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By O. J. Hassel, W. T. Maidens, J. H. Calbeck

The rotary gas fired reheating furnace used by the American Zinc Oxide Co. at Columbus, Ohio for Therotarygasfiredreheatingfurnacerefining lead-free zinc oxide is described. The outstanding features of this operation are that the color of the zinc oxide is greatly improved, sulphur is eliminated, and cadmium arethatrecovered without densifying the product to an objectionable degree. IN 1919 Leland S. Wemple obtained a patent for a process of reheating zinc oxide wherein the "coarsening of grain due to excessive heating was avoided." He taught in his specification that if solid carbonaceous material, such as lamp black, was added to the zinc oxide in proper amounts prior to reheating, objectionable sulphur compounds could be removed and the color would accordingly be improved and no objectionable densification would occur because of the relatively low temperature required. The situation that made this invention imperative was the newly opened zinc oxide plant of the American Zinc, Lead & Smelting Co. in Hills-boro, Ill. This was one of the early Western Type American Process zinc oxide operations. Characteristic of all of these early Western operations using Tri-State and Western ores was the great difficulty encountered in obtaining a product low enough in sulphur to compete with the Eastern Type American Process zinc oxides which were made from ores containing very low sulphur percentages. Wemple demonstrated that the refining process of his invention produced a superior color and although this was true and a most welcome feature, the primary purpose of the early refining operations at Hillsboro was to reduce substantially the high sulphur content of the crude zinc oxide. Although many and varied attempts had been made for refining zinc oxide none of the processes had a commercial history of any consequence until Wemple's invention became standard practice for the American Zinc, Lead & Smelting Co. in 1919 and their operations have been unique in that substantially all of their lead-free zinc oxide has been reheated since the first installation at Hillsboro. This process has become known in the industry as refining. The furnace developed by Wemple and continued in use by the company from 1919 until 1943 was unusual and merits some consideration by way of review in this paper. The furnace was essentially a double hearth coal-fired muffle furnace with a mechanical raking system consisting of a central shaft supporting six rabble arms in each muffle. The untreated or "crude" zinc oxide was fed onto the outer rim of the top muffle, moved to the center where it dropped to the lower muffle and progressed to the outer rim where it was discharged into an alloy screw conveyor. The retention in this furnace was extremely short, about 5 min, and the shallow zinc oxide bed on the hearths of the muffles was being continuously turned by the fast moving rabbles. Soft coal was burned on the grates below the lower muffle and the long yellow flame necessary to carry the heat around both muffles resulted in a very inefficient combustion of the fuel. The temperature of the top of the lower muffle seldom exceeded 65 °C although the oxide itself often reached 700°C before discharge. The capacity of this furnace was approximately 1/2 ton per hr. In our plant at Columbus it was necessary to keep four of these furnaces running in parallel to take care of the production because, as mentioned above, every pound of zinc oxide produced during these 24 yr passed through one of these refining furnaces. An essential part of this refining operation was the use of carbonaceous material admixed with the zinc oxide fed to the furnaces. Between 1 and 2 pct of a bran produced in the processing of cotton seed was added to all zinc oxide charged to the furnaces. The bran ignited on the top hearth and was still burning when the charge fell from the top hearth to the bottom hearth making a cascade of sparks. The rapid turning of the zinc oxide caused these particles of bran to flash on the hearths behind each rabble; but the combustion, of necessity, had to be complete by the time the charge reached the outer rim of the bottom hearth, otherwise the finished product would be contaminated with the charred particles of bran which would give the zinc oxide an unsatisfactory color. Although this operation was initiated to reduce objectionable sulphur percentages, as time went on new properties of the product were appreciated which made advisable continuing the refining process long after other methods of sulphur reduction became known in the industry. The particle size and particle size distribution, the absence of colloidal fines and perhaps a unique surface condition gave this product an outstanding performance when used in paints. The Wemple furnaces installed in Columbus in 1919 had to be rebuilt frequently and were extravagant in the use of fuel. The raking mechanism and the muffles required excessive maintenance expense and as the furnaces wore out the problem arose whether to continue along this line or to explore the possibilities of obtaining similar or better results in the simpler and more commonly used rotary furnace. To this end special research was initiated in 1941 on a small laboratory rotary

