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By Howard Martens, Pol Duwez

IN two papers published in 1949, alloys of chromium with the refractory metals tungsten, molybdenum, tantalum, and columbium were investigated in view of their possible use as high temperature resisting materials. For the Cr-Ta system, a partial phase diagram was presented and the only intermediate phase was identified at Ta2Cr3. A phase of the same composition was also observed in the Cb-Cr system. The X-ray diffraction data presented in these papers, however, were insufficient for crystal structure determination. It is shown in the present study that the only intermediate phase in both the Ta-Cr and the Cb-Cr systems corresponds to the ideal stoichiometric ratio TaCr2, or CbCr2. Both structures are cubic, MgCu, type. At high temperature, however, TaCr2 has a hexagonal MgZn, type structure, which can be retained at room temperature by fast cooling. The alloys were prepared by melting in a helium arc furnace on a water-cooled plate. The design of the furnace was essentially the same as that described in ref. 3. Some alloys were also obtained by sintering compacts made of the mixed powders pressed at 80,000 psi. The sintering was carried on for 4 hr at 1375°C. The tantalum and columbium powders were supplied by Fansteel Metallurgical Corp., North Chicago, 111. The tantalum powder was the reagent grade, with a particle size smaller than 400 mesh and a total impurity content less than 0.1 pct. The columbium powder was smaller than 325 mesh and contained approximately 0.1 pct C and traces of Fe, Ti, and Zr. The electrolytic chromium powder from Charles Hardy, Inc., New York, was smaller than 300 mesh and contained about 0.1 pct Na, 0.05 pct Ca, and traces of Cu, Al, Mg, Si, and Co. Powder diffraction patterns were obtained with a 14.32 cm camera, using copper Ka radiation filtered through nickel foil. The powder pattern of the TaCr2 alloy obtained by sintering at 1375'C was different from that obtained on the same alloy rapidly cooled from the melt. Contrary to this result, the powder pattern of CbCr2 was the same, whether the alloy was made by sintering at 1375°C or by melting, and was similar to that of the TaCr, sintered. It was also found that the structure of the TaCr2 specimen obtained by melting was retained after heating for 4 hr at 1590°C, but transformed into the structure found in the sintered specimen after heating for 4 hr at 1375°C. Hence, the structural change of TaCr2, appears to be a reversible polymorphic transformation. CbCr2 and ToCr2 Structure, Low Temperature Form By using large scale Hull-Davey charts, the powder pattern of CbCr, and of the low temperature form of TaCr2 were readily interpreted on the basis of a face-centered cubic lattice with a parameter of approximately 6.95 kX. The indices of the reflections together with the values of sin' 0 are given in Tables I and 11. From this list of observed reflections, it appears that the (200), (600), (024), (046), and (028) reflections are missing. The lack of (h00) reflections for h 4n indicates a four-fold screw axis. The missing (Okl) spectra for k + 1 An indicate the existence of a diamond glide d. The combination of these symmetry elements can be found in the O— Fd3m space group, which is therefore the most probable one. After having determined the approximate density of TaCr, by the immersion method, the number of molecules per unit cell was calculated and found to be nearly eight. This information, added to the fact that the most probable space group is O leads to the consideration of a structure of the MgCu2 type, in which the atoms have the following positions: 8 magnesium in a and 16 copper in d. On the basis of this structure, intensities were computed by means of the usual formula: 1 cos'20 I a sin2 cos where F is the structure factor; 8, the Bragg angle: and p, the multiplicity factor. As shown in Tables I

Jan 1, 1953

By J. L. Stokes, L. J. Demer

It has recently been shown' that epitaxial films of silicon carbide deposited on silicon single crystals possess desirable properties for semiconductor applications. There is one apparent disadvantage to such a system, however; since epitaxial deposition is a high-temperature process, it can result in plastic deformation of the silicon substrate. The accompanying Berg-Barrett X-ray diffraction photographs reveal plastic deformation in two silicon semiconductor crystals which occurred when the crystals were coated with an epitaxial layer of silicon carbide at 1150°C. Due to differences in thermal expansion between the silicon substrate and the epitaxial silicon carbide, the silicon was subjected to stresses while still in the plastic temperature range. Both crystals shown were 0.7 in. in diam and 0.0055 in. thick. The crystals were sliced from a larger crystal so that their polar axes were parallel to the [ill] direction. After cutting, the crystals were polished with diamond paste, and etched in HC1 vapor to remove surface damage re- sulting from the cutting and polishing operations. This provided clean, damage-free surfaces on which to deposit the silicon carbide. Figs. l(a) and l(b) are reflection and transmission photographs, respectively, of the same crystal. A smaller portion of the crystal is shown in the transmission geometry, because a vertical slit was

