually, above the tuyeres where the air enters. This means 600 lb. of coal. Every subsequent coal layer is 100 to 125 lb. of coal, and that 100 to 125 lb. of coal melts 1000 lb. of iron at around 2700° in the ladle. This quantity of coal represents a 3-in. layer spread across the cupola. The question arises: If this 3 in. of coal will melt 1000 lb. of metal, why was it necessary to use 600 lb., or 22 in., of coal beneath and between the first charge of iron and the air entrance?

Jan 1, 1944

By W. J., Kroll

MOST people believe that rare metals are always, scarce in nature, expensive to make, and therefore useless despite some miraculous properties which might make them a cure-all. There are' some metals, which are quite frequent in nature, such as zirconium, which are called rare only because our present methods for making them are elaborate, thus forcing the manufacturer to sell them at a high price. There are also truly rare metals, such as gallium, which do not occur frequently in ores, but are easily reducible from their oxides. In these cases the price of the concentration operation is the decisive factor. The distribution of the elements in the earth's crust is no indication as to the availability of a metal; the concentration operation is the critical factor. Concentration is frequently obtained in the course of metallurgical operations for the extraction of other metals, and the rare metal may be enriched in by-products, flue dusts, mother liquors or precipitates from electrolyte purification as are indium, thallium, selenium, and tellurium. A periodic table of the rare elements may serve as a basis for discussion of their properties and to establish a program. (Table 1.)

Jan 1, 1946

By David L. Holt, Walter A. Backofen, Anwar-uI Karim

Specimens of a hydrided Mg-0.5 Zr alloy were strained in tension at 500°C and constant rates of 2 x10-3 5 x 10-3, and 2 X 10" min-1. Hydride-denuded zones formed at grain boundaries normal to the tensile-stress direction as a result of magnesium transport during difusional flow. The width of the zones could be measured and the measurement used for calculating the diffusional component of the imposed tensile strain. The strain from diffusional flow was found to increase with imposed strain at a diminishing rate, tending to saturate at approximately 12 pct. Strain rate sensitivity of flow stress was low. The apparent non Newtonian character of the diffusional flow is attributed to a non Newtonian process acting in parallel with it which could be boundary shear. Fracture grows out of voids that form in the denuded zones. DEFORMATION of a grain by diffusion of atoms from boundaries stressed in compression to boundaries stressed in tension is Newtonian viscous,1-3 and evidence has accumulated in recent years that such a process may be responsible for the high strain-rate sensitivity of the flow stress of super-plastic alloys.4"7 One piece of evidence is that experimental stress: strain-rate relationships can be quantitatively explained.5-7 There is also metallo-graphic evidence of diffusional flow in superplas-ticity, but in a limited amount. The formation of striated bands on the surface of superplastically deformed specimens has been attributed to diffusional flow.5"7 The basis of that attribution came from experiments on a coarse-grained, nonsuperplastic and hydrided Mg-½ wt pct Zr alloy which formed hydride-denuded, light etching zones at tension-stressed boundaries when strained in tension at 270?C.6 The origin of these zones had already been traced to the diffusional flow of magnesium atoms to the boundaries.' The particular observations in the more recent work were of striated-band formation on the surface and denuded-zone formation internally, with both the bands and zones having the same width and appearing at tension-stressed boundaries. It was argued that the bands were a surface manifestation of the zones and hence of diffusional flow. Of course in superplastic alloys which do not contain internal metallographic "markers", the surface bands can be the only metallographic indication. In the present work, denuded-zone formation was utilized, as it has been by others,9-11 to extend the observations of diffusional flow and to measure the strain, ed, resulting from it. Grain size had to be large to measure ed with accuracy. The grain size chosen for this study was -30 , and with that a strain of 10 pct from diffusional flow produces a denuded zone only 3 µ in width. The large grain size naturally precludes superplasticity. The observations of diffusional flow were complemented by determining the strain from the other operative deformation modes: slip, e,, and grain boundary shear, egb. An incremental specimen extension is the sum of increments from slip, and grain boundary shear as well as diffusional flow. Division by a common length is required to convert to strain. If this length is taken as the initial specimen length, then imposed engineering strain, e, is given in terms of the component engineering strains by e = ed + es + egb [1] Stress:strain-rate relationships are determined by the way in which this "strain balance" is made up. EXPERIMENTAL Material. Zirconium hydride markers were introduced into the Mg-0.5Zr alloy by annealing in hydrogen at 450°C for 30 min. The hydride concentration was particularly high at zirconium rich stringers, which was fortunate in that the transverse boundaries at which denuded zones form lie perpendicular to the stringers. Grain size after annealing was 30 µ. Photomicrographs of unstrained and strained material are shown in Fig. 1. Procedure. Specimens were strained in tension with an Instron machine at crosshead velocities of either 2 x 10"3, 5 x X or 1 x 10-2 in. min-'. Specimen length and diameter were 1.0 and 0.2 in., respectively, so that initial strain rates in tests at constant crosshead speed were 2 x 10"3, 5 x X and 1 X l0-2 min-1. Tests were made at 500°C which is a compromise temperature at which diffusional flow is still measurable but grain growth is not active enough to interfere with metallographic measurements. The tests were made in a hydrogen atmosphere. Strain Balance. An equation additional to [I] is eg = ed + es [2] where eg is strain measured from grain elongation. Measurement was made of ed, eg, and, of course, e, which enabled all the strains in Eq. [I] to be determined. For this purpose, strained specimens were sectioned longitudinally, polished, and etched. The strain from diffusional flow, ed, was computed by measuring on photomicrographs the width in the tensile direction of denuded zones at either end of a grain XI, X2, adding them, and dividing by twice the initial longitudinal grain dimension L0, Fig. 2. Reported values are the results of measurements on seventy randomly selected grains; 95 pct confidence limits on ed were +1.5 pct strain. To measure eg, the maximum length, L, and the maximum width, W,