Jan 1, 1951

PUGET SOUND SECTION SIMON H. ASH, Chairman, I. F. LAUCKS, Vice Chairman, CHARLES SIMENSTAD, Sec.-Treas., 425 Lyon Building, Seattle, Wash. GLENVILLE A. COLLINS, JOHN N. POTT. The Puget Sound Section met at the Arctic Club, Seattle, Wash., on Jan. 20, 1917. Sixteen members and five guests were present. Dinner having been served, the meeting was called to order. A letter from secretary of Associated Engineering Societies was read, requesting payment of this section's assessment to the quarterly budget, and upon motion it was voted that the Secretary-Treasurer be instructed to pay this assessment. It was moved and carried that this section join with the Chemical Society in a meeting. At the, close of the business meeting, Mr. Asa C. Baldwin gave an illustrated lecture on the "Alaska Boundary Survey." On Feb. 24, the Puget Sound Section again held a meeting at the Arctic Club, 16 members and three guests being present. Chester F. Lee, as member of a committee representing this section in the joint council of the Associated Engineering Societies, reported that by lots it had been decided that the term of service of said committee would be as follows: Chester F. Lee, two years; George. Watkin Evans, one year. Following adjournment of the business meeting, Prof. Joseph Daniels, of the University of Washington, delivered a very interesting lecture on "Milling Practice of The Alaska-Castineau Mining Company." CHAS. SIMENSTAD, Secretary.

Jan 5, 1917

[ ] For President-Elect Leo F. Reinartz has been nominated for the Presidency of AIME in 1954. Mr. Reinartz is now vice-president, special operating development, Armco Steel Corp. He was born in East Liverpool, Ohio, and graduated from the Carnegie Institute of Technology as metallurgical engineer. He joined Armco in 1909 as a chemist and then became open hearth foreman; assistant superintendent, open hearth dept.; superintendent, open hearth dept.; assistant general superintendent; works manager, East works; manager, Middletown div.; and assistant vice-president, successively. Mr. Reinartz has been active in many technical societies and delivered papers before several. He has been the recipient of the Alumni Award from Carnegie and holds life honorary membership in the AIME National Open Hearth Conference. One of the organizers of the National Open Hearth Conference, Mr. Reinartz was Chairman, Executive Committee (1927 to 1946) and is presently Chairman of its Finance Committee. In October 1951 he was an American Conferee at the First World Metallurgical Congress held in Detroit. An AIME member since 1925, Mr. Reinartz has been active on numerous committees of the Institute.

Jan 1, 1952

By E. S. Machlin

THE function of this paper is to present certain results based on the fact that the strain energy arising from the solution of out-of-size solute atoms into the solid matrix is free energy and not internal energy, and that this strain energy is almost wholly shear strain energy as Zener1 pointed out. One natural consequence of this fact is an expression for the excess entropy of mixing due to the strain energy. Also, a derivation of the integral molar free energy of mixing partitioned to strain energy will be made using the model of Lawson2 and thermodynamics. This derivation has the advantage of showing in a simple way the assumptions involved in Lawson's treatment. The excess entropy of mixing partitioned to strain energy can be derived in two ways. The first way makes use of the fact that the strain energy is almost wholly in the form of shear strain energy. In this case, as Zener1 pointed out, the change in entropy due to the addition of shear strain energy is to a first approximation given by ?S/?? p,T = - ?lnµ/?T p,? Hence, the excess entropy of mixing partitioned to strain energy will be given by Sx ? = ?S/?? p,T Gx ? = - ?lnµ/?T p,? Gx ? where, Gx ? is the relative integral molar free en- ergy partitioned to strain energy; S is the entropy; is the shear strain energy; µ is the shear modulus; T is the absolute temperature; p is the pressure; and ? is the shear strain. Zener,1 as well as others, has pointed out that the shear strain energy stored in a compressible isotropic solid due to the insertion of an off-size incompres-sible sphere into a spherical hole in the solid, is approximately given by 2/3 µ/O (O°I - O)2 where a is the volume of spherical hole and no , is the volume of sphere. If we now consider the introduction of one mol of such spheres into an infinite volume of solid, then the relative partial molar free energy excess due to strain energy alone is GM ? = 2/3 µ/v (v ° 1 - v)2 where v is the molar volume of solvent and v°1, is the molar volume of pure solute type 1. Let us consider that these spheres are the two types of atoms in a binary solution, then there will be a similar relation for solute 2. The total relative integral molar free energy excess due to strain is then, to the approximations stated above GM ? = GM ? x1 + GM2 ? x2 = 2/3 µ/v [(v ° 1 - v)2 x1 + (v ° 1 - v)2 x2]. Lawson's relation for the strain energy can be de-