Jan 1, 1965

By F. D. George, M. J. Salkind

Al3Ni whisker-reinforced aluminum was found to exhibit good Charpy impact toughness and little notch sensitivity even though its room-temperature tensile elongation parallel to the whiskers is only 2 pct. This impact behavior was maintained d liquid nitrogen temperature (-196"C). It is postulated that this behavior is due primarily to the presence of the continuous aluminum matrix which provides sufficient 10calized ductility in the vicinity of the crack tip to absorb considerable energy from the advancing crack. The impact behavior of Al-Alni was found to be quite anisotropic. Of six orientations studied, the transverse orientation having the notch normal to the whisker axis was found to exhibit the lowest impact energy, whereas the transverse orientation having the notch parallel to the whisker axis was found to exhibit the highest impact energy. A significant differnce was noted between the impact behavior of material containing needlelike whiskers and that containing bladelike whiskers. Only two of the six orientations studied exhibited complete fracture for the material containing needlelike whiskers. On the other had, most of the specimens containing bladelike whiskers exhibited complete fracture. It was postulated that the bladelike whiskers block transverse flow, thus reducing the amount of plastic deformation ahead of the crack tip. One of the more significant advantages of composite materials is the prospect of combining high strength with toughness. In general, toughness is associated with materials which exhibit considerable ductility and can deform plastically in the presence of a stress concentration. Very strong materials which resist plastic deformation generally exhibit low toughness. At first glance, then, it would appear as though strength and toughness are mutually incompatible so that useful engineering materials would have to be a compromise between the two. One approach to the problem of combining the high intrinsic strength of ceramics with the toughness of metals was to mix them together to form a cermet. Unfortunately, the toughness of cermets was found to be rather disappointing. Whisker reinforcement of metals, however, appears to be a more promising approach. It has been demonstrated that whisker-reinforced metals produced by unidirectional solidification exhibit enhanced strength due to the presence of high strength nonmetallic whiskers. The total strain capacity of these composites in the direction of fiber alignment is limited to that of the fibers, the matrix being unable to carry the load once the fibers have failed. A characteristic, then, of whisker composites is low ductility in the direction of whisker alignment, on the order of a few percent elongation. This low elongation, which is usually associated with brittle behavior, should not be taken as an indication of low toughness. Such a material can exhibit significant ductility in directions other than parallel to the fibers7 and can therefore possess significant intrinsic toughness. Toughness in a fiber-reinforced metal is derived from several mechanisms. The first is due to the toughness of the matrix itself. A continuous ductile metal matrix can act as an effective crack arrest medium by undergoing localized plastic deformation. Cracks initiated from the surface of the composite or from a brittle fiber failure must travel through the matrix before reaching another brittle phase particle. A second crack arrest mechanism peculiar to fiber composites is due to the fact that, as a crack travels through the matrix and approaches a fiber, the plastic deformation ahead of the crack tip will result in loading of the fiber. This causes the matrix shear strength in the plastic zone to be apparently higher, thus extracting more energy from the crack and diverting the crack at an angle to the original direction of propagation. A third crack arrest mechanism occurs in fiber composites which exhibit a weak bond between fiber and matrix. The idea was proposed by Cook and Gordons that if a crack propagating transversely in a fiber composite were made to turn and run along the fibers by decohesion of the fiber-matrix bond, then toughness would be imparted by the blunting of the crack tip and the creation of new surfaces. The last mechanism, interfacial decohesion, is commonly noted in naturally occurring fiber composites such as wood, bone, and bamboo, and has been observed in man-made composites such as glass fiber-reinforced resins,g silica fiber-reinforced aluminum," laminated steel," and tungsten and silica fiber-reinforced electroplated copper.'' The first mechanism, crack arrest by plastic deformation in the matrix, has been noted in tungsten wire reinforced cast copper." The purpose of this investigation was to quantitatively assess the toughness of a whisker-reinforced metal as a function of orientation. Previous investigation considered only cracks propagating nominally perpendicular to the reinforcement. In this investigation, crack propagation in three mutually perpendicular directions as well as three intermediate orientations was investigated. The system chosen for study was the unidirectionally solidified A1-A13Ni eu-tectic alloy which has a microstructure consisting of 10 pct by volume of A13Ni whiskers in a matrix of aluminum This material exhibits two different kinds of whisker morphology, depending upon the rate at which it is solidified.' At low rates of solidification (less than 2 cm per hr) the whiskers are bladelike, whereas at higher rates of solidification they are

Jan 1, 1969

By W. M. Corse

AS THE outstanding contribution of the Committee on Correlation of Research of the Institute of Metals Division for 1932, may be mentioned the publication of Bureau of Mines Information Circular 6637, entitled "Research Activities in the Mineral Industries of the United States." This circular was compiled by A. C. Fieldner and Alden H. Emery, members of the Committee, in cooperation with the Bureau, and comprises a285-page list of research problems reported to the Bureau as engaging the attention of the various mineral industries. To obtain this information questionnaires were sent to 106 governmental agencies, 338 trade and professional associations, 524 colleges and universities, 9 endowed research institutions, and 1847 private companies and consulting laboratories. In order that the returns should be as complete as possible, the original mailing list included names from which it was not expected much pertinent information would be obtained. However, the procedure was justified as significant returns were obtained from many of these.