Jan 1, 1970

By W. C. Winegard, A. Galibois, C. J. Beingessner

The effects of solutes on the distribution of two-dimensional configurations of grains in zone-refined tin have been studied. When solutes with partition coefficients (ko) greater than unity are added, three-sided pains become more prevalent and the growth law changes. It is shown by electron-Probe micro-analysis that a solute buildup occurs ahead of a moving grain boundary when ko > 1. It has been found recently1, 2 that solutes with partition coefficients greater than unity have a larger retarding effect on grain growth than solutes with k, less than unity. ko is defined as the ratio of the concentration of solute in the solid to the concentration of solute in the liquid with which the solid is in equilibrium. Niessen and winegard2 have suggested that this effect is probably due to the complex shape changes which occur during the process of grain growth and that no theory based on single boundary motion3-5 can explain the results. They suggested that the dissociation of the unstable fourfold junction was delayed in alloys where ko was greater than 1 because the boundaries at the junction had to move into a region of high solute concentration. If indeed this mechanism were correct, it was felt that not only would the dissociation of fourfold junctions be affected by the solute buildup ahead of the boundaries, but the collapse of three-sided grains would be impaired. These combined effects would naturally lead to a modification in the distribution of the number of sides per grain seen on a two-dimensional section. The present investigation was undertaken to test these hypotheses by examining the grain-growth process in detail. EXPERIMENTS The Distribution of Grain Configurations in Zone-Refined Tin as Seen on a Two-Dimensional Section. Following the method of Bolling and Winegard,6 zone-refined tin was cast into button-shaped specimens and, subsequently, plastically deformed under a drop hammer at room temperature. The resulting flat coin-shaped samples were annealed at 200°C, some for 50 sec and others for 100 sec. The specimens were then examined to determine the distribution of the number of sides per grain, i.e., the num- ber of crystals adjacent to any particular grain in the section. For simplicity, the grains were classified as three-sided, four-sided, and so forth; this concept is schematically illustrated in Fig. 1. As indicated by smith,' it was necessary to examine every grain within an enclosed area to obtain a proper distribution of the relative frequency of each type. The distributions for the two annealing times are illustrated in Fig. 2. The total number of grains examined is also indicated on the figure. It is evi-

