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By R. L. Smith, J. L. Rutherford

ZONE refining, as developed by W. G. Pfann,1 has been used extensively for the purification of semiconductors. This method has made it possible to obtain the extremely high purity material necessary for the transistor industry. It has also been utilized to some extent for the purification of relatively low-melting-point metals. However, very little attention has been given to reactive, high-melting-point materials, with the exception of silicon. For this element, it has been necessary to use the floating zone technique in order to avoid contamination from the crucible containing the melt. The method is one in which a narrow molten zone is formed in a vertical rod by induction heating. The molten zone is supported between the two solid sections of the rod by surface tension. It is then moved longitudinally along the rod in order to effect a redistribution of solute. This technique has an advantage over the horizontal boat method, since crucible contamination is avoided. It has the disadvantage of being a much more difficult technique than zone refining in a crucible. Furthermore, it is necessarily a slow process, since only one zone at a time can be formed. However, the floating zone process offers a means of obtaining high-purity metals that are either not available, or can only be obtained in powder or pellet form as the result of complex chemical or electrochemical methods. It should be emphasized that the process is not effective in removing all impurity elements. Those that cannot be redistributed in an ingot during zone melting must be removed by some other means. Very little is known of the prope~ties of very high purity reactive metals such as iron, titanium, zirconium, beryllium, etc. It is quite likely that trace elements in such metals can affect their properties drastically. Therefore, one of the primary objectives of this work is to study the properties of metals which have been obtained in the purest form available and then zone refined. Trace elements can be introduced in a variety of ways, such as by inserting wafers between solid portions of the ingot to be melted, by placing the

Jan 1, 1958

By D. R. Hay, E. Scala

Electrotransport has been superimposed on the rate-limiling- step in zone refining which is the impurity diffusion through the liquid at the solid/liquid interface. The efficiency of zone refining is increased and relative resistivity ratios (P300°k/P4 2°K) he increased by 50 pel in tungsten for a given number of posses using- the electrotransport field-aided method. The effiect of zotze refining in the presence of an electric field on the relative resistivity ratio is examined as a function of its intensity and polarity. THE effect of electrodiffusion on the effective distribution coefficient of zone refining has been discussed by Pfann and Wagner.' Control of the distribution coefficient in zone refining is of twofold interest. A distribution coefficient of unity can be increased or decreased, making possible the transfer of some previously inseparable solutes. The general efficiency of zone refining can also be increased. In the conventional zone-refining process impurities are removed by their retention in the molten zone and subsequent deposition at the end of the rod after a complete passage of the zone. In higher-melting-point systems a second mechanism may also operate, the volatilization of impurities from the molten zone. It has been suggested by schadler2 that, in refractory metals, vacuum distillation plays the predominant role in purification. In Koo's results,3 the resistivity ratio decreased beyond a zone-refined length of 6 in. from the starting end, indicating that some purification does in fact occur by true zone-refining action. Hay and scala4 showed that the degree of purity as measured by the relative resistivity ratio method depends on the square root of time in the molten zone (number of passes) and thus appears to be limited by diffusion in the boundary layer at the solidifying interface assuming good mixing in the body of the molten zone where a linear rate would prevail. The final concentration of impurities in electron-beam floating-zone purification depends very much on the operating conditions and results obtained by various investigators2,3,5 are difficult to correlate. The diameter of the starting material, operating vacuum, and rate of traverse are among the factors to be considered. There are, nevertheless, some general observations to be obtained from the literature. Lawley5 reviewed the literature up to 1962 and concluded that the major contaminants generally remaining in tungsten after electron-beam zone refining are molybdenum and carbon. Molybdenum due to its high melting point and distribution coefficient of nearly unity would be expected to be difficult to remove by either volatilization or zone refining. Carbon is not only a common contaminant in vacuum systems, but is also very difficult to remove by conventional vacuum melting. even with vacuums of 10-7 mm Hg. For each of those impurities removed by zone refining the equation of Pfann and Wagner may be applied: It relates the effective distribution coefficient k to a superimposed driving force which accelerates the solute away from the interface with a terminal velocity L" and to the more conventional zone-refining parameters; v = rate of traverse, t = thickness of the diffusion layer at the solidifying interface, D = diffusivity of the solute in the molten zone, and ko = equilibrium distribution coefficient of the impurity.