Jan 1, 1933

Eckley B. Coxe, Drifton, Pa.: Anthracite coal differs from other fuels in its greater solidity. It does not burn like coke or wood, or like bituminous and coking coals, which become more or less spongy when heated, so that combustion can take place to some

Jan 1, 1892

By Cyril Stanley Smith

Although alloys of copper and silicon were examined several years ago,' and their excellent mechanical properties were shown, it was not until C. B. Jacobs 2 introduced manganese in small quantities to the alloys that they became of commercial importance. A few years ago The American Brass Company took over the patents and commenced to manufacture the alloy under the name "Everdur." The present study of the constitution of the ternary system was undertaken in order to reach a fuller understanding of the behavior of the alloy. Review of Previous WORK on the BinaRy Systems There have been no papers published dealing with the constitution of the ternary system, although some tests of the mechanical properties have been described," which indicate that there is a change in solubility with temperature. Copper-silicon System The copper-silicon system has been studied in detail by the author and is described in two papers published in 1928.V he portion of the diagram up to 8 per cent. silicon, as determined by this research, is reproduced in Fig. 1. The author's previous papers include a complete review of the work of other investigators and it is not necessary to deal further with this system here. Copper-manganese System The copper-manganese system has been investigated by several workers, notably Lewis,5 Wologdine,6 Sahmen7 and Schemtschuschny,

Jan 1, 1930

By J. Marvin Weller, M. King Hubbert

Preliminary investigations were undertaken with a Megger Ground Tester in 1931 by Hubbert to determine whether the faults in Hardin County, Illinois, could be located by earth-resistivity surveys. The results of these investigations, which were in part presented before this Institute in 1932,1 were sufficiently promising to warrant a more extensive field program in the same general area the following summer. During the second season an apparatus of the Gish-Rooney type was employed because of its greater sensitivity and to avoid the troublesome correction for resistance of potential electrodes necessitated by the use of a Megger instrument. The discussion of earth-resistivity traverses which constitute the main part of this paper is based entirely upon the results of the second season's work. All of the traverses were made with a constant electrode spacing of a equal to 100 ft., and the four-electrode technique was employed. Successive stations in these traverses were spaced at intervals of 100 ft. and the line of electrodes was carried parallel to the line of traverse. The graphs of resistivity profiles presented here (Figs. 1 to 3) are plotted with resistivities in ohm-centimeters as ordinates and with distance divided into stations at 100-ft. intervals as abscissas. After the traverses were run by Hubbert the results were computed, the profiles plotted, and tentative interpretations were made by him. These curves and interpretations were then taken into the field by Wellcr, who made a careful geological examination along the lines of traverse for the purpose of checking and supplementing Hubbert's interpretations. Weller then constructed a geologic cross-section extending along the line of each traverse. The accompanying diagrams graphically illustrate the correlation that can be made between earth resistivity and geology in this area.

Jan 1, 1934

By R. H. Wightman, G. H. ADAM

In order to secure good results in the prevention of accidents, it is generally recognized that the desire for such accomplishment, as well as the aggressive and constructive action to achieve it, must emanate from the Top Management and permeate successively down through the "Chart of Authority" to the workmen. Several years ago, with the above as a basis and with full support of the Top Management, the Mining Department started a program of selling the foremen and bosses the idea that safety could be achieved and that it was desired and required. Using psychology, persistence and numerous other methods, the foremen and bosses were finally impressed with the idea that "It can be done" and "It will be done." With this in mind, new ideas were brought forth by the foremen and bosses regarding the caving operation and the specific jobs in the operation. These new ideas were taken up in round-table discussions and resulted in certain changes in the undercutting method and the actual drawing of the blocks. These changes resulted in increasing fragmentation of the blocks which prevented the usual hang-up areas in the blocks. With the rock smaller in size and within reasonable reach from the tapping drifts, accidents were prevented in the tapping section. At the same time, an enforced campaign of housekeeping throughout the mine was undertaken with very beneficial results. The foremen and bosses then, in turn, educated and trained the workers themselves to become safely conscious. In so doing, a constant re- minder was given on all jobs assigned that the job was to be done safely as well as efficiently. No man is assigned a job who is not qualified for the type of work required. Efficiency and safety go hand in hand.

