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By James H. Hance

Several years ago the writer was connected with the Mint and Assay Service of the Federal Government as Assistant Assayer at the Salt Lake Assay Office. At that time cyanide bars formed approximately half of the bullion purchased by that office. Disagreement in valuat,ion between the producer and the office was not infrequent and to a lesser extent between the Assay Office and the Mint, this latter issue being soon obviated, however, by adopting uniform methods of sampling the bars. A nice problem seemed to offer itself for research and the writer began a series of experiments which were soon terminated, however, by his going into other work, and which he regrets have not since been completed. The results attained may suggest lines of approach to this problem and are, therefore, offered in this article. Frederic P. Dewey, Assayer of the Mint Scrvice, U. 5. Treasury, has had abundant opportunity to study this phase of metallurgy, and has published several articles relative thereto.1 In the last article cited Dewey quotes analyses of cyanide bullion similar in content to that with which the writer worked, and which show some of the variations met with. In the discussion of these papers,2 comparison has been made in terms of copper bullion, but to the writer this seems of questionable value. Copper bullion may resemble silver bullion, but its similarity to gold bullion with little or no silver content is another thing. The freezing-point diagram of Roozeboom, reproduced on page 881 of the discussion cited, is for the gold-silver series as stated. The original problem under discussion, however, is not this alloy but gold with base metals other than copper. As for the statement that the corners are the worst places or

Jan 1, 1916

By C. C. Clark, J. S. Iwanski

The purpose of this investigation was to study mi-crostructural changes that take place in a commercial nickel-chromium-iron alloy, such as Incoloy "901," over long periods of time at temperatures up to 13 50°F and to correlate such changes with creep-rupture properties. of the alloy. In the course of the investigation, some microstructural changes were observed which correspond to microstructural alterations found in previous studies of Inconel "X." Microstructural phases have been identified in both alloys with the aid of electron and X-ray diffraction and an electron probe microanalyzer. The materials used in this investigation were from commercial heats of the following chemical composition: Pct Cr Pct Ni Pct Mo Pct Fe Pct Cb Incoloy "901" 12.51 43.67 5.72 Bal. -Inconel "X" 14.61 73.44 - 6.61 1.02 Pct A1 Pct Ti Pct Mn Pct Si Pct C Incoloy "901" 0.10 2.46 0.46 0.24 0.05 Inconel "X" 0.70 2.43 0.51 0.36 0.04 Long-term creep-rupture tests were conducted on Incoloy "901" at temperatures of 1000°, 1200°1 and 1350°F. A summary of these results is shown in Table I along with the results of a long-term creep-rupture test conducted on Inconel "X" at 1500°F. The heat treatments given the specimens are also shown in Table I. When the creep-rupture results on Incoloy "901" are compared with shorter-tertn data, there is no evidence of any undue deterioration of the creep-rupture strength with time, nor is the elongation decreased more than would be expected from the influence of time alone. INCOLOY "901" PHASE IDENTIFICATION Microscopic examination of the Incoloy "901" specimens reveals a dark etching grain boundary constituent in the specimen which was under test for about 11,500 hr at 1000°F. This grain boundary constituent was seen to increase in size as the test temperature was increased to 1200" and 1350°F, Figs. 1, 2, and 3. Simultaneously, an acicular structure of definite crystallographic orientation appears within the grains of the 1350°F specimen, Fig. 3. Under examination with the electron microscope, a fine precipitate is observed in the 1200 °F specimen. Fig. 4. It becomes considerably larger in the 2850-hr 1350°F specimen, Fig. 5. In a few areas the precipitated particles have been replaced by, or transformed to, small needles or platelets. After 7380 hr at 1350°F, Figs. 3 and 6, the needles are much larger and have replaced nearly all of the fine precipitate. X-ray diffraction studies detected the presence of hexagonal Laves phase and hexagonal n phase (Ni,Ti) in the 1350°F specimens, Table 11. Only the Laves phase was detected by X-ray diffraction in the 1200°F specimen and none was detected in the 1000°F specimen. In this latter specimen, however, the small quantity of precipitate in the grain boundaries (presumed to be Laves phase) precludes its detection by X-ray diffraction. Composition of the hexagonal Laves phase is not yet known, although its diffraction