Jan 1, 1955

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

Jan 1, 1923

By H. A. Schwartz

By analyzing cementite separated electrolytically from white cast iron of known composition and history, the distribution of silicon between austenite and cementite during and after freezing has been followed. The results constitute a contribution to our knowledge of equilibria in the ternary (metastable) system iron-carbon-silicon. Incidental information was obtained, also, with respect to the distribution of manganese, silicon, and phosphorus, when only relatively small amounts of each are present. The major conclusion of the paper is that during solidification, equilibrium is attained when the silicon is all rejected to the liquid phase, permitting silicon-free austenite to separate. OF THE outstanding investigators of the system iron-carbon-silicon, Gontermann,1 Charpy and Cornu-Thenard,2 and Honda,3 only the first touched on the chemical composition of the solid and liquid phases in equilibrium with one another. He concluded that his data did not permit a decision as to which of an indefinitely large number of pairs of compositions of liquid and solid would be found in any given case. If through the three dimensional equilibrium diagram of the iron-carbon-silicon system an isothermal plane is passed in the region of partial solidification, two lines of intersection with the liquidus and solidus, respectively, are obtained, also a point marking the alloys' composition. If, in this, plane, a straight line is drawn through the point, and intersecting both the liquidus and solidus isothermals, the two intersections mark a liquid and a solid alloy that may be chemically in equilibrium at the chosen temperature. From thermal data alone, Gontermann could not assign any particular direction to the line and, hence, could not determine which pair of conjugate points to choose.

Jan 7, 1924

THOSE MARKED THUS * ARE MEMBERS, MARKED THUS t ARE ASSOCIATES THESE SIGNS DOUBLED INDICATE LIFE MEMBERS AND ASSOCIATES RESPECTIVELY THE FIGURES AT THE END OF THE ADDRESS INDICATE THE YEAR OF ELECTION HEAVY FACED TYPE SIGNIFIES HONORARY MEMBERSHIP ` *AARONS, JULIAN B , Mine Supt, The Boulder Deep Levels, Ltd , Boulder, Western Australia, '05 *ABADIE, EMILE R, Cons and Min Engr, 1004 James Flood Bldg, San Francisco, Cal '76 *ABBE, CLEVELAND, JR, GeOl Aid, U S Geological Survey, Washington, D C '00 *ABBOTT, AI ARTHUR, Cerro de Pasco Mining CO , Cerro de Pasco, Peru, So America '95 *ABBOTT, ARTHUR V , Electrical Engr , Westinghouse, Church, Kerr & CO , 8 Bridge St, New York, N Y '82 *ABBOTT, CLARENCE E, Chief Min Engr, Care Fayal Mine, Eveleth, Minn '04