Jan 1, 1949

By Hans Lundberg

IN last year's report on the progress of geophysics, the airborne magnetometer was the featured new development. At that time only a relatively small number of surveys had been made. During 1947, the airborne magnetometer was used in making many surveys and is again one of the high lights of the year in geophysics. This report is mainly concerned with geophysics as applied to the search for minerals exclusive of petroleum. In 194,5 and 1946, the use of the magnetic method reached a peak, partly because of an active period of prospecting brought on by an active mining market, particularly in Canada.

Jan 1, 1948

By Charles Y. Clayton

THE general public does not know that there is such a thing as metallurgy and it is very seldom that you see the word metallurgy in print except in technical magazines. Perhaps it is more to the front now than in former years; the Dee. 30, 1929, issue of Time mentioned under the heading of "Science7' certain new achievements in metallurgy, which may be cited as a rare instance of the use of the word in anything but the technical press. Too often the part the metallurgist plays in the advancement of the different branches of engineering is overlooked. To say that the public does not know there is such a profession as metallurgical engineering seems to be a bold statement, but had there beep time a questionnaire could have proved this beyond doubt. Suppose a carefully-planned questionnaire had been sent to all high school students asking them, among other questions, to list the different branches of engineering, I believe that the several professions would have been listed in this manner: (1) Electrical engineering; (2) mechanical; (3) civil, and (4)' mining. One in each hundred might have listed metallurgy as an engineering profession. Even the Society for the Promotion of Engineering Education in its Bulletin No. 10-"Investigation of Engineering Education" lists Civil, Mining, Mechanical, Electrical, and Chemical, leaving out Metallurgical Engineering.

Jan 1, 1930

By J. R. Schneider

INTRODUCTION Landowners in Texas for many years have freely granted, reserved and leased "oil, gas and other minerals" or interests therein. In recent years we have witnessed much litigation concerning what sub- stances should be included as "other minerals" within the phrase "oil, gas and other minerals," and this question has received the attention of numerous legal scholars. At the South Texas Uranium Seminar held in Corpus Christi, Texas, in September, 1978, Mr. William R. Dodson presented a paper dealing with this very subject and entitled "Uranium - Mineral or Surface? Who Owns It?" In his paper, Mr. Dodson reported on two recent Texas Supreme Court decisions, Acker v. a, 464 S.W.2d 348 (Tex. 1971) and Reed v. Wylie, 554 S.W.2d 169 (Tex. 1977). which held that the particular substance in question in each case is not a mineral within the phrase "oil, gas and other minerals" if substantial quantities of the substance lie so near the surface that production will entail the stripping away and substantial destruction of the surface. Since that time another chapter has been written in the Texas saga of "When is a Mineral not a Mineral?" and it is the intent of this paper to present an update of the Texas law. A review of the early Texas cases so ably covered by Mr. Dodson in his paper will not be repeated, except as is necessary to illustrate the evolution of the legal doc- trine which has been so aptly named "The Surface Destruction Test". BACKGROUND In order to appreciate the genesis of the problem, one must consider that oil and gas production commenced in Texas many years ago, Spindletop came in in 1901. As oil and gas became more valuable, land- owners with considerable frequency sold interest in the oil, gas and mineral estates in their lands, and reserved interest in the oil, gas and mineral estates in their lands when they disposed of their property. Due to the oil and gas background, and perhaps be- cause oil and gas was paramount in the minds of the parties, the traditional language employed in these grants and reservations was "oil, gas and other minerals" or variations thereof. There are literally hundreds of instruments employing this language constituting a link in the chains of title to thous- ands of acres of Texas land. In addition, there are thousands of acres of Texas land held by oil, gas and mineral leases, the primary terms of which have been perpetuated by production, containing similar language in their granting clauses. The severance of the mineral estate from the surface estate results in two separate and distinct estates, each having all of the incidents and attributes of an estate in land. with the surface estate being the serviant estate, and the mineral estate being the dominant estate and having certain easements in the surface estate to explore. produce and remove the minerals. Harris v. Currie. 176 S.W.2d 302, 305 (Tex. 1943). As observed by the court in the Harris case, this is because a grant or reservation of minerals would be wholly worthless if the grantee or reservor co~lld rwt enter upon the land in order to explore for and extract the minerals granted or reserved. Although the Texas law has recognized that an oil and gas lessee has the right to use so much of the surface as is reasonably necessary to produce the minerals. Warren Petroleum Corporation v. Monzingo, 304 S.W.2d 362, 363 (Tex. 1957), recent decisions of the Court have qualified this doctrine. In Getty Oil Company v. Jones. 470 S.W.2d 618 (Tex. 1971). Getty's pumpine, units were interfering with ones self-propelled sprinkler system utilized for irrigating the premises, and Jones sought to require Getty to install the-pumping units in cellars so that the sprinkler system could pass over them. In an effort to accommodate both the surface estate and the mineral estate, the court held (page 622) "...where there is an existing use by the surface owner which would otherwise be precluded or impaired, and where under the established practices in the industry there are alternatives available to the lessee whereby the minerals can be recovered, the rules of reasonable usage of the surface may require the adoption of an alternative by the lessee". Bearing in mind that the "reasonable use doctrine" grew up in the oil and gas industry involving sub- stances which can be produced by methods that do not destroy or deplete the surface estate, the question presented is whether the Texas courts will extend this doctrine to situations where claimants of "other minerals" seek to produce shallow deposits of iron ore, coal, lignite and uranium by surface mining methods which do destroy or deplete the surface estate? The surface destruction test has answered this question in the negative, at least as to iron. coal and lignite. However, the multitude of mineral estates in Texas which have been created by a grant. reservation or lease of "oil, gas and other minerals" will, doubtlessly, continue to fuel the fires of litigation. EARLY TEXAS DECISIONS In view of the evolution of the Surface Destruc- tion Test, an exhaustive review of the early Texas

