Search Documents

By J. P. Boisseau, C. N. J. Wagner, E. N. Aqua

An analysis ulas made of powder-paltern peaks from cold-rolled polycrystalline copper and from copper powders, compacted into briquets (1 in. diameter) with pressures up to about 106 psi. Powder-pattern peaks from both contact faces were measured with a diffractometer and CuKa radiation. Laltice-parameter measurements indicate the presence of residual stresses in the bulk specimen of the order of a - -10 kg per sq mm after 93 pct reduction in thickness, and give some evidence for the occurrence of deformation stacking faults (probability a - 0.003) in both bulk and powder samples. Fourier analyses of the line profiles were carried out on the (111) - (222) and (200) - (400) Pairs of reflections. The particle sizes decrease rapidly with increasing deformation and reach asymptotic values of De (111) = 550A and D, (200) = 350A at about 25 pct reduction in thickness or 80,000 psi pressure for compaction. The anisotropy of the particle sizes indicates the presence of microtwins and stacking faults on (111) planes. The rms strains increase also with deformation and reach limiting values of 2 x 10-3 in the [100] direction and 1 x 10-3 in the [Ill] direction at a distance L = 100A normal to the reflecting planes. THE diffraction of X-rays in cold-worked, polycrystalline, fcc metals and alloys yields Debye-Scherrer patterns in which the individual (hkl) lines may show a broadening, a shift, and an asymmetric shape.' These effects can be explained by the fragmentation of the small, coherently diffracting domains, the presence of residual elastic strains in the lattice, and the formation of stacking faults. X-ray studies of stacking faults in fcc metals and alloys have been methodically performed during the last few years, but so far most of the investigators dealt with cold-worked powder specimens obtained by filing.2-8,10-19 In such specimens, the crystals are randomly oriented and the average elastic strains are assumed to be zero, so that the observed peak shifts are due to stacking faults only. The agreement between X-ray diffraction theory1,20 and experiment is generally good. On the contrary, cold-worked, polycrystalline bulk specimens (after wire drawing, rolling, plastic deformation by tension or compression, etc.) contain residual elastic strains, which may not average to zero in the surface of the specimen and show very strong preferred orientation of certain lattice planes (texture) parallel to the specimen surface. Nonzero elastic strains also produce peak shifts, the magnitudes of which depend upon the crystallographic orientation of the reflecting lattice planes in elastically anisotropic materials as well as on the type of plastic deformation and which have to be taken into account when measuring stacking-fault probabilities in deformed bulk specimens.21-23 The purpose of the present investigations was to perform a detailed X-ray analysis on a bulk specimen of a fcc metal deformed by rolling at room temperature and on powder of the same material deformed by compaction, and to compare these results with those previously obtained on cold-worked filings.18 Pure copper was chosen for this study since it is known to produce only a small quantity of stacking faults by filing at room temperature.3,16,17,19 The residual elastic strain in the surface of the bulk copper should be the predominant factor determining