Jan 1, 1960

By Walter Kauzmann

All viscous or plastic flow of incompressible matter is the result of shear strain; the changing shape of any body that is being plastically deformed can be completely described in terms of the shear strain occurring at each point in the body.† Furthermore, the relative amounts of shear strain occurring in different parts of a body under stress depend upon the relative rates of shear strain at those different points, so that if the dependence of the shear rate of any material on the temperature, shear stress, previous history, etc., were understood, the principles of plastic deformation would be known, and we could calculate how a body made of a given material, having a given shape, and subject to a specified system of forces, would change its shape with time. It may be said, then, that the problem of plasticity resolves itself into, first, the problem of the rates of pure shear processes, and second, the application of what is known about pure shear to actual cases. It is the purpose of this work to investigate the former problem —i.e., the dependence of shear rates on temperature, stress, etc.—from the standpoint of .recent developments in the field of chemical-rate theory and with particular reference to the phenomena occurring in the creep of metals and in the plastic flow of crystalline solids in general. It is left for the mechanical engineer, and perhaps the expert in hydrodynamics, to deal with the problem of app1ications.l Resolution of Macroscopic Shear into Microscopic Movements; Resemblance to Chemical Reactions Just as any large body is made up of many small units, or atoms, so macro-scopically observable shear is the result of many microscopic unit shear processes; just as the understanding of the behavior of large bodies demands the understanding of the atoms of which it is made, so the understanding of macroscopic shear demands the understanding of these fundamental unit processes. The study of shear from this "atomistic" point of view has made considerable progress. There has been fairly complete understanding of shear processes in gases for a long time, at least for non-turbulent flow, as a chapter on gaseous viscosity in any text on the kinetic theory of gases will prove' In recent years Andrade2 and Eyring3 have presented important theories for the flow of liquids and amorphous solids. Becker14 Orowan,5 Taylor,6 Burgers,7 and Kanter8 have considered the plastic flow of crystalline solids from this

Jan 1, 1941

By Walter Kauzmann

All viscous or plastic flow of incompressible matter is the result of shear strain; the changing shape of any body that is being plastically deformed can be completely described in terms of the shear strain occurring at each point in the body.† Furthermore, the relative amounts of shear strain occurring in different parts of a body under stress depend upon the relative rates of shear strain at those different points, so that if the dependence of the shear rate of any material on the temperature, shear stress, previous history, etc., were understood, the principles of plastic deformation would be known, and we could calculate how a body made of a given material, having a given shape, and subject to a specified system of forces, would change its shape with time. It may be said, then, that the problem of plasticity resolves itself into, first, the problem of the rates of pure shear processes, and second, the application of what is known about pure shear to actual cases. It is the purpose of this work to investigate the former problem —i.e., the dependence of shear rates on temperature, stress, etc.—from the standpoint of .recent developments in the field of chemical-rate theory and with particular reference to the phenomena occurring in the creep of metals and in the plastic flow of crystalline solids in general. It is left for the mechanical engineer, and perhaps the expert in hydrodynamics, to deal with the problem of app1ications.l Resolution of Macroscopic Shear into Microscopic Movements; Resemblance to Chemical Reactions Just as any large body is made up of many small units, or atoms, so macro-scopically observable shear is the result of many microscopic unit shear processes; just as the understanding of the behavior of large bodies demands the understanding of the atoms of which it is made, so the understanding of macroscopic shear demands the understanding of these fundamental unit processes. The study of shear from this "atomistic" point of view has made considerable progress. There has been fairly complete understanding of shear processes in gases for a long time, at least for non-turbulent flow, as a chapter on gaseous viscosity in any text on the kinetic theory of gases will prove' In recent years Andrade2 and Eyring3 have presented important theories for the flow of liquids and amorphous solids. Becker14 Orowan,5 Taylor,6 Burgers,7 and Kanter8 have considered the plastic flow of crystalline solids from this

Jan 1, 1941

By R. B. Schluter, M. M. Fine

Processes for manufacturing prereduced pellets have heretofore required temperatures of 2100°F or higher. Sulfides will accelerate the liquid-phase sintering of metallic iron, yet do not deter the reduction of iron oxides. The sulfides may be introduced as gases to the kiln atmosphere or as solids in the re-ductants. The net result is that well metallized iron pellets with good crushing strength can now be produced at a little over 1800°F. One of the most persistent topics at technical gatherings and in the recent scientific press has been the reduction of iron ore. In May 1960, a symposium on the subject was sponsored by the Electrochemical Society. The proceedings, comprising two dozen papers, were later published.' More recently, in November 1966, a similar gathering took place at Michigan Technological University, Houghton, Mich. The latest meeting was the International Congress on Production and Utilization of Reduced Materials at Evian, France, in May 1967. If the volume of literature, symposia and conferences is a measure of industry concern, then the current interest in reduction must be at a high level. Barrett,2 one of the early pioneers, stated some years ago that "The history of sponge iron has been so discouraging that many men in the iron and steel industry are violently opposed to giving it any further consideration." In spite of the "violent opposition" noted by Barrett, research people in and out of the industry continue to be attracted by the elusive prospect of uncovering a simple, viable means of direct reduction. Wild,3 one of the speakers at Evian, listed no less than 48 direct reduction processes (laboratory, pilot plant and commercial). Some of these were of historical interest only, but many others had resulted from developments within this decade. The previous big thrust into direct reduction occurred under the artificial impetus of a wartime economy (World War 11) and was largely an effort to provide more melting stock without coke ovens and blast furnaces. The present-day inquiry is proceeding at a more leisurely pace and the emphasis is different. For one thing, there is much less anxiety to circumvent the blast furnace. On the contrary, a whole new research endeavor has grown from the discovery that metallized burdens are exceptionally productive.4 Although the search for a melting stock