Jan 1, 1980

By Ralph Wilcox

THE diamond drilling of certain characters of unstable rock forma-tion, as, for example, the copper-bearing schists of the Miami district in Arizona, is rendered most difficult by what is known as " caving" of the sides of the drill holes. As this caving is very greatly increased by the action of flowing water, it occurred to me, after experiencing a great deal of difficulty with caving in diamond-drill holes which I was drilling for the Miami Copper Co., that if I could substitute air for water, much of the caving-with resultant difficulties, such as decreased speed of sinking and increased consumption. of diamonds-would be overcome. After some experimenting, I found that it was perfectly practicable to substitute air for the water; forcing the air down the hollow rotating rods in the same manner as is done with water, the air passing out around the bit, which is thus cooled, and ascending on the outside of the rods to the collar of the hole, carrying the borings in just as satisfactory a manner as had been done by the water, but without the accompanying destruction or caving of the sides of the drill holes such as had been so generally experienced with the water. When water was encountered in the drilling this water was forced up to the collar just as it would have been had water been used in the .drilling, but with the correspondingly decreased flow there was relatively less washing or caving of the sides of the drill holes. The only change necessary in the arrangement of the drill is that a cross instead of a tee is used at the collar of the hole. A tightly woven jute bag is attached to one arm of the cross, for collecting and filtering the sample; and when drilling in dry ground a jet of water is attached to the opposite arm of the cross, to collect the dust and wash down the sample into the bag. The rods rotate through a stuffing box attached to the upper opening of the cross. The distention of the jute bag by the issuing air indicates the operating conditions as sufficiently as did the flow of water when using water in the drill hole.

Jan 10, 1913

By Robert Hunt

(New York Meeting, February, 1913.) I HAVE frequently stated that while the chemical composition of steel is important, yet even greater importance is connected with the mechanical and heat treatment of the metal. During the past year I encountered such a positive example of that fact that I deem it worth putting upon record. A prominent railway system divided an order for open-hearth steel rails between two steel works, both of which are under the control of the one corporation; giving to one about 18,000 tons, and to the other 7,500 tons of the same section and to be made under the same specifications. The rolling results obtained in the two mills varied so widely that a study of the figures is intensely interesting and serves to illustrate the advantages obtained by careful ingot casting, and, quite as pertinently, the possible benefits of careful subsequent heating and rolling with moderate reductions in the rolling process. The smaller order was rolled complete in four installments during the same months that the larger order was being made in six separate installments; but, to permit of exact comparisons, the totals of the four installments (completing the order with the mill which I will call A) are given with the totals of the first four installments of the larger order, made by the mill designated as B. These rolling results are:

Jan 5, 1913

MEMBERS-QUALIFICATIONS AND ELECTION SEC. 1. The membership of the Institute shall comprise seven classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Members; 6. Rocky Mountain Members; 7. Junior Foreign Affiliates. All shall be equally entitled to the privileges of membership, excepting that no member of any class whose residence shall be outside of the United States of America, except those residing in Mexico and Canada, shall he entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the class of Member must be at least 27 years of age and must have had at least six years' employment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which be must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain members. SEC. 3. Honorary Members: Each candidate for Honorary Membership must be recommended by at least ten Members and must be elected by ballot at a meeting of the Board of Directors by the unanimous vote of the Directors present; provided, however, that the number of Honorary Members shall at no time exceed twenty. Such election shall automatically act as a transfer of such member from any other class of membership to which be may belong.