Jan 1, 1965

By James A. McGurty, Walter J. Koshuba, Samuel G. Gordon, Gilbert E. Klein

ONE of the problems encountered in working with metals at elevated temperatures is the instability resulting from solid-solid diffusion at a -common interface. A determination of the nature and magnitude of this phenomenon is important as related to structural properties of materials potentially useful in high temperature applications. This paper is concerned with the solid state reaction between metallic molybdenum and beryllium at elevated temperatures. In the older literature,' there were no known inter-metallic compounds in the system Be-Mo, and the list of beryllium intermetallics was rather small. New compilations have been made by Smithells' and by Taylor," listing all the then known beryllium binary intermetallic compounds. In addition to these, some new phases have just been reported' in the system Zr-Be and some further compounds of the type MBe,3 have been currently described. The new compound MoBe,, which is reported upon in this paper differs considerably from the above mentioned MBe13 group, and will be discussed in detail. Diffusion Study The nature of the solid diffusion at a Mo-Be interface was determined by sealing a beryllium rod inside a molybdenum capsule and heating at a temperature of 2000°F' (1100°C) for 100 hr. The molybdenum capsule was fabricated from % in. swaged molybdenum rod obtained from the Fansteel Metallurgical Corp. The beryllium metal was obtained from Brush Beryllium Corp. as % in. cold-drawn rod. This material assayed 99.05 pct Be and contained as impurities 0.84 pct Be0 and 0.19 pct Be2C. The molybdenum capsule was % in. in OD x 2 in. long. To prepare it, a concentric hole 0.250 in. + 0.001 in. — 0.000 in. in diam was drilled and reamed in one end of a rod to a depth of 1 '/2 in. A 1 in. long beryllium rod 0.250 in. + 0.000 in. — 0.001 in. in diam was pressed into the molybdenum capsule. A molybdenum plug 0.250 in. & 0.001 in. in diam x 9/16 in. long was then used to seal the beryllium in place. The capsules were placed in a molybdenum resistance furnace and heated at 2000°F (1100°C) for 100 hr. On cooling, the specimens were cut and examined metallographically. Fig. 1 is a micrograph at X250 of a portion of the interface from a transverse section. Four phases are clearly visible, with sharp boundaries between them. Phase A is a section of the molybdenum capsule; phase B is the molybdenum-rich intermetallic composition MoBe,; phase C is the beryllium-rich compound MoBe13; phase D is a section of the beryllium rod. All phases were readily polished to a high metallic luster. The molybdenum-rich phase has a pronounced purple tinge. The beryllium-rich phase (C) is only slightly darker than the pure beryllium. In polarized reflected light, however, it shows striking birefringence between crossed Nicols. The black areas represent flaws or pores in the material. A small representative amount of powdered material from each of the phases was carefully removed under the microscope with a diamond tool. With this material, powder X-ray diffraction patterns were made for the identification of each phase. Table I lists the X-ray diffraction spacings and corresponding indexes characteristic of these intermetallic compounds. Synthesis To establish the formula of the new intermetallic compound, X-ray diffraction patterns were made from powders obtained from solidified melts of known composition. The syntheses were made by

Jan 1, 1952

By Frank Harris

THE strength of hard drawn copper wire is a question of considerable importance to both manufacturer and consumer. Unlike steel and alloy wires, in which strength is governed by both chemical and physical considerations, the high conductivity required for copper wire in the electrical industry generally precludes the possibility of obtaining tensile strength through the use of alloys. Consequently, this strength is largely a matter of the physical structure, and all factors known to affect this structure, such as rolling temperature, die contours, lubricants, drawing speeds, etc., are matters of prime importance. The experiments described here have been carried out during the past year at the Baltimore plant of the American Smelting & Refining Co., in connection with a general investigation of some of the questions mentioned above, with the object of studying the physical structure of hard drawn copper, wire and the influence of certain factors on that structure. The work has been of an exploratory nature, rather than comprehensive, but it was thought that the results might prove of sufficient general interest to warrant their publication. The bulk of the hard drawn copper wire used in places where strength is an important factor is manufactured to strict specification, based usually in the United States on that of the American Society for Testing Materials (B-1-23). This specification calls for almost as high a value of tensile strength; consistent with elongation, as it is possible practically to obtain, and only physically perfect material can be relied on to meet such a specification. Obvious defects, such as laminations produced through fins in the original rods or brittleness due to overdrawing, are usually recognized and need only passing reference. Laminations can be detected by twisting and untwisting the wire several times; they will show up on the surface in the form of fins. Fig. 1 shows a very bad example of this defect. The wire may be perfectly smooth before twisting but when such laminations are present they will readily show up under this treatment. This trouble is caused by similar defects in the original rod produced by overfills in rolling. Fig. 2 shows the cross-section of the rod from which the wire in Fig.1 was drawn.