Jan 1, 1965

By R. L. Fullman

Relationships are derived between average dimensions measured on a polished cross section and the spatial dimensions of particles dispersed as uniform cylinders. The equations are applicable to the measurement of rods or plates without the stipulation that they be extremely thin. QUANTITATIVE analysis of the elements of mi-crostructures has been limited by a lack of knowledge concerning the relationships between observations on plane surfaces and the spatial nature of the structure. This paper is an extension of previous efforts to establish equations suitable for the quantitative investigation of microstructures. The equations derived fill two gaps in the range of particle shapes for which measurements may be required, namely those shapes lying between extremely thin plates and equiaxed particles (approximately spherical), and those intermediate between equiaxed particles and extremely thin rods or needles. In a previous paper' equations were developed relating dimensions measured on a polished cross section to the average spatial dimensions of particles in the form of spheres, extremely thin plates, and extremely thin rods. For extremely thin rods the dimensions measured on a polished cross section were found to depend on the radius only, so that no information concerning the rod lengths or number of rods per unit volume could be obtained from observations on a cross section. In this paper equations are derived relating dimensions measured on a polished cross section to the spatial dimensions of particles in the form of identical cylinders. These equations may be used to evaluate the dimensions of rods, as well as the dimensions of plates, without the stipulation that the plates or rods be extremely thin. The impossibility of evaluating the length of extremely thin rods from planar measurements appears as an increase in the amount of data required for a given precision, as the length-radius ratio increases. Consider a sample containing particles of a phase in the form of cylinders of uniform radius T and height t. If the cylinders are randomly oriented, as in a sufficiently large sample of a fine grained poly-crystalline material, area and lineal analysis may be carried out with parallel cross-sectional planes and lineal traverses. If the cylinders are not randomly oriented, it is necessary to randomize the orientations of the cross-sectional planes and traverse lines. Let a unit cube be cut from the sample, and a cross-section plane be passed through the cube parallel to one of the cube faces. The number of particles N, cut by the cross-sectional plane per unit area is equal to the number of particles N, per unit volume times the probability p1 of a plane intersecting a single randomly positioned and randomly oriented cylinder in the cube. Let J be the maximum cylinder dimension in the direction normal to the cross-section planes, as shown in Fig. 1. Since, of the various possible positions for the cross-sectional plane over the unit length from top to bottom of the cube, only those positions existing over the length J

Jan 1, 1954

By C. H. Mathewson

EXCEPTING the joint sessions on gases in metals held during the day on Tuesday, the Institute of .Metals opened its activities with a division dinner at the Commodore on Tuesday evening, with Sam Tour, retiring chairman, presiding. W. M. Corse, secretary-treasurer, outlined the financial status of the division and stated the investment fund is becoming large enough so that in the near future it will be possible to pay all expenses of a foreign lecturer once in two years and not rely on an extended speaking tour to cover expenses. W. B. Price reported on his attendance at the Zurich, Switzerland, meeting of the International Society of Testing Materials and gave a graphic account of his visit to the Grand Salon, his meeting with Mussolini, and his audience with the Pope. Buffalo was announced as the place of the fall meeting, to be held during the week of Oct. 3.