Jan 1, 1910

By H. Rees

This paper supplements and brings up to date a report prepared earlier this year and presented at the Eleventh Pan American Railway Congress in Mexico City. Most of the original report is contained in this paper in order to acquaint the reader with the project background. On December 1, 1961, construction of this locomotive was completed. Stationary testing started immediately, and a host of problems in various areas were uncovered. Many of these had no relation to the use of coal in a direct fired gas turbine. All of them emphasized the problems which plagued previous projects of this kind. In 1944 the Locomotive Development Committee of Bituminous Coal Research, Inc., was formed to study the problems of combustion, coal handling, and fly ash removal which would have to be solved before coal could be used to fire a gas turbine. By 1947 this committee was composed of the chief executive officers of nine eastern railroads and five eastern coal companies. All of the members of this committee were vitally concerned in a coal fired gas turbine because coal cost only one-fourth as much per heat unit as fuel oil. A number of research projects were started to develop and test components on a small scale. This included work at John Hopkins University, Battelle Memorial Institute, Institute of Gas Technology at Chicago, Purdue University, and Southern Research Institute. By 1946 a pilot plant had been installed at the Dunkirk, New York plant of Alco Products Div. of American Locomotive Co. The U. S. Bureau of Mines made available to the Locomotive Development Committee (hereafter called LDC) a Houdry process gas turbine plant, originally destined for a Russian oil refinery. The full scale pilot plant was used to evaluate the results obtained from the small scale studies under actual gas turbine conditions. Operation of this plant disclosed a number of problems which had not been discovered in the small scale tests. By 1951 four 250 hr tests had been conducted with the Houdry gas turbine to test out a variety of equipment. The major problem concerned the removal of abrasive fly ash from the products of combustion so that wear on turbine blades would not be excessive. The first 250 hr test showed that the original fly ash separating equipment was inadequate. Large ash particles passing through the turbine blading were nicking the leading edges of the first row blades. At the conclusion of the second 250 hr test, erosion was so severe that the first row of stator and the first row of rotor blades were replaced. At the end of the third 250 hr test, it was necessary to replace the first three rows of stator blading. The fourth test was used to test out a new design fly ash separator developed by LDC and named the Dunlab tube. This device gave more encouraging results than any of the others tested. Early enthusiasm for overcoming major difficulties had resulted in placing an order in 1946 with Allis-Chalmers Mfg. Co. for a 3750 hp regenerative gas turbine. The gas turbine, together with associated combustion and ash removal equipment, coal handling equipment, generators and gear reduction unit was installed at Dunkirk by 1951. A 750 hr test was made in 1952 with the LDC-Allis Chalmers gas turbine power plant. At the end of this test it was necessary to replace the first four rows of both rotor and stator blading. Rows 5 and 6 did not require replacement. In 1953 the American Locomotive Co. joined with LDC and assumed an active role in equipment development and manufacture. During 1954 LDC-Alco operated the rebladed gas turbine 300 hr to determine if a new fly ash separator was adequate. Performance of the improved separator was considerably better, but trouble was experienced with clogged blowdown lines from the Dunlab tubes. When these lines clogged it permitted the passage of abrasive particles. In 1955 a total of 1421 hr was run. This included 243 hr of cycle operation on Union Pacific coal from the D. O. Clark mine at Superior, Wyoming. During the 243 hr a total of 370 tons of coal was consumed. The purpose of this test was to determine if U.P. coal was suitable for use in a coal fired turbine. It was the unofficial opinion that it was as good or better than the eastern coals that had been tested.

Jan 1, 1964

1938 ABERNATHY, G E Feb 6, 1948 Min & Met Apr 1948 1937 ADAMS, ARMY Aug 20, 1949 Min Eng Dec 1949 1946 ADDY, GEORGE E Sept 24, 1950 Min Eng July 1951 1920 ALDERSON, WILTON P Feb 1951 Min Eng Sept 1952 1896 ALDRICH, T H , JR May 24, 1950 Min Eng Aug 1950 1942 ALDRIDGE, LEONARD June 8, 1952Jrn Met Sept 1952 1919 ALLEN, ROLLAND C July 18, 1948 Min &Met Sept 1948 1950 ANDERSON, C P Unknown Min Eng Feb 1951 1937 ANDERSON, JOHN H May 10, 1950 Min Eng Aug 1950 1914 ANDERSON, L DOUGLASS Unknown Min Eng Nov 1951 1948 ANDRAU, E W K Oct 20, 1951 1936 ANDREWS, CHARLES B Apr 19, 1950 Min Eng June 1950 1918 ARMITAGE, PAUL June 28, 1949 Min Eng Oct 1949 1924 ARMSTRONG, PERCY A E Jan 23, 1949 Min Eng May 1949 1906 ARNOLD, CHARLES LE NEVE Aug 7, 1949 Min Eng Oct 1949 1945 ARNOLD, HAROLD S Aug 7, 1950 Min Eng Oct 1950 1936 ASH, JAMES E Dec 17. 1949 Min Eng Apr 1950

Jan 1, 1952

By Roger M. Nendick

The recovery of precious metals from heap leach solutions can be accomplished by two processes: 1. The Carbon Adsorption Process 2. The Merrill-Crowe Zinc Precipitation Process A brief review of the relative process economics is made. Each process presents certain design considerations that must be addressed during the evaluation and engineering design for the project. Discussion is presented on the design criteria for each process.