Jan 1, 1970

By C. G. Brehm

The anthracite-producing region is in the northeastern section of Pennsylvania, and has an area of approximately 484 square miles. It is divided geographically into three separate fields, known as the Northern, Middle and Southern. The Northern field, with Wilkes-Barre approximately at its center, is a basin about 60 miles long and almost 6 miles wide at its greatest distance across. Generally speaking, it may be said that the coal measures in this field lie horizontally, or on slight pitches, and consist of from 11 to 19 veins of coal, varying in thickness from several inches to several feet. The intervening strata between veins may be composed of slate, clay, rock or shale, or a combination of several, and are sometimes very thin. This condition often causes a treacherous roof, therefore roof support and the attending hazard of mining are problems of concern. The Middle field is made up of a number of small basins of not very great depth, and the measures, which are in like number to those of the Northern field, are varying inclinations running from nearly flat to steep pitches. The Lower, or Southern field, is made up of basins of great depth, some being 4000 ft. deep, and its measures are mostly on very steep pitches. In certain sections this Southern field is being mined at an elevation of 1300 ft. below sea level, on a pitch ranging from 50' to practically vertical, and because of the tremendous pressure and the inherent gas in the seams, outbursts of coal frequently occur at the face, locally known as "bumps." These outbursts are accompanied by a rumbling noise, after which gas is usually found. This condition makes mining a difficult and extremely hazardous undertaking, and unusual skill is required on the part of the miner to drive and maintain openings necessary to the production of coal. Miners working in such seams on the heavy pitch must carry face batteries (Fig. 1) to afford proper protection while working at the face, because of the outbursts and free running coal. To drive haulageways or gangways in this field it is

Jan 1, 1940

By C. G. Brehm

The anthracite-producing region is in the northeastern section of Pennsylvania, and has an area of approximately 484 square miles. It is divided geographically into three separate fields, known as the Northern, Middle and Southern. The Northern field, with Wilkes-Barre approximately at its center, is a basin about 60 miles long and almost 6 miles wide at its greatest distance across. Generally speaking, it may be said that the coal measures in this field lie horizontally, or on slight pitches, and consist of from 11 to 19 veins of coal, varying in thickness from several inches to several feet. The intervening strata between veins may be composed of slate, clay, rock or shale, or a combination of several, and are sometimes very thin. This condition often causes a treacherous roof, therefore roof support and the attending hazard of mining are problems of concern. The Middle field is made up of a number of small basins of not very great depth, and the measures, which are in like number to those of the Northern field, are varying inclinations running from nearly flat to steep pitches. The Lower, or Southern field, is made up of basins of great depth, some being 4000 ft. deep, and its measures are mostly on very steep pitches. In certain sections this Southern field is being mined at an elevation of 1300 ft. below sea level, on a pitch ranging from 50' to practically vertical, and because of the tremendous pressure and the inherent gas in the seams, outbursts of coal frequently occur at the face, locally known as "bumps." These outbursts are accompanied by a rumbling noise, after which gas is usually found. This condition makes mining a difficult and extremely hazardous undertaking, and unusual skill is required on the part of the miner to drive and maintain openings necessary to the production of coal. Miners working in such seams on the heavy pitch must carry face batteries (Fig. 1) to afford proper protection while working at the face, because of the outbursts and free running coal. To drive haulageways or gangways in this field it is

Jan 1, 1940

By C. E. MacQuigg

In this paper it is impossible to more than touch on many of the commercial alloys of iron, chromium, and carbon, therefore the discussion is confined to the properties of some of the less well-known alloys with upwards of 20-per cent. chromium. The discussion has been based largely on the strictly engineering aspects of the alloys. Chromium has well-defined effects when added to the iron-carbon system. These effects depend on the amount of chromium added and on the composition of the iron-carbon alloy to which the addition is made, i.e. whether low- or high-carbon steel, cast iron, etc. In the case of the low-carbon steels, the chromium addition, when not in excess of several per cent., appears to exert an influence on the properties by its influence on the critical range. In the higher chromium alloys, the physical properties are influenced chiefly by the formation of new complexes, such as iron-chromium solid solutions and, with higher carbon contents, iron-chromium carbides of great hardness. Examination of the published data1 on the critical range phenomena of chromium-bearing steels up to several per cent. chromium indicates an agreement on the following points:

Jan 1, 1923

By C. E. MacQuigg

In this paper it is impossible to more than touch on many of the commercial alloys of iron, chromium, and carbon, therefore the discussion is confined to the properties of some of the less well-known alloys with upwards of 20-per cent. chromium. The discussion has been based largely on the strictly engineering aspects of the alloys. Chromium has well-defined effects when added to the iron-carbon system. These effects depend on the amount of chromium added and on the composition of the iron-carbon alloy to which the addition is made, i.e. whether low- or high-carbon steel, cast iron, etc. In the case of the low-carbon steels, the chromium addition, when not in excess of several per cent., appears to exert an influence on the properties by its influence on the critical range. In the higher chromium alloys, the physical properties are influenced chiefly by the formation of new complexes, such as iron-chromium solid solutions and, with higher carbon contents, iron-chromium carbides of great hardness. Examination of the published data1 on the critical range phenomena of chromium-bearing steels up to several per cent. chromium indicates an agreement on the following points:

Jan 1, 1923

By R. D. Burlingame, T. L. Joseph, Gust Bitsianes

DESPITE almost fifty years of commercial practice, the sintering of iron ore has received little fundamental study. Much of the theoretical work1-'has dealt with the constitution of sinter produced under widely varying conditions. While these studies have broadened our knowledge of the changes that occur in the sintering zone and in the freshly formed sinter during the early stages of cooling, they provide little insight into the changes that precede the formation of sinter. These preliminary changes merit study as a part of the overall process. Hessle. working with beds of Swedish magnetite concentrates, was one of the first investigators to study the sintering process in its entirety. On the basis of temperatures observed at various levels of the bed during sintering, he postulated a number of distinct reaction zones to account for the chemical changes leading to the formation of sinter. A more direct method of attack is that of arresting the sintering zone after it has progressed part way through the bed. A study of a vertical cross section through such a quenched bed provides direct information on the changes taking place at various levels. This method was used by McBriar et al.' to show that several well-defined zones of chemical change existed within beds that were typical of British sintering practice. The same general method of attack was developed independently in the present investigation to study partially sintered beds typical of American practice. Experimental Sintering Equipment The sintering operation was carried out on an experimental scale with the equipment shown in Fig. 1. The refractory-walled sintering chamber A was 11 in. deep and averaged 9 in. in diameter. Air was introduced through a tapered flow section B, which contained the orifice C for accurate metering of the incoming air. This section was located directly above the square ignition housing D, which in turn rested upon the sintering chamber A. The bed was ignited with burner E. The required suction for the operation was furnished by a fan F, which had an air capacity of 500 cfm (stp). Hot exhaust gases from the sintering chamber were cleaned in the dustcatcher G before entering the exhaust fan. In the study of partially sintered beds, it was essential to find some technique for removing the entire charge from the sintering pot without disarranging the unsintered bottom portion. This problem was finally solved by sintering the charge in a removable basket, which snugly fitted the sintering chamber. This basket was constructed of two thicknesses of window screen and was lined with a 3/16-in. layer of asbestos paper. The bottom of the basket consisted of two thicknesses of wire screen, which were fastened to the basket wall. For high fuel mixtures, additional insulation was provided by a somewhat thicker layer of asbestos cement. Preparation of Partially Sintered Mixtures The moist feed was carefully placed in the sintering basket, to prevent segregation of the particles, which varied widely in size and composition. A thermocouple was placed in the center of the basket with the hot junction halfway down, and the mixture was evenly distributed around it. During ignition and throughout the sintering of the upper half of the bed, the hot junction temperature increased very little. When the sintering zone reached the halfway point, as indicated by the sudden increase in the hot junction temperature, the charge was quenched. During quenching the suction was turned off and the orifice was tightly stoppered to prevent further influx of air. At the same time, nitrogen was admitted to the sintering chamber through the orifice tap. As soon as the nitrogen had displaced the air and products of combustion, the charge was removed from the sintering pot for immediate dissection. It is impossible to preserve the exact zone structure of the bed at the instant that combustion is arrested unless the downward transmission of heat is also immediately stopped. Fortunately, heat transfer is very slow in beds containing a stationary fluid, especially if the particle size is small. It follows that the minimum quantity of nitrogen should be used to displace the air and that static conditions be established as soon as possible. A very steep temperature gradient across the combustion zone for some time after the quench was evidence of in-

Jan 1, 1957

By Joseph W. Leonard, T. S. Spicer

INTRODUCTION Reasons for Thermal Drying The continuing increase in the percentage of minus %-inch coal produced as a result of the increased use of mechanical mining methods has, over the years, tended to shift considerable portions of the work of producing saleable coal to the fine coal cleaning section of the preparation plant. Because a given weight of fine coal will contain substantially greater surface area than an equivalent weight of coarse coal, it follows that, when subjected to wet cleaning processes, the fines will absorb and retain consider- ably more moisture than coarser fractions. Increased moisture pickup in the finer sizes complicates fine coal cleaning since beneficiation may not be limited to the removal of ash and sulfur but often must be expanded to include the additional step of thermal drying to remove excessive moisture. Thus, water which provides the medium for cleaning fine coal is in itself detrimental and, like ash and sulfur, reduces coal quality. Removal of surface moisture by drying is done for one or more of the following 1 reasons: (1) To avoid freezing difficulties and to facilitate handling during shipment, storage and transfer to the points of use; (2) to maintain high pulverizer capacity; (3) to reduce heat loss due to evaporation of surface moisture from the coal in the burning process, thus increasing heating efficiency; (4) to improve the quality of coal used for special purposes, such as in the production of coke, briquettes, and chemicals; (5) to decrease transportation costs; and (6) to facilitate dry coal-cleaning processes. Because benefits to coal transportation and utilization are the most common reasons for thermal drying, the following sections will examine these areas in greater detail. Benefits to Transportation Initial benefits from drying are the reduction of shipping costs from the mine to the point of utilization since more coal can be concentrated into a given weight of product when worthless moisture is removed. Non- combustible~ such as water and mineral matter in railroad shipments of coal are billed the same as coal at $3.32 per ton, according to the recent average costs. Savings of 10 to 20 dollars from drying on the shipment cost of each 50 to 60 tons of coal contained in a typical railroad car is common. Savings on coal shipments from individual mines which result from coal drying can be expressed in terms of hundreds of thousands of dollars and more each year. For example, a reduction of shipping charges of only 5 percent on one million tons per year would mean a savings of 166,000