Jan 1, 1932

By Charles S. Barrett

There is a road into the microscopic realm that has remained untraveled through all these years of intense activity with high-power optical and electron microscopy. The road is worthy of careful scouting by metallurgists and other investigators, for it leads into relatively new country and it makes some areas accessible that heretofore could be reached only by very indirect paths or by the use of imagination. And when the road passes through familiar territory it frequently permits a new view of commonplace things that should prove of value from time to time. An accepted way to interest people in new sights such as this is to present an illustrated travelogue. This I propose to do, using many pictures taken in my recent exploration of this road. In the manner of travelogues, I shall touch briefly upon a large number of different subjects in physical metallurgy and shall attempt to give an exhaustive treatment of none, for the objective is to provide a means for further research, to interest others in it, and to indicate what appears at the moment to be profitable directions for it to take. The method I shall present involves X-rays, but does not make use of the usual accompaniments of X-ray research such as reciprocal lattices, Fourier series, or the stereographic projection. The method is so simple in its fundamentals that it could have been developed 2o years ago, or perhaps even 30 years ago. It is well to have a destination for our travels, so that when we are through we shall have explored some region of importance, despite our preoccupation with the novel means of transportation and our interest in the sights to be seen along the way. So let us name the Cold-worked State as our destination, and make side trips into the territories known as Recovery, Recrystallization, and Precipitation-hardening. A great many investigations have been made of the nature of cold-worked metal, and a great variety of methods used, many of which are indirect, such as X-ray line intensities, X-ray line widths, calori-metric measurements, and magnetic measurements. Since comprehensive reviews of these investigations have been published in recent years, they need not be discussed here. The investigations that were the direct forerunners of the present work should be first mentioned. In 1931 I became interested in the structure of individual spots in X-ray diffraction patterns.l When a crystal is placed in the narrow pencil of X-rays in a Laue camera, the spots recorded on the film are not always uniformly black, but may have an internal structure. The meaning of this may be understood from Fig. I, which represents a narrow beam containing X-rays of many wave lengths (''general radiation") penetrating a crystal in the direction of the arrow and forming a pattern on the vertical film at the right.

Jan 1, 1945

By AIME AIME

THE Institute of Metals Division of this Institute held a joint meeting with the American Foundry- men's Association on Oct. 5-9, at Syracuse, N. Y. The registration at this meeting was about 150. There were four meetings in all, three of which were in con- junction with the American Foundrymen's Association. This combination works out very nicely and gives the I Division a number of practical foundry papers that it would not get otherwise. The sessions were well attended and the discussion was active. The session on Monday morning was of a general nature and consisted of the following subjects : " Refractory Problems in the Non-ferrous Electric Furnace Casting Shop, " "Temperature Control of Non-ferrous Alloys," "Atomized Coal System of Non-ferrous Melting," "Material Handling in a Brass Foundry." On Tuesday morning, the session was on "Aluminum and Its Alloys." The paper on permanent mold castings created a large amount of discussion, in fact so much that it had to be renewed after the close of the regular program. Aluminum is assuming a more important place every year and adds greatly to the program as a whole. One of the most remarkable meetings that this Division has ever had was held on Tuesday at noon in the form of a Round Table discussion, headed by G. K. Elliott, chairman of the Division, Cincinnati, Ohio. Mr. Elliott divided the members present, numbering about 80, into groups as they were seated at the tables. Each of these groups suggested a topic for discussion. They were as follows : "Fluxes on Market ;" "Simplification of Alloys;" "Pyrometric Control;" "Effect of Gas- sing Metal and Control;" "Barium Sulfate Added to Electric Furnace to Create Slight Oxidation to Remove Aluminum and Silicon;" and" Nickel in Brass."

Jan 1, 1925

By E. A. Anderson

THIS seems to be the year for superlatives in A.I.M.E. meetings. The programs of the various Divisions and Institute committees offered an abundance of interesting and valuable information in the form of technical papers, symposia. and lectures to large and interested audiences. The Institute of Metals Division may hold up its head with pride for its own program. With six technical sessions, three full-day symposia, and the annual I.M.D. dinner, four meeting days were not enough and many simultaneous sessions were required. The quantity and quality of the paper were equaled by the numbers and interest of those attending.

Jan 1, 1944

THE papers presented by the Institute of Metals at the Detroit meeting in September, 1926, and the New York meeting, February, 1927, will be issued soon in one volume and mailed to all members of the Institute of Metals Divi-sion of this Institute. The, annual lecture given by Cecil H. Desch will begin the volume and the discussion occurring at the sessions, as well as subsequent written discussions, will be appended to each paper. The volume will contain about 600 pages, and will be sent without charge on request to any member of the Institute. The pre-subscription price to non-members is $5.