Jan 1, 1984

By L. K. Jetter, C. J. McHargue

The use of axis charts for representing the texture of cold-rolled thorium sheet was compared with conventional pole figures. Four texture components were deduced from the axis charts and shown to be consistent with the pole figures. It was shown that consideration of the pole figures alone could lead to an apparent component which is the average of two actually present. It was also shown that the spread about the "ideal" textures and the amount of material associated with each could be readily obtained Fom the axis chart method. BECAUSE of the crystallographic nature of the deformation mechanisms in metals, plastic flow results in the alignment of certain crystallographic directions with the primary flow directions. In the study of the "preferred orientation" thus developed, one wishes to discern the distribution of the crystallographic directions with respect to some reference direction, usually a direction related to the fabrication procedure, such as the rolling direction. The pole-figure method, introduced by ever,' involves the plotting of the distribution of the poles of some family of planes on a stereographic projection which places the reference direction(s) at the north pole and/or in the center. By noting the angles between the reference directions and concentrations of poles on several such pole figures, one can deduce the crystallographic directions which are aligned with the reference directions. If the preferred orientation is relatively simple and well-developed, one to three pole figures may be sufficient for obtaining the desired information; if there are several texture components, more pole figures may be needed. A significant improvement in the method of representing the textures in wires and rods resulted from the introduction of the "inverse pole figure" or axis-distribution chart by Harris.2 Such a chart gives directly the distribution of the reference axis relative to the standard stereographic projection. There has been widespread acceptance of this method for the representation of fiber textures, and methods have been proposed for converting observed diffraction intensities into axis densities.2-6 The suggestion by Mitchell and Rowland3 and Jetter, McHargue, and williams5 that sheet textures could be represented as distributions of rolling, normal, and transverse directions have been criticized on the basis that they offer no significant advantage over a combination of two ordinary pole figures and that it has not been proved that sheet textures can be treated as quasi fiber textures.6 If the purpose of a texture determination is to study some property which is related to the orientation of a particular crystallographic plane or direction, then conventional pole figures certainly are sufficient. For example, the distribution of the slip planes in face-centered cubic metals (the (111) pole figure) serves to indicate the variation in mechanical properties of sheet. On the other hand if the study is directed at an understanding of the factors influencing texture formation, it is desirable to know not only the preferred orientation but the kind and degree of spread from it and the relative amounts of material in each component, if there are more than one. Axis charts give this information as well as the orientation distributions. Consider the procedure for deducing a texture component from a pole figure for the (111) planes

Jan 1, 1961

CHICAGO SECTION CHARLES H. MACDOWELL, Chairman, Luther V. DICE, Vice-Chairman, HENRY WT. NICHOLS,. Secretary-Treasurer, 164.5 E. 68 St., Chicago; Ill. ALEXANDER K. HAMILTON-, HENRY P. HOWLAND, GEORGE P. HULST, FREDERICK 1. SNYDER. There were 32 members present at the dinner of the Chicago Section which was held at the Chicago Engineers' Club on Friday Evening, December 22. At the meeting after the dinner, the Chairman called attention to the work of Mr. Hoover in Belgium and spoke briefly of the assistance which' could be given him through the Belgian Kiddies, Ltd. Mr. Alonzo Kinyon read a paper on "Burring Powdered Coal" which so interested the members that many of them participated in the long discussion which followed. Prof. Harry B. Pulsifier then described the metallurgical plants about Chicago. He mentioned briefly the equipment and interesting features of 30 metallurgical plants of importance and stated that there were also 200 foundries in the district. He said that when number, size, quality and diversity of the plants are considered, the Chicago District is justified in calling itself the greatest metallurgical center on earth. The paper was followed by a brief discussion in Which attention was called to some smaller and incipient plants of an interesting character. HENRY T. NICHOLS, Secretary.

Jan 2, 1917

By Alan Probert

IN his inaugural address in 1949, President Truman made a policy declaration which launched the foreign technical assistance program known to the world as Point Four. Congress passed Public Law 535 defining the scope of the program and holding activities to certain limitations. It also provided $34.5 million for the first fiscal year. The Technical Cooperation Administration was established within the Department of State to coordinate and direct a program to include "economic, engineering, medical, educational, agricultural, fishery, mineral and fiscal surveys, demonstration, training and similar projects." The mineral programs of Point Four have been staffed and managed by two agencies of the Department of Interior, the Geological Survey and the Bureau of Mines. The Geological Survey is concerned primarily with water-supply problems, the discovery of mineral deposits, and the determination of habit, shape, and grade of mineral deposits. The Bureau of Mines is concerned with determining the commercial potentialities of mineral deposits, mineral technology, and the production and distribution of mineral commodities. Mineral projects comprised only 1 pet of the first year's budget. In spite of the relatively insignificant expenditure compared to those for food, agriculture, and health, a commendable record has been achieved.