Jan 1, 1928

By Frank W. Harris

THE strength of hard drawn copper wire is a question of considerable importance to both manufacturer and consumer. Unlike steel and alloy wires, in which strength is governed by both chemical and physical considerations, the high conductivity required for copper wire in the electrical industry generally precludes the possibility of obtaining tensile strength through the use of alloys. Consequently, this strength is largely a matter of the physical structure, and all factors known to affect this structure, such as rolling temperature, die contours, lubricants, drawing speeds, etc., are matters of prime importance. The experiments described here have been carried out during the past year at the Baltimore plant of the American Smelting & Refining Co., in connection with a general investigation of some of the questions mentioned above, with the object of studying the physical structure of hard drawn copper wire and the influence of certain factors on that structure. The work has been of an exploratory nature, rather than comprehensive, but it was thought that the results might prove of sufficient general interest to warrant their publication. The bulk of the hard drawn copper wire used in places where strength is an important factor is manufactured to strict specification, based usually in the United States on that of the American Society for Testing Materials (B-1-23). This specification calls for almost as high a value of tensile strength, consistent with elongation, as it is possible practically to obtain, and only physically perfect material can be relied on to meet such a specification. Obvious defects, such as laminations produced through fins in the original rods or brittleness due to overdrawing, are usually recognized and need only passing reference. Laminations can be detected by twisting and untwisting the wire several times; they will show up on the surface in the form of fins. Fig. 1 shows a very bad example of this defect. The wire may be perfectly smooth before twisting but when such laminations are present they will readily show up under this treatment. This trouble is caused by similar defects in the original rod produced by overfills in rolling. Fig. 2 shows the cross-section of the rod from which the wire in Fig. 1 was drawn.

Jan 1, 1928

By Arne F. Westgren

X-ray analysis and single-crystal study have been utilized in recent years as a new means of following constitutional changes in alloys. If such transformations can be suppressed by rapid cooling, they can be followed at room temperature in a particularly convenient manner. In the following we shall consider changes in solubility and polymorphic transformations with particular reference to phenomena of the age-hardening type. Finally a thermodynamic viewpoint is developed for examining such transformations. Changes in Solubility 1. Determinations of solubility limits in the solid state which show decreasing solubility with falling temperature are made as follows: A series of alloys extending into the heterogeneous region is prepared and quenched fromas high a temperature as possible, whereupon their lattice parameters are determined. Then one or more alloys are quenched from temperatures at which they are heterogeneous and their lattice parameters likwwise determined. For the purpose of determining the parameter the apparatus shown in Fig. 1 has been very useful for it produces sharp films in a short time which can be accurately read. High-order reflections (interferences) from the object are recorded on a film which is placed exactly perpendicular to the X-ray beam. The specimen usually has the shape of a small round bar.l Fig. 2 shows a selection of such exposures of silver-rich Cu-Ag alloys, and Fig. 3 gives the measurements made from these films. Fig. 4 gives the solubility curve which results.2 This curve is shifted to lower concentrations than the curve that is obtained from metallographic or physical methods. The X-ray method unquestionably gives more reliable data

Jan 1, 1931

By J. F. Wolff

CARL ZAPFFE, Brainerd, Minn. (communication to the Secretary*).¬Unless one has actually directed explorations for iron ore, it is doubtful whether the importance of Mr. Wolff's paper, the value of the information contained, and the large amount of detail work involved in what is set forth can be fully appreciated. It is indeed rare to get such a com-

Jan 3, 1917

By Richard Moldenke

The paper describes the making of pig iron from the Mayari iron ores of Cuba. The outstanding feature f this pig iron is a considerable content f nickel and chromium. As a marked improvement in the quality of castings has been noted when this iron is used in the foundry mixtures, a series f melting tests f mixtures of great variety of composition was conducted with the idea f getting comparative strengths from which the effect of nickel¬chromium could be seen. These tests, on account of their number, and degree of accuracy desired, were made by the crucible melting method. The paper gives the tables of results, a series f curves showing the inter-relation of the elements involved, and a summary of the conclusions derived. THE presence of nickel-chromium in pig iron made from Cuban ores is so well known that the word "Mayan" is unconsciously associated with it. Since 1904, when exploration of the Mayari deposits of iron ore in northeastern Cuba was undertaken, there has been increasing interest in these ores. The TRANSACTIONS contain numerous references to them. This iron ore, which is shipped to the. United States in the nodulized state, has been thoroughly tested and found very valuable; the deposit covers over 25,000 acres and there is in sight over 500,000,000 tons of ore that, by systematic mining, runs practically constant in composition. With nickel and chromium present, also titanium in sufficient quantities to attract attention, as well as extremely low phosphorus and sulfur contents, the iron founder is naturally interested in the utilization of Mayari ore for pig iron for the better grades of finished iron products. The present point of consumption of Mayari ore is at Sparrow's Point, where Mayari pig iron of any desired composition is made. The com-