Jan 4, 1927

By F. H. Spedding

From thermal, metallographic, X-ray, dilatometric, and electrical resistance data a Phase diagram is proposed for the La-C system. TWO compounds are formed, body-centered-cubic Laz C, having a large range of solid solubility, and body -centered-tetrago-nal Lac2 . The former melts incongruently at 1415°C, and at 25OC it has an electrical resistivity about two and one-half times that of bure lanthanum. The latter melts congruently at 2356°C and at room temperature has an electrical resistivity about equal to that of bure lanthanum. The addition of carbon to La lowers the melting Point of La about 115' C, raises the higher (B-Y) transfomzation about 10" C and appears to have no effect on the lower ( a-0) transformation. The addition of carbon appears to lower the oxygen content in the metal and improve the machinability; however, the tendency to oxidize is increased. Two eutectics are formed in the system. The first occurs at 2.2 pct C and melts at 806" C, while the second occurs between Lac2 and C with a melting point of2271"C. PETTERSSON,~ in 1895, was the first to prepare lanthanum dicarbide by heating the oxide with carbon in an electric furnace. He showed that this yellow, crystalline but brittle carbide had a formula corresponding to LaCz and that it reacted with water with the evolution of hydrogen and hydrocarbons and the formation of the hydrated oxide. Von Stackelberg's investigation of the crystal structure of the MCz carbides showed that the lanthanum dicarbide is of the tetragonal calcium dicarbide-type structure. He found the lattice parameters were a = 3.92 and c = 6.56.* Bredig,' using X-ray methods, showed that the room-temperature form of lanthanum dicarbide is stable up to 1750 °C and that above this temperature it transformsoto a face-centered-cubic structure, a = 6.0 ± O.lA, probably of the pyrite, FeSzstruc- typ? The reported discovery of two new cerium carbides, suggested that a corresponding face-centered-cubic lanthanum monocarbide and a body-centered-cubic lanthanum sesquicarbide might exist. This paper describes work on the lanthanum-carbon system which is part of a study of the rare earth metals and their alloys now in progress in this laboratory. EXPERIMENTAL PROCEDURE Source of Materials—The lanthanum metal was prepared at the Ames Laboratory by metal1o;hermic reduction of the fluoride with calcium metal. The results of spectrographic and chemical analysis indicated the presence of 0.01 pct Y, Al, Cu, Fe, and Si; 0.02 pct Ca and Mg; 230 ppm C; and 115 ppm N. The carbon used was of two types: 1) "National Special Graphite Spectroscopic Electrodes," and

Jan 1, 1960

By TRUMAN S. FULLER

THE GREAT INTEREST in decomposition and trans- formation, so evident in the study of alloys during the last two years, was reflected in the many papers on this subject, presented at the first session of the Institute of Metals, Tuesday morning. Dr. F. A. Thomson, of Montana State School of Mines, presented the first paper by C. Wilson, H. F. Silliman, and E. C. Little, "Rate of Precipitation of Nickel Silicide and Cobalt Silicide in the Hardenable Copper-nickel-silicon and Copper- cobalt-silicon Alloys." Dr. R. F. Mehl, in discussing this paper, stated that the title was somewhat deceptive, as it indicated that the rate of precipitation is determined; the method used is a measurement of electrical conductivity and hardness, neither of which is suitable for a quantitative measurement of rates of reaction or precipitation in the solid state. Hardness is also uncertain because it depends so much upon particle size. Of the various methods proposed for the study of rate of reaction and precipitation the evaluation of volume of reaction produced from the area of photomicrograph is the best.

Jan 1, 1933

Jan 1, 1934

By AIME AIME

THE Institute of Metals held a well rounded out symposium on the working of metals, distributed over two sessions. At the first session* four papers were presented, two dealing with the, cold working of metals and alloys and two with the hot working of non-ferrous alloys. The first paper by E. V. Crane, dealt with "Metal Working in Power Presses." Mr. Crane pointed out the empirical nature of engineering data available for use in calculating the probable stresses developed and power requirements, for the shearing, drawing, binding and other forming operations. He described the various operations, methods of determining stresses developed and presented data obtained. In the discussion C. F. Hammond took exception to Mr. Crane's objections to the rather too frequent. annealing operations in drawing of cartridge cases, pointing out that the material was-manufactured to meet specified structure and physical requirements, which could only be met by carefully controlled sequences of working and intermediate annealing operations.