Jan 1, 1952

By Frederick T. Williams

The purpose of this paper is to discuss the relative merits of the large 31/8-in. machine and the small 2 1/4-in. tappet machine in driving development-headings; and although the data here presented were obtained from cross-cut headings alone, experience has shown that the results are equally true in drifting, raising and winzing. Recently we drove two parallel cross-cuts through the same formation, using a 3 1/8-in. machine at the breast of one crosscut, and a 2 1/4-in. machine of the same make at the breast of the other. The results of this work afforded an ideal comparison, since in both cases the headings were advanced through rock practically of the same hardness and breaking-properties, the amount of sludging was equal, and there was no difference in the condition of the steel or the machines, the air-pressure or the experience of the operating crews. Some operators in the Cripple Creek district contend that there is ground which cannot be handled with the small machine, the holes being too small to contain enough powder to "pull " the ground, etc. The results obtained in working the property of the Portland Gold Mining Co., however, show that the ground worked by them does not fall in this class. During a period of two years there have been driven, with the small machine, 4 miles and 308 ft. of development-headings, through a diversity of ground, including Pike's Peak granite (a coarsely porphyritic type of granite), highly indurated andesitic or pho-nolytic breccia, true massive andesite, trachytic phonolyte, tuffs, and along dikes of decomposed basalt and hard phonolyte. In every instance a satisfactory record was made. The headings here describe? mere driven through highly indurated andesitic breccia, having a hardness of from 5.2 to 7.2 and a sp. gr. of from 2.2 to 2.8. The action of the breccia under the drill was not materially different from that of ordi-

Jan 1, 1907

By AIME AIME

0 N March 5, at Carnegie Hall, Cleveland, the Ohio Section held a joint meeting with the Cleveland Engineering Society, and the local sections of the American Chemical Society, American Society of Mechanical Engineers, and the American Society for Steel Treating. Prior to the meeting there was an informal dinner attended by 50 men. Then followed an address, "The Principles of Corrosion Protection," by Ulick R. Evans, the well-known British specialist in this problem. There were 266 present, presided over by Zay Jeffries, president of the American Society for Steel Treating and a member of the Cleveland Engineering Society. The address was well received and some discussion followed

Jan 1, 1929

By Robert H. Richards, E. E. Bugbee

Friends often ask how accurate the work of our little stamp mill is, or express the opinion that a little mill cannot do good work. As a reply we would like to place on record the results of a few tests. There are two periods of work in our laboratory; the fall term, when the class collectively goes through all our chief laboratory-processes, and the spring term, when the students work up their theses, each electing some one process or investigation and devoting himself wholly, or almost wholly, to that. Some of the tests, the results of which are recorded in this paper, were made in the fall term; the preparation of the apparatus, the sampling and the assaying being done largely by assistants, with the aid of the students. Others were made in the spring term as thesis-work, and the results are due wholly to. the students. The complete " tree " of our process is patterned after the-