Jan 1, 1938

By R. A. Vandermeer, J. C. Ogle

Two distinct types of depth-dependent variations in texture have been observed in niobium cold-rolled various amounts up to 99.5 pct reduction in thickness. These nonuniformities are thought to be the results of nonhomogeneous plastic dewmation during rolling. The first type is characterized by a zone at intermediate depths that tends to lack certain strong orientations which are present in the surface and center layers of the rolled stock. This type of texture modification seemed to be associuted with "high" body rolling and may be related to the shape of the zone of deformation in rolling. The second type of texture inhomogeneity found involved the formation of a unique texture in the surface layers of heavily rolled strip. High fiiction forces between work piece and rolls appear to be needed to generate and maintain this texture. We believe that this unique surface texture results from a shear mode of deformation in the surface layers. THE evolution of texture in both the surface and center regions of cold-rolled niobium as a function of increasing deformation from 43 to 99.5 pct reduction in thickness was reported in a previous paper.' It was noted that for strips rolled between 95 and 98 pct reduction a distinctly different texture appeared in the surface layers which was unlike the center texture. Certain other layer to layer textural variations were also detected during the experimental phase of that work but were not described in the paper. Surface textures have been reported previously for the bcc materials iron and Steel2-4 and are well known in the fcc metals.5 It is usually stated that these are shear textures which arise under conditions of high friction between specimen and rolls. Work by Mayer-Rosa and Haessner5 n niobium rolled under conditions presumed to be high roll friction gave no indication, however, of a surface texture in that material. This is indeed puzzling in view of our results.' Thus we undertook additional experiments designed to study the stability of the surface texture for certain rolling variables. The variables investigated were the presence or absence of lubrication, amount of reduction per pass, and reverse vs unidirectional rolling. It is the purpose of the present paper to describe the kinds of depth-dependent textural inhomogeneities that we have observed in rolled niobium as well as to present the results of our recent experiments on the stability of the surface texture. Possible explanations for the depth-dependent texture variations will be discussed in terms of nonhomogeneous plastic deformation during rolling. EXPERIMENTAL Specimens cut from the niobium rolled to different reductions in the previous study1 were examined at various layer levels throughout the strip thickness for textural inhomogeneity. The specimen surfaces were either etched or machine ground and etched to remove material to a specific depth. Textures were determined by means of the Schulz X-ray reflection pole figure method with a Siemens texture goniometer and Cum X radiation. Since the important intensity peaks of the textures in niobium are usually located on the normal direction (N.D.) to rolling direction (R.D.) radius of the (110) pole figures, it was sufficient in many cases to scan only along this radius. At selected depths or where additional information was required the entire (110) pole figure was also obtained. In studying the stability and formation of the surface texture, experiments were conducted on 0.400-in.-thick, fine-grained, randomly oriented niobium specimens extracted from the same starting stock as that used in the earlier study.' Two of these specimens were rolled at room temperature to a total reduction of 96.4 pct. One was rolled between cleaned and degreased rolls with no lubrication. The other was lubricated between passes with Welch Duo Seal vacuum pump oil. The rolling schedules of each were kept as nearly identical as possible. Drafts were of the order of 0.006 to 0.012 in. per pass. Other experiments consisted of rolling specimens at constant fractional reduction per pass, i.e., (ta- tb)/ta equals a constant where ta and tb are the entrance and exit thickness of the rolled stock, rather than at a constant draft, i.e., ta- tb equals a constant. Ten specimens were rolled at room temperature on a two-high, motor-driven rolling mill with 8-in.-diam rolls. These specimens were rolled to thicknesses of between 0.041 and 0.073 in. (82 to 90 pct total reduction) at approximately constant reductions per pass ranging from 9 to 45 pct. Kerosene was used as a lubricant. Half of the specimens were always rolled in the same direction while the other half were reversed end to end at each pass. The texture in the surface regions was determined with the X-ray technique described above. RESULTS The textural inhomogeneities noted in niobium rolled from fine-grained, randomly oriented stock 1.5 in. long by 0.75 in. wide by 0.40 in. thick can be classified into two types. The first may be discussed with the aid of Figs. 1 to 3. Fig. 1 is a three-dimensional plot of the X-ray intensity in units of times random vs f , the angle from the N.D. to any point along the N.D. to R.D. radius of the (110) pole figure, and depth, given as percent of the thickness (?t/to X 100, where at is the thickness of material removed and to is the as-rolled