Jan 1, 1965

By P. E. Doherty, B. Chalmers

Subboundaries may be revealed in aluminum by the formation of pits on the surface during cooling from elevated temperatures. The pits do not form in the vicinity of high- or low-angle boundaries. They are attributed to the condensation of vacancies from a super saturation produced during coolirzg. Using the vacancy pit and Schulz X-ray techniques for observing low-angle boundaries, a study was made of the transition from the nearly perfect seed to the striated structuke characterist-ic of aluminum crystals grown from the melt. It was found that the individual striation boundaries develop by the coalescence of very small-angle boundaries, as well as by the addition of individual dislocations. Several mechanisms for the formation of striations are discussed. Evidence was found suggesting that a super-saturation of vacancies exists near a growing interface, and it is proposed that the resulting climb of existing dislocalions produces "half'-loops" at the interface, which combine to form the low-angle striation boundaries. LINEAGE, or "striation" boundaries, have been studied in detail by Teghtsoonian and Chalmers 1,2 in crystals of tin grown from the melt, and by Atwater and Chalmers3 in lead. They found that single crystals grown from the melt consist of regions which are separated by subboundaries that lie roughly parallel to the growth direction. A difference in orientation of 0.5 to 3 deg exists between the striated regions; the misorientation is such that the lattice of one region could be brought into coincidence with the lattice of its neighbor by a rotation about an axis approximately parallel to the direction of growth of the crystal. They observed an incubation distance for the formation of striations which increased with decreasing growth rate. They also found that in any crystal, the sum of all rotations of the lattice in one sense, in going from one striation to the next, is very nearly equal to the sum of all the rotations in the opposite sense. A striation boundary, which is a low-angle grain boundary, can be described as an array of dislocations. If it is assumed that suitable dislocations are introduced into the crystal during solidification, the formation of striation boundaries can be explained as a result of the migration of the disloca- tions into arrays. The formation of arrays is energetically favorable since the energy of an assembly of dislocations can be reduced by the interaction of the stress fields when a suitable array is formed. This investigation presents and interprets new information concerning the nature and origin of striation boundaries in aluminum. EXPERIMENTAL TECHNIQUE Single crystals of high-purity aluminum (Alcoa 99.992 pct) were prepared by horizontal growth from the melt.'' The specimens were subsequently electropolished in a solution of 5 parts methanol to 1 part perchloric acid kept between -10° and 0°C in a bath of dry ice and alcohol. The current density was approximately 6 amps per sq in. Doherty and Davis9 have shown that in aluminum sub-boundaries with misorientations of not less than several seconds of arc may be revealed by the vacancy pit technique. During cooling from elevated temperatures pits form on electropolished surfaces of aluminum crystals as a result of the condensation of vacancies.11 Pits do not form in the vicinity of small- or large-angle grain boundaries, presumably because such boundaries act as sinks for vacancies. Boundaries of misorientations down to 3 sec of arc are revealed as pit-free regions, see Fig. 1. The Schulz X-ray technique12 was used to determine the angular misorientations of subboundaries. In this method, white radiation from a micro-focus X-ray tube is used to produce an image of a fairly large area of a single crystal surface. Subboundaries cause splitting in the diffracted image, see Fig. 2. Misorientations down to about 15 sec of arc may be observed with this technique. OBSERVATIONS AND DISCUSSION Figure 1 shows a striated aluminum crystal grown at 10 cm per hr etched by the vacancy pit technique. An incubation distance of about 1 cm is observed before the initiation of striation boundaries. Fig. 2 is a Schulz X-ray photograph of a striated crystal similar to that shown in Fig. 1. A large area of the crystal was studied by means of a series of photographs. Fig. 2, which is a reflection from the (100) plane, included about the first 4 cm of crystal to freeze. There is an incubation distance of about 1 cm, and a distance of about 2 cm over which the angle of misorientation builds up to its final value of approximately one degree. Some twist component can be seen in Fig. 2 at the right side of the photograph. From Fig. 2 it can be seen that the sum of all rotations of the lattice in one

Jan 1, 1962