Jan 1, 1968

By H. A. Coy, James A. Noble

The Mascot mines of the American Zinc Co. of Tennessee are situated at Mascot, Tenn., 14 miles northeast of Knoxville, on the Southern Railway. The district is centrally located in the Great Valley, or Appalachian Valley Province. Prior to 1900, a small output of zinc was obtained from oxidized ore mined in open pits. In 1900, a shaft was sunk to sulfide ore, and in 1903, a second shaft was put down, neither being as deep as 200 ft. The American Zinc Co. of Tennessee began drilling in 1911, and outlined an ore-body to which its No. 1 shaft was sunk, to a depth of 365 ft. Since that time, the American Zinc Co. of Tennessee has been the only operator in the district. The Federal mining laws have never been in operation in Tennessee and mining lands are as irregular in boundary and area as farm lands. Ownerships are generally held in fee. In most cases the surface and mineral rights are transferred together. Electric power is supplied at 66,000 volts by the Tennessee Power Co., from a hydro-electric plant at Parksville, Polk County, Tenn., 100 miles from Mascot. No other power is used, but an emergency steam plant is held ready in case of interruption of service. Labor is all native and non-union. Negroes are employed for most of the shoveling, and for a few miscellaneous jobs, but for almost no other work. Exploration Exploration is carried ahead of mining largely by surface drilling. Both churn and diamond drills are used. Holes are not spotted according to geometric plan, but to block out ore outlines with the least number of holes. Churn-drill cuttings from each 5-ft. run are mounted for formation record, and in ore ground, all the bailings from each 3 ft. of advance are sampled and assayed. Diamond-drill cores are sampled and a specimen core filed for formation record. In ore ground, all the core

Jan 1, 1925

By Wm. R. Webster

This is a contribution for the proposed new discussion on the physics of steel. The former discussion on the subject started with the consideration of five papers presented at the Chicago meeting in 1893, and continued for several years. The Suggested Lines of Discussion, prepared by Doctor Howe, covered a wide field and added greatly to the success of the work. Naturally, the first step in a new discussion will be to remodel and bring up to date the old Suggested Lines of Discussion so as to embody all the important advances in the metallurgy of steel that have a bearing on the physics of steel and keep the papers and discussions within the field of work undertaken. This paper will be devoted to the practical application, in rolling steel, of the effects of carbon, phosphorus, and manganese on its tensile strength, with some suggestions on further research work. Dr. J. E. Stead, in his paper Influence of Some Elements on the Mechanical Properties of Steel,' gave a complete review of all that had been done during the past thirty years. He gave full credit to all investigators who worked on these lines, also their results, with his views on same, and in many cases his own results. All of this data and much new valuable information were put in convenient shape for reference and study. To do this required a great deal of work, which is fully appreciated by the steel manufacturers and investigators. The variations in the values given by the different investigators for the increase of the tensile strength of steel for each 0.01 per cent. of carbon, phosphorus, and manganese were largely due to the steels they worked on, the large or small variations in the amount of the elcments present, and the omission to take into consideration all the factors, from the blast furnace through to finished rolled material, that affect the character of the steel. For instance, a poorly made dirty steel requires considerably more carbon to give the same ultimate strength than a well-made clean steel with the same phosphorus and manganese content.

Jan 1, 1922

By Wm. R. Webster

This is a contribution for the proposed new discussion on the physics of steel. The former discussion on the subject started with the consideration of five papers presented at the Chicago meeting in 1893, and continued for several years. The Suggested Lines of Discussion, prepared by Doctor Howe, covered a wide field and added greatly to the success of the work. Naturally, the first step in a new discussion will be to remodel and bring up to date the old Suggested Lines of Discussion so as to embody all the important advances in the metallurgy of steel that have a bearing on the physics of steel and keep the papers and discussions within the field of work undertaken. This paper will be devoted to the practical application, in rolling steel, of the effects of carbon, phosphorus, and manganese on its tensile strength, with some suggestions on further research work. Dr. J. E. Stead, in his paper Influence of Some Elements on the Mechanical Properties of Steel,' gave a complete review of all that had been done during the past thirty years. He gave full credit to all investigators who worked on these lines, also their results, with his views on same, and in many cases his own results. All of this data and much new valuable information were put in convenient shape for reference and study. To do this required a great deal of work, which is fully appreciated by the steel manufacturers and investigators. The variations in the values given by the different investigators for the increase of the tensile strength of steel for each 0.01 per cent. of carbon, phosphorus, and manganese were largely due to the steels they worked on, the large or small variations in the amount of the elcments present, and the omission to take into consideration all the factors, from the blast furnace through to finished rolled material, that affect the character of the steel. For instance, a poorly made dirty steel requires considerably more carbon to give the same ultimate strength than a well-made clean steel with the same phosphorus and manganese content.