Jan 1, 1970

By G. V. Sullivan, B. E. Davis, T. O. Llewellyn

The Bureau of Mines, US Department of the Interior, conducted studies to recover phosphate from four dolomitic southern Florida deposits not currently mined. The samples contained 5.8-10.2% P205 and 1.7-4.8% MgO. Chemical analyses of sized fractions indicated that no pebble concentrate, +1.2 mm (+14 mesh) could be produced from these samples. A scheme was developed that consisted of desliming, grinding, scrubbing, and redesliming the ore to produce a flotation feed. Conventional one-step fatty acid fuel oil batch flotation tests on the samples resulted in concentrates containing 29.0-31.3% P205 at flotation recoveries ranging from 72.4 to 96.1% of the flotation feed. The MgO content of the concentrates ranged from 0.47 to 1.36%. Continuous flotation of the Manatee No. 2 sample indicated that commercial-grade phosphate concentrates analyzing 31.3% P205 and 0.55% MgO could be produced with a flotation recovery of 89.9%. The MgO content of concentrates obtained from the Manatee No. 1 and Hardee samples was 1.20 -1.36 %, respectively. Leaching with aqueous SO2 reduced the MgO content of these phosphate concentrates to 0.5 and 0.8%, but with a concomitant loss in phosphate recovery of about 10%.

Jan 1, 1985

By T. H. Ramsey, Richard Shield

A process has been developed for fabricating thin-film resistors that are compatible with integrated circuits. Films are produced by evaporation of single refractory metals using an electron beam heating source. Resistor paths are then made using standard photoresist etching techniques. A low-temperature coefficient of resistance is obtained by control of nucleation during deposition of the film. One application of the process has been the development of a discrete resistor used for current setting in linear integrated circuits. Multiple thin-film resistors were formed on oxidized silicon substrates using molybdenum metal as a source. An evaporated protective layer of SiO2 over the resistor prevents resistance changes which might occur during subsequent high-temperature processing. Properties of a typical resistor are as follows: R = 15.7 ohm per sq, tolerance surface dimensions = 0.028 by 0.028 in., stable after 4000 hr at 0. 75 w without heat sink. THIN-FILM resistors have been investigated for many years with a large selection of usable resistors resulting from a wide variety of materials. Many of the processes necessitate a high degree of complexity but in nearly all cases the conclusions have been that the materials used in each case were acceptable provided the deposition process was reproducible and could be controlled sufficiently to give the required tolerances. It is our opinion that simplicity is still the key to thin-film resistor fabrication. In this regard, the single metal is obviously the simplest process to control, provided all the necessary properties can be obtained. The idea is not original in this laboratory by any means. Others have taken this approach.' It has been demonstrated that a fairly wide range of resistivities can be obtained by careful control of deposition parameters for any given metal, and by selection of several single metals a very broad range of stable resistors can be obtained. The transition from one metal to the next is made when a film becomes too thin for adequate process control or long-term stability. A great deal of emphasis is once again being placed on the thin-film resistor. Although they have been thoroughly studied in the past, new applications have been found that require the properties obtainable only from thin-film resistors. Integrated circuits, in general, are advancing toward higher speeds and radiation environments which require replacement of the present diffused resistors. Linear circuits in particular are requiring high-power, high-precision resistors for the more advanced applications. The particular requirements of some linear circuits are such that a discrete resistor is required. The resistor described in this paper was developed as a 15.7-ohm precision discrete resistor for use in a current regulating circuit requiring a +2 pct end of life overall tolerance, a dissipation of 750 mw, and the ability to operate over a fairly broad temperature range (i.e., a low temperature coefficient of resistance, TCR). State-of-the-art integrated circuit and silicon processing technology lends itself well to the fabrication of thin-film resistors. Not only is the resistor thin film well-suited to integration on individual circuits, but the oxidized silicon surface provides one of

Jan 1, 1969

By Eifu Moriyama

In 1953, Akita Plant, having a capacity of 560 tons per month, was built at Akita city by Mitsubishi Metal Mining Co., Ltd. for the purpose of treatment of the Ikuno and Akenobe Mines's zinc concentrates. Akita city, in whose neighborhood the black ore has been discovered, is located about 500 Km north of Tokyo and faced with the Japan Sea. This plant has been continuously expanded to have the capacity of 7,500 tons per month by the end of 1969. Efforts have been made to mechanize installations and to achieve continuous process. One of the characteristics of Akita Plant is the recent establishment of the residue treatment process. Many processes had been investigated, and finally commercial sulphate roasting of the residue has been carried out since 1965. At Akita Plant, special high grade electrolytic zinc, zinc alloy for die-casting (MAK brand), cadmium, cement copper and sulphur dioxide gas are produced. Sulphur dioxide gas is sent to the next door fertilizer plant to make acid. Table 1 shows production and the average assay of the electrolytic zinc and cadmium in 1969. This plant is divided into four main sections, two subsections, and residue treatment sections: Main sections are: (M-1) roasting section, (M-2) leaching and purification section, (M-3) electrolysis section, (M-4) melting and casting section,