Jan 1, 1904

By P. R. Sperry, P. A. Beck, J. Towers

Dahl and Pawlek1 found that electrolytic copper develops extremely coarse grains at 1000°C after about 90 pct reduction by rolling. This coarsening occurs only under conditions of penultimate grain size, deformation, and alloying which lead to the "cube" recrystallization texture.l,2,3,5 The peculiar angular shapes and straight grain boundaries of the coarse grains were noted by several investigator.1,4,5 On the other hand, coarsening in Fe-containing aluminum or in AI-Mn alloys8 does not depend on a "cube" (or any well developed) recrystallization texture. It is true that increasing deformation by rolling, and, therefore, an increasingly well developed re-crystallization texture, are associated with decreasing incubation periods of coarsening.6-7-8 Nevertheless, coarsening readily develops in aluminum even after only 30 pct reduction by rolling, where the recrystallization texture is very weak.6,8 Also, coarsening was observed by Jeffries9 many years ago in sintered thoriated tungsten, which presumably has no preferred orientation. In all these cases coarsening is associated with grain growth inhibition by a dispersed second phase.8,9 The annealing temperature has to be suficiently high to overcome the inhibition at a few locations. But if it is too high, growth starts at many points, and the resulting grain size becomes much smaller.9 Normally, the coarse grains are more or less equiaxed, and the boundaries have a typical ragged appearance.6.8 Cook and Macquarie4 demonstrated that, in addition to the texture-dependent coarsening previously found at 1000°C,l electrolytic tough pitch copper may also coarsen at 800°C after 50 pct reduction by cross rolling. The coarse grains formed under such conditions have rounded shapes and ragged boundaries, like those in aluminum. When the annealing temperature is higher, the tendency for their formation decreases. All these observations suggest that the coarsening at 800°C is associated with inhibition by a second phase. Actually, coarsening at 800°C after 50 pct reduction by cross rolling was observed only in tough pitch copper,4 which contains Cu2O particles. On the other hand, the texture-dependent 1000°C coarsening occurs in both tough pitch and oxygen-free copper;4 it does not appear to depend on the presence of a dispersed second phase. However, the interpretation of the 800°C coarsening in Cu after 50 pct rolling as an inhibition-dependent process, similar to the coarsening in A1-Mn alloys, is somewhat weakened by the fact that this coarsening was reported4 to occur only after cross rolling, and not after straight rolling. It was, therefore, decided to re-examine this question. A 1 in. diam electrolytic tough pitch copper rod, No. 2 hard drawn, was annealed for 20 min at 700°C, rolled to 0.5 in., annealed 10 min at 700°C, and straight rolled to 0.064 in. It was then given a penultimate anneal of 20 min at 500°C and it was cut into four sections, which were given final reductions by straight rolling as follows: A 30 pct reduction of area B 50 pct reduction of area C 70 pct reduction of area D 90 pct reduction of area Specimens cut from the four sections were finally annealed at 800°C in an oxidizing atmosphere. Strip A remained fine grained up to 10 hr, but the specimen annealed 12 hr consisted of only 2 large grains. Strip B had a few scattered large (1/2 to 3/4 mm) grains after 1 min, although the balance of the specimen consisted of fine grains of about 0.02 mm. After 5 min there were several 10 to 15 mm grains present, and after 1 hr strip B was completely coarsened. The coarse grains had the same characteristics (see Fig 1) as those obtained by Cook and Macquarie at 800°C after cross rolling. Strip C had several grains of 0.05 to 1 mm after 1 min, but it was still largely fine grained after 12 hr. After 48 hr it consisted entirely of grains of about 0.5 to 4 mm, with an extraordinarily large number of twin bands. Strip D remained com- pletely fine grained after 4 hr at 800°C. These results indicate that, in the deformation range of 30 to 70 pct reduction, the incubation period for coarsening as well as the rate of growth and the final size of the coarse grains decreases with increasing deformation. Similar

Jan 1, 1950

By H. N. Lawrie

Introduction. THIS study was undertaken on account of the lack of definite knowledge concerning the influence of bismuth on wire-bar copper, and the small elimination of bismuth from copper-matte during the smelting-operations. The early workers who studied the influence of bismuth on copper confined their investigations to malleability and ductility-two physical properties which are related to the others so intimately that their determination is of primary importance. Karsten ' and Levol,2 using bending- and mealleability-tests, seem to have been the first to take up the subject, and while their results are incomplete, they agree in the main with the later work of Hampe.3 The bending-tests used by the first investigators consisted in bending the specimen until it failed. The malleabilitytests were made by beating the material to a knife-edge with a hammer. Hampe not only determined the percentage of bismuth which would cause red-shortness and cold-shortness of the alloy, together with other influences of bismuth on the malleability and ductility of copper, but also took up the influence of the bismuth protoxide, BiO, on copper, and of bismuth sesquioxide, Bi2O3, on the copper protoxide, CuO. Hampe's conclusions of the influences of these two latter compounds of bismuth on copper are as follows "If the protoxide of bismuth be alloyed with metallic copper, it is not changed to metallic bismuth, but remains mechanically distributed throughout the copper.