Jan 1, 1922

By Jun Hino, P. G. Shewmon, P. A. Beck

THE investigations of Crussard,' of Guinier and Tennevin,' and of Dunn and Daniels," indicate that the subgrains formed in a cold worked and annealed metal are capable of growing at each other's expense during annealing, if the temperature of annealing is sufficiently high and the time is long enough. The results of Dunn and Daniels are particularly convincing in showing that subgrain growth is essentially the result of the free surface energy associated with the subboundaries. In subgrain growth, as in ordinary grain growth, energy is gained as a result of the decrease in total subboundary surface area per unit volume. Recently, Wood and Scrutton4 found that the rate of subgrain growth upon annealing increased very considerably, if simultaneously a creep strain was applied to the specimen at a low strain rate. Working with 99.98 pct pure fine-grained aluminum, these investigators found that the continuous X-ray diffraction back-reflection rings of material strained at room temperature remained continuous after heating for ten days at 250 °C. However, when heated at the same temperature under a stress of 1000 psi even for only three days, the formerly continuous X-ray diffraction rings broke up into numerous dots, which were fairly clearly separated from each other. The continuous X-ray diffraction rings were interpreted as indications of a very small subgrain size, not resolved by the X-ray diffraction method used. The breaking up of the continuous X-ray diffraction ring during annealing under stress was taken as an indication of a great increase in subgrain size, so that the individual subgrains could then be resolved. The effect of simultaneous strain at a low strain rate in accelerating subgrain growth, discovered by Wood and Scrutton and designated by them as "cell growth," is of fundamental importance. The experiments described in this note were carried out in order to confirm Wood and Scrutton's results by direct metallographic observation. Also, information was sought as to the minimum creep strain necessary to produce this effect. A fine grained high purity aluminum strip was prepared by alternate 33 pct rolling and annealing treatments for 1 hr at 350°C. Specimens cut from this strip were subjected to a relatively fast creep strain of 7.2 pct in 3.5 min at 300°C under a constant load initially corresponding to 1185 psi. The subgrains set up were large enough (about 0.015 to 0.03 mm) to be clearly observed (Fig. 1) at X200 magnification with polarized light, after electrolytic polishing and anodic etching, producing a fine oxide film." The corresponding X-ray diffraction pattern is shown in Fig. la. After the fast creep strain treatment a portion of the specimen was subjected to a creep strain of 8.3 pct in 44 hr at 350°C under a constant load initially corresponding to 320 psi. Another portion, annealed under the same conditions, but not strained, served as control specimen. The subgrain size of a typical area of the specimen annealed under strain and of the one annealed without strain is shown in Figs. 2 and 3 (X-ray diffraction patterns, Figs. 2a and 3a). Annealing without strain produced clearly observable subgrain growth (subgrain size: about 0.03 to 0.05 mm). The effect of simultaneous strain was to increase greatly the rate of subgrain growth (resulting in a subgrain size of approximately 0.05 to 0.13 mm), in accordance with Wood and Scrutton. In another experiment, the effect of the amount of simultaneous strain was studied. The initial subgrain structure was set up by fast creep, as described previously. The specimen was then heated at 350 °C under a constant load initially corresponding to 320 psi, as above, for 2.2 hr (0.24 pct strain), and 8.8 hr (0.58 pct strain). Comparison with the corresponding unstrained control specimens by means of X-ray diffraction showed that 0.58 pct strain definitely had an effect, but the effect of 0.24 pct strain was doubtful.

Jan 1, 1953

By C. S. Sivil

To modern civilization the platinum metals are of inestimable value. Their distinctive properties, both physical and chemical, render them indispensable in an age in which the processes of the laboratory are becoming an essential part of the daily life of the world. Generally, their function, though vital to particular processes, is not spectacular, and so remains unknown to all except the operators. EARLY METHODS OF MANUFACTURE The properties of platinum were recognized as of prime importance for scientific work at. a very early date, probably between 1750 and 1760. The difficulty of making articles from it seemed almost insurmountable, because no means of attaining the temperature necessary to melt it were known at that time. It is true that solid platinum could be obtained by fusing the metal with a more volatile metal such as arsenic, which was subsequently driven off by baking, but such a method, at its best, would give only a very brittle product, which was totally unsuitable for the purposes for which it was intended. Little, if any, progress could be made until it was discovered that platinum sponge, heated to white heat and hammered in an iron or clay mold, would metallize and retain the shape of the mold. This was a process that could not be wholly satisfactory but from it developed the method of pressing the sponge in a mold and forging it at white heat into wire or sheet. At present a somewhat similar process must be used for fabricating articles of tungsten, molybdenum and other metals of high fusing point, as with these metals we face today the same problems that the scientists of the eighteenth century encountered with platinum, but possibly the next significant advance in the metallurgy of these metals will be the devising of means to melt and cast them.