Jan 1, 1970

By H. T. Bowman

For more than 80 years the Bessemer process has depended upon the ability, skill, and judgment of the blower, although as early as the I860's it was recognized that the process would benefit by some type of instrumental contro1.l IIowever, instruments with sufficient recording speeds did not exist, so the end-point determination was always dependent upon the blower's eye. This placed an obstacle in the way of precise experimental work, because of the absence of the necessary records and reference points as reported by Work.2 The use of the photocell provided the instantaneous record of the blow that made this experimental work possible and provided more scientific control for the process as discussed by Graham,3 A brief description of the progress of the blow will illustrate the recording function of the instrument. The silicon in the iron is being oxidized during the first minutes of the blow, as pointed out by Henning4 in a table showing the order of metalloid elimination. The product of this oxidation is a solid that remains in the converter, so there is virtually no flame during this part of the blow. This low flame luminosity is illustrated by the flame recording shown in Fig. I, where the silicon blow is plainly marked. The dull flame of the silicon blow gradually gives way to the brilliant carbon flame as the increasing quantities of carbon monoxide formed inside the converter burn to dioxide upon contact with the atmosphere above the vessel. When the carbon reaches some low value under 0.20 per cent, there is insufficient menoxide formed to maintain the dioxide flame, so its intensity drops. Throughout the flame drop carbon continues to burn, until at some value around 0.05 per cent an arrest occurs in the recorded drop. This point has been designated as the end point. The period of time from this end point until the vessel is turned upon its side and blowing has stopped has been called the afterblow. This afterblow is used as a measure of the degree of metal oxidation, and uniformity demands that it be controlled within narrow limits. Iron and blowing conditions are likely to change several times during a turn, necessitating corresponding changes in end-point control. It is the purpose of this paper to discuss these changes, the factors that make them necessary, and their bearing upon the quality of steel. Carbon-FeO Relationship In the Bessemer process oxidation relationships are precise. Fig. 2 shows a graph of the carbon-FeO relationship. The familiar "bomb-test" method, described by Mccutcheon and Rautio,5 was used for obtaining these and all other dissolved FeO values herein reported, all tests being taken from the converter before deoxidation unless otherwise noted. All tests of 0.10 per. cent carbon and above were obtained from metal blown for duplexing. McGinley and Woodworth6 reported iron oxide values for blown metal, but their tests were obtained by a . different method than were those

Jan 1, 1942

By H. T. Bowman

For more than 80 years the Bessemer process has depended upon the ability, skill, and judgment of the blower, although as early as the I860's it was recognized that the process would benefit by some type of instrumental contro1.l IIowever, instruments with sufficient recording speeds did not exist, so the end-point determination was always dependent upon the blower's eye. This placed an obstacle in the way of precise experimental work, because of the absence of the necessary records and reference points as reported by Work.2 The use of the photocell provided the instantaneous record of the blow that made this experimental work possible and provided more scientific control for the process as discussed by Graham,3 A brief description of the progress of the blow will illustrate the recording function of the instrument. The silicon in the iron is being oxidized during the first minutes of the blow, as pointed out by Henning4 in a table showing the order of metalloid elimination. The product of this oxidation is a solid that remains in the converter, so there is virtually no flame during this part of the blow. This low flame luminosity is illustrated by the flame recording shown in Fig. I, where the silicon blow is plainly marked. The dull flame of the silicon blow gradually gives way to the brilliant carbon flame as the increasing quantities of carbon monoxide formed inside the converter burn to dioxide upon contact with the atmosphere above the vessel. When the carbon reaches some low value under 0.20 per cent, there is insufficient menoxide formed to maintain the dioxide flame, so its intensity drops. Throughout the flame drop carbon continues to burn, until at some value around 0.05 per cent an arrest occurs in the recorded drop. This point has been designated as the end point. The period of time from this end point until the vessel is turned upon its side and blowing has stopped has been called the afterblow. This afterblow is used as a measure of the degree of metal oxidation, and uniformity demands that it be controlled within narrow limits. Iron and blowing conditions are likely to change several times during a turn, necessitating corresponding changes in end-point control. It is the purpose of this paper to discuss these changes, the factors that make them necessary, and their bearing upon the quality of steel. Carbon-FeO Relationship In the Bessemer process oxidation relationships are precise. Fig. 2 shows a graph of the carbon-FeO relationship. The familiar "bomb-test" method, described by Mccutcheon and Rautio,5 was used for obtaining these and all other dissolved FeO values herein reported, all tests being taken from the converter before deoxidation unless otherwise noted. All tests of 0.10 per. cent carbon and above were obtained from metal blown for duplexing. McGinley and Woodworth6 reported iron oxide values for blown metal, but their tests were obtained by a . different method than were those

Jan 1, 1942