Jan 1, 1931

By AIME AIME

AT Williams College, in the quaint old New England town where people still go to the post office for their mail, an interesting institution has come into being as one of the aftermaths of the peace conference at Paris in 1919. The war taught the world many things about economics although much remains to be learned and more to be appreciated. B. M. Baruch, H. A. Garfield, president of Williams, and others who took part in the conference at Paris or in preparation for it, feeling that benefits would accrue from informal friendly discussion of the problems that lead to political differences between peoples, called together a summer conference in 1920. This has now become an annual affair and is coming to be looked upon as an important center for developing and stimulating public opinion. Membership in the Institute is by invitation and the lists change to correspond with the particular subjects taken up. Each year a number of distinguished foreign public men are invited to be the guests of the Institute and to meet men and women from various parts of the United States interested in their special subjects. Round tables, general conferences, and public lectures are the means employed to bring out discussion. The first are organized by groups, each including usually 25 to 40 people interested in a special subject and meeting three times a week for informal discussion. Teachers, writers, economists, engineers, business men, indeed men of all vocations and many shades of opinion, are brought together. Once a week each round table presents in general conference with the members of all other groups the more general conclusions reached in its own decisions. Afternoon and evening lectures are given by the foreign guests and these are open to the public. The lectures and the general conferences are reported widely in the press but the proceedings as a whole are not printed, no resolutions are passed, and no action is taken or contemplated. The whole plan is to furnish a forum for free discussion in hopes that the difficulties of various groups and peoples may be taken up sympathetically and good understanding promoted. There is no creed, doctrine or dogma to which the Institute is committed and widely different views are currently presented. The constant effort is to bring out points of view and the reasons for them rather than to build up convincing arguments favourable to a specific action

Jan 1, 1926

At its meeting on February 21, 1933, the Board of Directors passed the following resolution defining and expressing the policy of the Institute with respect to official participation or action in controversial matters: WHEREAS, the Board of Directors at its last meeting passed the following resolution: "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candidates for public office, the following statement of policy is formulated: "Whereas, the American Institute of Mining and Metallurgical Engineers is organized for purely professional and scientific purposes, and whereas diversity of opinion among its members on partisan or political questions is inevitable, it is the expressed policy of the Institute to refrain from official participation or action in political and semi-political matters." AND WHEREAS, appeals for additional advice have been received: NOW, THEREFORE, IT IS RESOLVED: (1) That the policy of the Institute is to refrain from official participation or action in controversial non-technical economic subjects; further (2) That if any Local Section is in doubt as to the application of this policy to any particular subject, it should communicate with the Secretary of the Institute for advice.

Jan 1, 1940

At its meeting on February 21, 1933, the Board of Directors the following resolution defining and expressing the policy of the Institute with respect to official participation or action in controversial matters: WHEREAS, the Board of Directors at its last meting passed the following resolution: "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candidates for public office, the following statement of policy is formulated:

Jan 1, 1941

At its meeting on February 21, 1933, the Board of Directors the following resolution defining and expressing the policy of the Institute with respect to official participation or action in controversial matters: WHEREAS, the Board of Directors at its last meting passed the following resolution: "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candidates for public office, the following statement of policy is formulated:

Jan 1, 1936

At its meeting on February 21, 1933, the Board of Directors the following resolution defining and expressing the policy of the Institute with respect to official participation or action in controversial matters: WHEREAS, the Board of Directors at its last meting passed the following resolution: "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candidates for public office, the following statement of policy is formulated:

Jan 1, 1934

At its meeting on February 21, 1933, the Board of Directors passed the following resolution defining and expressing the policy of the Institute with respect to official participation or action in controversial matters: WHEREAS, the Board of Directors at its last meeting passed the following resolution : "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candidates for public office, the following statement of policy is formulated;

Jan 1, 1934

At its meeting on February 21, 1933, the Board of Directors passed the following resolution defining and expressing the policy of the Institute with respect to official participation or action in controversial matters: WHEREAS, the Board of Directors at its last meeting passed the following resolution: "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candidates for public office, the following statement of

Jan 1, 1938

At its meeting on February 21, 1933, the Board of Directors passed the following resolution defining and expressing the policy of the Institute with respect to official participation or action in controversial matters: WHEREAS, the Board of Directors at its last meeting passed the following resolution : "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candidates for public office, the following statement of policy is formulated: "Whereas, the American Institute of Miming and Metallurgical Engineers is organized for purely professional and scientific purposes, and whereas diversity of opinion among its members on partisan or political questions is inevitable, it is the ex- pressed policy of the Institute to refrain from official participation or action in political and semi-political matters."

Jan 1, 1946