Jan 1, 1931

By L. D. Jaffe, F. W. Cotter, E. Cordon

The hardenability of titanium-base alloys was studied by metallographic examination and hardness survey of Jominy specimens end-quenched from the B range. Analyses of the data led to the equation log J = -0.57 + 0.25 @ct Fe + pct Mn + pct Mo) + 0.19 @ct Cr) +0.16 @ct V) + 0.03 @ct Zr). Here J is the distance, in sixteenths of an inch, from the quenched end of a Jominy hardenability specimen in the position of peak hardness, for material quenched from the B range. This equation fitted the experimental data with a standard deviation of approximately 0.29. The effects of the elements Al, Sn, W, Cu, Ni, B, C, N, 0, and H, and of pain size, were not statistically significant or not practically significant. A check against hardenability measurements in the literature showed agreement within the stated standard deviation. The equation should be useful in estimating hardenability of new or modified titanium alloys. HARDENABILITY in a titanium-base alloy is the ability of the alloy to retain the B structure on quenching. An alloy with high hardenability will retain the /3 structure even when cooled relatively slowly from a temperature at which B or P plus a is stable. A low hardenability material will retain P only if quenched extremely rapidly from the range of p or 0-plus-a stability, or will not retain it at all, at room temperature. High hardenability is desirable in titanium alloys to be heat-treated to high-strength levels. Its value is by no means limited to large section sizes. With high hardenability, a material can be solution-treated and cooled at a variety of rates, either to give high strength directly or, more generally, to give a soft ductile condition from which high strength can be obtained by subsequent aging. With low hardenability, high strength can be obtained, if at all, only by very rapid quenching, and there will generally be little increase in hardness on subsequent aging; an alloy of this type is limited in its applicability. On the other hand, alloys of very low hardenability have some advantages in weldability; essentially, they are always in the annealed condition, after welding as well as before. For commercial alloys, hardenability data are usually available, in the form either of property data after cooling from the solution temperature at various rates, with or without subsequent aging, or of results of a standard hardenability test, such as that originally developed for steels by Jominy and Boegehold.' When modifications of an available alloy are considered, or preparation of new alloy compositions, it would be Very convenient to be able to estimate the hardenability of the new material without having to make and test it. A method of estimating hardenability of titanium alloys from their composition was suggested by one of the authors some time ago, on a preliminary basis, utilizing scattered data found in the literature.' It seemed worthwhile to carry out a systematic experimental study of the effect of composition upon hardenability. EXPERIMENTAL PROCEDURE Approximately fifty heats of various compositions, weighing 8 to 10 Ib apiece, were melted in a small inert-gas tungsten-arc furnace with water-cooled copper walls. The starting material was 110 Brine11 titanium sponge, with high-purity metals added for alloying. Each heat was bottom-poured under vacuum through a molybdenum burnout strip into a cold graphite mold, to form an ingot approximately 4-1/2 by 3-1/2 by 3 in.* From each ingot were cut *The material was melted and cast by Pitman-Dunn Laboratory, Frankford Arsenal, to whom the authors must express their thanks. two pieces 4-1/2 by 1-1/2 by 1-1/2 in. These were forged, at temperatures adjusted to the composition, into 1-1/4-in. rounds, from which standard 1-in.-diam hardenability specimens3 were machined. A number of small samples were also prepared from forged materials of each heat, annealed, quenched from various temperatures, and examined metallographically. The P-transus temperature was determined by observation of the degree of resolution of primary a in these pieces. samples for chemical analyses were also taken from the forgings. One hardenability specimen of each heat was solution-treated for 1 hr approximately 50°F above the measured transus temperature, and the other for 1 hr approximately 250°F above the transus. (An additional hour was allowed for the specimens to reach furnace temperature.) These are not necessarily the temperatures that would be selected for

Jan 1, 1964

By David V. Ragone, James A. Craig, Richard E. Balzhiser

The Gibbs free energies of formation of UC2 and UC were measured by equilibrating two-phase mixtures of UC2 + C and UC, + UC with liquid bismuth. The measured equilibrium concentrations of uranium in the bismuth combined with available activity coefficient information yielded uranium activities in these two-phase regions. Measurements on UC2 were performed over the range 1015 to 1160 K and on UC over the range 1115° to 1165°K. The values obtained for UC2 are in excellent agveement with values determined using combustton calorimetry and low-temperature heat capacity measurements. The UC values are in fair agreement with the calorimetric values, differing by about 10 pct from the calorimetric determination. MUCH interest has been shown in the uranium carbides in recent years because of their potential as nuclear fuels. As nuclear reactor operating temperatures have been raised to increase thermal efficiency, new fuels have been required. The uranium carbides are of interest because of their high melting points, >2000°C, high thermal conductivity, and resistance to irradiation damage. The manufacture and use of uranium carbides are aided by a knowledge of their stability and reactivity under various conditions. In this regard the thermo-chemical properties of the carbides, i.e., heat capacity, heat of formation, free energy of formation, and so forth, are particularly important. A great amount of work has recently been done on the thermodynamics of the U-C system. Unfortunately, however, there has not been good agreement among the various investigations. This study of the free energies of formation of uranium monocarbide and uranium di-carbide in the temperature region 1100°-1200° K was undertaken to help clarify the situation. It should be noted that in the temperature range of this investigation, 1100°- 1200° K, the thermodynam-ically stable phase in equilibrium with graphite is U2C3, not UC2, Fig. 1. However, U2C3 is reported to be stable only under extremely low oxygen and nitrogen pressure. Although UC2 is metastable below 150O°C, it exists under most experimental conditions. It should also be noted that "UC," never exists as UC2 but with compositions near UC1.9. However, "UC2" will be used to designate the dicarbide phase except when the stoi-chiometry is necessary for clarity. METHOD The approach taken in this study of the free energies of formation of UC and UC2 was to determine the thermo- dynamic activities of uranium in the two-phase regions UC, + C and UC + UC, by equilibrating the two-phase mixtures with the liquid bismuth. When a mixture of solid UC2 + C is brought to equilibrium with liquid bismuth, the reaction that occurs is: Neither carbon nor UC, could be detected as dissolved material in the bismuth. The standard free energy for this reaction may be written: In the two-phase region UC, + C, Fig. 1, the thermo-dynamic activities of UC2 and carbon are unity. The activity of uranium in this region was determined by measuring the concentration of uranium in a liquid bismuth melt in equilibrium with the two-phase mixture. This concentration was then used in conjunction with the activity coefficient data of uranium in bismuth reported by Tien et al.' to determine the activity of uranium in the two-phase region, UC, + C. All of the quantities in Eq. [2] were then known, and the AG; (uc,) was evaluated. UC + UC2. For the studies involving UC + UC,, the reaction taking place when the two-phase mixture is brought to equilibrium with liquid bismuth is: The standard free-energy change for this reaction is given by:

Jan 1, 1969

By W. R. Hibbard

The increased strength of a polycrystal-line metallic aggregate compared with that of its individual crystals generally has been associated with complex stress distributions at the grain boundaries resulting from atomic irregularity between grains. This disregistry, together with the necessity for adjacent crystals to deform compatibly regardless of the single crystal crystallo-graphic strain mechanism, complicates this mechanism so as to increase the metal's resistance to deformation. Although Taylor1 has shown from purely mechanical considerations the requirement for at least five active slip systems to absorb the complexities during the homogeneous deformation of polycrystalline face-centered cubic metals, experimental studies by Barrett and Levenson2 indicate that this is feasible only in a qualitative sense because of deviations from homogeneous deformation. Seitz and Read in their review3 state: " Unfortunately . . . present knowledge of the grain boundary influence is not sufficient to complement the work in single crystals and provide us with a good foundation for treating polycrystals." The purpose of this investigation was to attempt to clarify the gap between single crystals and crystalline aggregates by an analysis of the effects of dcformational stresses. Some of the results were described by C. H. Mathewson in his 1943 Campbell Memorial Lecture.zl Previous Investigations Since the performance of single crystals deformed under pure stresses has been relatively thoroughly investigated, the most significant researches are concerned primarily with deviations from single crystal behavior of large grained specimens. Qualitative grain boundary effects involving the observed amount of slip werc reported by Carpenter and Elam5 in 1921. Individual crystals in a two or three grained aluminum specimen deformed by tension acted in the normal manner described by Taylor and Elarn4 except for marked modifications at the grain boundaries. There the power to withstand deformation was considerably increased, leaving a ridge on the specimen where decreased slip occurred, often noticeable yi in. from the boundary. Adcock,6 Yamaguchi,' Seumel, Hirstg and others have also reported this phenomenon as a qualitative trend. Yet attempts by O'Neill'o and Ljunggrenll to measure a difference in hardness at grain boundaries in undeformed specimens were unsuccessful. Miller12 measured quantitatively the reduction in slip near the boundary between the single crystal and polycrystalline areas of zinc specimens. These effects consisted of two parts: I. Next to the polycrystalline interface thc distribution of stresses was so altered

Jan 1, 1949

ARTHUR PHILLIPS,* Bridgeport, Conn. (written discussion?).-It is to, be regretted that the very valuable paper by Messrs. Bassett and Davis did not appear in the early war period. The data presented would have been of inestimable service to inspectors, of cartridge brass who, admittedly, had little or no knowledge regarding the relation of grain size to temperature of anneal, and no real appreciation of, the significance of the Brinell hardness test. The paper is of considerable interest to, metallurgists also. WALTER R. HIBBARD, ? Bridgeport. Conn. (written discussion§).-The writer has carefully studied Messrs. Bassett and Davis's paper with considerable interest, inasmuch as our laboratory has tested cartridge brass by means of a Brinell machine. In March, 1917, at the suggestion of the Technical Department of the American Brass Co., we started a comparison of grain-size measurements and Brinell hardness of-cartridge brass with a gage of 0.1 in. or greater. This was continued until March, 1918, when we adopted the Brinell hardness test as standard for brass 0.1 in. gage or greater, and discontinued grain-size measurements upon this metal. The data collected during the test showed that the Brinell hardness indicated more accurately how the metal acted in actual working operations. It was also more reliable because two manipulators check themselves closer by the Brinell test than by the grain-size measurements. It also consumed less time in making the tests. Alfred V. de Forest, formerly assistant research engineer of our laboratories, has described the apparatus and some of the checking results in a paper read June, 1918, before the American Society for Testing Materials.1 The writer hopes that a more satisfactory. method for testing cartridge brass and gilding in gages thinner than 0.1 in. may be devised than the present method of grain-size measurements.

Jan 3, 1919