Jan 9, 1922

By Thunaes, Arvid

Pilot plant test work in 1942 and 1943 showed that by a combination of desliming, fine-size classification, and Sullivan deck concentration it is possible to recover heavy minerals such as cassiterite at least as fine as 10 microns in size. This appreciable improvement in gravity concentration practice has been substantiated by several full-sized plants.

Jan 1, 1950

By Goerge F. Weaton

Since 1909, when an agreement between Minnesota's Tax Commission and the University of Minnesota's School of Mines was worked out, it has been the annual responsibility of the School to evaluate and classify the iron ore deposits within the State. These unique duties of an academic institution have provided School officials with an excellent view of the past, present and probable future of the mining industry in Minnesota as the average grade of iron ore (excluding taconite) * diminishes while at the same time it competes with beneficiated taconites and foreign high-grade ores for use in America's eastern blast furnaces. SYSTEM OF EVALUATION In the latter part of November of each year, the Mining Division of the Department of Taxation makes a preliminary study of the active mines which the Department wants the School of Mines to review. These are discussed with the engineers of the Ore Estimate Division of the School of Mines and with the mining companies. After these discussions, a list of the mines of each of the major operating companies is submitted to the Ore Estimate Division of the School of Mines with the request that these properties be reviewed by them as of the next assessment date (May 1st). At the same time, a letter is sent to the mining companies requesting that they submit to the Division their own estimates on the selected mines operated by them, together with all computations, drill records, maps and cross-sections. The mining companies are re- quested to send in this information during the first half of the year, and, as far as is possible, they have always complied with this request promptly. Much of this information received by the School of Mines is of a confidential nature and is treated as such.

Jan 1, 1965

By Clyde E. Williams, JAMES L. GREGG

THIS review of the past year's progress in iron and steel metallurgy presents examples of only a few of the interesting or important accomplishments made in the United States. In the field of iron ore concentration increased attention was given to the study of the more difficultly separated wash ores and some progress was made in tabling. One difficulty with the table, in concentrating iron ore where the percentage of concentrate in the feed is large, has been the removal of fine silica from the thick layer .of concentrates in the cleaning zone. One company has -Made an important contribution toward the solution of this problem by an extension of the well-known plateau principle. By a special riffling of the plateau section of the table, the concentrates are crowded together. This action forces the fine silica to the top of the bed in the cleaning zone, whence the cross-flowing currents of water -can wash it into the middling product. Some work has been done on the application of froth flotation to the concentration of iron ores. Laboratory experiments were made at the Colorado School of Mines in which hematite was, successfully floated. Using oleic acid as a frothing and collecting agent and sodium carbonate as the conditioning agent, a high recovery of rich ,concentrate was obtained. A laboratory flotation unit is in use at Taconite, on the Mesabi range, and a commer-

Jan 1, 1932

By F. X. Tartaron

F. C. Bond (Consulting Engineer, Processing Machinery Dept., Allis-Chalmers Manufacturing Co., Milwaukee, Wis.) — Papers such as this one which deal in a lucid manner with the obscure fundamentals of comminution theory are always welcome. The author has attempted to bring together several diverse theories and handles them interestingly. However, some of the ideas expressed and conclusions drawn require critical reviewing, for which amenities alone will not suffice. The author points out that the theoretical energy required to break across crystal lattices is of the order of 1000 times the actual energy required to crush or grind, and that this energy in turn is perhaps 1000 times the measured surface energy of the new surface area produced. The energy required to grind commercially is controlled by flaws and dislocations, rather than by the inner strength of the lattice structure. The measured surface energy is only a slight residue left after the face atoms are adjusted to their new environment. The dislocations in the crystal lattice structure, with a spacing of about O.l,u, or