Sep 1, 1909

By R. K. Buhr, H. Thresh, M. Bergeron, F. Weinberg

The microsegregation of nickel and chromium in directionally solidified AISI 4340 steel castings has been measured using electron probe microanalysis. Minimum concentrations were observed to occur at the center of the dendrite stalks, as reported previously. However, the position of the maximum concentrations could not be determined from the dendrite configuration. An etching technique has been developed which shows the position of maximum concentration. Measurements were made of the distribution of nickel and chromium in the dendritic structure. The ratio of maximum to minimum concentration was determined as a function of primary dendrite arm spacing for both as-cast and partially homogenized materials. The results are compared with observations reported in the literatuve. A S part of an investigation of solute segregation in directionally solidified AISI 4340 steel casting, electron probe microanalysis was used to measure the distribution of nickel and chromium in the dendritically segregated material. This complemented the observations on the segregation of radioactive phosphorus obtained by autoradiographic techniques in the same castings.' Kattamis and I?lemings2 have reported similar measurements, using electron probe microanalysis, on dendritically segregated AISI 4340 steels. They found minimum solute concentrations occurred at the center of dendrites, maximum concentrations occurred in the center of interdendritic regions, for symmetrically oriented dendrites, and a regular variation of concentration within dendrite arms. The ratio of maximum to minimum concentration was found to be essentially independent of position in the castings, except near the chill surface where it was somewhat higher. Assuming complete diffusion in the liquid and no diffusion in the solid during freezing, they considered that isoconcentration curves in the steel were homothetic. As a result, isoconcentration curves of the various elements, contour surfaces of dendrites produced by isothermal-transformation studies, and the contour of the solid-liquid interface would all be similar, and could be superimposed by a uniform expansion or contraction of the contours. Preliminary results of the present investigation suggested that isoconcentration curves were not homothetic. It was also evident that points of maximum concentration could not be predicted from the dendrite configuration. Since the ratio of maximum to minimum concentration appeared to be an important parameter in defining the overall segregation in a casting, other techniques for determining the point of maximum concentration were investigated. In addition the overall solute distribution associated with the dendritic structure was examined for both nickel and chromium, and the consistency of the distribution for neighboring dendrites was determined. METHOD Fifty-pound heats of AISI 4340 steel were cast in a manner similar to that used by Flemings et al3 with a water-cooled copper base plate and exothermic sides and top. The nominal composition of the material was C, 0.41 pct; Mn, 0.66; Si, 0.35; S, 0.012; P, 0.010; Ni, 1.88; Cr, 0.95; Mo, 0.28. The steel solidified directionally from the chill surface, with a dendritic structure which increased in dendrite arm spacing with increased distance from the chill. Results of the general investigation of the cast structure and segregation of radioactive phosphorus in these castings have been reported elsewhere.' For the present measurements, sections were cut from the casting at several distances from the chill surface. The sections were subsequently heat-treated, mounted, and then polished on a plane perpendicular to the general freezing direction of the casting. Electron probe microanalysis was carried out with the JEOL-JXA3 microprobe using a voltage of 25 kev and beam current of 0.15 µa. The take-off angle is 22 deg. Quartz crystals were used in the spectrometers and measurements made for Ka radiation from both nickel and chromium simultaneously. A thin layer of carbon was deposited on all specimen surfaces prior to examination in the microprobe. Early measurements were made on polished surfaces, with indentation marks produced by a hardness tester to indicate the area of interest. It was found desirable to use etched surfaces, as opposed to polished surfaces, to reduce sample preparation time and more readily relate the microprobe scan to the structure. To determine if this could be done, without introducing significant errors, a series of measurements were made on polished and etched surfaces of the same specimen. Both polished and etched surfaces produced similar results within normal scatter as shown in the observations. Subsequent measurements were then made on etched surfaces. Measurements with the microprobe analyzer were made by point counting, for periods of 100 sec, at 10-µ intervals. Ten-second counts were made on pure nickel and chromium standards, incorporated in the specimen mount before and after each set of measurements. The results were adjusted for background, then corrected for dead time using the expression:

Jan 1, 1969

By K. C. Li

TITANIUM, because of its high strength, weight ratio, and high melting point, became the metal of the jet age. Zirconium, because of its low neutron cross section and high corrosion resistance to hot water, became an integral part of the nuclear era. Since both metals are very similar chemically, more or less the same process is used for their production. The sudden rise of this new industry of titanium and zirconium seems to have caused some uncertainty as to the future development of processes for making these metals. Although zirconium was discovered in 1789 and titanium in 1790, it was not until 1945, six years after W. J. Kroll patented his process, that F, S. Wartman of the U. S. Bureau of Mines perfected the technique of producing ductile titanium, and it was not until 1946 that Kroll perfected the technique of producing ductile zirconium in commercial quantities. Since then the Government and private industry have spent millions of dollars each year constantly searching for new methods, with the hope that some day titanium can be produced as economically as aluminum and magnesium or as cheaply as stainless steel.

Jan 11, 1957