Jan 1, 1962

By Eugene S. Meieran

The effects of methods of crystal growing, wafer sawing, polishing, routine handling, diffusion, and epitaxial growth on the defects in GaAs are reviewed and studied using reflection and transmission X-ray topographic techniques. In general, it was found that boat-grown crystals exhibited fewer defects than Czochralski crystals, although all crystals showed large numbers of precipitates visible when examined in the electron microscope. Mechanical surface treatments such as sawing and mechanical polishing introduce damage to a depth of about 5 µ, most of which can be removed by suitable chemical or chem-mechanical polishing. In addition, defects can be introduced through routine handling of wafers, for example with metallic tweezers. These defects can be quite severe, and have been observed 20 µ below the wafer surface. Defects can also be introduced through diffusion and epitaxial growth. These defects, which include precipitates, growth pyramids, stacking faults, dislocations, and so forth, can be detrimental to device fabrication. It is shown that wafers or films which appear defect-free optically can contain defects visible in the X-ray topographs. WHILE the use of GaAs in the semiconductor industry has increased very rapidly in the last few years, due mainly to the recent development of many important GaAs devices,1,2 the major limit to the production of commercial quantities of many GaAs devices remains a severe lack of suitable materials technology. This lack is apparent in two critical areas. First, production quantities of high-quality GaAs crystals, reproducibly doped and precipitate-free, simply are not available commercially, although some reasonable quality material is available on a limited first-come, first-serve basis. Second, in comparison to silicon technology, little is known about the effects of processing variables on the defects either present in as-grown GaAs or introduced through processing and handling of wafers. These areas are now receiving some attention from semiconductor device manufacturers, who are studying defects in GaAs in order to better understand how either to prevent their occurrence or to cope with their existence. Most investigations of the defects in GaAs have been made by optical microscopy3-5 or transmission electron microscopy techniques.'-' Recently, however, the imaging techniques of X-ray topography, electron mi-croprobe analysis, and scanning electron microscopy are being applied to the study of GaAs.9-14 In the case of X-ray topography, a one-to-one image is obtained that must be photographically enlarged. In compensa- tion, the defects within entire wafers may be imaged by simple scanning (Lang technique15) if the wafer is reasonably perfect, or by using the scan oscillation technique developed by Schwuttke16 if the wafer is warped or distorted. The purpose of this paper is to both review and extend the general application of X-ray topographic techniques to GaAs. Emphasis will be placed on the effects of growth and process variables on the quality and perfection of both bulk and epitaxial GaAs. Reference to optical or electron microscopy results will be made when useful. Since the effects on defects of a wide variety of processing variables such as crystal growing, sawing, polishing, diffusion, and epitaxial growth will be somewhat superficially reviewed, a fairly extensive bibliography of the most important recent results in these areas is included. However, for completeness, important defects will be illustrated here, although such defects have been previously shown by others. While this paper is concerned with defects rather than with the physics of X-ray scattering, the mechanisms of contrast formation in the topographs will of necessity be briefly mentioned. EXPERIMENTAL GaAs crystals, both boat-grown18 and Czochralski-grown,'8 containing a variety of dopants of various concentrations, were purchased from outside vendors. Wafers were sliced from the crystals using a Hamco ID saw and were mechanically polished using 1 µ diamond paste. Chem-mechanical polishing was done in bromine-methanol as described by Sullivan and Kolb.18 Chemical polishing was done using a modified sulfuric-peroxide solution, 11 parts H2SO4, 1 part 30 pct H2O2, 1 part DI water.5 Zinc diffusion was carried out in a closed tube, using a 10 pct Zn-In source at 825°C for 1 hr. Oxide masking techniques were used to select the area to be diffused. Epitaxial wafers were either purchased or prepared here. All epitaxial runs prepared here were carried out using a Ga-GaAs-AsC13 source in a closed tube at a substrate temperature of 750°C. Wafers were chem-mechanically polished and gas-etched prior to deposition. The X-ray topographs were taken on a Krystallos Lang camera, operating in the transmission scanning geometry (Lang technique15) or in the reflection scanning geometry (modified Berg-Barrett technique20,21). MoKa, radiation was used for all transmission topographs using a Jarrell-Ash 100-µ spot focus. CuKal radiation was used for all reflection topographs using a General Electric CA-7 1-mm spot focus X- ray tube. Topographs were printed from an intermediate contrast inversion film, so the contrast shown in all figures here is the same as that of the original 50-µ-thick emulsion L4 Iiford nuclear plate used to record the topograph.

Jan 1, 1969

By CHRIS A. HARTNAGEL

For the second consecutive year, the production of crude petroleum in New York has fallen below the 5,000,000-bbl. Mark that had prevailed previously since 1937. In 1945, the output totaled 4,658,000 bbl., a decrease of slightly more, than one per cent from the 1944 production. This total represents 2 per cent of the stripper-well production of the United States, which in turn is I 3 per cent of the total annual yield of the nation's petroleum.

Jan 1, 1946

By James P. Kimball

Jan 1, 1885

By AIME AIME

FEW indeed are the sections of the country where trained or partly trained workers have not already been hired by a war industry plant or will be within the near future. Yet right in the midst of the heavily industrialized East lies the anthracite area, home of a million people, whose productive power has persistently been by-passed either by private industry or by the Government Plant Site Board. The chief reason given for not locating war plants in the area is that it is not within the strategic zone, but in numerous instances elsewhere this rule has been waived. Furthermore, the anthracite region is well protected on all sides by mountains and is at all points more than 100 miles inland. Continued depression in the anthracite industry and a crippling blow dealt by the war emergency to the production of silk and rayon goods, the chief manufacturing activity of the area, have resulted in a heavy migration, particularly of trained young workers, into near-by industrial areas. At least 50,000 people are currently unemployed, with the likelihood of an increase in coming months, and as many families are on relief.

Jan 1, 1942

By E. V. Daveler, Frank L. Antisell

CERTAIN physical and chemical properties of copper are so intimately related that a change in variation of the physical properties indicates a certain chemical change. The standard specifications of copper of the American Society for Testing Materials are based upon physical characteristics with one exception, namely, the copper contents. Certain phenomena of the surface indicate the adaptability of the metal for forging or rolling. The writer believes that it is much simpler to produce shapes that are metallurgically correct than those that are mechanically satisfactory. The appearance of the surface of the copper when cooled is considered as to its "pitch," or the general contour of the surface, and the "set," or the decail appearance of the surface of the shape. The set of the copper is, in a very large measure, directly related to the pitch; and so intimately are these characteristics connected that they are often used as synonymous terms by the refiner when he is speaking of well-refined copper. Oxygen is often spoken of as a medicine for copper, it being used to regulate the pitch.

Jan 1, 1920

Jan 1, 1923

Jan 1, 1923

By Gene D. Clayton, Robert R. Dimock

A time-consuming and expensive preshearing program to minimize the adverse effects of blasting on slope stability at Kennecott Copper Corp.'s Ruth Pit in east-central Nevada has been eliminated in favor of down-the-hole, nonelectric delayed blasting which can produce a smooth wall effect and improve blast fragmentation. The new blasting approach resulted from a Kennecott engineering investigation aimed at improving the stability of the extremely variable rock conditions found throughout the pit by reducing the vibrational energy imparted to the walls with conventional bench blasts.

Jan 4, 1977

By John G. McLain

OF all the zinc that the world consumed in 1936-'38 the United States took about 31 per cent, and almost 14 per cent of the world's zinc supply in that period was used for galvanizing purposes in the United States. Further examination of the statistics shows that about 71/2 per cent (147,500 tons in 1939) of the world zinc consumption goes into the galvanizing of sheets in the United States, which is what I am going to talk about in this paper. There is nothing especially new about galvanizing; in every year since 1921 somewhere between 41 and 49 per cent of the country's zinc consumption has been used for this purpose, and yet few people not specialists in its manufacture know much about how it is made. You take an iron or steel sheet and dip it in molten zinc and there you have a galvanized sheet-that about epitomizes popular knowledge of the subject even among engineers.

Jan 1, 1941